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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority from U.S. Provisional Application 60/657,675 having a filing date of Mar. 1, 2005, the contents of which are hereby incorporated by reference in their entirety.
TECHNICAL FIELD
[0002] This invention relates to a dryer seal and more particularly to a dryer seal providing a bearing surface to support the drum. The seal is adapted to be suitable for meltable bonding to an underlying surface such as a portion of a forward air duct thereby providing a bearing seal that both supports the drum and blocks undesired air flow.
BACKGROUND OF THE INVENTION
[0003] Automatic clothes dryers typically include a housing (also known as a bulkhead) and a rotating drum supported within the housing. It is known to use seal elements in the form of rings of felt which may be disposed between the housing and the drum so as to bear against the drum as it rotates. The use of a sealing element is desirable to prevent air leakage between the drum and the clothes dryer cabinet which could detrimentally affect the air flow system of the dryer.
[0004] It is known to utilize seals in the form of ring structures of fibrous material adhesively bonded to a supporting structural member so as to block undesired air flow. While such structures may be effective in blocking the air flow, their assembly utilizing adhesives may be problematic due to the need for precision placement in order to meet tight tolerances. Moreover, over time and exposure to heat, the adhesives may begin to degrade thereby causing a loss of efficiency.
SUMMARY OF THE INVENTION
[0005] This invention provides advantages and/or alternatives over the prior art by providing a dryer seal of multi-layer construction having a low friction bearing layer for disposition in contacting relation with a portion of the dryer drum and an underlying melt bonding layer adapted to be meltably attached to an underlying support surface within the dryer. The combination of the two layers provides an effective seal providing bearing support to the drum while eliminating the need for adhesives to hold the seal in place.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] The following drawings which are incorporated in and which constitute a part of this specification illustrate an exemplary embodiment of the present invention and, together with the general description above and the detailed description set forth below, serve to explain the principles of the invention wherein:
[0007] FIG. 1 is a perspective view of an exemplary clothes dryer with the rotating drum and seal illustrated in phantom; and
[0008] FIG. 2 is an exploded cut-away view of a dryer with the seal arranged for mounting with the seal at the interior of the drum; and
[0009] FIG. 3 is a view illustrating the ring configuration of the seal.
[0010] While the invention has been generally described above and will hereinafter be described in connection with certain potentially preferred embodiments and procedures, it is to be understood and appreciated that in no event is the invention to be limited to such illustrated and described embodiments and procedures. On the contrary, it is intended that the present invention shall extend to all alternatives and modifications as may embrace the broad principles of this invention within the true spirit and scope thereof.
DESCRIPTION
[0011] Reference will now be made to the various drawings wherein to the extent possible like reference numerals are utilized to designate corresponding components throughout the various views. In FIGS. 1 and 2 , there is illustrated a dryer 10 including a cabinet body 12 housing a heated rotating drum 14 . As illustrated, the cabinet body includes a door opening 16 for loading clothing articles into the mouth of the drum 14 . The door opening 16 may be closed by means of a door 18 .
[0012] As shown, a seal 30 in the form of a ring is disposed at a position within the forward portion of the dryer drum 14 thereby providing support between the drum 14 and a supporting structural member 32 such as a flange or the like while also blocking undesired air flow from the drum 14 into the surrounding cabinet 12 . As shown, the seal 30 has a first or inner layer 36 arranged to be secured to the supporting structural member 32 . The seal 30 also includes an outer layer 38 arranged to define a support surface for the drum 14 . The seal 30 may also include various intermediate layers if desired. The layers may be joined to one another by needling such that fibers from the adjacent layers are intermingled into a cohesive structure at the interface.
[0013] The inner layer 36 defines the interior of the seal 30 and is preferably formed of a meltably bondable material that can be welded to the supporting structural member 32 by techniques such as ultrasonic welding, RF welding, vibration welding and the like thereby eliminating the need for adhesives. One suitable material for the underlying layer 36 is believed to be a polypropylene based material such as a medium density polypropylene based felt. Such materials have similar melt temperatures to polypropylene structural members thereby facilitating adhesion. Of course, other suitable materials that can be meltably bonded to the supporting structural member 32 may likewise be utilized if desired.
[0014] The outer layer 38 preferably provides a relatively low coefficient of friction with the supported drum while nonetheless retaining its structural integrity under heated conditions. It has been found that a wool/polyester blend needled felt may be particularly suitable. However, other materials may likewise be utilized if desired.
[0015] If desired, it is also contemplated that the layers can be reversed such that the polypropylene layer may be bonded in sealing attachment to an interior portion of the drum 14 . The wool layer would then ride on the structural member.
[0016] The structure of the present invention provides excellent load bearing performance thereby eliminating the need for rollers, glides and the like. In addition, it provides sealing performance without the need for adhesive attachment.
[0017] While the present invention has been illustrated and described in relation to certain potentially preferred embodiments and practices, it is to be understood that such embodiments and practices are illustrative and exemplary only and that the present invention is in no event to be limited thereto. Rather, it is contemplated that modifications and variations to the present invention will no doubt occur to those of skill in the art upon reading the above description and/or through a practice of the invention. It is therefore contemplated and intended that the present invention shall extend to all such modifications and variations which incorporate the broad principles of the present invention within the full spirit and scope thereof.
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A dryer seal. The seal includes a first layer of fibrous material adapted to be disposed in contacting relation with a rotating dryer drum and at least one underlying layer held in melt bonded relation to a support structure.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to an air filter shaping mold, particularly to one having excellent efficiency in processing, provided with less components and able to form an air filter with one round of processing.
[0003] 2. Description of the Prior Art
[0004] A conventional air filter shaping mold, as shown in FIG. 1 , includes an upper, an intermediate and a lower mold base 11 , 12 and 13 combined together. The upper and the lower mold base 11 , 13 respectively and correspondingly have plural projecting separating plates 111 , 131 provided spaced apart equidistantly and interposing each other, and the intermediate mold base 12 is formed with a through cavity 121 in the center. After combined together, the intermediate mold base 12 is firmly sandwiched between the upper and the lower mold base 11 , 13 , and the projecting separation plates 111 , 131 of the upper and the lower mold base 11 , 13 are positioned in the cavity 121 of the intermediate mold base 12 .
[0005] To integrally form an air filter 14 by means of the conventional shaping mold 10 , the intermediate mold base 12 is first assembled closely on the lower mold base 13 , and then a plane filter cotton sheet 141 is placed on the upper side of the lower mold base 13 . Next, the upper mold base 11 is closely compressed on the intermediate and the lower mold base 12 , 13 , and simultaneously, the projecting separating plates 111 , 131 of the upper and the lower mold base 11 and 13 are arranged interposing each other to compress the filter cotton sheet 141 into continuous curves spaced apart equidistantly. Subsequently, raw material of rubber is poured into the cavity 121 of the intermediate mold base 12 by an injection device through the pouring passage 15 and the pouring gate 16 of the upper mold base 11 to form a gelatin frame 142 covering up the outer circumferential edge of the filter cotton sheet 141 . Lastly, the upper, the intermediate and the lower mold base 11 , 12 , 13 are orderly separated from one another and the finished product of an air filter 14 is removed out and then the intermediate mold base 12 is again assembled on the lower mold base 13 , thus obtaining an integrally formed air filter.
[0006] Although the conventional air filter-shaping mold 10 can integrally form an air filter 14 , yet the forming process is too complicated and inconvenient, and substantially the finished products are imperfect in quality. The reasons for these drawbacks are described below.
[0007] 1. To integrally form an air filter, it is necessary to use the upper, the intermediate and the lower mold base 11 , 12 and 13 at the same time, wasting much labor and time in making molds and much cost on material. Besides, in a forming process, precision of combination of the three mold bases must be taken into consideration, because it may greatly influence the external appearance of finished products.
[0008] 2. In a forming process, the filter cotton sheet 141 is directly made into continuous curves by the projecting separation plates 111 , 131 of the upper and the lower mold base 11 and 13 . Nevertheless, the upper and the lower mold base 11 , 13 are fixed on the injection device which has no auxiliary apparatus for fixedly positioning the filter cotton sheet 141 ; therefore the filter cotton sheet 141 may deflect and shift sideways when the upper mold base 11 is closely assembled on the lower mold base 13 . If the filter cotton sheet 141 is excessively deflected, its outer end 143 may shrink inward and fail to be bonded with the frame 142 , possible to render the entire filter cotton sheet 141 inclined on one side and hence influence the quality of products.
SUMMARY OF THE INVENTION
[0009] The objective of the invention is to offer an air filter-shaping mold composed of an upper and a lower mold base. The lower mold base is formed with a plurality of projecting separating plates, and a filter material of a preset shape is positioned on these separating plates for carrying out forming of an air filter, saving labor and time in making molds and cost on material, positioning the filter material precisely and stabilizing quality of products.
BRIEF DESCRIPTION OF DRAWINGS
[0010] This invention will be better understood by referring to the accompanying drawings, wherein:
[0011] FIG. 1 is a partial exploded perspective view of a conventional air filter-shaping mold:
[0012] FIG. 2 is a cross-sectional view of the conventional air filter-shaping mold having its three mold bases combined together:
[0013] FIG. 3 is a cross-sectional view of the conventional air filter-shaping mold having its three mold bases opened and separated:
[0014] FIG. 4 is an exploded perspective view of a first preferred embodiment of an air filter-shaping mold in the present invention:
[0015] FIG. 5 is a partial perspective view of the first preferred embodiment of the upper mold base of the air filter-shaping mold in the present invention:
[0016] FIG. 6 is a partial exploded and cross-sectional view of the first preferred embodiment of the air filter-shaping mold in the present invention:
[0017] FIG. 7 is a cross-sectional view of the first preferred embodiment of the air filter-shaping mold in the present invention, showing two mold bases combined together:
[0018] FIG. 8 is a cross-sectional view of the first preferred embodiment of the air filter-shaping mold in the present invention, showing the two mold bases combined together and poured therein with raw material of rubber:
[0019] FIG. 9 is an exploded and cross-sectional view of the first preferred embodiment of the air filter-shaping mold in the present invention, showing the two mold bases opened and separated after an air filter is formed:
[0020] FIG. 10 is a perspective view of the air filter formed by the air filter-shaping mold of the first preferred embodiment in the present invention: and
[0021] FIG. 11 is a partial cross-sectional view of a second preferred embodiment of an air filter-shaping mold in the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0022] A first preferred embodiment of an air filter-shaping mold in the present invention, as shown in FIGS. 4, 5 and 6 , includes an upper mold base 20 and a lower mold base 30 combined together.
[0023] The upper mold base 20 is a rectangular body having its lower side bored with an upper cavity 21 of a preset depth. The cavity 21 has its bottom side formed with a plurality of triangular separating plates 211 protruding downward and spaced apart equidistantly, and between every two separating plates 211 is formed a triangular upper accommodating groove 212 . An annular groove 213 of a preset width is formed between all the separating plates 211 and the circumferential edge of the upper cavity 21 and has plural through pouring holes 214 bored at preset locations in an upper surface and communicating to the topside of the upper mold base 20 . The upper mold base 20 further has its upper surface bored with plural pouring passages 215 communicating with one another and with the pouring holes 214 to pour raw material therein and guide it to get into and fill up the annular groove 213 through the pouring holes 214 , with some pouring gates 214 positioned close to the four corners of the annular groove 213 . Besides, the upper mold base 21 has four combining hole 216 respectively provided at four corners of the bottom.
[0024] The lower mold base 30 to be assembled with the bottom side of the upper mold base 20 is bored in the upper side with a lower cavity 31 having its bottom formed with a plurality of triangular separating plates 311 protruding upward and spaced apart equidistantly, and between every two separating plates 311 is formed a triangular lower accommodating groove 312 . Thus, when the upper and the lower mold base 20 , 30 are combined together, the separating plates 211 , 311 of the upper and the lower mold base 20 and 30 can be interposed with one another and positioned in the accommodating grooves 312 , 212 of the lower and the upper mold base 30 , 20 . In addition, an annular groove 313 of a preset width is formed between all the separating plates 311 and the circumferential edge of the lower cavity 31 . The annular groove 313 of the lower cavity 31 is formed with an arc-shaped surface and matches with the annular groove 213 of the upper cavity 21 . The lower mold base 30 further has four combining studs 314 respectively fixed at four corners of the upper surface to be respectively inserted in the four combining holes 216 of the upper mold base 20 .
[0025] To carry out forming of an air, as shown in FIGS. 6 and 7 , the air filter shaping mold is installed on an injecting device in advance, and a filter material 41 formed in advance with continuous saw teeth is deposited on the separating plates 311 of the lower cavity 31 , and then the upper and the lower mold base 20 , 30 are combined together. At this time, the separating plates 211 in the upper cavity 21 and the separating plates 311 in the lower cavity 31 are interposed with one another to clamp and compress the filter material 40 . Then, as shown in FIG. 8 , raw material of rubber is poured into the annular grooves 213 , 313 of the upper and the lower cavity 21 , 31 through the pouring passages 215 and the pouring holes 214 by the injection device, and the raw material of rubber is then covered on and bonded with part of the circumferential edge of the filter material 41 to form the outer frame 42 of an air filter 40 . After finishing pouring the raw material into the annular grooves 213 , 313 and forming the frame 42 of an air filter, the upper and the lower mold base 20 , 30 are opened and separated, and the finished product of an air filter 40 is removed out, thus finishing forming integrally an air filter 40 having a great strength and stable quality, as shown in FIGS. 9 and 10 .
[0026] The filter material 41 in the first preferred embodiment is composed of a filter fabric 411 and metallic gauze 412 . The filter fabric 411 is a non-woven fabric or cotton cloth having function of air filtering, and the metallic gauze 412 is covered on the surfaces of the filter fabric 411 so as to strengthen the whole structure of the filter material 41 . In addition, the filter material 41 can be metallic gauze made of stainless steel or a filter fabric or the like to meet different demands of customers. Furthermore, the annular groove 313 of the lower cavity 31 of the lower mold base 30 is formed with an arc-shaped surface; thus, after the frame 42 of an air filter 40 is formed, its upper edge can be formed with a current guiding surface 421 of a preset radian, which is able to smoothly guide air to move downward and pass through the filter material to be filtered, able to decrease reflected current of air and increase quantity of air sucked into the engine for use, as shown in FIG. 9 .
[0027] A second preferred embodiment of an air filter shaping mold in the present invention, as shown in FIG. 11 , includes an upper and a lower mold base 20 , 30 combined together. The upper and the lower mold base 20 , and 30 are respectively formed inside with a plurality of pillar-shaped separating plates 211 a , 311 a having their ends respectively formed with an arc-shaped surface, and between every two pillar-shaped separating plates 211 a , 311 a is formed a pillar-shaped groove 212 a , 312 a . And a filter material 41 a is formed with continuous curves to match with the pillar-shaped separating plates 211 a , 311 a . Although the shapes of the separating plates and the accommodating grooves in the second preferred embodiment are different from those in the first preferred embodiment, yet these two kinds of air filter shaping molds have equal effect in forming of a high-quality air filter.
[0028] To sum up, this invention has the following advantages.
[0029] 1. The air filter shaping mold in the invention can form an air filter with one round of processing only by employing an upper and a lower mold base, having fewer components than the conventional air filter shaping mold and hence able to save cost on molds and material.
[0030] 2. The air filter shaping mold in the invention only includes an upper and a lower mold base; therefore in the forming process of an air filter, these two mold bases can be combined or opened and separated quickly and conveniently, greatly elevating production efficiency.
[0031] 3. The filter material is formed in advance with continuous curves to match with the curved separating plates in the upper and the lower cavity; therefore the filter material can be quickly and stably positioned in the cavities to prevent it from deflecting and shifting sideways when the two mold bases are combined together, able to make the filter material and the frame bonded together precisely to enhance quality of products.
[0032] While the preferred embodiments of the invention have been described above, it will be recognized and understood that various modifications may be made therein and the appended claims are intended to cover all such modifications that may fall within the spirit and scope of the invention.
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An air filter-shaping mold includes an upper and a lower mold base combined together. The upper and the lower mold base are respectively formed with plural curved separating plates. A filter material having the same shape as the separating plates is placed on the separating plates of the lower mold base for carrying out forming of an air filter, able to save labor and time in making molds and cost on material, to position the filter material precisely, to elevate production efficiency and to stabilize quality of products.
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TECHNICAL FIELD
[0001] The present invention relates generally to computer systems, and more specifically to providing access to computer resources over a computer network such as the Internet.
BACKGROUND OF THE INVENTION
[0002] The architecture of computer networks has changed dramatically over the last several decades. In the seventies and early eighties, probably the most prevalent architecture was the mainframe architecture in which a very powerful mainframe computer contained all processing and storage power and users accessed the mainframe via so called “dumb” terminals, which had no processing power and acted merely as user interfaces to the mainframe. The mainframe architecture is prone to system failures because all processing power is located in the powerful mainframe computer, and while the mainframe computer is down no users can access the system. In the eighties, advancements in semiconductor technology enabled significant processing power to be placed on a user's desktop in the form of a personal computer. Consequently, the predominant computer network architecture defaulted into a distributed architecture, with a number of personal computers being interconnected via a communications network, such as a local area network. Under this type of architecture, each personal computer was able to share resources with the other computers, but many resources, such as application programs, were primarily stored and run independently on each personal computer, due, in part, to bandwidth limitations of communicating over the network.
[0003] In today's computing environment, the Internet forms part of a Global Communications Network that interconnects millions of computers via the client-server network architecture. In the client-server architecture, servers are powerful computers dedicated to managing network resources, and clients are personal computers or workstations that run application programs and rely on servers for computer resources such as files and even processing power. The client-server architecture has become a viable network architecture due in part to the dramatically increased bandwidth provided by the communications infrastructure forming the backbone of the Internet, as will be appreciated by those skilled in the art. The distributed processing power between the client and server systems has led to a myriad of third parties that provide software services to a number of users over the Internet or other wide area network. These third parties are known as Application Service Providers (“ASPs”) and they allow users to access software services provided by the ASPs by accessing a server maintained by the ASP over a suitable communications network. FIG. 1 is a functional block diagram illustrating a conventional ASP system 100 including a client computer system 102 that accesses an ASP server computer system 104 over a communications network 106 , which may be the Internet or other suitable communications network. The client computer system 102 accesses the server computer system 104 to utilize the specific software services provided by the server computer system, which may be simply downloading a desired application program or supplying input to an application running on the server computer system to obtain desired data, as will be described in more detail below.
[0004] In the example of FIG. 1, the client computer system 102 includes a browser 108 that sends Hypertext Transfer Protocol (“HTTP”) requests to the server computer system 104 over the communications network 106 . In response to the applied requests, a server engine 110 on the system 104 processes the requests and provides files to the client computer system 102 such as Web pages 112 and client application programs 114 . The client application programs 114 are shown as including a number of individual application programs AP1-APN, each of which may be independently selected and transferred to the client computer system 102 . The application programs 114 are an example of one type of computer resource that an ASP provider may make available to users, as will be appreciated by those skilled in the art. The Web pages 112 function as the client interface to the ASP server computer system and allow the client computer system 102 to, among other things, select which ones of application programs 114 are to be transferred.
[0005] In operation, a user of the client computer system 102 accesses the ASP server computer system 104 and typically provides a request that includes various user information, such as user name, credit information, and which ones of the client application programs 114 the user desires to access. The server engine 110 processes the request, which includes verifying the user's credit, and thereafter transfers the selected application programs 114 to the client computer system 102 . The user of the client computer system 102 thereafter utilizes the transferred application programs 114 as desired.
[0006] Depending on the type of service been provided by the ASP server computer system 104 , the transferred application programs 114 may correspond to either the entire executable application program including all required system files, such as any required dynamic link library files, or may be an application “stub” or module containing only a portion of the application. When the entire executable application program 114 is transferred, the user simply opens this program as he would any other programs stored on the system 102 and need not be connected to the server computer system 104 when using the application program. This situation may be termed a broken-connection mode of operation because the client computer system 102 and server computer system 104 are not communicating when the application program 114 is being run. In contrast, when an application module is transferred to the client computer system 102 , upon opening this module the application is initiated and the server computer system 104 is contacted and thereafter communicates with the client computer system to execute the application program. This situation may be termed a continuous-connection mode of operation because the client computer system 102 and server computer system 104 are communicating when the application program 114 is being run.
[0007] The user of the client computer system 102 must, of course, pay for the application programs 114 provided by the server computer system 104 . Typically, the user pays for the application programs 114 in one of two ways. In the broken-connection situation, a user typically pays as he goes, meaning that the user simply pays for each application program 114 downloaded to the client computer system 102 . In the continuous-connection situation, the user typically pays via a subscription agreement, allowing the user to pay a periodic subscription fee and obtain access to the services provided by the ASP server computer system 104 . A user is typically assigned a username and password, which the user supplies to gain access to the application programs 114 corresponding to his subscription agreement.
[0008] Each of the broken-connection and the continuous-connection situations has drawbacks, both from the user's and ASP's perspectives. When a user downloads an application program 114 to the client computer system 102 , the user may thereafter use the program on multiple computer systems and provide copies of the program to other users. While the terms of the license under which the user agrees to use the application program 114 may proscribe such conduct, the user may nonetheless take such action. In the continuous-connection environment, the user must connect to the server computer system 104 to run the selected application program 114 , and this connection can dramatically slow the operation of the program, such as when the server computer system 104 has a large number of client computer systems 102 requesting service. Moreover, although a subscription agreement may be limited to a single user and a single machine, a user may provide his password to others, enabling other users to access the computer resources.
[0009] There is a need for providing users access to computer resources offered by ASPs that overcomes at least some of the shortcomings of the existing ASP systems.
SUMMARY OF THE INVENTION
[0010] According to one aspect of the present invention, a method for providing access to computer resources on a computer system includes generating a token containing encrypted user information including credit, authorization, and authentication information. A request is initiated to open an encrypted computer resource stored on the computer system, and execution of a remote application manager component on the computer system is also initiated. Under the control of the remote application manager component, the token is decrypted and a user of the computer system is authenticated using authentication information stored in the token. Whether the user is authorized to use the requested computer resource using authorization information stored in the token is then verified, as is whether the user has sufficient credit contained in the token to use the requested computer resource using credit information stored in the token. When the user is authenticated, authorized, and has sufficient credit, the requested computer resource is decrypted and opened. Use of the computer resource is then monitored to determine whether the user has sufficient credit to continue using the computer resource. A notification is provided when the monitored usage of the opened computer resource has exceeded the credit. The computer system on which the above method is executed may be a client system.
[0011] According to another aspect of the present invention, a server system receives client requests from client computers, such client requests including authorization, authentication, and credit information, and verifies credit information contained in such requests. When the credit of a user is verified, the server system generates the token containing the associated user information. The server system also selects computer resources using information contained in the client requests and encrypts each selected computer resource. The server system transfers to the client system the token and the encrypted selected computer resources along with the remote application manager component. The server system may thereafter update credit information and authorization information in response to client request from the client system, and provide the client system with an updated token and updated selection of computer resources.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 is a functional block diagram of a conventional client-server system in which an application service provider server supplies services to the client system.
[0013] [0013]FIG. 2 is a functional block diagram illustrating a client-server system in which an application service provider server supplies services to client systems according to one embodiment of the present invention.
[0014] [0014]FIG. 3 is a diagram illustrating one embodiment of the token of FIG. 2.
[0015] [0015]FIG. 4 is a flow diagram illustrating in the operation of the remote application manager component of FIG. 2 in more detail.
DETAILED DESCRIPTION OF THE INVENTION
[0016] [0016]FIG. 2 is a functional block diagram illustrating an ASP system 200 according to one embodiment of the present invention. The ASP system 200 includes an ASP server computer system 202 and client computer systems 204 and 206 that allow an Application Service Provider operating the server computer system to provide computer resources to users in both the broken-connection and continuous-connection environments with reduced concern of unauthorized use and transfer of such computer resources, as will be described in more detail below. In the following description, certain details are set forth to provide a sufficient understanding of the invention. However, it will be clear to one skilled in the art that the invention may be practiced without these particular details. In other instances, well-known components, concepts, and details such as timing and other common software operations have not been shown in detail in order to avoid unnecessarily obscuring the invention.
[0017] The client computer systems 204 and 206 communicate with the server computer system 202 over communications links 208 and 210 , respectively. The communications links 208 and 210 are illustrated separately to depict a continuous-connection environment via the link 208 and a broken-connection environment via the link 210 , and each link corresponds to any of a variety of communications networks, such as the Internet, Local Area Networks, Wide Area Networks, a wireless network using the Wireless Application Protocol, and the like, as will be appreciated by those skilled in the art.
[0018] The server computer system 202 includes a client interface component 212 that processes requests received from the client computer systems 204 , 206 and communicates with other components on the server computer system to provide the client computer systems with responses to such requests. An accounting and billing component 214 receives credit and billing information from the client interface component 212 and processes such information to verify a user's credit and bill the user for his use of the selected computer resources. A plurality of application programs 216 are stored on the server computer system 202 , and correspond to one type of computer resource that may be supplied to the client computer systems 204 , 206 . The client interface component 212 selects particular ones of application programs 216 in response to corresponding client requests, encrypts the selected application programs, and provides the encrypted application programs to the client computer systems 204 , 206 . A token generation component 218 receives user information from the client interface component 212 and generates a token 220 using this information, where the token corresponds to a binary file containing encrypted user information, as will be described in more detail below. A key generation component 222 is responsible for generating encryption keys for use by the client interface component 212 in encrypting application programs 216 and the token generation component 218 in encrypting information. The key generation component 222 may utilize any of a variety of encryption methodologies in generating the encryption keys, and in one embodiment utilizes the Public Key encryption methodology to obtain public-private key pairs.
[0019] Each of the client computer systems 204 and 206 includes a number of components that have been downloaded from the server computer system 202 . The client computer system 204 includes the token 220 and a plurality of application modules AM1-AMN, each application module being an encrypted file corresponding to a selected application program 216 on the server computer system 202 . A remote application manager component 224 operates as a supervisory component to decrypt the token 220 and verify that a user is permitted to use a particular application module AM1-AMN, and thereafter decrypts the corresponding application module to enable the user to utilize the application module, as will be discussed in more detail below. The client computer system 204 is also shown as including a phantom application 226 , which corresponds to an object which, when opened, initiates execution of corresponding application program stored on the server computer system 202 . The phantom application 226 is thus similar to the application modules AM1-AMN except that no portion of the application program is actually stored on the client computer system 204 . The client computer system 204 may contain any combination of application modules AM1-AMN and phantom applications 226 .
[0020] The client computer system 206 also includes the token 220 and remote application manager component 224 , along with a plurality of application programs AP1-APN, each application program being an encrypted file corresponding to a selected program 216 on the server computer system 202 . Each application program AP1-APN is a complete executable program including any necessary system files, as previously discussed with reference to FIG. 1. The remote application manager component 224 once again operates as a supervisory component to decrypt the token 220 and verify that a user should be permitted to use a particular application program AP1-APN, and thereafter decrypts the corresponding application program to enable the user of the client computer system 206 to utilize the application program.
[0021] In one embodiment, the client computer system 206 includes a card reader 226 that is adapted to receive a “smart card” 228 on which the token 220 is stored. The card reader 226 reads the token 220 stored on the smart card 228 and provides the token to the remote application manager component 224 . The smart card 228 may be any type of compact card on which the token 220 may be stored, such as a true smart card containing embedded intelligence and memory, a credit card, an ATM card, and the like. The use of the smart card 228 enables a user to utilize multiple client computer systems to access the server computer system 202 , and also provides added security in that presumably only the authorized user will be in possession of the smart card. Although the card reader 226 and smart card 228 are shown connected to the client computer system 206 , they could also be utilized in the client computer system 204 .
[0022] The specific type of user information stored in the token 220 aids in understanding the overall operation of the ASP system 200 , and thus, before describing such overall operation, the token 220 will be described in more detail with reference to FIG. 3. FIG. 3 illustrates one embodiment of the token 220 which, as previously mentioned, corresponds to an encrypted binary file containing a variety of user information. In the example of FIG. 3, the user information is stored in a number of fields within the token 220 . Starting from the leftmost side of the token 220 , the token includes a plurality of authentication fields 300 that are utilized to ensure that only a particular user may access the associated computer resources. As will be understood by those skilled in the art, authentication is a process of identifying an individual to ensure that an individual is who he claims to be, and this is to be distinguished from authorization, which is a process of granting individuals access to specific computer resources based on their identity (i.e., their authentication).
[0023] In the embodiment of FIG. 3, the first authentication field 300 is a hardware tag field 302 containing information about the specific client computer system 204 , 206 on which the associated computer resources may be utilized. The hardware tag field 302 may, for example, correspond to a processor identification number of the microprocessor running on the client computer system 204 , 206 . Recall that the token generation component 218 on the server computer system 202 generates the token 220 , and thus during initialization appropriate information for generating this tag is transferred from the client computer system 204 , 206 to the server computer system. The second authentication field 300 is a user identification field 304 containing information such as a user's name, address, telephone number, and so on, to provide additional information for authenticating the user. The final illustrated authentication field 300 is a user Pretty Good Privacy (“PGP”) key 306 that references information contained on the server computer system 202 and in this way provides further user authentication since even if someone were to obtain the information in the fields 302 , 304 they should would not typically know the PGP key 306 . The PGP technique for encrypting messages is based on the public-key method and will be understood by those skilled in the art.
[0024] A maintenance field 308 includes a user timestamp 310 corresponding to the time on the client computer system 204 , 206 when the token 220 was generated. A server timestamp 312 stores the time on the server computer system 202 when the token 220 was generated. These timestamps 310 , 312 ensure that the duration for which a user accesses a computer resource may be accurately tracked. An authorization field 314 includes an application identification field 316 that includes an application identification number for each application program the user is authorized to use. The application identification number is a unique number associated with each application program, as will be appreciated by those skilled in the art. An application authorization level field 318 stores information regarding particular authorization levels for each authorized application (i.e., each application identification stored in the field 312 ). Each authorized application may have a number of different authorization levels, and which authorization level a particular user has is stored in the field 318 .
[0025] An accounting field 320 includes a use credit field 322 containing a value corresponding to the time for which a user may utilize the associated computer resources, and a use value field 324 corresponding to the time for which the user has actually utilized the computer resources. The difference between the fields 322 and 324 yields the time remaining for the user to utilize the computer resources. The fields 322 , 324 may contain values corresponding to different ways of measuring a user's use of the computer resources. For example, instead of the duration for which the resource is used, the fields 322 , 324 could include integer values, with the field 322 having a value indicating how many times a user is allowed to access the computer resource and the field 324 indicating how many times he has accessed the resource. In this way, the number of times the user may access the computer resource is limited, regardless of how long he accesses the resource each time. Other methods for measuring a user's use of the computer resource may also be utilized, as will be appreciated by those skilled in the art. The token 220 may further include additional fields 326 containing various other information such as error detection and correction fields, as will be understood by those skilled in the art.
[0026] The overall operation of the ASP system 200 will now be described in more detail. Initially, the client computer systems 204 , 206 contact the server computer system 202 to establish service with the Application Service Provider. In the following example, it is assumed the client computer system 206 has contacted the server computer system 202 . The client interface component 212 handles this interface with the client computer system 206 , and may, for example, provide Web pages to the client computer systems allowing users to supply billing, credit, and personal information, as well as information about the computer resources the user desires to access, in addition to any other information the server computer system 202 desires to collect. The client interface component 212 thereafter supplies billing and credit information to the accounting in billing component 214 which, in turn, verifies the user's credit and establishes billing records. If the user's credit is declined, the component 214 notifies the client interface component 212 , which then notifies the client computer system 206 . The component 214 similarly notifies the client interface component 212 when the user's credit is approved, and the following discussion assumes the credit has been approved.
[0027] The client interface component 212 supplies the user information to be contained in the token 220 to the token generation component 218 , and activates the key generation component 222 to generate an encryption key to be utilized for the client computer system 206 being processed. The token generation component 218 thereafter encrypts the user information received from the client interface component 212 using the encryption key to thereby generate the token 220 . The client interface component 212 uses the key to encrypt the application programs 216 corresponding to the selected application programs contained in the supplied user information. At this point, the client interface component 212 transfers the token 220 , the encrypted application programs 216 (designated application programs AP1-APN on the client computer system 206 ), and the remote application manager component 224 to the client computer system 206 .
[0028] When the user of the client computer system 206 attempts to open one of the transferred application programs AP1-APN, the remote application manager 224 operates in combination with the token 220 and the selected application program to provide the user access to the selected program. The process executed by the remote application manager component 224 will be described in more detail with reference to the flow diagram of FIG. 4. In step 400 , the user attempts to open the selected application program AP1-APN, which initiates execution of the remote application manager 224 and the process proceeds immediately to step 402 . In step 402 , the process determines whether the selected application program is loaded on the client computer system 206 . The Application Service Provider may load menus onto the client computer system 206 during the initialization process, and such menus may indicate all application programs AP1-APN provided by the Application Service Provider, regardless of whether the client computer system 206 is authorized to use such programs. When the determination in step 402 is negative, the process goes to step 404 , contacts the server computer system 202 , and steps the user through a process by which the user may gain access to the selected application program AP1-APN. This process would include the server computer system 202 transferring the encrypted application program to client computer system 206 .
[0029] Once step 404 is complete or if the determination in step 402 is positive, the process goes to step 406 and decrypts the token 220 . The process then goes to step 408 and examines the contents of the decrypted token component 224 to determine whether the selected application is authorized for use. When the determination in step 408 is positive, the process goes immediately to step 410 and decrypts and executes the selected application program. From step 410 , the process goes to step 412 and monitors the use of the selected application program. The process then goes to step 414 and determines whether the credit contained in the token 220 has expired. When the determination in step 414 is negative, the process proceeds to step 416 and determines whether the user has indicated a desire to stop running the selected application program. When the determination in step 416 is negative, the process goes back to step 412 and continues executing steps 412 and 414 to monitor the use of the selected application program AP1-APN and ensure that the user has sufficient credit to continue using the program. When the determination in step 416 is positive, indicating the user desires to stop running the selected application program, the process goes immediately to step 418 and the selected application program is once again encrypted along with the token 220 . From step 418 the process goes to step 420 and terminates.
[0030] When the determination in step 414 is positive, this indicates the user's credit contained in the token 220 has expired and the process goes to step 422 and warns the user to save his work. From step 422 , the process goes to step 424 and determines whether the user wishes to continue running the selected application program AP1-APN. When the determination in step 424 is negative, the process goes immediately step 418 and encrypts the selected application program and the token 220 , and then goes to step 420 terminates. When the determination in step 424 is positive, the process goes to step 426 and contacts the server computer system 202 to obtain additional credit for the user. Once the server computer system 202 has been contacted, the process goes to step 428 and determines whether the user has sufficient credit. When the process arrives at step 428 in this manner, the inquiry in step 428 is necessarily negative and the process goes immediately step 430 . In step 430 , the user is presented with a billing screen and provides required information to obtain additional credit.
[0031] From step 430 , the process goes to step 432 and supplies the information entered in step 430 to the server computer system 202 . From step 432 , the process goes to step 434 and determines whether the user's credit has been approved or declined by the server computer system 202 . When the determination in step 434 is negative, the users credit has been declined and the process goes immediately to step 420 and terminates. When the determination in step 434 is positive, the user's credit has been approved and the process goes to step 436 and a new token 220 is received from the server computer system 202 . The new token 220 contains updated credit information so that the user may access the desired application programs AP1-APN. From step 436 , the process goes back to step 406 . As indicated in FIG. 4 in step 436 , the new token 220 may also included updated authorization information, which occurs when the process arrives at step 436 via a different route, as will now be described in more detail.
[0032] Going back to step 408 , when the determination in step 408 is negative the selected application program AP1-APN is not authorized for use. As a result, the process goes to step 438 and contacts the server computer system 202 in order to obtain authorization for the selected application program AP1-APN. In step 438 , the user will supply any required information to obtain access to the selected application program AP1-APN. From step 438 , the process goes to step 428 and determines whether the user has sufficient credit. If the determination in step 428 is positive, the process goes to step 436 and receives a new token from the server computer system 202 . It should be noted that when the process arrives at the step 436 via the determination in step 408 being negative and the determination in step 428 being positive, the new token 220 received in step 436 will include only updated authorization information. Conversely, when the process arrives at step 436 via steps 426 and 428 , the new token 220 received in step 436 will include only updated credit information. When the process arrives at the step 436 via the step 434 , the new token 220 may include both updated credit and authorization information.
[0033] With the ASP system 200 , an Application Service Provider can provide application programs for certain periods of time in both broken-connection and continuous-connection environments. Moreover, with the system 200 the versions of application programs being run by users may be conveniently updated each time the client computer system 204 , 206 contacts the server computer system 202 to obtain additional credit. The system 200 also provides added security for Application Service Providers because unauthorized copies of the application programs may not be made, and users may be limited to a particular client computer system 204 , 206 on which they can use the selected application programs. In the embodiment where the token 220 is contained on a smart card 228 , each user also realizes added security in preventing unauthorized use of the application programs since the smart card is required to access to such programs.
[0034] It is to be understood that even though various embodiments and advantages of the present invention have been set forth in the foregoing description, the above disclosure is illustrative only, and changes may be made in detail, and yet remain within the broad principles of the invention. For example, although the components described above would typically be implemented in software on suitable processing circuitry, where appropriate such components may be also be implemented using either digital or analog circuitry, or a combination of both. Therefore, the present invention is to be limited only by the appended claims.
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A method and computer system for providing access to computer resources on a computer system and includes generating a token containing encrypted user information including credit, authorization, and authentication information. A request is initiated to open an encrypted computer resource stored on the computer system, and execution of a remote application manager component on the computer system is also initiated. The remote application manager component decrypts the token and authenticates a user using authentication information stored in the token. Whether the user is authorized and has sufficient credit are then verified. When the user is approved, the requested computer resource is decrypted and opened. Use of the computer resource is monitored to determine whether the user has sufficient credit to continue using the computer resource. A notification is provided when the monitored usage of the opened computer resource has exceeded the credit.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation of U.S. patent application Ser. No. 13/674,504, filed on Nov. 12, 2012, the entirety of which is incorporated herein by reference for all purposes.
BACKGROUND OF THE INVENTION
[0002] An ankle joint may become severely damaged and painful due to arthritis from prior ankle surgery, bone fracture, infection, osteoarthritis, posttraumatic osteoarthritis or rheumatoid arthritis, for example. Options for treating the injured ankle have included anti-inflammatory and pain medications, braces, physical therapy, amputation, joint arthrodesis, and total ankle replacement.
[0003] In the past the main-stay of ankle arthrosis has been joint arthrodesis, due to the poor prosthetic survival rate of total ankle replacements. This is primarily due to the clinical results of early ankle designs. Therefore, arthrodesis has been the only choice for many surgeons and patients. Arthrodesis improves stability and reduces pain, but also severely inhibits normal function of the ankle joint. Although some patients have very good results from ankle fusion, surrounding joints above and below the fusion may become arthritic and painful because the lack of ambulation places additional stress on these joints.
[0004] There have been numerous ankle joint replacement prostheses developed over the last 30 years. The Agility ankle is an example of an early implant design. It is comprised of two components—one part is cemented to the tibia and the other part is cemented to the talus. An issue with the design of the early ankle prostheses is that although they allow for some dorsiflexion/plantarflexion motion, the articulation surfaces restrict varus/valgus and rotation motions. Another problem surrounding early implant designs is their reliance on the surrounding soft tissues of the ankle to stabilize the implant. As a result, they are not well suited for implantation in individuals with compromised soft tissues.
[0005] Another example is the Salto Talaris ankle device, which is a fixed-bearing ankle prosthesis. This two-component ankle system utilizes a conical talar component with two different radii of curvature and a curved groove in the sagittal plane. The medial radius is smaller than the lateral to allow equal tensioning of the collateral ligaments. The tibial component is designed for a fixed insertion of a polyethylene bearing piece that is replaceable. Some issues with the fixed-bearing prostheses include high wear rate of the articulation surfaces, ambulatory constraint, and loosening of the implant.
[0006] Another ankle replacement device is the Scandanavian Total Ankle Replacement (STAR). In this device the tibial component is designed for less bone resection and has two parallel bars for insertion into the subchondral bone. The talar component is meant to mimic the talar dome and has a central ridge for stabilization of a polyethylene piece. The STAR prosthesis inhibits inversion/eversion coupling with plantarflexion/dorsiflexion motion. This leads to straining and potential damage to the deltoid ligaments on the medial side of the ankle. Another issue with this device is edge loading, which puts a great amount of stress on the ridge of the implant and results in the implant retracting from the talus.
[0007] More modern designs have attempted to increase the range of motion while maintaining the integrity of the surrounding soft tissues of the ankle. For example, U.S. Pat. No. 7,625,409 discloses a prosthesis designed to allow full range of motion while minimizing edge loading and subsidence. However, this prosthesis fails to address the need for an implant for use in patients with compromised soft tissues in the ankle.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 shows an anterior view of an ankle prosthesis according to an embodiment of the present invention;
[0009] FIG. 2 shows an anterior view of an ankle joint and surrounding soft tissues;
[0010] FIG. 3 shows an anterior view of exemplary means of attachment of an ankle prosthesis according to an embodiment of the present invention;
[0011] FIG. 4 shows a posterior view of an ankle prosthesis according to an embodiment of the present invention; and
[0012] FIG. 5 shows a medial view of an ankle prosthesis according to an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0013] Although detailed embodiments of the present invention are disclosed herein, it is to be understood that the invention is not restricted to the details of the embodiments. Many changes in design, composition, configuration and dimensions are possible without departing from the spirit and scope of the instant invention. Further, the figures are not necessarily to scale. Some features may be exaggerated to show details of particular components. Specific structural and functional details disclosed herein are not to be interpreted as limiting, but as an aid for teaching one skilled in the art how to variously employ the present invention. Accordingly, it should be readily understood that the embodiments described and illustrated herein are illustrative only, and are not to be considered as limitations upon the scope of the present invention.
[0014] An ankle joint is a very complex joint having three motions that occur simultaneously: dorsiflexsion/plantarflexion, varus/valgus, and internal/external rotation. In a healthy ankle, the ankle joint relies on soft tissues, including ligaments, to provide stability. These tissues include, for example, an anterior inferior tibiofibular ligament, a calcaneal-fibular ligament, a posterior talo-fibular ligament, a syndesmotic ligament, an anterior capsule of the ankle joint (which helps keep the ankle from anterior movement), and a deltoid ligament. These soft tissues contribute to the overall function of the ankle by ensuring joint stability.
[0015] In a healthy ankle these ligaments naturally stretch according to specific ankle motions in order to keep the joint secure. It is desirable that an ankle replacement prosthesis prevents stretching these ligaments beyond their natural range of motion. Further, because the ankle joint absorbs a stress greater than four times the body's weight with every step, an ankle replacement prosthesis ideally will be able to withstand the pressures associated with weight-bearing and motion.
[0016] In a patient with healthy soft tissue in the ankle, this tissue will provide stability to a prosthesis. However, when the soft tissue is compromised, a prosthesis can fail for various reasons, including instability. Therefore, there exists a need for an implant that provides ambulation of the ankle joint similar to that of a natural ankle and that remains stable when implanted in a patient with compromised soft tissues.
[0017] An ankle prosthesis 1 of the present invention addresses these and additional problems. Ankle prosthesis 1 of the present invention provides adequate range of motion for the primary degrees of freedom of the talar joint, including movement in a frontal plane and a sagittal plane. Additionally, ankle prosthesis 1 of the present invention provides stability for implantation into an ankle joint with compromised soft tissues by constraining movement in the general direction of compromised soft tissues.
[0018] As may be seen with reference to FIG. 2 , the natural anatomy of a talus bone 3 has a bicondylar contour 5 . The ankle prosthesis of the present invention comprises a talar component and a tibial component. In one embodiment, the talar component mimics the natural anatomy of the talus bone and the tibial component comprises a complimentary contour. In another embodiment depicted in FIG. 1 , the natural anatomy is mimicked in a reverse orientation, where a bicondylar contour is on a tibial component 7 and a talar component 9 comprises a complimentary contour.
[0019] In one embodiment of the present invention, ankle prosthesis 1 comprises a two-component design which is sufficiently sized to prevent subsidence. With reference to FIG. 1 , ankle prosthesis 1 comprises tibial component 7 and talar component 9 . Tibial component 7 is configured for attachment to a tibia 11 . As may be seen in FIG. 3 , tibial component 7 comprises an attachment surface 13 positioned on a proximal portion of tibial component 7 and an articulation surface 15 positioned on a distal portion of tibial component 7 , wherein at least a portion of attachment surface 13 is configured for attachment to tibia 11 . The attachment surface and the articulation surface of tibial component 7 may comprise a unitary piece, or in an alternative embodiment the surfaces may be two distinct units attached to one another by any suitable means of attachment.
[0020] Tibial component 7 may be attached to tibia 11 by any suitable means of attachment, e.g., one or more screws or one or more rods. An exemplary means of attachment 17 may be seen with reference to FIG. 3 . In one embodiment, tibial component 7 functions as the “male” component of ankle prosthesis 1 . For example, referring to FIGS. 1 and 3 , articulation surface 15 of tibial component 7 comprises at least one convex contour 19 extending anteriorly-posteriorly on a medial portion of tibial component 7 , at least one convex contour 21 extending anteriorly-posteriorly on a lateral portion of tibial component 7 , and at least one concave contour 23 extending anteriorly-posteriorly in a sagittal plane of tibial component 7 . In this embodiment, articulation surface 15 comprises a bicondylar contour which mimics the natural anatomy of the proximal portion of talus bone 3 . Radii of curvature of the at least one convex contour 19 on the medial portion and the at least one convex contour 21 on the lateral portion of articulation surface 15 of tibial component 13 may be the same, or in an alternative embodiment a radius of curvature of the medial portion may be greater, or in another embodiment a radius of curvature of the lateral portion may be greater.
[0021] In an alternative embodiment, tibial component 7 functions as the “female” component of ankle prosthesis 1 . In this embodiment articulation surface 15 of tibial component 7 comprises at least one concave contour extending anteriorly-posteriorly on a medial portion of tibial component 7 , at least one concave contour extending anteriorly-posteriorly on a lateral portion of tibial component 7 , and at least one convex contour extending anteriorly-posteriorly in a sagittal plane of tibial component 7 . In this embodiment, articulation surface 15 comprises a contour which is complimentary to a bicondylar contour. Radii of curvature of the at least one concave contour on the medial portion and the at least one concave contour on the lateral portion of articulation surface 15 of tibial component 13 may be the same, or in an alternative embodiment a radius of curvature of the medial portion may be greater, or in another embodiment a radius of curvature of the lateral portion may be greater.
[0022] Complimentary talar component 9 is configured for attachment to talus 3 . Talar component 9 comprises an attachment surface 25 on a distal portion of the component and an articulation surface 27 on a proximal side of the component. At least a portion of attachment surface 25 is configured for attachment to talus 3 . The attachment surface and the articulation surface of talar component 9 may comprise a unitary piece, or in an alternative embodiment the surfaces may be two distinct units attached to one another by any suitable means of attachment.
[0023] Talar component 9 may be attached to talus 3 by any suitable means of attachment, e.g., one or more screws or one or more rods. An exemplary means of attachment 29 may be seen with reference to FIG. 3 . Articulation surface 27 of talar component 9 is configured to compliment articulation surface 15 of tibial component 7 , and accordingly may comprise the “female” or “male” component of ankle prosthesis 1 depending on the configuration of tibial component 7 . Articulation surface 27 of talar component 9 comprises a contour for receiving articulation surface 15 of tibial component 7 . In one embodiment of the present invention in which talar component 9 comprises the “female” component of ankle prosthesis 1 , articulation surface 27 of talar component 9 has at least one concave contour 31 extending anteriorly-posteriorly on a medial portion of talar component 9 , at least one concave contour 33 extending anteriorly-posteriorly on a lateral portion of talar component 9 , and at least one convex contour 35 extending anteriorly-posteriorly on a sagittal plane of talar component 9 . Convex contour 35 is configured to compliment the at least one concave contour 23 on the sagittal plane of articulation surface 15 of tibial component 7 . At least one concave contour 31 on medial portion of articulation surface 27 of talar component 9 is configured to compliment the at least one convex contour 19 on the medial portion of articulation surface 15 of tibial component 7 and the at least one concave contour 33 on the lateral portion of articulation surface 27 of talar component 9 is configured to compliment the at least one convex contour 21 on the lateral portion of articulation surface 15 of tibial component 7 . Radii of curvature of the at least one concave contour 31 on the medial portion of talar component 9 and the at least one concave contour 33 on the lateral portion of talar component 9 may be the same, or in an alternative embodiment a radius of curvature on the medial portion may be greater, or in another embodiment a radius of curvature of the lateral portion may be greater.
[0024] In an alternative embodiment, talar component 9 comprises the “male” component of ankle prosthesis 1 . In this embodiment, articulation surface 27 of talar component 9 has at least one convex contour extending anteriorly-posteriorly on a medial portion of talar component 9 , at least one convex contour extending anteriorly-posteriorly on a lateral portion of talar component 9 , and at least one concave contour extending anteriorly-posteriorly on a sagittal plane of talar component 9 . Concave contour is configured to compliment the at least one convex contour on the sagittal plane of articulation surface 15 of tibial component 7 . At least one convex contour on medial portion of articulation surface 27 of talar component 9 is configured to compliment the at least one concave contour on the medial portion of articulation surface 15 of tibial component 7 , and the at least one convex contour on the lateral portion of articulation surface 27 of talar component 9 is configured to compliment the at least one concave contour on the lateral portion of articulation surface 15 of tibial component 7 . Radii of curvature of the at least one convex contour on the medial portion of talar component 9 and the at least one convex contour 33 on the lateral portion of talar component 9 may be the same, or in an alternative embodiment a radius of curvature on the medial portion may be greater, or in another embodiment a radius of curvature of the lateral portion may be greater.
[0025] Articulation surface 15 of tibial component 7 and articulation surface 27 of talar component 9 form an articulation interface 37 . Congruence of the articulation surfaces is maintained in all positions of an ankle joint movement, including dorsiflexion/plantarflexion, inversion/eversion, and internal/external rotation.
[0026] In order to maintain congruence of the articulation surfaces of prosthesis 1 when implanted in an ankle with compromised soft tissue, one embodiment of the present invention comprises a lip on the female component. The lip is configured to maintain congruence of the articulation surfaces in patients having compromised soft tissues by at least partially limiting mobility in a direction toward the compromised soft tissue. Congruence of the articulation surfaces may be maintained when the articulation surfaces correspond to one another and are in agreement for each direction of motion.
[0027] In one embodiment of the present invention, a lip 39 is configured to stabilize prosthesis 1 when implanted in patients with compromised soft tissues on a medial side of the ankle. For example, lip 39 may be configured for implantation in a patient with a compromised deltoid ligament 41 (depicted in FIG. 2 with talar component 9 being the “female” component). In this embodiment, lip 39 comprises a raised surface on a medial edge 43 of articulation surface 27 of talar component 9 such that the raised surface extends to a position which is in superior relation to a medial edge 45 of articulation surface 15 of tibial component 7 . In this embodiment, the raised surface constrains movement in a medial direction, or eversion of the implant. In an alternative embodiment in which tibial component 7 is the “female” component, the lip comprises a raised surface on a medial edge of articulation surface of tibial component 7 such that the raised surface extends to a position which is in inferior relation to a medial edge of the articulation surface of talar component 9 (not depicted).
[0028] In another embodiment of the present invention, the lip is configured to stabilize prosthesis 1 when implanted in patients with compromised soft tissues on a lateral side of the ankle, such as a compromised anterior inferior tibiofibular ligament 47 (depicted in FIG. 2 ), for example. In this embodiment, a lip 49 comprises a raised surface on a lateral edge 51 of talar component 9 such that the raised surface extends to a position which is in superior relation to a lateral edge 53 of articulation surface 15 of tibial component 7 . In this embodiment, the raised surface constrains movement in a lateral direction, or inversion of the implant. In an alternative embodiment in which tibial component 7 is the “female” component, the lip comprises a raised surface on a lateral edge of articulation surface of tibial component 7 such that the raised surface extends to a position which is in inferior relation to a lateral edge of the articulation surface of talar component 9 (not depicted).
[0029] In another embodiment, prosthesis 1 is provided for implantation in patients with compromised soft tissues on both the medial and lateral sides of the ankle. In this embodiment, the lip comprises a first raised surface 39 on medial edge 43 of talar component 9 such that the raised surface extends to a position which is in superior relation to medial edge 45 of articulation surface 15 of tibial component 7 and a second raised surface 49 on lateral edge 51 of talar component 9 such that the raised surface extends to a position which is in superior relation to lateral edge 53 of articulation surface 15 of tibial component 7 . In this embodiment, varus/valgus freedom of movement is constrained, but there is freedom of movement for dorsiflexion/plantarflexion. In an alternative embodiment, tibial component 7 is the “female” component and comprises the lip.
[0030] With reference to FIGS. 4 and 5 , in another embodiment prosthesis 1 is provided for implantation in patients with compromised soft tissue on a posterior side of the ankle. In this embodiment, the lip comprises a raised surface (see FIG. 5 ) on a posterior edge 55 of talar component 9 such that the raised surface extends to a position which is in superior relation to a posterior edge 57 of articulation surface 15 of tibial component 7 . In this embodiment, posterior displacement of tibial component 7 is prevented. In an alternative embodiment, tibial component 7 is the “female” component and comprises the lip to prevent posterior displacement of talar component 9 .
[0031] The lip may also be configured for implantation in patients with compromised soft tissue on an anterior side of the ankle. In this embodiment, the lip comprises a raised surface (see FIG. 5 ) on an anterior edge of talar component 9 such that the raised surface extends to a position which is in superior relation to an anterior edge of articulation surface 15 of tibial component 7 . In this embodiment, anterior displacement of tibial component 7 is prevented. In an alternative embodiment, tibial component 7 is the “female” component and comprises the lip to prevent anterior displacement of talar component 9 .
[0032] In another embodiment, prosthesis 1 is provided for implantation in patients with compromised soft tissue such that stabilization of the implant and constraint of movement is necessary in more than one direction of mobility. The lip comprises a raised surface (not shown) extending from medial edge 43 of articulation surface 27 of talar component 9 posteriorly curving to lateral edge 51 of articulation surface 27 of talar component 9 and continuing around returning to medial edge 43 . The lip extends to a position which is in superior relation to articulation surface 15 of tibial component 7 . In this configuration, the lip comprises a general cup-like contour providing stabile implantation in patients with more severe soft tissue impairment. In an alternative embodiment, tibial component 7 is the “female” component and comprises the cup-like lip.
[0033] Another consideration for providing a successful total ankle replacement prosthesis is the material or materials of construction. In order to reduce wearing of the components, and therefore failure of the prosthesis, it is desirable to use a material, or a combination of materials, which create minimal friction between the two components. Suitable materials include those which minimize friction and resultant wear of the articulation surfaces. Some exemplary materials include a metal, a polymer, or a ceramic material. However, other suitable materials are contemplated within the spirit and scope of the present invention. In one embodiment of the present invention, articulation surface 15 of tibial component 7 is comprised of a first material and articulation surface 27 of talar component 9 is comprised of a second material. The first material and the second material may be substantially the same. In an alternative embodiment, the first and second material are substantially different. Further, tibial component and talar component are each comprised of an attachment surface and an articulation surface. The articulation surface and attachment surface of tibial component 7 may comprise materials which are substantially the same, or in an alternative embodiment the surfaces may comprise materials which are substantially different. Likewise, the articulation surface and attachment surface of talar component 9 may comprise materials which are substantially the same, or in an alternative embodiment the surfaces may comprise materials which are substantially different.
[0034] Additionally, it may be desirable to use a material which promotes osseointegration, so that a direct interface between attachment surface 25 of talar component 9 and talus 3 , and in between attachment surface 13 of tibial component 7 and tibia 11 , are formed. To this end, one embodiment of the present invention comprises a material of construction which promotes osseointegration. For example, the material may comprise pores into which osteoblasts and supporting tissues can migrate.
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The present invention relates to a stabilized ankle prosthesis configured for use in patients with compromised soft tissue in the ankle. The prosthesis of the present invention is a two-component design comprising a stabilizing lip configured to constrain movement in the general direction of compromised soft tissue.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 60/741,526, filed on Dec. 1, 2005, the disclosure of which is herein incorporated by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to cardiovascular pumps, and more particularly, to cardiovascular roller pumps that create a pulsatile flow profile.
BACKGROUND
[0003] The American Heart Association indicates that 30,000 cardiopulmonary bypass (CPB) surgeries were done on patients of ages less than 15 years in the USA in 2002. Of these cases, 18,000 were specifically for the repair of congenital defects of the heart. Over the past decade, mortality rates associated with pediatric cardiopulmonary bypass procedures have been significantly reduced, yet morbidity remains a major clinical problem with patients suffering cerebral, myocardial, or renal dysfunction following CPB. Factors associated with extracorporeal circuit (ECC) technology, such as non-pulsatile perfusion, hemodilution, and acute injury due to mishap have been implicated in patient morbidity. Despite this evidence, innovation has been slow in coming. Roller pumps that were first used in perfusion studies in 1935 are still relied on in 98% of centers performing pediatric CPB today.
[0004] One visible side-effect of CPB in infants and children is systemic accumulation of edema fluid. In a prospective study of 100 neonates undergoing corrective cardiac surgery employing approximately 2 hours of CPB, the average fluid accumulation was greater than 600 ml. Much of this phenomenon is related to the hemodilution and foreign surface exposure of the blood loop. A typical infant of 3.5 kg weight has an estimated blood volume of 280 ml, and the extracorporeal loop with the venous reservoir, oxygenator, blood filter, and tubing can easily reach 700-800 ml of prime, resulting in a dilution factor of 2.5:1 to 3:1. Hemodilution in infants can far exceed that seen in adult patients, where 25% to 33% dilution rates are typical. Hemodilution results in lower hematocrit with associated reduction of oxygen delivery capacity, and is associated with a higher transfusion rate and increased use of all blood products with concomitant infection risk.
[0005] Deep hypothermic circulatory arrest is commonly used in the repair of congenital defects of the heart. Cessation of blood flow to the collateral circulation allows the surgeon to properly visualize the surgical field, while hypothermia reduces metabolism providing cellular protection despite lack of oxygen delivery. In recent practice, deep hypothermic circulatory arrest is conducted with intermittent periods of very low blood flow in the range of 10 to 20 cc/kg/min or “trickle flow”. It is commonly felt that this amount of flow can be provided without compromising the conduct of the surgical repairs, and will serve to preserve brain high energy phosphate concentrations and intracellular pH (20). In order to meet these requirements the arterial pump must be capable of maintaining flow accuracy over a broad range of flow rates and temperature from 10 cc/kg at 15° C., to 150 cc/kg at 37° C.
[0006] Centrifugal pumps are simply not practical in providing for extreme low flow rates due to excessive impeller speeds and resulting blood damage and in fact are relied on only in 2% of centers conducting pediatric heart surgery. Occlusive roller pumps are currently used; however, they are far from optimal in their use at low flow rates.
[0007] Generally, roller pumps rely on a roller pressing against a piece of tubing backed by a rigid raceway. In order to fully occlude the circular tubing for use in very low flow conditions, excessive roller forces are needed to squeeze the tubing between the roller and raceway. This significantly increases stress and wear on the tubing, potentially causing leaks or ruptures. A review of the Manufacturer and User Facility Device Experience Database (MAUDE) reports supports the conclusion that tubing leaks and rupture are common events with potentially injurious results.
[0008] Traditionally, roller pumps provided no inherent means of preventing draining of the venous reservoir, and if left unattended, would drain the reservoir and continue to pump air to the patient until rotation was halted. A minimum “safety volume” of blood had to be maintained in the reservoir when using a roller pump so as to provide sufficient time for the perfusionist to react to sudden interruptions of venous return flow before the reservoir was drained. For example, at a flow rate of 1.5 l/min, using the known state-of-the-art Terumo Capiox reservoir, 300 ml of reservoir volume would provide less than 12 seconds of response time.
[0009] This has prompted the use of reservoir level detectors and air detectors with pump shut off interconnections. 79.2% of centers conducting pediatric extracorporeal circulation (ECC) utilize reservoir level detectors, and 87.5% of these centers utilize air bubble detectors. However, despite their presence, these safety devices may fail to protect due to device failures and human errors. In practice, a typical circuit volume for a small infant could range from 600-800 ml.
[0010] In order to provide a safe operational venous reservoir level for use with roller pumps, 200 additional ml are typically added to the circuit, which is usually whole blood or packed red blood cells. This safety volume is highly variable amongst practitioners and could be minimized if a self-limiting safety system was designed into the pump. If this 200 ml volume could be eliminated, the savings in both hemodilution side-effects and risks to additional blood product transfusion would be of significant benefit.
[0011] Proper setting of the degree to which a roller pump occludes the tubing is also critical. If there is too little occlusion, the pump fails to create sufficient flow. Over occlusion creates excessive stress in the tubing which can lead to splitting with subsequent blood loss and air introduction to the arterial circulation. Split tubing continues to be a common problem with traditional roller pumps.
[0012] Current peristaltic pump technology typically operates with two pump rollers and a 180 degree arc over which the pump tubing is occluded by the rollers and a stator. In this design, fluid enters the pump tubing from the venous reservoir under low pressure head conditions, typically 50 mmHg or less. The purpose of the roller pump is to shuttle this fluid from the inlet to the outlet and force it to flow through the tubing circuit. Typically in heart surgery this involves moving blood from a low pressure inlet to a high pressure outlet. As the roller head (rotor) turns, a roller contacts and advances along the tubing filling it with low pressure blood. At approximately the 180 degree point of the stator arc, a second roller contacts the tubing and isolates the fluid between the rollers still at the low inlet pressure. This situation lasts only briefly as the first roller departs from the tubing exposing the low pressure isolated fluid to the high pressure outlet fluid. This causes an equilibration of pressure between the fluid volumes and is associated with a momentary drop in pressure in the outlet. As the second roller continues to advance it drives the fluid forward reestablishing pressure within the outlet tubing.
[0013] Another style of roller pump, without a stator, utilizes a roller head (rotor) with three rollers and a conduit having an occlusive portion. The conduit extends around the rollers. The occlusive portion remains occluded as long as the pressure on the outside of the conduit is equal to or greater than the pressure on the inside of the conduit. When the fluid inlet supply pressure exceeds the pressure acting on the exterior of the conduit, the occlusive segment will inflate and fill with fluid and the pump will force the fluid through the outlet of the conduit. Such a pump is described in more detail in U.S. Pat. No. 5,486,099, which is herein incorporated by reference.
[0014] There is an ongoing debate over pulsatile versus non-pulsatile circulatory support. Various published studies, however, have substantiated some advantages with pulsatile support, especially as it relates to cardiopulmonary support. These studies indicate that pulsatile support reduces systemic vascular resistance and attenuates the catecholamine response, improves myocardial blood flow, and improves overall clinical outcomes. Cerebral pressure-flow auto-regulation has been proven to be intact in adult patients when the mean arterial pressures (MAPS) were greater than 50 mmHg. However, for pediatric patients, where MAP often ranges between 20 to 40 mmHg before and after deep hypothermic cardiac arrest, pulsatile perfusion becomes important for maintaining cerebral blood flow.
[0015] Conventional roller pumps can be used to create pulsatile flow and pressure by rapidly accelerating the speed, revolutions per minute (RPM), of the rotor for a “systolic” period and reducing the speed (RPM) to create a “diastolic” period. This has significant disadvantages as it involves use of much greater power to accelerate the rotating mass, increases tubing wear, and increases blood exposure to damaging negative pressures. With this technique it is not possible to isolate the inlet conditions from the outlet conditions. Additionally, the inlet conditions vary as the speed (RPM) is modulated.
[0016] In view of the above limitations and drawbacks of the known technology, it is seen that there is a need for a ventricular roller pump that provides pulsatile pressure and flow profiles having amplitudes and rise times that approximate those of a human heart, while maintaining a constant speed (RPM).
BRIEF SUMMARY OF THE INVENTION
[0017] In meeting the above need, the present invention provides a roller pump conduit, defining a pump chamber, that includes a roller contact portion having a fill region and a delivery region, the fill region having a first taper and being configured to determine volume delivery per revolution of a roller head. The delivery region has a pressure region having a second taper and a discharge region having a third taper. The second taper has a greater degree of taper than the third taper. The delivery region is configured to produce a pulsatile flow out of the conduit.
[0018] In another aspect, a roller pump for pumping fluids is provided that comprises a plurality of rollers located in spaced apart relation. The rollers are attached to a rotor having a drive shaft. A flexible conduit is in mechanical communication with a plurality of rollers. The flexible conduit comprises a roller contact portion having a fill region and a delivery region, the fill region having a first taper. The fill region is configured to determine volume delivery per revolution of a roller head. The delivery region has a pressure region having a second taper and a discharge region having a third taper. The second taper has a greater degree of taper than the third taper. The delivery region is configured to produce a pulsatile flow out of the conduit.
[0019] These and other aspects and advantages of the present invention will become apparent upon reading the following detailed description of the invention in combination with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] FIG. 1 a is a side view of a roller pump conduit having a reduction in the cross sectional area within the delivery region of the conduit;
[0021] FIG. 1 b is a plan view of the roller pump conduit of FIG. 1 a;
[0022] FIG. 2 is a plan view of a roller pump having a flexible conduit as in FIGS. 1 a and 1 b;
[0023] FIG. 3 is a graph of the outlet pressure of a roller pump having the conduit of FIGS. 1 a and 1 b , compared with the outlet pressure of a roller pump having a conduit without a reduction in the cross sectional area within the delivery region of the conduit;
[0024] FIG. 4 is a graph of the flow rate of a roller pump having the conduit of FIGS. 1 a and 1 b , compared with the outlet pressure of a roller pump having a conduit without a reduction in the cross sectional area within the delivery region of the conduit.
[0025] These and other aspects and advantages of the present invention will become apparent upon reading the following detailed description of the invention in combination with the accompanying drawings.
DETAILED DESCRIPTION OF THE INVENTION
[0026] The following description is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses.
[0027] According to the present invention, a pulsatile rotary ventricular pump (PRVP) is provided as a significant advancement of pump technology, one also capable of addressing performance requirements unique to pediatric surgery. In particular, the innovative advances of the present invention in the chamber design create a pulsatile flow profile (see FIG. 4 ) that it is anticipated will assist in recovery from deep hypothermic cardiac arrest, a common surgical technique in pediatric patients. The present invention is capable of creating pressure and flow profiles that approximate the pressure and flow profiles created by a human heart. Also, the chamber design and the specification of roller contact on the chamber will allow very fine control at low flows, which is critical in cerebral perfusion of neonates and which cannot be safely delivered by previous roller pumps.
[0028] The PRVP will be significantly smaller than an adult pump. These and other features will close the gap between desired levels of performance and that provided by current pediatric arterial pumping technology, as noted in the table below.
[0000]
Adult pump (Affinity ®/MetaPlus ®)
PRVP
>50 mmHg inlet required for full flow
10 mmHg required for full flow
Min flow accuracy +/− 20 ml/min
Min flow accuracy +/− 2 ml/min
Chamber rated for 6 hours
Durable chamber rated for 1
week
[0029] The invention detailed herein is a cost effective innovation for arterial pumping, particularly to pediatric heart surgery, including physiologic pulsatile flow, very low volume extracorporeal fluid management, ultra fine resolution low flow control, and inherent safety to protect against operator error.
[0030] The pulsatile rotary ventricular pump (PRVP) of the present invention includes a flexible conduit 20 defining a pump chamber. The pump chamber includes specific regions, as shown in FIGS. 1 a and 1 b , which show the flexible conduit 20 in a side view and a plan view, respectively. These regions include the bias region L B , the low volume shut-off region L SO , the roller contact region L R , the fill region L E , the delivery region L D , the pressure region L P , and the discharge region L DC . Each region is designed to impart specific performance characteristics to the pump chamber. The exact dimensional parameters of each region can be adjusted to optimize the performance to the application.
[0031] The bias region L B receives fluid into the flexible conduit from a venous reservoir and provides for low pressure head passive filling. The bias region L B includes the low volume shut-off region L SO , which stops the flow of fluid into the fill region L F when the shut-off region L SO is compressed. The shut-off region L SO provides low suction head shut-off for management of very low reservoir volumes.
[0032] A roller contact region L R includes both the fill region L F and the delivery region L D . Each roller 24 contacts the fill region L F , and advances along the flexible conduit 20 through the fill region L F and into the delivery region L D .
[0033] The fill region L F is connected to the bias region L B . The fill region L F determines volume delivery per revolution of pump head, or maximum flow rate. In other words, the fill region L F of the pump chamber determines the “stroke volume” or the amount of blood delivered per roller pass. The width, depth and wall thickness of the fill region L E are such that they optimize filling under low pressure head conditions. The fill region L F has a taper, but that taper may have a magnitude or degree of taper equal to zero. The fill region L F of FIGS. 1 a and 1 b has a constant width, and therefore, a taper of zero magnitude or degree.
[0034] The delivery region L D includes a pressure region L P and a discharge region L DC . The pressure region L P is characterized by a tapering cross sectional area which results in pressurization of the advancing fluid. The tapering cross section of the pressure region L P couples the larger-width fill region L F to the smaller-width discharge region L DC of the delivery region L D . The discharge region L DC of the delivery region L D has a taper, but that taper may have a magnitude or degree of taper equal to zero. The discharge region L DC has a taper of lesser degree than the taper of the pressure region L. The discharge region L DC of FIGS. 1 a and 1 b has a constant width, and therefore, a taper of zero magnitude or degree. The amount of pressure developed is controlled by the total volume of the delivery region L D , as determined by the degree, or magnitude, and length of the taper of the pressure region L P and the position of the taper of the pressure region L P along the length of the flexible conduit 20 .
[0035] The pressure region L P provides augmented volume delivery for the “systolic” portion of pulsatile flow. The remainder of the delivery region L D , the discharge region L DC , provides the “diastolic” portion of pulsatile flow and fine flow resolution at low speeds (RPM). The resulting flow and pressure are pulsatile and periodic with each roller pass.
[0036] With reference to FIG. 2 , portion of a roller pump 22 is provided. The flexible conduit 20 of FIGS. 1 a and 1 b is wrapped around a plurality of freely rotating rollers 24 mounted to a rotor 26 , or roller head, of the roller pump 22 . The rollers 24 are located in spaced apart relation. The flexible conduit 20 contacts at least two rollers 24 at a time when the roller pump 22 is in operation. The roller pump 22 of FIG. 1 has an enclosure 28 , which serves as a protective shield around the moving rotor 26 .
[0037] When the roller pump 22 is in operation, fluid flows into the inlet 30 of the flexible conduit 20 from a venous reservoir (not shown). As the rollers 24 advance across the flexible conduit 20 , fluid is occluded in the fill region L E of the flexible conduit 20 between two rollers 24 . As the rollers 24 advance further along the flexible conduit 20 , the isolated fluid shuttles from the fill region L F to the pressure region L P , which has a tapering cross section, and further into the discharge region L DC , which has a reduced, constant cross section, its degree of taper being equal to about zero. Alternatively, the taper of the discharge region L DC could be of a magnitude, or degree, not equal to zero. As the rollers 24 advance along the flexible conduit 20 through the fill region L F and into the delivery region L D , the captured fluid remains isolated between the rollers 24 . This causes the fluid to pressurize within the flexible conduit 20 between the rollers 24 . Ideally the isolated fluid is brought to the same pressure or higher pressure than the fluid located in a portion of the flexible conduit 20 that is not isolated.
[0038] In the delivery region L D , the roller 24 on the leading edge of the isolated fluid finally advances away from the flexible conduit 20 , and the previously isolated fluid is exposed to the outlet 32 . An initial pressurized discharge of fluid from the outlet 32 into the extracorporeal circuit (ECC) (not shown) occurs, followed by a reduced period of steady flow as the roller 24 passes over the discharge region L DC of the flexible conduit 20 . This causes the flow rate and pressure to be initially higher, followed by a relatively lower pressure and flow rate. As a result, a periodic pulsatile flow and pressure that is of significant amplitude and rise is created, which more closely represent physiologic conditions than non-pulsatile flow and pressure profiles, although the rotor 26 turns at a constant rate.
[0039] Design parameters of the roller contact region L R and the delivery region L D can be varied until the desired pulsatility is achieved. An “energy equivalent pressure” (EEP) is used to quantify pulsatile pressure and flow waveforms. EEP is the ratio of the area under the hemodynamic power curve and the flow curve at the end of the flow and pressure cycles. The following formula is used for defining EEP:
[0000]
EEP
=
∫
Q
·
P
t
∫
Q
t
[0000] where Q is the pump flow and P is the arterial pressure. The units for EEP are units of pressure, such as mmHg.
[0040] During pulsatile perfusion, EEP is always higher than the mean arterial pressure (MAP), whereas during non-pulsatile flow, EEP is very similar to the MAP. Existing research has shown that pulsatile flow generated higher hemodynamic energy compared with non-pulsatile flow. By way of example, the human heart has been reported to have a 10% increase in EEP, whereas pulsatile roller pumps have previously had approximately a 4% increase in the EEP over the MAP. Non-pulsatile pumps, on the other hand, only have an increase of about 1%. The PRVP according to the present invention can readily reach 10% and higher increase in EEP.
[0041] In order to achieve the desired pulsatility specifications, the pump chamber design of the flexible conduit 20 can be modified to increase the stroke volume of the roller pump 22 . Parameters that can be varied include the width and thickness of the roller contact region L R and the width and thickness of the delivery region L D . If the pulse is too low, then the fill volume can be increased and/or the discharge volume can be decreased. If the pulse is too high, then a reduction in fill volume can be made or a change in the pressure region L P taper can be made.
[0042] FIGS. 3 and 4 respectively illustrate an outlet pressure/time graph and a flow rate/time graph. In both the outlet pressure graph ( FIG. 3 ) and the flow rate graph ( FIG. 4 ), a prior art style pump chamber, without a pressure build region L P and without a reduction in the degree of the taper within the delivery region L D , is designated as “Original”. A PRVP style pump chamber embodying the principles of the present invention and as generally illustrated in FIGS. 1 a and 1 b , and 2 , i.e. a conduit having a pressure build region L P and a reduction in the degree of taper within the delivery region L D , is designated as “Pulse” in the graphs. In both instances, the traces were recorded under identical operation conditions using a 4 inch diameter pediatric-sized rotor 26 having three rollers 24 and operating at an average outlet pressure of 50 mmHg, with an average flow rate of 1 liter/min, and water at room temperature as the pumped medium.
[0043] As is readily apparent from the graphs, the “Pulse” trace exhibits a pronounced increase in pulse pressure ( FIG. 3 ) including rise time and amplitude, and a similarly steep rise in flow rate ( FIG. 4 ) and pulsatile flow amplitude, when compared to the “Original” trace.
[0044] In contrast to the techniques required to create pulsatile flow with prior technologies, the present invention achieves pulsatile flow using a constant speed rotor 26 , and, therefore, can implement pulsatile conditions at the outlet 32 , all without affecting inlet conditions and without creating pulsatility at the inlet 30 . This has advantages in avoiding low pressure at the inlet, keeping the speed of the rotor 26 low, avoiding excessive wear of the flexible conduit 20 , and avoiding damage to the blood pumped through the flexible conduit 20 .
[0045] The flexible conduit 20 is made from polyurethane or another suitable flexible material. In order to reduce wear on the flexible conduit 20 , the flexible conduit 20 is manufactured by injection molding. By injection molding the pump chamber, a durable disposable flexible conduit 20 is produced that can be used for prolonged support after surgery, without the need for changing pumps.
[0046] The foregoing disclosure is the best mode contemplated by the inventor for practicing this invention. It is apparent, however, that methods incorporating modifications and variations will be obvious to one skilled in the art. Inasmuch as the foregoing disclosure is intended to enable one skilled in the pertinent art to practice the instant invention, it should not be construed to be limited thereby but should be construed to include such aforementioned obvious variations and be limited only by the spirit and scope of the following claims.
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A roller pump conduit defining a pump chamber is provided. The roller pump conduit includes a roller contact portion having a fill region and a delivery region. The fill region has a first taper configured to determine volume delivery per revolution of a roller head. The delivery region has a pressure region having a second taper and a discharge region having a third taper. The third taper has a lesser degree of taper than the second taper. The delivery region is configured to produce a pulsatile flow out of the conduit.
Furthermore, a roller pump having a roller pump conduit is provided. The roller pump conduit of the roller pump has a fill region and a delivery region, the fill region having a first taper, and the delivery region having a second and third taper, wherein the third taper has lesser degree of taper than the second taper.
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CROSS REFERENCE TO RELATED APPLICATION
This application claims the benefit of U.S. provisional patent application Ser. No. 60/816,174, filed on Jun. 23, 2006, the disclosure of which is herein incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The subject invention generally relates to a steering column assembly for a vehicle.
2. Description of the Related Art
Vehicles typically include an instrument panel attached to a cross beam extending between a pair of front pillars. An instrument cluster is usually attached to the instrument panel, and is typically located above a steering column assembly. The instrument cluster includes instrumentation necessary for a driver to properly operate the vehicle, such as a speedometer, tachometer, fuel gauge, coolant temperature gauge, etc. The driver views the instrumentation by looking through and around a steering wheel attached to the steering column.
Currently, many vehicles are equipped with adjustable steering column assemblies. The adjustable steering column assemblies may include rake adjustments for adjusting the height of the steering wheel, telescopic adjustments for adjusting the distance of the steering wheel from the driver, or may include both the rake adjustment and the telescopic adjustment. Accordingly, the steering wheel may be positioned in a manner that obstructs the view of the instrumentation of the instrument cluster.
Mounting the instrument cluster on the steering column allows the instrument cluster to move with the steering column in both the rake and the telescoping adjustments. Accordingly, the instrument cluster maintains a fixed spatial relationship relative to the steering wheel, thereby ensuring the driver has a continuous unobstructed view of the instrument cluster regardless of the position of the steering wheel. U.S. Pat. No. 4,527,444 discloses a steering column assembly having both rake and telescopic adjustments with the instrument cluster permanently mounted to the steering column assembly.
Modern vehicles incorporate a collapsible column jacket into the adjustable steering column assemblies, and further include energy absorption mechanisms. The energy absorption mechanisms absorb energy transmitted through the steering column as the steering column collapses along a longitudinal axis in response to an emergency event, such as a vehicular crash.
However, the effectiveness of the energy absorption mechanism is reduced or eliminated by having the instrument cluster permanently mounted to the steering column assembly because the instrument cluster abuts against the instrument panel, thereby restricting movement of the collapsible column jacket. Additionally, the added weight of the instrument cluster onto the steering column assembly increases vibration of the steering column assembly felt by the driver, which is an undesirable effect.
SUMMARY OF THE INVENTION AND ADVANTAGES
The subject invention discloses a steering column assembly for a vehicle. The steering column assembly comprises a mounting bracket for attaching the steering column assembly to the vehicle. A rake bracket is coupled to the mounting bracket, and is pivotable relative to the mounting bracket about a rake axis. The rake bracket extends from the mounting bracket along a longitudinal axis to a distal end. A column jacket is supported by the mounting bracket and detachable supported by the rake bracket. The column jacket is longitudinally moveable relative to the mounting bracket along the longitudinal axis in response to an emergency event. The column jacket is also pivotably moveable with the rake bracket relative to the mounting bracket about the rake axis. An instrument cluster is coupled to the distal end of the rake bracket. The instrument cluster is rotatably moveable with the rake bracket and the column jacket relative to the mounting bracket about the rake axis.
Accordingly, the subject invention provides a steering column assembly in which the instrument cluster is coupled to the rake bracket. The instrument cluster moves with the rake bracket as the steering column assembly is adjusted about the rake axis to maintain an unobstructed view of the instrument cluster. The instrument cluster is not directly mounted onto the column jacket and therefore does not interfere with the collapse of the column jacket in response to the emergency event.
BRIEF DESCRIPTION OF THE DRAWINGS
Other advantages of the present invention will be readily appreciated, as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings wherein:
FIG. 1 is a perspective view of a steering column assembly;
FIG. 2 is a side view of the steering column assembly shown in FIG. 1 ;
FIG. 3 is a schematic side view of the steering column assembly;
FIG. 4 is a perspective view of a first alternative embodiment of the steering column assembly;
FIG. 5 is a partial fragmentary perspective view of the first alternative embodiment of the steering column assembly shown in FIG. 4 ;
FIG. 6 is a perspective view of a second alternative embodiment of the steering column assembly;
FIG. 7 is a partial perspective view of the second alternative embodiment of the steering column assembly shown in FIG. 6 ; and
FIG. 8 is fragmentary cross sectional perspective view of the second alternative embodiment of the steering column assembly shown in FIG. 6 .
DETAILED DESCRIPTION OF THE INVENTION
Referring to the Figures, wherein like numerals indicate corresponding parts throughout the several views, a steering column assembly is generally shown at 20 . The steering column assembly 20 is for a vehicle, and includes an energy absorption mechanism 22 . The energy absorption mechanism 22 absorbs energy transmitted through a column jacket 24 in response to an emergency event. The emergency event typically includes a vehicular impact. The energy absorption mechanism 22 reduces the amount of energy transmitted through the steering column assembly 20 , thereby reducing injury to a driver. There are several energy absorption mechanisms 22 known in the art capable of absorbing energy transmitted through the steering column assembly 20 that may be incorporated into the subject invention. Accordingly, the energy absorption mechanism 22 is not described in detail herein, and the scope of the claims should not be limited to the exact configuration or type of energy absorption mechanism 22 utilized.
Referring to FIGS. 1 and 2 , the steering column assembly 20 comprises a mounting bracket 26 for attachment to the vehicle. A rake bracket 28 is coupled to the mounting bracket 26 and also to the vehicle. The rake bracket 28 is pivotable relative to the mounting bracket 26 about a rake axis R, and extends from the mounting bracket 26 along a longitudinal axis L to a distal end 30 . The mounting bracket 26 includes a hinge 32 extending transverse to the longitudinal axis L, with the hinge 32 defining the rake axis R therethrough.
The steering column assembly 20 further comprises a rake adjustment mechanism 34 . The rake adjustment mechanism 34 rotationally adjusts the column jacket 24 and the rake bracket 28 about the rake axis R relative to the mounting bracket 26 . The rake adjustment mechanism 34 also locks the column jacket 24 and the rake bracket 28 in position relative to the mounting bracket 26 . There are several known rake adjustment mechanisms 34 capable of adjusting and locking the rake position of the column jacket 24 and the rake bracket 28 that may be incorporated into the subject invention. Accordingly, the rake adjustment mechanism 34 is not described in detail herein, and the scope of the claims should not be limited to the exact configuration or type of rake adjustment mechanism 34 utilized.
The column jacket 24 is supported by the mounting bracket 26 and detachably supported by the rake bracket 28 . The column jacket 24 is longitudinally moveable relative to the mounting bracket 26 along the longitudinal axis L in response to an emergency event, i.e., the column jacket 24 is collapsible in response to an emergency event. The column jacket 24 is also pivotably moveable with the rake bracket 28 relative to the mounting bracket 26 about the rake axis R. A steering wheel 36 is attached to an end of the column jacket 24 as is well known in the art.
An instrument cluster 38 is coupled to the distal end 30 of the rake bracket 28 . The instrument cluster 38 is rotatably moveable with the rake bracket 28 and the column jacket 24 relative to the mounting bracket 26 about the rake axis R. The instrument cluster 38 includes an outer casing 40 , preferably manufactured from a plastic material. At least one gauge 42 , and preferably a plurality of gauges 42 are supported by the outer casing 40 . The gauges 42 typically include a speedometer, a tachometer, a fuel gauge, a temperature gauge, an oil pressure gauge, etc. It should be understood that the number and kind of gauges may vary depending upon the vehicular requirements, and that the scope of the claims are not limited to the number and kind of gauges.
Referring also to FIG. 3 , which is a schematic representation of the steering column assembly 20 , the steering column assembly 20 further comprises a dynamic absorber 44 interconnecting the instrument cluster 38 and the rake bracket 28 . The column jacket 24 and the attached steering wheel 36 vibrate at a resonance frequency as is well known in the art. The dynamic absorber 44 reduces the vibration transmitted to the instrument cluster 38 and also the vibration in the steering wheel 36 . Preferably, the dynamic absorber 44 includes a linear spring 48 having a pre-determined spring constant K z . The linear spring 48 supports the instrument cluster 38 , which includes a mass M z . The dynamic absorber 44 and the instrument cluster 38 are therefore cantilevered from the rake bracket 28 . Accordingly, the mass M z of the instrument cluster 38 is coupled to the rake bracket 28 by the spring constant K z and cooperate together to counteract the vibration in the column jacket 24 to reduce the overall vibration in the instrument cluster 38 and the steering wheel 36 . The linear spring 48 includes a cluster bracket 46 . The cluster bracket 46 includes a flange 50 interconnecting the cluster bracket 46 and the instrument cluster 38 . Accordingly, it should be understood that the outer casing 40 is attached to the flange 50 of the cluster bracket 46 . The instrument cluster 38 is fixedly mounted to the dynamic absorber 44 , and is therefore stationary relative to the mounting bracket 26 in response to the emergency event. It should be understood that the dynamic absorber 44 may include some other device capable of reducing vibration in the column jacket 24 . Accordingly, the scope of the claims should not be limited to the exact configuration of the dynamic absorber 44 described herein.
As depicted in the embodiment shown in FIGS. 1 and 2 with reference to the schematic representation shown in FIG. 3 , the dynamic absorber 44 is integral with the rake bracket 28 . As such, the linear spring 48 is an extension of the rake bracket 28 . The pre-determined spring constant K z is therefore dependent upon the geometric design of the dynamic absorber 44 and the material utilized to manufacture the dynamic absorber 44 . As is known in the art, the ability to reduce vibration is a factor of the spring constant K z and the mass M z of the object interconnected by the dynamic absorber 44 . Accordingly, the effect on vibration in the steering column assembly 20 by the dynamic absorber 44 is dependent upon the mass M z of the instrument cluster 38 and the spring constant K z of the dynamic absorber 44 . Knowing the mass of the instrument cluster 38 and the physical properties of the material utilized for the dynamic absorber 44 , one skilled in the art can customize the exact shape and configuration of the dynamic absorber 44 to best fit the specific design considerations and requirements.
It should be understood that upon an emergency event, the column jacket 24 collapses along the longitudinal axis L. As the column jacket 24 collapses, the column jacket 24 detaches from the rake bracket 28 as is well known in the art. Accordingly, the instrument cluster 38 remains fixed in place, continuously attached to the rake bracket 28 and stationary relative to the mounting bracket 26 and the instrument panel, thereby permitting proper operation of the collapsible column jacket 24 and the energy absorption mechanism 22 .
A first alternative embodiment of the steering column assembly is generally shown at 120 in FIGS. 4 and 5 . A second alternative embodiment of the steering column assembly is generally shown at 220 in FIGS. 6 through 8 . Features of the steering column assembly 20 shown in FIGS. 1 and 2 that correspond to Features of the first alternative embodiment shown in FIGS. 4 and 5 are represented by the same reference numeral preceded by the numeral “1”. Accordingly, the steering column assembly 20 shown in FIGS. 1 and 2 is referenced in the first alternative embodiment as the steering column assembly 120 . Likewise, features of the steering column assembly 20 shown in FIGS. 1 and 2 that correspond to features of the second alternative embodiment shown in FIGS. 6 through 8 are represented by the same reference numeral preceded by the numeral “2”. Accordingly, the steering column assembly 20 shown in FIGS. 1 and 2 is referenced in the second alternative embodiment as the steering column assembly 220 .
Both the first and second alternative embodiments of the steering column assembly 120 , 220 further comprise a telescoping mechanism 152 , 252 . The telescoping mechanism 152 , 252 adjusts the column jacket 124 , 224 axially along the longitudinal axis L. Also, the telescoping mechanism 152 , 252 locks the column jacket 124 , 224 in position relative to the mounting bracket 126 , 226 . There are several known telescoping mechanisms 152 , 252 capable of adjusting and locking the telescoping position of the column jacket 124 , 224 that may be incorporated into the subject invention. Accordingly, the telescoping mechanism 152 , 252 is not described in detail herein and the scope of the claims should not be limited to the exact configuration or type of the telescoping mechanism 152 , 252 utilized.
Referring to the first alternative embodiment shown in FIGS. 4 and 5 , the rake bracket 128 is axially adjustable along the longitudinal axis L with the column jacket 124 . The rake bracket 128 is in telescopic engagement with the mounting bracket 126 for axial movement along the longitudinal axis L relative to the mounting bracket 126 . The dynamic absorber 144 is fixedly mounted to the rake bracket 128 , and the instrument cluster 138 is fixedly mounted to the dynamic absorber 144 . It should be understood that the dynamic absorber 144 of the first alternative embodiment is identical to and operates in the same manner as the dynamic absorber 44 described in relation to FIGS. 1 through 3 .
The steering column assembly 120 of the first alternative embodiment allows the instrument cluster 138 to move with the column jacket 124 in both the rake direction and the telescoping direction during normal use. In response to the emergency event, the column jacket 124 collapses. As the column jacket 124 collapses, the column jacket 124 detaches from the rake bracket 128 and the instrument cluster 138 . The instrument cluster 138 , being fixedly mounted to the rake bracket 128 via the dynamic absorber 144 , remains stationary relative to the mounting bracket 126 and the instrument panel, thereby permitting proper operation of the collapsible column jacket 124 and the energy absorption mechanism 122 .
Referring to the second alternative embodiment shown in FIGS. 6 through 8 , the dynamic absorber 244 includes an arm 254 in telescopic engagement with the rake bracket 228 . The instrument cluster 238 is fixedly mounted to the dynamic absorber 244 and is axially moveable with the dynamic absorber 244 along the longitudinal axis L relative to the mounting bracket 226 in response to the emergency event. The dynamic absorber 244 defines a notch 256 , and a release capsule 258 is disposed in the notch 256 . A pin 260 extends through the column jacket 224 , the release capsule 258 and the rake bracket 228 for interconnecting the column jacket 224 , the dynamic absorber 244 , and the rake bracket 228 . It should be understood that the dynamic absorber 244 of the second alternative embodiment is identical to and operates in the same manner as the dynamic absorber 44 described in relation to FIGS. 1 through 3 .
The steering column assembly 220 of the second alternative embodiment allows the instrument cluster 238 to move with the column jacket 224 in both the rake direction and the telescoping direction during normal use. In response to the emergency event, the column jacket 224 collapses. As the column jacket 224 collapses, the dynamic absorber 244 and the column jacket 224 remain coupled together, and both the column jacket 224 and the dynamic absorber 244 detach from the rake bracket 228 . Accordingly, both the column jacket 224 and the dynamic absorber 244 collapse, and the instrument cluster 238 thereby moves relative to the mounting bracket 226 and the instrument panel during the emergency event.
The invention has been described in an illustrative manner, and it is to be understood that the terminology which has been used is intended to be in the nature of words of description rather than of limitation. As is now apparent to those skilled in the art, many modifications and variations of the present invention are possible in light of the above teachings. It is, therefore, to be understood that within the scope of the appended claims, wherein reference numerals are merely for convenience and are not to be in any way limiting, the invention may be practiced otherwise than as specifically described.
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A steering column assembly includes a rake adjustment mechanism, and is attached to a vehicle by a mounting bracket. A rake bracket is coupled to the mounting bracket. A column jacket is collapsible in response to an emergency event and is supported by the mounting bracket and the rake bracket, and is rotationally moveable with the rake bracket about a rake axis relative to the mounting bracket. An instrument cluster is coupled to the rake bracket for movement along with the rake bracket and the column jacket to prevent obstruction of the instrument cluster by a steering wheel upon re-positioning the steering wheel, while not restricting movement of the column jacket during collapse of the column jacket in response to the emergency event. A dynamic absorber interconnects the instrument cluster and the rake bracket to reduce vibration of the steering column assembly caused by additional weight of the instrument cluster.
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This is a continuation-in-part of my copending application Ser. No. 618,467, filed Nov. 27, 1990, now abandoned which is a continuation of my application Ser. No. 383,404, filed Jul. 24, 1989 and now abandoned.
BACKGROUND OF THE INVENTION
This invention relates to pet litter containing water-activated adhesive material to bind the litter particles together when activated by liquid excreta from the pet. In particular, it relates to pet litter treated with liquid-activated adhesive material that forms clumps of good structural integrity to permit the affected material to be easily separated from litter material that has not been contaminated by pet excreta.
Many of the brands of pet litter now on the market have been treated to control odor, dust, and bacteria but not for the specific purpose of forming clumps that allow easy separation of the clumped material from the particular material that has not been in contact with the pet excreta.
When a pet deposits liquid excreta, normally urine, on a bed of untreated litter, the liquid progresses down through the particulate material and wets the particles as it comes to them. The litter is commonly said to absorb the liquid, although it may be more accurate to say that the liquid is adsorbed on the many surfaces of the particulate material. For the sake of simplicity in the following description, the words "sorption" and "sorbent", which cover both, will be used. The force of adhesion causes the wetted particles to cling together to some extent, but this force is not very strong and it substantially entirely disappears when the liquid evaporates. As a result, there is little or no clumping effect, and the only way to be certain of getting rid of litter that has been affected by the urine, is to dispose of the entire tray of litter. While this need not be done after every use by the pet, it is usually done by pet owners at least about once a week in order to avoid the build-up of obnoxious odors in the vicinity of the litter tray.
Even litter that has odor-controlling material in it, must be disposed of every few days. Since there is no way of separating litter that has come in contact with the pet urine from litter that has not, it is common to throw away the entire contents of the litter tray and to replace it with a new bed of litter. This means that a considerable quantity of litter will be used, and a recent study indicated that pet owners typically use about 15 kg of pet litter per month. Not only is there a constant expense involved in replacing litter so frequently, there is also a considerable problem of disposing of the used material, particularly by pet owners who live in apartments or who, for any reason, are unable to remove the used litter to an acceptable disposal location.
OBJECTS AND SUMMARY OF THE INVENTION
The principal object of this invention is be able to separate out litter that has been contaminated by liquid excreta from pets from a mixture of that litter with litter that has not been thus contaminated.
Another object is to achieve such separation easily by mechanical means.
A further object is to provide pet litter that includes non-toxic adhesive material to form clumps that have good structural integrity when activated by liquid in excreta from pets. Good structural integrity means that the clumps do not easily break apart when being removed from litter that remains in particulate form due to never having come in contact with liquid excreta from pets.
In accordance with this invention, a suitable non-toxic, urine-activated adhesive material is mixed with the basic particulate litter material, which is commonly a clay, such as southern bentonite, in proportions to form clumps of good structural integrity when contacted by liquid excreta from pets. Suitable adhesive materials include: starches, such as wheat paste; cellulosic materials, such as methylhydroxypropylcellulose (MHPC), sodium carboxymethylcellulose (CMC), methylcellulose (MC), and Metylan Cellulose; and mixtures of the foregoing materials with each other and with gums, such as gum arabic.
The adhesive material is mixed as a dry powder with the powdered, or particulate, litter material to produce a coating of the adhesive material on all of the particles of litter material. This assures that any particle of litter material that comes into contact with liquid from the pet will have adhesive material on that particle to be activated by the liquid and to bond that particle of litter material with any other particle with which the activated adhesive comes into contact. Thus, substantially all of the wetted, adhesive-coated litter particles will bind together in a clump of sufficient size and structural integrity to be easily separated by mechanical means from the unaffected particulate material that has not been wet. One form of mechanical means is a hand-held scoop, but other mechanical means can also be used.
DETAILED DESCRIPTION OF THE INVENTION
A wide variety of commercial pet litters have been tried, including a premium white grade of clay, several gray clays, and a dark gray generic clay. Most of the litter material is finely ground, but I have also found that litter material in the form of tiny pebbles, which may be referred to as agglomerated material, is also satisfactory. While white clay is the preferred litter material, the gray and dark gray clays are also satisfactory.
A number of factors would determine which brand and type of pet litter would be best for commercial use in the product of this invention. Economic considerations naturally rank high. Other factors include odor control, clump mass per unit wetting, dust control, and the strength and toughness of the clumps.
Odor control is of distinct benefit. Some litters currently on the market use a perfume on the litter; others incorporate the odor-controlling material in microcapsules. Odor protection is more crucial in high-humidity environments. In low humidities, the mixtures exude only a scant odor after more than a month of use if the mechanical cleaning procedure is executed every couple of days. If left unused, this mechanically cleaned litter will completely lose its odor after several days, indicating that the odor was generated by airborne permeation rather than direct contamination by the waste. Deodorized litters are meant to mask the strong odors generated by large quantities of waste left for a dozen or more days, and thus the deodorant materials provide more masking power than is required when the odor-producing pet excreta is removed every few days, as the present invention makes possible. Even so, they are helpful. I have found it beneficial to add about 1% to 10%, by weight, of baking soda for odor reduction (low pH) to adhesives in the range of about 0.1% to about 25%, by weight, of the total mixture.
The adhesive added to the litter material must meet several, main requirements: it must be activated by pet urine and liquid in other forms of pet excreta, it must bond with the litter material, and it must not be toxic. It is also important that the adhesives be cost-effective and that they have good shelf life. While pet urine contains chemicals other than water, water is the main constituent, and by tests, I have found that there is not much difference between water and pet urine in initiating the clumping action toward which this invention is directed.
Many types of water-activated adhesives can be employed to accomplish the clumping function with litter material that takes up liquid. They can be categorized into starches, cellulose, and gums.
Of the starches, I have found that wheat paste, when used in the ratio of at least about 2% to about 25%, by weight, relative to the mixture of adhesive and litter material, is quite satisfactory. Preferably, the ratio of wheat paste to the total mixture should be about 8% to about 14%. Wheat paste is a pre-gelatinized starch that does not require the heating and swelling processes that must be carried out on raw starches prior to bonding them to the litter material. However, for optimum performance, wheat paste requires generally larger percentages of adhesive in the mixture of adhesive and litter material than do some other adhesives. Also, clumps formed of litter material mixed with wheat paste require several hours to harden fully, although they harden sufficiently in an hour to be easily separable from litter material that has not been wet.
A large family of suitable adhesives is derived from processes involving various forms of vegetable cellulose. These materials are more expensive per pound than wheat paste, but the quantity of a vegetable cellulose adhesive that must be used is much smaller than the quantity of wheat paste to achieve equal clumping action. The processed cellulosic adhesives are further modified by addition of other substances, usually inorganic substances, to meet specific application needs. I have found several cellulosic adhesives to be particularly satisfactory, including: methylhydroxypropylcellulose (MHPC), sodium carboxymethyl-cellulose (CMC), and methylcellulose (MC). These materials are sold by the Aqualon Division of Henkel-Hercules Company. I found that CMC is the most effective cellulose material, but another cellulose product, also manufactured by Aqualon but distributed by Conros Adhesives of Michigan as a high-strength wallpaper adhesive under the trade name Metylan Cellulose, is quite effective, with a performance roughly equivalent to CMC. Satisfactory clumps can be produced using a mixture of clay litter and either CMC or Metylan Cellulose in a mixture which the weight of the adhesive is at least about 0.1% of the total weight. Increasing the amount of these adhesives beyond 10% of the total weight produces little or no further improvement in clump-forming ability, and preferably, the weight of these adhesives should be between 0.7% and 2.65%.
MC is the second most effective adhesive and forms satisfactory clumps when mixed with the clay litter material when the weight of MC is in the range of about 0.1% to about 10%, or, preferably, between about 0.7% and 2.65%, of the total weight of the mixture of adhesive and litter. MHPC is somewhat less effective but is still satisfactory in the range of about 0.1% to 10%, or, preferably, between about 0.7% and 2.65%, of the total mixture weight.
Several gums have been tried with less success than the cellulose materials. Tamarind gum has characteristics that make it satisfactory as an adhesive, but its shelf life is not as good as desired. Gum arabic was tried as a substitute for tamarind, but the results were poor.
I have found that the dry, powdered, adhesive material can best be mixed with dry litter material by first mixing some of the adhesive material with a small amount of litter material, preferably in a ratio of adhesive-to-litter that is about 10 times the final ratio of adhesive-to-litter material. This distributes the fine particles, or granules, of litter material more evenly in the mixture and avoids forming regions that consist almost entirely of adhesive and other regions that contain almost no adhesive. The two-stage mixing process is particularly advantageous in the case of cellulosic adhesives since they are used in much smaller quantities than is wheat paste. After vigorous mechanical agitation, the rest of the litter material is added, and the mixture is again vigorously shaken to allow the adhesive powder to coat the litter particles or granules fully.
One of the tests I made was to measure the clump mass per unit volume of the water used in forming the clump. This is relevant and important because, the larger the clumps for a given volume of liquid, the more litter material will be used up as the result of each usage of the litter tray by a pet. However, large clumps can be more easily separated from unclumped material than smaller clumps can.
In the clump size test, the following results were obtained:
Water Tests
TABLE 1______________________________________ Clump Mass (gm)Adhesive Type Litter Type per gm. water______________________________________Wheat paste White premium 2.18Wheat paste Dark gray generic 2.54Metylan Cellulose #1 Gray #1 2.64Metylan Cellulose #1 White premium 3.13Metylan Cellulose #1 Gray #2 3.19Metylan Cellulose #1 Gray #3 2.25Metylan Cellulose #2 Gray #1 2.12Metylan Cellulose #2 White premium 2.76Metylan Cellulose #2 Gray #2 2.15CMC White premium 1.96Metylan Cellulose #2 Gray #1 2.03______________________________________ (37 gms. per clump) Metylan Cellulose #1 = Special Vinyl Conros Wallpaper Paste Metylan Cellulose #2 = Metylan Cellulose Prof. Paste
In this test, the white premium clay to which CMC had been added as a water-activated adhesive was the most efficient in that less litter was used in forming a clump with a given weight of water.
In forming each clump, 37 gms. of water were used since I had determined from separate tests in a litter box that the clumps formed by cat urinations averaged out to about the same size as clumps formed by approximately 37 gms. of water.
Water was used in most of the experiments. Where a correlation was made with cat urine, the results were close enough to validate the water tests.
Clump strength, or structural integrity, is of primary importance since it determines how well clumps can be mechanically separated from particles. I have employed several methods of measuring clumps in efforts to quantify this parameter: by hardness, toughness, and subjective clump integrity ratings.
All of these qualities are important in forming clumps that do not fall apart or shatter when the bed of litter is raked or otherwise shifted around to separate the clumps from the litter that has not been wetted. Three test methods were used to check different formulations of litter and adhesive with respect to these qualities. These test methods are:
Test Method #1--Subjective Rating
A quantity of water, 37 gms., was added to the mixture of adhesive and litter materials to form clumps, and clump tensile strength was evaluated on a scale of 1-5 (5 being highest) by judging subjectively how difficult it was to pull each clump apart by hand. The stronger the clump, the higher the value.
Test Method #2--Clump Toughness
A quantity of water, 37 gms., was added to the mixture of adhesive and litter material and the resulting clump was weighed. The clump was then dropped from 30 cm. onto a grid of 3/16" wooden dowels that were approximately 45 cm. long and were spaced 6 mm. apart. The mass remaining above the grid was then reweighed and that weight divided by the original weight to obtain a percentage representative of the toughness of the clump.
Test Method #3--Clump Hardness
The clump mass, generally measuring about 60 mm. diameter in roughly spherical form, was set on a scale. The side of a 3/16" dowel that extended parallel to the scale platform was forced down against the uppermost surface of the clump until a general split or collapse of the clump occurred. As the pressure on the clump increased, the scale reading increased as if more weight were being put on the platform. The maximum reading registered on the scale minus the clump weight (in oz.) was considered to be representative of the hardness value.
Table 2 summarizes my findings on the strength of clumps formed with different constituents and tested by the three foregoing tests:
TABLE 2______________________________________Clump Strength Summary Test Avg.Adhesive Type Type Litter Method Value______________________________________(CMC & MC in Gray #1 1 1.5various ratios) White premium 1 3.5(Metylan Cellulose Gray #1 2 91.1%#2 various ratios) White premium 2 92.0%(Metylan Cellulose Gray #2 2 90.6%#2 various ratios) Gray #3 2 86.8%(Metylan Cellulose Gray #1 2 89.7%#1 various ratios) White premium 2 93.0(Metylan Cellulose Gray #2 2 89.0#1 various ratios)(Metylan Cellulose Gray #3 2 78.3#1 various ratios)(Wheat paste at Dark gray generic 2 77.8various ratios) White premium 2 85.6(Wheat paste Dark gray generic 3 6.04 oz.6-25% ratios) White premium 3 10.04 oz.______________________________________
The majority of the data and derived conclusions were based on a designed experiment approach specifically employing Taguchi fractional factorial matrices. These procedures show whether average differences observed between variables are the result of chance or are statistically significant. In addition, the procedures determine whether the effect is present in the global sense or just at that particular level of the other variables involved.
Several tests were conducted by wetting untreated litter with 37 gms. of water to determine the clumping ability of litter without any clumping adhesive present. All results showed near zero readings on all three test measurements employed. This was consistent with the assumption that, in the absence of a specific adhesive, the only thing holding the grains together was the force of adhesion between the grains and the water. When the water evaporated, this small force disappeared.
Mixtures of various percentages of CMC with white premium litter in which CMC constituted between about 1% and about 10% of the total weight of the mixture were tested for clump toughness by test method #2. Some of the tests were performed about 1 hour after water was added to the dry mixture and other tests, using the same method #2, were performed about 72 hours after the water was added. The results showed an average toughness value of about 93%.
Mixtures of Metylan Cellulose #2 and white premium litter in which the weight of the Metylan Cellulose constituted between about 1% and about 10% of the weight of the total mixture were tested for clump toughness by test method #2 and yielded average toughness values of 86-97%. However, when the amount of Metylan Cellulose was reduced so that it constituted only about 0.6% of the mixture, the result obtained by applying test method #2 dropped sharply to about 49%, which compared poorly with the toughness value at 1% of the total weight. The cost of the cellulosic adhesives makes it inadvisable to go above 10%, and, in fact, I have found that 2.65% is a perfectly satisfactory maximum weight of these adhesives in comparison with the total weight of the product comprising litter material and the adhesive.
Four sets of tests were run to determine the effects of varying the components, procedures, and times. The test variables, the parenthetical explanatory remarks, and the conclusions drawn from the test are described next.
First Set of Tests
Wheat paste was the only adhesive used in this test.
Test Variables
Stratification of mixture; (by dropping a container of the dry mixture of adhesive and litter 20 times vs. not dropping it at all)
Mixture wetting; (using no water vs. using an extremely low mist while mixing adhesive with litter)
Ratio of weight of wheat paste to total weight of mixture; (6%, 8%, 12%, 25%)
Fines; (fines removed by passing the mixture across a plate having a 2.65 mm. gap to sieve the mixture vs. not sieving it)
Depth of bed of litter in litter tray; (having a deep bed of 4-5" vs. having a shallow bed of 1-2")
Litter Type; (white premium vs. dark gray generic)
Sample size, or quantity of water/clump; (large sample based on 36 gms. of water vs. small sample based on 10 gms. of water, corresponding to the fact that pets do not expel the same amount of urine each time)
Results
These clumps were tested for hardness using test method #3 with readings given in oz.
(a) A first series of such tests was performed about 1 hour after adding the water. The results were:
Overall average 8.04.
White premium litter was 10.04 vs. 6.04 for dark gray generic.
Tests made with litter from which fines had been removed yielded a value of 10.58 vs. 5.50 as packaged.
With stratification gave 9.58 vs. 6.50 without.
(b) A second series of tests run after the material had had about 11 hours to harden gave the following results:
Overall average was 26.70.
White premium litter was 34.7 vs. dark gray generic value of 18.7.
With stratification was 31.3 vs. 22.10 without.
Small sample size yielded a value of 35.5 vs. 17.91 for the large sample.
Shallow bed 30.6 vs. 22.83 deep bed.
An interaction was noted between container depth and sample size.
All other variables were insignificant.
Conclusions
The results of this set of test showed that white premium clay litter produced harder clumps than dark gray generic and that removing the fines may have eliminated particles of litter so small that they had no adhesive on them. The stratification results showed that the jouncing expected to be encountered when containers of mixture are shipped does not have an adverse effect on clump hardness and is even somewhat beneficial.
The difference between the results after 11 hours as compared with those after 1 hour showed that clumps formed with wheat paste as the adhesive grew harder with time. In addition, the use of a deep bed of litter was somewhat preferable to using a shallow bed.
Second Set of Tests
Wheat paste was the only adhesive used in this set of test.
Test Variables
Stratification; (by dropping a container of dry, mixed adhesive and litter 20 times vs. not dropping it at all)
Ratio of the weight of wheat paste to the total weight of the mixture of adhesive and litter; (6%, 8%, 12%, 25%)
Fines; (fines removed by being sieved through a 2.65 mm. gap vs. fines not being removed)
Litter type; (white premium vs. dark gray generic)
Amount of water used per clump; (36 gms. vs. 10 gms.)
Results
The samples in this set of test were checked for toughness by test method #2 two hours after putting the water in the dry mixture. The only significant variable in these samples was the ratio of the weight of wheat paste to the total weight of the mixture.
______________________________________Ratio of weight of wheat Weight of clump remaining on gridpaste to total weight as percent of initial clump______________________________________ 6% 64% 8% 70%12% 75%25% 88%______________________________________
Conclusions
While there is some increase in the toughness of the clumps with an increase in the amount of wheat paste, increasing the amount of wheat paste to four times the original value increased the toughness by only 40%.
Third Set of Tests
Wheat paste was the only adhesive used in this set of tests.
Test Variables
Time from wetting to measurement; (2.5 hrs. vs. 8 hrs.)
Litter type; (white premium vs. dark gray generic)
Amount of wheat paste in the mixture; (either: (1) a quantity of wheat paste far in excess of 14% of the total mixture was vigorously mixed with the litter material and then the mixture was sieved to remove excess wheat paste, the particles of which were much smaller than particles of the litter material; or (2) an amount of wheat paste approximately equal to 14% of the total weight of the mixture was used. The first is identified as "excessive and sieved" and the second "14% paste".)
Results
The foregoing samples were checked for toughness by test method #2 with the following results:
Overall average was 80.43%.
White premium litter was 87.1% vs. 78% for dark gray generic litter. 14% paste was 92.7% vs. 73% for excessive and sieved paste.
Other variables were insignificant.
Conclusions
This set of tests showed that white premium litter was somewhat better than dark gray generic litter and that using an excessive amount of wheat paste was not as satisfactory as using 14%.
Fourth Set of Tests
Test Variable
Ratio of adhesive weight to total weight of the mixture; (0.7%, 1.35%, 2.0%, 2.65%)
Adhesive type; (CMC vs. MC)
Litter type; (gray #1 vs. white premium)
Results
Based on using toughness test method #2 two hours after water had been applied to the mixture, the average toughness value for CMC was 91% and for MC was 81%.
At the following ratios of the weight of the adhesive to the weight of the total quantity of the mixture, the values were:
______________________________________ .7% 1.35% 2.0% 2.65%______________________________________MC 79% 89% 65% 92%CMC 90% 92% 91% 94%______________________________________
Based on using test method #1 to test the tensile strength of the clumps, the following values were determined:
For white premium, the value was 3.5 vs. 1.5 for Gray #1.
For CMC, the value was 3.0 vs. 2.25 for MC.
At the following ratios of the weight of the adhesive to the weight of the total quantity of the mixture, the values were:
______________________________________ .7% 1.35% 2.0% 2.65%______________________________________MC 2.7 1.7 1.7 3.0CMC 2.0 4.5 3.8 1.6______________________________________
Conclusions
The clumps produced when CMC is the adhesive are somewhat tougher than those produced using MC. When the weight of the adhesive is between about 0.7% and 2.0% of the total weight of the mixture, the tensile strength of clumps made from a mixture that had CMC as the adhesive component was greater than that of clumps made from a mixture that contained MC.
Overall, the most satisfactory mixtures have been:
(1) White cat litter material and common wheat paste adhesive material in powdered form mixed together as a dry mixture by vigorous mechanical agitation, with the weight of the adhesive material being between about 11% and 14% of the total weight of the mixture;
(2) Premium white cat litter material in a dry mechanical mixture with CMC or MC as an adhesive material in powdered form and constituting about 1.2% to about 1.4% of the weight of the total product, including the litter material and the adhesive material. In the case of MC, it is preferable, but not necessary, to use a high molecular weight CMC; and
(3) Premium white grade or other cat litter in mechanical mixture with about 2.5% by weight of Metylan Cellulose.
Using these mixtures and mechanically cleaning clumps out of the litter tray each day resulted in usage of about 2 kg., or less, per month of the mixture per cat as compared with a mean of about 15 kg. per month determined by a recent survey of cat owners. The specific amounts of my product used in a household having two cats is shown in Table 3.
TABLE 3______________________________________Litter Box TrialsAdhesive Type Litter Type gms./day usage______________________________________Metylan Cellulose #2 White premium 95.3Metylan Cellulose #2 Gray #1 113.5Wheat Paste White premium 131.7CMC White premium 100.0______________________________________
The amount of litter used per day was also determined by another series of tests on numerous types of clay litter mixed with varying percentages of adhesives. These tests were conducted in actual litter box usage by two adult cats weighing about 10 lbs., each. For each formulation of litter material, the response variable measured was the weight loss in litter per day. The clumps were carefully scooped out to make their removal uniform. Assuming that the cat excretion was also constant, the loss of weight of the litter material would be an indication of the clumping performance of the adhesive. It was expected that the weight of the litter tray would increase each day due to the addition of excreta, although some loss would be expected to occur due to evaporation and to the amount thrown out by the cats during use of the tray. Removal of the clumps formed by reason of the adhesive would be the major cause of loss of weight of the litter material in the tray, and a measure of the weight lost was made to determine the effectiveness of removal of the urine via the clumps. The number of clumps found and their general integrity were also determined.
Table 4 summarizes these tests. Hartz Mountain Corp. cat litter was used in tests A, C, E, and F. Test B was made with white Georgian clay supplied by Georgia Tennessee Mining Co., a subsidiary of Hartz Mountain Corp. Other commercially available floor sorbents were used in tests G-I. Test H was made using a clumping clay cat litter marketed by Oil-Dri Corp. It is not known to contain any additives and therefore relies on moisture-related adhesion for clump strength. Tests indicated that, although it presented a removable clump following liquid application, the clump was substantially too weak, or was nonexistent, for removal after a day's period of time.
Tests C-F depict decreasing adhesive concentrations, with litter mass dropping to -1.30 lbs/day, i.e., a gain in weight due to accumulation of urine, when no adhesives were employed. Even as little as 0.14% CMC can be seen to have a positive effect on clump formation, resulting in a loss of -0.072 lbs./day.
Clump size, quantity, and quality were also recorded, indicating that even when the weight percentage of the adhesives relative to the total weight of the litter and adhesive mixture was as low as 0.14%, some beneficial effect was obtained by having the adhesives in the litter material.
TABLE 4__________________________________________________________________________ Lbs. lost Avg. # clumps Avg. oz. % sub- Avg # days Duration ofType litter % Adhesive per day per day per clump st'd'd clumps betw. clean. test__________________________________________________________________________ (days)A Hartz 1% CMC 2% WP .37 3.2 1.85 6.2% 2.5 15 7% Baking SodaB Floor Absor- 1% CMC 2% WP .31 3.8 1.85 3.7% 2.3 16 bent, Georgia Tenn MiningC Hartz 1% CMC 2% WP .23 3.0 1.21 26% 2.1 36D Hartz 0.3% CMC .028 2.2 0.20 34% 2.9 17E Hartz 0.14% CMC -.072 0.57 N/A 50% 2.8 14F Hartz No Adhesive -.130 0 N/A N/A 2.5 10G Floricon X 1% CMC 2% WP .23 3.61 1.02 41% 1.6 16 Floridon Co.H Lasting Pride No Adhesive 0* N/A N/A 100% 1.25 5I Absorball K 1% CMC 2% WP .083 3.66 .36 50% 1.50 6 Absorbent Sales, Inc.__________________________________________________________________________ *It was found at each time of cleaning that all clumps had disintegrated. However, clumps were observed to exist for a limited period of time after the cats urinated. CMC = AqualonSodium Carboxymethylcellulose Type 7H3SFX Tests conducted with 2 cats, 10 lbs. each
The same ratio of adhesive to litter was used in the litter material in both test A and test C, but in test A, the litter material also contained 7%, by weight, of baking soda. Comparison of these tests shows that both the weight loss and the clump size are substantially higher with the baking soda than without it, indicating that the use of baking soda is beneficial in clump formation. It is also beneficial in odor reduction.
The overall conclusion to be drawn from the test results in Table 4 is that adhesives, even in amounts that are nearly immeasurable, have a beneficial effect on forming clumps in response to liquid excreta from pets, but that the preferred amount of adhesive, as a percentage of the total weight of the litter material, should be at least a large fraction of one percent.
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A particulate material having liquid-responsive, adhesive material mixed with sorbent material in particulate form to be wet. After being wet, the adhesive material dries and causes particles that have been wet to adhere together in clumps that can easily be separated from the particles that have not been wet.
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FIELD OF THE INVENTION
[0001] This invention relates in general to the use of 4amino-azepan-3-one protease inhibitors, particularly such inhibitors of cathepsin S, in the treatment of diseases in which cathepsin S is implicated, especially treatment or prevention of autoimmune disease; treatment or prevention of a disease state caused by the formation of atherosclerotic lesions and complications arising therefrom; and diseases requiring inhibition, for therapy, of a class II MHC-restricted immune response, inhibition of an asthmatic response, inhibition of an allergic response, inhibition of immune response against a transplanted organ or tissue, or inhibition of elastase activity in atheroma; and novel compounds for treating same.
BACKGROUND OF THE INVENTION
[0002] Cathepsins are a family of enzymes that are part of the papain superfamily of cysteine proteases. Cathepsins K, B, H, L, N and S have been described in the literature.
[0003] Cathepsins function in the normal physiological process of protein degradation in animals, including humans, e.g., in the degradation of connective tissue. However, elevated levels of these enzymes in the body can result in pathological conditions leading to disease. Thus, cathepsins have been implicated as causative agents in various disease states, including but not limited to, infections by pneumocystis carinii, trypsanoma cruzi, trypsanoma brucei brucei , and Crithidia fusiculata ; as well as in schistosomiasis, malaria, tumor metastasis, metachromatic leukodystrophy, muscular dystrophy, amytrophy, and the like. See International Publication Number WO 94/04172, published on Mar. 3, 1994, and references cited therein. See also International Publication Number WO 97/16433 , published on May 9, 1997, and references cited therein.
[0004] Pathological levels of cathepsin S have been implicated in a variety of disease states. For instance, mice treated with inhibitor exhibited attenuated antibody response indicating that selective inhibition of cathepsin S may provide a therapeutic strategy for asthma and autoimmune disease processes. Thus, selective inhibition of cathepsin S may provide an effective treatment for diseases requiring, for therapy or prevention: inhibition of a class II MHC-restricted immune response; treatment and/or prevention of an autoimmune disease state such as rheumatoid arthritis, multiple sclerosis, juvenile-onset diabetes, sytemic lupus erythematosus, discoid lupus erythematosus, pemphigus vulgaris, pemphigoid, Grave's disease, myasthenia gravis, Hashimoto's thyroiditis, scleroderma, dermatomysositis, Addison's disease, pernicious anemia, primary myxoedema, thyrotoxicosis, autoimmune atrophic gastritis, stiff-man syndrome, Goodpasture's syndrome, sympathetic opthalamia, phacogenic uveitis, autoimmune haemolytic anaemia, idiopathic thrombocytopenic purpura, idiopathic leucopenia, primary biliary cirrhosis, active chronic hepatitis, cryptogenic cirrhosis, ulcerative colitis, Sjogren's syndrome, and mixed connective tissue diease; inhibition of an asthmatic response; inhibition of an allergic response; inhibition of immune response against transplanted organ or tissue inhibition of elastase activity in atheroma; and treatment or prevention of a disease state caused by the formation of atherosclerotic lesions or complications arising therefrom.
[0005] We have now discovered that certain 4-amino-azepan-3-one compounds inhibit cathepsin S, and are useful in the treatment of diseases in which cathepsin S is implicated.
SUMMARY OF THE INVENTION
[0006] An object of this invention is the use of compounds of Formula I or II for inhibiting the activity of the protease inhibitors known as cathepsin S.
[0007] Another object of the present invention is to provide novel 4-amino-azepan-3-one carbonyl compounds of Formula II, as described below.
[0008] A further object of this invention is the use of a compound of Formula I or II in the manufacture of a medicament for treating or preventing a condition associated with the inhibition of cathepsin S.
[0009] Another aspect of this invention is that of a pharamceutical formulations comprising a compound of Formula II alone in admixture with a pharmaceutically acceptable excipient and administering this preparation to a mammal in need thereof in an amount effective for inhibiting cathepsin S to a degree which effects prevention of a condition or treatment of a condition associated with the inhibition of cathepsin S.
[0010] In a particular aspect, the methods of this invention are especially useful for treatment or prevention of autoimmune disease; treatment or prevention of a disease state caused by the formation of atherosclerotic lesions and complications arising therefrom; and diseases requiring inhibition, for therapy, of a class II MHC-restricted immune response, inhibition of an asthmatic response, inhibition of an allergic response, inhibition of immune response against a transplanted organ or tissue, or inhibition of elastase activity in atheroma.
DETAILED DESCRIPTION OF THE INVENTION
[0011] The present invention provides a method for treating a disease by inhibiting cathepsin S comprising administering at least one compound of Formula I neat or as a pharmaceutically acceptable formulation, in an effective amount, wherein Formula I comprises:
wherein:
[0012] R 1 is:
[0013] R 2 is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, Het-C 0-6 alkyl, R 9 C(O)—, R 9 C(S)—, R 9 SO 2 —, R 9 OC(O)—, R 9 R 11 NC(O)—, R 9 R 11 NC(S)—, R 9 (R 11 )NSO 2 —
[0014] R 3 is H or substituted or unsubstituted C 1-6 alkyl, C 3-7 cycloalkylC 0-6 alkyl, C 4-7 cycloalkenylC 0-6 alkyl, C 5-8 bicycloalkylC 0-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, HetC 0-6 alkyl, ArC 0-6 alkyl, Ar—ArC 0-6 alkyl, Ar-HetC 0-6 alkyl, Het-ArC 0-6 alkyl, or Het-HetC 0-6 alkyl;
[0015] R 3 and R′ may be connected to form a pyrrolidine, piperidine or morpholine ring;
[0016] R 4 is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, Het-C 0-6 alkyl, R 5 C(O)—, R 5 C(S)—, R 5 SO 2 —, R 5 NSO 2 —, R 5 OC(O)—, R 5 R 13 NC(O)—, or R 5 R 13 NC(S)—;
[0017] R 5 is H, C 1-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, Ar—ArC 0-6 alkyl, Ar-HetC 0-6 alkyl, Het-ArC 0-6 alkyl, Het-HetC 0-6 alkyl, or Het-C 0-6 alkyl;
[0018] R 6 is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0019] R 7 is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, Het-C 0-6 alkyl, R 10 C(O)—, R 10 C(S)—, R 10 SO 2 —, R 10 OC(O)—, R 10 R 14 NC(O)—, or R 10 R 14 NC(S)—;
[0020] R 8 is H, C 1-6 alkyl, C 1-6 alkenyl, C 2-6 alkynyl, HetC 0-6 alkyl or ArC 0-6 alkyl;
[0021] R 9 is C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl or Het-C 0-6 alkyl;
[0022] R 10 is C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl or Het-C 0-6 alkyl;
[0023] R 11 is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0024] R 12 is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0025] R 13 is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0026] R 14 is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0027] R′ is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0028] R″ is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0029] R′″ is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0030] X is CH 2 , S, or O;
[0031] Z is C(O) or CH 2 ; or
[0032] a pharmaceutically acceptable salt, hydrate or solvate thereof
[0033] This invention further provides the compounds of Formula II:
wherein:
[0034] R 1 is:
[0035] R 2 is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, Het-C 0-6 alkyl, R 9 C(O)—, R 9 C(S)—, R 9 SO 2 —, R 9 OC(O)—, R 9 R 11 NC(O)—, R 9 R 11 NC(S)—, R 9 (R 11 )NSO 2 —
[0036] R 3 is H or substituted or unsubstituted C 1-6 alkyl, C 3-7 cycloalkylC 0-6 alkyl, C 4-7 cycloalkenylC 0-6 alkyl, C 5-8 bicycloalkylC 0-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, HetC 0-6 alkyl, ArC 0-6 alkyl, Ar—ArC 0-6 alkyl, Ar-HetC 0-6 alkyl, Het-ArC 0-6 alkyl, or Het-HetC 0-6 alkyl;
[0037] R 4 is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, Het-C 0-6 alkyl, R 5 C(O)—, R 5 C(S)—, R 5 SO 2 —, R 5 NSO 2 —, R 5 OC(O)—, R 5 R 12 NC(O)—, or R 5 R 12 NC(S)—;
[0038] R 5 is H, C 1-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, Ar—ArC 0-6 alkyl, Ar-HetC 0-6 alkyl, Het-ArC 0-6 alkyl, Het-HetC 0-6 alkyl, or Het-C 0-6 alkyl;
[0039] R 6 is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0040] R 7 is H, C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, Het-C 0-6 alkyl, R 10 C(O)—, R 10 C(S)—, R 10 SO 2 —, R 10 OC(O)—, R 10 R 13 NC(O)—, or R 10 R 13 NC(S)—;
[0041] R 8 is H, C 1-6 alkyl, C 2-6 alkenyl, C 2-6 alkynyl, HetC 0-6 alkyl or ArC 0-6 alkyl;
[0042] R 9 is C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl or Het-C 0-6 alkyl;
[0043] R 10 is C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl or Het-C 0-6 alkyl;
[0044] R 11 is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0045] R 12 is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0046] R 13 is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0047] R′ is H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0048] R″ is C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl;
[0049] X is CH 2 , S, or O;
[0050] Z is C(O) or CH 2 ; or
[0051] a pharmaceutically acceptable salt, hydrate or solvate thereof.
[0052] In compounds of Formula I or II, R 1 is preferably group (a)
wherein:
[0053] R 3 is preferably substituted or unsubstituted C 3-7 cycloalkylC 0-6 alkyl, C 4-7 cycloalkenylC 0-6 alkyl, C 5-8 bicycloalkylC 0-6 alkyl, Ar—ArC 0-6 alkyl, Ar-HetC 0-6 alkyl, Het-ArC 0-6 alkyl, or Het-HetC 0-6 alky.
[0054] More preferably R 3 is substituted or unsubstituted C 5-7 cycloalkylC 1-2 alkyl, C 4-5 cycloalkenylC 1-2 alkyl, C 5-8 bicycloalkylC 1-2 alkyl or Ar-HetC 0-6 alkyl.
[0055] Most preferably R 3 is cyclopentylmethyl, cyclopentylethyl, cyclopentenylmethyl, cyclopentenylethyl, cyclohexylmethyl, 4-methylcyclohexylmethyl, 2-cyclohexylprop-1-yl, cyclohexylethyl, cycloheptylmethyl, 7,7-dimethylbicyclo[2.2.1]hept-1ylmethyl, or indol-2-ylmethyl;
[0056] R 4 is R 5 C(O)— or R 5 SO 2 — wherein R 5 is C 3-6 cycloalkyl-C 0-6 alkyl, Ar—ArC 0-6 alkyl, Ar-HetC 0-6 alkyl, Het-ArC 0-6 alkyl, or Het-HetC 0-6 alkyl.
[0057] More preferably R 5 is:
[0058] unsubstituted or substituted furanyl, especially furan-2-yl or furan-3-yl, or alkyl-substituted furanyl such as 2-methylfuran-3-yl, 2,4-dimethylfuran-3-yl, or aryl substituted furanyl, even more especially 5-phenylfuran-2-yl, 5-(2-chlorophenyl)furan-2-yl, 5-(3-chlorophenyl)furan-2-yl, 5-(4-chlorophenyl)furan-2-yl, 5-(4-fluorophenyl)furan-2-yl, 5-(4-hydroxyphenyl)furan-2-yl, 5-(3-trifluoromethylphenyl)furan-2-yl, 5-(4-trifluoromethylphenyl)furan-2-yl, 5-(3-trifluoromethylphenyl)furan-2-yl, 5-(4-methylphenyl)furan-2-yl, 5-(4-acetylphenyl)furan-2-yl, or 5-trifluoromethylfuran-2-yl;
[0059] unsubstituted or substituted tetrahydrofuranyl, particularly tetrahydrofuran-2-yl or tetrahydrofuran-3-yl
[0060] unsubstituted or substituted morpholinyl;
[0061] unsubstitutetd or substituted pyrrolyl, particularly pyrrol-2-yl;
[0062] unsubstituted or substituted piperazinyl, particularly piperzin-1-yl or 4-alkylpiperazinyl, e.g., 4methylpeperzin-1-yl;
[0063] unsubstituted or substituted pyrazolyl, particularly 1H-pyrazol-2-yl, 1H-pyrazol-4-yl, 1- or 2-methyl-2H-pyrazol-2-yl or 1- or 2-methyl-2H-pyrazol-3-yl;
[0064] unsubstituted or substituted isoxazolyl, particularly isoxazol-5-yl, 3-methylisoxazol-4-yl, 5-methylisoxazol-3-yl, 5-methylisoxazol-4-yl, or 3,5-dimethylisoxazol-4-yl;
[0065] unsubstituted or substituted thiazolyl, particularly thiazol-2-yl, 2-methylthiazol-2-yl, 2,4-dimethylthiazol-5-yl, 2-(2,3-dihydrobenzo[1,4]dioxin-2-yl)thiazol-4-yl, or 4-methyl-2-phenylthiazol-5-yl;
[0066] unsubsituted or C 1-2 alkylsubstituted pyrazolo[5,1-c]triazinyl, particularly 4,7-dimethylpyrazolo[5,1-c]triazin-3-yl;
[0067] unsubstituted or substituted pyrazolyl, particularly alkyl-substituted pyrazolyl including 2-methyl-2H-pyrazol-2-yl;
[0068] C 1-2 alkyl substituted pyrazolo[5,1-c]pyrimidinyl, particularly 2,7-dimethylpyrazol[5,1-c]pyrimidin-6-yl;
[0069] unsubstituted or aryl-substituted triazolyl, particularly phenyl-substituted triazoles including 3-phenyl-3H-{1,2,3]triazol-3-yl;
[0070] unsubstituted or substituted pyrazinyl, particularly pyrazin-2-yl and 5-methylpyrazin-2-yl;
[0071] unsubstituted or substituted imadazolyl, particularly 1-H-imidazol-2-yl, 1-methyl-1H-imidazol-4-yl or 1-methyl-1H-imidazol-2-yl;
[0072] benzofuranyl, especially benzofuran-2-yl, more especially C 1-6 alkoxy substituted benzofuranyl, particularly 5,6-dimethoxybenzofuran-2-yl, more especially Het-C 0-6 alkyl-benzofuran-2-yl, particularly 5-(2-morpholin-4-yl-ethoxy)benzofuran-2-yl;
[0073] thiophenyl, especially thiophene-3-yl and thiophen-2-yl, more especially Het-C 0-6 alkylthiophenyl; particularly 5-pyridin-2-ylthiophen-2-yl, more especially C 1-6 alkylthiophenyl, particularly 5-methylthiophen-yl or 3-methylthiophen-2-yl; more especially C 1-6 alkoxythiophenyl, particularly 3-ethoxythiophen-2-yl;
[0074] furo[3,2-b]-pyridine-2-yl, especially 3-methylfuro[3,2-b]pyridin-2-yl;
[0075] phenyl, especially alkyl-substituted phenyl, halogen-substitutedphenyl, trihaloalkyl-substituted phenyl, alkoxy-substituted phenyl, or acetoxy-substitutedphenyl, especially 4-methylphenyl, 3-chlorophenyl, 4-chlorophenyl, 3-trifluoromethylphenyl, 4-trifluoromethylphenyl, 2-chlorophenyl, 4-fluorophenyl, 4-hydroxyphenyl, or 4-acetylphenyl;
[0076] unsubstituted or substituted pyridinyl, particularly pyridin-2-yl;
[0077] cyclobutyl or cyclopentyl;
[0078] unsubstituted or substituted, for example thieno[3,2-b]thiopheneyl, especially thieno[3,2-b]thiophen-2-yl or 5-isoxazol-3-ylthiophen-2-yl.
[0079] In group (a) R′ is preferably H, C 1-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl, preferably H.
[0080] In compounds of Formula I and II, R 2 is preferably R 9 SO 2 or C 1-6 alkyl. When R 2 is C 1-6 alkyl, C 1-6 alkyl is preferably propyl. R 2 is most preferably R 9 SO 2 .
[0081] R 9 is C 1-6 alkyl, C 3-6 cycloalkyl-C 0-6 alkyl, Ar—C 0-6 alkyl, or Het-C 0-6 alkyl, preferably Het-C 0-6 alkyl, more preferably pyridinyl or 1-oxy-pyridinyl. When R 2 is R 9 SO 2 , R 9 is even more preferably pyridin-2-yl or 1-oxy-pyridin-2-yl. Most preferably, R 9 is pyridin-2-yl.
[0082] Most preferred compounds of Formula I or II are those wherein:
[0083] R 1 is group (a)
[0084] R 2 is R 9 SO 2 ;
[0085] R 3 is cyclopentylmethyl, cyclopentylethyl, cyclopentenylmethyl, cyclopentenylethyl, cyclohexylmethyl, 4-methylcyclohexylmethyl, 2-cyclohexylprop-1-yl, cyclohexylethyl, cycloheptylmethyl, 7,7-dimethylbicyclo[2.2.1]hept-1-ylmethyl, or indol-2-ylmethyl;
[0086] R 4 is R 5 C(O) or R 5 SO 2 ;
[0087] R 5 is 5-phenylfuran-2-yl, 5-(2-chlorophenyl)furan-2-yl, 5-(3-chlorophenyl)furan-2-yl, 5-(4chlorophenyl)furan-2-yl, 5-(4-fluorophenyl)furan-2-yl, 5-(4-hydroxyphenyl)furan-2-yl, 5-(3-trifluoromethylphenyl)furan-2-yl, 5-(4-trifluoromethylphenyl)furan-2-yl, 5-(3-trifluoromethylphenyl)furan-2-yl, 5-(4-methylphenyl)furan-2-yl, 5-(4-acetylphenyl)furan-2-yl, or 5-trifluoromethylfuran-2-yl;
[0088] tetrahydrofuran- 2 -yl or tetrahydrofuran-3-yl
[0089] N-morpholinyl;
[0090] pyrrol-2-yl
[0091] piperzin-1-yl or 4-alkylpiperazinyl, e.g., 4-methylpeperzin-1-yl;
[0092] 1H-pyrazol-2-yl, 1H-pyrazol-4-yl, 1- or 2-methyl-2H-pyrazol-2-yl or 1- or 2-methyl-2H-pyrazol-3-yl;
[0093] isoxazol-5-yl, 3-methylisoxazol-4-yl, 5-methylisoxazol-3-yl, 5-methylisoxazol-4-yl, or 3,5-dimethylisoxazol-4-yl;
[0094] thiazol-2-yl, 2-methylthiazol-2-yl, 2,4-dimethylthiazol-5-yl, 2-(2,3-dihydrobenzo[1,4]dioxin-2-yl)thiazol-4-yl, or 4-methyl-2-phenylthiazol-5-yl;
[0095] 4,7-dimethylpyrazolo[5,1-]triazin-3-yl;
[0096] 2-methyl-2H-pyrazol-2-yl;
[0097] 2,7-dimethylpyrazol[5,1-]pyrimidin-6-yl;
[0098] 3-phenyl-3H-{1,2,3]triazol-3-yl;
[0099] pyrazin-2-yl or 5-methylpyrazin-2-yl;
[0100] 1-H-imidazol-2-yl, 1-methyl-1H-imidazol-4-yl or 1-methyl-1H-imidazol-2-yl;
[0101] benzofuran-2-yl, 5,6-dimethoxybenzofuran-2-yl, 5-(2-morpholin-4-yl-ethoxy)benzofuran-2-yl;
[0102] thiophene-3-yl, thiophen-2-yl, 5-pyridin-2-ylthiophen-2-yl, 5-methylthiophen-yl or 3-methylthiophen-2-yl, or 3-ethoxythiophen-2-yl;
[0103] furo[3,2-b]-pyridine-2-yl or 3-methylfuro[3,2-b]pyridin-2-yl;
[0104] phenyl, 4-methylphenyl, 3-chlorophenyl, 4-chlorophenyl, 3-trifluoromethylphenyl, 4-trifluoromethylphenyl, 2-chlorophenyl, 4-fluorophenyl, 4-hydroxyphenyl, or 4-acetylphenyl;
[0105] pyridin-2-yl;
[0106] thieno[3,2-b]thiophen-2-yl or 5-isoxazol-3-ylthiophen-2-yl
[0107] R 9 is pyridin-2-yl or 1-oxy-pyridin-2-yl, preferably pyridin-2-yl;
[0108] R′ is H
[0109] R″ is H; and
[0110] in Formula I R′″ is C 1-6 alkyl.
[0111] R′″ is preferably methyl, ethyl, propyl, butyl, pentyl and hexyl, more especially methyl; or preferably 5-, 6- or 7-C 1-6 alkyl, especially 5-, 6- or 7-methyl, -ethyl, -propyl, -butyl, -pentyl or -hexyl, more especially 5-, 6- or 7-methyl; more preferably 6- or 7-C 1-6 alkyl, especially 6- or 7-methyl, -ethyl, -propyl, -butyl, -pentyl and -hexyl, more especially 6- or 7-methyl; yet more preferably, in Formula I, cis-7-C 1-6 alkyl as shown in Formula Ia:
wherein R′″ is C 1-6 alkyl, especially selected from the group consisting of: methyl, ethyl, propyl, butyl, pentyl and hexyl; most preferably cis-7-methyl, as shown in Formula Ia wherein R′″ is methyl.
[0112] As for the preferred substituents of Formula I, the definition are the same as those of the preferred compounds of Formula I with the exception of R 3 . For it the preferred groups are cyclopentylmethyl, [1-methylcyclopentyl]methyl, cyclopentylethyl, cyclopent-1-enylmethyl, cyclohexylmethyl, cycloheptylmethyl, [4-methylyclohexyl]methyl, [1-methylyclohexyl]methyl, and [2-7,7-dimethylbicyclo[2.2.1]hept-1-yl]ethyl. These preferred compounds, in particular, as well as other compounds of Formula II, are highly selective for inhibition of the cathepsin S enzyme as compared with their inhibition of the cathepsin K enzyme. Expressed as the ratio of the K i for cathepsin K over the K i of cathepsin S, (K i Cat K/K i Cat S) these novel compounds exhibit a ratio of 4 or greater in (define assay). The assay is described below.
[0000] Methods of Preparation
[0113] Compounds of the general formula Ia may be prepared in a fashion analogous to that outlined in Schemes 1 to 7. Carbobenyzloxy-D-alaninol (Cbz-D-alaninol)1 is first converted into an iodide and is then reacted with allyl Grignard with a copper (I) catalyst or a similar allyl organometallic reagent. The amine is then alkylated with allyl iodide. Grubbs' catalyst is then used to form the azepine ring 3 by ring closing metathesis. Epoxidation of the alkene followed by separation of the diastereomers and opening of the epoxide of the minor component with sodium azide provides the intermediate azido alcohol 5. Reduction of the azide 5 produces amine 6.
Reagents and conditions: (a) PPh 3 , I 2 ; (b) 2-propenyl magnesium chloride, Cat. CuI; (c) allyl bromide, NaH; (d) Grubbs; (e) mCPBA; f) KOAc/HOAc, 18-crown-6; g) MeSO 2 Cl, Et3N; h) KOH, MeOH; i) NaN 3 ; j) PPh 3
[0114] Commercially available methyl cyclopentane carboxylate was methylated with LDA and iodomethane to give 8 (scheme 2) Hydrolysis of the ester with LiOH followed by treatment with oxalyl chloride gives acid chloride 9. Subsequent Wolff rearrangement with diazomethane and silver benzoate produces ester 11. Reduction of the ester followed by oxidition with Dess-Martin periodinane produces aldehyde 13. This in turn is treated with KCN and (NH 4 )CO 3 followed by hydrolysis with NaOH and protection of the free amine as its BOC carbamate to give amino acid 15.
[0115] Reagents and conditions: (a) BuLi, diisopropylamine, MeI; b) LiOH, oxalylchloride; (c) CH 2 N 2 , Et 3 N; (d) silver benzoate, Et 3 N, MeOH; (e) LiAlH 4 ; f) Dess-Martin; g) KCN, (NH 4 ) 2 CO 3 , HCl; h) NaOH; i) (Boc) 2 O.
[0116] The amine 6 may be protected with di-tert-butyldicarbonate to provide the N-Boc derivative 16 (Scheme 3). Removal of the benzyloxycarbonyl protecting group may be effected by treatment of 16 with hydrogen gas in the presence of a catalyst such as 10% Pd/C to provide the amine 17. Treatment of amine 17 with a sulfonyl chloride such as 2-pyridinesulfonyl chloride in the presence of a base such as N-methylmorpholine or triethylamine provides the sulfonamide derivative 18. Removal of the tert-butoxycarbonyl protecting group may be effected with an acid such as hydrochloric acid to provide intermediate 19. Coupling of 19 with an acid such as N-Boc-(1-methyl)cyclohexylalanine in the presence of a coupling agent common to the art such as HBTU or polymer supported EDC provides the alcohol intermediate 20. Removal of the tert-butoxycarbonyl protecting group under acidic conditions provides amine 21. Coupling of 21 with an acid such as furan-2-carboxylic acid in the presence of a coupling agent such as HBTU or polymer supported EDC provides alcohol 22. Alcohol 22 may be oxidized with an oxidant common to the art such as pyridine sulfur trioxide complex in DMSO and triethylamine or the Dess-Martin periodinane to provide the ketone 23.
[0117] Reagents and conditions: (a) Di-tert-butyldicarbonate, THF; (b) H 2 , 10% Pd/C, EtOAc; (c) 2-pyridinesulfonyl chloride, TEA, DMF; (d) HCl, MeOH; (e) N-Boc-1-methylcylohexylalanine, HBTU, 4-methylmorpholine, DMF; (f) HCl, MeOH; (g) furan-2-carboxylic acid, HBTU, 4-methylmorpholine, DMF; (h) Dess-Martin periodinane, methylene chloride.
[0118] The individual diastereomers of furan-2-carboxylic acid {(S)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide 23a and 23b may be prepared as outlined in Scheme 4. The mixture of diastereomers are separated by HPLC to provide the compounds 23a and 23b.
Reagents and Conditions: a.) HPLC separation.
[0119] Alternatively, the compounds of formula Ia may be prepared in a fashion analogous to Scheme 5. Thus, 1,4-pentadien-3-ol was epoxidized under Sharpless epoxidation conditions using cumene hydroperoxide and D-(−)-diisopropyl tartrate. The resulting secondary alcohol was inverted under Mitsonobu conditions with phthalimide to reveal epoxide 26. Opening of this epoxide with pyridine-2-sulfonic acid allylamide in the presence of DBU and subsequent ring-closing metathesis with Grubb's catalyst provided alkene 28. The olefin was hydrogenated over palladium on carbon and the phthalimide protecting group removed with hydrazine to reveal amine 30. The amine can then be used to couple to (S)-2-tert-Butoxycarbonylamino-3-cyclohexyl-propionic acid to provide intermediate 31. Subsequent removal of the tert-butoxycarbonyl protecting group, coupling with a carboxylic acid, and oxidation of the C3 secondary alcohol to the ketone provided 32.
Reagents and conditions: a) Ti(OiPr) 4 , cumene hydroperoxide, 4A molecular sieves, D-(−)-DIPT; b) phthalimide, Ph 3 P,DIAD; c) Pyridine-2-sulfonic acid allylamide, DBU; d) Tricyclohexylphosphine(1,3-bistrimethylphenyl 4,5-dihydroimidazol-2-ylidene)benzylidene ruthenium (IV) dichloride; e) H 2 (g), Pd/C, 45° C.; f) NH 2 NH 2 , MeOH, reflux; g) i) (S)-2-tert-butoxycarbonylamino-3-cyclohexyl-propionic acid, HBTU, 4-methylmorpholine; ii) 4N HCl; h) i) 2-methyl-2H-pyrazole-3-carboxylic acid, HBTU, 4-methylmorpholine; ii) Dess-Martin Periodinane
[0120] Compounds of the general formula Ia may also be prepared in a fashion analogous to that outlined in Schemes 6 to 7. Alkylation of benzyl-N-allylcarbamate (33) with a base such as sodium hydride and 5-bromo-1-pentene provides the diene 34 (Scheme 1). Treatment of 2 bis(tricyclohexylphosphine)benzylidine ruthenium (IV) dichloride olefin metathesis catalysts developed by Grubbs provides the tetrahydroazepine 35. Epoxidation of 35 with oxidizing agents common to the art such as m-CPBA provides the epoxide 36. Nucleophilic epoxide ring opening may be effected with a reagent such as sodium azide to provide the azido alcohol 37 which may be reduced to the amino alcohol 38 under conditions common to the art such as 1,3-propanedithiol and triethylamine in methanol or triphenylphosphine in THF and water. Treatment of amine 38 with S-Boc-cyclopentyl alanine in the presence of HBTU and 4-methylmorpholine affords compound 39. Removal of the tert-butoxycarbonyl protecting group may be effected by treatment of 39 with hydrogen chloride in dioxane to produce the amine 40. Treatment of amine 40 with 2-furoic acid in the presence of HBTU and 4-methylmorpholine produces compound 41. The benzyloxycarbonyl protecting group may be removed by treatment with TMSI in methylene chloride to provide amine 42. Treatment of amine 42 with a sulfonyl chloride such as 2-pyridinesulfonyl chloride in the presence of a base such as sodium bicarbonate gives secondary alcohol 43. Alcohol 43 may be oxidized with an oxidant common to the art such as pyridine sulfur trioxide complex in DMSO and triethylamine or the Dess-Martin periodinane to provide the ketone 44.
Reagents and conditions: (a) NaH, 5-bromo-1-pentene, NaH; (b) bis(tricyclohexylphosphine)benzylidine ruthenium (IV) dichloride, CH 2 Cl 2 , reflux; (c) m-CPBA, CH 2 Cl 2 ; (d) NaN 3 , NH 4 Cl, CH 3 OH, H 2 O; (e) TEA, 1,3-propanedithiol, CH 3 OH.
Reagents and conditions: (a) N-Boc-cylcopentylalanine, HBTU, 4-methylmorpholine, DMF; (b) HCl, dioxane; (c) 2-furoic acid, HBTU, 4-methylmorpholine, DMF; (d) TMSI, CH 2 Cl 2 ; (e) 2-pyridyl sulfonylchloride, 10% sodium bicarbonate; (f) Dess-Martin periodinane, methylene chloride.
UTILITY OF THE PRESENT INVENTION
[0121] The compounds of Formula I and II are useful as inhibitors of cathepsin S. The present invention provides methods of treatment of diseases caused by pathological levels of cathepsin S, which methods comprise administering to an animal, particularly a mammal, most particularly a human in need thereof a therapeutically effective amount of an inhibitor of cathepsin S, including a compound of the present invention.
[0122] The present invention particularly provides methods for treating the following diseases in which cathepsin S is implicated:
[0123] treatment and/or prevention of an autoimmune disease state such as rheumatoid arthritis, multiple sclerosis, juvenile-onset diabetes, systemic lupus erythematosus, discoid lupus erythematosus, pemphigus vulgaris, pemphigoid, Grave's disease, myasthenia gravis, Hashimoto's thyroiditis, scleroderma, dermatomysositis, Addison's disease, pernicious anemia, primary myxoedema, thyrotoxicosis, autoimmune atrophic gastritis, stiff-man syndrome, Goodpasture's syndrome, sympathetic opthalamia, phacogenic uveitis, autoimmune haemolytic anaemia, idiopathic thrombocytopenic purpura, idiopathic leucopenia, primary biliary cirrhosis, active chronic hepatitis, cryptogenic cirrhosis, ulcerative colitis, Sjogren's syndrome, and mixed connective tissue diease; and
[0124] treatment and/or prevention of a disease state caused by the formation and/or complications of atherosclerotic lesions.
[0125] Diseases which require therapy:
[0126] inhibition of a class II MHC-restricted immune response;
[0127] inhibition of an asthmatic response;
[0128] inhibition of an allergic response such as allergic rhinitis or atopic dermatitis;
[0129] inhibition of immune response against transplanted organ or tissue; and
[0130] inhibition of elastase activity in atheroma.
[0131] The present methods contemplate the use of one or more compounds of Formula I or II alone or in combination with other therapeutic agents.
[0132] For acute therapy, parenteral administration of a compound of Formula I or II is preferred. An intravenous infusion of the compound in 5% dextrose in water or normal saline, or a similar formulation with suitable excipients, is most effective, although an intramuscular bolus injection is also useful. Typically, the parenteral dose will be about 0.01 to about 100 mg/kg; preferably between 0.1 and 20 mg/kg, in a manner to maintain the concentration of drug in the plasma at a concentration effective to inhibit cathepsin S. The compounds are administered one to four times daily at a level to achieve a total daily dose of about 0.4 to about 400 mg/kg/day. The precise amount of a compound which is therapeutically effective, and the route by which such compound is best administered, is readily determined by one of ordinary skill in the art by comparing the blood level of the agent to the concentration required to have a therapeutic effect.
[0133] The compounds of Formula I or II may also be administered orally to the patient in a manner such that the concentration of drug is sufficient to inhibit bone resorption or to achieve any other therapeutic indication as disclosed herein. Typically, a pharmaceutical composition containing the compound is administered at an oral dose of between about 0.1 to about 50 mg/kg in a manner consistent with the condition of the patient. Preferably the oral dose would be about 0.5 to about 20 mg/kg.
[0134] No unacceptable toxicological effects are expected when compounds of Formula I or II are administered in accordance with the present methods.
[0000] Biological Assays
[0135] The compounds used in the present methods may be tested in one of several biological assays to determine the concentration of compound which is required to have a given pharmacological effect.
[0000] Determination of Cathepsin S Proteolytic Catalytic Activity
[0136] All assays for cathepsin S were carried out with human recombinant enzyme. Standard assay conditions for the determination of kinetic constants used a fluorogenic peptide substrate, typically Ac-Lys-Gln-Lys-Leu-Arg-AMC, and were determined in 50 mM Mes at pH 6.5 containing 10 mM cysteine and 5 mM EDTA. Stock substrate solutions were prepared at a concentration of 10 mM in 10% DMSO with 30 uM final substrate concentration in the assays. All assays contained 6% DMSO. All assays were conducted at 30° C. Product fluorescence (excitation at 360 nM; emission at 460 nM) was monitored either with a Perceptive Biosystems Cytofluor II fluorescent plate reader or a Tecan Spectraflour Plus plate reader. Product progress curves were generated over 20 to 30 minutes following formation of AMC product.
[0000] Determination of Cathepsin K Proteolytic Catalytic Activity
[0137] All assays for cathepsin K were carried out with human recombinant enzyme. Standard assay conditions for the determination of kinetic constants used a fluorogenic peptide substrate, typically Cbz-Phe-Arg-AMC, and were determined in 100 mM Na acetate at pH 5.5 containing 20 mM cysteine and 5 mM EDTA. Stock substrate solutions were prepared at a concentration of 10 mM in DMSO with 20 uM final substrate concentration in the assays. All assays contained 10% DMSO. All assays were conducted at 30° C. Product fluorescence (excitation at 360 nM; emission at 460 nM) was monitored either with a Perceptive Biosystems Cytofluor II fluorescent plate reader or a Tecan Spectraflour Plus plate reader. Product progress curves were generated over 20 to 30 minutes following formation of AMC product.
[0000] Determination of Cathepsin L Proteolytic Catalytic Activity
[0138] All assays for cathepsin L were carried out with human liver cathepsin L purchased from Enzyme Systems Products. Standard assay conditions are the same as cathepsin K except that the final substrate concentration was 5.0 uM.
[0000] Inhibition Studies
[0139] Potential inhibitors were evaluated using the progress curve method. Assays were carried out in the presence of variable concentrations of test compound. Reactions were initiated by addition of enzyme to buffered solutions of inhibitor and substrate. Data analysis was conducted according to one of two procedures depending on the appearance of the progress curves in the presence of inhibitors. For those compounds whose progress curves were linear, apparent inhibition constants (K i,app ) were calculated according to equation 1 (Brandt et al., Biochemitsry, 1989, 28, 140):
v=V m A/[K a (1+1 /K i, app )+ A] (1)
where v is the velocity of the reaction with maximal velocity V m , A is the concentration of substrate with Michaelis constant of K a , and I is the concentration of inhibitor.
[0140] For those compounds whose progress curves showed downward curvature characteristic of time-dependent inhibition, the data from individual sets was analyzed to give k obs according to equation 2:
[ AMC]=v ss t +( v 0 - v ss )[1−exp(− k obs t )]/ k obs (2)
where [AMC] is the concentration of product formed over time t, v 0 is the initial reaction velocity and v ss is the final steady state rate. Values for k obs were then analyzed as a linear function of inhibitor concentration to generate an apparent second order rate constant (k obs /inhibitor concentration or k obs /[I]) describing the time-dependent inhibition. A complete discussion of this kinetic treatment has been fully described (Morrison et al., Adv. Enzymol. Relat. Areas Mol. Biol., 1988, 61, 201).
General
[0141] Nuclear magnetic resonance spectra were recorded at 400 MHz using, respectively, a Bruker AC 400 spectrometer. CDCl 3 is deuteriochloroform, DMSO-d 6 is hexadeuteriodimethylsulfoxide, and CD 3 OD is tetradeuteriomethanol. Chemical shifts are reported in parts per million (δ) downfield from the internal standard tetramethylsilane. Abbreviations for NMR data are as follows: s=singlet, d=doublet, t=triplet, q=quartet, m=multiplet, dd=doublet of doublets, dt=doublet of triplets, app=apparent, br=broad. J indicates the NMR coupling constant measured in Hertz. Continuous wave infrared (IR) spectra were recorded on a Perkin-Elmer 683 infrared spectrometer, and Fourier transform infrared (FTIR) spectra were recorded on a Nicolet Impact 400 D infrared spectrometer. IR and FTIR spectra were recorded in transmission mode, and band positions are reported in inverse wavenumbers (cm −1 ). Mass spectra were taken on either VG 70 FE, PE Syx API III, or VG ZAB HF instruments, using fast atom bombardment (FAB) or electrospray (ES) ionization techniques. Elemental analyses were obtained using a Perkin-Elmer 240C elemental analyzer. Melting points were taken on a Thomas-Hoover melting point apparatus and are uncorrected. All temperatures are reported in degrees Celsius.
[0142] Analtech Silica Gel GF and E. Merck Silica Gel 60 F-254 thin layer plates were used for thin layer chromatography. Both flash and gravity chromatography were carried out on E. Merck Kieselgel 60 (230-400 mesh) silica gel.
[0143] Where indicated, certain of the materials were purchased from the Aldrich Chemical Co., Milwaukee, Wis., Chemical Dynamics Corp., South Plainfield, N.J., and Advanced Chemtech, Louisville, Ky.
EXAMPLES
[0144] In the following synthetic examples, temperature is in degrees Centigrade (° C). Unless otherwise indicated, all of the starting materials were obtained from commercial sources. Without further elaboration, it is believed that one skilled in the art can, using the preceding description, utilize the present invention to its fullest extent. These Examples are given to illustrate the invention, not to limit its scope. Reference is made to the claims for what is reserved to the inventors hereunder.
Example 1
Preparation of 1A: Morpholine 4-carboxylic acid {(S)-2-[1-methylcyclopentyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0145]
Preparation of 1B: Morpholine 4-carboxylic acid {(L)-2-[1-methylcyclopentyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0146]
1a.) 1-Methyl methylcyclopentanecarboxylate
[0147] Butyllithium (1.6 M, 48.75 mL, 78 mmol) was added dropwise to a stirred solution of diisopropylamine (7.88 g, 44.5 mmol) in tetrahydrofuran (12 mL) at −78° C. The solution was warmed to room temperature to ensure the evaporation of butane and then cooled to −78° C. again. Methylcyclopentanecarboxylate (10.0 g, 78 mmol) in tetrahydrofuran (100 mL) was added to the reaction mixture at −78° C. After addition, the reaction mixture was warmed to 0° C. temperature for 30 mins. After cooling to −78° C., iodomethane (11.1 g, 78 mmol) in tetrahydrofuran (30 mL) was added. After addition, the reaction mixture was warmed to room temperature and stirred for 18 hours. Ammonium chloride solution (saturated) was added and the suspension was extracted with ether (3×). The combined organic phase was washed with water, brine, dried (MgSO 4 ), filtered and concentrated. Column chromatography (5% ethyl acetate:hexanes) of the residue provided 5.3 g of the title compound: 1 HNMR: (CDCL 3 ) δ 3.7 (s, 3H), 2.10 (s, 3H), 1.28-1.70 (m, 8H).
1b.) 1-Methylcyclopentanecarboxlic acid
[0148] To a solution of compound of Example 1a (5.3 g) in methanol was added lithium hydroxide (15.68 g, 0.4 mol). The reaction was stirred at room temperature for 18 hours. The reaction was concentrated in vacuo. The solution was adjusted to pH=1 with 10% HCl solution, and extracted with ethyl acetate. The combined organic phase was washed with water, brine, dried (MgSO 4 ), filtered and concentrated to give 5.0 g of the title compound: 1 HNMR: (CDCL 3 ) δ 2.10 (s, 3H), 1.26-1.73 (m, 8H).
1c.) 1-Methyl cyclopentanecarbonyl chloride
[0149] To a solution of the compound of Example 1b (5.0 g, 38.5 mmol) and oxalylchloride (3.6 mL) in CH 2 Cl 2 , 0.2 mL of DMF was added. The mixture was stirred overnight at room temperature. The solvent was removed under reduced pressure to give 5.0 g (crude) of the title compound which was used directly in the next step without further purification.
1d.) 1-Diazomethyl-1-methyl-cyclopentane
[0150] Triethylamine (6.12 mL, 43.94 mmol) was added to a solution of the 1-methyl cyclopentanecarbonyl chloride from Example 1c (5.0 g, 33.8 mmol) and diazomethane (1.47 g, 35 mmol) in a mixture of CH 3 CN (25 mL) and THF (25 mL) at 0° C. After the addition was complete, the reaction mixture was allowed to warm room temperature for 20 hours. The solvent was removed under reduced pressure and the resulting residue washed with NaHCO 3 (sat.) solution and was extracted with ether (3×). The combined organic layers were washed with brine, dried (MgSO 4 ), filtered and concentrated to provide 4.0 g of the title compound: IR: N═N 2112.29 (cm −1 )
1e.) (1-Methyl-cyclopentyl)-acetic acid methyl ester
[0151] To a solution of the title compound of Example 1d (4.0 g, 25.8 mmol) in methanol (106 mL), 4 mL of silver benzoate (1.07 g) in triethyl amine (13.8 mL) was added. After addition, the reaction mixture was stirred at room temperature for 2 hours whereupon it was filtered to remove the solids. The filtrate was evaporated in vacuo. Column chromatography of the residue (20% ethyl acetate:hexane) provided 1.8 g of the title compound: 1 H NMR: (CDCl 3 ) δ 3.70 (s, 3H), 2.27 (s, 2H), 2.02 (s, 3H), 1.21-1.60 (m, 8H).
1f.) (1-Methyl-cyclopentyl)-ethanol
[0152] To a stirring solution of lithium aluminum hydride (24.73 mL, 23 mmol) in THF, the title compound of Example 1e (1.8 g, 11.5 mmol) was added slowly. After the addition, the mixture was stirred at reflux temperature for 2 hours after which time it was cooled to 0° C. Benzene (45 mL), water (1.77 mL) (added very slowly) and sodium fluoride (3.14 g) were added and stirred at 0° C. for 1 hour whereupon the suspension it was filtered to remove the solids. The filtrate was evaporated in vacuo to give the title compound (1.2 g).: 1 H NMR: (CDCl 3 ) δ 3.74 (m, 2H), 1.2-1.6 (m, 13H).
1g.) (1-Methyl-cyclopentyl)-acetaldehyde
[0153] To a solution of (1-methyl-cyclopentyl)-ethanol (Example 1f, 1.2 g, 9.37 mmol) in CH 2 Cl 2 (20 mL), Dess-Martin periodinane (1.2 g) was added. After stirring for 2 hours, solutions of sodium thiosulfate (10% in water, 0.50 mL) and saturated aqueous sodium bicarbonate (0.50 mL) were added simultaneously to the reaction. The mixture was then extracted with ethyl acetate (2×). The organic layer was dried with MgSO 4 , filtered, concentrated and purified via silica gel chromatography to give the title compound (1.1 g). 1 H NMR: (CDCl 3 ) δ 9.8 (s, 1H), 2.2 (s, 2H), 0.8-1.8 (m, 11H).
1h.) N-Boc-beta-(1-methylcyclopentyl)ala-OH
[0154] To a solution of (1-methyl-cyclopentyl)-acetaldehyde (Example 1g, 1.1 g, 8.73 mmol) in a mixture of ethanol (12 mL) and water (12 mL), potassium cyanide (624 mg, 9.6 mmol) and ammonium carbonate (2.26 g, 23.57 mmol) were added. The reaction mixture was stirred at 60° C. for 24 hours after which time the ethanol was removed in vacuo and the resultant aqueous solution was acidified to pH=1 with conc. HCl. The resultant white solid was collected by filtration, washed with water and dried under vacuum (420 mg). The product (420 mg) was refluxed in aqueous NaOH (aq.) (12 mL, 0.7 M) for 24 hours after which time the reaction mixture was concentrated to about 4 ml, and a solution of di-tert-butyldicarbonate 970 mg) in THF (10 mL) was added. After 2 hours, the THF was removed under vacuum, the residue was diluted with water (30 mL), and the mixture was washed with ether (2×). The aqueous phase was acidified to pH=1 with 1N aqueous HCl and then extracted with ethyl acetate (3×). The combined organic phase was washed with brine, dried, filtered, concentrated to give the title compound (300 mg). LC-MS m/z 271.2 (M + ).
1i.) (1S,4R,7R)-4-Methyl-8-oxa-3-azabicyclo[5.1.0]octane-3-carboxylic acid benzyl ester
[0155] To a solution of (1R,4R,7S)-4-methyl-8-oxa-3-azabicyclo[5.1.0]octane-3-carboxylic acid benzyl ester (25 g, 95.4 mmol) in a mixture of toluene (210 mL) and DMSO (210 mL), potassium acetate (93.5 g, 954 mmol), acetic acid (5.72 g, 95.4 mmol) and 18-crown-6 (12.6 g, 47.7 mmol) were added at room temperature. The reaction mixture was stirred at 110° C. for 24 hours after which time the solvent was evaporated under reduced pressure. The residue was diluted with ethyl acetate and was washed with water, sodium bicarbonate (sat.) and brine. The combined organic layer was dried over MgSO 4 , filtered and concentrated under reduced pressure to give a mixture of products which was used directly in the next step without further purification (27.86 g). LC-MS m/z 322.0 (M + ).
[0156] To solution of the mixture compounds (from above) (27.86 g, 86.8 mmol) in methylene chloride (400 mL), methanesulfonyl chloride (10.12 ml, 130.2 mmol) and triethylamine (24.2 mL, 173.6 mmol) were added. The reaction mixture was stirred at room temperature for 5 hours. It was then partitioned between methylene chloride and water. The combined organic layer was dried over MgSO 4 , filtered and concentrated under reduced pressure to give a mixture of products which were used directly in the next step without further purification (30.5 g). LC-MS m/z 400.0 (M + ).
[0157] To a solution of the mixture of compounds (from above) (30.5 g, 76.2 mmol) in methanol (100 mL), 10% potassium hydroxide solution (100 mL) was added at room temperature. The reaction mixture was stirred at room temperature for 24 hours, after which time the solvent was removed under reduce pressure. The residue was partitioned between ethyl acetate and water. The combined organic layer was dried over MgSO 4 , filtered and concentrated under reduced pressure to give a mixture of products. Silica gel chromatography of the mixture of epoxides (20% Ethyl acetate/80% Hexane) gave the title compound (7.47 g) and undesired epoxide product (10.5 g). LC-MS m/z 262 (M + ).
1j.) (2R,5S,6S)-5-Azido-6-hydroxy-2-methyl-azepane-1-carboxylic acid benzyl ester
[0158] A 1-liter round bottom flask was charged with (1S,4R,7R)-4-methyl-8-oxa-3-azabicyclo[5.1.0]octane-3-carboxylic acid benzyl ester (Example 1i, 7.47 g, 28.3 mmol). Ethylene glycol (46 ml) was then added. Triethanolamine (23.7 ml, 169.8 mmol) was dissolved in H 2 O (46 ml), then was added. NH 4 Cl (4.54 g, 84.9 mmol), then sodium azide (5.52 g, 84.9 mmol) was added and the reaction was stirred behind a blast shield at 80° C. overnight. The reaction mixture was cooled to RT, then poured into 10% aqueous NaCl. The mixture was extracted with CH 2 Cl 2 , and the combined organics were back extracted with aqueous NaHCO 3 , then brine, dried with MgSO 4 , filtered, concentrated in vacuo, and purified by flash column chromatography (20% to 33% ethyl acetatelhexanes, silica gel) to yield the title compound (7.4 g, 86%). LC-MS m/z 305.0 (M + ).
1k.) (2R,5S,6S)-5-Amino-6-hydroxy-2-methyl-azepane-1-carboxylic acid benzyl ester, HCl salt
[0159] (2R,5S,6S)-5-Azido-6-hydroxy-2-methyl-azepane-1-carboxylic acid benzyl ester (Example 1j, 6.6 g, 21.7 mmol) was dissolved in THF (100 ml) and H 2 O (2.8 ml), then triphenylphosphine (8.5 g, 32.6 mmol) was added and the reaction was stirred at R.T overnight. The reaction mixture was concentrated in vacuo, and the remaining solid dissolved in MeOH (10 ml). 1 M HCl in Et 2 O (20 ml) was added, then the solution was concentrated in vacuo to a solid. This was dissolved in a minimum amount of MeOH in a round bottle flask and the solution triturated with Et 2 O (˜500 mL) to precipitate triphenylphospine oxide. The solid was removed via filtration and the above procedure repeated several times until no UV active component was being further extracted (<10% UV absorption of triphenylphospine oxide by LC-MS). The remaining solid was used in the next reaction without further purification (6.6 g, 91%). LC-MS m/z 279.2 (M + ).
1l.) (2R,5S,6S)-5-N-Bocamino-6-hydroxy-2-methyl-azepane-1-carboxylic acid benzyl ester
[0160] To a solution of (2R,5S,6S)-5-amino-6-hydroxy-2-methyl-azepane-1-carboxylic acid benzyl ester, HCl salt (Example 1k, 6.91 g, 22 mmol) in dioxane (74 mL), sodium hydroxide (1.76 g, 44 mmol) and water (13 mL) were added. Then the reaction mixture was cooled to 0° C. Di-tert-butyl dicarbonate (5.28 g, 24.2 mmol) was added, and the reaction mixture was allowed to warm to room temperature for 16 hours. The solvent was evaporated, and the residue was diluted with ethyl acetate and washed with H 2 O, 10% HCl solution, NaHCO 3 (aq.) and brine. The combined organic layer was dried over MgSO 4 , filtered and concentrated under reduced pressure to give a crude product. Chromatography of the resulting solid on silica gel (30% Ethyl acetate/70% Hexane) gave the title compound (7.94 g, 95%). LC-MS m/z 379.2 (M + ).
1m.) [(3S,4S,7R)-3-Hydroxy-7-methyl-azepan-4-yl]-carbamic acid tert-butyl ester
[0161] To a solution of (2R,5S,6S)-5-N-bocamino-6-hydroxy-2-methyl-azepane-1-carboxylic acid benzyl ester (Example 1l, 7.94 g, 20.9 mmol) in ethanol (200 mL), palladium (10 wt. % on activated carbon) (1.7 g) was added. The reaction mixture was hydrogenated at 45 psi for 5 hours. The reaction mixture was filtered through celite, concentrated in vacuo by rotary evaporation to give the title compound which was used without further purification (5.0 g, 97%). LC-MS m/z 245.0 (M + ).
1n.) [(3S,4S,7R)-3-Hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-carbamic acid tert-butyl ester
[0162] A solution of 2-mercaptopyridine (10 g, 90 mmol) in a mixture of conc. HCl (116 mL) and H 2 O (34 mL) was cooled to 0° C. Chlorine gas was bubbled into the solution at 0° C. for 3.0 hours. Ice was added to the reaction mixture, followed by extraction with cold ether (2×). The ether layer was washed with cold 10% NaHCO 3 solution, and cold brine. The ether layer was dried over MgSO 4 , filtered and concentrated under reduced pressure to give 2-pyridine sulfonyl chloride which was used without further purification (12.86 g, 80%). LC-MS m/z 178.0 (M + ).
[0163] Triethyl amine (9.38 mL, 67.32 mmol) was added to a solution of [(3S,4S,7R)-3-hydroxy-7-methyl-azepan-4-yl]-carbamic acid tert-butyl ester (Example 1m, 5.0 g, 20.4 mmol) in methylene chloride (50 mL). The reaction mixture was cooled to 0° C., whereupon a solution of 2-pyridine sulfonyl chloride (3.26 g, 18.36 mmol) in methylene chloride (10 mL) was added dropwise. The resulting solution was stirred at room temperature for 4 hours. The reaction mixture was partitioned between methylene chloride and water. The aqueous phase extracted further with methylene chloride. The combined organic layer was dried over MgSO 4 , filtered and concentrated under reduced pressure to give a crude product. Chromatography of the resulting solid on silica gel (70% Ethyl acetate/30% Hexane) gave the desired product (5.6 g, 71%). LC-MS m/z 386.0 (M + ).
1o.) (3S,4S,7R)-3-Hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-3-ol, HCl salt
[0164] HCl in dioxane (4.0 M, 89 mL) was added to a stirred solution of [(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-carbamic acid tert-butyl ester (Example 1n, 5.6 g, 14.5 mL) in MeOH (30 mL). The reaction mixture was stirred for 2 hours at room temperature, then concentrated in vacuo to yield a white solid. This was used in the next reaction reaction without further purification (5.7 g). LC-MS m/z 286.0 (M + ).
1p.) 2-Amino-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-3-(1-methyl-cyclopentyl)-propionamide, HCl salt
[0165] To a solution of (3S,4S,7R)-4-amino-7-methyl-1-(pyridine-2-sulfonyl)-azepan-3-ol, HCl salt (Example 1o, 358 mg, 1.11 mmol) in DMF, N-Boc-beta-(1-methylcyclopentyl)ala-OH (Example 1h, 300 mg, 1.11 mmol), HBTU (547 mg, 1.47 mmol) and 4-methylmorpholine (561 mg, 5.55 mmol) were added. After the reaction mixture was stirred at room temperature for 16 hours, it was partitioned between ethyl acetate and water. The combined organic phase was washed with water, brine, dried (MgSO 4 ), filtered and concentrated. Column chromatography (5% methanol:CH 2 Cl 2 ) of the residue provided the N-Boc title compound (220 mg, 37%). MS (m/z) 539.0 (M + ).
[0166] To a stirring solution of N-Boc-2-amino-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-3-(1-methyl-cyclopentyl)-propionamide (220 mg, 0.41 mmol) in methanol (1 mL) was added HCl (4M in dioxane) (2.54 mL). After stirring at room temperature for 2 hours, the mixture was concentrated, giving a white solid. The white solid was azeotroped with toluene (2×) and then concentrated to give the title compound as a solid (200 mg). MS (m/z) 439.0 (M + ).
1q.) Morpholine-4-carboxylic acid [1-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine sulfonyl)-azepan-4-ylcarbamoyl]-2-(1-methyl-cyclopentyl)-ethyl]-amide
[0167] To a stirring solution of 2-amino-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-3-1-methylcyclopentyl)-propionamide (Example 1p, 0.2 g, 0.46 mmol) in CH 2 Cl 2 (5 mL) were added 4-morpholinecarbonyl chloride (69 mg, 0.46 mmol) and triethyl amine (0.384 ml, 2.76 mmol). After stirring at room temperature for 16 hours, the reaction mixture was washed with water, brine, dried (MgSO 4 ), filtered and concentrated. Column chromatography (5% methanol:CH 2 Cl 2 ) of the residue provided the title compound (120 mg, 47%). MS m/z 552.2 (M + ).
1r.) Morpholine 4-carboxylic acid {(S)-2-[1-methylcyclopentyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0168] To a stirring solution of morpholine-4-carboxylic acid [1-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-2-(1-methyl-cyclopentyl)-ethyl]-amide (Example 1q, 100 mg, 0.18 mmol) in CH 2 Cl 2 (2 mL) was added Dess-Martin periodinane (100 mg, 0.23 mmol). After stirring for 2 hours, solutions of sodium thiosulfate (10% in water, 0.50 mL) and saturated aqueous sodium bicarbonate (0.50 mL) were added simultaneously to the reaction. The mixture was then extracted with ethyl acetate (2 times). The organic layer was dried with MgSO 4 , filtered, and concentrated. Column chromatography (5% methanol:CH 2 Cl 2 ) of the residue provided the tide compound (100 mg, 99%). This compound was purified on a preparative R,R-Whelk-O column by HPLC to yield the two diastereomers of the title compound as solids [first eluting (1A): 30 mg, second eluting (1B): 25 mg]. MS m/z 550.0 (M + ); The 1 H NMR data of 1A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.78 (d, 1H), 8.0 (m, 2H), 7.53 (m, 1H), 6.9 (d, 1H), 5.1 (m, 1H), 4.91 (d, 1H), 4.80 (d, 1H), 4.40 (m, 2H), 3.9 (d, 1H), 3.70 (t, 4H), 3.40 (t, 4H), 2.2 (m, 3H), 0.93-1.93 (m, 17H). The 1 H NMR data of 1B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.7 (d, 1H), 8.0 (m, 2H), 7.53 (m, 1H), 7.2 (d, 1H), 5.1 (m, 1H), 4.8 (d, 1H), 4.48 (d, 1H), 3.86 (d, 1H), 3.75 (m, 4H), 3.40 (m, 4H), 2.2 (m, 2H), 2.05 (m, 1H), 0.93-1.65 (m, 17H).
Example 2
Preparation of 2A: Morpholine 4-carboxylic acid {(S)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0169]
Preparation of 2B: Morpholine 4-carboxylic acid {(L)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0170]
[0171] Following the procedure of Example 1(b-r), except substituting “1-methylcyclohexyl” for “1-methylcyclopentyl” gave the title compound: 1 HNMR data of 2A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.72 (d, 1H), 7.95 (m, 2H), 7.5 (d, 1H), 6.91 (d, 1H), 5.10 (m, 1H), 4.95 (d, 1h), 4.75 (d, 1H), 4.40 (m, 2H), 3.82 (d, 1H), 3.70 (t, 4h), 3.40 (t, 4H), 2.20 (m, 3H), 0.95-1.80 (m, 19H). The 1 H NMR data of 2B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.70 (d, 1H), 7.95 (m, 2H), 7.52 (m, 1H), 7.2 (d, 1H), 5.10 (m, 1H), 4.83 (d, 1H), 4.70 (d, 1H), 4.44 (m, 2H), 3.82 (d, 1H), 3.70 (t, 4H), 3.40 (t, 4H), 2.2 (m, 2H), 1.9 (m, 1H), 0.95-1.5 (m, 8H).
Example 3
Preparation of 3A: Furan-carboxylic acid {(S)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0172]
Preparation 3B: Furan-carboxylic acid {(L)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0173]
3a) Furan-2-carboxylic acid [1-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2 sulfonyl)-azepan-4-ylcarbamoyl]-2-(1-methyl-cyclopentyl)-ethyl]-amide
[0174] To a solution of 2-amino-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-3-(1-methyl-cyclohexyl)-propionamide, HCl salt (Example 2o, 357 mg, 0.73 mmol) in DMF, 2-furoic acid (81.8 mg, 0.73 mmol), HBTU (360 mg, 0.95 mmol) and 4-methylmorpholine (369 mg, 3.65 mmol) were added. After the reaction mixture was stirred at room temperature for 16 hours, it was partitioned between ethyl acetate and water. The combined organic phase was washed with water, brine, dried (MgSO 4 ), filtered and concentrated. Column chromatography (5% methanol:CH 2 Cl 2 ) of the residue provided the N-Boc title compound (376 mg, 94%) MS m/z 547.2 (M + ).
[0175] 3b) Following the procedure of Example 1(b-p, r), except substituting “4-methylcyclohexyl” for “1-methylcyclopentyl” and “furan-2-carboxylic acid” for “morpholine 4-carboxylic acid” gave the title compound: The 1 H NMR data of 3A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.72 (d, 1H), 8.0 (m, 2H), 7.54 (t, 1H), 7.50 (s, 1H), 7.15 (s, 1H), 6.96 (d, 1H), 6.70 (d, 1H), 6.52 (d, 1H), 5.1 (m, 1H), 4.75 (d, 1H), 4.66 (m, 1H), 4.45 (m, 1H), 3.85 (d, 1H), 2.2 (m, 3H), 1.95 (m, 1H), 0.95-1.60 (m, 18H). The 1 H NMR data of 3B: 1 H NMR (400 Hz, CDCl 3 ): δδ 8.72 (d, 1H), 8.0 (m, 2H), 7.5 (m, 2H), 7.12 (m, 2H), 6.6 (d, 1H), 6.54 (d, 1H), 5.10 (m, 1H), 4.66 (m, 2H), 4.42 (m, 1H), 3.80 (d, 1H), 2.2 (m, 3H), 2.08 (m, 1H), 0.95-1.60 (m, 18H).
Example 4
Preparation 4A: Furan-carboxylic acid {(S)-2-[4-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0176]
Preparation 4B: Furan-carboxylic acid {(L)-2-[4-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0177]
[0178] Following the procedure of Example 3(f-r), except substituting “4-methylcyclohexyl” for “1-methylcyclohexyl” gave the title compound: The 1 H NMR data of 4A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.75 (d, 1H), 8.0 (m, 2H), 7.60 (m, 2H), 7.1 (d, 1H), 6.90 (d, 1H), 6.75 (d, 1H), 6.5 (s, 1H), 5.15 (m, 1H), 4.80 (d, 1H), 4.70 (m, 1H), 4.45 (m, 1H), 3.9 (d, 1H), 2.2 (m, 3H), 0.85-1.90 (m, 19H). The 1 H NMR data of 4B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.75 (d, 1H), 8.0 (m, 2H), 7.50 (m, 2H), 7.20 (d, 1H), 7.06 (d, 1H), 6.70 (m, 1H), 6.5 (s, 1H), 5.1 (m, 1H), 4.70 (m, 2H), 4.45 (m, 1H), 3.85 (d, 1H), 2.2 (m, 3H), 0.85-1.90 (m, 19H).
Example 5
Preparation of 5A: Furan-carboxylic acid {(S)-2-[homocyclopentyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0179]
Preparation of 5B: furan-carboxylic acid {(L)-2-[homocyclopentyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0180]
[0181] Following the procedure of Example 3(f-r), except substituting “homocyclopentyl” for “1-methylcyclohexyl” gave the title compound: The 1 H NMR data of 5A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.75 (d, 1H), 8.0 (d, 1H), 7.95 (t, 1H), 7.55 (m, 1H), 7.48 (s, 1H), 7.15 (d, 1H), 6.85 (t, 2H), 6.54 (d, 1H), 5.15 (d, 1H), 4.80 (d, 1H), 4.60 (m, 1H), 4.45 (m, 1H), 3.85 (d, 1H), 2.20 (m, 2H), 1.90 (m, 1H), 1.0-1.83 (m, 17H). The 1 H NMR data of 5B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.70 (d, 1H), 8.0 (d, 1H), 7.95 (t, 1H), 7.5 (m, 2H), 7.2 (d, 1H), 7.0 (d, 1H), 6.8 (d, 1H), 6.5 (d, 1H), 5.15 (m, 1H), 4.75 (d, 1H), 4.6 (q, 1H), 4.45 (q, 1H), 3.85 (d, 1H), 2.2 (m, 2H), 2.0 (m, 1H), 1.0-1.80 (m, 17H).
Example 6
Preparation of 6A: Morpholine 4-carboxylic acid {(S)-2-[homocyclopentyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0182]
Preparation of 6B: morpholine 4-carboxylic acid {(L)-2-[homocyclopentyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0183]
[0184] Following the procedure of Example 1(f-r), except substituting “homocyclopentyl” for “1-methylcyclopentyl” gave the title compound: The 1 H NMR data of 6A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.7 (d, 1H), 7.9 (m, 2H), 7.50 (m, 1H), 7.0 (m, 1H), 5.30 (d, 1H), 5.10 (m, 1H), 4.70 (d, 1H), 4.35 (m, 2H), 3.80 (d, 1H), 3.65 (t, 4H), 3.35 (t, 4H), 2.20 (m, 3H), 0.90-1.75 (m, 17H). The 1 H NMR data of 6B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.70 (d, 1H), 8.0 (d, 1H), 7.95 (t, 1H), 7.50 (m, 1H), 7.0 (d, 1H), 5.10 (m, 1H), 5.0 (d, 1H), 4.70 (d, 1H), 4.50 (m, 1H), 4.40 (m, 1H), 3.85 (d, 1H), 3.70 (t, 4H), 3.40 (t, 4H), 2.20 (m, 3H), 1.0-1.9 (m, 17H).
Example 7
Preparation of 7A: furan-carboxylic acid {(S)-2-[cycloheptyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0185]
Preparation of 7B: furan-carboxylic acid {(L)-2-[cycloheptyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0186]
[0187] Following the procedure of Example 3(f-r), except substituting “cycloheptyl” for “1-methylcyclohexyl” gave the title compound: The 1 H NMR data of 7A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.70 (d, 1H), 8.0 (d, 1H), 7.90 (t, 1H), 7.55 (m, 1H), 7.5 (s, 1H), 7.15 (d, 1H), 6.90 (d, 1H), 6.80 (d, 1H), 6.5 (d, 1H), 5.15 (m, 1H), 4.80 (d, 1H), 4.60 (q, 1H), 4.40 (q, 1H), 3.9 (d, 1H), 2.2 (m, 2H), 1.0-1.80 (m, 20H). The 1 H NMR data of 7B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.70 (d, 1H), 8.0 (d, 1H), 7.90 (t, 1H), 7.55 (d, 1H), 7.50 (s, 1H), 7.15 (d, 1H), 7.05 (d, 1H), 6.7 (d, 1H), 6.5 (d, 1H), 5.10 (m, 1H), 4.75 (d, 1H), 4.65 (m, 1H), 4.5 (m, 1H), 3.85 (d, 1H), 2.20 (m, 2H), 1.0-1.90 (m, 20H).
Example 8
Preparation of 8A: morpholine 4-carboxylic acid {(S)-2-[cycloheptyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0188]
Preparation of 8B: morpholine 4-carboxylic acid {(L)-2-[cycloheptyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0189]
[0190] Following the procedure of Example 1(f-r), except substituting “cycloheptyl” for “1-methylcyclopentyl” gave the title compound: The 1 H NMR data of 8A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.75 (d, 1H), 8.0 (m, 2H), 7.55 (m, 1H), 6.85 (m, 1H), 5.15 (m, 1H), 4.95 (m, 1H), 4.80 (d, 1H), 4.45 (m, 2H), 3.90 (d, 1H), 3.7 (t, 4H), 3.40 (t, 4H), 2.2 (m, 3H), 1.0-1.80 (m, 19H). The 1 H NMR data of 8B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.75 (d, 1H), 8.0 (m, 2H), 7.55 (m, 1H), 7.10 (m, 1H), 5.10 (m, 1H), 4.80 (m, 1H), 4.75 (d, 1H), 4.40 (m, 2H), 3.85 (d, 1H), 3.70 (t, 4H), 3.40 (t, 4H), 2.2 (m, 3H), 1.0-1.80 (m, 19H).
Example 9
Preparation of 9A: furan-carboxylic acid {(S)-2-[cyclopentenyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0191]
Preparation of 9B: furan-carboxylic acid {(L)-2-[cyclopentenyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0192]
[0193] Following the procedure of Example 3(f-r), except substituting “cyclopentenyl” for “1-methylcyclohexyl” gave the title compound: The 1 H NMR data of 9A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.7 (d, 1H), 8.0 (m, 2H), 7.5 (m, 2H), 7.1 (d, 1H), 7.0 (d, 1H), 6.85 (d, 1H), 6.5 (d, 1H), 5.6 (m, 1H), 5.1 (m, 1H), 4.7 (m, 2H), 4.4 (m, 1H), 3.80 (m, 1H), 2.7 (m, 2H), 2.3 (m, 4H), 2.2 (m, 2H), 1.9 (m, 2H), 1.0-1.7 (m, 5H). The 1 H NMR data of 9B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.7 (d, 1H), 8.0 (m, 2H), 7.5 (m, 2H), 7.2 (d, 1H), 7.1 (d, 1H), 6.80 (d, 1H), 6.5 (d, 1H), 5.5 (d, 1H), 5.1 (m, 1H), 4.7 (m, 2H), 4.4 (m, 1H), 3.8 (d, 1H), 2.7 (m, 2H), 2.3 (m, 4H), 2.2 (m, 2H), 1.9 (m, 2H), 1.0-1.6 (m, 5H).
Example 10
Preparation of 10A: furan-carboxylic acid {(S)-2-[tryptophanyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0194]
[0195] Following the procedure of Example 3(f-r), except substituting “tryptophanyl” for “1-methylcyclhexyl” gave the title compound: 1 H NMR (400 Hz, CDCl 3 ): δ 8.65 (m, 2H), 8.05 (d, 1H), 7.9 (t, 1H), 7.8 (d, 1H), 7.5 (m, 1H), 7.45 (s, 1H), 7.40 (d, 1H), 7.35 (d, 1H), 7.2 (m, 4H), 6.5 (d, 1H), 5.7 (d, 1H), 5.0 (m, 1H), 3.85 (m, 2H), 3.65 (m, 1H), 3.45 (m, 1H), 3.2 (m, 1H), 3.05 (m, 1H), 2.40 (d, 1H), 0.8-1.6 (m, 6H).
Example 11
Preparation of 11A: morpholine 4-carboxylic acid {(S)-2-(7,7-dimethyl-bicyclo[2.2.1]hepty-1-yl)-1-[(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0196]
Preparation of 11B: morpholine 4-carboxylic acid {(L)-2-(7,7-dimethyl-bicyclo[2.2.1]hepty-1-yl)-1-[(4S,7R)-7-methyl-3-oxo-1-(1-oxy-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0197]
[0198] Following the procedure of Example 1(f-r), except substituting “2-(7,7-dimethyl-bicyclo[2.2.1]hepty-1-yl)” for “1-methylcyclopentyl” gave the title compound: The 1 H NMR data of 11A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.65 (d, 1H), 7.9 (m, 2H), 7.40 (m, 1H), 6.9 (d, 1H), 4.9 (m, 2H), 4.65 (d, 1H), 4.3 (m, 2H), 3.75 (d, 1H), 3.6 (t, 4H), 3.3 (t, 4H), 2.1 (m, 2H), 0.8-1.7 (m, 22H).: The 1 H NMR data of 11B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.70 (d, 1H), 8.0 (m, 2H), 7.55 (d, 1H), 7.2 (d, 1H), 5.1 (m, 1H), 4.7 (m, 2H), 4.4 (m, 2H), 3.85 (d, 1H), 3.7 (t, 4H), 3.4 (t, 4H), 2.2 (m, 2H), 0.9-1.9 (m, 22H).
Example 12
Preparation of 12c: 2-methyl-2H-pyrazole-3-carboxylic acid {(S)-2-cyclopentyl-1-[(4S, 7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0199]
12a.) (S)-2-tert-Butoxycarbonylamino-3-cyclopentyl-propionic acid
[0200] The solution of (S)-2-amino-3-cyclopentyl-propionic acid (3.0 g, 19.1 mmol) in 30 mL of 1,4dioxane and water (1:1 ratio) was cooled to 0° C., sodium hydroxide (1.5 g, 38 mmol) and di-tert-butyldicarbonate (5.0 g, 22.9 mmol) were added. After stirring at room temperature overnight, the mixture was adjusted to pH 1 with concentrated HCl. The resulting mixture was extracted with ethyl acetate (3×), the combined organic phase was washed with brine, dried over MgSO 4 , filtered, and concentrated to give the title compound (4.9 g ). LC-MS m/z 258.2 (M + ), 1.84 min.
12b.) (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt
[0201] Following the procedure of Example 1p, (S)-2-tert-butoxycarbonylamino-3-cyclopentyl-propionic acid (4.42 g, 17.2 mmol) and (3S,4S,7R)-4-amino-7-methyl-1-(pyridine-2-sulfonyl)-azepan-3-ol, HCl salt (Example 1o, 7.26 g, 22.5 mmol) were reacted, followed by deprotection with 4N HCl in 1,4-dioxane to give title product (7.9 g, 72%). LC-MS m/z 452.0 (M + ), 1.54 min.
12c.) 2-Methyl-2H-pyrazole-3-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0202] To a solution of (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 125 mg, 0.27 mmol) in DMF, 2-methyl-2H-pyrazole-3-carboxylic acid (33 mg, 0.26 mmol), HBTU (128 mg, 0.34 mmol) and 4-methylmorpholine (143 μl, 1.3 mmol) were added. After the reaction mixture was stirred at room temperature for 16 hours, it was partitioned between ethyl acetate and water. The combined organic phase was washed with water, brine, dried over MgSO 4 , filtered and concentrated. Column chromatography (5% methanol:CH 2 Cl 2 ) of the residue provided 2-methyl-2H-pyrazole-3-carboxylic acid {(S)-2-cyclopentyl-1-[(3S,4S,7R)-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (74 mg, 51%). MS (m/z) 533.0 (M + ), 1.88 min.
[0203] To a stirring solution 2-methyl-2H-pyrazole-3-carboxylic acid {(S)-2-cyclopentyl-1-[(3S,4S,7R)-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl)-ethyl}-amide (74 mg, 0.14 mmol) in CH 2 Cl 2 (2 mL) was added Dess-Martin periodinane (77 mg, 0.18 mmol). After stirring for 3 hours, the mixture was concentrated. The residue was diluted with ethyl acetate and washed with water (2×). The organic layer was dried with MgSO 4 , filtered, and concentrated. Column chromatography (5% methanol:CH 2 Cl 2 ) of the residue, followed by recrystallization from dichloromethane and hexane provided the title compound (50 mg, 67%). LC-MS m/z 530.6 (M + ), 1.85 min.
Example 13
Preparation of 13: 1H-pyrazole-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0204]
[0205] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 200 mg, 0.43 mmol) was coupled with 1H-pyrrole-2-carboxylic acid (53 mg, 0.49 mmol), followed by oxidation with Dess-Martin periodinane (135 mg, 0.32 mmol) to give the title compound (50 mg, 23%). LC-MS m/z 516.2 (M + ), 1.94 min.
Example 14
Preparation of 14: 1-Methyl-1H-pyrrole-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0206]
[0207] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol) was coupled with 1-methyl-1H-pyrrole-2-carboxylic acid (50 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (20 mg, 18%). LC-MS m/z 530.0(M + ), 2.08 min.
Example 15
Preparation of 15: Isoxazole-5-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0208]
[0209] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 100 mg, 0.22 mmol) was coupled with isoxazole-5-carboxylic acid (25 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (15 mg, 0.27 mmol) to give the title compound (20 mg, 18%). LC-MS m/z 518 (M + ), 1.88 min.
Example 16
Preparation of 16b: Thiazole-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0210]
16a.) Thiazole-2-carboxylic acid
[0211] The mixture of thiazole-2-carboxylic acid ethyl ester (100 mg, 0.64 mmol) and lithium hydroxide monohydrate (134 mg, 3.18 mmol) in 5 mL of methanol was stirred at room temperature for 16 hours. After removing solvent, the residue was acidified with aq. 1N HCl, extracted with ethyl acetate (2×), washed with brine. The combined organic layer was dried over MgSO 4 , filtered and concentrated under reduced pressure to give crude material which was used directly in the next step without further purification (53 mg).
16b.) Thiazole-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0212] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 94 mg, 0.20 mmol) was coupled with thiazole-2-carboxylic acid (26 mg, 0.20 mmol), followed by oxidation with Dess-Martin reagent (121 mg, 0.29 mmol) to give the title compound (30 mg, 28%). LC-MS m/z 534.2(M + ), 2.04 min.
Example 17
Preparation of 17: 5-trifluoromethyl-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0213]
[0214] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol) was coupled with 5-trifluoromethyl-furan-2-carboxylic acid (72 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (29 mg, 15%). LC-MS m/z 585.0(M + ), 2.25 min.
Example 18
Preparation of 18b: 1H-pyrazole-4-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0215]
18a.) Pyrazole-1,4-dicarboxylic acid-1-tert-butyl ester
[0216] Following the general procedure in Example 12a, 1H-pyrazole-4-carboxylic acid (300 mg, 2.68 mmol), sodium hydroxide (214 mg, 5.36 mmol) and di-tert-butyldicarbonate (700 mg, 2.68 mmol) were reacted to give the title compound (153 mg, 27%). 1 H NMR (400 Hz, CDCl3) δ 8.66(s, 1H), 8.14 (s, 1H), 1.70 (s, 9H).
18b.) 1H-Pyrazole-4-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0217] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 166 mg, 0.36 mmol) was coupled with pyrazole-1,4-dicarboxylic acid-1-tert-butyl ester (77 mg, 0.36 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) and then removing the tert-butoxycarbonyl protecting group with 4N HCl to give the title compound (49 mg, 26%). LC-MS m/z 517.2 (M + ), 1.70 min.
Example 19
Preparation of 19: tetrahydrofuran-3-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0218]
[0219] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 200 mg, 0.43 mmol) was coupled with tetrahydro-furan-3-carboxylic acid (75 mg, 0.65 mmol), followed by oxidation with Dess-Martin periodinane (244 mg, 0.57 mmol) to give the title compound (88 mg, 39%). LC-MS m/z 521.2(M + ), 1.79 min.
Example 20
Preparation 20: 4,7-dimethyl-pyrazolo[5,1-c][1,2,4]triazine-3-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0220]
[0221] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol) was coupled with 4,7dimethyl-pyrazolo[5,1-c][1,2,4]triazine-3-carboxylic acid (77 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (3 mg, 2%). LC-MS m/z 597.0 (M + ), 2.13 min.
Example 21
Preparation of 21: 2,7-dimethyl-pyrazolo[5,1-a]pyrimidine-6-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0222]
[0223] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol) was coupled with 2,7-dimethyl-pyrazolo[5,1-a]pyrimidine-6-carboxylic acid (70 mg, 0.36 mmol), followed by oxidation with Dess-Martin periodinane (210 mg, 0.49 mmol) to give the title compound (80 mg, 41%). LC-MS m/z 596.0 (M + ), 1.92 min.
Example 22
Preparation of 22: 3-Phenyl-3H-[1,2,3]triazole-4-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0224]
[0225] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 180 mg, 0.39 mmol) was coupled with 3-phenyl-3H-[1,2,3]triazole-4-carboxylic acid (81 mg, 0.43 mmol), followed by oxidation with Dess-Martin periodinane (225 mg, 0.53 mmol) to give the title compound (77 mg, 37%). LC-MS m/z 594.2 (M + ), 2.02 min.
Example 23
Preparation of 23: 2-(2,3-Dihydro-benzo[1,4]dioxin-2-yl)-thiazole-4-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0226]
[0227] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol) was coupled with 2-(2,3-dihydro-benzo[1,4]dioxin-2-yl)-thiazole-4-carboxylic acid (99 mg, 0.37 mmol), followed by oxidation with Dess-Martin periodinane (230 mg, 0.54 mmol) to give the title compound (96 mg, 41%). LC-MS m/z 668.0 (M + ), 2.42 min.
Example 24
Preparation of 24: N-{(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-2-pyrazol-1-yl-benzamide
[0228]
[0229] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol) was coupled with 2-pyrazol-1-yl-benzoic acid (75 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (30 mg, 15%). LC-MS m/z 593.0 (M + ), 2.00 min.
Example 25
Preparation of 25: 4-Methyl-2-phenyl-thiazole-5-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0230]
[0231] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol) was coupled 4-methyl-2-phenyl-thiazole-5-carboxylic acid (88 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (117 mg, 57%). LC-MS m/z 624.2 (M + ), 2.50 min.
Example 26
Preparation of 26: 5-(4-Chloro-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0232]
[0233] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol) was coupled 5-(4chloro-phenyl)-furan-2-carboxylic acid (82 mg, 0.37 mmol), followed by oxidation with Dess-Martin periodinane (210 mg, 0.50 mmol) to give the title compound (82 mg, 40%). LC-MS m/z 627.2 (M + ), 2.57 min.
Example 27
Preparation of 27: 5-(3-trifluoromethyl-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0234]
[0235] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 100 mg, 0.22 mmol) was coupled 5-(3-trifluoromethyl-phenyl)-furan-2-carboxylic acid (56 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the tide compound (60 mg, 40%). LC-MS m/z 661.2 (M + ), 2.57 min.
Example 28
Preparation of 28b: 5-(2-Chloro-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0236]
28a.) 5-Bromo-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0237] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 1.0 g, 2.17 mmol) was coupled 5-bromo-furan-2-carboxylic acid (415 mg, 2.17 mmol) to give the title compound (780 mg, 60%). LC-MS m/z 597.0(M + ), 1.99 min.
28b.) 5-(2-Chloro-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0238] The mixture of 5-bromo-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (25 mg, 0.04 mmol), 2-chlorophenylboronic acid (7 mg, 0.04 mmol), tetrakis-(triphenylphosphine)palladium(o) (2.4 mg, 5%) and potassium carbonate (17.4 mg, 0.13 nmnol) in the mixture of 2 mL of 1,4-dioxane and 0.5 mL of water was heated at 100° C. in the Smith Creator microwave for 800 seconds. The mixture was then diluted with ethyl acetate, washed with water, brine, dried over Anhydrous sodium sulfate, filtered and concentrated to give crude 3-hydroxy intermediate. Upon oxidation as described in Example 12c with Dess-Martin periodinane (50 mg, 0.12 mmol), the title compound was obtained (4 mg, 15%). LC-MS m/z 627.2 (M + ), 2.49 min.
Example 29
Preparation of 29: 5-(4-fluoro-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0239]
[0240] Following the general procedure described in Example 28b, the coupling of 5-bromo-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (Example 28a, 25 mg, 0.04 mmol) with 4-fluorophenylboronic acid (6.4 mg, 0.05 mmol), followed by oxidation with Dess-Martin periodinane (50 mg, 0.12 mmol), the title compound was obtained (6.2 mg, 24%). LC-MS m/z 611.2(M + ), 2.42min.
Example 30
Preparation of 30: 5-(4-methoxy-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0241]
[0242] Following the general procedure described in Example 28b, the coupling of 5-bromo-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (Example 28a, 25 mg, 0.04 mmol) with 4-methoxyphenylboronic acid (7.0 mg, 0.05 mmol), followed by oxidation with Dess-Martin periodinane (50 mg, 0.12 mmol), the title compound was obtained (18 mg, 69%). LC-MS m/z 623.4(M + ), 2.42 min.
Example 31
Preparation of 31: 5-phenyl-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0243]
[0244] Following the general procedure described in Example 28b, the coupling of 5-bromo-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (Example 28a, 25 mg, 0.04 mmol) with phenylboronic acid (5.6 mg, 0.05 mmol), followed by oxidation with Dess-Martin periodinane (50 mg, 0.12 mmol), the title compound was obtained (10 mg, 42%). LC-MS m/z 593.2(M + ), 2.40 min.
Example 32
Preparation of 32: 5-(4-trifluoromethyl-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0245]
[0246] Following the general procedure described in Example 28b, the coupling of 5-bromo-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (Example 28a, 25 mg, 0.04 mmol) with 4-trifluoromethyl-phenylboronic acid (8.7 mg, 0.05 mmol), followed by oxidation with Dess-Martin periodinane (50 mg, 0.12 mmol), the title compound was obtained (15 mg, 56%). LC-MS m/z 661.2(M + ), 2.59 min.
Example 33
Preparation of 33: 5-(3-chloro-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0247]
[0248] Following the general procedure described in Example 28b, the coupling of 5-bromo-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (Example 28a, 25 mg, 0.04 mmol) with 3-chloro-phenylboronic acid (7.2 mg, 0.05 mmol), followed by oxidation with Dess-Martin periodinane (23 mg, 0.05 mmol), the title compound was obtained (7 mg, 28%). LC-MS m/z 627.2(M + ), 2.59 min
Example 34
Preparation of 34: 5-(4-methylphenyl)furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0249]
[0250] Following the general procedure described in Example 28b, the coupling of 5-bromofuran-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (Example 28a, 25 mg, 0.04 mmol) with p-toylboronic acid (6.3 mg, 0.05 mmol), followed by oxidation with Dess-Martin periodinane (48 mg, 0.11 mmol), the title compound was obtained (6.2 mg, 25%). LC-MS miz 607.4(M + ), 2.59 min.
Example 35
Preparation of 35: 5-(4-acetyl-phenyl)-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0251]
[0252] Following the general procedure described in Example 28b, the coupling of 5-bromo-furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (Example 28a, 25 mg, 0.04 mmol) with 4-acetyl-phenylboronic acid (7.5 mg, 0.05 mmol), followed by oxidation with Dess-Martin periodinane (50 mg, 0.12 mmol), the title compound was obtained (15 mg, 59%). LC-MS m/z 635.2(M + ), 2.30 min
Example 36
Preparation of 36: 4-Methyl-piperazine-1-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0253]
[0254] The mixture (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol), 4-methyl-piperazine-1-carbonyl chloride (66 mg, 0.33 mmol) and 0.5 mL of pyridine in 2 mL of dichloromethane was stirred at room temperature for 18 hours. The mixture was then diluted with dichloromethane, washed with water, brine, dried over Anhydrous sodium sulfate, filtered and concentrated to give the crude 3-hydroxy intermediate (117 mg). Upon oxidation as described in Example 12c with Dess-Martin reagent (121 mg, 0.29 mmol), the title compound was obtained (50 mg, 43%). LC-MS m/z 549.2 (M + ), 1.46 min.
Example 37
Preparation of 37c: Piperazine-1-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0255]
37a.) 4-(1-Imidazol-1-yl-methanoyl)-piperazine-1-carboxylic acid tert-butyl ester
[0256] The mixture of piperazine-1-carboxylic acid tert-butyl ester (2.0 g, 10.7 mmol) and 1,1-di-imidazol-1-yl-methanone (1.9 g, 11.8 mmol) in 40 mL of tetrohydrofuran was heated to 60° C. for 18 hr. The mixture was concentrated and purified via silica gel column chromatography (ethyl acetate 100%) to provide the title compound (3.9 g, 100%). 1 H NMR (400 Hz, CDCl 3 ): δ 7.90 (s, 1H), 7.22 (s, 1H), 7.14 (s, 1H), 3.61 (t, 4H), 3.55 (t, 4H), 1.50 (s, 9H).
37b.) 4-(1-Imidazol-1-yl-methanoyl)-piperazine-1-carboxylic acid tert-butyl ester methyl iodide salt
[0257] The mixture of 4-(1-Imidazol-1-yl-methanoyl)-piperazine-1-carboxylic acid tert-butyl ester (3.9 g, 10.7 mmol) and iodomethane (2.67 mL, 42.8 mmol) in 20 mL of acetonitrile was stirred at room temperature for 18 hr. The mixture was concentrated and the residue was triturated with diethyl ether and hexanes to give the crude material which was used directly in the next step without further purification.
37c.) Piperazine-1-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0258] The mixture of (S)-2-amino-3-cyclopentyl-N-[(3S,4S,7R)-3-hydroxy-7-methyl-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 12b, 150 mg, 0.33 mmol), 4-(1-imidazol-1-yl-methanoyl)-piperazine-1-carboxylic acid tert-butyl ester methyl iodide salt (139 mg, 0.33 mmol) and triethylamine was heated at 70° C. for 10 min in the Smithcreator microwave to give the 3-hydroxy intermediate. Upon oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) followed by removal of the tert-butoxycarbonyl protecting group with 4N HCl the title compound was obtained (50 mg, 28%). LC-MS m/z 535.2 (M + ), 1.44 min.
Example 38
Preparation of 38h: 5-Trifluoromethyl-furan-2-carboxylic acid {(S)-2-cyclohexyl-1-[(s)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0259]
38a.) (S)—(R)-1-Oxiranyl-prop-2-en-1-ol
[0260] To a mixture of 4A molecular sieves (20 g) in 500 mL of dichloromethane at −30° C., was added titanium (IV) isopropoxide (17.7 mL, 59.4 mmol), followed by diisopropyl D-tartrate (16.4 mL, 77.3 mmol). The mixture was stirred at −30° C. for 30 min. 1,4-pentadien-3-ol (50 g, 0.59 mol) was added, follewed by cumene hydroperoxide (153 mL, 0.92 mol). After standing at −15° C. for 72 hr, 300 mL of diethyl ether and 50 mL of saturated aqueous Anhydrous sodium sulfate were added. The resulting mixture was stirred for 3.5 hours at room temperature, then filtered through celite. The organic phase was separated and concentrated. Column chromatography (5% diethyl ether/95% hextan to 50% diethyl ether/50% hexane) provided the crude title compound (56 g), which was used in next step without further purification.
38b.) 2-((R)—(S)-1-Oxiranyl-allyl)-isoindole-1,3-dione
[0261] The mixture of (S)—(R)-1-Oxiranyl-prop-2-en-1-ol (50 g, 0.5 mol), triphenylphosphine (196 g, 0.75 mol) and phthalimide (110 g, 0.75 mmol) in 300 mL of toluene was cooled to 0° C. where diisopropyl azodicarboxylate (147 mL 0.75 mol) in 100 mL of toluene was added dropwise. The resulting mixture was allowed to warm to ambient temperature and stirred for 18 hours. After standing at −15° C. for 60 min, the mixture was filtered and washed with toluene. The filtrate was washed with aqueous 1N NaOH (2×), water, then concentrated. Flash chromatography of the residue (20% diethyl ether/80% hexanes), followed by recrystallization from methanol provided the desired product (41 g, 36% two steps). 1 H NMR (400 Hz, DMSO-d6): δ 7.87-7.93 (m, 4H), 6.05-6.13 (m, 1H), 5.37-5.34 (m, 2H), 4.40-4.43 (m, 1H), 3.59-3.62 (m, 1H), 2.51-2.92 (m, 2H).
38c.) Pyridine-2-sulfonic acid allyl-[(2S,3S)-3-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-hydroxy-pent-4-enyl]-amide
[0262] To a mixture of 2-((R)—(S)-1-oxiranyl-allyl)-isoindole-1,3-dione (30 g, 132 mmol) and pyridine-2-sulfonic acid allylamide (26 g, 132 mmol) in 300 mL of isopropanol at room temperature, was added 1,8-diazabicyclo[5.4.0]undec-7-ene (1.97 mL, 13.2 mmol). The mixture was heated to reflux for 18 hours. The mixture was then cooled to ambient temperature, diluted with dichloromethane, washed with aqueous 1N HCl, water, and brine. The organic phase was dried over anhydrous sodium sulfate, filtered and concentrated to give the crude material which was used in the next step without further purification.
38d.) 2-[(3S,4S)-3-Hydroxy-1-(pyridine-2-sulfonyl)-2,3,4,7-tetrahydro-1H-azepin-4-yl]-isoindole-1,3-dione
[0263] The mixture of pyridine-2-sulfonic acid allyl-[(2S,3S)-3-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-2-hydroxy-pent-4-enyl]-amide (53 g, 12c4 mmol) in 700 mL of 1,2-dichloroethane was degassed for 5 min. Grubbs reagent (5.27 g, 6.21 mmol) was then added. The mixture was heated to 70° C. for 18 hours. The mixture was cooled to room temperature and filtered. The solid was washed with ethyl acetate and dried to yield the title compound (22 g, 44%). 1 H NMR (400 Hz, DMSO-d6): δ 8.78 (s, 1H), 8.13 (t, 1H), 7.96 (d, 1H), 7.85-7.89 (m, 4H), 7.73(m, 1H), 5.67-5.74 (m, 2H), 5.51 (m, 1H), 4.93-4.95 (m, 1H), 4.23-4.25 (m, 1H), 3.95 (m, 2H), 3.5980-3.83 (m, 1H), 3.36-3.39 (m, 1H).
38e.) 2-[(3S,4S)-3-Hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-isoindole-1,3-dione
[0264] To the mixture of 2-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-2,3,4,7-tetrahydro-1H-azepin-4-yl]-isoindole-1,3-dione (5 g, 12c.5 mmol) in 80 mL of N,N-dimethylformamide and 20 mL of ethanol was bubbled argon for 5 min, followed by addition of palladium (10 wt % on activated carbon, 2.5 g). The mixture was hydrogenated on a Parr hydrogenation apparatus at 50° C. for 2 hours and at room temperature for 16 hours. The mixture was filtered through celite and the filtrate concentrated to give the desired product (4.6 g, 91%). LC-MS m/z 402.2(M + ), 1.62 min
38f.) (3S,4S)-4-Amino-1-(pyridine-2-sulfonyl)-azepan-3-ol
[0265] To a suspension of 2-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-isoindole-1,3-dione (29 g, 72 mmol) in 500 mL of ethanol, hydrazine (8.8 mL, 281 mmol) was added. The mixture was heated at reflux for 2 hours. After cooling, the mixture was filtered and the filtrate concentrated. The residue was diluted with dichloromethane, washed with aqueous 10% Na 2 CO 3 , water, and brine. The organic phase was dried over anhydrous sodium sulfate, filtered and concentrated to give desired product (15 g, 76%). LC-MS m/z 272.0(M + ), 0.75 min,
38g.) (S)-2-Amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt
[0266] Following the procedure of Example 1p, (S)-2-tert-Butoxycarbonylamino-3-cyclohexyl-propionic acid (5.58 g, 20.6 mmol) and (3S,4S)-4-Amino-1-(pyridine-2-sulfonyl)-azepan-3-ol, (Example 38f, 5.07 g, 18.7 mmol) were reacted, followed by deprotection with 4N HCl in 1,4-dioxane to give the title product. LC-MS m/z 425.2 (M + ), 1.33 min.
38h.) 5-Trifluoromethyl-furan-2-carboxylic acid {(S)-2-cyclohexyl-1-[(s)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0267] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (150 mg, 0.33 mmol) was coupled with 5-trifluoromethyl-furan-2-carboxylic acid (72 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (17 mg, 6%). LC-MS m/z 585.2 (M + ), 2.34 min.
Example 39
Preparation of 39: 2,4-Dimethyl-thiazole-5-carboxylic acid {(S)-2-cyclohexyl-1-[(s)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0268]
[0269] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 150 mg, 0.33 mmol) was coupled with 2,4-dimethyl-thiazole-5-carboxylic acid (63 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (88 mg, 48%). LC-MS m/z 562.0 (M + ), 2.09 min.
Example 40
Preparation of 40: 5-Methyl-pyrazine-2-carboxylic acid {(S)-2-cyclohexyl-1-[(s)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0270]
[0271] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 150 mg, 0.33 mmol) was coupled with 5-methyl-pyrazine-2-carboxylic acid (55 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (62 mg, 35%). LC-MS m/z 543.2 (M + ), 2.07 min.
Example 41
Preparation of 41: 1-Methyl-1H-imidazole-2-carboxylic acid {(S)-2-cyclohexyl-1-[(s)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0272]
[0273] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 150 mg, 0.33 mmol) was coupled with 1-methyl-1H-imidazole-2-carboxylic acid (50 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (70 mg, 40%). LC-MS m/z 531.0 (M + ).
Example 42
Preparation of 42: 1H-Pyrazol-4-carboxylic acid {(S)-2-cyclohexyl-1-[(s)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0274]
[0275] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 165 mg, 0.36 mmol) was coupled with pyrazole-1,4-dicarboxylic acid-1-tert-butyl ester (Example 18a, 77 mg, 0.36 mmol), followed by removal of the tert-butoxycarbonyl protecting group with 4N HCl. Oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) gave the title compound (40 mg, 21%). LC-MS m/z 517.2 (M + ), 1.72 min.
Example 43
Preparation of 43: 4-Methyl-2-phenyl-thiazole-5-carboxylic acid {(S)-2-cyclohexyl-1-[(s)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0276]
[0277] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 150 mg, 0.33 mmol) was coupled with 4-methyl-2-phenyl-thiazole-5-carboxylic acid (88 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the tide compound (117 mg, 57%). LC-MS m/z 624.2 (M + ), 2.50 min.
Example 44
Preparation of 44: 2,5-Dimethyl-furan-3-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0278]
[0279] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 150 mg, 0.33 mmol) was coupled with 2,5-dimethyl-furan-3-carboxylic acid (56 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (42 mg, 23%). LC-MS m/z 545.0 (M + ), 2.27 min.
Example 45
Preparation of 45: 2-Methyl-furan-3-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0280]
[0281] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 150 mg, 0.33 mmol) was coupled with 2-methyl-furan-3-carboxylic acid (50 mg, 0.40 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (39 mg, 22%). LC-MS m/z 531.0 (M + ), 2.13 min.
Example 46
Preparation of 46: Isoxazole-5-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0282]
[0283] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with isoxazole-5-carboxylic acid (25 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (40 mg, 35%). LC-MS m/z 518.2 (M + ), 1.94 min.
Example 47
Preparation of 47: 5-Methyl-isoxazole-3-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0284]
[0285] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with 5-methyl-isoxazole-3-carboxylic acid (28 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) to give the title compound (53 mg, 45%). LC-MS m/z 531.8 (M + ), 2.14 min.
Example 48
Preparation of 48: 5-Methyl-isoxazole-4-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]ethyl}-amide
[0286]
[0287] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with 5-methyl-isoxazole-carboxylic acid (28 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (26 mg, 22%). LC-MS m/z 532.0 (M + ), 2.04 min.
Example 49
Preparation of 49: 3-Methyl-isoxazole-4-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0288]
[0289] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with 3-methyl-isoxazole-4-carboxylic acid (28 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (16 mg, 14%). LC-MS m/z 532.0 (M + ), 2.04 min.
Example 50
Preparation of 50: 2-Methyl-2H-pyrazole-3-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0290]
[0291] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with 2-methyl-2H-pyrazole-3-carboxylic acid (28 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (20 mg, 16%). LC-MS m/z 531.2 (M + ), 1.97 min.
Example 51
Preparation of 51: Pyrazine-2-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0292]
[0293] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with pyrazine-2-carboxylic acid (27 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (15 mg, 13%). LC-MS m/z 529.2 (M + ), 2.02 min.
Example 52
Preparation of 52: Thiazole-2-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0294]
[0295] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 94 mg, 0.20 mmol) was coupled with thiazole-2-carboxylic acid (Example 16a, 26 mg, 0.20 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (45 mg, 28%). LC-MS m/z 534.0 (M + ), 2.10 min.
Example 53
Preparation of 53: 2-Methyl-thiazole-4-carboxylic acid {(S)-2-cyclohexyl-1-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0296]
[0297] Following the general procedure described in Example 12c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with 2-methyl-thiazole-4-carboxylic acid (32 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (34 mg, 28%). LC-MS m/z 548.0 (M + ), 2.10 min.
Example 54
Preparation of 54: (S)-3-Cyclohexyl-N-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-yl]-2-(thiophene-2-sulfonylamino)-propionamide
[0298]
[0299] The mixture of (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol), thiophene-2-sulfonyl chloride (40 mg, 0.22 mmol) and triethyl amine (0.15 mL, 1.1 mmol) in 1 mL of dichloromethane was stirred at room temperature for 18 hours. The mixture was then diluted with ethyl acetate, washed with water and brine and dried over anhydrous sodium sulfate, filtered and concentrated to give the crude 3-hydroxy intermediate. Upon oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) the title compound was obtained (95 mg, 76%). LC-MS m/z 569.0 (M + ), 2.15 min.
Example 55
Preparation of 55: (S)-3-Cyclohexyl-2-(1-methyl-1H-imdiazole-4-sulfonylamino)-N-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide
[0300]
[0301] Following the general procedure described in Example 54, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with 1-methyl-1H-imdiazole-4-sulfonyl chloride (20 mg, 0.11 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (19 mg, 30%). LC-MS m/z 567.4 (M + ), 1.77 min.
Example 56
Preparation of 56: (S)-3-Cyclohexyl-2-(3,5-dimethyl-isoxazole-4-sulfonylamino)-N-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide
[0302]
[0303] Following the general procedure described in Example 54, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with 3,5-dimethyl-isoxazole-4-sulfonyl chloride (43 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (46 mg, 36%). LC-MS m/z 582.4 (M + ), 2.08 min.
Example 57
Preparation of 57b: (S)-3-Cyclohexyl-2-(furan-2-sulfonylamino)-N-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide
[0304]
57 a.) Furan-2-sulfonyl chloride
[0305] To a solution of furan (1.0 g, 15 mmol) in 10 mL of tetrahydrofuran at −78° C., n-butyl lithium (1.6M in hexane, 10 mL, 16 mmol) was added dropwise. The mixture was stirred at −78° C. for 30 min, after which time sulfur dioxide was bubbled through the solution for 5 min. The resulting mixture was then stirred for an additional 1 hour and warmed to ambient temperature. After re-cooling to 0° C., sulphuryl chloride (1.17 mL, 14.7 mmol) was added and the mixture stirred for 2 hours. The mixture was diluted with ethyl acetate, washed with water and brine, dried over MgSO 4 , filtered and concentrated to give crude material (1.5 g) which was used in the next step without further purification.
57b.) (S)-3-Cyclohexyl-2-(furan-2-sulfonylamino)-N-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide
[0306] Following the general procedure described in Example 54, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 150 mg, 0.33 mmol) was coupled with furan-2-sulfonyl chloride (54 mg, 0.33 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (34 mg, 19%). LC-MS m/z 553.2 (M + ), 2.00 min.
Example 58
Preparation of 58: (S)-3-Cyclohexyl-N-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-yl]-2-(pyridine-2-sulfonylamino)-propionamide
[0307]
[0308] Following the general procedure described in Example 54, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl)-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with pyridine-2-sulfonyl chloride (39 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (19 mg, 15%). LC-MS m/z 564.0 (M + ), 1.88 min.
Example 59
Preparation of 59: (S)-3-Cyclohexyl-2-(morpholine-4-sulfonylamino)-N-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide
[0309]
[0310] Following the general procedure described in Example 54, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with morpholine-4-sulfonyl chloride (prepared from coupling of morpholing with sulphuryl chloride, 41 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (7 mg, 6%). LC-MS m/z 572.0 (M + ).
Example 60
Preparation of 60: (S)-3-Cyclohexyl-2-(5-isoxazol-3-yl-thiophene-2-sulfonylamino)-N-[(S)-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide
[0311]
[0312] Following the general procedure described in Example 54, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 100 mg, 0.22 mmol) was coupled with 5-isoxazol-3-yl-thiophene-2-sulfonyl chloride (55 mg, 0.22 mmol), followed by oxidation with Dess-Martin periodinane (121 mg, 0.29 mmol) to give the title compound (38 mg, 27%). LC-MS m/z 636.2 (M + ), 2.12 min.
Example 61
Preparation of 61: 4-{(S)-3-Cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino]-propanoylamino}-3-oxo-azepane-1-carboxylic acid benzyl ester (first diastereomer eluted)
[0313]
61a.) Allyl-pent-4-enyl-carbamic acid benzyl ester
[0314] To a suspension of NaH (1.83 g, 76.33 mmol of 90% NaH) in DMF was added benzyl allyl-carbamic acid benzyl ester (7.3 g, 38.2 mmol) in a dropwise fashion. The mixture was stirred at room temperature for approximately 10 minutes whereupon 5-bromo-1-pentene (6.78 mL, 57.24 mmol) was added in a dropwise fashion. The reaction was heated to 40° C. for approximately 4 hours whereupon the reaction was partitioned between dichloromethane and water. The organic layer was washed with water (2×'s), brine, dried (MgSO 4 ), filtered and concentrated. Column chromatography of the residue (10% ethyl acetate:hexanes) provided 10.3 grams of the title compound as an oil: MS(EI) 260 (M+H + ).
61b.) 2,3,4,7-Tetrahydro-azepine-1-carboxylic acid benzyl ester
[0315] To a solution of compound of Example 1a (50 g) in dichloromethane was added bis(tricyclohexylphosphine)benzylidine ruthenium (W) dichloride (5.0 g). The reaction was heated to reflux until complete as determined by TLC analysis. The reaction was concentrated in vacuo. Column chromatography of the residue (50% dichloromethane:hexanes) gave 35 g of the title compound: MS(EI) 232 (M+H + ).
61c.) 8-Oxa-3-aza-bicyclo[5.1.0]octane-3-carboxylic acid benzyl ester
[0316] To a solution of the compound of Example 1b (35 g, 1.5 mol) in CH 2 Cl 2 was added m-CPBA (78 g, 0.45 mol). The mixture was stirred overnight at room temperature whereupon it was filtered to remove the solids. The filtrate was washed with water and saturated NaHCO 3 (several times). The organic layer was dried (MgSO 4 ), filtered and concentrated to give 35 g of the title compound which was of sufficient purity to use in the next step: MS(EI) 248 (M+H + ), 270 (M+Na + ).
61d.) 4-azido-3-hydroxy-azepane-1-carboxylic acid benzyl ester
[0317] To a solution of the epoxide from Example 1c (2.0 g, 8.1 mmol) in methanol:water (8:1 solution) was added NH 4 Cl (1.29 g, 24.3 mmol) and sodium azide (1.58 g, 24.30 mmol). The reaction was heated to 40° C. until complete consumption of the starting epoxide was observed by TLC analysis. The majority of the solvent was removed in vacuo and the remaining solution was partitioned between ethyl acetate and pH 4 buffer. The organic layer was washed with sat. NaHCO 3 , water, brine dried (MgSO 4 ), filtered and concentrated. Column chromatography (20% ethyl acetate:hexanes) of the residue provided 1.3 g of the title compound: MS(E) 291 (M+H + ) plus 0.14 g of trans-4-hydroxy-3-azido-hexahydro-1H-azepine
61e.) 4-Amino-3-hydroxy-azepane-1-carboxylic acid benzyl ester
[0318] To a solution of the azido alcohol of Example 1d (1.1 g, 3.79 mmol) in methanol was added triethylamine (1.5 mL, 11.37 mmol) and 1,3-propanedithiol (1.1 mL, 11.37 mL). The reaction was stirred until complete consumption of the starting material was observed by TLC analysis whereupon the reaction was concentrated in vacuo. Column chromatography of the residue (20% methanol:dichloromethane) provided 0.72 g of the title compound: MS(EI) 265 (M+H + ).
61f.) 4-((S)-2-tert-Butoxycarbonylamino-3-cyclopentyl-propanoylamino)-3-hydroxy-azepan-1-carboxylic acid benzyl ester
[0319] To a mixture of the hydrochloride salt of 4-amino-3-hydroxy-azepane-1-carboxylic acid benzyl ester (Example 61e, 1.17 g, 3.89 mmol), (S)-2-tert-butoxycarbonylamino-3-cyclopentylpropionic acid (1.0 g, 3.89 mmol), and 4-methylmorpholine (1.985 g, 19.45 mmol) stirring in DMF (40 mL) was added HBTU (1.915 g, 5.05 mmol). The resulting mixture was stirred under argon at room temperature for 90 minutes. The reaction was concentrated in vacuo, and the residue was partitioned between ethyl acetate and water. The organic phase was washed with water (3×), brine (1×), dried over anhydrous sodium sulfate, filtered and evaporated to give the crude product which was flash chromatographed on silica gel (70 g) eluted with 0-4% methanol in methylene chloride to give the title compound (a mixture of diastereomers) as a white foam. LC-MS M+H + =504.
61g.) 4((S)-2-Amino-3-cyclopentyl-propanoylamino)-3-hydroxy-azepane-1-carboxylic acid benzyl ester
[0320] 4((S)-2-tert-Butoxycarbonylamino-3-cyclopentyl-propanoylamino)-3-hydroxy-azepane-1-carboxylic acid benzyl ester (Example 61f, 1.81 g, 3.6 mmol) was dissolved in methanol (55 mL), and treated with HCL in dioxane (4.0 M, 13.5 mL). The mixture was stirred under argon at room temperature for 6 hours. The reaction was concentrated in vacuo. The residue was mixed with toluene and concentrated in vacuo (2×). The residue was triturated with ether (2×), and the residue dried in vacuo overnight to give the crude title product (a mixture of diastereomers) as a white foam which was used without further purification.h LC-MS M+H + =404.
61h.) 4-{(S)-3-Cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino]-propanoylamino}-3-hydroxy-azepane-1-carboxylic acid benzyl ester
[0321] To a mixture of 4-((S)-2-amino-3-cyclopentyl-propanoylamino)-3-hydroxy-azepane-1-carboxylic acid benzyl ester (Example 61g, 1.6 g, 3.64 mmol), 2-furoic acid (0.416 g, 3.64 mmol), and 4-methylmorpholine (1.84 g, 18.2 mmol) stirring in DMF (46 mL) was added HBTU (1.79 g, 4.73 mmol). The resulting mixture was stirred under argon at room temperature for 1 hour. The reaction was concentrated in vacuo, and the residue partitioned between ethyl acetate and water. The organic phase was washed with water (3×), brine (1×), dried over anhydrous sodium sulfate, filtered and evaporated to give the crude product which was flash chromatographed on silica gel (90 g) eluted with 14% methanol in methylene chloride. This material was rechromatographed on silica gel (120 g) eluted with 0-4% methanol in methylene chloride to give the title compound (a mixture of diastereomers) as a white solid. LC-MS M+H + =498.
61i.) 4-{(S)-3Cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino]-propanoylamino}-3-oxo-azepane-1-carboxylic acid benzyl ester
[0322] To a solution of 4-{(S)-3-cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino]-propanoylamino}-3-hydroxy-azepane-1-carboxylic acid benzyl ester (Example 61h, 103 mg, 0.207 mmol) stirring under argon in methylene chloride (10 mL) was added Dess-Martin periodinane (132 mg, 0.311 mmol). The mixture was stirred for 1 hour at room temperature. The reaction was worked up by diluting with methylene chloride and washing the organic phase three times with a 1:1 mixture of 10% NaHCO 3 and 10% Na 2 S 2 O 5 . The organic phase was dried over anhydrous sodium sulfate, filtered and evaporated. The crude product was chromatographed on silica gel (10 g) eluted with 0-4% methanol in methylene chloride to give the title compound as a mixture of diastereomers. LC-MS M+H + =496.
61j.) 4-{(S)-3-Cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino]-propanoylamino}-3-oxo-azepane-1-carboxylic acid benzyl ester (first diastereomer eluted)
[0323] The mixture of diastereomers from Example 61i was separated on a preparative R,R Whelk-O column. The first diastereomer eluted was the title compound, a white amorphous solid. mp 72-74° C.; LC-MS M+H + =496; 1 H NMR (400 Hz, CDCl 3 ): δ 7.48 (s, 1H), 7.36-7.41 (m, 5H), 6.94-6.99 (m, 1H), 6.78-6.84 (m, 2H), 6.53 (s, 1H), 5.09-5.28 (m, 2H), 4.22-4.82 (m, 4H), 3.62-3.71 (m, 1H), 1.17-2.67 (m, 16H).
Example 62
Preparation of 62: 4-{(S)-3-Cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino]-propanoylamino)-3-oxo-azepane-1-carboxylic acid benzyl ester (second diastereomer eluted)
[0324]
[0325] The mixture of diastereomers from Example 61i was separated on a preparative R,R Whelk-O column. The second diastereomer eluted was the title compound, a white amorphous solid. mp 66-68° C.; LC-MS M+H + =496; 1 H NMR (400 Hz, CDCl 3 ): δ 7.49 (s, 1H), 6.74-7.39 (m, 8H), 6.53 (s, 1H), 4.23-4.28 (m, 6H), 3.59-3.70 (m, 1H), 1.18-2.67 (m, 16H).
Example 63
Preparation of 63b: Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]ethyl}-amide (first diastereomer eluted)
[0326]
63a.) Furan-2-carboxylic acid [(S)-2-cyclopentyl-1-(3-hydroxy-azepan-4-ylcarbamoyl)-ethyl]-amide
[0327] 4-{(S)-3Cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino]-propanoylamino}-3-hydroxy-azepane-1-carboxylic acid benzyl ester (Example 61h, 0.5 g, 1 mmol) was dissolved in methylene chloride (10 mL) and stirred under argon in an ice bath. Trimethylsilyl iodide (0.5 mL, 3.5 mmol)was added dropwise, and the ice bath was removed. After stirring for three hours at room temperature the solvent was removed in vacuo. The residue was taken up in ether and extracted three times with IN HCl. The combined aqueous HCl phases were neutralized with solid sodium carbonate, and extracted with methylene chloride (5×). The combined organic phases were dried over anhydrous sodium sulfate, filtered, and evaporated to give the title compound (a mixture of diastereomers) as a white solid which was used without further purification. LC-MS M+H + =364.
63b.) Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0328] Furan-2-carboxylic acid [(S)-2-cyclopentyl-1-(3-hydroxy-azepan-4-ylcarbamoyl)-ethyl]-amide (Example 63a, 72 mg, 0.2 mmol) was dissolved in methylene chloride (5 mL), and a solution of 10% aqueous sodium bicarbonate (0.84 mL) was added. The mixture was stirred rapidly at room temperature, and pyridine-2-sulfonyl chloride (35.4 mg, 0.2 mmol) was added. After two hours, the reaction was diluted with methylene chloride, and water, and extracted with methylene chloride (3{). The combined organic phases were dried over anhydrous sodium sulfate filtered and evaporated to give the crude product. Flash chromatography on silica gel eluted with 0-4% methanol in methylene chloride gave the title compound as a mixture of diastereomers; C-MS M+H + =505.
63c.) Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0329] Following the procedure of Example 61i, except substituting furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (the product of Example 63b) for 4-{(S)-3-cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino]-propanoylamino}-3-hydroxy-azepane-1-carboxylic acid benzyl ester. gave the title compound as a mixture of diastereomers. LC-MS M+H + =503.
63d.) Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (first diastereomer eluted)
[0330] The mixture of diastereomers from Example 63c was separated on a preparative Chiralpak AD column. The first diastereomer eluted was the title compound, a white amorphous solid. mp 81-84° C.; LC-MS M+H + =503; 1 H NMR (400 Hz, CDCl 3 ): δ 8.71 (d, 1H), 7.94-7.99 (m, 2H), 7.50-7.54 (m, 2H), 7.16-7.17 (m, 1H), 7.08-7.09 (m, 1H), 6.77-6.80 (m, 1H), 6.53-6.54 (m, 1H), 5.14-5.17 (m, 1H), 4.64-4.76 (m, 2H), 4.11-4.30 (m, 1H), 3.85 (d, 1H), 2.74-2.75 (m, 1H), 1.15-2.25 (m, 15H).
Example 64
Preparation of 64: Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]ethyl}-amide (second diastereomer eluted)
[0331]
[0332] The mixture of diastereomers from Example 63c was separated on a preparative Chiralpak AD column. The second diastereomer eluted was the title compound, a white amorphous solid. mp 77-80° C.; LC-MS M+H + =503; 1 H NMR (400 Hz, CDCl 3 ): δ 8.71 (d, 1H), 7.93-8.01 (m, 2H), 7.48-7.56 (m, 2H), 7.13-7.14 (m, 1H), 6.96-6.97 (m, 1H), 6.84-6.86 (m, 1H), 6.51-6.52 (m, 1H), 5.14-5.22 (m, 1H), 4.64-4.76 (m, 2H), 4.11-4.16 (m, 1H), 3.85 (d, 1H), 2.68-2.75 (m, 1H), 1.19-2.27 (m, 15H).
Example 65
Preparation of 65: Furan-2-carboxylic acid [(S)-2-cyclopentyl-1-(1-methanesulfonyl-3-oxo-azepan-4ylcarbamoyl)-ethyl]-amide (first diastereomer eluted)
[0333]
[0334] Following the procedure of Example 63(b-d), except substituting methanesulfonyl chloride for pyridine-2-sulfonyl chloride in step 63b, and separating the diastereomers on a preparative R,R Whelk-O column, gave the title compound as the first diastereomer eluted, an off-white amorphous solid. mp 167-170° C.; LC-MS M+H + =440; 1 H NMR (400 Hz, CDCl 3 ): δ 7.48 (s, 1H), 7.15-7.16 (m, 1H), 6.93 (m, 1H), 6.85(m, 1H), 6.51-6.523(m, 1H), 5.14-5.22 (m, 1H), 4.52-4.71 (m, 2H), 4.11-4.16 (m, 1H), 3.65 (d, 1H), 2.93 (s, 3H) 1.16-2.93 (m, 16H).
Example 66
Preparation of 66: Furan-2-carboxylic acid [(S)-2-cyclopentyl-1-(1-methanesulfonyl-3-oxo-azepan-4-ylcarbamoyl)-ethyl]-amide (second diastereomer eluted)
[0335]
[0336] Following the procedure of Example 63(b-d), except substituting methanesulfonyl chloride for pyridine-2-sulfonyl chloride in step 63b, and separating the diastereomers on a preparative R,R Whelk-O column, gave the title compound as the second diastereomer eluted, an off-white amorphous solid. mp 158-161° C.; LC-MS M+H + =440; 1 H NMR (400 Hz, CDCl 3 ): δ 7.49 (s, 1H), 7.16-7.17 (m, 1H), 7.12-7.13 (m, 1H), 6.75-6.78(m, 1H), 6.52-6.54(m, 1H), 5.14-5.22 (m, 1H), 4.48-4.70 (m, 2H), 4.01-4.06 (m, 1H), 3.68 (d, 1H), 2.92 (s, 3H) 1.15-2.82 (m, 16H).
Example 67
Preparation of 67: Furan-2-carboxylic acid [(S)-1-(1-benzenesulfonyl-3-oxo-azepan-4 ylcarbamoyl)-2-cyclopentyl-ethyl]-amide (first diastereomer eluted)
[0337]
[0338] Following the procedure of Example 63(b-d), except substituting benzenesulfonyl chloride for pyridine-2-sulfonyl chloride in step 63b, and separating the diastereomers on a preparative R,R Whelk-O column, gave the title compound as the first diastereomer eluted, an off-white amorphous solid. mp 88-90° C.; LC-MS M+H + =502; 1 H NMR (400 Hz, CDCl 3 ): δ 7.82 (d, 2H), 7.48-7.66 (m, 4H), 7.13-7.14 (m, 1H), 6.82-6.91 (m, 2H), 6.52-6.53(m, 1H), 5.05-5.09 (m, 1H), 4.59-4.63 (m, 2H), 4.04-4.07 (m, 1H), 3.45 (d, 1H), 1.19-2.51 (m, 16H).
Example 68
Preparation of 68: Furan-2-carboxylic acid [(S)-1-(1-benzenesulfonyl-3-oxo-azepan-4-ylcarbamoyl)-2-cyclopentyl-ethyl]-amide (second diastereomer eluted)
[0339]
[0340] Following the procedure of Example 63(b-d), except substituting benzenesulfonyl chloride for pyridine-2-sulfonyl chloride in step 63b, and separating the diastereomers on a preparative R,R Whelk-O column, gave the title compound as the second diastereomer eluted, a white crystalline solid. mp 166-167° C.; LC-MS M+H + =502; 1 H NMR (400 Hz, CDCl 3 ): δ 7.80 (d, 2H), 7.50-7.66 (m, 4H), 7.17-7.18 (m, 1H.), 7.04 (m, 1H), 6.78 (m, 1H), 6.53-6.54(m, 1H), 5.03-5.08 (m, 1H), 4.50-4.66 (m, 2H), 3.98-4.02 (m, 1H), 3.48 (d, 1H), 1.18-2.56 (m, 16H).
Example 69
Preparation of 69: Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[1-(1-furan-2-yl-methanoyl)-3-oxo-azepan-4-ylcarbamoyl]-ethyl}-amide (first diastereomer eluted)
[0341]
69a.) Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[1-(1-furan-2-yl-methanoyl)-3-hydroxy-azepan-4-ylcarbamoyl]-ethyl}-amide
[0342] To a mixture of furan-2-carboxylic acid [(S)-2-cyclopentyl-1-(3-hydroxy-azepan-4-ylcarbamoyl)-ethyl]-amide (Example 63a,70 mg, 0.19 mmol), 2-furoic acid (22.4 mg, 0.19 mmol), and 4-methylmorpholine (0.1 mL, 0.95 mmol) stirring in DMF (2 mL) was added HBTU (93 mg, 0.25 mmol). The resulting mixture was stirred under argon at room temperature for 80 minutes. The reaction was concentrated in vacuo, and the residue was partitioned between ethyl acetate and water. The organic phase was washed with water (4×), brine (1×), dried over anhydrous sodium sulfate, filtered and evaporated to give the crude product which was flash chromatographed on silica gel (10 g) eluted with 0-5% methanol in methylene chloride to give the title compound as a mixture of diastereomers. LC-MS M+H + =458.
69b.) Furan-2-carboxylic acid {(S)2-cyclopentyl-1-[1-(1-furan-2-yl-methanoyl)-3-oxo-azepan-4-ylcarbamoyl]-ethyl}-amide
[0343] Following the procedure of Example 61i,_except substituting furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[1-(1-furan-2-yl-methanoyl)-3-hydroxy-azepan-4-ylcarbamoyl]-ethyl}-amide (the product of Example 69a) for 4-{(S)-3-cyclopentyl-2-[(1-furan-2-yl-methanoyl)-amino-propanoylamino}-3-hydroxy-azepane-1-carboxylic acid benzyl ester. gave the title compound as a mixture of diastereomers. LC-MS M+H + =456.
69c.) Furan-2-carboxylic acid {(S)2-cyclopentyl-1-[1-(1-furan-2-yl-methanoyl)-3-oxo-azepan-4-ylcarbamoyl]-ethyl}-amide (first diastereomer eluted)
[0344] The mixture of diastereomers from Example 69b was separated on a preparative R,R Whelk-O column. The first diastereomer eluted, an off-white amorphous solid, was the title compound. mp 88-89° C.; LC-MS M+H + =456; 1 H NMR (400 Hz, CDCl 3 ): δ 7.48-7.55 (m, 2H), 7.14-7.24 (m, 2H), 6.98 (m, 1H), 6.80 (m, 1H), 6.52-6.55(m, 2H), 5.4 (m, 1H), 4.60-4.90 (m, 4H), 3.70 (m, 1H), 1.18-2.30 (m, 15H).
Example 70
Preparation of 70: Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[1-(1-furan-2-yl-methanoyl)-3-oxo-azepan-4-ylcarbamoyl]-ethyl}-amide (second diastereomer eluted)
[0345]
[0346] The mixture of diastereomers from Example 69b was separated on a preparative R,R Whelk-O column. The second diastereomer eluted, an off-white amorphous solid, was the title compound. mp 85-88° C.; LC-MS M+H + =456; 1 H NMR (400 Hz, CDCl 3 ): δ 7.47-7.52 (m, 2H), 7.14-7.19 (m, 3H), 6.75-6.76 (m, 1H), 6.51-6.53 (m, 2H), 5.20-5.30 (m, 1H), 4.61-4.67 (m, 4H), 3.65-3.95 (m, 1H), 1.18-3.05 (m, 15H).
Example 71
Preparation of 71: Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[3-oxo-1-(1-phenyl-methanoyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (first diastereomer eluted)
[0347]
[0348] Following the procedure of Example 69(a-c) except substituting benzoic acid for furan-2-carboxylic acid in step 69a gave the title compound, as the first diastereomer eluted. mp 101-103° C.; LC-MS M+H + =466; 1 H NMR (400 Hz, CDCl 3 ): δ 7.48 (m, 5H), 7.14-7.15 (m, 1H), 6.75-6.76 (m, 1H), 7.03 (m, 1H), 6.83 (m, 1H) 6.52-6.53 (m, 1H) 5.30-5.40 (m, 1H), 3.64-4.79 (m, 5H), 1.18-3.05 (m, 15H).
Example 72
Preparation of 72: Furan-2-carboxylic acid {(S)-2-cyclopentyl-1-[3-oxo-1-(1-phenyl-methanoyl)-azepan-4-ylcarbamoyl]-ethyl}-amide (second diastereomer eluted)
[0349]
[0350] Following the procedure of Example 69(a-c) except substituting benzoic acid for furan-2-carboxylic acid in step 69a gave the title compound, as the second diastereomer eluted. mp 97-100° C.; LC-MS M+H + =466; 1 H NMR (400 Hz, CDCl 3 ): δ 7.20-7.45 (m, 6H), 7.14-7.15 (m, 1H), 7.03 (m, 1H), 6.82-6.84 (m, 1H) 6.51-6.52 (m, 1H) 5.20-5.40 (m, 1H), 3.64-4.90 (m, 5H), 1.18-3.05 (m, 15H).
Example 73
Preparation of 73: Piperazine-1-carboxylic acid {(S)-2-cyclopentyl-1-[(4S,7R)-7-methyl-3-oxo-1-(pyridine-2-sulfonyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0351]
[0352] Following the general procedure described in Example 37c, (S)-2-amino-3-cyclohexyl-N-[(3S,4S)-3-hydroxy-1-(pyridine-2-sulfonyl)-azepan-4-yl]-propionamide HCl salt (Example 38g, 150 mg, 0.33 mmol) was coupled with 4-(1-imidazol-1-yl-methanoyl)-piperazine-1-carboxylic acid tert-butyl ester methyl iodide salt (Example 37b, 139 mg, 0.33 mmol) to give the 3-hydroxy intermediate. Upon oxidation with Dess-Martin periodinane (182 mg, 0.43 mmol) followed by removal of the tert-butoxycarbonyl protecting group with 4N HCl the title compound was obtained (8 mg, 4%). LC-MS m/z 535.2 (M + ), 1.45 min.
Example 74
Preparation of 74A: morpholine 4-carboxylic acid {(S)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-pyridin-2-yl-meyhanoyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0353]
Preparation of 74B: morpholine 4-carboxylic acid {(L)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-pyridin-2-yl-methanoyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0354]
[0355] Following the procedure of Example 1(b-r), except substituting “1-pyridin-2-yl-methanoyl” for “1-oxy-pyridine-2-sulfonyl” gave the title compound: 1 HNMR data of 74A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.4 (d, 1H), 7.65 (m, 2H), 7.35 (m, 1H), 6.95 (d, 1H), 5.35 (m, 1H), 4.97 (m, 2H), 4.55 (d, 1H), 4.45 (m, 1H), 3.80 (d, 1H), 3.70 (t, 4H), 3.35 (t, 4H), 2.4 (m, 1H), 2.15 (m, 1H), 0.95-1.9 (m, 18H). The 1 H NMR data of 75B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.5 (d, 1H), 7.82 (m, 2H), 7.35 (m, 1H), 7.1 (d, 1H), 5.25 (m, 1H), 4.97 (m, 2H), 4.6 (d, 1H), 4.45 (m, 1H), 3.80 (d, 1H), 3.70 (t, 4H), 3.35 (t, 4H), 2.4 (m, 1H), 2.15 (m, 1H), 0.95-1.9 (m, 18H).
Example 75
Preparation of 75A: 2-Methyl-thiazole-4-carboxylic acid {(S)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo-1-(1-pyridin-2-yl-meyhanoyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0356]
Preparation of 74B: 2-Methyl-thiazole-4-carboxylic acid {(L)-2-[1-methylcyclohexyl-1-(4S,7R)-7-methyl-3-oxo1-(1-pyridin-2-yl-methanoyl)-azepan-4-ylcarbamoyl]-ethyl}-amide
[0357]
[0358] Following the procedure of Example 3(f-r), except substituting “2-Methyl-thiazole-4-carboxylic acid” for “morpholine-4-carboxylic acid” gave the title compound: 1 HNMR data of 74A: 1 H NMR (400 Hz, CDCl 3 ): δ 8.7 (d, 1H), 8.08 (d, 1H), 7.92 (s, 1H), 7.6 (d, 1H), 7.54 (d, 1H), 6.88 (d, 1H), 5.1 (m, 1H), 4.6 (m, 1H), 4.2 (d, 1H), 4.0 (m, 2H), 3.8 (m, 1H), 3.4 (d, 1H), 2.7 (s, 3H), 2.2 (m, 2H), 0.9-1.7 (m, 19H). The 1 H NMR data of 75B: 1 H NMR (400 Hz, CDCl 3 ): δ 8.7 (d, 1H), 8.1 (d, 1H), 7.92 (s, 1H), 7.65 (d, 1H), 7.52 (d, 1H), 6.9 (d, 1H), 5.10 (m, 1H), 4.6 (m, 1H), 4.1 (d, 1H), 4.0 (m, 2H), 3.8 (m, 1H), 3.4 (d, 1H), 2.7 (s, 3H), 2.2 (m, 2H), 0.9-1.7 (m, 19H).
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This invention relates 4-amino-azepan-3-ones of formula (I)
which are useful as protease inhibitors, particularly of cathepsin S, and as such are useful for preventing a number of diseases amongst which are atherosclerotic lesions and pulmonary diseases such as asthma and allergic reactions.
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TECHNICAL FIELD
This invention relates in general to a method of communication system channel management, or more particularly to overlapping radio patch operation.
BACKGROUND
In today's public safety environment, various municipalities and public agencies are searching for new ways to consolidate their operations and improve efficiency. These improvements must be accomplished without compromising the quality of service provided to the public. Therefore, the communications systems which are utilized by these entities must be very flexible, even when numerous users are contending for resources within the system.
During busy periods, it often becomes difficult for a dispatch console operator to quickly and efficiently manage activity on numerous pre-designated communications channels. Moreover, several dispatch consoles currently support a "channel assignment" concept requiring a distinct representation (i.e. radio panel, channel control module, etc.) for each individual channel. Dispatchers that are required to manage activity on more than one channel must assign the necessary channels, each with their own distinct representation.
With a multitude of individual channel representations, confusion may subsequently arise as to the source of call activity. This is especially true if the dispatcher is not watching the call indicators at all times; which often tends to be the case since many dispatchers focus their attention on computer based dispatching aids.
One way to address this problem is to allow the dispatcher to consolidate their assigned channels by collapsing several distinct channels into a single operational entity. A single entity representing multiple channel resources is referred to as a Composite Channel. All members of a composite channel are managed from a single channel representation and all are patched together. The composite channel enables the operator to focus their attention on a single operational entity; hence, the risk of confusion is reduced and efficiency is improved.
In a multi-operator dispatch environment, with Composite Channel and traditional Patch capabilities, it is reasonable to expect that individual channels will need to be placed into more than one patch group to satisfy the needs of all operators. For example, individual operators may wish to create composite channels that have one or more channels in common. Another example would be the establishment of a patch that involves one or more composite channels. Scenarios such as these lead to contention among operators for individual channel resources.
Existing dispatch systems provide limited patch capabilities to ensure that channel resource contention does not adversely affect system operation. For example, a dispatcher or operator is typically not permitted to place a communications channel into a patch if it is already involved in another patch. Were this to be allowed, such an "overlap" condition between the respective patches would result in one large patch consisting of all channels involved in each of the overlapping patches. This condition would bring many operational difficulties to both the communications system and the dispatcher. When each distinct patch is established, it is neither the desire nor the intent of the dispatcher to create a patch involving channels other than those that have been explicitly designated.
The benefits of consolidation previously described cannot be realized if individual channels can be involved in only one patch at a time. Therefore, the need exists for a method which can manage system audio connections by allowing a channel to be involved in multiple patches, established at different dispatch positions, while preventing interaction between channels which are not part of the same radio patch. Thus, a method is needed to manage dispatcher/radio channel interactions in such a way that the need to restrict access to radio patch capabilities is eliminated. Eliminating these restrictions while maintaining an orderly dispatch environment will improve the overall flexibility of the dispatch system. Additionally, a composite channel assignment method is needed which is an extension of the traditional channel assignment concept and can address the above requirements allowing a single point of control.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram showing the configuration of a communications system utilizing the method of the present invention.
FIG. 2 is a flow chart showing a general overview of the method of the present invention.
FIG. 3 is a flow chart showing the operation of the method of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1, a typical dispatch system 100 includes dispatch positions 101, 103 and 105 which are used with channels 107, 109, 111, 113, and 115. The directional arrows indicate the assignment of channels 107-115 through switching network 117 with dispatch positions 101, 103 and 105. In this configuration, two overlap conditions exist on channels 109 and 113 with dispatch positions 101 and 105 respectively. This configuration is by way of example only, and it will be evident to those skilled in the art that any type of configuration, channel assignment or overlap condition is possible.
The platform to which the method of the invention is applied consists of a multitude of radio channel resources and dispatch console positions as shown in FIG. 1. Dispatchers 101, 103, 105 control channel assignment. Channel assignment is the means by which dispatchers establish operations on designated channels 107-115. This is in contrast to channel patching where dispatchers combine operations of designated channels.
In order to facilitate non-interactive overlapping patches, the method of the invention is based on the following general precepts:
A Dispatcher receives all transmissions that "involve" their assigned channels. The term involve includes inbound traffic from subscribers on the channel, outbound traffic from subscribers on channels that are explicitly patched to the channel (at any dispatch position) and outbound traffic from other dispatchers who have the same channel assigned at their positions. A Dispatcher transmits only on those channels that are assigned at their position, regardless of any patch conditions.
A Subscriber receives all transmissions that "involve" their assigned channel. The term involve includes outbound traffic from dispatchers with the subscriber channel assigned at their position and outbound traffic from subscribers on other channels that are explicitly patched to the channel (at any dispatch position).
A flow chart showing the general operation of the method of the present invention is shown in FIG. 2. The method 150 requires that all individual dispatcher channel assignments be profiled and maintained 153, for example an Assignment Table. This table is organized in such a way that all dispatchers, that have a particular channel assigned, may be directly associated with activity on the channel. The contents of the assignment table are dynamic and are changed to reflect either the deletion of existing assignments or the creation of new assignments at any dispatch position in the system. The method uses this table to determine which dispatch positions are affected by a change in the state of a communication channel.
Further, the method also requires that all individual patches be profiled and maintained 155, for example in a Patch Table. This table is organized in such a way that each patch, its originating dispatcher and its constituent member channels are distinctly defined and maintained for the duration of the patch. The contents of the patch table are dynamic and are changed to reflect the deletion of existing patches or the creation of new patches at any dispatch position in the system. The method uses this table to determine which channel resources are affected by a change in the state of a particular channel. Further, the method also requires that all channel activity be detected and tracked 157. By its very nature, channel activity is dynamic and it is therefore tracked in real-time.
Finally, the method requires that a Connection Instance Count (CIC) be maintained for every individual audio connection in the system 159. This element is essential since multiple instances of a particular audio connection can be established by different aspects of system operation. For example, two instances of a connection will be established between a dispatcher and an assigned channel that is patched to another assigned channel and is receiving a signal. One instance of the connection will be due to the channel assignment since the dispatcher must receive all inbound activity on an assigned channel. The other connection instance will be due to the channel patch since the dispatcher must receive all patch related outbound activity that is destined for an assigned channel. Should the patch condition be cleared while the channel is active, the connection must be maintained because the assignment related connection instance remains. Hence, a particular connection is established only when the associated CIC is incremented from zero to one and the connection is removed only when the associated CIC is decremented from one to zero 161. Subsequent creation of new instances or deletion of existing instances are reflected as increments to the CIC or decrements to the CIC respectively.
One scenario that will arise repeatedly when using this method involves the connection of multiple audio sources to a single audio destination. This will occur, for example, when an individual channel is involved in two or more patches, and there is activity on other member channels of each of the patches. In this case, audio from the patches will be destined for the common channel and will be mixed on that channel.
FIG. 3 shows a flow chart diagram describing the method 200 of audio connection management which supports an overlapping radio patch operation. A communications system initiates the method 201 which designates a "change" in the system audio configuration (i.e. channel assignment, channel patch and/or channel activity). It is important to note that the method utilizes a dynamic connection scheme which establishes individual connections only when they are needed to carry traffic. Hence, upon any change to the system audio configuration, the potential need for new connections is analyzed and the status of existing connections is reviewed.
If there is a change in activity, assignment or patch status 203 the method looks to determine the nature of the change. The occurrence of new activity 205 will take the following forms:
(1) Receive activity is detected on the channel;
(2) The channel is involved in a new assignment at any dispatch position in the system; or
(3) The channel is involved in a new patch created at any dispatch position in the system.
The conclusion of ongoing activity 223 will take the following forms:
(1) There is no longer any receive activity on the channel;
(2) The channel is reassigned at any dispatch position in the system; or
(3) A patch involving the channel is cleared at any dispatch position in the system.
When new channel activity is detected 205, the method first determines the need for channel-to-dispatcher connections on the basis of explicit channel assignments 207. If the new activity is a result of new channel activity or a new channel assignment, the appropriate channel-to-dispatcher CIC(s) will be incremented. If the CIC is incremented from zero to one 209, the audio connection is established; otherwise 211, the method recognizes that the necessary connection is already in place and continues without further action. This portion of the method ensures that dispatchers receive all inbound activity on their assigned channels. It is also possible that the channel is not explicitly assigned to a dispatcher in which case this portion of the method is bypassed 208.
The method then determines the need for channel-to-channel connections on the basis of established patches 213. If new activity is a result of new channel activity or a new patch involving the channel, the appropriate channel-to-channel CIC(s) will be incremented. If the CIC is incremented from zero to one 215, the audio connection is established; otherwise 217, the method recognizes that the necessary connection is already in place and continues without further action. This portion of the method ensures that activity on a channel is routed to all other channels to which it is patched.
Finally, as a result of new channel activity or a new patch involving the channel, the appropriate channel-to-dispatcher CIC(s) will be incremented. If the CIC is incremented from zero to one 219, the audio connection is established; otherwise 221, the method recognizes that the necessary connection is already in place and continues without further action. This portion of the method ensures that outbound activity, on a channel resulting from a patch, is received by all dispatchers that have the channel assigned. It is also possible that the channel is not involved in any patches in which case this portion of the method is bypassed 214.
When ongoing channel activity has concluded 223, the method first determines the need to remove channel-to-dispatcher connections on the basis of explicit channel assignments 225. If the conclusion is a result of the cessation of channel activity or a channel deassignment, the appropriate channel-to-dispatcher CIC(s) will be decremented. If the CIC is decremented from one to zero 229, the audio connection is removed; otherwise 227, the method recognizes the ongoing need for the connection and continues without further action. It is also possible that the channel is not explicitly assigned to a dispatcher in which case this portion of the method is bypassed 226.
The method then determines the need to remove channel-to-channel connections on the basis of established patches 231. If the conclusion is a result of the cessation of channel activity or removal of a patch involving the channel, the appropriate channel-to-channel CIC(s) will be decremented. If the CIC is decremented from one to zero 233, the audio connection is removed; otherwise 235, the method recognizes the ongoing need for the connection and continues without further action.
Finally, as a result of the cessation of channel activity or removal of a patch involving the channel, the appropriate channel-to-dispatcher CIC(s) will be decremented. If the CIC is decremented from one to zero 237, the audio connection is removed; otherwise 239, the method recognizes the ongoing need for the connection and continues without further action. It is also possible that the channel is not involved in any patches in which case this portion of the method is bypassed 232.
In summary, the method of the present invention allows the communications system, having a plurality of channels, to support overlapping patches in such a way that there is no interaction between channels not explicitly patched. This occurs even though the channels may be involved in patch groups that contain common channels. The instant method does this by tracking each distinct channel assignment, tracing each radio patch and tracking the activity on each channel. Dynamic switching is then performed on the basis of each of these parameters. In tracking each channel during each instance of each connection the system ensures that connections are in place only when needed so latent connections do not result in unnecessary resource contention. When contention for an audio destination arises, the instant method will mix the audio signals from the various stations or sources. This however, will not preclude the system operation from giving preference to on audio source over others on the basis of a predetermined priority scheme or on a first-come-first-served basis.
There are many benefits arising from the use of the present method. These include allowing a multi-channel communications system to give better performance by allowing a channel to be involved in more than one patch. The ability to introduce a workable composite channel scheme. The creation of composite channels without regard for pre-existing patch activity within a system. The ability to freely patch composite channels without regard for preexisting patch activity within the system. The ability to patch or connect patches, i.e. establish a patch between existing patches, without regard for pre-existing patch activity within the system.
While the preferred embodiments of the invention have been illustrated and described, it will be clear that the invention is not so limited. Numerous modifications, changes, variations, substitutions and equivalents will occur to those skilled in the art without departing from the spirit and scope of the present invention as defined by the appended claims.
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A method of managing (150) an overlapping radio patch which allows a audio channel to be involved in multiple patches which are established at different dispatch positions. The method prevents interaction between channels that are not part of the same radio patch by maintaining dynamic profiles of channel assignments (153) and channel patches (155). Channel activity is tracked (157) and a connection instance count (CIC) is determined using the assignment and patch profiles as well as the channel activity. Audio connections are then managed (161) using the corresponding CIC's to dynamically switch connections. This ensures the connections are in place only when needed thereby avoiding any latent connections which would contend for network resources. The invention allows for the implementation of a composite channel concept which improves the overall capability of radio dispatch services in a multi-channel, multi-dispatcher environment.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention pertains to a method for hydraulically fracturing an earth formation from a wellbore by over-pressuring the wellbore with a pressure drive fluid and using one or more nearby wells in communication with the wellbore to be fractured to act as accummulators for the pressure drive fluid.
2. Background
U.S. patent application Ser. No. 07/874,159, filed Apr. 27, 1992 in the name of Joseph H. Schmidt, et al and assigned to the assignee of the present invention, is incorporated herein by reference. The Schmidt, et al patent application describes improved methods for over-pressuring a well to initiate or extend hydraulic fractures into an earth formation in communication with the well at a sustained flow rate to provide a near wellbore fracture which will not pinch off, in the near wellbore region, in a subsequent conventional hydraulic fracturing operation. The fracturing methods described in the Schmidt, et al patent application include the steps of providing a charge of compressed gas for urging fracturing fluid into the formation upon perforation of the well casing or upon release of the fracturing fluid to flow into the formation from a tubing string closed by a frangible closure member.
The methods described in the Schmidt, et al patent application, as well as the methods described in the prior art of record in the Schmidt, et al patent application, are, however, limited in their effectiveness by the amount of pressure gas charge that may be used to force the fracturing fluid into the formation during the fracture treatment. In this regard, there has been a recognized need to provide additional gas charge at the fracture or breakdown pressure to assure sufficient driving force for the fracturing fluid that is actually forced into the formation and which may include at least some of the gas charge itself. Further in this regard, pressure vessels full of pressure gas may be placed in communication with the well to be fractured. However, there are certain disadvantages to using pressure vessels charged with the pressure driving fluid. Since the fluid pressures required for the fracture treatment are usually relatively high any vessels charged with gas at the required pressures pose additional hazards to operating personnel and structure at or near the wellhead.
Still further, in certain well installations, such as on offshore platforms and the like, there is usually inadequate space for placing the pressure vessels or accummulators which might be used to supplement the pressure fluid charge used to effect the fracturing operation. However, in accordance with the present invention, a unique method has been developed for providing an accumulator for additional fluid charge available for driving the fracturing fluid into the formation to initiate or extend a suitable well fracture, which method is described in further detail hereinbelow.
SUMMARY OF THE INVENTION
The present invention provides a unique method for initiating or extending fractures in an earth formation through a well by forcing a hydraulic fracturing fluid into the formation at or above formation breakdown pressure and at a sustained flow rate provided by one or more accumulator wells which are placed in communication with the well to be fractured and which hold a charge of drive fluid at or above the pressure of the drive fluid charge in the well being fractured.
In accordance with an important aspect of the present invention, a charge of compressed gas is provided in a well conduit which is in communication with the wellbore region from which the fracture is to be extended and additional gas charge is built up in one or more wells adjacent to or capable of being placed in fluid flow communication with the well being fractured to provide additional drive fluid for driving fracturing fluid into the formation to be fractured. Accordingly, one or more "accumulator" vessels are provided by utilizing the volume of a nearby wellbore or a tubing string disposed in a nearby wellbore. In this way, additional drive fluid capacity is made available for use in the fracture initiation and extension without the requirement of providing pressure vessels at the surface and adjacent to the well being fractured. Accordingly, the costs and hazards associated with providing pressure vessels for pressure fluids used to initiate and extend a fracture from a wellbore using a so-called over-pressured method are eliminated or minimized by utilizing the fluid receiving and holding space of one or more wells which are near the well to be fractured and which may be easily placed in fluid flow communication with the well to be fractured.
Those skilled in the art will recognize the above-described features and advantages of the present invention together with other superior aspects thereof upon reading the detailed description which follows in conjunction with the drawing.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic diagram of a well to be fractured in accordance with the method of the invention and showing a drive fluid accumulator well in conjunction therewith; and
FIG. 2 is a section view of a shear disk and support body for use in connection with the method of the present invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIG. 1, there is illustrated a well 10 which extends into an earth formation 12 and is provided with a conventional casing 14, wellhead 15 and a tubing string 16 extending within the casing from the wellhead to a point adjacent a zone of interest 13 in the formation from which fluids are desired to be produced, for example. The formation zone of interest 13 lies generally below a conventional packer 18 which serves to pack off a space 20 in the casing 14 from an annular space 22 between the tubing string 16 and the casing 14.
The wellhead 15 is adapted to include a suitable wireline lubricator assembly 26 mounted thereon in a conventional manner and capable of being isolated from the interior of the tubing string 16 by a suitable wireline valve 27. In the arrangement illustrated in FIG. 1, the well 10 has been configured to prepare for perforation of the casing 14 and subsequent fracturing of the earth formation in the zone 13. In this regard, a conventional casing perforating tool or gun 28 is disposed in the space 20 and suspended from a conventional electric line 30. The gun 28 is operable to perforate the casing 14 to provide perforations or ports 32 into the formation zone 13. The tubing string 16 is also provided with a suitable landing nipple 34 at the lower distal end thereof whereby, if the perforations 32 already exist, an alternate embodiment of the method of the invention may be carried out as will be explained in further detail herein.
In the condition of the well 10 illustrated, the space 20 and the tubing string 16 are filled with a suitable fracturing liquid up to a level indicated by numeral 40. Liquid may be introduced into the space 20 and the tubing string 16 by way of a pump 42 in communication with the wellhead 15 by way of a shutoff valve 44 or the liquid level 40 may be achieved by the methods described in U.S. patent application Ser. No. 07/874,159. The annular space 22 is also operable to be in communication with a source of pressure fluid, not shown, by way of a conduit 45.
In many oil and gas well installations and similar wells used for the production or injection of fluids with respect to a subterranean earth formation, other wells are in proximity to the well in question. For example, in offshore oil and gas well platforms several wells are drilled from a relatively small space such as the deck of the platform and the wellheads are located relatively close to each other. In other well installations including those on land, wells are sufficiently close together to enable one to practice the method of the present invention.
FIG. 1 also illustrates a second well 50 which may be a fluid production or injection well and includes a conventional casing 51 and wellhead 52. A tubing string 54 extends within the casing 51 and may terminate in a suitable landing nipple 56 in which a conventional closure plug 58 may be retrievably disposed, as illustrated. Accordingly, the tubing string 54 provides a suitable space 55 for the containment of pressure fluid for use in accordance with the method of the present invention.
In the diagram of FIG. 1, the wells 10 and 50 are in communication with each other by way of a suitable high-pressure conduit 60 interconnecting the wellheads 15 and 52 in such a way that the interior of the tubing string 16 is in communication with the interior of the tubing string 54 as defined by the space 55. A suitable shutoff valve 63 may be interposed in the conduit 60 and is normally open during operation of the method described herein. The well 50 also includes a suitable annulus 62 defined by the casing 51 and the tubing string 54 and delimited by a conventional packer 64, for example. The space 62 may be filled with pressure fluid by way of a conduit 66 in communication with the annulus through the wellhead 52. Pressure gas may be introduced into the interior 55 of the tubing string 54, the space 17 and the conduit 60 by way of a compressor 70 in communication with the wellhead 52, for example. The compressor 70 may also be connected directly to the conduit 60 or the wellhead 15 for pressurizing the space 55, the conduit 60 and the interior space 17 of the conduit 16. Liquid may be introduced into the interior of the conduit 54 by way of a pump 72 operable to be in communication with the wellhead 52 so as to reduce the amount of space in the interior of the tubing string 54 occupied by gas as a method of compressing the gas in the space 55, the conduit 60 and the space 17 to a predetermined pressure. FIG. 1 shows a quantity of liquid 74 disposed in the lower portion of the tubing string 54 as indicated.
Although only one "accumulator" well 50 is illustrated connected to the well 10 by way of a pressure fluid flow conduit 60, those skilled in the art will recognize that several accumulator wells such as the well 50 may be placed in flow communication with the tubing string 16 in accordance with the method of the invention. The well 50 may be a well which is temporarily taken out of fluid production by placing the plug 58 at the lower end of the tubing string 54 or, if the tubing string 54 is not capable of standing the predetermined pressure desired to be built up therein, it may be replaced by a so-called workstring or a tubing string having suitably strong conduit to withstand the fluid pressures exerted thereon. Alternatively, or in addition to providing a tubing string of suitable pressure rating, the annular space 62 may be filled with liquid and pressurized to a predetermined pressure to reduce the differential pressure acting on the tubing string 54. In like manner, the annulus 22 of the well 10 may also be filled with pressure fluid to reduce the pressure differential acting on the tubing string 16 when it is pressurized in accordance with the invention.
As mentioned previously, the perforations 32 may already exist when it is desired to initiate or extend a fracture in the formation zone 13. In this regard, the perforating gun 28 and electric line 30 would not be disposed in the well 10, but fluid pressure may be built up in the space 17 by placing a frangible member in the landing nipple 34 such as illustrated in FIG. 2. In FIG. 2, a so-called shear disk assembly 80 is shown disposed in the landing nipple 34 using a conventional locking mechanism known to those skilled in the art and including movable locking key members 82. The shear disk assembly 80 includes a frangible closure member or shear disk 84 disposed in a tubular support member 86 and retained therein by suitable shear keys or pins 88. At a predetermined pressure acting on the shear disk 84 within the space 17, the pins 88 will fail and the disk 84 will be displaced to the alternate position shown to allow fluid to flow out of the member 86 through suitable ports 87.
In preparation for a fracturing operation to be carried out by the method of the invention, suitable fracturing liquid may be introduced into the space 20 and the tubing string 16 up to the predetermined level 40 so that a sufficient quantity of fluid is available to initiate and/or extend the fracture into the zone 13 a desired amount. With the wells 10 and 50 in communication with each other as illustrated, and the plug 58 disposed in the tubing string 54, pressure gas may be introduced into the spaces 55 and 17 by way of the compressor 70 or, if sufficient volume is available in the tubing strings 16 and 54, gas at ambient surface pressure may be allowed to flow into the spaces 55 and 17. Thereafter, the pressure of the gas in the spaces 55 and 17 may be built up by introducing liquid into the tubing string 54 by way of the pump 72 to compress the gas up to a predetermined pressure as measured by a suitable pressure gauge 61. The closure valves shown in FIG. 1 are, of course, placed in their appropriate operative positions to enable the method described herein to be executed.
Once the pressure in the conduits 16 and 54 has been raised to a predetermined value, the perforating gun 44 may be activated to form the perforations 32 in the casing 14. The liquid, under substantial gas drive pressure present in the conduits 54 and 16 will then be driven forcibly into the formation zone 13 to provide a suitable fracture extending either radially or having the desired radius of curvature as discussed in U.S. Pat. No. 5,074,359 to Joseph H. Schmidt and assigned to the assignee of the present invention.
Alternatively, if the perforations 32 are already formed, the shear disk assembly 80 may be disposed in the landing nipple 34 with, of course, the perforating gun 28 and electric line 30 removed from the tubing string 16 and the wellbore space 20. A suitable quantity of fracture fluid is disposed in the tubing string 16 and in the space 20 before placement of the shear disk assembly 80 in the landing nipple 34. Gas pressure is then built up in the tubing string 16 and the tubing string 54 in a manner generally as described above until the pressure exceeds that which will cause the shear disk 84 to be displaced to the alternate position shown in FIG. 2 to allow fracture fluid to flow through the ports 87 into the space 20 and into the formation zone of interest 13.
Accordingly, by placing a well such as the well 50 in communication with the tubing string 16 and by building up gas pressure in the tubing string 54 and the tubing string 16, a substantial "gas accumulator" effect is provided by the well 50 so that a sufficient volume of fracturing fluid is propelled into the formation zone of interest 13 to provide a suitable fracture. In this way, not only is a fracture formed and extended without substantial fluid pressure losses, which would be incurred in conventional fracturing operations where the fracture fluid is pumped from the surface through the entire length of the tubing string 16, but a substantial amount of gas accumulator volume is provided by the tubing string 54. Moreover, the tubing string 54 is disposed substantially below the earth's surface, is protected by a casing such as the casing 51 and the pressure differential across the tubing string 54 may be minimized by predisposing pressure fluid in the annulus 62.
Those skilled in the art will appreciate that substantially all of the casing 51 may be disposed below the earth's surface or extending below the water surface if the well is in a marine environment. The well 50 provides a readily available accumulator without requiring the use of pressure vessels having the strength to withstand high fluid pressures and placed in proximity to and in communication with the tubing string 16. In this way the hazards associated with high-pressure gas operations are minimized by using the gas accumulator space of an existing well and a tubing string disposed therein of suitable strength.
Although preferred embodiments of the invention have been described in detail herein, those skilled in the art will recognize that various substitutions and modifications may be made to the methods described without departing from the scope and spirit of the invention as defined by the appended claims.
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Hydraulic fractures are initiated or extended into earth formations from a first well by filling a space within the wellbore and a tubing string extending within the well with a fracturing fluid, placing the first well in fluid flow communication with a tubing string extending within a second well and increasing the pressure of fluid in the respective tubing strings sufficient to initiate or extend the fracture. The second well serves as an accumulator for accumulating a sufficient charge of pressure fluid, such as gas, to drive the fracturing fluid in the first well into the formation to a suitable extent.
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BACKGROUND OF THE INVENTION
1. Technical Field
The present invention relates to a method and apparatus for dispensing powder or other particulate matter and, more particularly, to dispensing powders in a gaseous stream.
2. Discussion of the Prior Art
It is well known to dispense powder and other particulate matter via a gaseous stream. Examples of methods and apparatus for effecting such dispensing may be found in U.S. Pat. Nos.: 1,551,877 (Henning); 2,792,151 (Wagner); 2,802,302 (Yost); 2,961,129 (Bullock); 3,304,647 (Szekely); 3,174,251 (West); and 4,033,511 (Chamberlin).
Prior art dispensers of particulate matter are generally bulky and unwieldy and involve complex mechanisms to effect dispersal of the particulate matter in the gaseous stream. In addition, the particulate matter is generally required to pass through stream producing fan blades, hopper mechanisms or mixing blades which tend to clog as the particulate matter agglomerates thereon. Usually, there is no attempt to control the rate at which the particulate matter is entrained in the gaseous stream; however, where such attempts exist, they usually employ failure-prone and annoying agitating or vibrating mechanisms, or mechanical members which tend to clog. Because of these problems, none of the prior art devices of which I am aware are suitable for use in dispensing particulate matter, such as insecticide powder, in homes, offices and other commercial and industrual establishments.
OBJECTS AND SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a method and apparatus for dispensing particulate matter via a gaseous stream where the rate of entrainment of the particulate matter into the stream is easily controllable without the need for complex mechanisms or mechanisms which tend to clog and fail due to agglomeration of the particulate matter.
It is another object of the present invention to provide a simplified method and apparatus for dispensing powder and other particulate matter via an air stream.
In accordance with the present invention powder to be dispensed is placed in an amorphous bag or pouch which can be easily manipulated to re-orient the powder therein. A gas inlet at one end of the pouch is adapted to receive a pressurized gaseous stream from an air blower, or the like. A gas outlet at the opposite end of the pouch directs the gas stream out of the pouch, preferably to an elongated delivery tube. By squeezing and manipulating the pouch and the powder therein, the amount of powder entrained in the gas stream within the pouch can be controlled. Structure is provided to support the pouch outlet downstream of the inlet in order to establish a direct, rather than a tortuous, path for the gas through the pouch.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects, features and many of the attendant advantages of the present invention will be better understood upon a reading of the following detailed description when considered in connection with the accompanying drawings wherein like parts in each of the several figures are identified by the same references numerals, and wherein:
FIG. 1 is a side view in elevation of a preferred embodiment of the present invention;
FIG. 2 is a detailed view, partially broken away, of the interior of the pouch employed as part of the preferred embodiment, the pouch being shown in a relaxed state;
FIG. 3 is a view similar to that of FIG. 2 but showing the pouch in a manipulated state;
FIG. 4 is a view similar to FIG. 1 of a further embodiment of the present invention;
FIG. 5 is an end view in elevation taken along lines 5--5 of FIG. 1 and showing the air intake opening closed; and
FIG. 6 is a view similar to FIG. 5 but showing the air intake opening open.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring specifically to FIG. 1 of the accompanying drawings, an air blower assembly 10 serves as a source of pressurized gas for issuing a gaseous stream into a pouch or bag 11. In this embodiment, the air blower 10 is the motor and fan portion of a commercially available electric broom; however, any assembly for providing a stream of air or any other gas may be employed. The air blower assembly includes an air intake opening 12 and an air output port in the form of a short rigid cylindrical tube 13. Handle 15 of assembly 10 has a trigger switch 17 for selectively actuating the internal motor and fan using convenience a.c. electrical power delivered via power cord 19.
Pouch 11 is an amorphous sack-like member having a soft flexible cylindrical extention serving as an inlet opening 20 and adapted to fit over tube 13. Hose clamps 21, 23 radially compress the pouch inlet 20 about air blower output tube 13. The pouch 11 is preferably made of leather, although any suitably manipulable material may be employed. Importantly, the pouch must be sufficiently soft and manipulable to permit it to be squeezed, compressed and shaken to reorient its powdered contents. An outlet opening 25, in the form of a soft flexible cylindrical extension of the pouch, is disposed at an opposite end of the pouch from inlet opening 20. Outlet opening 25 is disposed about an elongated discharge tube 27 extending outwardly from the pouch. Outlet opening 25 is secured about the discharge 27 in sealing relation by means of a hose clamp 29 and adapter 30. The hose clamp 29 radially compresses the outlet 25 about the adapter 30 which is of larger diameter than the discharge tube 27. The adapter serves to reduce the outflow path diameter to accomodate the smaller discharge tube.
A support rod 31 extends from air blower assembly 10 in a generally downstream direction and is secured at its distal end to the outlet opening extension 25 of the pouch by means of a clamp, or the like. The support rod serves to maintain a physical separation between the inlet 20 and outlet 25 of the amorphous pouch so that the gas flow through the pouch is along a generally direct downstream path rather than through a tortious path. For reasons to be described below, the inlet opening 20 of pouch 11 is disposed somewhat below the level of the outlet opening 25 when the discharge tube 27 is oriented horizontally.
The embodiment illustrated in FIG. 1 is intended for dispensing insecticide powder so that, in use, the discharge tube 27 and the flow path through pouch 11 are oriented downwardly from horizontal, normally at a declination in the range of 30° to 75°. When the unit is so oriented, powder in pouch 11 tends to collect at the forward or downstream end of the pouch, leaving an unblocked flow path between inlet opening and outlet opening 25 for the stream of gas delivered by air blower assembly 10. With the pouch relaxed (i.e., not manipulated by the user, as illustrated in FIG. 2), the stream passing through the pouch tends to entrain a small amount of contained powder or particulate matter which is issued through the discharge tube 27. Greater amounts of the particulate matter can be dispensed into the discharge tube by appropriately manipulating, squeezing, shaking, etc. the pouch 11 in the manner illustrated in FIG. 3.
For intended use with the flow path and discharge tube oriented horizontally, the inlet and outlet opening can be appropriately aligned in the manner illustrated in the embodiment of FIG. 4. In fact, any appropriate alignment of the inlet and outlet openings of the pouch may be provided to accomodate the orientation of the unit in use.
The air intake opening 12 of air blower assembly 10 may be provided with a slidable cover to permit selective adjustment of the air flow through pouch 11. Such an arrangement is illustrated in FIGS. 5 and 6 of the accompanying drawings to which specific reference is now made. The air blower assembly includes an end panel 41 having large opening 42, 43 defined therein for admitting air into the blower assembly. An elongated slot 44 is also defined in end panel 41 at a location intermediate openings 42 and 43. A cover 45 is slidably mounted on the end of the air blower assembly in front of end panel 41. A bolt 46 has its head disposed on the side of panel 41 opposite cover 45 and projects through slot 44 and a suitably provided hole in cover 45. A wing-nut 47 engages the outwardly projecting opposite end of bolt 46. Cover 45 can be slid from one position to another along panel 41 and the dimension of slot 44 to selectively cover and uncover more or less of openings 42, 43. In any position, wing-nut 47 may be tightened to hold cover 45 in place.
The essence of the invention is the use of a manipulable pouch to control the orientation of particulate matter therein so that the particulate matter can be controllably dispensed into a stream of gas flowing through the pouch. The dispensing mechanism thereby eliminates mechanical parts which tend to clog and fail. The device is simple to use and inexpensive to fabricate.
Having described several embodiments of a new and improved dispenser for particulate matter constructed in accordance with the present invention, it is believed that other modifications, variations and changes will be suggested to those skilled in the art in view of the disclosure set forth hereinabove. It is therefore to be understood that all such variations, modifications and changes are believed to fall within the scope of the present invention as defined in the appended claims.
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Dispensing of particulate matter such as powder via a gaseous stream is facilitated by placing the powder in an amorphous, manipulable pouch through which the gaseous stream flows. Squeezing and manipulating the pouch results in manipulation of the contained powder to control the amount of powder entrained in the gas stream. The pouch is supported with its outlet opening disposed generally downstream of its inlet opening in order to provide a direct, rather than a tortious, flow path through the pouch.
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FIELD OF THE INVENTION
[0001] The present invention relates to a method for adjusting the clamping force exerted by a parking brake in a vehicle.
BACKGROUND INFORMATION
[0002] Parking brakes in vehicles, with which a vehicle can be continuously immobilized at a standstill by generating a constant clamping force, are known. Parking brakes can encompass an electric brake motor whose positioning motion acts via a linkage, for example a spindle drive, directly on the brake pistons at the hydraulic wheel brakes. The electric brake motor is dimensioned so that up to a specific slope angle, the vehicle can be held exclusively via the braking effect of the brake motor. For slope angles beyond that, an additional, hydraulic braking force is generated by actuating the hydraulic wheel brake device.
SUMMARY OF THE INVENTION
[0003] An underlying object of the invention is to make the application or clamping force in the parking brake of a vehicle available in economical fashion, and at the same time to decrease the stress on the parking brake.
[0004] This object may be achieved according to the present invention with the features described herein. The further descriptions herein indicate useful refinements.
[0005] The method according to the present invention serves to adjust the clamping force exerted by a parking brake when a vehicle is at a standstill. The parking brake encompasses an electric-motor braking apparatus having an electric brake motor, and furthermore a hydraulic braking apparatus with which a hydraulic clamping force can be generated. The hydraulic braking apparatus is, advantageously, identical to the hydraulic wheel brake with which the vehicle is decelerated in normal driving operation. The electric brake motor acts on the brake piston of the hydraulic braking apparatus. An adjustable portion of the total clamping force can be generated respectively via the electric and the hydraulic braking apparatus, the respective portion being modifiably adjustable between zero and a maximum value.
[0006] In the method according to the present invention, the hydraulic inlet pressure generated by a driver actuation and existing in the hydraulic braking apparatus is utilized, at least within a defined operating range, to generate a hydraulic clamping force. For the case in which the hydraulic clamping force is not sufficient to reach a predefined target clamping force, a clamping force produced in the electric-motor braking apparatus is generated in supplementary fashion. The inlet pressure is generated by a manual intervention by the driver in the hydraulic braking apparatus. If the hydraulic braking apparatus that is a constituent of the parking brake is identical to the hydraulic wheel brake, the driver intervention is the brake pedal actuation by which a hydraulic braking force is generated by the driver, which force can be utilized as an inlet pressure for generating a clamping force in the parking brake.
[0007] The hydraulic clamping force and the electric clamping force supplement one another additively to yield the target clamping force that is to be established by the parking brake. This on the one hand ensures that the necessary clamping force is achieved, and on the other hand the stress on the components of the parking brake is decreased, since (at least in specific, defined operating situations) no force exceeding the target clamping force is generated in the electrical or hydraulic braking apparatus. The forces acting on the brake piston are decreased as compared with the existing art.
[0008] To ensure that the hydraulic clamping force is continuously active while the vehicle is at a standstill, the electric brake motor is usefully shifted into a position that immobilizes a brake piston of the hydraulic braking apparatus. This applies both for the case in which the clamping force is achieved exclusively via the hydraulic inlet pressure, and also in cases in which the clamping force is generated via a portion from the hydraulic inlet pressure and also via a portion from the electric brake motor. The effect of the hydraulic pressure can thereby be conserved.
[0009] If applicable, a hydraulic clamping force exceeding the clamping force that can be made available only on the basis of the hydraulic inlet pressure is generated by a driver-independent actuation of the hydraulic braking apparatus. This occurs in particular in phases in which the necessary target clamping force cannot be achieved solely from the sum of the electric clamping force and the hydraulic clamping force attributable to the inlet pressure, for example with steep slope angles. In standard cases, on the other hand, in which the slope angle does not exceed a defined magnitude of, for example, 20%, a constant target clamping force associated with that slope angle is defined, which force is made available solely from the sum of the electric clamping force and the clamping force attributable to the hydraulic inlet pressure, the electric clamping force portion being adjusted variably or complementarily to the hydraulic clamping force portion.
[0010] According to a further useful embodiment, for the case in which the hydraulic inlet pressure is below a first threshold pressure value, the target clamping force is made available entirely via the electric clamping force. What is available in the electric braking apparatus is, in particular, a nominal clamping force that is matched to a specific slope angle of, for example, 20%. The first threshold pressure value is equal to, for example, 65 bar. If the inlet pressure does not exceed the first threshold pressure value, the electric braking apparatus generates the nominal clamping force regardless of the hydraulic clamping force attributable to the inlet pressure, which force combines additively with the electric clamping force to yield the total clamping force.
[0011] According to a further useful embodiment, the target clamping force is generated via the hydraulic clamping force, and in supplementary fashion via the electric-motor clamping force, if the hydraulic inlet pressure is between a first threshold pressure value and a second, higher threshold pressure value. The first threshold pressure value is equal to, for example 65 bar; the second threshold pressure value is at, for example, 140 bar. The electric-motor portion of the clamping force participates in supplementary fashion, the level of the electric clamping force being dimensioned so that a required target clamping force is achieved, which force is, as described above, usefully adjusted so that the vehicle can be securely held in place at a standstill on a defined slope angle.
[0012] According to yet another useful embodiment, for the case in which the hydraulic inlet pressure exceeds a threshold pressure value, the electric-motor clamping force portion of the target clamping force is reduced by a constant amount. The relevant threshold pressure value is, in particular, identical to the second, upper threshold pressure value, which marks the upper limit of the range in which the electric and the hydraulic clamping forces supplement one another, each at a variable proportion, to yield the target clamping force. The fact that in working ranges above the second threshold pressure value, the portion from the electric-motor clamping force is now reduced not by an amount equal to a variable constituent of the hydraulic inlet pressure, but instead only by a constant amount, ensures that for safety reasons, a minimum electric clamping force is made available even with very high hydraulic inlet pressures. This ensures secure bracing of the brake piston via the electric brake motor and the spindle. The constant amount by which the portion to be supplied by the electric brake motor is reduced usefully corresponds to the hydraulic clamping force that is present at the upper threshold pressure value.
[0013] To ascertain the hydraulic inlet pressure, a pressure measurement in the hydraulic braking system of the vehicle is usefully carried out. It can be advantageous to ascertain the inlet pressure, at a hydraulic wheel brake constituting the parking brake, from the inlet pressure of a further wheel brake, in particular by subtracting a pressure tolerance of, for example, 50%. As a rule, the current inlet pressure at the wheel brakes on the front axle of the vehicle is ascertainable via a pressure sensor. If this value is available, the inlet pressure at the wheel brakes on the rear axle of the vehicle, which constitute the parking brake, can be estimated therefrom, optionally in consideration of the pressure tolerance.
[0014] The method according to the present invention executes in a closed- or open-loop control device that is a constituent of the parking brake in the vehicle or communicates with the parking brake or with components of the parking brake. The closed- or open-loop control device is optionally a constituent of an electronic stability program (ESP) control device, or constitutes an additional function in an ESP control device, or is made available as an independent control device that can communicate with the ESP control device.
[0015] Further advantages and useful embodiments may be gathered from the further descriptions herein, the description of the Figures.
BRIEF DESCRIPTION OF THE DRAWING
[0016] The FIGURE shows an execution diagram for carrying out the method for adjusting the clamping force exerted by a parking brake.
DETAILED DESCRIPTION
[0017] The execution diagram depicted in the FIGURE refers to a parking brake in a vehicle, which brake encompasses both an electric-motor braking apparatus and a hydraulic braking apparatus, such that a respective clamping force portion for achieving a target clamping force F N,target can be established via the electric-motor and the hydraulic braking apparatus. The electric-motor braking apparatus encompasses an electric brake motor that exerts a positioning force on the brake piston of the hydraulic braking apparatus, the hydraulic braking apparatus being a constituent of the hydraulic wheel brake in the vehicle by which the vehicle can be decelerated in ordinary driving operation.
[0018] In a first method step 1 , firstly a locking request to the parking brake is identified. In the next method step 2 , the hydraulic inlet pressure p h,inlet in the hydraulic braking apparatus, which is a constituent of the parking brake, is ascertained. The hydraulic inlet pressure is the hydraulic pressure generated in the braking apparatus as a result of actuation of the brake pedal by the driver. The hydraulic inlet pressure p h,RA at the wheel brakes on the rear axle of the vehicle (which constitute the parking brake) is ascertained from the hydraulic inlet pressure p h,inlet of the braking system, which is measured with the aid of a pressure sensor. Because the hydraulic pressure at the rear axis can deviate from that at the front axle, for example because of an intervention by an electronic brake differential, a safety deduction for the hydraulic inlet pressure at the rear axle is carried out, equal e.g. to 50%; in this case the hydraulic inlet pressure at the rear axle is equal to only 50% of the hydraulic inlet pressure at the front axle.
[0019] In method step 3 , a query occurs as to whether the hydraulic inlet pressure p h,inlet falls below a lower, first threshold pressure value p h,65 . If this is the case, i.e. if the hydraulic inlet pressure is less than the lower threshold pressure value p h,65 , execution continues along the Yes branch (Y) to the next method steps 4 and 4 a, which constitute a first execution block I in which the target clamping force F N,target is made available entirely via the electric clamping force F N,el of the electric brake motor. Any hydraulic clamping force F N,h that may exist, attributable to the hydraulic inlet pressure p n,inlet , combines additively with the electric clamping force F N,el to yield a total clamping force F N . The electric braking apparatus nevertheless makes available a nominal clamping force that is directed toward a slope angle having a defined slope of, for example, 20°. In method step 4 the electric clamping force F N,el is accordingly set to the nominal value, and in method step 4 a the clamping force is implemented by corresponding application of control to the electric brake motor.
[0020] If the result of the query in method step 3 is that the hydraulic inlet pressure p h,inlet is not less than the lower threshold pressure value p h,65 , execution continues along the No branch (N) to the second execution block having method steps 5 to 7 . Execution block II requires, as additional information, the magnitude of a hydraulic portion F adapt , which is ascertained in an execution block III that is run through in parallel after method step 2 and contains method steps 8 to 10 . In accordance with the query in method step 8 , execution block III firstly queries whether the hydraulic inlet pressure P h,inlet is below a lower threshold p h,15 . If so, execution continues along the Yes branch to method step 9 ; otherwise to method step 10 . In method step 9 , the hydraulic portion F adapt is set to a value of zero; in method step 10 , the hydraulic portion F adapt is ascertained as a function of the inlet pressure p h,inlet , but with subtraction of the pressure at the lower threshold, which is e.g. 15 bar.
[0021] The hydraulic portion F adapt ascertained in execution block III flows as additional information into execution block II. There, in a method step 5 , a query is started as to whether the hydraulic portion F adapt (present as a force) is within a value range between zero and an upper limit F lim,8.5 which marks the value exerted by the hydraulic braking apparatus of the parking brake upon reaching an upper threshold value p h,140 . If the query in method step 5 is answered positively, i.e. if the hydraulic portion F adapt is within the range marked by the upper limit F lim,8.5 , execution continues along the Yes branch to method step 6 , in which the clamping force F N,el to be effected by the electric brake motor is ascertained as the difference between the nominal clamping force and the hydraulic portion F adapt . In the next method step 7 , the total clamping force is then established by acting on the electric brake motor with the electric clamping force F N,el ascertained in method step 6 , in which context the hydraulic clamping force F N,h attributable to the current inlet pressure p h,inlet in the hydraulic braking system is additionally effective. Method steps 5 to 7 in execution block II thus adapt the electric portion of the clamping force variably to the existing portion of the hydraulic clamping force so as to achieve the target clamping force F N,target . The target clamping force F N,target target is set, in particular, to a value such that the vehicle remains securely at a standstill at a defined slope angle of, for example, 20%.
[0022] If the result of the query in method step 5 is that the hydraulic portion F adapt exceeds the upper limit F lim,8.5 , there is also an exceedance of the upper threshold pressure value p h,140 of the hydraulic inlet pressure p h,inlet . In this case execution continues along the No branch to method step 11 , which together with a further method step 12 constitutes an execution block IV. In method step 11 , the electric clamping force F N,el is limited to a maximum value that is obtained by subtracting the upper limit F lim,8.5 from the nominal clamping force in the context of a defined slope angle of, for example, 20%. In the next method step 12 the total clamping force is then established; this results from the electric-motor portion and the hydraulic portion, the electric-motor portion being established in the electric brake motor as ascertained in method step 11 , and the hydraulic portion being based on the current inlet pressure that is above the upper threshold pressure value p h,140 .
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In a method for adjusting the clamping force exerted by a parking brake, which force is applied by an electric-motor braking apparatus and by a hydraulic braking apparatus, the hydraulic inlet pressure generated by the driver and existing in the hydraulic braking apparatus is utilized to generate a hydraulic clamping force; and for the case in which the hydraulic clamping force is not sufficient to reach a target clamping force, an electric clamping force is generated in supplementary fashion.
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[0001] The present application is a continuation-in-part of application Ser. No. 09/915,069 filed Jul. 25, 2001.
FIELD OF THE INVENTION
[0002] The present invention relates to a connector and more particularly, relates to a connector for use in a flooring system.
BACKGROUND OF THE INVENTION
[0003] There are many different types of flooring which are used both in residential and commercial applications. Flooring systems range from hardwood floors to various composite wood products, tiles, linoleum, slate, carpets, etc. Each of the aforementioned types of flooring has various advantages and disadvantages, with some of the parameters for suitability for any particular installation being cost of the flooring material, cost of installation, durability, appearance, ease of maintenance, etc.
[0004] For a residential and many commercial installations, the use of wood and notably a hardwood is considered desirable particularly from an aesthetic viewpoint. Historically, some of the drawbacks associated with hardwood flooring have been the cost of installation and maintenance. Typically, hardwood flooring comes in slats of solid wood which must be secured to a substrate. In most instances, the wood slats have a tongue and groove arrangement formed on their side walls and the slats are secured by toenailing a nail through the tongue portion. Although there are a number of automatic nailing guns which are suitable for performing this operation, thus speeding up the installation, it is still a time consuming operation. Still further, many of the woods used in the flooring have a tendency to split when the nail is driven. In order to prevent this splitting, it then becomes necessary to pre-drill a pilot hole for the nail. This is again very time consuming and thus increases the expense of installation.
[0005] Still further, wood floors, in high traffic areas, are subject to a wear factor. After a certain period of time, it becomes necessary to refinish the floors which typically comprises an operation to remove the old surface coating by means of a sander and subsequently refinishing the floors. This operation is one which requires some skill on the part of the operator of the sander in order to maintain a level and smooth surface. It is also an extremely messy and possibly health threatening operation as fine particles of dust spread throughout the area. Before applying the coating to the wood, all dust particles must be removed; this is often a tedious process.
SUMMARY OF THE INVENTION
[0006] It is an object of the present invention to provide a flooring system for installing a plurality of elongated slats, the system being one wherein installation is substantially faster than the use of nails.
[0007] It is a further object of the present invention to provide a system for the installation of wood slats having a tongue and groove configuration.
[0008] It is a further object of the present invention to provide a connector suitable for use in installing elongated slats having a tongue and groove arrangement.
[0009] It is a still further object of the present invention to provide a method for installing elongated hardwood slats to form a floor.
[0010] According to one aspect of the present invention, there is provided a floor comprising a plurality of elongated slats, each slat having a top wall, a bottom wall, and first and second opposed side walls, the slats being laid in a side by side relationship with a first side wall of a first slat abutting a second side wall of a second slat, a groove formed in each of the first side walls, a side wall recessed portion formed in one of the first and second side walls below the groove, a bottom recess formed in each of the bottom walls of each of the slats adjacent the second side wall, a plurality of connectors, each connector comprising a base secured to a substrate, a vertical portion extending upwardly from the base and fitting within the side wall recessed portion, and a generally horizontal portion extending into the groove formed in the first side wall to thereby secure the slat in position.
[0011] According to one aspect of the present invention, there is provided a flooring system for installing a floor of individual boards, each board comprising an elongated slat having a top wall, a bottom wall, and first and second opposed side walls, a groove formed in the first side wall, a first recessed portion formed in the first side wall below the groove and extending to the bottom wall, a tongue formed on the second side wall, the tongue being sized and shaped to fit within the groove formed in the first side wall, a second recess formed in the second side wall, the second recess being located below the tongue and above the bottom wall, and a plurality of connectors, each connector having a main body portion sized to fit within the first recessed portion formed in the first side wall, and a lip extending outwardly from the body portion, the lip being sized to engage the recess formed in the second side wall.
[0012] According to a further aspect of the present invention, there is provided a floor comprised of a plurality of elongated slats, each slat having a top wall, a bottom wall, and first and second opposed side walls, the slats being laid in a side by side relationship with a first side wall of first slat abutting a second side wall of a second slat, a groove formed in each of the first side walls, a first recessed portion formed in each of the bottom walls so each of the slats adjacent the first side wall, a tongue formed on each of the second side walls, a second recessed portion formed in each of the second side walls below the tongue portion, and a plurality of discrete connectors, each connector comprising a body portion and a lip extending from the body portion, the body portion fitting within the first recess below the groove in the first side walls, and the lip portion engaging the second recessed portion in the second side walls, each of the connectors being secured to a substrate.
[0013] According to a further aspect of the present invention, there is provided a method of installing a wood floor comprising a plurality of elongated slats, each slat having a top wall, a bottom wall and first and second opposed side walls, a groove formed in each of the first side walls of each of the slats, a side wall recessed portion formed in one of the first and second side walls of each of the slats below the groove, a bottom recess formed in each of the bottom walls of each of the slats adjacent a respective second side wall, a method comprising the steps of supplying a plurality of connectors, a vertical portion extending upwardly from the base and a generally horizontal portion, a method comprising the steps of securing a connector to a substrate, placing a slat on the substrate with the horizontal portion extending into the groove formed in the first side wall to thereby secure the slat in position, and continuing to place subsequent slats in a side by side abutting relationship with a connector holding each slat in position.
[0014] The connector used in the present invention has a first portion thereof which is adapted to be secured to the substrate. Typically, the substrate is of a wood material such as a plywood or composite wood material. Typically, the connector may be secured to the substrate by mechanical means such as nails or screws. Screws are a preferred securing mechanism for reasons which will become apparent hereinbelow. However, it will be understood that other securement means such as adhesive or the like may be utilized particularly in the instance wherein the substrate is not a material easily penetrable by screws.
[0015] The connector will include a upwardly extending vertical portion having at its upper end thereof at least one horizontally extending tab portion. The horizontally extending tab portion is designed to engage a slot or recess formed in a side wall of a slat. In one embodiment, the horizontally extending tab portion may engage the groove in a conventional tongue and groove type of flooring.
[0016] In a preferred embodiment, the upwardly extending vertical portion has at least a pair of horizontally extending tab portions, at least one tab portion extending outwardly in each horizontal direction such that a single connector will engage both of a pair of abutting slats.
[0017] The connector is designed to be used, as aforementioned, in a flooring system comprising a plurality of slats engaged in an abutting side by side relationship. To this end, the slats are formed with recessed portions to receive both the base portion of the connector and the vertical portion thereof.
[0018] The connector may be formed of any suitable material and thus is preferably either of a metal or plastic material. A formed metal material would be suitable while an extruded plastic material could also be utilized.
[0019] In one embodiment, the connector is formed of a metallic material and may easily be formed by a suitable mechanical means to have the desired configuration. In this configuration, the connector has a base which has means for securement to the substrate. Typically, such means may include apertures formed within the base which lies co-planer with the substrate and may be secured thereto by a mechanical means such as a screw or the like.
[0020] The connector also includes a vertical portion which extends upwardly adjacent to at least a portion of a side wall of abutting slats. To provide space for the upwardly extending wall, one of the side walls of the slats has a recess formed therein.
[0021] One or both of the side walls of each of the slats has a longitudinally extending groove formed therein. A corresponding tab extends outwardly from the upwardly extending wall of the connector and is designed to engage within the longitudinally extending slot and thereby retain the slat in position.
[0022] The bottom end side recesses are formed of a size sufficient to accommodate the connector. Typically, the bottom recess would have a width of between 6 mm and 50 mm and a depth of between 3 mm and 12 mm. Similarly, the side wall recessed portion would be sized to receive the vertical portion of the connector and accordingly would generally have a depth of between 3 mm and 12 mm.
[0023] In an alternative embodiment, the connector of the present invention may be arranged to be used in conjunction with a conventional tongue and groove flooring with the tab portion being arranged to engage the groove formed within the slat. Again, proper sizing of the tongue to permit the same would be provided.
[0024] As above described, the wood slats may have different configurations. In one embodiment, the side walls of the slats may also be formed such that one side wall will have a upper recessed portion designed to receive a projecting portion of an adjacent slat.
[0025] In a further embodiment of the invention, the connector is preferably formed of a plastic material and comprises a body portion having an aperture extending therethrough and a lip designed to engage the recess in the side wall of the slat.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] Having thus generally described the invention, reference will be made to the accompanying drawings illustrating an embodiment thereof, in which:
[0027] [0027]FIG. 1 is a perspective view of a connector according to one embodiment of the present invention, with the connector being shown in place with a slat in broken lines;
[0028] [0028]FIG. 2 is an end view of the connector;
[0029] [0029]FIG. 3 is a side elevational view thereof;
[0030] [0030]FIG. 4 is a top plan view thereof;
[0031] [0031]FIG. 5 is a side sectional view illustrating placement of the connector in conjunction with a pair of slats;
[0032] [0032]FIG. 6 is a side view, partially in section, of a conventional tongue and groove flooring system utilizing a connector according to the present invention;
[0033] [0033]FIG. 7 is a view similar to FIG. 5 showing a modified form of a slat which may be used in the present invention;
[0034] [0034]FIG. 8 is an end elevational view of a slat according to a further embodiment of the present invention;
[0035] [0035]FIG. 9 is a side elevational view of a connector according to this embodiment of the present invention;
[0036] [0036]FIG. 10 is an end elevational view, partially in section, illustrating the joining together of two slats; and
[0037] [0037]FIG. 11 is a perspective view of a flooring system according to the embodiment of FIGS. 8 to 10 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0038] Referring to the drawings in greater detail and by reference characters thereto, and referring initially to FIG. 5, there are illustrated a first slat 10 and a second slat 12 lying in an abutting relationship. A connector generally designated by reference numeral 14 (FIG. 1) is used to secure slats 10 and 12 in position.
[0039] First slat 10 has an upper wall 18 , a bottom wall 20 , a first side wall 22 , and a second side wall 24 .
[0040] Second slat 12 is placed in an abutting relationship to first slat 10 . Second slat 12 includes an upper wall 28 which will be co-planer with upper wall 18 of first slat 10 ; a first side wall 32 which lies in an abutting relationship with second side wall 24 of first slat 10 ; a bottom wall 30 which is also substantially co-planer with bottom wall 20 of first slat 10 ; and a second side wall 34 .
[0041] As may be seen in FIG. 5, slat 10 has a long first side wall 22 in which there is a longitudinally extending slot which is generally designated by reference numeral 38 . Similarly, along second side wall 24 , there is provided an inwardly directed longitudinally extending slot 40 .
[0042] There is also provided a bottom wall recess generally designated by reference numeral 42 and which is provided within bottom wall 20 and extends to first side wall 22 . A conventional groove 44 within bottom wall 20 is provided intermediate first side wall 22 and second side wall 24 in a conventional fashion to provide dimensional stability to slat 10 .
[0043] A side wall recess 46 is provided within second side wall 24 and is located at the point of juncture of second side wall 24 and bottom wall 20 .
[0044] Slat 12 has a similar configuration to slat 10 —i.e. slat 12 includes a first longitudinally extending slot 50 within first side wall 32 and a second longitudinally extending slot 52 within second side wall 34 . A bottom wall recess 54 is provided adjacent first side wall 32 while a side wall recess 58 is provided in second side wall 34 . A centrally located longitudinally extending groove 56 is also formed in bottom wall 30 .
[0045] As may be best seen in FIGS. 1 to 4 , connector 14 has a base portion 64 which is adapted to lie flat on a substrate to which it is to be secured. To this end, an aperture 66 is provided within base portion 64 .
[0046] Extending upwardly from base portion 64 is a vertical wall 68 . At the distal end of vertical wall 68 , there is provided a first tab member 70 which is substantially perpendicular with respect to vertical wall 68 . A pair of tabs 72 are formed on either side of first tab 70 , tabs 72 lie in the same horizontal plane as tab 70 but extend in an opposite direction.
[0047] In use, and as may be seen in FIG. 5, a connector is secured by means of a screw 76 to a substrate through aperture 66 of base 64 . Vertical wall 68 fits within side wall recess 46 of slat 10 . Tab 70 then is designed and sized to fit within longitudinally extending slot 40 while tabs 72 fit within slot 50 formed in side wall 32 of slat 12 . Connector 14 thus functions to stabilize and maintain slats 10 and 12 in position.
[0048] When installing a floor comprised of a plurality of longitudinally extending slats such as 10 and 12 , a first slat 10 may be placed in position along a wall. In this respect, first side wall 22 of slat 10 could abut the wall and then a connector 14 secured as shown in FIG. 5. A second slat 12 would then be placed in position and the process repeated.
[0049] Alternatively, a first row of connectors 14 may be provided for initial slat 10 . The first row of connectors may utilize tab 72 as a spacer from an adjacent wall or alternatively, a special connector not having a tab 72 may be utilized.
[0050] Utilizing the above system, the only connection required is the attachment of connector 14 to the substrate by means of a member such as screw 76 . This could be accomplished rapidly using automated equipment for driving screws 76 .
[0051] The connectors 14 may be spaced apart by a suitable distance. Generally, the spacers may be provided at a distance of between 10 to 15 centimeters. Naturally, it will be understood that a continuous connector strip could be utilized. It will also be understood that the slats may comprise individual slats connected in an end to end arrangement with a connector being used where the ends abut each other.
[0052] In FIG. 7, a slightly modified version of the system shown in FIGS. 1 to 5 is illustrated. In this embodiment, there is provided a pair of slats 110 and 112 lying in a side by side abutting relationship. A connector generally designated by reference numeral 114 is employed between slats 110 , 112 and is secured to the substrate by means of screw 176 . Connector 114 is identical to that previously described.
[0053] In the embodiment of FIG. 7, slat 112 has a first side wall generally designated by reference numeral 132 and which includes an upper vertical portion 133 and a lower tapered portion 135 . A recess generally designated by reference numeral 158 and which is similar to recess 58 of the previous embodiment is formed in side wall 132 .
[0054] Side wall 134 includes a vertical section 137 and an outwardly tapered wall section 139 . A bottom recess 154 is provided to receive base 164 of connector 114 . In this arrangement, a thinner slat may be utilized.
[0055] Turning to FIG. 6, there are illustrated two slats 210 and 212 . Referring to slat 212 , this is formed in a substantially conventional manner in that there is provided a tongue 220 and a groove 230 on the opposite side wall. In this arrangement, a connector generally designated by reference 214 has a base portion 264 with apertures therein to permit the passage of screws 276 . A vertical portion 268 is also provided as well as a tab 270 .
[0056] In this arrangement, groove 230 is formed to have a sufficient height to accommodate both tongue 220 and the thickness of tab 270 . The side wall having groove 230 has the bottom portion thereof forming a recess to accommodate vertical portion 268 while a bottom recess 254 is provided to accommodate base 264 and the head of screw 276 .
[0057] Turning now to FIGS. 8 to 11 , there is illustrated a further embodiment of the present invention and to which reference will now be made.
[0058] In this embodiment, and as seen in FIG. 8, there are provided slats generally designated by reference numeral 310 . Slat 310 has a top wall 312 , a bottom wall 314 , a first side wall 316 , and a second side wall 318 .
[0059] First side wall 316 has a generally V-shaped groove 320 extending inwardly thereof. Located below groove 320 is a recess generally designated by reference numeral 322 and which is defined by an upper surface 324 and a vertical surface 326 .
[0060] Located on second side wall 318 is a tongue 328 which is sized and located to fit within the groove 320 of an adjacent slat. Situated below tongue 328 is a second side wall recess 330 .
[0061] A connector generally designated by reference numeral 334 includes a body portion 336 of a rectangular configuration and having an aperture 338 formed therein. Extending outwardly from one side is a lip 340 which is sized and positioned so as to fit within second side wall recess 330 . In this respect, body portion 336 is of a length and height to substantially fill recess 322 formed in first side wall 316 .
[0062] In use, and as shown in FIG. 11, connector 334 is secured to a substrate (not shown) by means of an attachment member such as a screw through aperture 338 . It will engage second side wall recess 330 formed within second side wall 318 and securely hold the member.
[0063] An advantage of using the above system is that the floor may be securely attached in a manner which permits removal of the same. Thus, in a typical residential application, the sub-flooring or substrate would be plywood or similar material. When it is desired to refinish the floor, it can be rapidly lifted and the individual slats forwarded to a commercial facility for refinishing. The floor, after refinishing, could then be reinstalled. For the average consumer, this would both be less time consuming and less expensive than performing the refinishing on site. The use of this system will also permit one to replace a floor and use the removed floor in another location.
[0064] It will be understood that the above described embodiments are for purposes of illustration only and that changes or modifications may be made thereto without departing from the spirit and scope of the invention.
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There is provided a flooring system for hardwood floors comprised of a plurality of elongated slats wherein the slats are held in position by a plurality of connectors, each connector having a base secured to a substrate, a vertical portion extending upwardly from the base, and a generally horizontal portion extending into a groove formed in a side wall of the elongated slat. The system permits the slats to be installed with a minimum of labor and also permits removal of the slats and their later re-use.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates generally to a vapor generator for use in vapor deposition equipment. In particular, the present invention relates to a vapor generator designed for the requirements of vapor phase epitaxy and other chemical vapor deposition equipment.
[0002] Group III-V compound semiconductor materials including different monocrystalline layers with varying compositions and with thickness ranging from fractions of a micron to a few microns are used in the production of many electronic and optoelectronic devices such as lasers and photodetectors. Chemical vapor deposition methods using organometallic compounds are typically employed in the chemical vapor deposition (“CVD”) art for the deposition of metal thin-films or semiconductor thin-films of Group III-V compounds. Compounds typically used as precursors in CVD for the semiconductor industry include cyclopentadienyl magnesium (“Cp 2 Mg”), trimethyl aluminum (“TMA”), trimethyl gallium (“TMG”), triethyl gallium (“TEG”), trimethyl antimony (“TMSb”), dimethyl hydrazine (“DMHy”), trimethyl indium (“TMI”) and the like. Solid precursors, such as TMI, are used in the metal-organic-vapor-phaseepitaxy (“MOVPE”) of indium containing semiconductors.
[0003] Typically, such solid precursors are placed in a cylindrical vessel or container referred to as a “bubbler” and subjected to a constant temperature wherein the solid precursor is vaporized. A carrier gas, such as hydrogen, is employed to pick up the precursor compound vapor and transport it to a deposition system. Most solid precursors exhibit poor and erratic delivery rates when used in conventional bubbler-type precursor vessels. Such conventional bubblers include both bubbler vessels having a dip-tube attached to the inlet, see for example U.S. Pat. No. 4,506,815 (Melas et al.), or the gas-feeding device as disclosed in U.S. Pat. No. 5,755,885, which has a plurality of gas-ejecting holes in the dip-tube to introduce the carrier gas into the container. Such conventional bubbler systems can result in a non-stable, non-uniform flow rate of the precursor vapors, especially when solid organometallic precursor compounds are used. Non-uniform flow rates produce an adverse affect on the compositions of the films, particularly semiconductor films, being grown in MOVPE reactors.
[0004] Other bubbler systems have been developed, such as that developed by Morton International, Inc., which eliminates the use of a dip-tube. However, while such dip-tube free bubblers were found to provide a uniform flow rate, they failed to provide a consistently high concentration of precursor material. The inability to achieve a stable supply of feed vapor from solid precursors at a consistently high concentration is problematic to the users of such equipment, particularly in semiconductor device manufacture. The unsteady organometallic precursor flow rate can be due to a variety of factors including progressive reduction in the total surface area of chemical from which evaporation takes place, channeling through the solid precursor compound where the carrier gas has minimal contact with the precursor compound and the sublimation of the precursor solid material to parts of the bubbler where efficient contact with the carrier gas is difficult or impossible.
[0005] Various methods have been adopted to overcome the flow problems such as the use of revers flow bubblers, the use of dispersion materials in the precursor materials, employing diffuser plates beneath the bed of solid precursor material, employing conical cylinder designs and beating on the cylinder to de-agglomerate the solid precursor material. For example, U.S. Pat. No. 4,704,988 (Mellet) discloses a bubbler wherein the vessel is separated by a porous partition into first and second compartments. In this design, the precursor material is contained in the first compartment in a liquid state and when vaporized diffuses through the partition into the second compartment where it contacts and is entrained in a carrier gas for transport from the vessel into the appropriate deposition chamber.
[0006] U.S. Pat. No. 5,603,169 (Kim) discloses a bubbler design having lower and upper porous plates through which the carrier gas passes. The lower porous plate is located above the carrier gas feed inlet and supports the solid precursor material. In operation, carrier gas passes through the lower porous plate before contacting the solid precursor material. A compressing plate is located above the lower porous plate for pressing the precursor material by its weight. Such bubbler design is quite complex and suffers from a problem of fluidizing the solid precursor material due to carrier flow through the porous plug before passing upward, i.e. against gravity, through the bubbler. This causes changes in the effective area of the solid precursor material which adversely affects the performance of the bubbler.
[0007] Conventional bubbler designs fail to provide a uniform flow rate with maximum pick-up of precursor material. There is thus a continuing need for stable flow/pick-up of solid precursor material vapor. Further, there is a need for bubbler devices that are tailored to provide a uniform and high concentration of precursor material vapor until total depletion of the vapor source.
SUMMARY OF THE INVENTION
[0008] It has been surprisingly found that the bubbler designs of the present invention provide a stable flow rate of precursor material vapor, provide a high concentration of precursor vapor in the carrier gas, can be used at lower pressures than conventional bubblers, and provides maximum contact of the carrier gas with the precursor material.
[0009] In one aspect, the present invention provides a device for providing vaporized organometallic compound to a chemical vapor deposition system including a vessel having an elongated cylindrical shaped portion having an inner surface defining a substantially constant cross-section throughout the length of the cylindrical portion, a top closure portion, a bottom closure portion, and inlet and outlet chambers in fluid communication and separated by a porous element, the top closure portion having a fill plug and a gas inlet opening, the fill plug and gas inlet opening communicating with the inlet chamber, the outlet opening communicating with the outlet chamber, the inlet chamber having a conical shaped lower portion containing the porous element, the porous element being spaced from the bottom closure portion.
[0010] In a second aspect, the present invention provides a method for providing organometallic precursor compound in the vapor phase to a chemical vapor deposition system including the steps of: a) introducing an organometallic precursor compound into the device described above; b) heating the organometallic precursor compound; c) passing a carrier gas through the organometallic precursor compound to provide a gas stream containing vaporized organometallic precursor compound; and d) delivering the gas stream to a chemical vapor deposition system.
[0011] In a third aspect, the present invention provides an apparatus for chemical vapor deposition of an organometallic precursor compound including the device described above.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 is a cross-sectional view illustrative of a conventional dip-tube bubbler.
[0013] [0013]FIG. 2 is a cross-sectional view illustrative of a bubbler of the present invention having an annular design.
[0014] [0014]FIG. 2A is a cross-sectional view of the conical section of the inlet chamber of the bubbler of FIG. 2.
[0015] [0015]FIG. 3 is a cross-sectional view illustrative of a bubbler of the present invention having a non-annular design.
[0016] [0016]FIG. 3A is a cross-sectional view of the conical section of the inlet chamber of the bubbler of FIG. 3.
DETAILED DESCRIPTION OF THE INVENTION
[0017] As used throughout the specification, the following abbreviations shall have the following meanings unless the context clearly indicates otherwise: cm=centimeter, sccm=standard cubic centimeter per minute; and ° C.=degrees Centigrade. All numerical ranges are inclusive and combinable.
[0018] The vapor generator or bubbler of the present invention is designed to eliminate poor and erratic delivery rates exhibited by known designs as well as their inability to provide complete uniform depletion of the organometallic precursor material.
[0019] The bubbler of the present invention includes a dual chambered cylindrically shaped vessel for producing vapors of solid organometallic precursor using a carrier gas. Such bubblers have an elongated cylindrical shaped portion having an inner surface defining a substantially constant cross-section throughout the length of the cylindrical portion, a top closure portion, a bottom closure portion, and inlet and outlet chambers in fluid communication and separated by a porous element, the top closure portion having a fill plug and a gas inlet opening, the fill plug and gas inlet opening communicating with the inlet chamber, the outlet opening communicating with the outlet chamber, the inlet chamber having a conical shaped lower portion containing the porous element, the porous element being spaced from the bottom closure portion.
[0020] These bubblers may be constructed of any suitable material, such as glass, poly(tetrfluoroethylene) or metal, as long as the material is inert to the organometallic compound contained therein. Metals are preferred, and particularly nickel alloys and stainless steels. Suitable stainless steels include, but are not limited to, 304, 304 L, 316, 316 L, 321, 347 and 430. Suitable nickel alloys include, but are not limited to, INCONEL, MONEL, HASTELLOY and the like. It will be appreciated by those skilled in the art that a mixture of materials may be used in the manufacture of the present bubblers.
[0021] The porous element is typically a frit having a controlled porosity. Porous elements having a wide variety of porosities may be used in the present invention. The particular porosity will depend upon the a variety of factors well within the ability of one skilled in the art. Typically, the porous element has a pore size of from about 1 to about 100 microns, preferably from about 1 to about 10 microns. However, porous elements having porosities greater than 100 microns may be suitable for certain applications. Any material may be used to construct the frit provided it is inert to the organometallic compound used and the desired porosity can be controlled. Suitable materials include, but are not limited to, glass, poly(tetrfluoroethylene) or metals such as stainless steels or nickel alloys. It is preferred that the porous element is sintered metal, and more preferably stainless steel. The suitable stainless steels and nickel alloys suitable for preparing the porous element are those described above for the manufacture of the bubbler.
[0022] The porous element is contained in the conical lower portion of the inlet chamber. The porous element retains the solid organometallic precursor in the inlet chamber and the combination of the conical section and porous element provides a restriction for the gas flow. This restriction affords uniform carrier gas flow through the packed solid organometallic precursor. The conical section enhances the movement of solid precursor within the bubbler and directs the solid material onto the porous, i.e. fritted, surface. This is particularly important towards the end of the bubbler life and improves the yield from the bubbler. The conical section of the lower portion of the inlet chamber may be of any angle, such as from 1 to 89 degrees. Preferably, the conical section has an angle of about 60 degrees or greater.
[0023] The size of the porous element is not critical. For example, the porous member may be a disk having a diameter of about 1 inch (2.54 cm) and a thickness of about 0.125 inches (0.32 cm). In an alternative embodiment, the porous element may have an inner tube concentric with its outer diameter.
[0024] The cross-sectional dimension of the bubbler is critical to the performance of the cylinder, otherwise the dimensions of the bubbler are not critical and are dependent upon the carrier gas flow, the precursor compound to be used, the particular chemical vapor deposition system used and the like. The cross-sectional dimension determines at a given pressure and flow rate the linear velocity of the gas in the cylinder, which in turn controls the contact time between the precursor material and carrier gas and thus saturation of the carrier gas. Typically, the bubbler has a cross-sectional dimension of about 2 inches (5 cm) to about 6 inches (15 cm). The other dimensions for a particular bubbler are thus well within the ability of one skilled in the art.
[0025] A wide variety of organometallic compound precursors may be used with the bubblers of the present invention. While solid or liquid organometallic precursors may be used with the present bubblers, it is preferred that solid organometallic precursors are used. Suitable organometallic precursors include, but are not limited to, cyclopentadienyl magnesium, trialkyl aluminum such as trimethyl aluminum and triethyl aluminum, trialkyl gallium such as trimethyl gallium and triethyl gallium, trialkyl antimony such as trimethyl antimony, dimethyl hydrazine, trialkyl indium such as trimethyl indium, and the like. It is preferred that the organometallic precursor is cyclopentadienyl magnesium and trialkyl indium and more preferably trimethyl indium. Such organometallic precursors are generally commercially available from a variety of suppliers.
[0026] Any suitable carrier gas may be used with the present bubblers as long as it does not react with the organometallic precursor. The particular choice of carrier gas depends upon a variety of factors such as the organometallic precursor, the particular chemical vapor deposition system employed and the like. Suitable carrier gasses include, but are not limited to, hydrogen, nitrogen, argon, helium and the like. Hydrogen is preferred. The carrier gas may be used with the present bubblers at a wide variety of flow rates. Such flow rates are a function of the bubbler cross-sectional dimension and pressure. Larger cross-sectional dimensions allow higher carrier gas flows, i.e. linear velocity, at a given pressure. For example, when the bubbler has a 2 inch cross-sectional dimension, carrier gas flow rates of up to about 500 sccm may be used, although higher gas flow rates may be used. The carrier gas flow entering the bubbler, exiting the bubbler or both entering and exiting the bubbler may be regulated by a control means. Any conventional control means may be used, such as manually activated control valves or computer activated control valves.
[0027] In general, the organometallic precursor compound is added to the bubbler inlet chamber through a fill port in the top portion of the bubbler. In use, the bubbler may be used at a variety of temperatures. The exact temperature will depend upon the particular precursor compound used and desired application. The temperature controls the vapor pressure of the precursor compound, which controls the flux of the material needed for specific growth rates or alloy compositions. Such temperature selection is well within the ability of one skilled in the art. For example, when the organometallic precursor compound is trimethyl indium, the temperature of the bubbler may be from about 10° to about 60° C., preferably from about 35° to about 55°, and more preferably from about 35° to about 50° C. The present bubblers may be heated by a variety of heating means, such as by placing the bubbler in a thermostatic bath, by direct immersion of the bubbler in a heated oil bath or by the use of a halocarbon oil flowing through a metal tube, such as a copper tube, surrounding the bubbler.
[0028] The carrier gas enters the bubbler inlet chamber through the inlet opening at the top of the bubbler. The carrier gas then passes through the organometallic precursor and picks-up vaporized precursor to form a gas stream including vaporized precursor admixed with carrier gas. The amount of vaporized precursor picked-up by the carrier gas may be controlled. It is preferred that the carrier gas is saturated with vaporized precursor. The carrier gas is then directed by means of a conical shaped lower portion of the inlet chamber to a porous element located at the tip of the conical section. The carrier gas exits the inlet chamber through the porous element to the outlet chamber which is in fluid contact with the inlet chamber. The carrier gas then exits the outlet chamber through the outlet opening and is directed to a chemical vapor deposition system. The bubblers of the present invention may be used with any chemical vapor deposition system.
[0029] [0029]FIG. 1 illustrates a conventional dip-tube bubbler design of the type disclosed in U.S. Pat. No. 4,506,815 including an elongated cylindrical container 1 , an inlet tube 2 for delivering carrier gas, and an outlet tube 3 for exhausting the precursor vapor which terminates in a dip-tube 4 which extends into the precursor material contained in the vessel.
[0030] [0030]FIG. 2 illustrates cross-sectional view of a bubbler of the present invention having an annular design. In this embodiment, an elongated cylindrical container 10 having an inner surface 11 defining a substantially constant cross-section throughout the length of cylinder 10 , a top closure portion 15 and a bottom closure portion 16 having a flat inner bottom portion 17 . Top closure portion 15 has fill port 18 , inlet opening 19 and outlet opening 20 . Inlet tube 12 and outlet tube 13 communicate with inlet opening 19 and outlet opening 20 respectively, in closure portion 15 of the container. Carrier gas flow entering the container through inlet tube 12 is regulated by control valve CV 1 . Carrier gas flow exiting the container through outlet tube 13 is regulated by control valve CV 2 . The lower end of the inlet opening 19 communicates directly with inlet chamber 25 having a conical shaped lower portion 21 . Inlet chamber 25 and out let chamber 30 are in fluid communication by means of porous member 14 . Porous member 14 is located at the tip or bottom of the conical section 21 of the inlet chamber. Outlet opening 20 communicates directly with outlet chamber 30 .
[0031] [0031]FIG. 2A shows a cross-section through A of the conical section 21 of the lower portion of the inlet chamber 25 of the bubbler of FIG. 2, including porous element 14 .
[0032] Carrier gas enters the container through inlet tube 12 and into inlet chamber 25 containing the organometallic precursor. The carrier gas picks up the vaporized organometallic precursor to form a gas stream. The gas stream exits the inlet chamber 25 through porous element 14 and enters outlet chamber 30 . The gas stream then exits the outlet chamber 30 through outlet opening 20 into outlet tube 13 and then is directed into a chemical vapor deposition system.
[0033] [0033]FIG. 3 illustrates cross-sectional view of a bubbler of the present invention having a non-annular design. In this embodiment, an elongated cylindrical container 10 having an inner surface 11 defining a substantially constant cross-section throughout the length of cylinder 10 , a top closure portion 15 and a bottom closure portion 16 having a flat inner bottom portion 17 . Top closure portion 15 has fill port 18 , inlet opening 19 and outlet opening 20 . Inlet tube 12 and outlet tube 13 communicate with inlet opening 19 and outlet opening 20 respectively, in closure portion 15 of the container. Carrier gas flow entering the container through inlet tube 12 is regulated by control valve CV 1 . Carrier gas flow exiting the container through outlet tube 13 is regulated by control valve CV 2 . The lower end of the inlet opening 19 communicates directly with inlet chamber 25 having a center tube 31 concentric to its outer diameter and a conical shaped lower portion 21 . Inlet chamber 25 and out let chamber 30 are in fluid communication by means of porous member 14 . Porous member 14 is located at the tip or bottom of the conical section 21 of the inlet chamber. Outlet opening 20 communicates with outlet chamber 30 by means of center tube 31 .
[0034] [0034]FIG. 3A is shows a cross-section through A of the conical section 21 of the lower portion of the inlet chamber 25 of the bubbler of FIG. 3, including porous element 14 and center tube 31 .
[0035] Carrier gas enters the container through inlet tube 12 and into inlet chamber 25 containing the organometallic precursor. The carrier gas picks up the vaporized organometallic precursor to form a gas stream. The gas stream exits the inlet chamber 25 through porous element 14 and enters outlet chamber 30 . The gas stream then passes through center tube 31 and exits the outlet chamber 30 through outlet opening 20 into outlet tube 13 and then is directed into a chemical vapor deposition system.
[0036] While the present invention may be used at a variety of system pressures, an advantage of the present invention is that lower pressures may be used. The bubblers of the present invention have the additional advantage of providing bubblers having uniform carrier gas flow through the packed solid organometallic precursor. The conical sections of the present bubblers also enhance the movement of solid precursor within the bubbler and direct the solid material onto the surface of the element.
[0037] The non-annular bubbler design of the present invention has the further advantage of having improved heat transfer. The single wall of the non-annular design and the lack of an annular space leads to improved heat transfer. The center tube of the non-annular design affords additional heat transfer to the center of the solid precursor material. Such non-annular design provides a more consistent operation temperature.
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Disclosed are dual chambered bubbler designs for use with solid organometallic source material for chemical vapor phase deposition systems, and a method for transporting a carrier gas saturated with source material for delivery into such systems.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority from U.S. Provisional Application Ser. No. 60/832,375 filed on Jul. 21, 2006, which is incorporated herein by reference in its entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable.
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC
[0003] The Sequence Listing, which is a part of the present disclosure, includes a computer file “10000-0027_ST25.txt” generated by U.S. Patent & Trademark Office Patent In Version 3.4 software comprising nucleotide and/or amino acid sequences of the present invention. The subject matter of the Sequence Listing is incorporated herein by reference in its entirety.
FIELD
[0004] The present invention relates to a three-dimensional structure of a receptor tyrosine kinase from the erythropoietin-producing hepatocellular carcinoma family of receptor tyrosine kinases (“Eph”), particularly EphB4 or similar polypeptide complexed with an ephrinB2 or ephrinB2 analog (“Receptor-Ligand Complex”), three-dimensional coordinates of a Receptor-Ligand Complex, models thereof, and uses of such structures and models.
INTRODUCTION
[0005] The Eph receptor tyrosine kinases and their ligands, the ephrins, regulate numerous biological processes in developing and adult tissues and have been implicated in cancer progression and in pathological forms of angiogenesis. For example, the Eph receptors and their ligands, the ephrins, play critical roles in angiogenesis during embryonic development as well as in adult tissues (Brantley-Sieders and Chen, 2004; Cheng et al., 2002; Gale and Yancopoulos, 1999; Kullander and Klein, 2002). The Eph family of receptor tyrosine kinases also regulates many other biological processes, including tissue patterning, axonal guidance, and as more recently discovered, tumorigenesis (Carmeliet and Collen, 1999; Ferrara, 1999; Pasquale, 2005; Wilkinson, 2000). Both the Eph receptor and the ephrin ligand are membrane bound, and therefore require cell-cell contact to signal a cellular response. The interaction between Eph receptors and ephrins on adjacent cell surfaces results in multimerization and clustering of the Eph-ephrin complexes, leading to forward signaling in the Eph-expressing cell and reverse signaling in the ephrin-expressing cell. EphB4 belongs to the Eph (erythropoietin-producing hepatocellular carcinoma) family of receptor tyrosine kinases, which is divided into two subclasses, A and B. based on binding preferences and sequence conservation (Gale et al., 1996). In general, EphA receptors (EphA1-EphA10) bind to glycosyl phosphatidyl inositol-(GPI) anchored ephrin-A ligands (ephrin-A1-ephrin-A6), while EphB receptors (EphB1-EphB6) interact with transmembrane ephrin-B ligands (ephrin-B1-ephrin-B3) (Eph Nomenclature Committee, 1997). While interactions between the Eph receptors and ephrin ligands of the same subclass are quite promiscuous, interactions between subclasses are rare. A few cross-subclass exceptions include the EphA4-ephrin-B2/B3 interactions (Takemoto et al., 2002), and the EphB2-ephrinA5 interaction, which has been characterized structurally (Himanen et al., 2004). EphB4 is unique within the Eph family in that it selectively binds ephrin-B2, while demonstrating only weak binding for both ephrin-B1 and ephrin-B3.
[0006] Eph receptors have a modular structure, consisting of an N-terminal ephrin binding domain adjacent to a cysteine-rich domain and two fibronectin type III repeats in the extracellular region. The intracellular region consists of a juxtamembrane domain, a conserved tyrosine kinase domain, a C-terminal sterile α-domain (SAM), and a PDZ binding motif. The N-terminal 180 amino acid globular domain is sufficient for high-affinity ligand binding (Himanen et al., 2001).
[0007] The EphB4-ephrinB2 interaction is important in angiogenesis and given that EphB4 is overexpressed in several tumor types (Dodelet, V. C., and Pasquale, E. B. (2000) Oncogene 19, 5614-5619; Nakamoto, M., and Bergemann, A. D. (2002) Microsc Res Tech 59, 58-67; Liu, W., Ahmad, S. A., Jung, Y. D., Reinmuth, N., Fan, F., Bucana, C. D., and Ellis, L. M. (2002) Cancer 94, 934-939; Berclaz, G., Karamitopoulou, E., Mazzucchelli, L., Rohrbach, V., Dreher, E., Ziemiecki, A., and Andres, A. C. (2003) Ann Oncol 14, 220-226), modulating this protein-protein interaction is a potential approach to slowing tumor angiogenesis and tumor growth. In mouse models of breast cancer, high EphB4 expression correlates with increased malignancy and tumor aggressiveness (Andres, A. C., Reid, H. H., Zurcher, G., Blaschke, R. J., Albrecht, D., and Ziemiecki, A. (1994) Oncogene 9, 1461-1467; Nikolova, Z., Djonov, V., Zuercher, G., Andres, A. C., and Ziemiecki, A. (1998) J Cell Sci 111 (Pt 18), 2741-2751; Munarini, N., Jager, R., Abderhalden, S., Zuercher, G., Rohrbach, V., Loercher, S., Pfanner-Meyer, B., Andres, A. C., and Ziemiecki, A. (2002) J Cell Sci 115, 25-37). EphB4 expression is also increased in human primary infiltrating ductal breast carcinoma and is correlated to increased malignancy (Berclaz, G., Andres, A. C., Albrecht, D., Dreher, E., Ziemiecki, A., Gusterson, B. A., and Crompton, M. R. (1996) Biochem Biophys Res Commun 226, 869-875). There is evidence that the EphB4 ectodomain stimulates endothelial cell migration and proliferation, suggesting that ephrinB2-expressing endothelial cells interact with the EphB4 ectodomain to promote angiogenesis and tumor progression. Furthermore, a kinase-deficient EphB4 mutant has been shown to increase breast cancer cell growth indicating that downstream forward kinase signaling is not an absolute requirement for tumorigenesis, at least in breast cancer cells (Noren, N. K., Lu, M., Freeman, A. L., Koolpe, M., and Pasquale, E. B. (2004) Proc Natl Acad Sci USA 101, 5583-5588). Several groups have more recently demonstrated that the full extracellular domain of EphB4 is indeed a viable therapeutic target First, the soluble extracellular domain of EphB4 was described to block both forward and reverse signaling, resulting in an inhibition of tumor growth in vivo (Kertesz, N., Krasnoperov, V., Reddy, R., Leshanski, L., Kumar, S. R., Zozulya, S., and Gill, P. S. (2006) Blood 107, 2330-2338; Martiny-Baron, G., Korff, T., Schaffner, F., Esser, N., Eggstein, S., Marme, D., and Augustin, H. G. (2004) Neoplasia 6, 248-257).
[0008] Second, phage display studies have identified a peptide (TNYL-RAW) which antagonizes the EphB4-ephrinB2 interaction in the high nanomolar range (Koolpe, M., Burgess, R., Dail, M., and Pasquale, E. B. (2005) J Biol Chem 280, 17301-17311). The crystal structure of the EphB4 receptor in complex with the phage-derived TNYL-RAW peptide (SEQ ID NO: 1) revealed that the peptide binds to the ephrin binding cavity of the receptor, effectively inhibiting interaction with the ligand (Chrencik, J. E., Brooun, A., Recht, M. I., Kraus, M. L., Koolpe, M., Kolatkar, A. R., Bruce, R. H., Martiny-Baron, G., Widmer, H., Pasquale, E. B., and Kuhn, P. (2006) Structure 14, 321-330). However, a more complete understanding of the biological role of EphB4-ephrinB2 signaling in tumorigenesis and in forms of pathological angiogenesis is now required.
[0009] Despite attempts to model the structural changes of EphB4 upon ligand binding, a detailed view of conformational arrangements of an EphB4 receptor in complex with ephrinB2 has remained elusive. Thus, the development of useful reagents for treatment or diagnosis of disease was hindered by lack of structural information of such a Receptor-Ligand Complex. Therefore, there is a need in the art to elucidate the three-dimensional structure and models of Receptor-Ligand Complexes, and to use such structures and models in therapeutic strategies, such as drug design.
DRAWINGS
[0010] Those of skill in the art will understand that the drawings, described below, are for illustrative purposes only. The drawings are not intended to limit the scope of the present teachings in any way.
[0011] FIG. 1 . The ephrin binding domain of the EphB4 receptor in complex with the ephrinB2 extracellular domain. The EphB4 receptor (right) consists of a jellyroll folding topology with 13 anti-parallel B-sheets connected by loops of varying lengths, whereas the ephrin ligand (left) is similar to the Greek key folding topology. The interface is formed by insertion of the ligand G-H loop into the hydrophobic binding cleft of EphB4.
[0012] FIG. 2 . Stereoview of the superposition of the Eph receptor ligand binding domains from the EphB4.ephrinB2 (thick grey line), EphB2.ephrinB2 (thin grey line), and EphB4.TNYL-RAW complex structures (thick line with spheres). Clear deviation is seen at the J-K loop, whereas more minor changes are seen in the receptor D-E and G-H loops (Protein Data Bank code 1 KGY). The overall root mean square deviation between the EphB4.ephrinB2 and the EphB2.ephrinB2 and EphB4-TNYL-RAW structures is 5.0 and 2.5 Å, respectively. FIG. 3 . Stereoview of σA weighted 2 F obs -F calc electron density at 2.0 Å resolution, contoured at 1σ for the EphB4.ephrinB2 interface. The ephrinB2 is the leftmost molecule (labeled) and the EphB4 is at the right (labeled). Clear density of the interface shows Phe-120 in a novel position with respect to previously described structures in order to interact with Leu-95.
[0013] FIG. 4 . Detailed ligplot diagram of critical EphB4.ephrinB2 interactions. All interactions are less than 4 Å and are indicated by dashed lines. The ligand is depicted with all bonds shown, whereas receptor residues are drawn schematically.
[0014] FIG. 5 . EphrinB2 specificity region in the EphB2/EphB4.ephrinB2 complexes. Left, the region near the EphB4 Leu-95R of the EphB4.ephrinB2 complex structure is shown in schematic representation. The van der Waals interaction between the ephrinB2 Phe-120L and the EphB4 Leu-95R is depicted as a dotted line. Right, the region near the EphB2 Arg-103R of the EphB2.ephrinB2 complex structure is shown in the same orientation as that on the left. The EphB2 Arg-103R, Ser-156R, and Ser-107R side chains are shown as grey sticks. Hydrogen bonds between Arg-103R and the two serines are shown as dotted lines. The J-K loops of EphB2 and EphB4 are labeled highlighting the change in loop position between the two complexes.
[0015] FIG. 6 . This figure illustrates binding of fluorescent peptide to wild type EphB4, EphB4 K149Q (A) and EphB4 L95R mutants. Increasing amount of EphB4 protein was added to wells containing 75 nM of fluorescent TNYL-RAW peptide. Fluorescent polarization was measured at room temperature after 30 min of incubation. Based on the structure of EphB4-ephrin-B2 complex, the substitution of L95 was predicted to impair EphB4 binding to ephrin-B2.
[0016] FIG. 7 . This figure illustrates determination of K i for TNYL-RAW. K i were determined for both wild-type EphB4 (filled triangles) and EphB4 (K149Q) mutant (filled squares).
[0017] FIG. 8 . This figure illustrates binding of fluorescent TNYL-RAW peptide in the presence of increasing concentration of DMSO. Increasing amounts of EphB4 protein were added to wells containing 75 nM of TNYL-RAW-Alexa-532 peptide. Fluorescent polarization was measured at room temperature.
[0018] FIG. 9 . This figure illustrates Z-factor determination for EphB4-Alexa-532-TNYL-RAW fluorescent polarization assay.
DETAILED DESCRIPTION
[0019] The present invention relates to the discovery of the three-dimensional structure of a Receptor-Ligand Complex, models of such three-dimensional structures, a method of structure-based drug design using such structures, the compounds identified by such methods and the use of such compounds in therapeutic compositions. In particular, the present invention involves the crystal structure of the EphB4 receptor in complex with ephrinB2 at a resolution of 2.0 Å. EphrinB2 is situated in a hydrophobic cleft of EphB4 corresponding to the cleft in EphB2 occupied by the ephrinB2 G-H loop. The crystal reveals critical structural features of EphB4 that, when in complex ephrinB2, provides a basis for antagonist design and modeling.
[0020] In particular, the structural and thermodynamic characterization of the EphB4 receptor in complex with ephrinB2 is described. The structure reveals that the flexible J-K loop of EphB4 shifts significantly as compared to previous crystal structures, providing a new network of contacts to secure the interaction. In addition, using biophysical analysis, one amino acid, Leu-95, is identified which lines the ligand binding cavity of the EphB4 receptor and provides the molecular determinants for the unique specificity exhibited by the EphB4 receptor for the ephrinB2 ligand.
[0021] A multiple sequence alignment with members of the EphB subclass reveals that the EphB4 receptor lacks a conserved arginine and instead contains a leucine at position 95. A Leu-95-Arg mutation was previously predicted to result in steric interference with the antagonistic TNYL-RAW peptide ligand (Chrencik et al., Structure, 2006, incorporated herein by reference in its entirety; SEQ ID NO: 1). This mutation also results in steric interference with Phe-120 in the G-H loop of ephrinB2 due to the different positioning of the J-K loop of EphB4. A leucine instead of an arginine at position 95 of the EphB4 receptor is sufficient to cause substantial structural rearrangement of the receptor J-K loop. Also provided is a novel position of the conserved Phe-120 in the high affinity FSPN sequence of the ephrinB2 G-H loop, suggesting that although ephrinB2 is conserved in structure in both receptor-bound and apo structures, there is variability within the rigid G-H loop to conform to a specific receptor.
[0022] EphB4 binds only weakly to both ephrinB1 and ephrinB3, while exhibiting high affinity for ephrinB2. Considering the B-subclass ephrin G-H loop (ephrinB1-B3), it is interesting to speculate on why EphB4 preferentially binds ephrinB2 over other B-subclass ligands. EphrinB1 shares significant sequence identity with the high affinity ephrinB2 G-H loop, except at position 124, which is a Tyr in ephrinB1 and a Leu in ephrinB2. While Leu-124 forms no integral interactions with EphB4, the small size of the leucine allows tight packing within the receptor binding cavity. A leucine also maintains the hydrophobic nature of the binding cleft. Superposition of a tyrosine on the ephrinB2 structure would require the rearrangement of the EphB4 J-K loop in order to accommodate the bulky tyrosine, and, without being bound by a particular theory, this likely accounts for the reduced affinity of EphB4 for ephrinB1. The ephrinB3 G-H loop is also very similar to the ephrinB2 G-H loop but deviates in the FSPN sequence, which contains a tyrosine instead of the phenylalanine (YSPN). Phe-120 forms critical interactions with residues lining the EphB receptor-ephrinB2 binding cavity in the three complex crystal structures thus far described. In the previous crystal structures, Phe-120 extends to the surface of the binding cavity, adjacent to the receptor G-H loop. Superposition of a tyrosine on the EphB2-ephrinB2 structure would not affect the dynamics of the ligand binding cavity, and this residue is predicted to interact with several water molecules on the surface of the complex. However, in the present crystal structure, the Phe-120 of ephrinB2 is observed in a novel position, buried within the hydrophic binding cleft and forming interactions with Leu-95R and the Cys-61-Cys-184 disulfide bridge. Insertion of a tyrosine at this position would therefore result in both steric interference within the receptor binding cavity and a polar redistribution of the active site.
[0023] Thermodynamic discrepancies between Eph receptor and ephrin binding can be considered in the design of therapeutics to treat disease related to the Eph receptor family. Iterative rounds of structure based drug design provide an understanding of the enthalpic and entropic contributions of small molecule compounds. In the case of the ephrin ligand, the G-H loop is predicted to reduce conformational entropy losses due to its rigidity, maximizing the effects of solvation entropy due to the hydrophobic nature of the Eph ligand binding cavity. The ephrin, on the other hand, can experience large losses in conformational entropy upon receptor binding which are compensated by favorable enthalpic gains between receptor and ephrin residues. The ephrin ligand, with entropically-driven binding, can interact with multiple members of the EphB family. In contrast, the TNYL-RAW peptide, with enthalpically-driven binding, is a specific inhibitor of the EphB4-ephrinB2 interaction.
[0024] Accordingly, one aspect of the present invention includes a model of a Receptor-Ligand Complex in which the model represents a three-dimensional structure of a Receptor-Ligand Complex. Another aspect of the present invention includes the three-dimensional structure of a Receptor-Ligand Complex. A three-dimensional structure of a Receptor-Ligand Complex substantially conforms with the atomic coordinates represented in Table 1. According to the present invention, the use of the term “substantially conforms” refers to at least a portion of a three-dimensional structure of a Receptor-Ligand Complex which is sufficiently spatially similar to at least a portion of a specified three-dimensional configuration of a particular set of atomic coordinates (e.g., those represented by Table 1) to allow the three-dimensional structure of a Receptor-Ligand Complex to be modeled or calculated using the particular set of atomic coordinates as a basis for determining the atomic coordinates defining the three-dimensional configuration of a Receptor-Ligand Complex.
[0025] More particularly, a structure that substantially conforms to a given set of atomic coordinates is a structure wherein at least about 50% of such structure has an average root-mean-square deviation (RMSD) of less than about 2.0 Å for the backbone atoms in secondary structure elements in each domain, and in various aspects, less than about 1.25 Å for the backbone atoms in secondary structure elements in each domain, and, in various aspects less than about 1.0 Å, in other aspects less than about 0.75 Å, less than about 0.5 Å, and, less than about 0.25 Å for the backbone atoms in secondary structure elements in each domain. In one aspect of the present invention, a structure that substantially conforms to a given set of atomic coordinates is a structure wherein at least about 75% of such structure has the recited average RMSD value, and in some aspects, at least about 90% of such structure has the recited average RMSD value, and in some aspects, about 100% of such structure has the recited average RMSD value. In particular, the above definition of “substantially conforms” can be extended to include atoms of amino acid side chains. As used herein, the phrase “common amino acid side chains” refers to amino acid side chains that are common to both the structure which substantially conforms to a given set of atomic coordinates and the structure that is actually represented by such atomic coordinates.
[0026] In another aspect of the present invention, a three-dimensional structure that substantially conforms to a given set of atomic coordinates is a structure wherein at least about 50% of the common amino acid side chains have an average RMSD of less than about 2.0 Å, and in various aspects, less than about 1.25 Å, and, in other aspects, less than about 1.0 Å, less than about 0.75 Å, less than about 0.5 Å, and less than about 0.25 Å. In one aspect of the present invention, a structure that substantially conforms to a given set of atomic coordinates is a structure wherein at least about 75% of the common amino acid side chains have the recited average RMSD value, and in some aspects, at least about 90% of the common amino acid side chains have the recited average RMSD value, and in some aspects, about 100% of the common amino acid side chains have the recited average RMSD value.
[0027] A three-dimensional structure of a Receptor-Ligand Complex which substantially conforms to a specified set of atomic coordinates can be modeled by a suitable modeling computer program such as MODELER (A. Sali and T. L. Blundell, J. Mol. Biol., vol. 234:779-815, 1993 as implemented in the Insight II software package Insight II, available from Accelerys (San Diego, Calif.)) and those software packages listed in the Examples, using information, for example, derived from the following data: (1) the amino acid sequence of the Receptor-Ligand Complex; (2) the amino acid sequence of the related portion(s) of the protein represented by the specified set of atomic coordinates having a three-dimensional configuration; and, (3) the atomic coordinates of the specified three-dimensional configuration. A three-dimensional structure of a Receptor-Ligand Complex which substantially conforms to a specified set of atomic coordinates can also be calculated by a method such as molecular replacement, which is described in detail below.
[0028] A suitable three-dimensional structure of the Receptor-Ligand Complex for use in modeling or calculating the three-dimensional structure of another Receptor-Ligand Complex comprises the set of atomic coordinates represented in Table 1. The set of three-dimensional coordinates set forth in Table 1 is represented in standard Protein Data Bank format. The atomic coordinates have been deposited in the Protein Data Bank, having Accession No. 2HLE. According to the present invention, a Receptor-Ligand Complex has a three-dimensional structure which substantially conforms to the set of atomic coordinates represented by Table 1. As used herein, a three-dimensional structure can also be a most probable, or significant, fit with a set of atomic coordinates. According to the present invention, a most probable or significant fit refers to the fit that a particular Receptor-Ligand Complex has with a set of atomic coordinates derived from that particular Receptor-Ligand Complex. Such atomic coordinates can be derived, for example, from the crystal structure of the protein such as the coordinates determined for the Receptor-Ligand Complex structure provided herein, or from a model of the structure of the protein. For example, the three-dimensional structure of a dimeric protein, including a naturally occurring or recombinantly produced EphB4 receptor protein in complex with ephrinB2, substantially conforms to and is a most probable fit, or significant fit, with the atomic coordinates of Table 1. The three-dimensional crystal structure of the Receptor-Ligand Complex may comprise the atomic coordinates of Table 1. Also as an example, the three-dimensional structure of another Receptor-Ligand Complex would be understood by one of skill in the art to substantially conform to the atomic coordinates of Table 1. This definition can be applied to the other EphB4 receptor proteins in a similar manner.
[0029] For example, the structure of the EphB4 receptor establishes the general architecture of the EphB receptor family. Accordingly, in some configurations, EphB4 receptor protein sequence homology across eukaryotes can be used as a basis to predict the structure of such receptors, in particular the structure for such receptor-ligand binding sites and other conserved regions.
[0030] In various aspects of the present invention, a structure of a Receptor-Ligand Complex substantially conforms to the atomic coordinates represented in Table 1. Such values as listed in Table 1 can be interpreted by one of skill in the art. In other aspects, a three-dimensional structure of a Receptor-Ligand Complex substantially conforms to the three-dimensional coordinates represented in Table 1. In other aspects, a three-dimensional structure of a Receptor-Ligand Complex is a most probable fit with the three-dimensional coordinates represented in Table 1. Methods to determine a substantially conforming and probable fit are within the expertise of skill in the art and are described herein in the Examples section.
[0031] A Receptor-Ligand Complex that has a three-dimensional structure which substantially conforms to the atomic coordinates represented by Table 1 includes an EphB4 receptor protein having an amino acid sequence that is at least about 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, or 100% identical to an amino acid sequence of a human EphB4 receptor protein, in particular an amino acid sequence having SEQ ID NO: 4, across the full-length of the EphB4 receptor sequence. A sequence alignment program such as BLAST (available from the National Institutes of Health Internet web site http://www.ncbi.nlm.nih.gov/BLAST) may be used by one of skill in the art to compare sequences of an EphB receptor to the EphB4 receptor.
[0032] A three-dimensional structure of any Receptor-Ligand Complex can be modeled using methods generally known in the art based on information obtained from analysis of a Receptor-Ligand Complex crystal, and from other Receptor-Ligand Complex structures which are derived from a Receptor-Ligand Complex crystal. The Examples section below discloses the production of a Receptor-Ligand Complex crystal, in particular a truncated EphB4 receptor having SEQ ID NO: 2 or 3 complexed with ephrinB2 (SEQ ID NO: 6), and a model of a Receptor-Ligand Complex, in particular a truncated EphB4 receptor having SEQ ID NO: 2 or 3 complexed with ephrinB2, using methods generally known in the art based on the information obtained from analysis of a Receptor-Ligand Complex crystal.
[0033] An aspect of the present invention comprises using the three-dimensional structure of a crystalline Receptor-Ligand Complex to derive the three-dimensional structure of another Receptor-Ligand Complex. Therefore, the crystalline EphB4 receptor complexed with ephrinB2 (SEQ ID NO: 6), and the three-dimensional structure of EphB4 complexed with ephrinB2 permits one of ordinary skill in the art to now derive the three-dimensional structure, and models thereof, of another Receptor-Ligand Complex having highly specific EphB4 binding characteristics. The derivation of the structure of such Receptor-Ligand Complexes can now be achieved even in the absence of having crystal structure data for such other Receptor-Ligand Complexes, and when the crystal structure of another Receptor-Ligand Complex is available, the modeling of the three-dimensional structure of the new Receptor-Ligand Complex can be refined using the knowledge already gained from the Receptor-Ligand Complex structure.
[0034] In some configurations of the present teachings, the absence of crystal structure data for other Receptor-Ligand Complexes, the three-dimensional structures of other Receptor-Ligand Complexes can be modeled, taking into account differences in the amino acid sequence of the other Receptor-Ligand Complex. Moreover, the present invention allows for structure-based drug design of compounds which affect the activity of virtually any EphB receptor, and particularly, of EphB4.
[0035] One aspect of the present invention includes a three-dimensional structure of a Receptor-Ligand Complex, in which the atomic coordinates of the Receptor-Ligand Complex are generated by the method comprising: (a) providing an EphB4 receptor complexed with ephrinB2 in crystalline form; (b) generating an electron-density map of the crystalline EphB4 receptor complexed with ephrinB2; and (c) analyzing the electron-density map to produce the atomic coordinates. For example, the structure of human EphB4 receptor in complex with ephrinB2 (SEQ ID NO: 6) is provided herein.
[0036] The present invention also provides a three-dimensional structure of the EphB4 receptor protein complexed with ephrinB2 (SEQ ID NO: 6), can be used to derive a model of the three-dimensional structure of another Receptor-Ligand Complex (i.e., a structure to be modeled). As used herein, a “structure” of a protein refers to the components and the manner of arrangement of the components to constitute the protein. As used herein, the term “model” refers to a representation in a tangible medium of the three-dimensional structure of a protein, polypeptide or peptide. For example, a model can be a representation of the three-dimensional structure in an electronic file, on a computer screen, on a piece of paper (i.e., on a two dimensional medium), and/or as a ball-and-stick figure. Physical three-dimensional models are tangible and include, but are not limited to, stick models and space-filling models. The phrase “imaging the model on a computer screen” refers to the ability to express (or represent) and manipulate the model on a computer screen using appropriate computer hardware and software technology known to those skilled in the art. Such technology is available from a variety of sources including, for example, Accelrys, Inc. (San Diego, Calif.). The phrase “providing a picture of the model” refers to the ability to generate a “hard copy” of the model. Hard copies include both motion and still pictures. Computer screen images and pictures of the model can be visualized in a number of formats including space-filling representations, α-carbon traces, ribbon diagrams and electron density maps.
[0037] Suitable target Receptor-Ligand Complex structures to model using a method of the present invention include any EphB receptor protein, polypeptide or peptide that is substantially structurally related to an EphB4 receptor protein complexed with ephrinB2. In various embodiments, a target Receptor-Ligand Complex structure that is substantially structurally related to an EphB4 receptor protein includes a target Receptor-Ligand Complex structure having an amino acid sequence that is at least about 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, or 100% identical to an amino acid sequence of a human EphB4 receptor protein, in particular an amino acid sequence having SEQ ID NO: 4, across the full-length of the EphB4 receptor sequence when using, for example, a sequence alignment program such as BLAST (supra). In various aspects of the present invention, target Receptor-Ligand Complex structures to model include proteins comprising amino acid sequences that are at least about 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, or 100% identical to amino acid sequence of a truncated EphB4 receptor, EphB4(17-196), having SEQ ID NO: 2 or EphB4 17-198, having SEQ ID NO: 3, when comparing suitable regions of the sequence, such as the amino acid sequence for an ephrin binding site of any one of the amino acid sequences, when using an alignment program such as BLAST (supra) to align the amino acid sequences.
[0038] According to the present invention, a structure can be modeled using techniques generally described by, for example, Sali, Current Opinions in Biotechnology, vol. 6, pp. 437-451, 1995, and algorithms can be implemented in program packages such as Insight II, available from Accelerys (San Diego, Calif.). Use of Insight II HOMOLOGY requires an alignment of an amino acid sequence of a known structure having a known three-dimensional structure with an amino acid sequence of a target structure to be modeled. The alignment can be a pairwise alignment or a multiple sequence alignment including other related sequences (for example, using the method generally described by Rost, Meth. Enzymol., vol. 266, pp. 525-539, 1996) to improve accuracy. Structurally conserved regions can be identified by comparing related structural features, or by examining the degree of sequence homology between the known structure and the target structure. Certain coordinates for the target structure are assigned using known structures from the known structure. Coordinates for other regions of the target structure can be generated from fragments obtained from known structures such as those found in the Protein Data Bank. Conformation of side chains of the target structure can be assigned with reference to what is sterically allowable and using a library of rotamers and their frequency of occurrence (as generally described in Ponder and Richards, J. Mol. Biol., vol. 193, pp. 775-791, 1987). The resulting model of the target structure, can be refined by molecular mechanics to ensure that the model is chemically and conformationally reasonable.
[0039] Accordingly, one embodiment of the present invention is a method to derive a model of the three-dimensional structure of a target Receptor-Ligand Complex structure, the method comprising the steps of: (a) providing an amino acid sequence of a Receptor-Ligand Complex and an amino acid sequence of a target ligand-complexed EphB receptor; (b) identifying structurally conserved regions shared between the Receptor-Ligand Complex amino acid sequence and the target ligand-complexed EphB4 receptor amino acid sequence; (c) determining atomic coordinates for the target ligand-complexed EphB4 receptor by assigning said structurally conserved regions of the target ligand-complexed EphB4 receptor to a three-dimensional structure using a three-dimensional structure of a Receptor-Ligand Complex based on atomic coordinates that substantially conform to the atomic coordinates represented in Table 1, to derive a model of the three-dimensional structure of the target ligand-complexed EphB4 receptor amino acid sequence. A model according to the present invention has been previously described herein. In one aspect, the model comprises a computer model. The method can further comprise the step of electronically simulating the structural assignments to derive a computer model of the three-dimensional structure of the target ligand-complexed EphB4 receptor amino acid sequence.
[0040] Another embodiment of the present invention is a method to derive a computer model of the three-dimensional structure of a target ephrinB2-complexed EphB4 receptor structure for which a crystal has been produced (referred to herein as a “crystallized target structure”). A suitable method to produce such a model includes the method comprising molecular replacement. Methods of molecular replacement are generally known by those of skill in the art and are performed in a software program including, for example, X-PLOR available from Accelerys (San Diego, Calif.). In various aspects, a crystallized target ligand-complexed EphB receptor structure useful in a method of molecular replacement according to the present invention has an amino acid sequence that is at least about 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, or 100% identical to the amino acid sequence of the search structure (e.g., human EphB4), when the two amino acid sequences are compared using an alignment program such as BLAST (supra). A suitable search structure of the present invention includes a Receptor-Ligand Complex having a three-dimensional structure that substantially conforms with the atomic coordinates listed in Table 1.
[0041] Another aspect of the present invention is a method to determine a three-dimensional structure of a target Receptor-Ligand Complex structure, in which the three-dimensional structure of the target Receptor-Ligand Complex structure is not known. Such a method is useful for identifying structures that are related to the three-dimensional structure of a Receptor-Ligand Complex based only on the three-dimensional structure of the target structure. For example, the present method enables identification of structures that do not have high amino acid identity with an EphB4 receptor protein but which share three-dimensional structure similarities of a ligand-complexed EphB4 receptor. In various aspects of the present invention, a method to determine a three-dimensional structure of a target Receptor-Ligand Complex structure comprises: (a) providing an amino acid sequence of a target structure, wherein the three-dimensional structure of the target structure is not known; (b) analyzing the pattern of folding of the amino acid sequence in a three-dimensional conformation by fold recognition; and (c) comparing the pattern of folding of the target structure amino acid sequence with the three-dimensional structure of a Receptor-Ligand Complex to determine the three-dimensional structure of the target structure, wherein the three-dimensional structure of the Receptor-Ligand Complex substantially conforms to the atomic coordinates represented in Table 1. For example, methods of fold recognition can include the methods generally described in Jones, Curr. Opinion Struc. Biol., vol. 7, pp. 377-387, 1997. Such folding can be analyzed based on hydrophobic and/or hydrophilic properties of a target structure.
[0042] One aspect of the present invention includes a three-dimensional computer image of the three-dimensional structure of a Receptor-Ligand Complex. In one aspect, a computer image is created to a structure which substantially conforms with the three-dimensional coordinates listed in Table 1. A computer image of the present invention can be produced using any suitable software program, including, but not limited to, Pymol available from DeLano Scientific, LLC (South San Francisco, Calif.). Suitable computer hardware useful for producing an image of the present invention are known to those of skill in the art.
[0043] Another aspect of the present invention relates to a computer-readable medium encoded with a set of three-dimensional coordinates represented in Table 1, wherein, using a graphical display software program, the three-dimensional coordinates create an electronic file that can be visualized on a computer capable of representing said electronic file as a three-dimensional image. Yet another aspect of the present invention relates to a computer-readable medium encoded with a set of three-dimensional coordinates of a three-dimensional structure which substantially conforms to the three-dimensional coordinates represented in Table 1, wherein, using a graphical display software program, the set of three-dimensional coordinates create an electronic file that can be visualized on a computer capable of representing said electronic file as a three-dimensional image.
[0044] The present invention also includes a three-dimensional model of the three-dimensional structure of a target structure, such a three-dimensional model being produced by the method comprising: (a) providing an amino acid sequences of an EphB4 receptor comprised by a Receptor-Ligand Complex and an amino acid sequence of a target Receptor-Ligand Complex structure; (b) identifying structurally conserved regions shared between the EphB4 receptor amino acid sequence and the amino acid sequence comprised by the target Receptor-Ligand Complex structure; (c) determining atomic coordinates for the target Receptor-Ligand Complex by assigning the structurally conserved regions of the target Receptor-Ligand Complex to a three-dimensional structure using a three-dimensional structure of the EphB4 receptor comprised by a Receptor-Ligand Complex based on atomic coordinates that substantially conform to the atomic coordinates represented in Table 1 to derive a model of the three-dimensional structure of the target Receptor-Ligand Complex. In one aspect, the model comprises a computer model.
[0045] Another isolated EphB receptor protein can be used with the methods of the present invention. An isolated EphB receptor protein can be isolated from its natural milieu or produced using recombinant DNA technology (e.g., polymerase chain reaction (PCR) amplification, cloning) or chemical synthesis. To produce recombinant EphB receptor protein, a nucleic acid molecule encoding EphB receptor protein (e.g., SEQ ID NO: 5) can be inserted into any vector capable of delivering the nucleic acid molecule into a host cell. A nucleic acid molecule of the present invention can encode any portion of an EphB receptor protein, in various aspects a full-length EphB receptor protein, and in various aspects a soluble or truncated form of EphB4 receptor protein (i.e., a form of EphB4 receptor protein capable of being secreted by a cell that produces such protein). A suitable nucleic acid molecule to include in a recombinant vector, and particularly in a recombinant molecule, includes a nucleic acid molecule encoding a protein having the amino acid sequence represented by SEQ ID NOs: 2 or 3 and SEQ ID NO: 4.
[0046] A recombinant vector can be either RNA or DNA, either prokaryotic or eukaryotic, and typically is a virus or a plasmid. In various aspects, a nucleic acid molecule encoding an EphB4 receptor protein is inserted into a vector comprising an expression vector to form a recombinant molecule. As used herein, an expression vector is a DNA or RNA vector that is capable of transforming a host cell and of affecting expression of a specified nucleic acid molecule. Expression vectors of the present invention include any vectors that function (i.e., direct gene expression) in recombinant cells of the present invention, including in bacterial, fungal, endoparasite, insect, other animal, and plant cells.
[0047] An expression vector can be transformed into any suitable host cell to form a recombinant cell. A suitable host cell includes any cell capable of expressing a nucleic acid molecule inserted into the expression vector. For example, a prokaryotic expression vector can be transformed into a bacterial host cell. One method to isolate EphB4 receptor protein useful for producing ligand-complexed EphB4 receptor crystals includes recovery of recombinant proteins from cell cultures of recombinant cells expressing such EphB4 receptor protein.
[0048] EphB4 receptor proteins of the present invention can be purified using a variety of standard protein purification techniques, such as, but not limited to, affinity chromatography, ion exchange chromatography, filtration, electrophoresis, hydrophobic interaction chromatography, gel filtration chromatography, reverse phase chromatography, chromatofocusing and differential solubilization. In various aspects of the present invention, an EphB4 receptor protein is purified in such a manner that the protein is purified sufficiently for formation of crystals useful for obtaining information related to the three-dimensional structure of a Receptor-Ligand Complex. In some aspects, a composition of EphB4 receptor protein is about 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, or 100% pure.
[0049] Another embodiment of the present invention includes a composition comprising a Receptor-Ligand Complex in a crystalline form (i.e., Receptor-Ligand Complex crystals). As used herein, the terms “crystalline Receptor-Ligand Complex” and “Receptor-Ligand Complex crystal” both refer to crystallized a Receptor-Ligand Complex and are intended to be used interchangeably. In various aspects of the present invention, a crystalline Receptor-Ligand Complex is produced using the crystal formation method described in the Examples.
[0050] In particular, the present invention includes a composition comprising EphB4 receptor complexed with ephrinB2 in a crystalline form (i.e., ephrinB2-complexed EphB4 crystals). As used herein, the terms “crystalline ephrinB2-complexed EphB4” and “ephrinB2-complexed EphB4 crystal” both refer to crystallized EphB4 receptor complexed with ephrinB2 and are intended to be used interchangeably. In various aspects of the present invention, a crystal ephrinB2-complexed EphB4 is produced using the crystal formation method described in the Examples. In some aspects, a composition of the present invention includes ephrinB2-complexed EphB4 molecules arranged in a crystalline manner in a space group P4 1 so as to form a unit cell of dimensions a=81.09 Å, b=81.09 Å, and c=50.95 Å. A suitable crystal of the present invention provides X-ray diffraction data for determination of atomic coordinates of the ephrinB2-complexed EphB4 to a resolution of about 2.0 Å, and in some aspects about 1.8 Å, and in other aspects at about 1.6 Å.
[0051] According to an aspect of the present invention, crystalline Receptor-Ligand Complex can be used to determine the ability of a compound of the present invention to bind to an EphB4 receptor in a manner predicted by a structure based drug design method of the present invention. In various aspects of the present invention, a Receptor-Ligand Complex crystal is soaked in a solution containing a chemical compound of the present invention. Binding of the chemical compound to the crystal is then determined by methods standard in the art.
[0052] One aspect of the present invention is a therapeutic composition. A therapeutic composition of the present invention comprises one or more therapeutic compounds. In one aspect, a therapeutic composition is provided that is capable of antagonizing the EphB4 receptor. For example, a therapeutic composition of the present invention can inhibit (i.e., prevent, block) binding of an EphB4 receptor on a cell having an EphB4 receptor (e.g., human cells) to a, e.g., ephrinB2 or ephrinB2 analog by interfering with the ligand binding domain of an EphB4 receptor. As used herein, the term “ligand binding domain” refers to the region of a molecule to which another molecule specifically binds.
[0053] Suitable inhibitory compounds of the present invention are compounds that interact directly with an EphB4 receptor protein or truncated EphB4 receptor protein (e.g., SEQ ID NOs: 2 or 3), thereby inhibiting the binding of ephrin-B2 to an EphB4 receptor by blocking the ligand binding domain of an EphB4 receptor (referred to herein as substrate analogs). An EphB4 receptor substrate analog refers to a compound that interacts with (e.g., binds to, associates with, modifies) the ligand binding domain of an EphB4 receptor. An EphB4 receptor substrate analog can, for example, comprise a chemical compound that mimics a polypeptide having SEQ ID NO: 6, truncated polypeptides comprised by SEQ ID NO: 6, or that binds specifically to the ephrin binding globular domain of an EphB4 receptor. Particularly, a substrate analog can comprise the G-H loop of ephrinB2 (SEQ ID NO: 7). Additionally, amino acids 120 through 127 of SEQ ID NO: 6 are useful in various aspects. In various aspects, an EphB4 receptor substrate analog useful in the present invention has an amino acid sequence that is at least about 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, or 100% identical to the amino acid sequence of SEQ ID NO: 7 and amino acids 120 through 127 of SEQ ID NO: 6.
[0054] According to the present invention, suitable therapeutic compounds of the present invention include peptides or other organic molecules, and inorganic molecules. Suitable organic molecules include small organic molecules. In various aspects, a therapeutic compound of the present invention is not harmful (e.g., toxic) to an animal when such compound is administered to an animal. Peptides refer to a class of compounds that is small in molecular weight and yields two or more amino acids upon hydrolysis. A polypeptide is comprised of two or more peptides. As used herein, a protein is comprised of one or more polypeptides. Suitable therapeutic compounds to design include peptides composed of “L” and/or “D” amino acids that are configured as normal or retroinverso peptides, peptidomimetic compounds, small organic molecules, or homo- or hetero-polymers thereof, in linear or branched configurations.
[0055] Therapeutic compounds of the present invention can be designed using structure based drug design. Structure based drug design refers to the use of computer simulation to predict a conformation of a peptide, polypeptide, protein, or conformational interaction between a peptide or polypeptide, and a therapeutic compound. In the present teachings, knowledge of the three-dimensional structure of the EphB4 ligand binding domain of an EphB4 receptor when bound with ephrinB2 provide one of skill in the art the ability to design a therapeutic compound that binds to EphB4 receptors, is stable and results in inhibition of a biological response, such as tumorigenesis. For example, knowledge of the three-dimensional structure of the EphB4 ligand binding domain of an EphB4 receptor in complex with ephrinB2 provides to a skilled artisan the ability to design a ligand or an analog of a ligand which can function as a substrate or ligand of an EphB4 receptor.
[0056] Suitable structures and models useful for structure-based drug design are disclosed herein. Models of target structures to use in a method of structure-based drug design include models produced by any modeling method disclosed herein, such as, for example, molecular replacement and fold recognition related methods. In some aspects of the present invention, structure based drug design can be applied to a structure of EphB4 in complex with ephrinB2 (SEQ ID NO: 6), and to a model of a target EphB receptor structure.
[0057] One embodiment of the present invention is a method for designing a drug which interferes with an activity of an EphB4 receptor. In various configurations, the method comprises providing a three-dimensional structure of a Receptor-Ligand Complex comprising the EphB4 receptor and at least one ligand of the receptor; and designing a chemical compound which is predicted to bind to the EphB4 receptor. The designing can comprise using physical models, such as, for example, ball-and-stick representations of atoms and bonds, or on a digital computer equipped with molecular modeling software. In some configurations, these methods can further include synthesizing the chemical compound, and evaluating the chemical compound for ability to interfere with an activity of the EphB4 receptor.
[0058] Suitable three-dimensional structures of a Receptor-Ligand Complex and models to use with the present method are disclosed herein. According to the present invention, designing a compound can include creating a new chemical compound or searching databases of libraries of known compounds (e.g., a compound listed in a computational screening database containing three-dimensional structures of known compounds). Designing can also include simulating chemical compounds having substitute moieties at certain structural features. In some configurations, designing can include selecting a chemical compound based on a known function of the compound. In some configurations designing can comprise computational screening of one or more databases of compounds in which three-dimensional structures of the compounds are known. In these configurations, a candidate compound can be interacted virtually (e.g., docked, aligned, matched, interfaced) with the three-dimensional structure of a Receptor-Ligand Complex by computer equipped with software such as, for example, the AutoDock software package, (The Scripps Research Institute, La Jolla, Calif.) or described by Humblet and Dunbar, Animal Reports in Medicinal Chemistry, vol. 28, pp. 275-283, 1993, M Venuti, ed., Academic Press. Methods for synthesizing candidate chemical compounds are known to those of skill in the art.
[0059] Various other methods of structure-based drug design are disclosed in references such as Maulik et al., 1997, Molecular Biotechnology: Therapeutic Applications and Strategies , Wiley-Liss, Inc., which is incorporated herein by reference in its entirety. Maulik et al. disclose, for example, methods of directed design, in which the user directs the process of creating novel molecules from a fragment library of appropriately selected fragments; random design, in which the user uses a genetic or other algorithm to randomly mutate fragments and their combinations while simultaneously applying a selection criterion to evaluate the fitness of candidate ligands; and a grid-based approach in which the user calculates the interaction energy between three-dimensional structures and small fragment probes, followed by linking together of favorable probe sites.
[0060] In one aspect, a chemical compound of the present invention that binds to the ligand binding domain of a Receptor-Ligand Complex can be a chemical compound having chemical and/or stereochemical complementarity with an EphB4 receptor, e.g., an EphB4 receptor or ligand such as, for example, ephrinB2. In particular, the amino acid sequence of SEQ ID NO: 7, amino acids 120 through 127 of SEQ ID NO: 6, and analogs thereof can be complimentary. In some configurations, a chemical compound that binds to the ligand binding domain of an EphB4 receptor can associate with an affinity of at least about 10 −6 M, at least about 10 −7 M, or at least about 10 −8 M.
[0061] Several sites of an EphB4 receptor can be targeted for structure based drug design. These sites include, in non-limiting example residues which contact ephrin-B2 or a polypeptide having SEQ ID NO: 1, e.g., EphB4 D-E and J-K loops; Leu-48, Cys-61, Leu-95, Ser-99 Leu-100, Pro-101, Thr-147, Lys-149, Ala-155, and Cys-184 of SEQ ID NO: 6. Conversely, the structure based drug design can be based upon the sites of the ligand which bind to the EphB4 receptor, e.g., Phe-120, Pro-122, Leu-124, Trp-125, and Leu-127 of ephrinB2.
[0062] Drug design strategies as specifically described above with regard to residues and regions of the ligand-complexed EphB4 receptor crystal can be similarly applied to the other EphB structures, including other EphB receptors disclosed herein. One of ordinary skill in the art, using the art recognized modeling programs and drug design methods, many of which are described herein, can modify the EphB4 design strategy according to differences in amino acid sequence. For example, this strategy can be used to design compounds which regulate a function of the EphB4 receptor in EphB receptors. In addition, one of skill in the art can use lead compound structures derived from one EphB receptor, such as the EphB4 receptor, and take into account differences in amino acid residues in other EphB4 receptors.
[0063] In the present method of structure-based drug design, it is not necessary to align a candidate chemical compound (i.e., a chemical compound being analyzed in, for example, a computational screening method of the present invention) to each residue in a target site. Suitable candidate chemical compounds can align to a subset of residues described for a target site. In some configurations of the present invention, a candidate chemical compound can comprise a conformation that promotes the formation of covalent or noncovalent crosslinking between the target site and the candidate chemical compound. In certain aspects, a candidate chemical compound can bind to a surface adjacent to a target site to provide an additional site of interaction in a complex. For example, when designing an antagonist (i.e., a chemical compound that inhibits the binding of ephrinB2 to an EphB4 receptor by blocking a ligand binding domain or interface), the antagonist can be designed to bind with sufficient affinity to the binding site or to substantially prohibit a ligand from binding to a target area. It will be appreciated by one of skill in the art that it is not necessary that the complementarity between a candidate chemical compound and a target site extend over all residues specified here.
[0064] In various aspects, the design of a chemical compound possessing stereochemical complementarity can be accomplished by means of techniques that optimize, chemically or geometrically, the “fit” between a chemical compound and a target site. Such techniques are disclosed by, for example, Sheridan and Venkataraghavan, Acc. Chem. Res., vol. 20, p. 322, 1987: Goodford, J. Med. Chem., vol. 27, p. 557, 1984; Beddell, Chem. Soc. Reviews, vol. 279, 1985; Hol, Angew. Chem., vol. 25, p. 767, 1986; and Verlinde and Hol, Structure, vol. 2, p. 577, 1994, each of which are incorporated by this reference herein in their entirety.
[0065] Some embodiments of the present invention for structure-based drug design comprise methods of identifying a chemical compound that complements the shape of an EphB4 receptor, particularly one that substantially conforms to the atomic coordinates of Table 1, or a structure that is related to an EphB4 receptor. Such method is referred to herein as a “geometric approach”. In a geometric approach of the present invention, the number of internal degrees of freedom (and the corresponding local minima in the molecular conformation space) can be reduced by considering only the geometric (hard-sphere) interactions of two rigid bodies, where one body (the active site) contains “pockets” or “grooves” that form binding sites for the second body (the complementing molecule, such as a ligand).
[0066] The geometric approach is described by Kuntz et al., J. Mol. Biol., vol. 161, p. 269, 1982, which is incorporated by this reference herein in its entirety. The algorithm for chemical compound design can be implemented using a software program such as AutoDock, available from the The Scripps Research Institute (La Jolla, Calif.). One or more extant databases of crystallographic data (e.g., the Cambridge Structural Database System maintained by University Chemical Laboratory, Cambridge University, Lensfield Road, Cambridge CB2 IEW, U.K. or the Protein Data Bank maintained by Rutgers University) can then be searched for chemical compounds that approximate the shape thus defined. Chemical compounds identified by the geometric approach can be modified to satisfy criteria associated with chemical complementarity, such as hydrogen bonding, ionic interactions or Van der Waals interactions.
[0067] In some embodiments, a therapeutic composition of the present invention can comprise one or more therapeutic compounds. A therapeutic composition can further comprise other compounds capable of inhibiting an EphB4 receptor. A therapeutic composition of the present invention can be used to treat disease in an animal such as, for example, a human in need of treatment by administering such composition to the human. Non-limiting examples of animals to treat include mammals, reptiles and birds, companion animals, food animals, zoo animals and other economically relevant animals (e.g., race horses and animals valued for their coats, such as minks). Additional animals to treat include dogs, cats, horses, cattle, sheep, swine, chickens, turkeys. Accordingly, in some aspects, animals to treat include humans.
[0068] A therapeutic composition of the present invention can also include an excipient, an adjuvant and/or carrier. Suitable excipients include compounds that the animal to be treated can tolerate. Examples of such excipients include water, saline, Ringer's solution, dextrose solution, Hank's solution, and other aqueous physiologically balanced salt solutions. Nonaqueous vehicles, such as fixed oils, sesame oil, ethyl oleate, or triglycerides may also be used. Other useful formulations include suspensions containing viscosity enhancing agents, such as sodium carboxymethylcellulose, sorbitol, or dextran. Excipients can also contain minor amounts of additives, such as substances that enhance isotonicity and chemical stability. Examples of buffers include phosphate buffer, bicarbonate buffer and Tris buffer, while examples of preservatives include thimerosal, o-cresol, formalin and benzyl alcohol. Standard formulations can either be liquid injectables or solids which can be taken up in a suitable liquid as a suspension or solution for injection. Thus, in a non-liquid formulation, the excipient can comprise dextrose, human serum albumin, preservatives, etc., to which sterile water or saline can be added prior to administration.
[0069] In one embodiment of the present invention, a therapeutic composition can include a carrier. Carriers include compounds that increase the half-life of a therapeutic composition in the treated animal. Suitable carriers include, but are not limited to, polymeric controlled release vehicles, biodegradable implants, liposomes, bacteria, viruses, other cells, oils, esters, and glycols.
[0070] Acceptable protocols to administer therapeutic compositions of the present invention in an effective manner include individual dose size, number of doses, frequency of dose administration, and mode of administration. Determination of such protocols can be accomplished by those skilled in the art. Modes of administration can include, but are not limited to, subcutaneous, intradermal, intravenous, intranasal, oral, transdermal, intraocular and intramuscular routes.
[0071] In yet another embodiment, a method is provided for crystallizing an EphB4 receptor which includes providing an EphB4 receptor in contact with a polypeptide having SEQ ID NO: 1, followed by contacting the EphB4 receptor in contact with the polypeptide with a therapeutic compound as provided above, wherein the EphB4 receptor in contact with the polypeptide and the compound forms an EphB4 receptor crystal.
[0072] In another embodiment, a composition is provided comprising EphB4 receptor, a ligand, and a therapeutic compound as provided above. The EphB4 receptor can be a polypeptide having SEQ ID NO: 2 or 3. The EphB4 receptor can also consist essentially of EphB4 D-E and J-K loops or Leu-48, Cys-61, Leu-95, Ser-99 Leu-100, Pro-101, Thr-147, Lys-149, Ala-155, and Cys-184 of SEQ ID NO: 6. In certain embodiments, the EphB4 receptor can be a human EphB4 receptor.
[0073] In certain embodiments, the ligand can be a polypeptide having SEQ ID NO: 7 and amino acids 120 through 127 of SEQ ID NO: 6. In other embodiments, the ligand can be a polypeptide having at least 50%, 75% or 90% sequence identity to a polypeptide selected from the group consisting of polypeptides having SEQ ID NO: 7 and amino acids 120 through 127 of SEQ ID NO: 6.
[0074] In some aspects, the present teachings include mutants of EphB4. In various configurations, these mutants can include at least one amino acid substitution, at least one amino acid addition, and/or at least one amino acid deletion. Such mutant EphB4 polypeptides and proteins can be constructed by methods well known to skilled artisans, such as site-directed mutagenesis. In some configurations, an EphB4 mutant can exhibit lower binding affinity (compared to wild type) for an EphB4 ligand such as EphrinB2, a TNYL-RAW peptide, or a labeled, e.g., fluorescently tagged, TNYL-RAW peptide. In some aspects, the binding affinity to an EphB4 ligand can be lower than that of wild type EphB4 (wtEphB4), without altering the binding specificity of the EphB4. Some non-limiting examples of EphB4 mutants of these aspects include T147F (i.e., threonine-147 to phenylalanine), K149Q (i.e., lysine-149 to glutamine), and A186S (i.e., alanine-186 to serine) as well as those found in FIG. 4 . Accordingly, the dynamic range of binding of an EphB4 ligand to a mutant EphB4 can be greater than that of binding of an EphB4 ligand to wtEphB4. In some configurations, the dynamic range can be greater than about 2-fold (i.e., the dynamic range for a wtEphB4-ligand binding assay), such as, without limitation, a 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, and 12-fold dynamic range.
[0075] In some aspects, a mutant EphB4 can be used in a screening assay for an EphB4 ligand, such as an EphB4 agonist or an EphB4 inhibitor. In a non-limiting example, an assay can comprise a fluorescence polarization (FP) assay using a fluorescent ligand such as a TNYL-RAW peptide labeled with a fluorophore such as Alexa-532 (Invitrogen). In various configurations, an assay can comprise contacting a complex comprising a mutant EphB4 and a fluorescent ligand with a candidate EphB4 ligand, and measuring a shift in the FP of the fluorescent ligand (Park, S. H., and Raines, R. T., Methods Mol. Biol. 261: 161-166, 2004). In some configurations, a mutant EphB4 can show a lower specificity to a ligand such as EphrinB2 or a fluorescent TNYL-RAW peptide. A shift in FP in such assays can indicate that a candidate EphB4 ligand binds to the EphB4. A compound identified by such a screening assay can be further tested, e.g., for pharmacological effectiveness and toxicity, using standard cell biological, biochemical and pharmacological tests well known to skilled artisans. Such assays can be used individually with candidate molecules, or at any scale of screening, such as, without limitation, high-throughput screening in which several thousand compounds can be rapidly tested for activity as ligands for EphB4.
TABLE 1 Protein Databank Coordinates of EphB4 Receptor Complexed ephrinB2 REMARK 3 PROGRAM: REFMAC 5.2.0019 REMARK 3 AUTHORS: MURSHUDOV, VAGIN, DODSON REMARK 3 REMARK 3 REFINEMENT TARGET: MAXIMUM LIKELIHOOD REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS): 1.91 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS): 36.27 REMARK 3 DATA CUTOFF (SIGMA(F)): NONE REMARK 3 COMPLETENESS FOR RANGE (%): 99.07 REMARK 3 NUMBER OF REFLECTIONS: 24232 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 CROSS-VALIDATION METHOD: THROUGHOUT REMARK 3 FREE R VALUE TEST SET SELECTION: RANDOM REMARK 3 R VALUE (WORKING + TEST SET): 0.26396 REMARK 3 R VALUE (WORKING SET): 0.26082 REMARK 3 FREE R VALUE: 0.32142 REMARK 3 FREE R VALUE TEST SET SIZE (%): 5.1 REMARK 3 FREE R VALUE TEST SET COUNT: 1304 REMARK 3 REMARK 3 FIT IN THE HIGHEST RESOLUTION BIN. REMARK 3 TOTAL NUMBER OF BINS USED: 20 REMARK 3 BIN RESOLUTION RANGE HIGH: 1.912 REMARK 3 BIN RESOLUTION RANGE LOW: 1.962 REMARK 3 REFLECTION IN BIN (WORKING SET): 1659 REMARK 3 BIN COMPLETENESS (WORKING + TEST) (%): 92.46 REMARK 3 BIN R VALUE (WORKING SET): 0.331 REMARK 3 BIN FREE R VALUE SET COUNT: 94 REMARK 3 BIN FREE R VALUE: 0.413 REMARK 3 REMARK 3 NUMBER OF NON-HYDROGEN ATOMS USED IN REFINEMENT. REMARK 3 ALL ATOMS: 2510 REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2): NULL REMARK 3 MEAN B VALUE (OVERALL, A**2): 46.363 REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2): −0.18 REMARK 3 B22 (A**2): −0.18 REMARK 3 B33 (A**2): 0.36 REMARK 3 B12 (A**2): 0.00 REMARK 3 B13 (A**2): 0.00 REMARK 3 B23 (A**2): 0.00 REMARK 3 REMARK 3 ESTIMATED OVERALL COORDINATE ERROR. REMARK 3 ESU BASED ON R VALUE (A): 0.214 REMARK 3 ESU BASED ON FREE R VALUE (A): 0.202 REMARK 3 ESU BASED ON MAXIMUM LIKELIHOOD (A): 0.220 REMARK 3 ESU FOR B VALUES BASED ON MAXIMUM LIKELIHOOD (A**2): 16.948 REMARK 3 REMARK 3 CORRELATION COEFFICIENTS. REMARK 3 CORRELATION COEFFICIENT FO-FC: 0.934 REMARK 3 CORRELATION COEFFICIENT FO-FC FREE: 0.893 REMARK 3 REMARK 3 RMS DEVIATIONS FROM IDEAL VALUES COUNT RMS WEIGHT REMARK 3 BOND LENGTHS REFINED ATOMS (A): 2577; 0.013; 0.022 REMARK 3 BOND ANGLES REFINED ATOMS (DEGREES): 3512; 1.579; 1.950 REMARK 3 TORSION ANGLES, PERIOD 1 (DEGREES): 323; 7.895; 5.000 REMARK 3 TORSION ANGLES, PERIOD 2 (DEGREES): 109; 37.322; 24.404 REMARK 3 TORSION ANGLES, PERIOD 3 (DEGREES): 406; 20.218; 15.000 REMARK 3 TORSION ANGLES, PERIOD 4 (DEGREES): 9; 14.327; 15.000 REMARK 3 CHIRAL-CENTER RESTRAINTS (A**3): 392; 0.103; 0.200 REMARK 3 GENERAL PLANES REFINED ATOMS (A): 1955; 0.006; 0.020 REMARK 3 NON-BONDED CONTACTS REFINED ATOMS (A): 976; 0.233; 0.200 REMARK 3 NON-BONDED TORSION REFINED ATOMS (A): 1665; 0.309; 0.200 REMARK 3 H-BOND (X . . . Y) REFINED ATOMS (A): 89; 0.168; 0.200 REMARK 3 SYMMETRY VDW REFINED ATOMS (A): 52; 0.228; 0.200 REMARK 3 SYMMETRY H-BOND REFINED ATOMS (A): 9; 0.218; 0.200 REMARK 3 REMARK 3 ISOTROPIC THERMAL FACTOR RESTRAINTS. COUNT RMS WEIGHT REMARK 3 MAIN-CHAIN BOND REFINED ATOMS (A**2): 1660; 2.151; 3.000 REMARK 3 MAIN-CHAIN ANGLE REFINED ATOMS (A**2): 2588; 3.180; 5.000 REMARK 3 SIDE-CHAIN BOND REFINED ATOMS (A**2): 1065; 4.640; 7.000 REMARK 3 SIDE-CHAIN ANGLE REFINED ATOMS (A**2): 924; 5.442; 9.000 REMARK 3 REMARK 3 NCS RESTRAINTS STATISTICS REMARK 3 NUMBER OF NCS GROUPS: NULL REMARK 3 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS: 2 REMARK 3 ATOM RECORD CONTAINS RESIDUAL B FACTORS ONLY REMARK 3 REMARK 3 TLS GROUP: 1 REMARK 3 NUMBER OF COMPONENTS GROUP: 1 REMARK 3 COMPONENTS C SSSEQI TO C SSSEQI REMARK 3 RESIDUE RANGE: A 9 A 196 REMARK 3 ORIGIN FOR THE GROUP (A): 6.5459 29.3924 −8.9085 REMARK 3 T TENSOR REMARK 3 T11: −0.0510 T22: −0.0163 REMARK 3 T33: 0.0412 T12: 0.0109 REMARK 3 T13: −0.0201 T23: 0.0639 REMARK 3 L TENSOR REMARK 3 L11: 1.0238 L22: 1.0652 REMARK 3 L33: 0.1402 L12: −0.0578 REMARK 3 L13: 0.0466 L23: 0.0816 REMARK 3 S TENSOR REMARK 3 S11: −0.0398 S12: 0.2633 S13: 0.0085 REMARK 3 S21: 0.0822 S22: 0.0447 S23: 0.2172 REMARK 3 S31: −0.0545 S32: 0.0708 S33: −0.0048 REMARK 3 REMARK 3 TLS GROUP: 2 REMARK 3 NUMBER OF COMPONENTS GROUP: 1 REMARK 3 COMPONENTS C SSSEQI TO C SSSEQI REMARK 3 RESIDUE RANGE: B 31 B 167 REMARK 3 ORIGIN FOR THE GROUP (A): 24.0838 25.2120 12.7894 REMARK 3 T TENSOR REMARK 3 T11: −0.0009 T22: −0.0420 REMARK 3 T33: −0.0654 T12: 0.0636 REMARK 3 T13: −0.0312 T23: 0.0420 REMARK 3 L TENSOR REMARK 3 L11: 1.3724 L22: 1.0673 REMARK 3 L33: 2.6076 L12: 0.8437 REMARK 3 L13: 1.4287 L23: 0.6393 REMARK 3 S TENSOR REMARK 3 S11: 0.1162 S12: 0.1266 S13: −0.1332 REMARK 3 S21: 0.2137 S22: 0.0292 S23: −0.0248 REMARK 3 S31: 0.1770 S32: 0.2825 S33: −0.1455 REMARK 3 REMARK 3 REMARK 3 BULK SOLVENT MODELLING. REMARK 3 METHOD USED: MASK REMARK 3 PARAMETERS FOR MASK CALCULATION REMARK 3 VDW PROBE RADIUS: 1.20 REMARK 3 ION PROBE RADIUS: 0.80 REMARK 3 SHRINKAGE RADIUS: 0.80 REMARK 3 REMARK 3 OTHER REFINEMENT REMARKS: REMARK 3 HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS REMARK 3 SSBOND 1 CYS A 61 CYS A 184 SSBOND 2 CYS A 97 CYS A 107 SSBOND 3 CYS B 65 CYS B 104 SSBOND 4 CYS B 92 CYS B 156 CISPEP 1 PHE A 35 PRO A 36 0.00 CISPEP 2 THR A 127 PRO A 128 0.00 CISPEP 3 ASN A 133 PRO A 134 0.00 CISPEP 4 GLY A 167 PRO A 168 0.00 CISPEP 5 ASP B 90 ARG B 91 0.00 CRYST1 81.085 81.085 50.945 90.00 90.00 90.00 P 41 SCALE1 0.012333 0.000000 0.000000 0.00000 SCALE2 0.000000 0.012333 0.000000 0.00000 SCALE3 0.000000 0.000000 0.019629 0.00000 ATOM 10 N HIS A 11 24.448 54.004 −27.877 1.00 49.00 N ATOM 11 CA HIS A 11 23.039 54.322 −27.723 1.00 47.86 C ATOM 12 CB HIS A 11 22.253 53.916 −28.974 1.00 48.48 C ATOM 13 CG HIS A 11 22.560 54.756 −30.174 1.00 46.99 C ATOM 14 ND1 HIS A 11 21.891 55.929 −30.454 1.00 47.84 N ATOM 15 CE1 HIS A 11 22.369 56.455 −31.566 1.00 44.85 C ATOM 16 NE2 HIS A 11 23.333 55.672 −32.016 1.00 48.34 N ATOM 17 CD2 HIS A 11 23.473 54.602 −31.163 1.00 49.20 C ATOM 18 C HIS A 11 22.494 53.661 −26.468 1.00 46.86 C ATOM 19 O HIS A 11 22.657 52.455 −26.254 1.00 46.50 O ATOM 20 N HIS A 12 21.858 54.459 −25.620 1.00 44.51 N ATOM 21 CA HIS A 12 21.462 53.973 −24.313 1.00 43.01 C ATOM 22 CB HIS A 12 22.056 54.854 −23.211 1.00 43.91 C ATOM 23 CG HIS A 12 23.320 54.305 −22.635 1.00 46.33 C ATOM 24 ND1 HIS A 12 23.372 53.706 −21.396 1.00 47.69 N ATOM 25 CE1 HIS A 12 24.605 53.299 −21.160 1.00 52.21 C ATOM 26 NE2 HIS A 12 25.351 53.602 −22.207 1.00 51.06 N ATOM 27 CD2 HIS A 12 24.569 54.227 −23.145 1.00 49.90 C ATOM 28 C HIS A 12 19.962 53.828 −24.139 1.00 40.46 C ATOM 29 O HIS A 12 19.191 54.727 −24.500 1.00 41.03 O ATOM 30 N HIS A 13 19.556 52.677 −23.624 1.00 39.88 N ATOM 31 CA HIS A 13 18.184 52.506 −23.152 1.00 39.98 C ATOM 32 CB HIS A 13 17.414 51.459 −23.973 1.00 39.69 C ATOM 33 CG HIS A 13 15.982 51.315 −23.562 1.00 40.91 C ATOM 34 ND1 HIS A 13 15.410 50.100 −23.255 1.00 43.46 N ATOM 35 CE1 HIS A 13 14.154 50.287 −22.890 1.00 36.43 C ATOM 36 NE2 HIS A 13 13.895 51.579 −22.942 1.00 39.44 N ATOM 37 CD2 HIS A 13 15.021 52.242 −23.359 1.00 38.36 C ATOM 38 C HIS A 13 18.174 52.172 −21.661 1.00 39.78 C ATOM 39 O HIS A 13 18.660 51.131 −21.228 1.00 38.65 O ATOM 40 N HIS A 14 17.617 53.068 −20.866 1.00 38.90 N ATOM 41 CA HIS A 14 17.507 52.802 −19.451 1.00 39.71 C ATOM 42 CB HIS A 14 17.974 54.017 −18.639 1.00 41.36 C ATOM 43 C HIS A 14 16.049 52.499 −19.153 1.00 40.66 C ATOM 44 O HIS A 14 15.159 53.220 −19.604 1.00 38.87 O ATOM 45 N HIS A 15 15.797 51.424 −18.419 1.00 37.90 N ATOM 46 CA HIS A 15 14.455 51.188 −17.913 1.00 39.77 C ATOM 47 CB HIS A 15 13.713 50.239 −18.844 1.00 38.53 C ATOM 48 CG HIS A 15 12.236 50.372 −18.753 1.00 36.65 C ATOM 49 ND1 HIS A 15 11.388 49.846 −19.698 1.00 36.72 N ATOM 50 CE1 HIS A 15 10.141 50.136 −19.372 1.00 37.69 C ATOM 51 NE2 HIS A 15 10.155 50.844 −18.256 1.00 36.35 N ATOM 52 CD2 HIS A 15 11.454 51.002 −17.845 1.00 37.33 C ATOM 53 C HIS A 15 14.438 50.663 −16.465 1.00 42.34 C ATOM 54 O HIS A 15 14.945 49.583 −16.197 1.00 45.21 O ATOM 55 N HIS A 16 13.877 51.449 −15.542 1.00 42.50 N ATOM 56 CA HIS A 16 13.849 51.102 −14.115 1.00 44.89 C ATOM 57 CB HIS A 16 13.544 52.349 −13.269 1.00 46.52 C ATOM 58 CG HIS A 16 14.588 53.417 −13.375 1.00 54.62 C ATOM 59 ND1 HIS A 16 14.398 54.577 −14.100 1.00 57.87 N ATOM 60 CE1 HIS A 16 15.486 55.323 −14.023 1.00 52.34 C ATOM 61 NE2 HIS A 16 16.378 54.684 −13.286 1.00 53.86 N ATOM 62 CD2 HIS A 16 15.843 53.488 −12.870 1.00 51.85 C ATOM 63 C HIS A 16 12.856 49.985 −13.768 1.00 44.45 C ATOM 64 O HIS A 16 11.720 50.017 −14.218 1.00 38.53 O ATOM 65 N GLU A 17 13.296 49.033 −12.940 1.00 43.15 N ATOM 66 CA GLU A 17 12.510 47.851 −12.579 1.00 45.72 C ATOM 67 CB GLU A 17 13.325 46.576 −12.794 1.00 46.52 C ATOM 68 CG GLU A 17 13.479 46.141 −14.242 1.00 45.21 C ATOM 69 CD GLU A 17 14.404 44.935 −14.428 1.00 48.39 C ATOM 70 OE1 GLU A 17 14.909 44.363 −13.436 1.00 53.51 O ATOM 71 OE2 GLU A 17 14.645 44.557 −15.587 1.00 49.07 O ATOM 72 C GLU A 17 12.077 47.943 −11.131 1.00 45.46 C ATOM 73 O GLU A 17 12.914 48.171 −10.252 1.00 47.09 O ATOM 74 N GLU A 18 10.775 47.812 −10.879 1.00 46.25 N ATOM 75 CA GLU A 18 10.287 47.795 −9.500 1.00 47.01 C ATOM 76 CB GLU A 18 9.270 48.907 −9.194 1.00 50.02 C ATOM 77 CG GLU A 18 9.553 49.578 −7.827 1.00 53.61 C ATOM 78 CD GLU A 18 8.322 50.164 −7.143 1.00 58.47 C ATOM 79 OE1 GLU A 18 7.339 49.415 −6.922 1.00 58.46 O ATOM 80 OE2 GLU A 18 8.356 51.370 −6.792 1.00 52.49 O ATOM 81 C GLU A 18 9.737 46.439 −9.101 1.00 45.25 C ATOM 82 O GLU A 18 8.859 45.885 −9.760 1.00 46.79 O ATOM 83 N THR A 19 10.265 45.937 −7.993 1.00 43.60 N ATOM 84 CA THR A 19 10.022 44.578 −7.547 1.00 40.92 C ATOM 85 CB THR A 19 11.154 44.128 −6.611 1.00 40.82 C ATOM 86 OG1 THR A 19 12.355 43.937 −7.372 1.00 46.16 O ATOM 87 CG2 THR A 19 10.790 42.835 −5.855 1.00 41.51 C ATOM 88 C THR A 19 8.719 44.532 −6.793 1.00 38.18 C ATOM 89 O THR A 19 8.506 45.332 −5.877 1.00 38.71 O ATOM 90 N LEU A 20 7.869 43.573 −7.155 1.00 35.11 N ATOM 91 CA LEU A 20 6.598 43.341 −6.454 1.00 35.09 C ATOM 92 CB LEU A 20 5.582 42.814 −7.455 1.00 32.21 C ATOM 93 CG LEU A 20 5.228 43.763 −8.593 1.00 42.07 C ATOM 94 CD1 LEU A 20 4.775 43.011 −9.829 1.00 41.64 C ATOM 95 CD2 LEU A 20 4.192 44.745 −8.158 1.00 31.95 C ATOM 96 C LEU A 20 6.783 42.315 −5.308 1.00 35.93 C ATOM 97 O LEU A 20 6.192 42.424 −4.227 1.00 39.65 O ATOM 98 N LEU A 21 7.647 41.347 −5.560 1.00 37.15 N ATOM 99 CA LEU A 21 7.866 40.212 −4.662 1.00 36.59 C ATOM 100 CB LEU A 21 6.704 39.210 −4.790 1.00 35.23 C ATOM 101 CG LEU A 21 6.824 37.819 −4.076 1.00 30.98 C ATOM 102 CD1 LEU A 21 7.141 37.996 −2.622 1.00 42.83 C ATOM 103 CD2 LEU A 21 5.549 37.070 −4.163 1.00 31.48 C ATOM 104 C LEU A 21 9.193 39.556 −5.034 1.00 37.39 C ATOM 105 O LEU A 21 9.445 39.256 −6.193 1.00 39.08 O ATOM 106 N ASN A 22 10.053 39.357 −4.050 1.00 39.54 N ATOM 107 CA ASN A 22 11.326 38.676 −4.273 1.00 40.39 C ATOM 108 CB ASN A 22 12.473 39.693 −4.295 1.00 36.59 C ATOM 109 CG ASN A 22 13.795 39.073 −4.663 1.00 42.16 C ATOM 110 OD1 ASN A 22 13.963 37.854 −4.578 1.00 37.60 O ATOM 111 ND2 ASN A 22 14.759 39.910 −5.068 1.00 32.02 N ATOM 112 C ASN A 22 11.525 37.720 −3.110 1.00 39.65 C ATOM 113 O ASN A 22 11.721 38.195 −1.992 1.00 40.60 O ATOM 114 N THR A 23 11.447 36.403 −3.362 1.00 43.19 N ATOM 115 CA THR A 23 11.631 35.394 −2.304 1.00 39.47 C ATOM 116 CB THR A 23 11.247 33.931 −2.746 1.00 39.83 C ATOM 117 OG1 THR A 23 12.103 33.496 −3.803 1.00 29.00 O ATOM 118 CG2 THR A 23 9.793 33.845 −3.201 1.00 37.70 C ATOM 119 C THR A 23 13.062 35.354 −1.755 1.00 41.75 C ATOM 120 O THR A 23 13.241 35.056 −0.571 1.00 39.34 O ATOM 121 N LYS A 24 14.058 35.605 −2.613 1.00 42.15 N ATOM 122 CA LYS A 24 15.497 35.577 −2.231 1.00 47.84 C ATOM 123 CB LYS A 24 16.430 35.906 −3.417 1.00 44.41 C ATOM 124 CG LYS A 24 16.713 34.791 −4.408 1.00 36.81 C ATOM 125 CD LYS A 24 17.426 35.348 −5.632 1.00 51.46 C ATOM 126 CE LYS A 24 16.468 36.179 −6.495 1.00 59.42 C ATOM 127 NZ LYS A 24 17.187 37.004 −7.498 1.00 60.14 N ATOM 128 C LYS A 24 15.843 36.550 −1.107 1.00 53.13 C ATOM 129 O LYS A 24 16.809 36.334 −0.372 1.00 57.22 O ATOM 130 N LEU A 25 15.069 37.619 −0.974 1.00 54.53 N ATOM 131 CA LEU A 25 15.320 38.588 0.085 1.00 59.86 C ATOM 132 CB LEU A 25 15.531 40.002 −0.491 1.00 60.08 C ATOM 133 CG LEU A 25 16.786 40.121 −1.390 1.00 60.60 C ATOM 134 CD1 LEU A 25 16.740 41.310 −2.344 1.00 63.05 C ATOM 135 CD2 LEU A 25 18.090 40.118 −0.596 1.00 66.00 C ATOM 136 C LEU A 25 14.269 38.521 1.205 1.00 62.83 C ATOM 137 O LEU A 25 13.371 39.363 1.295 1.00 65.96 O ATOM 138 N GLU A 26 14.417 37.481 2.034 1.00 63.60 N ATOM 139 CA GLU A 26 13.557 37.151 3.180 1.00 64.36 C ATOM 140 CB GLU A 26 12.164 36.740 2.703 1.00 65.26 C ATOM 141 CG GLU A 26 11.181 36.462 3.840 1.00 68.35 C ATOM 142 CD GLU A 26 10.195 35.365 3.503 1.00 69.03 C ATOM 143 OE1 GLU A 26 10.611 34.373 2.866 1.00 72.16 O ATOM 144 OE2 GLU A 26 9.006 35.483 3.885 1.00 70.04 O ATOM 145 C GLU A 26 14.182 35.967 3.926 1.00 62.58 C ATOM 146 O GLU A 26 14.503 34.958 3.303 1.00 61.58 O ATOM 147 N THR A 27 14.358 36.078 5.244 1.00 62.75 N ATOM 148 CA THR A 27 14.928 34.965 6.031 1.00 62.27 C ATOM 149 CB THR A 27 16.365 35.278 6.593 1.00 62.72 C ATOM 150 OG1 THR A 27 17.247 35.654 5.526 1.00 60.03 O ATOM 151 CG2 THR A 27 16.959 34.054 7.245 1.00 56.16 C ATOM 152 C THR A 27 13.979 34.389 7.117 1.00 62.81 C ATOM 153 O THR A 27 14.427 33.864 8.148 1.00 63.93 O ATOM 154 N ALA A 28 12.673 34.504 6.868 1.00 62.26 N ATOM 155 CA ALA A 28 11.630 33.803 7.634 1.00 60.61 C ATOM 156 CB ALA A 28 10.916 34.758 8.558 1.00 62.26 C ATOM 157 C ALA A 28 10.646 33.186 6.647 1.00 58.58 C ATOM 158 O ALA A 28 10.582 33.623 5.516 1.00 61.77 O ATOM 159 N ASP A 29 9.867 32.197 7.080 1.00 57.43 N ATOM 160 CA ASP A 29 9.059 31.336 6.188 1.00 51.76 C ATOM 161 CB ASP A 29 8.248 30.372 7.029 1.00 52.60 C ATOM 162 CG ASP A 29 9.024 29.852 8.206 1.00 54.73 C ATOM 163 OD1 ASP A 29 9.472 28.696 8.133 1.00 65.52 O ATOM 164 OD2 ASP A 29 9.221 30.597 9.195 1.00 57.50 O ATOM 165 C ASP A 29 8.133 32.114 5.268 1.00 48.96 C ATOM 166 O ASP A 29 7.583 33.121 5.686 1.00 50.09 O ATOM 167 N LEU A 30 7.954 31.637 4.027 1.00 44.57 N ATOM 168 CA LEU A 30 7.173 32.357 2.999 1.00 38.90 C ATOM 169 CB LEU A 30 7.469 31.824 1.593 1.00 33.40 C ATOM 170 CG LEU A 30 8.847 32.055 0.993 1.00 31.55 C ATOM 171 CD1 LEU A 30 9.081 30.975 −0.047 1.00 34.59 C ATOM 172 CD2 LEU A 30 8.873 33.455 0.382 1.00 35.00 C ATOM 173 C LEU A 30 5.692 32.186 3.288 1.00 37.96 C ATOM 174 O LEU A 30 4.886 33.060 2.968 1.00 38.81 O ATOM 175 N LYS A 31 5.352 31.042 3.872 1.00 36.60 N ATOM 176 CA LYS A 31 3.986 30.689 4.309 1.00 36.65 C ATOM 177 CB LYS A 31 3.524 31.555 5.506 1.00 38.57 C ATOM 178 CG LYS A 31 4.378 31.527 6.791 1.00 46.53 C ATOM 179 CD LYS A 31 4.249 30.238 7.593 1.00 57.30 C ATOM 180 CE LYS A 31 4.170 30.493 9.118 1.00 60.83 C ATOM 181 NZ LYS A 31 5.181 31.459 9.679 1.00 65.93 N ATOM 182 C LYS A 31 2.977 30.782 3.181 1.00 39.42 C ATOM 183 O LYS A 31 1.858 31.305 3.381 1.00 41.43 O ATOM 184 N TRP A 32 3.371 30.358 1.973 1.00 35.13 N ATOM 185 CA TRP A 32 2.453 30.416 0.834 1.00 33.15 C ATOM 186 CB TRP A 32 3.161 30.207 −0.500 1.00 28.95 C ATOM 187 CG TRP A 32 4.039 31.317 −0.919 1.00 34.75 C ATOM 188 CD1 TRP A 32 4.205 32.537 −0.312 1.00 33.11 C ATOM 189 NE1 TRP A 32 5.093 33.291 −1.021 1.00 29.19 N ATOM 190 CE2 TRP A 32 5.511 32.583 −2.117 1.00 31.35 C ATOM 191 CD2 TRP A 32 4.872 31.332 −2.081 1.00 32.07 C ATOM 192 CE3 TRP A 32 5.140 30.397 −3.090 1.00 28.33 C ATOM 193 CZ3 TRP A 32 6.044 30.747 −4.096 1.00 29.85 C ATOM 194 CH2 TRP A 32 6.681 32.008 −4.088 1.00 33.09 C ATOM 195 CZ2 TRP A 32 6.443 32.928 −3.108 1.00 29.70 C ATOM 196 C TRP A 32 1.381 29.360 1.045 1.00 34.03 C ATOM 197 O TRP A 32 1.475 28.597 1.979 1.00 31.83 O ATOM 198 N VAL A 33 0.387 29.316 0.166 1.00 36.83 N ATOM 199 CA VAL A 33 −0.813 28.472 0.377 1.00 34.51 C ATOM 200 CB VAL A 33 −2.075 29.329 0.158 1.00 39.47 C ATOM 201 CG1 VAL A 33 −3.367 28.480 0.048 1.00 38.42 C ATOM 202 CG2 VAL A 33 −2.180 30.345 1.283 1.00 29.62 C ATOM 203 C VAL A 33 −0.811 27.254 −0.516 1.00 35.90 C ATOM 204 O VAL A 33 −0.618 27.372 −1.721 1.00 35.14 O ATOM 205 N THR A 34 −1.031 26.075 0.077 1.00 36.36 N ATOM 206 CA THR A 34 −1.112 24.856 −0.726 1.00 36.51 C ATOM 207 CB THR A 34 −0.110 23.848 −0.259 1.00 29.05 C ATOM 208 OG1 THR A 34 −0.276 23.679 1.146 1.00 30.25 O ATOM 209 CG2 THR A 34 1.324 24.336 −0.559 1.00 36.15 C ATOM 210 C THR A 34 −2.504 24.202 −0.691 1.00 36.01 C ATOM 211 O THR A 34 −3.244 24.330 0.293 1.00 39.89 O ATOM 212 N PHE A 35 −2.836 23.508 −1.777 1.00 40.71 N ATOM 213 CA PHE A 35 −4.038 22.661 −1.865 1.00 37.31 C ATOM 214 CB PHE A 35 −5.242 23.488 −2.352 1.00 39.56 C ATOM 215 CG PHE A 35 −6.458 22.656 −2.745 1.00 31.37 C ATOM 216 CD1 PHE A 35 −7.425 22.323 −1.800 1.00 38.00 C ATOM 217 CE1 PHE A 35 −8.536 21.564 −2.155 1.00 34.26 C ATOM 218 CZ PHE A 35 −8.710 21.162 −3.467 1.00 41.72 C ATOM 219 CE2 PHE A 35 −7.770 21.507 −4.424 1.00 38.74 C ATOM 220 CD2 PHE A 35 −6.652 22.255 −4.061 1.00 37.81 C ATOM 221 C PHE A 35 −3.799 21.477 −2.807 1.00 38.54 C ATOM 222 O PHE A 35 −3.222 21.649 −3.876 1.00 41.98 O ATOM 223 N PRO A 36 −4.272 20.275 −2.435 1.00 36.71 N ATOM 224 CA PRO A 36 −4.947 19.954 −1.169 1.00 37.64 C ATOM 225 CB PRO A 36 −5.768 18.692 −1.504 1.00 39.48 C ATOM 226 CG PRO A 36 −5.523 18.410 −2.972 1.00 38.36 C ATOM 227 CD PRO A 36 −4.236 19.098 −3.318 1.00 40.07 C ATOM 228 C PRO A 36 −3.904 19.700 −0.087 1.00 40.22 C ATOM 229 O PRO A 36 −2.750 19.379 −0.420 1.00 41.14 O ATOM 230 N GLN A 37 −4.267 19.883 1.186 1.00 36.93 N ATOM 231 CA GLN A 37 −3.271 19.770 2.261 1.00 39.87 C ATOM 232 CB GLN A 37 −3.542 20.763 3.406 1.00 40.23 C ATOM 233 CG GLN A 37 −2.965 22.128 3.109 1.00 42.03 C ATOM 234 CD GLN A 37 −3.673 23.293 3.765 1.00 44.82 C ATOM 235 OE1 GLN A 37 −4.184 23.192 4.876 1.00 50.61 O ATOM 236 NE2 GLN A 37 −3.697 24.422 3.068 1.00 47.44 N ATOM 237 C GLN A 37 −3.103 18.329 2.732 1.00 41.85 C ATOM 238 O GLN A 37 −3.605 17.935 3.802 1.00 43.80 O ATOM 239 N VAL A 38 −2.413 17.550 1.889 1.00 40.81 N ATOM 240 CA VAL A 38 −2.108 16.133 2.121 1.00 40.56 C ATOM 241 CB VAL A 38 −2.824 15.199 1.098 1.00 44.60 C ATOM 242 CG1 VAL A 38 −4.312 15.348 1.189 1.00 41.50 C ATOM 243 CG2 VAL A 38 −2.366 15.498 −0.335 1.00 46.63 C ATOM 244 C VAL A 38 −0.623 15.866 1.983 1.00 40.11 C ATOM 245 O VAL A 38 0.122 16.692 1.460 1.00 33.72 O ATOM 246 N ASP A 39 −0.191 14.686 2.413 1.00 39.32 N ATOM 247 CA ASP A 39 1.187 14.302 2.188 1.00 39.86 C ATOM 248 CB ASP A 39 1.489 12.950 2.845 1.00 42.53 C ATOM 249 CG ASP A 39 2.889 12.892 3.446 1.00 54.40 C ATOM 250 OD1 ASP A 39 3.849 13.397 2.806 1.00 56.20 O ATOM 251 OD2 ASP A 39 3.032 12.338 4.564 1.00 62.34 O ATOM 252 C ASP A 39 1.494 14.312 0.682 1.00 38.22 C ATOM 253 O ASP A 39 0.734 13.790 −0.121 1.00 39.89 O ATOM 254 N GLY A 40 2.598 14.938 0.294 1.00 36.82 N ATOM 255 CA GLY A 40 2.906 15.094 −1.115 1.00 36.32 C ATOM 256 C GLY A 40 2.726 16.504 −1.637 1.00 36.89 C ATOM 257 O GLY A 40 3.230 16.826 −2.713 1.00 40.19 O ATOM 258 N GLN A 41 1.959 17.320 −0.910 1.00 34.90 N ATOM 259 CA GLN A 41 1.794 18.743 −1.202 1.00 31.38 C ATOM 260 CB GLN A 41 0.938 19.401 −0.098 1.00 34.79 C ATOM 261 CG GLN A 41 1.706 19.597 1.237 1.00 31.27 C ATOM 262 CD GLN A 41 0.855 19.958 2.420 1.00 32.64 C ATOM 263 OE1 GLN A 41 0.175 20.974 2.428 1.00 37.65 O ATOM 264 NE2 GLN A 41 0.921 19.135 3.456 1.00 36.27 N ATOM 265 C GLN A 41 3.165 19.451 −1.292 1.00 32.83 C ATOM 266 O GLN A 41 4.113 19.037 −0.633 1.00 30.94 O ATOM 267 N TRP A 42 3.246 20.579 −2.015 1.00 27.39 N ATOM 268 CA TRP A 42 4.499 21.331 −2.053 1.00 30.30 C ATOM 269 CB TRP A 42 4.362 22.691 −2.791 1.00 30.12 C ATOM 270 CG TRP A 42 4.056 22.655 −4.294 1.00 24.67 C ATOM 271 CD1 TRP A 42 2.866 22.342 −4.887 1.00 29.46 C ATOM 272 NE1 TRP A 42 2.993 22.421 −6.268 1.00 26.03 N ATOM 273 CE2 TRP A 42 4.270 22.836 −6.574 1.00 26.75 C ATOM 274 CD2 TRP A 42 4.969 22.988 −5.367 1.00 22.65 C ATOM 275 CE3 TRP A 42 6.310 23.374 −5.402 1.00 35.38 C ATOM 276 CZ3 TRP A 42 6.902 23.641 −6.633 1.00 25.44 C ATOM 277 CH2 TRP A 42 6.173 23.493 −7.821 1.00 33.53 C ATOM 278 CZ2 TRP A 42 4.838 23.106 −7.808 1.00 26.55 C ATOM 279 C TRP A 42 4.829 21.626 −0.614 1.00 25.05 C ATOM 280 O TRP A 42 3.940 21.655 0.198 1.00 26.88 O ATOM 281 N GLU A 43 6.102 21.934 −0.351 1.00 28.52 N ATOM 282 CA GLU A 43 6.648 22.065 0.960 1.00 28.30 C ATOM 283 CB GLU A 43 7.221 20.708 1.368 0.50 29.79 C ATOM 284 CG GLU A 43 7.855 20.711 2.685 0.50 27.80 C ATOM 285 CD GLU A 43 7.621 19.437 3.393 0.50 29.66 C ATOM 286 OE1 GLU A 43 7.052 19.510 4.485 0.50 28.25 O ATOM 287 OE2 GLU A 43 7.976 18.362 2.850 0.50 33.51 O ATOM 288 C GLU A 43 7.764 23.091 0.953 1.00 29.96 C ATOM 289 O GLU A 43 8.672 23.045 0.108 1.00 30.23 O ATOM 290 N GLU A 44 7.694 23.981 1.942 1.00 28.74 N ATOM 291 CA GLU A 44 8.696 24.984 2.273 1.00 32.50 C ATOM 292 CB GLU A 44 7.990 26.178 2.925 1.00 29.06 C ATOM 293 CG GLU A 44 8.921 27.058 3.729 1.00 42.19 C ATOM 294 CD GLU A 44 8.514 28.502 3.654 1.00 35.09 C ATOM 295 OE1 GLU A 44 7.329 28.813 3.928 1.00 45.10 O ATOM 296 OE2 GLU A 44 9.387 29.325 3.332 1.00 44.69 O ATOM 297 C GLU A 44 9.898 24.539 3.154 1.00 27.75 C ATOM 298 O GLU A 44 9.733 23.944 4.232 1.00 33.26 O ATOM 299 N LEU A 45 11.102 24.921 2.734 1.00 28.38 N ATOM 300 CA LEU A 45 12.330 24.400 3.255 1.00 33.31 C ATOM 301 CB LEU A 45 12.556 23.055 2.501 1.00 37.82 C ATOM 302 CG LEU A 45 13.623 21.985 2.685 1.00 45.75 C ATOM 303 CD1 LEU A 45 13.124 20.793 1.949 1.00 39.39 C ATOM 304 CD2 LEU A 45 14.894 22.391 2.058 1.00 47.39 C ATOM 305 C LEU A 45 13.422 25.417 2.902 1.00 32.67 C ATOM 306 O LEU A 45 13.383 26.031 1.850 1.00 31.80 O ATOM 307 N SER A 46 14.375 25.625 3.804 0.50 25.99 N ATOM 308 CA SER A 46 15.545 26.385 3.455 0.50 25.69 C ATOM 309 CB SER A 46 16.319 26.790 4.722 0.50 21.08 C ATOM 310 OG SER A 46 15.673 27.845 5.444 0.50 17.40 O ATOM 311 C SER A 46 16.411 25.501 2.538 0.50 25.37 C ATOM 312 O SER A 46 16.470 24.281 2.688 0.50 27.19 O ATOM 313 N GLY A 47 17.042 26.131 1.567 1.00 35.25 N ATOM 314 CA GLY A 47 18.069 25.515 0.770 1.00 37.20 C ATOM 315 C GLY A 47 19.112 26.509 0.272 1.00 40.71 C ATOM 316 O GLY A 47 19.031 27.723 0.479 1.00 37.07 O ATOM 317 N LEU A 48 20.083 25.974 −0.444 1.00 42.16 N ATOM 318 CA LEU A 48 21.090 26.788 −1.071 1.00 46.36 C ATOM 319 CB LEU A 48 22.472 26.147 −0.882 1.00 47.59 C ATOM 320 CG LEU A 48 23.420 26.858 0.095 1.00 46.13 C ATOM 321 CD1 LEU A 48 22.890 26.860 1.523 1.00 40.81 C ATOM 322 CD2 LEU A 48 24.840 26.268 0.015 1.00 45.26 C ATOM 323 C LEU A 48 20.769 26.947 −2.526 1.00 47.20 C ATOM 324 O LEU A 48 20.149 26.061 −3.134 1.00 47.47 O ATOM 325 N ASP A 49 21.135 28.103 −3.069 1.00 48.27 N ATOM 326 CA ASP A 49 21.056 28.332 −4.499 1.00 51.38 C ATOM 327 CB ASP A 49 20.188 29.567 −4.845 1.00 50.70 C ATOM 328 CG ASP A 49 20.680 30.869 −4.195 1.00 53.56 C ATOM 329 OD1 ASP A 49 21.425 30.828 −3.196 1.00 53.57 O ATOM 330 OD2 ASP A 49 20.299 31.962 −4.694 1.00 58.12 O ATOM 331 C ASP A 49 22.474 28.435 −5.069 1.00 52.11 C ATOM 332 O ASP A 49 23.446 28.314 −4.329 1.00 53.92 O ATOM 333 N GLU A 50 22.576 28.657 −6.375 1.00 54.51 N ATOM 334 CA GLU A 50 23.860 28.606 −7.063 1.00 56.83 C ATOM 335 CB GLU A 50 23.663 28.272 −8.543 1.00 57.48 C ATOM 336 CG GLU A 50 24.955 28.198 −9.341 1.00 58.63 C ATOM 337 CD GLU A 50 24.747 28.485 −10.815 1.00 63.28 C ATOM 338 OE1 GLU A 50 23.826 29.261 −11.147 1.00 62.81 O ATOM 339 OE2 GLU A 50 25.505 27.935 −11.641 1.00 64.02 O ATOM 340 C GLU A 50 24.615 29.924 −6.920 1.00 58.52 C ATOM 341 O GLU A 50 25.752 30.052 −7.375 1.00 58.64 O ATOM 342 N GLU A 51 24.016 30.884 −6.229 1.00 60.08 N ATOM 343 CA GLU A 51 24.755 32.014 −5.680 1.00 61.33 C ATOM 344 CB GLU A 51 23.862 33.246 −5.596 1.00 60.98 C ATOM 345 CG GLU A 51 24.093 34.229 −6.720 1.00 65.33 C ATOM 346 CD GLU A 51 25.552 34.338 −7.099 1.00 66.61 C ATOM 347 OE1 GLU A 51 26.153 33.321 −7.491 1.00 63.39 O ATOM 348 OE2 GLU A 51 26.100 35.448 −7.000 1.00 70.97 O ATOM 349 C GLU A 51 25.355 31.726 −4.313 1.00 60.91 C ATOM 350 O GLU A 51 26.225 32.444 −3.835 1.00 59.55 O ATOM 351 N GLN A 52 24.893 30.666 −3.681 1.00 60.48 N ATOM 352 CA GLN A 52 25.602 30.174 −2.532 1.00 60.49 C ATOM 353 CB GLN A 52 25.917 28.705 −2.692 1.00 61.75 C ATOM 354 C GLN A 52 24.854 30.424 −1.242 1.00 59.29 C ATOM 355 O GLN A 52 25.237 29.908 −0.197 1.00 60.10 O ATOM 356 N HIS A 53 23.804 31.235 −1.297 1.00 56.75 N ATOM 357 CA HIS A 53 23.253 31.737 −0.044 1.00 54.55 C ATOM 358 CB HIS A 53 23.006 33.245 −0.134 1.00 52.15 C ATOM 359 CG HIS A 53 24.232 34.039 −0.458 1.00 59.55 C ATOM 360 ND1 HIS A 53 24.213 35.409 −0.608 1.00 58.63 N ATOM 361 CE1 HIS A 53 25.431 35.837 −0.890 1.00 60.64 C ATOM 362 NE2 HIS A 53 26.239 34.793 −0.929 1.00 65.96 N ATOM 363 CD2 HIS A 53 25.515 33.657 −0.662 1.00 62.27 C ATOM 364 C HIS A 53 21.959 31.015 0.317 1.00 52.31 C ATOM 365 O HIS A 53 21.175 30.649 −0.558 1.00 50.31 O ATOM 366 N SER A 54 21.743 30.812 1.613 1.00 50.47 N ATOM 367 CA SER A 54 20.530 30.169 2.094 1.00 47.56 C ATOM 368 CB SER A 54 20.596 29.927 3.613 1.00 48.43 C ATOM 369 OG SER A 54 19.286 29.843 4.172 1.00 45.67 O ATOM 370 C SER A 54 19.287 30.986 1.758 1.00 45.87 C ATOM 371 O SER A 54 19.123 32.128 2.237 1.00 48.05 O ATOM 372 N VAL A 55 18.402 30.407 0.953 1.00 40.45 N ATOM 373 CA VAL A 55 17.105 31.085 0.673 1.00 39.01 C ATOM 374 CB VAL A 55 17.015 31.617 −0.788 1.00 36.82 C ATOM 375 CG1 VAL A 55 17.864 32.882 −0.951 1.00 44.80 C ATOM 376 CG2 VAL A 55 17.440 30.537 −1.781 1.00 37.51 C ATOM 377 C VAL A 55 15.919 30.179 1.016 1.00 34.20 C ATOM 378 O VAL A 55 16.091 28.989 1.260 1.00 37.43 O ATOM 379 N ARG A 56 14.731 30.761 1.043 1.00 31.69 N ATOM 380 CA ARG A 56 13.461 30.033 1.228 1.00 34.24 C ATOM 381 CB ARG A 56 12.380 31.019 1.670 1.00 34.51 C ATOM 382 CG ARG A 56 12.499 31.406 3.120 1.00 40.35 C ATOM 383 CD ARG A 56 11.870 30.286 3.920 1.00 42.68 C ATOM 384 NE ARG A 56 12.569 30.118 5.162 1.00 54.07 N ATOM 385 CZ ARG A 56 12.264 29.246 6.110 1.00 45.17 C ATOM 386 NH1 ARG A 56 11.208 28.431 6.026 1.00 32.64 N ATOM 387 NH2 ARG A 56 13.020 29.249 7.184 1.00 43.41 N ATOM 388 C ARG A 56 13.050 29.358 −0.068 1.00 36.72 C ATOM 389 O ARG A 56 12.933 30.049 −1.074 1.00 37.99 O ATOM 390 N THR A 57 12.898 28.028 −0.054 1.00 37.40 N ATOM 391 CA THR A 57 12.555 27.264 −1.269 1.00 36.12 C ATOM 392 CB THR A 57 13.657 26.239 −1.669 1.00 31.88 C ATOM 393 OG1 THR A 57 13.665 25.129 −0.746 1.00 32.23 O ATOM 394 CG2 THR A 57 15.055 26.937 −1.774 1.00 30.55 C ATOM 395 C THR A 57 11.198 26.536 −1.150 1.00 30.38 C ATOM 396 O THR A 57 10.690 26.366 −0.049 1.00 32.87 O ATOM 397 N TYR A 58 10.671 26.073 −2.281 1.00 29.60 N ATOM 398 CA TYR A 58 9.463 25.211 −2.336 1.00 25.84 C ATOM 399 CB TYR A 58 8.204 25.927 −2.875 1.00 33.81 C ATOM 400 CG TYR A 58 7.373 26.568 −1.769 1.00 32.75 C ATOM 401 CD1 TYR A 58 6.581 25.762 −0.919 1.00 36.07 C ATOM 402 CE1 TYR A 58 5.857 26.309 0.107 1.00 33.85 C ATOM 403 CZ TYR A 58 5.909 27.681 0.318 1.00 28.13 C ATOM 404 OH TYR A 58 5.143 28.196 1.340 1.00 39.16 O ATOM 405 CE2 TYR A 58 6.675 28.495 −0.494 1.00 32.86 C ATOM 406 CD2 TYR A 58 7.385 27.940 −1.549 1.00 30.61 C ATOM 407 C TYR A 58 9.759 23.931 −3.119 1.00 27.75 C ATOM 408 O TYR A 58 10.237 23.944 −4.251 1.00 30.30 O ATOM 409 N GLU A 59 9.493 22.808 −2.518 1.00 26.84 N ATOM 410 CA GLU A 59 9.743 21.517 −3.207 1.00 28.50 C ATOM 411 CB GLU A 59 10.734 20.698 −2.395 1.00 25.37 C ATOM 412 CG GLU A 59 12.194 21.194 −2.554 1.00 32.71 C ATOM 413 CD GLU A 59 13.169 20.434 −1.708 1.00 35.65 C ATOM 414 OE1 GLU A 59 12.752 19.458 −1.043 1.00 42.68 O ATOM 415 OE2 GLU A 59 14.373 20.788 −1.734 1.00 38.99 O ATOM 416 C GLU A 59 8.445 20.719 −3.429 1.00 29.63 C ATOM 417 O GLU A 59 7.573 20.699 −2.581 1.00 29.86 O ATOM 418 N VAL A 60 8.304 20.114 −4.597 1.00 32.15 N ATOM 419 CA VAL A 60 7.342 19.043 −4.786 1.00 28.58 C ATOM 420 CB VAL A 60 6.074 19.527 −5.482 1.00 30.98 C ATOM 421 CG1 VAL A 60 6.353 19.831 −6.910 1.00 23.51 C ATOM 422 CG2 VAL A 60 4.903 18.501 −5.270 1.00 28.38 C ATOM 423 C VAL A 60 8.023 17.825 −5.495 1.00 32.59 C ATOM 424 O VAL A 60 8.836 17.970 −6.418 1.00 31.84 O ATOM 425 N CYS A 61 7.706 16.628 −5.036 1.00 32.96 N ATOM 426 CA CYS A 61 8.172 15.412 −5.731 1.00 35.72 C ATOM 427 CB CYS A 61 9.667 15.181 −5.499 1.00 36.99 C ATOM 428 SG CYS A 61 10.357 13.789 −6.460 1.00 35.75 S ATOM 429 C CYS A 61 7.320 14.168 −5.440 1.00 39.90 C ATOM 430 O CYS A 61 7.784 13.212 −4.847 1.00 37.78 O ATOM 431 N ASP A 62 6.070 14.192 −5.902 1.00 42.20 N ATOM 432 CA ASP A 62 5.098 13.145 −5.583 1.00 46.74 C ATOM 433 CB ASP A 62 3.882 13.839 −4.937 1.00 44.78 C ATOM 434 CG ASP A 62 2.847 12.878 −4.360 1.00 47.88 C ATOM 435 OD1 ASP A 62 3.210 11.852 −3.750 1.00 41.91 O ATOM 436 OD2 ASP A 62 1.648 13.198 −4.502 1.00 40.24 O ATOM 437 C ASP A 62 4.748 12.325 −6.856 1.00 50.85 C ATOM 438 O ASP A 62 3.567 12.170 −7.223 1.00 49.30 O ATOM 439 N VAL A 63 5.792 11.771 −7.494 1.00 51.88 N ATOM 440 CA VAL A 63 5.747 11.308 −8.913 1.00 54.74 C ATOM 441 CB VAL A 63 7.166 11.296 −9.566 1.00 54.31 C ATOM 442 CG1 VAL A 63 7.692 12.700 −9.757 1.00 51.43 C ATOM 443 CG2 VAL A 63 8.139 10.455 −8.736 1.00 54.86 C ATOM 444 C VAL A 63 5.123 9.933 −9.169 1.00 59.46 C ATOM 445 O VAL A 63 4.803 9.596 −10.319 1.00 59.09 O ATOM 446 N GLN A 64 4.992 9.134 −8.108 1.00 62.97 N ATOM 447 CA GLN A 64 4.441 7.787 −8.205 1.00 67.89 C ATOM 448 CB GLN A 64 5.523 6.735 −7.964 1.00 69.08 C ATOM 449 C GLN A 64 3.331 7.600 −7.193 1.00 70.54 C ATOM 450 O GLN A 64 2.381 6.841 −7.433 1.00 71.49 O ATOM 451 N ARG A 65 3.469 8.300 −6.065 1.00 72.75 N ATOM 452 CA ARG A 65 2.538 8.217 −4.937 1.00 73.43 C ATOM 453 CB ARG A 65 3.107 8.979 −3.739 1.00 73.53 C ATOM 454 CG ARG A 65 4.643 8.994 −3.671 1.00 74.34 C ATOM 455 CD ARG A 65 5.151 9.895 −2.553 1.00 74.16 C ATOM 456 NE ARG A 65 6.539 9.612 −2.185 1.00 78.12 N ATOM 457 CZ ARG A 65 6.912 8.709 −1.276 1.00 81.38 C ATOM 458 NH1 ARG A 65 8.203 8.535 −1.008 1.00 81.84 N ATOM 459 NH2 ARG A 65 6.001 7.979 −0.630 1.00 80.28 N ATOM 460 C ARG A 65 1.175 8.781 −5.319 1.00 74.40 C ATOM 461 O ARG A 65 0.137 8.308 −4.848 1.00 75.23 O ATOM 462 N ALA A 66 1.187 9.752 −6.221 1.00 75.02 N ATOM 463 CA ALA A 66 −0.022 10.410 −6.687 1.00 75.51 C ATOM 464 CB ALA A 66 0.324 11.758 −7.268 1.00 74.75 C ATOM 465 C ALA A 66 −0.772 9.571 −7.719 1.00 76.66 C ATOM 466 O ALA A 66 −0.182 8.738 −8.406 1.00 75.96 O ATOM 467 N PRO A 67 −2.081 9.805 −7.831 1.00 76.02 N ATOM 468 CA PRO A 67 −2.860 9.213 −8.920 1.00 76.11 C ATOM 469 CB PRO A 67 −3.444 7.964 −8.264 1.00 76.99 C ATOM 470 CG PRO A 67 −3.465 8.286 −6.762 1.00 76.64 C ATOM 471 CD PRO A 67 −2.737 9.576 −6.533 1.00 75.96 C ATOM 472 C PRO A 67 −4.001 10.095 −9.427 1.00 73.84 C ATOM 473 O PRO A 67 −5.117 9.990 −8.927 1.00 74.12 O ATOM 474 N GLY A 68 −3.731 10.931 −10.422 1.00 71.47 N ATOM 475 CA GLY A 68 −4.781 11.685 −11.088 1.00 68.41 C ATOM 476 C GLY A 68 −4.893 13.125 −10.618 1.00 65.77 C ATOM 477 O GLY A 68 −5.894 13.791 −10.859 1.00 65.68 O ATOM 478 N GLN A 69 −3.854 13.607 −9.946 1.00 62.00 N ATOM 479 CA GLN A 69 −4.019 14.608 −8.911 1.00 58.03 C ATOM 480 CB GLN A 69 −3.807 13.999 −7.541 1.00 57.70 C ATOM 481 CG GLN A 69 −4.617 14.674 −6.473 1.00 60.32 C ATOM 482 CD GLN A 69 −3.768 15.263 −5.391 1.00 63.50 C ATOM 483 OE1 GLN A 69 −2.571 15.035 −5.343 1.00 69.20 O ATOM 484 NE2 GLN A 69 −4.383 16.027 −4.509 1.00 64.13 N ATOM 485 C GLN A 69 −3.103 15.810 −9.075 1.00 54.71 C ATOM 486 O GLN A 69 −2.022 15.710 −9.640 1.00 52.38 O ATOM 487 N ALA A 70 −3.554 16.948 −8.567 1.00 50.26 N ATOM 488 CA ALA A 70 −2.866 18.217 −8.769 1.00 45.28 C ATOM 489 CB ALA A 70 −3.709 19.146 −9.653 1.00 46.12 C ATOM 490 C ALA A 70 −2.513 18.911 −7.461 1.00 40.85 C ATOM 491 O ALA A 70 −3.392 19.227 −6.667 1.00 40.28 O ATOM 492 N HIS A 71 −1.226 19.190 −7.258 1.00 38.57 N ATOM 493 CA HIS A 71 −0.776 19.932 −6.072 1.00 34.83 C ATOM 494 CB HIS A 71 0.567 19.415 −5.531 1.00 33.42 C ATOM 495 CG HIS A 71 0.567 17.965 −5.101 1.00 36.67 C ATOM 496 ND1 HIS A 71 −0.248 17.483 −4.094 1.00 42.49 N ATOM 497 CE1 HIS A 71 −0.032 16.189 −3.928 1.00 37.72 C ATOM 498 NE2 HIS A 71 0.924 15.816 −4.764 1.00 35.72 N ATOM 499 CD2 HIS A 71 1.314 16.912 −5.507 1.00 40.69 C ATOM 500 C HIS A 71 −0.633 21.421 −6.445 1.00 36.72 C ATOM 501 O HIS A 71 0.255 21.811 −7.240 1.00 30.07 O ATOM 502 N TRP A 72 −1.458 22.244 −5.819 1.00 35.14 N ATOM 503 CA TRP A 72 −1.437 23.690 −6.072 1.00 34.04 C ATOM 504 CB TRP A 72 −2.853 24.250 −6.076 1.00 35.63 C ATOM 505 CG TRP A 72 −3.670 23.874 −7.269 1.00 30.19 C ATOM 506 CD1 TRP A 72 −4.373 22.721 −7.443 1.00 37.72 C ATOM 507 NE1 TRP A 72 −4.994 22.715 −8.654 1.00 37.02 N ATOM 508 CE2 TRP A 72 −4.722 23.892 −9.300 1.00 41.37 C ATOM 509 CD2 TRP A 72 −3.877 24.648 −8.455 1.00 43.82 C ATOM 510 CE3 TRP A 72 −3.443 25.912 −8.885 1.00 41.53 C ATOM 511 CZ3 TRP A 72 −3.857 26.370 −10.124 1.00 37.00 C ATOM 512 CH2 TRP A 72 −4.701 25.594 −10.945 1.00 37.71 C ATOM 513 CZ2 TRP A 72 −5.139 24.352 −10.549 1.00 45.05 C ATOM 514 C TRP A 72 −0.591 24.390 −5.020 1.00 32.97 C ATOM 515 O TRP A 72 −0.574 23.956 −3.862 1.00 30.07 C ATOM 516 N LEU A 73 0.198 25.379 −5.463 1.00 29.15 N ATOM 517 CA LEU A 73 0.924 26.326 −4.587 1.00 28.01 C ATOM 518 CB LEU A 73 2.450 26.140 −4.720 1.00 24.79 C ATOM 519 CG LEU A 73 3.354 27.007 −3.870 1.00 28.60 C ATOM 520 CD1 LEU A 73 3.116 26.818 −2.389 1.00 28.15 C ATOM 521 CD2 LEU A 73 4.848 26.781 −4.220 1.00 30.48 C ATOM 522 C LEU A 73 0.587 27.771 −4.989 1.00 28.82 C ATOM 523 O LEU A 73 0.741 28.143 −6.166 1.00 32.47 O ATOM 524 N ARG A 74 0.229 28.601 −4.016 1.00 26.25 N ATOM 525 CA ARG A 74 −0.171 29.997 −4.349 1.00 31.34 C ATOM 526 CB ARG A 74 −1.692 30.180 −4.242 1.00 32.48 C ATOM 527 CG ARG A 74 −2.258 31.453 −4.942 1.00 30.02 C ATOM 528 CD ARG A 74 −3.720 31.633 −4.574 1.00 36.24 C ATOM 529 NE ARG A 74 −3.803 31.821 −3.132 1.00 39.56 N ATOM 530 CZ ARG A 74 −4.863 31.571 −2.383 1.00 40.38 C ATOM 531 NH1 ARG A 74 −6.001 31.116 −2.916 1.00 38.53 N ATOM 532 NH2 ARG A 74 −4.767 31.798 −1.085 1.00 37.96 N ATOM 533 C ARG A 74 0.553 31.020 −3.470 1.00 31.04 C ATOM 534 O ARG A 74 0.638 30.847 −2.258 1.00 32.22 O ATOM 535 N THR A 75 1.075 32.077 −4.084 1.00 33.16 N ATOM 536 CA THR A 75 1.679 33.193 −3.289 1.00 34.65 C ATOM 537 CB THR A 75 2.319 34.284 −4.147 1.00 34.94 C ATOM 538 OG1 THR A 75 1.299 34.906 −4.943 1.00 31.24 O ATOM 539 CG2 THR A 75 3.385 33.710 −5.035 1.00 38.97 C ATOM 540 C THR A 75 0.649 33.872 −2.415 1.00 32.75 C ATOM 541 O THR A 75 −0.566 33.639 −2.562 1.00 30.37 O ATOM 542 N GLY A 76 1.134 34.708 −1.493 1.00 36.03 N ATOM 543 CA GLY A 76 0.280 35.638 −0.751 1.00 34.99 C ATOM 544 C GLY A 76 −0.168 36.709 −1.711 1.00 34.57 C ATOM 545 O GLY A 76 0.262 36.700 −2.865 1.00 35.49 O ATOM 546 N TRP A 77 −1.032 37.612 −1.238 1.00 32.47 N ATOM 547 CA TRP A 77 −1.626 38.650 −2.085 1.00 34.91 C ATOM 548 CB TRP A 77 −2.565 39.510 −1.255 1.00 33.83 C ATOM 549 CG TRP A 77 −3.507 40.357 −2.092 1.00 38.76 C ATOM 550 CD1 TRP A 77 −4.293 39.951 −3.139 1.00 36.42 C ATOM 551 NE1 TRP A 77 −4.986 41.040 −3.659 1.00 35.07 N ATOM 552 CE2 TRP A 77 −4.662 42.153 −2.933 1.00 38.58 C ATOM 553 CD2 TRP A 77 −3.735 41.760 −1.937 1.00 42.72 C ATOM 554 CE3 TRP A 77 −3.244 42.726 −1.047 1.00 45.06 C ATOM 555 CZ3 TRP A 77 −3.675 44.034 −1.182 1.00 37.42 C ATOM 556 CH2 TRP A 77 −4.611 44.396 −2.177 1.00 39.82 C ATOM 557 CZ2 TRP A 77 −5.117 43.471 −3.055 1.00 41.18 C ATOM 558 C TRP A 77 −0.528 39.545 −2.587 1.00 34.98 C ATOM 559 O TRP A 77 0.240 40.023 −1.792 1.00 35.74 O ATOM 560 N VAL A 78 −0.450 39.804 −3.888 1.00 38.30 N ATOM 561 CA VAL A 78 0.580 40.746 −4.342 1.00 39.04 C ATOM 562 CB VAL A 78 1.558 40.141 −5.392 1.00 39.37 C ATOM 563 CG1 VAL A 78 2.797 41.050 −5.563 1.00 39.09 C ATOM 564 CG2 VAL A 78 1.994 38.700 −4.983 1.00 33.31 C ATOM 565 C VAL A 78 −0.020 42.079 −4.854 1.00 42.68 C ATOM 566 O VAL A 78 −0.694 42.105 −5.910 1.00 41.94 O ATOM 567 N PRO A 79 0.235 43.176 −4.110 1.00 42.96 N ATOM 568 CA PRO A 79 −0.097 44.504 −4.588 1.00 46.35 C ATOM 569 CB PRO A 79 0.378 45.420 −3.449 1.00 44.48 C ATOM 570 CG PRO A 79 0.432 44.527 −2.236 1.00 38.83 C ATOM 571 CD PRO A 79 0.876 43.222 −2.777 1.00 41.53 C ATOM 572 C PRO A 79 0.611 44.806 −5.934 1.00 49.47 C ATOM 573 O PRO A 79 1.832 44.949 −6.009 1.00 51.20 O ATOM 574 N ARG A 80 −0.183 44.829 −6.997 1.00 53.14 N ATOM 575 CA ARG A 80 0.249 45.329 −8.281 1.00 54.18 C ATOM 576 CB ARG A 80 −0.769 44.923 −9.340 1.00 55.34 C ATOM 577 CG ARG A 80 −0.888 45.833 −10.533 1.00 51.62 C ATOM 578 CD ARG A 80 −2.346 45.943 −10.982 1.00 47.92 C ATOM 579 NE ARG A 80 −3.010 47.189 −10.538 1.00 43.68 N ATOM 580 CZ ARG A 80 −2.977 48.363 −11.174 1.00 53.21 C ATOM 581 NH1 ARG A 80 −2.282 48.541 −12.304 1.00 48.15 N ATOM 582 NH2 ARG A 80 −3.642 49.389 −10.660 1.00 50.73 N ATOM 583 C ARG A 80 0.281 46.825 −8.058 1.00 56.38 C ATOM 584 O ARG A 80 −0.765 47.478 −8.004 1.00 57.66 O ATOM 585 N ARG A 81 1.476 47.362 −7.852 1.00 57.34 N ATOM 586 CA ARG A 81 1.607 48.768 −7.490 1.00 58.23 C ATOM 587 CB ARG A 81 3.054 49.083 −7.124 1.00 58.75 C ATOM 588 CG ARG A 81 3.430 48.515 −5.765 1.00 57.81 C ATOM 589 CD ARG A 81 4.811 47.914 −5.769 1.00 65.79 C ATOM 590 NE ARG A 81 4.846 46.682 −4.989 1.00 69.25 N ATOM 591 CZ ARG A 81 5.910 46.228 −4.334 1.00 71.96 C ATOM 592 NH1 ARG A 81 7.049 46.912 −4.349 1.00 73.08 N ATOM 593 NH2 ARG A 81 5.830 45.086 −3.655 1.00 75.90 N ATOM 594 C ARG A 81 1.057 49.687 −8.584 1.00 59.36 C ATOM 595 O ARG A 81 −0.012 50.285 −8.418 1.00 60.97 O ATOM 596 N GLY A 82 1.775 49.786 −9.698 1.00 57.47 N ATOM 597 CA GLY A 82 1.291 50.512 −10.849 1.00 56.99 C ATOM 598 C GLY A 82 1.528 49.695 −12.092 1.00 56.65 C ATOM 599 O GLY A 82 1.475 50.219 −13.206 1.00 56.18 O ATOM 600 N ALA A 83 1.801 48.407 −11.892 1.00 55.51 N ATOM 601 CA ALA A 83 2.078 47.474 −12.984 1.00 55.06 C ATOM 602 CB ALA A 83 2.622 46.159 −12.439 1.00 53.08 C ATOM 603 C ALA A 83 0.877 47.208 −13.868 1.00 54.91 C ATOM 604 O ALA A 83 −0.272 47.183 −13.416 1.00 56.83 O ATOM 605 N VAL A 84 1.156 46.989 −15.140 1.00 55.31 N ATOM 606 CA VAL A 84 0.123 46.541 −16.053 1.00 56.06 C ATOM 607 CB VAL A 84 −0.135 47.546 −17.203 1.00 56.51 C ATOM 608 CG1 VAL A 84 −0.933 46.892 −18.338 1.00 54.38 C ATOM 609 CG2 VAL A 84 −0.863 48.773 −16.661 1.00 51.88 C ATOM 610 C VAL A 84 0.555 45.187 −16.569 1.00 56.01 C ATOM 611 O VAL A 84 −0.244 44.242 −16.603 1.00 57.12 O ATOM 612 N HIS A 85 1.818 45.103 −16.965 1.00 52.37 N ATOM 613 CA HIS A 85 2.404 43.814 −17.268 1.00 52.72 C ATOM 614 CB HIS A 85 2.900 43.727 −18.711 1.00 52.43 C ATOM 615 CG HIS A 85 1.810 43.911 −19.713 1.00 54.23 C ATOM 616 ND1 HIS A 85 1.059 42.864 −20.195 1.00 50.36 N ATOM 617 CE1 HIS A 85 0.154 43.327 −21.038 1.00 53.21 C ATOM 618 NE2 HIS A 85 0.284 44.639 −21.109 1.00 54.30 N ATOM 619 CD2 HIS A 85 1.308 45.031 −20.283 1.00 52.00 C ATOM 620 C HIS A 85 3.485 43.516 −16.267 1.00 49.96 C ATOM 621 O HIS A 85 4.397 44.310 −16.049 1.00 51.17 O ATOM 622 N VAL A 86 3.332 42.366 −15.630 1.00 47.91 N ATOM 623 CA VAL A 86 4.242 41.911 −14.610 1.00 47.10 C ATOM 624 CB VAL A 86 3.431 41.339 −13.414 1.00 49.81 C ATOM 625 CG1 VAL A 86 4.221 40.335 −12.580 1.00 46.34 C ATOM 626 CG2 VAL A 86 2.883 42.469 −12.557 1.00 49.43 C ATOM 627 C VAL A 86 5.190 40.892 −15.246 1.00 43.83 C ATOM 628 O VAL A 86 4.804 40.171 −16.172 1.00 42.11 O ATOM 629 N TYR A 87 6.438 40.879 −14.781 1.00 39.95 N ATOM 630 CA TYR A 87 7.384 39.865 −15.203 1.00 37.91 C ATOM 631 CB TYR A 87 8.724 40.475 −15.541 1.00 35.88 C ATOM 632 CG TYR A 87 8.811 41.281 −16.830 1.00 42.37 C ATOM 633 CD1 TYR A 87 9.646 40.873 −17.871 1.00 44.12 C ATOM 634 CE1 TYR A 87 9.779 41.618 −19.021 1.00 47.12 C ATOM 635 CZ TYR A 87 9.074 42.791 −19.142 1.00 39.76 C ATOM 636 OH TYR A 87 9.179 43.539 −20.295 1.00 50.68 O ATOM 637 CE2 TYR A 87 8.238 43.218 −18.129 1.00 35.52 C ATOM 638 CD2 TYR A 87 8.134 42.478 −16.972 1.00 42.43 C ATOM 639 C TYR A 87 7.576 38.915 −14.037 1.00 31.73 C ATOM 640 O TYR A 87 7.516 39.330 −12.899 1.00 32.92 O ATOM 641 N ALA A 88 7.833 37.653 −14.327 1.00 35.28 N ATOM 642 CA ALA A 88 7.884 36.654 −13.274 1.00 35.57 C ATOM 643 CB ALA A 88 6.521 35.941 −13.123 1.00 35.79 C ATOM 644 C ALA A 88 8.986 35.707 −13.607 1.00 35.70 C ATOM 645 O ALA A 88 8.839 34.833 −14.436 1.00 37.89 O ATOM 646 N THR A 89 10.126 35.931 −12.958 1.00 39.19 N ATOM 647 CA THR A 89 11.313 35.161 −13.225 1.00 38.72 C ATOM 648 CB THR A 89 12.560 36.058 −13.114 1.00 41.64 C ATOM 649 OG1 THR A 89 12.479 37.065 −14.125 1.00 39.96 O ATOM 650 CG2 THR A 89 13.850 35.262 −13.291 1.00 40.09 C ATOM 651 C THR A 89 11.350 34.037 −12.208 1.00 38.27 C ATOM 652 O THR A 89 11.327 34.284 −11.016 1.00 36.78 O ATOM 653 N LEU A 90 11.391 32.810 −12.712 1.00 41.20 N ATOM 654 CA LEU A 90 11.473 31.597 −11.899 1.00 37.67 C ATOM 655 CB LEU A 90 10.400 30.599 −12.345 1.00 35.91 C ATOM 656 CG LEU A 90 8.978 31.122 −12.557 1.00 42.98 C ATOM 657 CD1 LEU A 90 8.040 30.101 −13.249 1.00 37.76 C ATOM 658 CD2 LEU A 90 8.416 31.577 −11.249 1.00 37.89 C ATOM 659 C LEU A 90 12.845 30.939 −12.031 1.00 35.29 C ATOM 660 O LEU A 90 13.357 30.750 −13.129 1.00 34.84 O ATOM 661 N ARG A 91 13.414 30.524 −10.908 1.00 32.23 N ATOM 662 CA ARG A 91 14.578 29.704 −10.970 1.00 31.68 C ATOM 663 CB ARG A 91 15.729 30.367 −10.213 1.00 29.26 C ATOM 664 CG ARG A 91 16.186 31.702 −10.714 1.00 39.83 C ATOM 665 CD ARG A 91 17.422 32.123 −9.918 1.00 48.82 C ATOM 666 NE ARG A 91 18.182 33.162 −10.597 1.00 48.28 N ATOM 667 CZ ARG A 91 19.207 32.929 −11.415 1.00 54.96 C ATOM 668 NH1 ARG A 91 19.832 33.957 −11.994 1.00 48.94 N ATOM 669 NH2 ARG A 91 19.607 31.674 −11.657 1.00 41.81 N ATOM 670 C ARG A 91 14.230 28.388 −10.333 1.00 29.39 C ATOM 671 O ARG A 91 13.650 28.379 −9.267 1.00 30.64 O ATOM 672 N PHE A 92 14.603 27.283 −10.965 1.00 29.19 N ATOM 673 CA PHE A 92 14.179 25.976 −10.483 1.00 28.13 C ATOM 674 CB PHE A 92 12.672 25.695 −10.853 1.00 25.35 C ATOM 675 CG PHE A 92 12.392 25.582 −12.330 1.00 31.38 C ATOM 676 CD1 PHE A 92 12.298 24.318 −12.957 1.00 30.18 C ATOM 677 CE1 PHE A 92 12.057 24.206 −14.311 1.00 29.16 C ATOM 678 CZ PHE A 92 11.846 25.370 −15.072 1.00 39.78 C ATOM 679 CE2 PHE A 92 11.894 26.646 −14.463 1.00 28.29 C ATOM 680 CD2 PHE A 92 12.161 26.743 −13.098 1.00 36.30 C ATOM 681 C PHE A 92 15.075 24.896 −10.979 1.00 28.40 C ATOM 682 O PHE A 92 15.770 25.050 −11.991 1.00 33.15 O ATOM 683 N THR A 93 15.024 23.775 −10.304 1.00 28.13 N ATOM 684 CA THR A 93 15.649 22.555 −10.797 1.00 32.26 C ATOM 685 CB THR A 93 16.770 22.043 −9.843 0.50 30.79 C ATOM 686 OG1 THR A 93 16.238 21.847 −8.539 0.50 24.15 O ATOM 687 CG2 THR A 93 17.892 23.084 −9.725 0.50 28.99 C ATOM 688 C THR A 93 14.528 21.525 −11.044 1.00 35.09 C ATOM 689 O THR A 93 13.461 21.541 −10.390 1.00 37.83 O ATOM 690 N MET A 94 14.748 20.661 −12.022 1.00 37.88 N ATOM 691 CA MET A 94 13.738 19.691 −12.440 1.00 34.08 C ATOM 692 CB MET A 94 13.082 20.163 −13.741 1.00 37.68 C ATOM 693 CG MET A 94 12.132 19.187 −14.384 1.00 31.33 C ATOM 694 SD MET A 94 10.563 19.099 −13.517 1.00 37.28 S ATOM 695 CE MET A 94 10.084 20.829 −13.643 1.00 24.37 C ATOM 696 C MET A 94 14.466 18.376 −12.660 1.00 37.15 C ATOM 697 O MET A 94 15.519 18.350 −13.326 1.00 37.61 O ATOM 698 N LEU A 95 13.968 17.313 −12.049 1.00 32.63 N ATOM 699 CA LEU A 95 14.611 16.001 −12.199 1.00 36.65 C ATOM 700 CB LEU A 95 14.500 15.178 −10.912 1.00 35.07 C ATOM 701 CG LEU A 95 15.630 15.458 −9.894 1.00 40.28 C ATOM 702 CD1 LEU A 95 15.447 16.766 −9.120 1.00 39.97 C ATOM 703 CD2 LEU A 95 15.799 14.331 −8.946 1.00 41.34 C ATOM 704 C LEU A 95 14.126 15.196 −13.401 1.00 37.05 C ATOM 705 O LEU A 95 12.951 15.165 −13.680 1.00 38.21 O ATOM 706 N GLU A 96 15.064 14.546 −14.093 1.00 40.05 N ATOM 707 CA GLU A 96 14.788 13.649 −15.213 1.00 39.08 C ATOM 708 CB GLU A 96 16.103 13.106 −15.779 1.00 40.73 C ATOM 709 CG GLU A 96 15.936 12.029 −16.850 1.00 41.96 C ATOM 710 CD GLU A 96 17.259 11.583 −17.456 1.00 43.00 C ATOM 711 OE1 GLU A 96 18.244 11.364 −16.718 1.00 46.73 O ATOM 712 OE2 GLU A 96 17.299 11.443 −18.693 1.00 54.87 O ATOM 713 C GLU A 96 13.931 12.497 −14.738 1.00 38.39 C ATOM 714 O GLU A 96 14.320 11.774 −13.818 1.00 40.49 O ATOM 715 N CYS A 97 12.764 12.313 −15.372 1.00 40.12 N ATOM 716 CA CYS A 97 11.810 11.294 −14.934 1.00 39.96 C ATOM 717 CB CYS A 97 10.527 11.350 −15.772 1.00 43.34 C ATOM 718 SG CYS A 97 9.358 12.560 −15.204 1.00 46.32 S ATOM 719 C CYS A 97 12.397 9.893 −14.973 1.00 41.63 C ATOM 720 O CYS A 97 12.295 9.135 −13.992 1.00 41.45 O ATOM 721 N LEU A 98 13.045 9.563 −16.089 1.00 45.11 N ATOM 722 CA LEU A 98 13.628 8.226 −16.258 1.00 49.04 C ATOM 723 CB LEU A 98 13.860 7.892 −17.743 1.00 51.09 C ATOM 724 CG LEU A 98 12.548 7.587 −18.510 1.00 51.68 C ATOM 725 CD1 LEU A 98 12.708 7.541 −20.017 1.00 49.01 C ATOM 726 CD2 LEU A 98 11.843 6.315 −18.019 1.00 57.57 C ATOM 727 C LEU A 98 14.859 7.951 −15.405 1.00 49.53 C ATOM 728 O LEU A 98 15.338 6.828 −15.373 1.00 47.03 O ATOM 729 N SER A 99 15.338 8.969 −14.688 1.00 52.06 N ATOM 730 CA SER A 99 16.509 8.844 −13.803 1.00 53.05 C ATOM 731 CB SER A 99 17.356 10.125 −13.826 1.00 53.42 C ATOM 732 OG SER A 99 16.784 11.140 −12.992 1.00 59.05 O ATOM 733 C SER A 99 16.081 8.591 −12.366 1.00 55.03 C ATOM 734 O SER A 99 16.879 8.135 −11.542 1.00 53.98 O ATOM 735 N LEU A 100 14.828 8.926 −12.060 1.00 57.16 N ATOM 736 CA LEU A 100 14.355 8.903 −10.689 1.00 58.91 C ATOM 737 CB LEU A 100 13.036 9.658 −10.554 1.00 57.21 C ATOM 738 CG LEU A 100 12.907 11.112 −10.971 1.00 51.47 C ATOM 739 CD1 LEU A 100 11.448 11.472 −10.926 1.00 45.58 C ATOM 740 CD2 LEU A 100 13.689 12.003 −10.050 1.00 48.85 C ATOM 741 C LEU A 100 14.147 7.471 −10.250 1.00 63.37 C ATOM 742 O LEU A 100 13.775 6.629 −11.062 1.00 63.99 O ATOM 743 N PRO A 101 14.391 7.187 −8.960 1.00 66.45 N ATOM 744 CA PRO A 101 13.936 5.891 −8.477 1.00 67.84 C ATOM 745 CB PRO A 101 14.775 5.656 −7.218 1.00 68.56 C ATOM 746 CG PRO A 101 15.326 7.009 −6.814 1.00 68.23 C ATOM 747 CD PRO A 101 15.054 7.995 −7.916 1.00 66.48 C ATOM 748 C PRO A 101 12.440 5.954 −8.161 1.00 69.98 C ATOM 749 O PRO A 101 11.956 6.967 −7.632 1.00 72.74 O ATOM 750 N ARG A 102 11.721 4.899 −8.540 1.00 69.84 N ATOM 751 CA ARG A 102 10.292 4.709 −8.226 1.00 69.18 C ATOM 752 CB ARG A 102 10.066 4.608 −6.705 1.00 68.31 C ATOM 753 C ARG A 102 9.309 5.706 −8.876 1.00 68.61 C ATOM 754 O ARG A 102 8.196 5.884 −8.384 1.00 66.90 O ATOM 755 N ALA A 103 9.712 6.321 −9.991 1.00 69.15 N ATOM 756 CA ALA A 103 8.840 7.246 −10.735 1.00 68.27 C ATOM 757 CB ALA A 103 9.659 8.135 −11.660 1.00 68.20 C ATOM 758 C ALA A 103 7.751 6.512 −11.519 1.00 67.94 C ATOM 759 O ALA A 103 8.043 5.742 −12.430 1.00 69.95 O ATOM 760 N GLY A 104 6.496 6.761 −11.159 1.00 67.03 N ATOM 761 CA GLY A 104 5.353 6.130 −11.813 1.00 65.29 C ATOM 762 C GLY A 104 5.013 6.728 −13.168 1.00 64.79 C ATOM 763 O GLY A 104 5.795 7.490 −13.734 1.00 64.68 O ATOM 764 N ARG A 105 3.835 6.371 −13.681 1.00 64.75 N ATOM 765 CA ARG A 105 3.313 6.884 −14.958 1.00 62.98 C ATOM 766 CB ARG A 105 2.082 6.076 −15.373 1.00 63.28 C ATOM 767 C ARG A 105 2.960 8.380 −14.900 1.00 60.94 C ATOM 768 O ARG A 105 2.906 9.062 −15.932 1.00 61.36 O ATOM 769 N SER A 106 2.738 8.884 −13.690 1.00 58.17 N ATOM 770 CA SER A 106 2.346 10.276 −13.477 1.00 56.11 C ATOM 771 CB SER A 106 1.752 10.438 −12.066 1.00 56.25 C ATOM 772 OG SER A 106 1.128 11.702 −11.881 1.00 62.27 O ATOM 773 C SER A 106 3.492 11.282 −13.733 1.00 52.57 C ATOM 774 O SER A 106 3.240 12.458 −13.955 1.00 51.79 O ATOM 775 N CYS A 107 4.736 10.802 −13.767 1.00 48.78 N ATOM 776 CA CYS A 107 5.914 11.679 −13.824 1.00 45.90 C ATOM 777 CB CYS A 107 7.197 10.838 −13.856 1.00 41.55 C ATOM 778 SG CYS A 107 8.708 11.772 −13.436 1.00 45.62 S ATOM 779 C CYS A 107 5.902 12.687 −14.992 1.00 44.80 C ATOM 780 O CYS A 107 5.721 12.296 −16.133 1.00 45.74 O ATOM 781 N LYS A 108 6.108 13.973 −14.680 1.00 42.56 N ATOM 782 CA LYS A 108 6.171 15.074 −15.656 1.00 38.35 C ATOM 783 CB LYS A 108 5.080 16.126 −15.390 1.00 38.46 C ATOM 784 CG LYS A 108 3.617 15.631 −15.344 1.00 41.65 C ATOM 785 CD LYS A 108 3.130 15.220 −16.728 1.00 48.57 C ATOM 786 CE LYS A 108 1.623 15.055 −16.780 1.00 49.47 C ATOM 787 NZ LYS A 108 1.183 13.739 −16.226 1.00 51.52 N ATOM 788 C LYS A 108 7.512 15.802 −15.536 1.00 39.54 C ATOM 789 O LYS A 108 8.128 15.818 −14.465 1.00 30.07 O ATOM 790 N GLU A 109 7.944 16.427 −16.625 1.00 38.56 N ATOM 791 CA GLU A 109 9.128 17.239 −16.574 1.00 38.64 C ATOM 792 CB GLU A 109 10.181 16.730 −17.560 1.00 39.02 C ATOM 793 CG GLU A 109 11.197 15.800 −16.920 1.00 38.15 C ATOM 794 CD GLU A 109 11.851 14.822 −17.899 1.00 44.21 C ATOM 795 OE1 GLU A 109 11.980 15.168 −19.088 1.00 43.35 O ATOM 796 OE2 GLU A 109 12.272 13.717 −17.467 1.00 42.06 O ATOM 797 C GLU A 109 8.712 18.710 −16.798 1.00 36.56 C ATOM 798 O GLU A 109 9.471 19.530 −17.304 1.00 34.15 O ATOM 799 N THR A 110 7.487 19.022 −16.383 1.00 38.64 N ATOM 800 CA THR A 110 6.890 20.354 −16.584 1.00 36.73 C ATOM 801 CB THR A 110 6.025 20.451 −17.885 1.00 39.68 C ATOM 802 OG1 THR A 110 4.742 19.859 −17.655 1.00 36.91 O ATOM 803 CG2 THR A 110 6.686 19.780 −19.096 1.00 41.93 C ATOM 804 C THR A 110 5.997 20.727 −15.410 1.00 37.56 C ATOM 805 O THR A 110 5.683 19.887 −14.551 1.00 38.82 O ATOM 806 N PHE A 111 5.558 21.984 −15.397 1.00 34.68 N ATOM 807 CA PHE A 111 4.613 22.485 −14.422 1.00 36.33 C ATOM 808 CB PHE A 111 5.316 22.834 −13.062 1.00 30.29 C ATOM 809 CG PHE A 111 6.288 24.008 −13.127 1.00 37.23 C ATOM 810 CD1 PHE A 111 5.861 25.295 −12.849 1.00 29.32 C ATOM 811 CE1 PHE A 111 6.719 26.368 −12.916 1.00 32.48 C ATOM 812 CZ PHE A 111 8.045 26.184 −13.242 1.00 30.71 C ATOM 813 CE2 PHE A 111 8.505 24.895 −13.522 1.00 28.43 C ATOM 814 CD2 PHE A 111 7.604 23.816 −13.469 1.00 30.30 C ATOM 815 C PHE A 111 3.880 23.675 −15.070 1.00 35.66 C ATOM 816 O PHE A 111 4.361 24.226 −16.043 1.00 37.01 O ATOM 817 N THR A 112 2.709 24.032 −14.559 1.00 34.15 N ATOM 818 CA THR A 112 1.902 25.099 −15.158 1.00 38.08 C ATOM 819 CB THR A 112 0.476 24.609 −15.513 1.00 33.33 C ATOM 820 OG1 THR A 112 0.534 23.264 −15.995 1.00 47.68 O ATOM 821 CG2 THR A 112 −0.151 25.509 −16.580 1.00 43.08 C ATOM 822 C THR A 112 1.757 26.252 −14.190 1.00 33.68 C ATOM 823 O THR A 112 1.636 26.024 −12.992 1.00 37.19 O ATOM 824 N VAL A 113 1.739 27.477 −14.725 1.00 34.66 N ATOM 825 CA VAL A 113 1.595 28.699 −13.935 1.00 34.20 C ATOM 826 CB VAL A 113 2.762 29.695 −14.172 1.00 34.07 C ATOM 827 CG1 VAL A 113 2.620 30.929 −13.250 1.00 34.89 C ATOM 828 CG2 VAL A 113 4.084 29.039 −13.945 1.00 33.82 C ATOM 829 C VAL A 113 0.278 29.398 −14.298 1.00 39.57 C ATOM 830 O VAL A 113 −0.137 29.379 −15.457 1.00 42.20 O ATOM 831 N PHE A 114 −0.343 30.032 −13.301 1.00 38.25 N ATOM 832 CA PHE A 114 −1.679 30.608 −13.385 1.00 40.31 C ATOM 833 CB PHE A 114 −2.721 29.729 −12.651 1.00 37.24 C ATOM 834 CG PHE A 114 −3.128 28.487 −13.382 1.00 41.83 C ATOM 835 CD1 PHE A 114 −4.214 28.508 −14.269 1.00 36.65 C ATOM 836 CE1 PHE A 114 −4.609 27.380 −14.934 1.00 39.00 C ATOM 837 CZ PHE A 114 −3.969 26.144 −14.676 1.00 45.82 C ATOM 838 CE2 PHE A 114 −2.897 26.096 −13.756 1.00 47.68 C ATOM 839 CD2 PHE A 114 −2.500 27.271 −13.113 1.00 46.54 C ATOM 840 C PHE A 114 −1.569 31.905 −12.622 1.00 41.06 C ATOM 841 O PHE A 114 −0.599 32.136 −11.923 1.00 38.95 O ATOM 842 N TYR A 115 −2.559 32.774 −12.778 1.00 45.00 N ATOM 843 CA TYR A 115 −2.713 33.895 −11.855 1.00 42.70 C ATOM 844 CB TYR A 115 −1.955 35.146 −12.293 1.00 42.83 C ATOM 845 CG TYR A 115 −2.521 35.945 −13.454 1.00 40.85 C ATOM 846 CD1 TYR A 115 −3.338 37.058 −13.234 1.00 41.69 C ATOM 847 CE1 TYR A 115 −3.841 37.820 −14.326 1.00 48.11 C ATOM 848 CZ TYR A 115 −3.491 37.468 −15.640 1.00 49.33 C ATOM 849 OH TYR A 115 −3.957 38.193 −16.727 1.00 51.63 O ATOM 850 CE2 TYR A 115 −2.657 36.384 −15.876 1.00 42.04 C ATOM 851 CD2 TYR A 115 −2.175 35.626 −14.771 1.00 46.72 C ATOM 852 C TYR A 115 −4.167 34.175 −11.557 1.00 44.47 C ATOM 853 O TYR A 115 −5.062 33.587 −12.167 1.00 44.61 O ATOM 854 N TYR A 116 −4.389 35.025 −10.565 1.00 42.10 N ATOM 855 CA TYR A 116 −5.712 35.412 −10.169 1.00 41.46 C ATOM 856 CB TYR A 116 −6.248 34.439 −9.125 1.00 45.18 C ATOM 857 CG TYR A 116 −7.594 34.821 −8.566 1.00 44.71 C ATOM 858 CD1 TYR A 116 −8.756 34.651 −9.322 1.00 48.20 C ATOM 859 CE1 TYR A 116 −9.997 34.998 −8.815 1.00 51.58 C ATOM 860 CZ TYR A 116 −10.091 35.515 −7.532 1.00 48.34 C ATOM 861 OH TYR A 116 −11.322 35.864 −7.042 1.00 50.58 O ATOM 862 CE2 TYR A 116 −8.953 35.692 −6.758 1.00 48.96 C ATOM 863 CD2 TYR A 116 −7.709 35.339 −7.279 1.00 43.17 C ATOM 864 C TYR A 116 −5.627 36.809 −9.594 1.00 39.41 C ATOM 865 O TYR A 116 −4.892 37.039 −8.643 1.00 39.20 O ATOM 866 N GLU A 117 −6.354 37.755 −10.187 1.00 41.63 N ATOM 867 CA GLU A 117 −6.451 39.109 −9.619 1.00 39.85 C ATOM 868 CB GLU A 117 −6.656 40.172 −10.689 1.00 44.57 C ATOM 869 CG GLU A 117 −5.696 40.238 −11.861 1.00 41.68 C ATOM 870 CD GLU A 117 −5.987 41.478 −12.708 1.00 43.45 C ATOM 871 OE1 GLU A 117 −6.151 42.558 −12.099 1.00 39.22 O ATOM 872 OE2 GLU A 117 −6.076 41.379 −13.958 1.00 47.74 O ATOM 873 C GLU A 117 −7.645 39.214 −8.703 1.00 40.05 C ATOM 874 O GLU A 117 −8.720 38.631 −8.972 1.00 40.21 O ATOM 875 N SER A 118 −7.496 40.010 −7.649 1.00 38.81 N ATOM 876 CA SER A 118 −8.635 40.341 −6.784 1.00 40.06 C ATOM 877 CB SER A 118 −8.714 39.353 −5.647 1.00 36.38 C ATOM 878 OG SER A 118 −7.464 39.353 −4.975 1.00 41.44 O ATOM 879 C SER A 118 −8.408 41.723 −6.204 1.00 41.25 C ATOM 880 O SER A 118 −7.277 42.107 −5.969 1.00 41.14 O ATOM 881 N ASP A 119 −9.476 42.466 −5.945 1.00 43.52 N ATOM 882 CA ASP A 119 −9.331 43.849 −5.464 1.00 44.39 C ATOM 883 CB ASP A 119 −10.632 44.642 −5.659 1.00 42.41 C ATOM 884 CG ASP A 119 −10.730 45.267 −7.050 1.00 46.99 C ATOM 885 OD1 ASP A 119 −9.777 45.987 −7.479 1.00 44.22 O ATOM 886 OD2 ASP A 119 −11.768 45.046 −7.708 1.00 53.14 O ATOM 887 C ASP A 119 −8.795 43.944 −4.011 1.00 45.57 C ATOM 888 O ASP A 119 −8.150 44.928 −3.645 1.00 46.79 O ATOM 889 N ALA A 120 −9.059 42.912 −3.208 1.00 42.24 N ATOM 890 CA ALA A 120 −8.488 42.778 −1.873 1.00 41.91 C ATOM 891 CB ALA A 120 −9.523 43.085 −0.814 1.00 41.29 C ATOM 892 C ALA A 120 −7.958 41.342 −1.718 1.00 41.62 C ATOM 893 O ALA A 120 −8.149 40.506 −2.605 1.00 41.95 O ATOM 894 N ASP A 121 −7.279 41.080 −0.607 1.00 40.39 N ATOM 895 CA ASP A 121 −6.760 39.750 −0.304 1.00 38.92 C ATOM 896 CB ASP A 121 −5.603 39.842 0.695 1.00 39.88 C ATOM 897 CG ASP A 121 −4.986 38.485 0.986 1.00 38.88 C ATOM 898 OD1 ASP A 121 −5.368 37.528 0.286 1.00 43.21 O ATOM 899 OD2 ASP A 121 −4.135 38.370 1.901 1.00 35.63 O ATOM 900 C ASP A 121 −7.877 38.869 0.267 1.00 39.74 C ATOM 901 O ASP A 121 −7.956 38.631 1.469 1.00 40.54 O ATOM 902 N THR A 122 −8.724 38.356 −0.608 1.00 38.18 N ATOM 903 CA THR A 122 −9.920 37.670 −0.167 1.00 42.04 C ATOM 904 CB THR A 122 −11.102 38.158 −0.958 1.00 39.56 C ATOM 905 OG1 THR A 122 −10.799 38.009 −2.350 1.00 39.83 O ATOM 906 CG2 THR A 122 −11.348 39.643 −0.668 1.00 47.23 C ATOM 907 C THR A 122 −9.819 36.149 −0.322 1.00 43.00 C ATOM 908 O THR A 122 −10.737 35.417 0.059 1.00 45.82 O ATOM 909 N ALA A 123 −8.712 35.668 −0.880 1.00 43.76 N ATOM 910 CA ALA A 123 −8.527 34.207 −1.066 1.00 39.96 C ATOM 911 CB ALA A 123 −7.500 33.946 −2.149 1.00 38.69 C ATOM 912 C ALA A 123 −8.162 33.452 0.231 1.00 39.42 C ATOM 913 O ALA A 123 −7.456 33.976 1.079 1.00 38.76 O ATOM 914 N THR A 124 −8.630 32.207 0.354 1.00 37.16 N ATOM 915 CA THR A 124 −8.381 31.380 1.544 1.00 30.14 C ATOM 916 CB THR A 124 −9.759 31.027 2.267 1.00 27.28 C ATOM 917 OG1 THR A 124 −10.609 30.385 1.321 1.00 37.96 O ATOM 918 CG2 THR A 124 −10.449 32.264 2.782 1.00 34.09 C ATOM 919 C THR A 124 −7.628 30.114 1.121 1.00 31.09 C ATOM 920 O THR A 124 −7.161 29.992 −0.002 1.00 34.92 O ATOM 921 N ALA A 125 −7.516 29.143 2.006 1.00 34.69 N ATOM 922 CA ALA A 125 −6.966 27.857 1.594 1.00 35.09 C ATOM 923 CB ALA A 125 −6.557 27.037 2.822 1.00 35.57 C ATOM 924 C ALA A 125 −7.905 27.045 0.668 1.00 35.61 C ATOM 925 O ALA A 125 −7.450 26.100 0.025 1.00 35.88 O ATOM 926 N LEU A 126 −9.183 27.433 0.580 1.00 35.52 N ATOM 927 CA LEU A 126 −10.170 26.725 −0.244 1.00 38.01 C ATOM 928 CB LEU A 126 −11.158 25.926 0.629 1.00 40.30 C ATOM 929 CG LEU A 126 −10.687 24.875 1.642 1.00 35.50 C ATOM 930 CD1 LEU A 126 −11.925 24.464 2.443 1.00 35.12 C ATOM 931 CD2 LEU A 126 −10.053 23.662 0.975 1.00 43.01 C ATOM 932 C LEU A 126 −10.956 27.560 −1.259 1.00 39.41 C ATOM 933 O LEU A 126 −11.697 26.987 −2.064 1.00 38.78 O ATOM 934 N THR A 127 −10.819 28.892 −1.208 1.00 39.87 N ATOM 935 CA THR A 127 −11.417 29.795 −2.201 1.00 40.08 C ATOM 936 CB THR A 127 −12.495 30.751 −1.616 1.00 37.17 C ATOM 937 OG1 THR A 127 −11.920 31.565 −0.589 1.00 37.12 O ATOM 938 CG2 THR A 127 −13.710 29.964 −1.068 1.00 36.23 C ATOM 939 C THR A 127 −10.309 30.639 −2.849 1.00 38.11 C ATOM 940 O THR A 127 −9.397 31.072 −2.167 1.00 39.91 O ATOM 941 N PRO A 128 −10.389 30.879 −4.160 1.00 38.97 N ATOM 942 CA PRO A 128 −11.419 30.490 −5.120 1.00 38.25 C ATOM 943 CB PRO A 128 −11.309 31.579 −6.193 1.00 37.19 C ATOM 944 CG PRO A 128 −9.917 32.012 −6.167 1.00 36.47 C ATOM 945 CD PRO A 128 −9.318 31.665 −4.813 1.00 41.36 C ATOM 946 C PRO A 128 −11.145 29.112 −5.707 1.00 37.82 C ATOM 947 O PRO A 128 −10.157 28.501 −5.356 1.00 39.53 O ATOM 948 N ALA A 129 −12.025 28.630 −6.581 1.00 39.78 N ATOM 949 CA ALA A 129 −11.854 27.318 −7.208 1.00 41.22 C ATOM 950 CB ALA A 129 −12.845 27.149 −8.367 1.00 44.36 C ATOM 951 C ALA A 129 −10.430 27.106 −7.684 1.00 41.46 C ATOM 952 O ALA A 129 −9.931 27.854 −8.514 1.00 42.01 O ATOM 953 N TRP A 130 −9.781 26.070 −7.148 1.00 41.79 N ATOM 954 CA TRP A 130 −8.420 25.722 −7.528 1.00 40.28 C ATOM 955 CB TRP A 130 −7.839 24.792 −6.481 1.00 40.07 C ATOM 956 CG TRP A 130 −7.519 25.415 −5.177 1.00 37.59 C ATOM 957 CD1 TRP A 130 −8.231 25.310 −4.029 1.00 36.75 C ATOM 958 NE1 TRP A 130 −7.599 25.972 −3.007 1.00 41.38 N ATOM 959 CE2 TRP A 130 −6.447 26.532 −3.490 1.00 37.52 C ATOM 960 CD2 TRP A 130 −6.355 26.184 −4.859 1.00 39.29 C ATOM 961 CE3 TRP A 130 −5.265 26.625 −5.594 1.00 36.95 C ATOM 962 CZ3 TRP A 130 −4.283 27.382 −4.939 1.00 37.64 C ATOM 963 CH2 TRP A 130 −4.390 27.671 −3.578 1.00 27.48 C ATOM 964 CZ2 TRP A 130 −5.468 27.269 −2.837 1.00 38.20 C ATOM 965 C TRP A 130 −8.357 25.051 −8.897 1.00 42.27 C ATOM 966 O TRP A 130 −8.089 23.840 −9.012 1.00 43.07 O ATOM 967 N MET A 131 −8.590 25.839 −9.940 1.00 42.81 N ATOM 968 CA MET A 131 −8.682 25.324 −11.305 1.00 46.53 C ATOM 969 CB MET A 131 −9.995 24.548 −11.502 1.00 44.82 C ATOM 970 CG MET A 131 −11.234 25.302 −11.084 1.00 50.50 C ATOM 971 SD MET A 131 −12.714 24.275 −10.951 1.00 56.25 S ATOM 972 CE MET A 131 −12.308 23.173 −9.583 1.00 56.94 C ATOM 973 C MET A 131 −8.664 26.499 −12.258 1.00 44.91 C ATOM 974 O MET A 131 −9.043 27.602 −11.872 1.00 42.46 O ATOM 975 N GLU A 132 −8.228 26.265 −13.491 1.00 46.13 N ATOM 976 CA GLU A 132 −8.370 27.253 −14.554 1.00 47.13 C ATOM 977 CB GLU A 132 −7.908 26.671 −15.892 1.00 47.45 C ATOM 978 CG GLU A 132 −7.460 27.716 −16.901 1.00 47.99 C ATOM 979 CD GLU A 132 −6.957 27.101 −18.192 1.00 49.03 C ATOM 980 OE1 GLU A 132 −6.709 25.877 −18.212 1.00 56.50 O ATOM 981 OE2 GLU A 132 −6.810 27.841 −19.187 1.00 59.16 O ATOM 982 C GLU A 132 −9.811 27.741 −14.665 1.00 50.42 C ATOM 983 O GLU A 132 −10.747 26.942 −14.675 1.00 49.36 O ATOM 984 N ASN A 133 −9.980 29.056 −14.747 1.00 51.67 N ATOM 985 CA ASN A 133 −11.273 29.680 −14.489 1.00 52.45 C ATOM 986 CB ASN A 133 −12.287 29.272 −15.559 1.00 53.87 C ATOM 987 CG ASN A 133 −12.849 30.462 −16.312 1.00 58.00 C ATOM 988 OD1 ASN A 133 −12.264 30.925 −17.291 1.00 55.56 O ATOM 989 ND2 ASN A 133 −13.991 30.965 −15.857 1.00 60.24 N ATOM 990 C ASN A 133 −11.810 29.341 −13.102 1.00 51.46 C ATOM 991 O ASN A 133 −12.643 28.449 −12.949 1.00 53.60 O ATOM 992 N PRO A 134 −11.326 30.060 −12.094 1.00 48.44 N ATOM 993 CA PRO A 134 −11.125 31.508 −12.207 1.00 46.49 C ATOM 994 CB PRO A 134 −11.608 32.030 −10.853 1.00 48.19 C ATOM 995 CG PRO A 134 −11.380 30.898 −9.917 1.00 44.82 C ATOM 996 CD PRO A 134 −11.634 29.649 −10.713 1.00 45.15 C ATOM 997 C PRO A 134 −9.656 31.862 −12.412 1.00 46.83 C ATOM 998 O PRO A 134 −9.334 33.013 −12.705 1.00 42.89 O ATOM 999 N TYR A 135 −8.778 30.876 −12.256 1.00 43.64 N ATOM 1000 CA TYR A 135 −7.359 31.064 −12.529 1.00 41.33 C ATOM 1001 CB TYR A 135 −6.551 29.927 −11.896 1.00 42.40 C ATOM 1002 CG TYR A 135 −6.391 30.116 −10.420 1.00 38.37 C ATOM 1003 CD1 TYR A 135 −5.328 30.856 −9.917 1.00 43.89 C ATOM 1004 CE1 TYR A 135 −5.165 31.047 −8.565 1.00 35.67 C ATOM 1005 CZ TYR A 135 −6.073 30.497 −7.686 1.00 40.40 C ATOM 1006 OH TYR A 135 −5.892 30.710 −6.340 1.00 41.61 O ATOM 1007 CE2 TYR A 135 −7.143 29.734 −8.147 1.00 40.34 C ATOM 1008 CD2 TYR A 135 −7.289 29.543 −9.518 1.00 46.85 C ATOM 1009 C TYR A 135 −7.035 31.247 −14.014 1.00 43.30 C ATOM 1010 O TYR A 135 −7.694 30.675 −14.873 1.00 42.09 O ATOM 1011 N ILE A 136 −6.031 32.078 −14.308 1.00 45.98 N ATOM 1012 CA ILE A 136 −5.689 32.424 −15.693 1.00 45.22 C ATOM 1013 CB ILE A 136 −5.611 33.966 −15.879 1.00 45.25 C ATOM 1014 CG1 ILE A 136 −6.674 34.667 −15.018 1.00 43.90 C ATOM 1015 CD1 ILE A 136 −6.852 36.169 −15.294 1.00 44.67 C ATOM 1016 CG2 ILE A 136 −5.625 34.329 −17.376 1.00 45.40 C ATOM 1017 C ILE A 136 −4.360 31.802 −16.125 1.00 44.75 C ATOM 1018 O ILE A 136 −3.317 32.244 −15.674 1.00 49.92 O ATOM 1019 N LYS A 137 −4.405 30.788 −16.996 1.00 45.67 N ATOM 1020 CA LYS A 137 −3.193 30.056 −17.437 1.00 45.23 C ATOM 1021 CB LYS A 137 −3.550 29.029 −18.517 1.00 46.80 C ATOM 1022 CG LYS A 137 −2.568 27.881 −18.636 1.00 51.30 C ATOM 1023 CD LYS A 137 −2.822 27.038 −19.864 1.00 43.64 C ATOM 1024 CE LYS A 137 −1.485 26.684 −20.499 1.00 52.43 C ATOM 1025 NZ LYS A 137 −1.427 25.316 −21.121 1.00 52.54 N ATOM 1026 C LYS A 137 −2.165 31.036 −17.974 1.00 44.80 C ATOM 1027 O LYS A 137 −2.483 31.823 −18.865 1.00 44.54 O ATOM 1028 N VAL A 138 −0.968 31.044 −17.371 1.00 44.85 N ATOM 1029 CA VAL A 138 0.159 31.840 −17.855 1.00 42.62 C ATOM 1030 CB VAL A 138 1.112 32.308 −16.722 1.00 44.21 C ATOM 1031 CG1 VAL A 138 2.292 33.090 −17.295 1.00 42.19 C ATOM 1032 CG2 VAL A 138 0.391 33.175 −15.727 1.00 39.45 C ATOM 1033 C VAL A 138 0.926 31.034 −18.905 1.00 47.65 C ATOM 1034 O VAL A 138 1.017 31.471 −20.063 1.00 50.24 O ATOM 1035 N ASP A 139 1.449 29.855 −18.516 1.00 48.26 N ATOM 1036 CA ASP A 139 2.147 28.942 −19.445 1.00 47.50 C ATOM 1037 CB ASP A 139 3.486 29.565 −19.865 1.00 49.54 C ATOM 1038 CG ASP A 139 3.863 29.271 −21.313 1.00 55.87 C ATOM 1039 OD1 ASP A 139 2.962 29.260 −22.189 1.00 55.59 O ATOM 1040 OD2 ASP A 139 5.078 29.094 −21.572 1.00 56.27 O ATOM 1041 C ASP A 139 2.384 27.557 −18.816 1.00 46.73 C ATOM 1042 O ASP A 139 2.370 27.425 −17.603 1.00 46.01 O ATOM 1043 N THR A 140 2.571 26.533 −19.648 1.00 46.52 N ATOM 1044 CA THR A 140 3.020 25.213 −19.200 1.00 46.71 C ATOM 1045 CB THR A 140 2.359 24.089 −20.025 1.00 45.93 C ATOM 1046 OG1 THR A 140 0.941 24.093 −19.804 1.00 54.04 O ATOM 1047 CG2 THR A 140 2.891 22.720 −19.639 1.00 47.66 C ATOM 1048 C THR A 140 4.552 25.235 −19.364 1.00 47.71 C ATOM 1049 O THR A 140 5.044 25.308 −20.489 1.00 51.63 O ATOM 1050 N VAL A 141 5.286 25.212 −18.245 1.00 45.47 N ATOM 1051 CA VAL A 141 6.731 25.536 −18.205 1.00 43.47 C ATOM 1052 CB VAL A 141 7.122 26.334 −16.913 1.00 43.73 C ATOM 1053 CG1 VAL A 141 8.620 26.701 −16.885 1.00 39.47 C ATOM 1054 CG2 VAL A 141 6.309 27.599 −16.782 1.00 41.94 C ATOM 1055 C VAL A 141 7.551 24.264 −18.277 1.00 45.44 C ATOM 1056 O VAL A 141 7.346 23.347 −17.484 1.00 42.78 O ATOM 1057 N ALA A 142 8.479 24.214 −19.232 1.00 46.34 N ATOM 1058 CA ALA A 142 9.357 23.061 −19.394 1.00 44.60 C ATOM 1059 CB ALA A 142 9.303 22.534 −20.807 1.00 43.31 C ATOM 1060 C ALA A 142 10.784 23.412 −19.003 1.00 44.91 C ATOM 1061 O ALA A 142 11.166 24.586 −18.984 1.00 44.97 O ATOM 1062 N ALA A 143 11.548 22.371 −18.673 1.00 45.80 N ATOM 1063 CA ALA A 143 12.940 22.477 −18.238 1.00 43.20 C ATOM 1064 CB ALA A 143 13.218 21.450 −17.176 1.00 42.14 C ATOM 1065 C ALA A 143 13.871 22.258 −19.422 1.00 44.18 C ATOM 1066 O ALA A 143 13.738 21.272 −20.138 1.00 44.34 O ATOM 1067 N GLU A 144 14.822 23.174 −19.606 1.00 45.90 N ATOM 1068 CA GLU A 144 15.860 23.046 −20.625 1.00 45.98 C ATOM 1069 CB GLU A 144 16.443 24.409 −21.000 1.00 46.26 C ATOM 1070 C GLU A 144 16.952 22.147 −20.105 1.00 46.83 C ATOM 1071 O GLU A 144 17.680 21.548 −20.886 1.00 47.83 O ATOM 1072 N HIS A 145 17.062 22.066 −18.771 1.00 47.47 N ATOM 1073 CA HIS A 145 18.045 21.228 −18.103 1.00 43.60 C ATOM 1074 CB HIS A 145 19.171 22.083 −17.531 1.00 41.41 C ATOM 1075 CG HIS A 145 19.817 22.965 −18.550 1.00 49.97 C ATOM 1076 ND1 HIS A 145 20.679 22.482 −19.514 1.00 50.33 N ATOM 1077 CE1 HIS A 145 21.067 23.480 −20.288 1.00 55.83 C ATOM 1078 NE2 HIS A 145 20.470 24.585 −19.876 1.00 50.08 N ATOM 1079 CD2 HIS A 145 19.686 24.289 −18.790 1.00 50.75 C ATOM 1080 C HIS A 145 17.436 20.361 −17.002 1.00 42.09 C ATOM 1081 O HIS A 145 16.716 20.847 −16.135 1.00 39.62 O ATOM 1082 N LEU A 146 17.765 19.075 −17.051 1.00 40.69 N ATOM 1083 CA LEU A 146 17.326 18.092 −16.075 1.00 41.21 C ATOM 1084 CB LEU A 146 16.898 16.793 −16.786 1.00 43.31 C ATOM 1085 CG LEU A 146 15.739 16.923 −17.800 1.00 45.78 C ATOM 1086 CD1 LEU A 146 15.507 15.612 −18.551 1.00 52.48 C ATOM 1087 CD2 LEU A 146 14.444 17.386 −17.131 1.00 42.70 C ATOM 1088 C LEU A 146 18.414 17.824 −15.032 1.00 39.66 C ATOM 1089 O LEU A 146 19.626 17.831 −15.328 1.00 40.07 O ATOM 1090 N THR A 147 17.986 17.616 −13.794 1.00 39.07 N ATOM 1091 CA THR A 147 18.914 17.270 −12.723 1.00 36.70 C ATOM 1092 CB THR A 147 18.558 18.011 −11.401 1.00 37.46 C ATOM 1093 OG1 THR A 147 18.771 19.419 −11.542 1.00 32.66 O ATOM 1094 CG2 THR A 147 19.418 17.501 −10.239 1.00 36.18 C ATOM 1095 C THR A 147 18.847 15.737 −12.552 1.00 39.09 C ATOM 1096 O THR A 147 17.742 15.142 −12.547 1.00 35.10 O ATOM 1097 N ARG A 148 20.014 15.098 −12.483 1.00 37.07 N ATOM 1098 CA ARG A 148 20.090 13.707 −12.031 1.00 37.30 C ATOM 1099 CB ARG A 148 20.887 12.827 −13.001 1.00 36.01 C ATOM 1100 CG ARG A 148 20.231 12.730 −14.351 1.00 42.87 C ATOM 1101 CD ARG A 148 21.219 12.497 −15.435 1.00 46.15 C ATOM 1102 NE ARG A 148 20.558 12.599 −16.732 1.00 49.73 N ATOM 1103 CZ ARG A 148 20.535 13.696 −17.480 1.00 54.09 C ATOM 1104 NH1 ARG A 148 21.159 14.796 −17.073 1.00 55.32 N ATOM 1105 NH2 ARG A 148 19.886 13.687 −18.643 1.00 48.49 N ATOM 1106 C ARG A 148 20.781 13.718 −10.689 1.00 37.62 C ATOM 1107 O ARG A 148 21.837 14.357 −10.536 1.00 40.62 O ATOM 1108 N LYS A 149 20.197 13.006 −9.729 1.00 33.82 N ATOM 1109 CA LYS A 149 20.717 12.989 −8.374 1.00 38.43 C ATOM 1110 CB LYS A 149 19.724 13.631 −7.391 1.00 36.45 C ATOM 1111 CG LYS A 149 19.349 15.063 −7.677 1.00 39.04 C ATOM 1112 CD LYS A 149 18.851 15.705 −6.408 1.00 31.27 C ATOM 1113 CE LYS A 149 20.019 16.113 −5.543 1.00 33.52 C ATOM 1114 NZ LYS A 149 19.519 16.702 −4.262 1.00 31.74 N ATOM 1115 C LYS A 149 20.888 11.548 −7.968 1.00 39.40 C ATOM 1116 O LYS A 149 20.194 10.675 −8.488 1.00 43.92 O ATOM 1117 N ARG A 150 21.794 11.293 −7.032 1.00 38.52 N ATOM 1118 CA ARG A 150 21.841 9.999 −6.426 1.00 37.72 C ATOM 1119 CB ARG A 150 23.048 9.212 −6.913 1.00 39.83 C ATOM 1120 CG ARG A 150 22.677 7.815 −7.416 1.00 40.68 C ATOM 1121 CD ARG A 150 23.919 7.066 −7.884 1.00 50.69 C ATOM 1122 NE ARG A 150 25.109 7.751 −7.419 1.00 48.61 N ATOM 1123 CZ ARG A 150 25.889 7.366 −6.419 1.00 50.11 C ATOM 1124 NH1 ARG A 150 25.659 6.244 −5.744 1.00 40.80 N ATOM 1125 NH2 ARG A 150 26.919 8.124 −6.113 1.00 45.14 N ATOM 1126 C ARG A 150 21.770 10.108 −4.899 1.00 41.36 C ATOM 1127 O ARG A 150 22.707 10.607 −4.252 1.00 42.41 O ATOM 1128 N PRO A 151 20.643 9.645 −4.314 1.00 40.04 N ATOM 1129 CA PRO A 151 20.352 9.965 −2.926 1.00 43.16 C ATOM 1130 CB PRO A 151 19.275 8.954 −2.566 1.00 44.97 C ATOM 1131 CG PRO A 151 18.535 8.737 −3.854 1.00 42.32 C ATOM 1132 CD PRO A 151 19.592 8.813 −4.923 1.00 40.05 C ATOM 1133 C PRO A 151 21.600 9.831 −2.018 1.00 47.19 C ATOM 1134 O PRO A 151 22.261 8.794 −2.040 1.00 45.98 O ATOM 1135 N GLY A 152 21.922 10.913 −1.299 1.00 47.18 N ATOM 1136 CA GLY A 152 22.973 10.945 −0.277 1.00 44.93 C ATOM 1137 C GLY A 152 24.383 11.075 −0.813 1.00 43.32 C ATOM 1138 O GLY A 152 25.353 11.273 −0.062 1.00 45.52 O ATOM 1139 N ALA A 153 24.503 10.996 −2.122 1.00 42.03 N ATOM 1140 CA ALA A 153 25.791 10.730 −2.711 1.00 42.81 C ATOM 1141 CB ALA A 153 25.779 9.348 −3.358 1.00 41.08 C ATOM 1142 C ALA A 153 26.205 11.781 −3.717 1.00 43.37 C ATOM 1143 O ALA A 153 27.284 12.352 −3.606 1.00 45.89 O ATOM 1144 N GLU A 154 25.372 12.042 −4.716 1.00 38.19 N ATOM 1145 CA GLU A 154 25.889 12.780 −5.851 1.00 36.09 C ATOM 1146 CB GLU A 154 26.600 11.797 −6.763 1.00 34.29 C ATOM 1147 CG GLU A 154 27.493 12.370 −7.838 1.00 38.73 C ATOM 1148 CD GLU A 154 28.005 11.307 −8.808 1.00 37.40 C ATOM 1149 OE1 GLU A 154 27.908 10.093 −8.512 1.00 44.61 O ATOM 1150 OE2 GLU A 154 28.460 11.691 −9.898 1.00 40.39 O ATOM 1151 C GLU A 154 24.793 13.458 −6.631 1.00 40.06 C ATOM 1152 O GLU A 154 23.649 12.986 −6.641 1.00 36.30 O ATOM 1153 N ALA A 155 25.169 14.505 −7.359 1.00 38.96 N ATOM 1154 CA ALA A 155 24.204 15.221 −8.171 1.00 37.58 C ATOM 1155 CB ALA A 155 23.518 16.297 −7.339 1.00 41.18 C ATOM 1156 C ALA A 155 24.837 15.832 −9.388 1.00 35.95 C ATOM 1157 O ALA A 155 25.998 16.229 −9.358 1.00 38.79 O ATOM 1158 N THR A 156 24.083 15.898 −10.476 1.00 36.21 N ATOM 1159 CA THR A 156 24.470 16.730 −11.607 1.00 39.46 C ATOM 1160 CB THR A 156 24.920 15.915 −12.849 1.00 41.34 C ATOM 1161 OG1 THR A 156 23.904 14.953 −13.171 1.00 43.78 O ATOM 1162 CG2 THR A 156 26.249 15.214 −12.622 1.00 38.27 C ATOM 1163 C THR A 156 23.276 17.509 −12.046 1.00 39.87 C ATOM 1164 O THR A 156 22.122 17.050 −11.933 1.00 37.90 O ATOM 1165 N GLY A 157 23.529 18.690 −12.578 1.00 39.18 N ATOM 1166 CA GLY A 157 22.428 19.490 −13.084 1.00 37.13 C ATOM 1167 C GLY A 157 22.780 20.950 −13.226 1.00 35.38 C ATOM 1168 O GLY A 157 23.866 21.396 −12.823 1.00 33.71 O ATOM 1169 N LYS A 158 21.850 21.680 −13.825 1.00 37.34 N ATOM 1170 CA LYS A 158 21.886 23.131 −13.921 1.00 37.93 C ATOM 1171 CB LYS A 158 22.192 23.560 −15.358 1.00 40.53 C ATOM 1172 C LYS A 158 20.519 23.694 −13.496 1.00 39.02 C ATOM 1173 O LYS A 158 19.456 23.080 −13.744 1.00 37.62 O ATOM 1174 N VAL A 159 20.553 24.859 −12.861 1.00 38.06 N ATOM 1175 CA VAL A 159 19.336 25.622 −12.551 1.00 39.03 C ATOM 1176 CB VAL A 159 19.653 26.888 −11.699 1.00 38.12 C ATOM 1177 CG1 VAL A 159 18.378 27.596 −11.228 1.00 31.20 C ATOM 1178 CG2 VAL A 159 20.479 26.510 −10.502 1.00 42.87 C ATOM 1179 C VAL A 159 18.653 26.083 −13.829 1.00 38.78 C ATOM 1180 O VAL A 159 19.295 26.642 −14.719 1.00 37.57 O ATOM 1181 N ASN A 160 17.347 25.864 −13.911 1.00 37.96 N ATOM 1182 CA ASN A 160 16.555 26.480 −14.968 1.00 40.09 C ATOM 1183 CB ASN A 160 15.339 25.630 −15.291 1.00 37.65 C ATOM 1184 CG ASN A 160 15.735 24.343 −15.924 1.00 41.03 C ATOM 1185 OD1 ASN A 160 16.012 24.295 −17.115 1.00 40.31 O ATOM 1186 ND2 ASN A 160 15.850 23.304 −15.127 1.00 39.22 N ATOM 1187 C ASN A 160 16.195 27.909 −14.653 1.00 39.02 C ATOM 1188 O ASN A 160 16.020 28.284 −13.504 1.00 40.50 O ATOM 1189 N VAL A 161 16.152 28.736 −15.676 1.00 41.64 N ATOM 1190 CA VAL A 161 15.680 30.090 −15.492 1.00 41.07 C ATOM 1191 CB VAL A 161 16.807 31.143 −15.573 1.00 44.12 C ATOM 1192 CG1 VAL A 161 16.272 32.503 −15.082 1.00 42.61 C ATOM 1193 CG2 VAL A 161 18.065 30.722 −14.755 1.00 39.53 C ATOM 1194 C VAL A 161 14.604 30.348 −16.546 1.00 42.83 C ATOM 1195 O VAL A 161 14.835 30.185 −17.737 1.00 43.10 O ATOM 1196 N LYS A 162 13.401 30.676 −16.090 1.00 43.32 N ATOM 1197 CA LYS A 162 12.305 31.009 −17.004 1.00 44.78 C ATOM 1198 CB LYS A 162 11.214 29.918 −17.004 1.00 42.48 C ATOM 1199 CG LYS A 162 10.145 30.062 −18.115 1.00 45.76 C ATOM 1200 CD LYS A 162 10.761 29.861 −19.514 1.00 47.76 C ATOM 1201 CE LYS A 162 10.063 30.707 −20.577 1.00 45.12 C ATOM 1202 NZ LYS A 162 10.982 30.966 −21.720 1.00 45.05 N ATOM 1203 C LYS A 162 11.740 32.350 −16.563 1.00 43.17 C ATOM 1204 O LYS A 162 11.532 32.581 −15.374 1.00 42.04 O ATOM 1205 N THR A 163 11.538 33.254 −17.512 1.00 43.54 N ATOM 1206 CA THR A 163 10.833 34.481 −17.193 1.00 39.40 C ATOM 1207 CB THR A 163 11.658 35.711 −17.533 1.00 42.58 C ATOM 1208 OG1 THR A 163 12.816 35.742 −16.676 1.00 44.30 O ATOM 1209 CG2 THR A 163 10.846 37.006 −17.339 1.00 29.43 C ATOM 1210 C THR A 163 9.516 34.409 −17.951 1.00 40.40 C ATOM 1211 O THR A 163 9.499 34.187 −19.154 1.00 42.46 O ATOM 1212 N LEU A 164 8.427 34.532 −17.211 1.00 39.29 N ATOM 1213 CA LEU A 164 7.082 34.513 −17.756 1.00 41.09 C ATOM 1214 CB LEU A 164 6.223 33.580 −16.903 1.00 37.65 C ATOM 1215 CG LEU A 164 6.527 32.079 −17.062 1.00 34.39 C ATOM 1216 CD1 LEU A 164 5.534 31.295 −16.280 1.00 33.44 C ATOM 1217 CD2 LEU A 164 6.491 31.624 −18.505 1.00 30.97 C ATOM 1218 C LEU A 164 6.520 35.944 −17.753 1.00 41.72 C ATOM 1219 O LEU A 164 6.925 36.765 −16.935 1.00 41.65 O ATOM 1220 N ARG A 165 5.618 36.240 −18.685 1.00 46.79 N ATOM 1221 CA ARG A 165 4.950 37.552 −18.728 1.00 48.66 C ATOM 1222 CB ARG A 165 5.210 38.285 −20.048 1.00 49.34 C ATOM 1223 CG ARG A 165 4.630 39.706 −20.067 1.00 54.33 C ATOM 1224 CD ARG A 165 5.512 40.673 −19.295 1.00 55.25 C ATOM 1225 NE ARG A 165 6.735 40.850 −20.050 1.00 63.03 N ATOM 1226 CZ ARG A 165 6.834 41.649 −21.098 1.00 59.03 C ATOM 1227 NH1 ARG A 165 5.794 42.374 −21.471 1.00 63.76 N ATOM 1228 NH2 ARG A 165 7.978 41.732 −21.761 1.00 63.22 N ATOM 1229 C ARG A 165 3.452 37.432 −18.484 1.00 48.66 C ATOM 1230 O ARG A 165 2.830 36.449 −18.860 1.00 52.45 O ATOM 1231 N LEU A 166 2.871 38.466 −17.891 1.00 46.26 N ATOM 1232 CA LEU A 166 1.573 38.344 −17.273 1.00 45.06 C ATOM 1233 CB LEU A 166 1.798 37.906 −15.831 1.00 46.66 C ATOM 1234 CG LEU A 166 0.794 37.731 −14.709 1.00 47.10 C ATOM 1235 CD1 LEU A 166 1.252 36.507 −13.939 1.00 47.69 C ATOM 1236 CD2 LEU A 166 0.767 38.977 −13.813 1.00 42.28 C ATOM 1237 C LEU A 166 0.835 39.685 −17.337 1.00 44.50 C ATOM 1238 O LEU A 166 1.422 40.738 −17.068 1.00 43.18 O ATOM 1239 N GLY A 167 −0.444 39.627 −17.692 1.00 44.34 N ATOM 1240 CA GLY A 167 −1.286 40.830 −17.818 1.00 46.04 C ATOM 1241 C GLY A 167 −2.089 40.951 −19.117 1.00 46.16 C ATOM 1242 O GLY A 167 −2.277 39.969 −19.851 1.00 48.83 O ATOM 1243 N PRO A 168 −2.604 42.155 −19.404 1.00 44.04 N ATOM 1244 CA PRO A 168 −2.568 43.359 −18.579 1.00 42.19 C ATOM 1245 CB PRO A 168 −3.125 44.437 −19.517 1.00 42.07 C ATOM 1246 CG PRO A 168 −3.995 43.694 −20.446 1.00 47.01 C ATOM 1247 CD PRO A 168 −3.278 42.402 −20.690 1.00 45.76 C ATOM 1248 C PRO A 168 −3.411 43.262 −17.308 1.00 40.54 C ATOM 1249 O PRO A 168 −4.488 42.655 −17.313 1.00 38.18 O ATOM 1250 N LEU A 169 −2.921 43.906 −16.250 1.00 43.31 N ATOM 1251 CA LEU A 169 −3.546 43.889 −14.918 1.00 45.25 C ATOM 1252 CB LEU A 169 −2.505 43.511 −13.880 1.00 45.68 C ATOM 1253 CG LEU A 169 −1.920 42.103 −14.059 1.00 45.04 C ATOM 1254 CD1 LEU A 169 −0.397 42.117 −13.926 1.00 50.43 C ATOM 1255 CD2 LEU A 169 −2.553 41.196 −13.072 1.00 44.32 C ATOM 1256 C LEU A 169 −4.225 45.212 −14.519 1.00 45.55 C ATOM 1257 O LEU A 169 −3.719 46.295 −14.828 1.00 47.38 O ATOM 1258 N SER A 170 −5.337 45.087 −13.794 1.00 43.84 N ATOM 1259 CA SER A 170 −6.237 46.193 −13.435 1.00 48.14 C ATOM 1260 CB SER A 170 −7.617 45.992 −14.085 1.00 44.83 C ATOM 1261 OG SER A 170 −7.590 46.294 −15.470 1.00 50.91 O ATOM 1262 C SER A 170 −6.484 46.371 −11.941 1.00 47.63 C ATOM 1263 O SER A 170 −6.701 47.502 −11.490 1.00 47.42 O ATOM 1264 N LYS A 171 −6.486 45.257 −11.195 1.00 44.02 N ATOM 1265 CA LYS A 171 −6.991 45.256 −9.817 1.00 43.48 C ATOM 1266 CB LYS A 171 −7.645 43.905 −9.455 1.00 43.41 C ATOM 1267 CG LYS A 171 −8.737 43.410 −10.428 1.00 42.89 C ATOM 1268 CD LYS A 171 −9.921 42.790 −9.677 1.00 45.77 C ATOM 1269 CE LYS A 171 −10.862 42.045 −10.613 1.00 48.97 C ATOM 1270 NZ LYS A 171 −10.337 40.673 −10.938 1.00 43.91 N ATOM 1271 C LYS A 171 −5.904 45.615 −8.823 1.00 42.35 C ATOM 1272 O LYS A 171 −4.744 45.750 −9.203 1.00 43.62 O ATOM 1273 N ALA A 172 −6.262 45.775 −7.554 1.00 40.15 N ATOM 1274 CA ALA A 172 −5.296 46.286 −6.592 1.00 40.64 C ATOM 1275 CB ALA A 172 −5.963 46.540 −5.291 1.00 40.23 C ATOM 1276 C ALA A 172 −4.120 45.317 −6.425 1.00 39.80 C ATOM 1277 O ALA A 172 −2.984 45.726 −6.184 1.00 43.11 O ATOM 1278 N GLY A 173 −4.399 44.031 −6.543 1.00 40.73 N ATOM 1279 CA GLY A 173 −3.365 43.015 −6.434 1.00 37.01 C ATOM 1280 C GLY A 173 −3.745 41.677 −7.017 1.00 38.09 C ATOM 1281 O GLY A 173 −4.871 41.495 −7.536 1.00 35.36 O ATOM 1282 N PHE A 174 −2.814 40.720 −6.921 1.00 30.39 N ATOM 1283 CA PHE A 174 −3.020 39.450 −7.557 1.00 32.18 C ATOM 1284 CB PHE A 174 −2.507 39.466 −9.014 1.00 31.00 C ATOM 1285 CG PHE A 174 −1.004 39.557 −9.138 1.00 33.53 C ATOM 1286 CD1 PHE A 174 −0.220 38.387 −9.184 1.00 39.87 C ATOM 1287 CE1 PHE A 174 1.160 38.447 −9.279 1.00 40.76 C ATOM 1288 CZ PHE A 174 1.804 39.678 −9.356 1.00 36.30 C ATOM 1289 CE2 PHE A 174 1.038 40.872 −9.305 1.00 40.79 C ATOM 1290 CD2 PHE A 174 −0.372 40.794 −9.206 1.00 34.74 C ATOM 1291 C PHE A 174 −2.364 38.312 −6.746 1.00 30.68 C ATOM 1292 O PHE A 174 −1.698 38.568 −5.748 1.00 34.70 O ATOM 1293 N TYR A 175 −2.504 37.100 −7.254 1.00 34.65 N ATOM 1294 CA TYR A 175 −1.825 35.917 −6.697 1.00 31.11 C ATOM 1295 CB TYR A 175 −2.859 34.963 −6.139 1.00 36.87 C ATOM 1296 CG TYR A 175 −3.695 35.498 −5.041 1.00 36.55 C ATOM 1297 CD1 TYR A 175 −3.246 35.442 −3.722 1.00 34.78 C ATOM 1298 CE1 TYR A 175 −4.004 35.942 −2.709 1.00 37.57 C ATOM 1299 CZ TYR A 175 −5.241 36.488 −2.985 1.00 35.98 C ATOM 1300 OH TYR A 175 −6.003 36.966 −1.953 1.00 34.98 O ATOM 1301 CE2 TYR A 175 −5.719 36.555 −4.281 1.00 39.64 C ATOM 1302 CD2 TYR A 175 −4.939 36.044 −5.306 1.00 34.73 C ATOM 1303 C TYR A 175 −1.215 35.129 −7.800 1.00 34.83 C ATOM 1304 O TYR A 175 −1.844 34.963 −8.839 1.00 36.19 O ATOM 1305 N LEU A 176 −0.063 34.506 −7.533 1.00 34.99 N ATOM 1306 CA LEU A 176 0.505 33.635 −8.516 1.00 36.02 C ATOM 1307 CB LEU A 176 1.978 33.991 −8.765 1.00 32.58 C ATOM 1308 CG LEU A 176 2.568 33.556 −10.093 1.00 33.93 C ATOM 1309 CD1 LEU A 176 1.971 34.305 −11.256 1.00 35.00 C ATOM 1310 CD2 LEU A 176 4.068 33.794 −10.077 1.00 34.45 C ATOM 1311 C LEU A 176 0.340 32.206 −8.048 1.00 33.83 C ATOM 1312 O LEU A 176 0.550 31.923 −6.871 1.00 34.45 O ATOM 1313 N ALA A 177 −0.007 31.307 −8.961 1.00 31.16 N ATOM 1314 CA ALA A 177 −0.165 29.924 −8.570 1.00 31.94 C ATOM 1315 CB ALA A 177 −1.672 29.506 −8.480 1.00 33.96 C ATOM 1316 C ALA A 177 0.632 28.995 −9.461 1.00 35.75 C ATOM 1317 O ALA A 177 0.909 29.258 −10.658 1.00 35.44 O ATOM 1318 N PHE A 178 1.033 27.900 −8.836 1.00 34.91 N ATOM 1319 CA PHE A 178 1.835 26.896 −9.493 1.00 36.95 C ATOM 1320 CB PHE A 178 3.173 26.699 −8.768 1.00 37.01 C ATOM 1321 CG PHE A 178 4.025 27.931 −8.725 1.00 40.04 C ATOM 1322 CD1 PHE A 178 5.022 28.135 −9.690 1.00 34.45 C ATOM 1323 CE1 PHE A 178 5.826 29.267 −9.655 1.00 41.39 C ATOM 1324 CZ PHE A 178 5.630 30.221 −8.645 1.00 38.98 C ATOM 1325 CE2 PHE A 178 4.617 30.043 −7.695 1.00 38.28 C ATOM 1326 CD2 PHE A 178 3.830 28.896 −7.727 1.00 31.99 C ATOM 1327 C PHE A 178 1.019 25.652 −9.361 1.00 36.21 C ATOM 1328 O PHE A 178 0.613 25.292 −8.255 1.00 37.32 O ATOM 1329 N GLN A 179 0.771 25.001 −10.490 1.00 35.99 N ATOM 1330 CA GLN A 179 0.151 23.696 −10.481 1.00 37.46 C ATOM 1331 CB GLN A 179 −1.193 23.726 −11.248 1.00 37.59 C ATOM 1332 CG GLN A 179 −1.779 22.345 −11.528 1.00 34.22 C ATOM 1333 CD GLN A 179 −2.739 22.326 −12.728 1.00 39.93 C ATOM 1334 OE1 GLN A 179 −2.403 22.777 −13.817 1.00 45.97 O ATOM 1335 NE2 GLN A 179 −3.922 21.754 −12.529 1.00 45.45 N ATOM 1336 C GLN A 179 1.068 22.583 −10.991 1.00 35.94 C ATOM 1337 O GLN A 179 1.540 22.601 −12.105 1.00 33.60 O ATOM 1338 N ASP A 180 1.271 21.592 −10.138 1.00 39.76 N ATOM 1339 CA ASP A 180 2.028 20.410 −10.456 1.00 40.59 C ATOM 1340 CB ASP A 180 2.898 20.092 −9.250 1.00 37.86 C ATOM 1341 CG ASP A 180 3.454 18.706 −9.294 1.00 39.57 C ATOM 1342 OD1 ASP A 180 4.226 18.446 −10.237 1.00 39.93 O ATOM 1343 OD2 ASP A 180 3.141 17.893 −8.384 1.00 35.30 O ATOM 1344 C ASP A 180 1.106 19.214 −10.744 1.00 40.58 C ATOM 1345 O ASP A 180 0.119 19.009 −10.048 1.00 41.81 O ATOM 1346 N GLN A 181 1.417 18.427 −11.769 1.00 41.23 N ATOM 1347 CA GLN A 181 0.612 17.229 −12.057 1.00 40.16 C ATOM 1348 CB GLN A 181 −0.197 17.361 −13.365 1.00 38.15 C ATOM 1349 CG GLN A 181 −0.923 18.687 −13.561 1.00 41.10 C ATOM 1350 CD GLN A 181 −1.592 18.821 −14.926 1.00 43.97 C ATOM 1351 OE1 GLN A 181 −1.923 17.826 −15.577 1.00 43.86 O ATOM 1352 NE2 GLN A 181 −1.807 20.066 −15.362 1.00 46.46 N ATOM 1353 C GLN A 181 1.478 15.981 −12.087 1.00 37.45 C ATOM 1354 O GLN A 181 1.018 14.916 −12.448 1.00 38.23 O ATOM 1355 N GLY A 182 2.733 16.097 −11.679 1.00 35.03 N ATOM 1356 CA GLY A 182 3.569 14.916 −11.563 1.00 31.33 C ATOM 1357 C GLY A 182 5.061 15.219 −11.657 1.00 32.94 C ATOM 1358 O GLY A 182 5.853 14.337 −11.965 1.00 33.01 O ATOM 1359 N ALA A 183 5.455 16.446 −11.376 1.00 27.42 N ATOM 1360 CA ALA A 183 6.916 16.789 −11.503 1.00 34.16 C ATOM 1361 CB ALA A 183 7.084 18.245 −11.905 1.00 31.51 C ATOM 1362 C ALA A 183 7.730 16.465 −10.224 1.00 36.88 C ATOM 1363 O ALA A 183 7.165 16.305 −9.146 1.00 38.15 O ATOM 1364 N CYS A 184 9.054 16.330 −10.362 1.00 38.55 N ATOM 1365 CA CYS A 184 9.983 16.326 −9.232 1.00 37.77 C ATOM 1366 CB CYS A 184 10.821 15.026 −9.216 1.00 40.69 C ATOM 1367 SG CYS A 184 11.729 14.712 −7.696 1.00 37.47 S ATOM 1368 C CYS A 184 10.866 17.571 −9.390 1.00 36.58 C ATOM 1369 O CYS A 184 11.808 17.554 −10.162 1.00 34.19 O ATOM 1370 N MET A 185 10.509 18.667 −8.705 1.00 35.34 N ATOM 1371 CA MET A 185 11.161 19.976 −8.863 1.00 36.03 C ATOM 1372 CB MET A 185 10.379 20.827 −9.856 1.00 34.42 C ATOM 1373 CG MET A 185 8.902 21.024 −9.488 1.00 34.05 C ATOM 1374 SD MET A 185 8.089 22.180 −10.598 1.00 36.69 S ATOM 1375 CE MET A 185 8.821 23.708 −10.012 1.00 44.23 C ATOM 1376 C MET A 185 11.317 20.774 −7.567 1.00 29.84 C ATOM 1377 O MET A 185 10.536 20.592 −6.637 1.00 29.27 O ATOM 1378 N ALA A 186 12.397 21.553 −7.464 1.00 30.72 N ATOM 1379 CA ALA A 186 12.518 22.596 −6.450 1.00 27.77 C ATOM 1380 CB ALA A 186 13.910 22.553 −5.745 1.00 25.18 C ATOM 1381 C ALA A 186 12.336 23.979 −7.125 1.00 24.78 C ATOM 1382 O ALA A 186 12.961 24.251 −8.150 1.00 31.56 O ATOM 1383 N LEU A 187 11.565 24.864 −6.507 1.00 27.48 N ATOM 1384 CA LEU A 187 11.519 26.299 −6.879 1.00 27.38 C ATOM 1385 CB LEU A 187 10.101 26.887 −6.703 1.00 30.71 C ATOM 1386 CG LEU A 187 9.980 28.385 −7.052 1.00 29.76 C ATOM 1387 CD1 LEU A 187 9.960 28.497 −8.550 1.00 25.31 C ATOM 1388 CD2 LEU A 187 8.780 29.029 −6.446 1.00 38.88 C ATOM 1389 C LEU A 187 12.439 27.016 −5.931 1.00 26.96 C ATOM 1390 O LEU A 187 12.136 27.168 −4.765 1.00 31.63 O ATOM 1391 N LEU A 188 13.585 27.419 −6.445 1.00 23.82 N ATOM 1392 CA LEU A 188 14.649 28.033 −5.680 1.00 22.42 C ATOM 1393 CB LEU A 188 15.952 27.928 −6.492 1.00 18.60 C ATOM 1394 CG LEU A 188 16.336 26.464 −6.872 1.00 22.31 C ATOM 1395 CD1 LEU A 188 17.713 26.386 −7.539 1.00 28.31 C ATOM 1396 CD2 LEU A 188 16.255 25.517 −5.679 1.00 28.43 C ATOM 1397 C LEU A 188 14.302 29.477 −5.412 1.00 22.74 C ATOM 1398 O LEU A 188 14.529 29.936 −4.329 1.00 28.62 O ATOM 1399 N SER A 189 13.673 30.153 −6.382 1.00 27.21 N ATOM 1400 CA SER A 189 13.270 31.519 −6.173 1.00 31.26 C ATOM 1401 CB SER A 189 14.515 32.436 −6.114 1.00 36.03 C ATOM 1402 OG SER A 189 15.019 32.681 −7.411 1.00 31.51 O ATOM 1403 C SER A 189 12.252 32.016 −7.211 1.00 32.45 C ATOM 1404 O SER A 189 12.127 31.446 −8.302 1.00 30.70 O ATOM 1405 N LEU A 190 11.481 33.035 −6.801 1.00 33.70 N ATOM 1406 CA LEU A 190 10.455 33.696 −7.616 1.00 35.24 C ATOM 1407 CB LEU A 190 8.999 33.318 −7.175 1.00 33.65 C ATOM 1408 CG LEU A 190 7.879 34.252 −7.704 1.00 37.98 C ATOM 1409 CD1 LEU A 190 7.758 34.196 −9.248 1.00 38.61 C ATOM 1410 CD2 LEU A 190 6.494 34.037 −7.064 1.00 34.04 C ATOM 1411 C LEU A 190 10.680 35.193 −7.476 1.00 35.25 C ATOM 1412 O LEU A 190 10.779 35.711 −6.376 1.00 33.56 O ATOM 1413 N HIS A 191 10.780 35.893 −8.594 1.00 37.40 N ATOM 1414 CA HIS A 191 10.920 37.330 −8.519 1.00 38.52 C ATOM 1415 CB HIS A 191 12.402 37.758 −8.720 1.00 37.86 C ATOM 1416 CG HIS A 191 12.617 39.246 −8.734 1.00 41.14 C ATOM 1417 ND1 HIS A 191 13.565 39.845 −9.531 1.00 38.74 N ATOM 1418 CE1 HIS A 191 13.539 41.156 −9.344 1.00 41.60 C ATOM 1419 NE2 HIS A 191 12.627 41.424 −8.430 1.00 40.15 N ATOM 1420 CD2 HIS A 191 12.039 40.244 −8.024 1.00 30.90 C ATOM 1421 C HIS A 191 9.921 37.957 −9.487 1.00 39.05 C ATOM 1422 O HIS A 191 9.977 37.744 −10.702 1.00 37.50 O ATOM 1423 N LEU A 192 8.976 38.674 −8.890 1.00 38.54 N ATOM 1424 CA LEU A 192 7.912 39.401 −9.592 1.00 40.13 C ATOM 1425 CB LEU A 192 6.566 39.221 −8.876 1.00 39.90 C ATOM 1426 CG LEU A 192 5.960 37.835 −8.772 1.00 36.90 C ATOM 1427 CD1 LEU A 192 4.835 37.864 −7.800 1.00 42.75 C ATOM 1428 CD2 LEU A 192 5.498 37.403 −10.150 1.00 33.58 C ATOM 1429 C LEU A 192 8.274 40.859 −9.531 1.00 37.03 C ATOM 1430 O LEU A 192 8.557 41.381 −8.457 1.00 36.49 O ATOM 1431 N PHE A 193 8.241 41.502 −10.687 1.00 38.07 N ATOM 1432 CA PHE A 193 8.650 42.894 −10.841 1.00 36.70 C ATOM 1433 CB PHE A 193 10.216 43.035 −10.959 1.00 29.97 C ATOM 1434 CG PHE A 193 10.802 42.363 −12.180 1.00 31.12 C ATOM 1435 CD1 PHE A 193 11.097 43.105 −13.328 1.00 37.50 C ATOM 1436 CE1 PHE A 193 11.596 42.500 −14.467 1.00 34.28 C ATOM 1437 CZ PHE A 193 11.853 41.124 −14.481 1.00 45.74 C ATOM 1438 CE2 PHE A 193 11.563 40.350 −13.352 1.00 30.73 C ATOM 1439 CD2 PHE A 193 11.067 40.985 −12.190 1.00 37.59 C ATOM 1440 C PHE A 193 7.950 43.450 −12.090 1.00 40.02 C ATOM 1441 O PHE A 193 7.271 42.732 −12.840 1.00 44.09 O ATOM 1442 N TYR A 194 8.097 44.747 −12.297 1.00 41.11 N ATOM 1443 CA TYR A 194 7.673 45.348 −13.580 1.00 41.03 C ATOM 1444 CB TYR A 194 6.236 45.880 −13.495 1.00 42.85 C ATOM 1445 CG TYR A 194 6.023 47.133 −12.652 1.00 45.26 C ATOM 1446 CD1 TYR A 194 5.865 47.056 −11.268 1.00 45.47 C ATOM 1447 CE1 TYR A 194 5.635 48.201 −10.499 1.00 41.30 C ATOM 1448 CZ TYR A 194 5.566 49.425 −11.108 1.00 41.62 C ATOM 1449 OH TYR A 194 5.318 50.549 −10.355 1.00 41.25 O ATOM 1450 CE2 TYR A 194 5.703 49.532 −12.480 1.00 44.15 C ATOM 1451 CD2 TYR A 194 5.928 48.391 −13.248 1.00 45.95 C ATOM 1452 C TYR A 194 8.650 46.430 −13.974 1.00 41.04 C ATOM 1453 O TYR A 194 9.456 46.856 −13.147 1.00 40.79 O ATOM 1454 N LYS A 195 8.592 46.864 −15.236 1.00 44.73 N ATOM 1455 CA LYS A 195 9.456 47.945 −15.729 1.00 46.28 C ATOM 1456 CB LYS A 195 10.152 47.561 −17.037 1.00 43.48 C ATOM 1457 CG LYS A 195 10.979 46.305 −16.912 1.00 47.45 C ATOM 1458 CD LYS A 195 11.676 45.924 −18.202 1.00 50.29 C ATOM 1459 CE LYS A 195 12.404 44.596 −18.004 1.00 50.32 C ATOM 1460 NZ LYS A 195 12.635 43.846 −19.282 1.00 59.34 N ATOM 1461 C LYS A 195 8.624 49.217 −15.860 1.00 47.80 C ATOM 1462 O LYS A 195 7.537 49.218 −16.454 1.00 45.96 O ATOM 1463 N LYS A 196 9.144 50.290 −15.277 1.00 49.37 N ATOM 1464 CA LYS A 196 8.323 51.432 −14.872 1.00 53.18 C ATOM 1465 CB LYS A 196 9.160 52.333 −13.968 1.00 53.61 C ATOM 1466 CG LYS A 196 8.409 52.877 −12.787 1.00 57.05 C ATOM 1467 CD LYS A 196 9.326 52.905 −11.589 1.00 56.96 C ATOM 1468 CE LYS A 196 9.150 54.183 −10.795 1.00 56.02 C ATOM 1469 NZ LYS A 196 10.319 54.447 −9.912 1.00 49.28 N ATOM 1470 C LYS A 196 7.673 52.246 −16.004 1.00 54.46 C ATOM 1471 O LYS A 196 8.045 52.167 −17.184 1.00 52.26 O ATOM 1472 OXT LYS A 196 6.733 53.018 −15.746 1.00 55.97 O ATOM 1473 N ILE B 31 6.202 17.357 11.661 1.00 52.51 N ATOM 1474 CA ILE B 31 6.652 17.466 13.083 1.00 51.68 C ATOM 1475 CB ILE B 31 7.195 16.099 13.642 1.00 51.99 C ATOM 1476 CG1 ILE B 31 8.524 15.693 12.959 1.00 56.45 C ATOM 1477 CD1 ILE B 31 9.378 14.656 13.701 1.00 48.38 C ATOM 1478 CG2 ILE B 31 6.139 15.008 13.502 1.00 57.59 C ATOM 1479 C ILE B 31 7.694 18.588 13.242 1.00 51.74 C ATOM 1480 O ILE B 31 8.867 18.423 12.904 1.00 49.06 O ATOM 1481 N VAL B 32 7.254 19.737 13.751 1.00 51.69 N ATOM 1482 CA VAL B 32 8.155 20.860 13.927 1.00 49.76 C ATOM 1483 CB VAL B 32 7.409 22.216 13.764 1.00 49.19 C ATOM 1484 CG1 VAL B 32 8.381 23.405 13.799 1.00 48.91 C ATOM 1485 CG2 VAL B 32 6.606 22.225 12.458 1.00 50.33 C ATOM 1486 C VAL B 32 8.812 20.697 15.292 1.00 51.68 C ATOM 1487 O VAL B 32 8.130 20.724 16.318 1.00 55.62 O ATOM 1488 N LEU B 33 10.130 20.483 15.307 1.00 51.40 N ATOM 1489 CA LEU B 33 10.881 20.426 16.570 1.00 49.84 C ATOM 1490 CB LEU B 33 12.181 19.648 16.400 1.00 49.11 C ATOM 1491 CG LEU B 33 12.026 18.219 15.866 1.00 50.26 C ATOM 1492 CD1 LEU B 33 13.092 17.915 14.844 1.00 45.27 C ATOM 1493 CD2 LEU B 33 12.059 17.216 17.001 1.00 49.51 C ATOM 1494 C LEU B 33 11.157 21.838 17.081 1.00 51.22 C ATOM 1495 O LEU B 33 10.961 22.817 16.350 1.00 51.79 O ATOM 1496 N GLU B 34 11.587 21.956 18.334 1.00 48.63 N ATOM 1497 CA GLU B 34 11.756 23.283 18.942 1.00 50.49 C ATOM 1498 CB GLU B 34 11.951 23.178 20.458 1.00 52.60 C ATOM 1499 C GLU B 34 12.914 24.043 18.303 1.00 47.30 C ATOM 1500 O GLU B 34 14.019 23.514 18.216 1.00 45.62 O ATOM 1501 N PRO B 35 12.651 25.282 17.841 1.00 46.68 N ATOM 1502 CA PRO B 35 13.663 26.137 17.253 1.00 44.35 C ATOM 1503 CB PRO B 35 12.961 27.492 17.191 1.00 46.18 C ATOM 1504 CG PRO B 35 11.535 27.136 16.959 1.00 44.55 C ATOM 1505 CD PRO B 35 11.319 25.926 17.817 1.00 46.72 C ATOM 1506 C PRO B 35 14.940 26.229 18.079 1.00 46.44 C ATOM 1507 O PRO B 35 14.912 26.212 19.326 1.00 46.98 O ATOM 1508 N ILE B 36 16.058 26.291 17.377 1.00 47.07 N ATOM 1509 CA ILE B 36 17.354 26.348 18.024 1.00 47.75 C ATOM 1510 CB ILE B 36 18.272 25.214 17.548 1.00 45.95 C ATOM 1511 CG1 ILE B 36 17.727 23.879 18.073 1.00 46.11 C ATOM 1512 CD1 ILE B 36 18.656 22.714 17.974 1.00 48.49 C ATOM 1513 CG2 ILE B 36 19.708 25.452 18.031 1.00 52.98 C ATOM 1514 C ILE B 36 17.994 27.717 17.845 1.00 47.45 C ATOM 1515 O ILE B 36 18.367 28.116 16.739 1.00 47.44 O ATOM 1516 N TYR B 37 18.090 28.444 18.951 1.00 48.70 N ATOM 1517 CA TYR B 37 18.714 29.751 18.920 1.00 49.10 C ATOM 1518 CB TYR B 37 18.089 30.679 19.948 1.00 48.08 C ATOM 1519 CG TYR B 37 16.632 30.929 19.657 1.00 53.20 C ATOM 1520 CD1 TYR B 37 16.201 32.116 19.037 1.00 55.88 C ATOM 1521 CE1 TYR B 37 14.841 32.323 18.784 1.00 52.31 C ATOM 1522 CZ TYR B 37 13.933 31.333 19.131 1.00 53.25 C ATOM 1523 OH TYR B 37 12.585 31.480 18.900 1.00 55.81 O ATOM 1524 CE2 TYR B 37 14.343 30.168 19.727 1.00 49.90 C ATOM 1525 CD2 TYR B 37 15.675 29.969 19.988 1.00 55.92 C ATOM 1526 C TYR B 37 20.208 29.644 19.095 1.00 48.06 C ATOM 1527 O TYR B 37 20.705 29.188 20.135 1.00 47.00 O ATOM 1528 N TRP B 38 20.902 30.081 18.055 1.00 44.34 N ATOM 1529 CA TRP B 38 22.343 30.031 17.993 1.00 44.89 C ATOM 1530 CB TRP B 38 22.794 29.823 16.533 1.00 45.89 C ATOM 1531 CG TRP B 38 24.191 29.337 16.424 1.00 43.47 C ATOM 1532 CD1 TRP B 38 25.320 30.086 16.476 1.00 46.09 C ATOM 1533 NE1 TRP B 38 26.432 29.279 16.364 1.00 48.98 N ATOM 1534 CE2 TRP B 38 26.015 27.980 16.247 1.00 42.45 C ATOM 1535 CD2 TRP B 38 24.610 27.980 16.292 1.00 42.52 C ATOM 1536 CE3 TRP B 38 23.930 26.763 16.179 1.00 47.79 C ATOM 1537 CZ3 TRP B 38 24.653 25.621 16.043 1.00 46.68 C ATOM 1538 CH2 TRP B 38 26.051 25.649 16.007 1.00 47.89 C ATOM 1539 CZ2 TRP B 38 26.746 26.821 16.101 1.00 45.11 C ATOM 1540 C TRP B 38 22.912 31.312 18.589 1.00 45.43 C ATOM 1541 O TRP B 38 23.237 32.274 17.882 1.00 41.46 O ATOM 1542 N ASN B 39 22.980 31.315 19.914 1.00 43.47 N ATOM 1543 CA ASN B 39 23.587 32.390 20.669 1.00 47.07 C ATOM 1544 CB ASN B 39 22.561 33.489 21.025 1.00 48.07 C ATOM 1545 CG ASN B 39 21.403 32.981 21.887 1.00 48.17 C ATOM 1546 OD1 ASN B 39 21.589 32.193 22.806 1.00 61.41 O ATOM 1547 ND2 ASN B 39 20.207 33.467 21.607 1.00 56.57 N ATOM 1548 C ASN B 39 24.274 31.798 21.893 1.00 47.83 C ATOM 1549 O ASN B 39 23.880 30.722 22.380 1.00 48.70 O ATOM 1550 N SER B 40 25.332 32.453 22.361 1.00 50.06 N ATOM 1551 CA SER B 40 26.136 31.882 23.459 1.00 49.21 C ATOM 1552 CB SER B 40 27.442 32.647 23.649 1.00 48.57 C ATOM 1553 OG SER B 40 27.218 33.898 24.280 1.00 47.90 O ATOM 1554 C SER B 40 25.336 31.785 24.776 1.00 50.37 C ATOM 1555 O SER B 40 25.692 30.999 25.677 1.00 51.05 O ATOM 1556 N SER B 41 24.249 32.554 24.875 1.00 48.80 N ATOM 1557 CA SER B 41 23.325 32.428 26.008 1.00 52.76 C ATOM 1558 CB SER B 41 22.504 33.714 26.211 1.00 51.67 C ATOM 1559 OG SER B 41 21.575 33.924 25.161 1.00 57.98 O ATOM 1560 C SER B 41 22.424 31.174 25.920 1.00 54.80 C ATOM 1561 O SER B 41 21.563 30.955 26.782 1.00 55.52 O ATOM 1562 N ASN B 42 22.665 30.329 24.914 1.00 53.48 N ATOM 1563 CA ASN B 42 21.954 29.058 24.777 1.00 52.76 C ATOM 1564 CB ASN B 42 21.929 28.601 23.303 1.00 52.32 C ATOM 1565 CG ASN B 42 20.840 27.578 23.016 1.00 50.95 C ATOM 1566 OD1 ASN B 42 20.252 26.984 23.931 1.00 61.15 O ATOM 1567 ND2 ASN B 42 20.567 27.360 21.736 1.00 51.55 N ATOM 1568 C ASN B 42 22.582 27.975 25.657 1.00 52.92 C ATOM 1569 O ASN B 42 23.527 27.296 25.236 1.00 52.05 O ATOM 1570 N SER B 43 22.051 27.813 26.868 1.00 52.45 N ATOM 1571 CA SER B 43 22.571 26.817 27.819 1.00 54.85 C ATOM 1572 CB SER B 43 22.026 27.063 29.231 1.00 53.84 C ATOM 1573 OG SER B 43 20.659 26.694 29.333 1.00 57.96 O ATOM 1574 C SER B 43 22.343 25.358 27.378 1.00 54.62 C ATOM 1575 O SER B 43 22.959 24.447 27.926 1.00 56.78 O ATOM 1576 N LYS B 44 21.479 25.152 26.378 1.00 53.79 N ATOM 1577 CA LYS B 44 21.264 23.840 25.758 1.00 51.82 C ATOM 1578 CB LYS B 44 20.148 23.919 24.720 1.00 52.94 C ATOM 1579 C LYS B 44 22.530 23.276 25.109 1.00 50.94 C ATOM 1580 O LYS B 44 22.605 22.071 24.860 1.00 50.22 O ATOM 1581 N PHE B 45 23.504 24.152 24.821 1.00 49.62 N ATOM 1582 CA PHE B 45 24.847 23.737 24.377 1.00 48.32 C ATOM 1583 CB PHE B 45 25.553 24.826 23.572 1.00 47.65 C ATOM 1584 CG PHE B 45 24.955 25.064 22.207 1.00 45.89 C ATOM 1585 CD1 PHE B 45 25.111 24.129 21.172 1.00 45.96 C ATOM 1586 CE1 PHE B 45 24.572 24.365 19.904 1.00 50.10 C ATOM 1587 CZ PHE B 45 23.862 25.541 19.669 1.00 47.05 C ATOM 1588 CE2 PHE B 45 23.710 26.476 20.686 1.00 40.41 C ATOM 1589 CD2 PHE B 45 24.253 26.226 21.951 1.00 47.70 C ATOM 1590 C PHE B 45 25.692 23.372 25.580 1.00 49.49 C ATOM 1591 O PHE B 45 26.274 24.243 26.245 1.00 50.60 O ATOM 1592 N LEU B 46 25.767 22.079 25.849 1.00 50.95 N ATOM 1593 CA LEU B 46 26.364 21.592 27.087 1.00 51.22 C ATOM 1594 CB LEU B 46 25.730 20.261 27.487 1.00 51.08 C ATOM 1595 CG LEU B 46 24.203 20.190 27.619 1.00 46.10 C ATOM 1596 CD1 LEU B 46 23.796 18.761 27.883 1.00 43.82 C ATOM 1597 CD2 LEU B 46 23.662 21.111 28.694 1.00 48.08 C ATOM 1598 C LEU B 46 27.878 21.452 26.985 1.00 54.27 C ATOM 1599 O LEU B 46 28.397 21.095 25.924 1.00 55.19 O ATOM 1600 N PRO B 47 28.592 21.756 28.088 1.00 55.99 N ATOM 1601 CA PRO B 47 30.002 21.439 28.289 1.00 58.57 C ATOM 1602 CB PRO B 47 30.085 21.210 29.807 1.00 58.59 C ATOM 1603 CG PRO B 47 28.908 21.978 30.394 1.00 59.61 C ATOM 1604 CD PRO B 47 28.053 22.487 29.245 1.00 55.29 C ATOM 1605 C PRO B 47 30.423 20.159 27.568 1.00 60.23 C ATOM 1606 O PRO B 47 29.753 19.124 27.703 1.00 60.06 O ATOM 1607 N GLY B 48 31.512 20.242 26.801 1.00 60.39 N ATOM 1608 CA GLY B 48 32.012 19.118 26.020 1.00 60.52 C ATOM 1609 C GLY B 48 31.089 18.599 24.925 1.00 62.42 C ATOM 1610 O GLY B 48 31.405 18.716 23.725 1.00 62.21 O ATOM 1611 N ALA B 49 29.954 18.032 25.348 1.00 61.80 N ATOM 1612 CA ALA B 49 28.988 17.361 24.474 1.00 61.62 C ATOM 1613 CB ALA B 49 27.858 16.757 25.302 1.00 60.60 C ATOM 1614 C ALA B 49 28.420 18.229 23.345 1.00 62.36 C ATOM 1615 O ALA B 49 28.463 17.833 22.180 1.00 64.81 O ATOM 1616 N GLY B 50 27.894 19.404 23.690 1.00 61.93 N ATOM 1617 CA GLY B 50 27.206 20.263 22.722 1.00 60.75 C ATOM 1618 C GLY B 50 25.706 20.038 22.758 1.00 59.01 C ATOM 1619 O GLY B 50 25.154 19.714 23.818 1.00 58.98 O ATOM 1620 N LEU B 51 25.051 20.190 21.607 1.00 56.06 N ATOM 1621 CA LEU B 51 23.600 19.988 21.513 1.00 55.72 C ATOM 1622 CB LEU B 51 22.923 21.197 20.861 1.00 55.78 C ATOM 1623 CG LEU B 51 21.510 21.607 21.317 1.00 56.57 C ATOM 1624 CD1 LEU B 51 21.260 23.086 21.016 1.00 54.35 C ATOM 1625 CD2 LEU B 51 20.410 20.740 20.712 1.00 51.01 C ATOM 1626 C LEU B 51 23.231 18.687 20.783 1.00 55.37 C ATOM 1627 O LEU B 51 23.654 18.454 19.650 1.00 56.89 O ATOM 1628 N VAL B 52 22.455 17.834 21.449 1.00 52.14 N ATOM 1629 CA VAL B 52 22.091 16.532 20.898 1.00 49.64 C ATOM 1630 CB VAL B 52 22.656 15.331 21.729 1.00 49.25 C ATOM 1631 CG1 VAL B 52 22.280 13.976 21.106 1.00 47.08 C ATOM 1632 CG2 VAL B 52 24.181 15.425 21.866 1.00 51.63 C ATOM 1633 C VAL B 52 20.576 16.444 20.713 1.00 47.40 C ATOM 1634 O VAL B 52 19.796 16.668 21.658 1.00 44.14 O ATOM 1635 N LEU B 53 20.206 16.136 19.465 1.00 46.22 N ATOM 1636 CA LEU B 53 18.839 16.015 18.990 1.00 46.52 C ATOM 1637 CB LEU B 53 18.545 17.067 17.899 1.00 45.04 C ATOM 1638 CG LEU B 53 18.416 18.522 18.330 1.00 49.63 C ATOM 1639 CD1 LEU B 53 18.373 19.404 17.093 1.00 41.47 C ATOM 1640 CD2 LEU B 53 17.178 18.711 19.223 1.00 46.52 C ATOM 1641 C LEU B 53 18.710 14.674 18.333 1.00 46.61 C ATOM 1642 O LEU B 53 19.693 14.160 17.789 1.00 45.23 O ATOM 1643 N ALA B 54 17.488 14.136 18.377 1.00 48.27 N ATOM 1644 CA ALA B 54 17.104 12.922 17.662 1.00 51.02 C ATOM 1645 CB ALA B 54 16.871 11.748 18.636 1.00 54.27 C ATOM 1646 C ALA B 54 15.841 13.229 16.845 1.00 52.58 C ATOM 1647 O ALA B 54 14.711 13.093 17.344 1.00 50.37 O ATOM 1648 N PRO B 55 16.035 13.722 15.606 1.00 51.74 N ATOM 1649 CA PRO B 55 14.941 14.004 14.667 1.00 50.37 C ATOM 1650 CB PRO B 55 15.546 15.065 13.753 1.00 48.25 C ATOM 1651 CG PRO B 55 17.011 14.775 13.743 1.00 49.23 C ATOM 1652 CD PRO B 55 17.352 14.098 15.044 1.00 51.76 C ATOM 1653 C PRO B 55 14.538 12.782 13.846 1.00 49.88 C ATOM 1654 O PRO B 55 15.357 11.906 13.592 1.00 49.10 O ATOM 1655 N GLN B 56 13.281 12.748 13.422 1.00 50.05 N ATOM 1656 CA GLN B 56 12.789 11.680 12.590 1.00 49.58 C ATOM 1657 CB GLN B 56 11.439 11.207 13.119 1.00 49.76 C ATOM 1658 CG GLN B 56 11.343 9.697 13.288 1.00 51.96 C ATOM 1659 CD GLN B 56 12.022 9.182 14.553 1.00 53.57 C ATOM 1660 OE1 GLN B 56 12.667 9.934 15.296 1.00 48.95 O ATOM 1661 NE2 GLN B 56 11.867 7.884 14.805 1.00 44.22 N ATOM 1662 C GLN B 56 12.647 12.193 11.165 1.00 50.12 C ATOM 1663 O GLN B 56 12.295 13.349 10.967 1.00 49.01 O ATOM 1664 N ILE B 57 12.940 11.338 10.185 1.00 50.19 N ATOM 1665 CA ILE B 57 12.631 11.616 8.774 1.00 52.05 C ATOM 1666 CB ILE B 57 12.797 10.340 7.884 1.00 50.70 C ATOM 1667 CG1 ILE B 57 14.270 9.879 7.814 1.00 52.97 C ATOM 1668 CD1 ILE B 57 15.269 10.917 7.322 1.00 50.34 C ATOM 1669 CG2 ILE B 57 12.200 10.527 6.505 1.00 55.73 C ATOM 1670 C ILE B 57 11.211 12.192 8.661 1.00 53.21 C ATOM 1671 O ILE B 57 10.235 11.604 9.151 1.00 52.05 O ATOM 1672 N GLY B 58 11.116 13.365 8.041 1.00 54.38 N ATOM 1673 CA GLY B 58 9.867 14.110 7.975 1.00 56.00 C ATOM 1674 C GLY B 58 9.901 15.371 8.822 1.00 56.89 C ATOM 1675 O GLY B 58 9.095 16.282 8.619 1.00 57.36 O ATOM 1676 N ASP B 59 10.839 15.415 9.769 1.00 57.12 N ATOM 1677 CA ASP B 59 10.966 16.522 10.724 1.00 55.47 C ATOM 1678 CB ASP B 59 12.019 16.195 11.775 1.00 55.05 C ATOM 1679 C ASP B 59 11.341 17.828 10.060 1.00 53.03 C ATOM 1680 O ASP B 59 11.925 17.823 8.984 1.00 53.44 O ATOM 1681 N LYS B 60 10.992 18.933 10.723 1.00 51.30 N ATOM 1682 CA LYS B 60 11.409 20.285 10.345 1.00 47.93 C ATOM 1683 CB LYS B 60 10.238 21.096 9.783 1.00 48.26 C ATOM 1684 CG LYS B 60 9.889 20.884 8.297 1.00 46.39 C ATOM 1685 CD LYS B 60 9.229 22.177 7.740 1.00 47.01 C ATOM 1686 CE LYS B 60 8.534 21.992 6.395 1.00 52.74 C ATOM 1687 NZ LYS B 60 7.991 23.324 5.847 1.00 44.78 N ATOM 1688 C LYS B 60 11.979 20.988 11.586 1.00 46.25 C ATOM 1689 O LYS B 60 11.384 20.949 12.655 1.00 45.18 O ATOM 1690 N LEU B 61 13.142 21.608 11.435 1.00 45.65 N ATOM 1691 CA LEU B 61 13.799 22.335 12.521 1.00 44.72 C ATOM 1692 CB LEU B 61 14.975 21.527 13.077 1.00 45.50 C ATOM 1693 CG LEU B 61 15.939 22.130 14.107 1.00 47.54 C ATOM 1694 CD1 LEU B 61 15.354 22.084 15.519 1.00 39.59 C ATOM 1695 CD2 LEU B 61 17.286 21.432 14.072 1.00 46.47 C ATOM 1696 C LEU B 61 14.325 23.667 12.016 1.00 42.76 C ATOM 1697 O LEU B 61 14.990 23.713 10.980 1.00 42.46 O ATOM 1698 N ASP B 62 14.022 24.732 12.754 1.00 39.20 N ATOM 1699 CA ASP B 62 14.588 26.045 12.507 1.00 40.51 C ATOM 1700 CB ASP B 62 13.553 27.146 12.773 1.00 38.33 C ATOM 1701 CG ASP B 62 12.304 27.020 11.914 1.00 43.05 C ATOM 1702 OD1 ASP B 62 11.233 27.448 12.381 1.00 53.67 O ATOM 1703 OD2 ASP B 62 12.363 26.508 10.779 1.00 50.75 O ATOM 1704 C ASP B 62 15.791 26.280 13.419 1.00 40.29 C ATOM 1705 O ASP B 62 15.676 26.176 14.649 1.00 44.71 O ATOM 1706 N ILE B 63 16.941 26.612 12.824 1.00 39.54 N ATOM 1707 CA ILE B 63 18.070 27.149 13.567 1.00 40.77 C ATOM 1708 CB ILE B 63 19.371 26.483 13.157 1.00 41.56 C ATOM 1709 CG1 ILE B 63 19.243 24.966 13.300 1.00 38.50 C ATOM 1710 CD1 ILE B 63 20.358 24.219 12.616 1.00 50.40 C ATOM 1711 CG2 ILE B 63 20.556 27.016 13.981 1.00 41.42 C ATOM 1712 C ILE B 63 18.112 28.688 13.321 1.00 40.07 C ATOM 1713 O ILE B 63 18.179 29.139 12.167 1.00 42.17 O ATOM 1714 N ILE B 64 18.039 29.468 14.402 1.00 40.38 N ATOM 1715 CA ILE B 64 17.839 30.952 14.299 1.00 42.37 C ATOM 1716 CB ILE B 64 16.539 31.409 15.011 1.00 44.09 C ATOM 1717 CG1 ILE B 64 15.325 30.676 14.458 1.00 40.39 C ATOM 1718 CD1 ILE B 64 15.048 29.389 15.178 1.00 47.96 C ATOM 1719 CG2 ILE B 64 16.338 32.965 14.883 1.00 40.44 C ATOM 1720 C ILE B 64 18.945 31.742 14.953 1.00 45.33 C ATOM 1721 O ILE B 64 19.215 31.530 16.138 1.00 44.27 O ATOM 1722 N CYS B 65 19.576 32.658 14.212 1.00 47.81 N ATOM 1723 CA CYS B 65 20.440 33.650 14.849 1.00 50.81 C ATOM 1724 CB CYS B 65 21.625 34.041 13.976 1.00 52.46 C ATOM 1725 SG CYS B 65 22.840 32.737 13.887 1.00 57.22 S ATOM 1726 C CYS B 65 19.604 34.870 15.232 1.00 52.50 C ATOM 1727 O CYS B 65 19.169 35.632 14.361 1.00 51.32 O ATOM 1728 N PRO B 66 19.427 35.090 16.523 1.00 52.38 N ATOM 1729 CA PRO B 66 18.436 36.051 17.007 1.00 56.14 C ATOM 1730 CB PRO B 66 18.428 35.810 18.510 1.00 56.30 C ATOM 1731 CG PRO B 66 18.947 34.448 18.672 1.00 55.10 C ATOM 1732 CD PRO B 66 19.955 34.262 17.611 1.00 53.36 C ATOM 1733 C PRO B 66 18.780 37.503 16.701 1.00 57.91 C ATOM 1734 O PRO B 66 19.943 37.887 16.680 1.00 55.40 O ATOM 1735 N LYS B 67 17.742 38.289 16.445 1.00 61.44 N ATOM 1736 CA LYS B 67 17.760 39.738 16.596 1.00 63.19 C ATOM 1737 CB LYS B 67 16.324 40.238 16.522 1.00 63.03 C ATOM 1738 CG LYS B 67 16.105 41.449 15.671 1.00 63.45 C ATOM 1739 CD LYS B 67 14.634 41.608 15.386 1.00 61.61 C ATOM 1740 CE LYS B 67 14.307 43.020 14.962 1.00 65.44 C ATOM 1741 NZ LYS B 67 13.998 43.916 16.102 1.00 65.01 N ATOM 1742 C LYS B 67 18.341 40.152 17.937 1.00 65.68 C ATOM 1743 O LYS B 67 17.926 39.645 18.972 1.00 66.30 O ATOM 1744 N VAL B 68 19.271 41.098 17.938 1.00 66.29 N ATOM 1745 CA VAL B 68 19.561 41.816 19.174 1.00 67.49 C ATOM 1746 CB VAL B 68 20.942 41.501 19.750 1.00 66.82 C ATOM 1747 CG1 VAL B 68 21.073 40.009 20.042 1.00 66.77 C ATOM 1748 CG2 VAL B 68 22.021 41.977 18.826 1.00 63.95 C ATOM 1749 C VAL B 68 19.320 43.312 19.154 1.00 68.26 C ATOM 1750 O VAL B 68 20.061 44.068 18.532 1.00 68.98 O ATOM 1751 N ASP B 69 18.285 43.722 19.874 1.00 69.20 N ATOM 1752 CA ASP B 69 17.631 45.029 19.687 1.00 70.92 C ATOM 1753 CB ASP B 69 16.119 44.881 19.934 1.00 69.99 C ATOM 1754 CG ASP B 69 15.638 43.433 19.795 1.00 67.08 C ATOM 1755 OD1 ASP B 69 15.978 42.783 18.785 1.00 72.72 O ATOM 1756 OD2 ASP B 69 14.922 42.943 20.695 1.00 57.27 O ATOM 1757 C ASP B 69 18.207 46.160 20.561 1.00 72.50 C ATOM 1758 O ASP B 69 19.151 45.945 21.321 1.00 72.58 O ATOM 1759 N SER B 70 17.640 47.363 20.434 1.00 74.73 N ATOM 1760 CA SER B 70 18.004 48.508 21.287 1.00 77.16 C ATOM 1761 C SER B 70 17.679 48.211 22.755 1.00 79.24 C ATOM 1762 O SER B 70 18.492 48.469 23.649 1.00 78.89 O ATOM 1763 N LYS B 71 16.472 47.687 22.980 1.00 81.34 N ATOM 1764 CA LYS B 71 16.098 47.035 24.233 1.00 82.67 C ATOM 1765 CB LYS B 71 14.669 47.409 24.636 1.00 82.35 C ATOM 1766 C LYS B 71 16.220 45.520 24.021 1.00 84.04 C ATOM 1767 O LYS B 71 15.557 44.961 23.145 1.00 84.71 O ATOM 1768 N THR B 72 17.059 44.882 24.841 1.00 84.98 N ATOM 1769 CA THR B 72 17.545 43.485 24.692 1.00 85.61 C ATOM 1770 CB THR B 72 16.758 42.603 23.646 1.00 85.57 C ATOM 1771 OG1 THR B 72 15.358 42.607 23.953 1.00 85.29 O ATOM 1772 CG2 THR B 72 17.245 41.149 23.662 1.00 85.71 C ATOM 1773 C THR B 72 19.066 43.520 24.425 1.00 85.75 C ATOM 1774 O THR B 72 19.580 42.865 23.508 1.00 85.63 O ATOM 1775 N VAL B 73 19.754 44.316 25.251 1.00 85.63 N ATOM 1776 CA VAL B 73 21.222 44.480 25.269 1.00 85.19 C ATOM 1777 CB VAL B 73 21.959 43.217 25.841 1.00 85.28 C ATOM 1778 CG1 VAL B 73 23.410 43.546 26.233 1.00 83.57 C ATOM 1779 CG2 VAL B 73 21.210 42.646 27.045 1.00 85.78 C ATOM 1780 C VAL B 73 21.832 44.916 23.925 1.00 84.59 C ATOM 1781 O VAL B 73 21.193 44.830 22.878 1.00 83.42 O ATOM 1782 N GLY B 74 23.063 45.414 23.979 1.00 84.51 N ATOM 1783 CA GLY B 74 23.854 45.647 22.777 1.00 84.58 C ATOM 1784 C GLY B 74 24.647 44.398 22.419 1.00 84.25 C ATOM 1785 O GLY B 74 24.482 43.338 23.053 1.00 85.08 O ATOM 1786 N GLN B 75 25.505 44.526 21.403 1.00 81.57 N ATOM 1787 CA GLN B 75 26.417 43.453 20.965 1.00 78.55 C ATOM 1788 CB GLN B 75 27.350 42.999 22.102 1.00 78.75 C ATOM 1789 CG GLN B 75 28.402 44.045 22.503 1.00 80.96 C ATOM 1790 CD GLN B 75 28.668 44.097 24.009 1.00 83.13 C ATOM 1791 OE1 GLN B 75 27.757 43.914 24.820 1.00 84.28 O ATOM 1792 NE2 GLN B 75 29.919 44.367 24.384 1.00 81.04 N ATOM 1793 C GLN B 75 25.697 42.268 20.311 1.00 74.88 C ATOM 1794 O GLN B 75 24.789 41.663 20.884 1.00 75.60 O ATOM 1795 N TYR B 76 26.122 41.964 19.091 1.00 70.64 N ATOM 1796 CA TYR B 76 25.579 40.870 18.305 1.00 65.82 C ATOM 1797 CB TYR B 76 25.256 41.387 16.895 1.00 62.96 C ATOM 1798 CG TYR B 76 24.610 40.413 15.931 1.00 60.95 C ATOM 1799 CD1 TYR B 76 23.314 39.923 16.135 1.00 59.30 C ATOM 1800 CE1 TYR B 76 22.729 39.027 15.221 1.00 60.32 C ATOM 1801 CZ TYR B 76 23.449 38.640 14.090 1.00 58.00 C ATOM 1802 OH TYR B 76 22.931 37.778 13.142 1.00 58.90 O ATOM 1803 CE2 TYR B 76 24.721 39.138 13.879 1.00 60.57 C ATOM 1804 CD2 TYR B 76 25.285 40.017 14.784 1.00 54.01 C ATOM 1805 C TYR B 76 26.608 39.745 18.286 1.00 63.37 C ATOM 1806 O TYR B 76 27.806 39.995 18.413 1.00 62.55 O ATOM 1807 N GLU B 77 26.138 38.508 18.149 1.00 59.87 N ATOM 1808 CA GLU B 77 27.034 37.352 18.091 1.00 57.95 C ATOM 1809 CB GLU B 77 26.501 36.220 18.980 1.00 58.47 C ATOM 1810 C GLU B 77 27.268 36.895 16.648 1.00 54.89 C ATOM 1811 O GLU B 77 26.396 36.283 16.024 1.00 53.41 O ATOM 1812 N TYR B 78 28.445 37.217 16.117 1.00 52.94 N ATOM 1813 CA TYR B 78 28.764 36.914 14.721 1.00 52.55 C ATOM 1814 CB TYR B 78 29.841 37.877 14.187 1.00 53.56 C ATOM 1815 CG TYR B 78 29.332 39.285 13.930 1.00 49.81 C ATOM 1816 CD1 TYR B 78 29.291 40.237 14.950 1.00 55.06 C ATOM 1817 CE1 TYR B 78 28.813 41.535 14.712 1.00 51.22 C ATOM 1818 CZ TYR B 78 28.382 41.875 13.446 1.00 48.74 C ATOM 1819 OH TYR B 78 27.919 43.147 13.187 1.00 53.04 O ATOM 1820 CE2 TYR B 78 28.427 40.953 12.419 1.00 46.58 C ATOM 1821 CD2 TYR B 78 28.904 39.670 12.660 1.00 51.58 C ATOM 1822 C TYR B 78 29.184 35.451 14.537 1.00 55.29 C ATOM 1823 O TYR B 78 30.229 35.031 15.035 1.00 55.26 O ATOM 1824 N TYR B 79 28.352 34.674 13.835 1.00 54.89 N ATOM 1825 CA TYR B 79 28.705 33.305 13.441 1.00 52.92 C ATOM 1826 CB TYR B 79 27.939 32.276 14.265 1.00 53.97 C ATOM 1827 CG TYR B 79 27.973 32.471 15.754 1.00 55.14 C ATOM 1828 CD1 TYR B 79 26.875 33.015 16.422 1.00 55.96 C ATOM 1829 CE1 TYR B 79 26.891 33.184 17.792 1.00 58.12 C ATOM 1830 CZ TYR B 79 28.014 32.806 18.514 1.00 55.57 C ATOM 1831 OH TYR B 79 28.030 32.989 19.863 1.00 57.86 O ATOM 1832 CE2 TYR B 79 29.121 32.269 17.875 1.00 56.26 C ATOM 1833 CD2 TYR B 79 29.091 32.099 16.501 1.00 53.27 C ATOM 1834 C TYR B 79 28.420 32.995 11.981 1.00 54.07 C ATOM 1835 O TYR B 79 27.498 33.556 11.392 1.00 52.83 O ATOM 1836 N LYS B 80 29.220 32.085 11.415 1.00 53.13 N ATOM 1837 CA LYS B 80 28.866 31.360 10.191 1.00 52.07 C ATOM 1838 CB LYS B 80 29.990 31.406 9.149 1.00 51.71 C ATOM 1839 CG LYS B 80 30.016 32.654 8.280 1.00 56.46 C ATOM 1840 CD LYS B 80 31.021 32.499 7.152 1.00 55.08 C ATOM 1841 CE LYS B 80 30.814 33.552 6.082 1.00 59.80 C ATOM 1842 NZ LYS B 80 30.966 34.942 6.603 1.00 62.51 N ATOM 1843 C LYS B 80 28.605 29.907 10.582 1.00 51.02 C ATOM 1844 O LYS B 80 29.467 29.247 11.169 1.00 49.01 O ATOM 1845 N VAL B 81 27.425 29.402 10.255 1.00 48.00 N ATOM 1846 CA VAL B 81 27.048 28.066 10.703 1.00 48.41 C ATOM 1847 CB VAL B 81 25.668 28.073 11.413 1.00 45.24 C ATOM 1848 CG1 VAL B 81 25.360 26.732 12.037 1.00 49.15 C ATOM 1849 CG2 VAL B 81 25.649 29.118 12.482 1.00 46.44 C ATOM 1850 C VAL B 81 27.101 27.130 9.509 1.00 50.06 C ATOM 1851 O VAL B 81 26.679 27.501 8.411 1.00 50.73 O ATOM 1852 N TYR B 82 27.620 25.923 9.722 1.00 50.39 N ATOM 1853 CA TYR B 82 27.909 24.998 8.622 1.00 51.80 C ATOM 1854 CB TYR B 82 29.422 24.860 8.414 1.00 50.05 C ATOM 1855 CG TYR B 82 30.088 26.033 7.741 1.00 55.29 C ATOM 1856 CD1 TYR B 82 30.609 27.094 8.492 1.00 60.37 C ATOM 1857 CE1 TYR B 82 31.237 28.183 7.871 1.00 59.32 C ATOM 1858 CZ TYR B 82 31.357 28.209 6.486 1.00 60.82 C ATOM 1859 OH TYR B 82 31.973 29.283 5.860 1.00 56.78 O ATOM 1860 CE2 TYR B 82 30.862 27.153 5.726 1.00 60.90 C ATOM 1861 CD2 TYR B 82 30.221 26.079 6.361 1.00 56.29 C ATOM 1862 C TYR B 82 27.352 23.617 8.889 1.00 51.81 C ATOM 1863 O TYR B 82 27.264 23.196 10.039 1.00 52.65 O ATOM 1864 N MET B 83 26.999 22.916 7.815 1.00 52.67 N ATOM 1865 CA MET B 83 26.743 21.484 7.884 1.00 54.74 C ATOM 1866 CB MET B 83 25.601 21.099 6.941 1.00 55.19 C ATOM 1867 CG MET B 83 25.406 19.614 6.751 1.00 55.78 C ATOM 1868 SD MET B 83 24.629 18.846 8.168 1.00 62.13 S ATOM 1869 CE MET B 83 22.912 18.982 7.717 1.00 53.46 C ATOM 1870 C MET B 83 28.047 20.750 7.522 1.00 55.00 C ATOM 1871 O MET B 83 28.531 20.846 6.387 1.00 53.90 O ATOM 1872 N VAL B 84 28.621 20.054 8.505 1.00 55.21 N ATOM 1873 CA VAL B 84 29.917 19.375 8.347 1.00 52.74 C ATOM 1874 CB VAL B 84 30.977 19.860 9.389 1.00 50.47 C ATOM 1875 CG1 VAL B 84 31.411 21.268 9.096 1.00 46.44 C ATOM 1876 CG2 VAL B 84 30.466 19.738 10.816 1.00 49.60 C ATOM 1877 C VAL B 84 29.801 17.856 8.434 1.00 55.22 C ATOM 1878 O VAL B 84 28.712 17.308 8.613 1.00 55.27 O ATOM 1879 N ASP B 85 30.946 17.194 8.289 1.00 57.58 N ATOM 1880 CA ASP B 85 31.090 15.759 8.523 1.00 59.75 C ATOM 1881 CB ASP B 85 32.035 15.146 7.471 1.00 61.05 C ATOM 1882 CG ASP B 85 33.409 15.825 7.436 1.00 65.18 C ATOM 1883 OD1 ASP B 85 33.598 16.760 6.623 1.00 67.19 O ATOM 1884 OD2 ASP B 85 34.298 15.421 8.224 1.00 68.81 O ATOM 1885 C ASP B 85 31.603 15.485 9.949 1.00 57.67 C ATOM 1886 O ASP B 85 32.138 16.374 10.606 1.00 59.66 O ATOM 1887 N LYS B 86 31.433 14.256 10.423 1.00 57.11 N ATOM 1888 CA LYS B 86 31.936 13.859 11.738 1.00 54.53 C ATOM 1889 CB LYS B 86 31.798 12.349 11.916 1.00 52.85 C ATOM 1890 CG LYS B 86 32.434 11.817 13.179 1.00 44.47 C ATOM 1891 CD LYS B 86 32.959 10.389 12.950 1.00 41.89 C ATOM 1892 CE LYS B 86 32.765 9.541 14.174 1.00 38.48 C ATOM 1893 NZ LYS B 86 33.495 10.036 15.379 1.00 47.23 N ATOM 1894 C LYS B 86 33.389 14.294 12.000 1.00 55.95 C ATOM 1895 O LYS B 86 33.713 14.762 13.093 1.00 55.26 O ATOM 1896 N ASP B 87 34.253 14.147 10.999 1.00 57.71 N ATOM 1897 CA ASP B 87 35.673 14.480 11.149 1.00 60.04 C ATOM 1898 CB ASP B 87 36.528 13.745 10.107 1.00 59.81 C ATOM 1899 CG ASP B 87 37.035 12.406 10.606 1.00 64.01 C ATOM 1900 OD1 ASP B 87 37.633 12.362 11.709 1.00 62.33 O ATOM 1901 OD2 ASP B 87 36.847 11.399 9.882 1.00 62.56 O ATOM 1902 C ASP B 87 35.941 15.980 11.078 1.00 60.97 C ATOM 1903 O ASP B 87 36.953 16.449 11.581 1.00 61.10 O ATOM 1904 N GLN B 88 35.057 16.738 10.446 1.00 61.32 N ATOM 1905 CA GLN B 88 35.265 18.178 10.363 1.00 63.39 C ATOM 1906 CB GLN B 88 34.473 18.784 9.208 1.00 63.94 C ATOM 1907 C GLN B 88 34.837 18.810 11.667 1.00 64.84 C ATOM 1908 O GLN B 88 35.222 19.929 11.983 1.00 65.42 O ATOM 1909 N ALA B 89 34.040 18.061 12.417 1.00 65.49 N ATOM 1910 CA ALA B 89 33.424 18.533 13.644 1.00 65.15 C ATOM 1911 CB ALA B 89 31.989 18.034 13.731 1.00 65.66 C ATOM 1912 C ALA B 89 34.212 18.022 14.824 1.00 64.18 C ATOM 1913 O ALA B 89 34.544 18.765 15.735 1.00 63.09 O ATOM 1914 O ASP B 90 36.855 17.048 17.406 1.00 20.00 O ATOM 1915 N ASP B 90 34.503 16.731 14.795 1.00 20.00 N ATOM 1916 CA ASP B 90 35.305 16.114 15.829 1.00 20.00 C ATOM 1917 C ASP B 90 36.371 17.098 16.280 1.00 20.00 C ATOM 1918 CB ASP B 90 35.928 14.827 15.303 1.00 20.00 C ATOM 1919 CG ASP B 90 35.238 13.602 15.839 1.00 20.00 C ATOM 1920 OD1 ASP B 90 34.100 13.741 16.329 1.00 20.00 O ATOM 1921 OD2 ASP B 90 35.838 12.510 15.788 1.00 20.00 O ATOM 1922 O ARG B 91 38.909 20.743 14.930 1.00 20.00 O ATOM 1923 N ARG B 91 36.693 18.021 15.390 1.00 20.00 N ATOM 1924 CA ARG B 91 38.029 18.543 15.278 1.00 20.00 C ATOM 1925 C ARG B 91 37.934 19.999 14.865 1.00 20.00 C ATOM 1926 CB ARG B 91 38.794 17.757 14.225 1.00 20.00 C ATOM 1927 N CYS B 92 36.744 20.402 14.436 1.00 65.62 N ATOM 1928 CA CYS B 92 36.377 21.803 14.449 1.00 63.54 C ATOM 1929 CB CYS B 92 36.658 22.414 15.813 1.00 62.30 C ATOM 1930 SG CYS B 92 35.415 22.029 17.030 1.00 61.91 S ATOM 1931 C CYS B 92 37.103 22.560 13.364 1.00 63.64 C ATOM 1932 O CYS B 92 37.751 23.557 13.622 1.00 62.94 O ATOM 1933 N THR B 93 36.973 22.076 12.139 1.00 66.00 N ATOM 1934 CA THR B 93 37.644 22.682 10.998 1.00 69.32 C ATOM 1935 CB THR B 93 38.992 21.965 10.653 1.00 69.46 C ATOM 1936 OG1 THR B 93 39.501 22.457 9.406 1.00 71.08 O ATOM 1937 CG2 THR B 93 38.813 20.447 10.563 1.00 67.96 C ATOM 1938 C THR B 93 36.711 22.682 9.798 1.00 70.96 C ATOM 1939 O THR B 93 36.174 21.638 9.422 1.00 72.14 O ATOM 1940 N ILE B 94 36.500 23.868 9.231 1.00 72.37 N ATOM 1941 CA ILE B 94 35.749 24.019 7.985 1.00 73.47 C ATOM 1942 CB ILE B 94 34.519 24.973 8.129 1.00 72.37 C ATOM 1943 CG1 ILE B 94 34.943 26.416 8.425 1.00 71.50 C ATOM 1944 CD1 ILE B 94 34.846 27.339 7.244 1.00 65.08 C ATOM 1945 CG2 ILE B 94 33.571 24.464 9.211 1.00 72.82 C ATOM 1946 C ILE B 94 36.699 24.430 6.851 1.00 74.87 C ATOM 1947 O ILE B 94 36.281 24.598 5.701 1.00 74.36 O ATOM 1948 N LYS B 95 37.979 24.587 7.201 1.00 76.69 N ATOM 1949 CA LYS B 95 39.050 24.828 6.236 1.00 78.11 C ATOM 1950 CB LYS B 95 40.345 25.209 6.955 1.00 77.98 C ATOM 1951 C LYS B 95 39.231 23.555 5.414 1.00 79.85 C ATOM 1952 O LYS B 95 40.318 22.964 5.359 1.00 80.52 O ATOM 1953 N LYS B 96 38.132 23.164 4.770 1.00 80.67 N ATOM 1954 CA LYS B 96 37.946 21.878 4.109 1.00 80.88 C ATOM 1955 CB LYS B 96 38.263 20.732 5.106 1.00 80.35 C ATOM 1956 CG LYS B 96 37.430 19.457 5.056 1.00 79.50 C ATOM 1957 CD LYS B 96 36.505 19.334 6.265 1.00 77.17 C ATOM 1958 CE LYS B 96 35.924 20.675 6.665 1.00 77.09 C ATOM 1959 NZ LYS B 96 34.524 20.596 7.133 1.00 76.80 N ATOM 1960 C LYS B 96 36.494 21.937 3.589 1.00 81.93 C ATOM 1961 O LYS B 96 35.881 23.011 3.640 1.00 82.40 O ATOM 1962 N GLU B 97 35.953 20.832 3.071 1.00 82.44 N ATOM 1963 CA GLU B 97 34.574 20.804 2.541 1.00 82.95 C ATOM 1964 CB GLU B 97 34.245 19.415 1.978 1.00 82.71 C ATOM 1965 C GLU B 97 33.513 21.250 3.575 1.00 82.95 C ATOM 1966 O GLU B 97 33.406 20.664 4.663 1.00 83.36 O ATOM 1967 N ASN B 98 32.746 22.291 3.233 1.00 81.59 N ATOM 1968 CA ASN B 98 31.794 22.911 4.171 1.00 79.66 C ATOM 1969 CB ASN B 98 32.549 23.709 5.239 1.00 80.02 C ATOM 1970 C ASN B 98 30.731 23.801 3.511 1.00 78.31 C ATOM 1971 O ASN B 98 31.048 24.644 2.660 1.00 77.79 O ATOM 1972 N THR B 99 29.478 23.620 3.932 1.00 76.30 N ATOM 1973 CA THR B 99 28.321 24.312 3.327 1.00 74.52 C ATOM 1974 CB THR B 99 27.334 23.301 2.663 1.00 74.67 C ATOM 1975 OG1 THR B 99 27.823 21.957 2.811 1.00 73.98 O ATOM 1976 CG2 THR B 99 27.139 23.624 1.182 1.00 73.78 C ATOM 1977 C THR B 99 27.570 25.185 4.363 1.00 72.17 C ATOM 1978 O THR B 99 26.920 24.645 5.274 1.00 72.60 O ATOM 1979 N PRO B 100 27.641 26.530 4.214 1.00 68.26 N ATOM 1980 CA PRO B 100 27.251 27.464 5.286 1.00 65.84 C ATOM 1981 CB PRO B 100 28.052 28.743 4.960 1.00 65.48 C ATOM 1982 CG PRO B 100 28.612 28.545 3.556 1.00 66.33 C ATOM 1983 CD PRO B 100 28.070 27.252 3.005 1.00 68.07 C ATOM 1984 C PRO B 100 25.752 27.753 5.352 1.00 62.59 C ATOM 1985 O PRO B 100 25.240 28.596 4.605 1.00 63.79 O ATOM 1986 N LEU B 101 25.071 27.056 6.259 1.00 59.41 N ATOM 1987 CA LEU B 101 23.617 27.127 6.403 1.00 56.35 C ATOM 1988 CB LEU B 101 23.105 25.985 7.290 1.00 56.25 C ATOM 1989 CG LEU B 101 23.449 24.556 6.871 1.00 53.36 C ATOM 1990 CD1 LEU B 101 22.629 23.566 7.659 1.00 57.33 C ATOM 1991 CD2 LEU B 101 23.255 24.344 5.374 1.00 48.21 C ATOM 1992 C LEU B 101 23.126 28.455 6.951 1.00 56.12 C ATOM 1993 O LEU B 101 22.025 28.905 6.620 1.00 55.96 O ATOM 1994 N LEU B 102 23.923 29.074 7.812 1.00 54.26 N ATOM 1995 CA LEU B 102 23.641 30.435 8.253 1.00 52.03 C ATOM 1996 CB LEU B 102 23.173 30.459 9.708 1.00 52.13 C ATOM 1997 CG LEU B 102 21.954 29.702 10.235 1.00 50.45 C ATOM 1998 CD1 LEU B 102 22.041 29.695 11.719 1.00 55.04 C ATOM 1999 CD2 LEU B 102 20.692 30.392 9.827 1.00 60.55 C ATOM 2000 C LEU B 102 24.870 31.323 8.140 1.00 52.59 C ATOM 2001 O LEU B 102 25.984 30.933 8.523 1.00 51.55 O ATOM 2002 N ASN B 103 24.655 32.521 7.621 1.00 53.64 N ATOM 2003 CA ASN B 103 25.600 33.615 7.793 1.00 54.00 C ATOM 2004 CB ASN B 103 25.998 34.252 6.467 1.00 54.78 C ATOM 2005 CG ASN B 103 26.931 35.436 6.665 1.00 58.33 C ATOM 2006 OD1 ASN B 103 28.084 35.271 7.084 1.00 58.48 O ATOM 2007 ND2 ASN B 103 26.424 36.643 6.399 1.00 45.80 N ATOM 2008 C ASN B 103 25.015 34.670 8.720 1.00 53.18 C ATOM 2009 O ASN B 103 24.442 35.657 8.267 1.00 54.82 O ATOM 2010 N CYS B 104 25.172 34.463 10.023 1.00 52.46 N ATOM 2011 CA CYS B 104 24.649 35.394 11.007 1.00 51.44 C ATOM 2012 CB CYS B 104 24.466 34.700 12.341 1.00 53.41 C ATOM 2013 SG CYS B 104 23.832 33.036 12.178 1.00 49.61 S ATOM 2014 C CYS B 104 25.604 36.556 11.139 1.00 53.20 C ATOM 2015 O CYS B 104 26.565 36.513 11.915 1.00 51.74 O ATOM 2016 N ALA B 105 25.335 37.578 10.338 1.00 52.80 N ATOM 2017 CA ALA B 105 26.121 38.783 10.298 1.00 52.86 C ATOM 2018 CB ALA B 105 27.202 38.669 9.219 1.00 53.20 C ATOM 2019 C ALA B 105 25.188 39.945 10.006 1.00 53.19 C ATOM 2020 O ALA B 105 25.501 40.812 9.184 1.00 54.31 O ATOM 2021 N ARG B 106 24.030 39.929 10.668 1.00 54.23 N ATOM 2022 CA ARG B 106 23.018 40.988 10.559 1.00 53.54 C ATOM 2023 CB ARG B 106 21.984 40.637 9.480 1.00 53.56 C ATOM 2024 C ARG B 106 22.319 41.211 11.900 1.00 53.50 C ATOM 2025 O ARG B 106 21.322 40.545 12.206 1.00 53.50 O ATOM 2026 N PRO B 107 22.847 42.136 12.715 1.00 53.15 N ATOM 2027 CA PRO B 107 22.255 42.466 14.024 1.00 54.11 C ATOM 2028 CB PRO B 107 23.089 43.666 14.488 1.00 55.59 C ATOM 2029 CG PRO B 107 24.428 43.483 13.797 1.00 51.19 C ATOM 2030 CD PRO B 107 24.091 42.894 12.459 1.00 52.06 C ATOM 2031 C PRO B 107 20.745 42.804 14.041 1.00 56.24 C ATOM 2032 O PRO B 107 20.048 42.480 15.012 1.00 57.46 O ATOM 2033 N ASP B 108 20.245 43.423 12.978 1.00 56.84 N ATOM 2034 CA ASP B 108 18.905 44.009 13.004 1.00 56.83 C ATOM 2035 CB ASP B 108 18.933 45.389 12.354 1.00 58.06 C ATOM 2036 CG ASP B 108 17.754 46.242 12.761 1.00 60.68 C ATOM 2037 OD1 ASP B 108 17.196 46.004 13.857 1.00 64.10 O ATOM 2038 OD2 ASP B 108 17.386 47.154 11.988 1.00 66.86 O ATOM 2039 C ASP B 108 17.823 43.138 12.362 1.00 56.19 C ATOM 2040 O ASP B 108 16.689 43.573 12.151 1.00 53.32 O ATOM 2041 N GLN B 109 18.170 41.887 12.085 1.00 56.39 N ATOM 2042 CA GLN B 109 17.298 41.022 11.324 1.00 55.55 C ATOM 2043 CB GLN B 109 17.632 41.124 9.827 1.00 55.41 C ATOM 2044 CG GLN B 109 17.483 39.837 9.023 1.00 58.46 C ATOM 2045 CD GLN B 109 17.142 40.063 7.561 1.00 61.57 C ATOM 2046 OE1 GLN B 109 17.045 41.204 7.089 1.00 66.19 O ATOM 2047 NE2 GLN B 109 16.949 38.971 6.831 1.00 64.69 N ATOM 2048 C GLN B 109 17.368 39.593 11.852 1.00 57.37 C ATOM 2049 O GLN B 109 18.452 39.029 12.060 1.00 57.65 O ATOM 2050 N ASP B 110 16.192 39.038 12.100 1.00 56.55 N ATOM 2051 CA ASP B 110 16.039 37.669 12.534 1.00 57.00 C ATOM 2052 CB ASP B 110 14.552 37.452 12.871 1.00 58.93 C ATOM 2053 CG ASP B 110 14.329 36.698 14.179 1.00 61.20 C ATOM 2054 OD1 ASP B 110 15.110 36.866 15.149 1.00 64.56 O ATOM 2055 OD2 ASP B 110 13.335 35.946 14.236 1.00 62.44 O ATOM 2056 C ASP B 110 16.481 36.773 11.360 1.00 55.17 C ATOM 2057 O ASP B 110 15.835 36.771 10.316 1.00 56.87 O ATOM 2058 N VAL B 111 17.581 36.039 11.523 1.00 51.13 N ATOM 2059 CA VAL B 111 18.119 35.158 10.471 1.00 47.12 C ATOM 2060 CB VAL B 111 19.647 35.389 10.217 1.00 48.87 C ATOM 2061 CG1 VAL B 111 20.219 34.352 9.227 1.00 53.14 C ATOM 2062 CG2 VAL B 111 19.938 36.818 9.728 1.00 42.07 C ATOM 2063 C VAL B 111 17.921 33.693 10.852 1.00 46.36 C ATOM 2064 O VAL B 111 18.266 33.289 11.975 1.00 42.74 O ATOM 2065 N LYS B 112 17.400 32.898 9.915 1.00 43.12 N ATOM 2066 CA LYS B 112 17.032 31.485 10.162 1.00 43.58 C ATOM 2067 CB LYS B 112 15.546 31.455 10.558 1.00 42.82 C ATOM 2068 CG LYS B 112 14.766 30.199 10.270 1.00 44.74 C ATOM 2069 CD LYS B 112 13.271 30.542 10.259 1.00 48.96 C ATOM 2070 CE LYS B 112 12.691 30.498 11.670 1.00 45.37 C ATOM 2071 NZ LYS B 112 11.754 31.661 11.947 1.00 45.29 N ATOM 2072 C LYS B 112 17.346 30.504 9.003 1.00 42.43 C ATOM 2073 O LYS B 112 17.477 30.921 7.847 1.00 45.59 O ATOM 2074 N PHE B 113 17.513 29.216 9.327 1.00 40.79 N ATOM 2075 CA PHE B 113 17.572 28.148 8.331 1.00 38.79 C ATOM 2076 CB PHE B 113 18.998 27.550 8.153 1.00 39.14 C ATOM 2077 CG PHE B 113 19.104 26.543 6.997 1.00 34.85 C ATOM 2078 CD1 PHE B 113 19.549 26.945 5.741 1.00 35.55 C ATOM 2079 CE1 PHE B 113 19.640 26.015 4.697 1.00 38.24 C ATOM 2080 CZ PHE B 113 19.250 24.709 4.892 1.00 34.91 C ATOM 2081 CE2 PHE B 113 18.807 24.299 6.148 1.00 40.75 C ATOM 2082 CD2 PHE B 113 18.737 25.208 7.177 1.00 44.17 C ATOM 2083 C PHE B 113 16.634 27.073 8.800 1.00 39.23 C ATOM 2084 O PHE B 113 16.731 26.593 9.956 1.00 43.15 O ATOM 2085 N THR B 114 15.728 26.686 7.916 1.00 36.48 N ATOM 2086 CA THR B 114 14.768 25.619 8.184 1.00 36.83 C ATOM 2087 CB THR B 114 13.384 25.985 7.687 1.00 40.83 C ATOM 2088 OG1 THR B 114 12.968 27.231 8.286 1.00 37.54 O ATOM 2089 CG2 THR B 114 12.394 24.877 7.993 1.00 36.72 C ATOM 2090 C THR B 114 15.214 24.313 7.502 1.00 38.84 C ATOM 2091 O THR B 114 15.307 24.201 6.286 1.00 40.09 O ATOM 2092 N ILE B 115 15.501 23.317 8.311 1.00 38.37 N ATOM 2093 CA ILE B 115 15.934 22.042 7.802 1.00 38.31 C ATOM 2094 CB ILE B 115 16.914 21.365 8.790 1.00 38.74 C ATOM 2095 OG1 ILE B 115 18.233 22.145 8.874 1.00 40.45 C ATOM 2096 CD1 ILE B 115 19.179 21.628 9.988 1.00 41.07 C ATOM 2097 CG2 ILE B 115 17.189 19.957 8.376 1.00 37.17 C ATOM 2098 C ILE B 115 14.696 21.197 7.693 1.00 39.26 C ATOM 2099 O ILE B 115 13.905 21.146 8.626 1.00 40.19 O ATOM 2100 N LYS B 116 14.508 20.566 6.539 1.00 38.88 N ATOM 2101 CA LYS B 116 13.586 19.455 6.452 1.00 39.98 C ATOM 2102 CB LYS B 116 12.647 19.601 5.253 1.00 39.37 C ATOM 2103 CG LYS B 116 11.972 18.305 4.805 1.00 40.21 C ATOM 2104 CD LYS B 116 10.761 18.025 5.630 1.00 40.79 C ATOM 2105 CE LYS B 116 9.630 17.361 4.844 1.00 47.35 C ATOM 2106 NZ LYS B 116 10.037 16.252 3.926 1.00 43.81 N ATOM 2107 C LYS B 116 14.408 18.162 6.350 1.00 41.05 C ATOM 2108 O LYS B 116 15.163 17.961 5.393 1.00 40.58 O ATOM 2109 N PHE B 117 14.250 17.299 7.347 1.00 40.29 N ATOM 2110 CA PHE B 117 14.894 15.997 7.368 1.00 40.81 C ATOM 2111 CB PHE B 117 14.958 15.425 8.801 1.00 41.73 C ATOM 2112 CG PHE B 117 15.737 16.291 9.761 1.00 39.87 C ATOM 2113 CD1 PHE B 117 15.091 17.297 10.487 1.00 40.27 C ATOM 2114 CE1 PHE B 117 15.791 18.118 11.354 1.00 36.48 C ATOM 2115 CZ PHE B 117 17.174 17.971 11.468 1.00 40.12 C ATOM 2116 CE2 PHE B 117 17.845 16.976 10.706 1.00 36.80 C ATOM 2117 CD2 PHE B 117 17.121 16.151 9.874 1.00 34.89 C ATOM 2118 C PHE B 117 14.109 15.078 6.451 1.00 42.46 C ATOM 2119 O PHE B 117 13.074 14.534 6.839 1.00 42.34 O ATOM 2120 N GLN B 118 14.599 14.956 5.220 1.00 43.34 N ATOM 2121 CA GLN B 118 14.001 14.143 4.168 1.00 42.93 C ATOM 2122 CB GLN B 118 13.223 15.038 3.177 1.00 47.34 C ATOM 2123 CG GLN B 118 14.085 16.077 2.491 1.00 34.74 C ATOM 2124 CD GLN B 118 13.336 16.995 1.531 1.00 41.59 C ATOM 2125 OE1 GLN B 118 13.710 18.137 1.385 1.00 41.26 O ATOM 2126 NE2 GLN B 118 12.277 16.508 0.896 1.00 37.39 N ATOM 2127 C GLN B 118 15.137 13.401 3.453 1.00 43.86 C ATOM 2128 O GLN B 118 16.281 13.882 3.422 1.00 40.85 O ATOM 2129 N GLU B 119 14.817 12.239 2.873 1.00 45.99 N ATOM 2130 CA GLU B 119 15.833 11.342 2.277 1.00 46.54 C ATOM 2131 CB GLU B 119 15.266 9.924 2.128 1.00 49.19 C ATOM 2132 CG GLU B 119 16.253 8.817 2.513 1.00 54.11 C ATOM 2133 CD GLU B 119 15.932 8.188 3.859 1.00 62.40 C ATOM 2134 OE1 GLU B 119 14.732 8.144 4.211 1.00 69.97 O ATOM 2135 OE2 GLU B 119 16.864 7.725 4.560 1.00 62.46 O ATOM 2136 C GLU B 119 16.375 11.802 0.913 1.00 45.75 C ATOM 2137 O GLU B 119 17.486 11.447 0.523 1.00 46.08 O ATOM 2138 N PHE B 120 15.579 12.606 0.212 1.00 41.97 N ATOM 2139 CA PHE B 120 15.842 13.014 −1.161 1.00 41.19 C ATOM 2140 CB PHE B 120 15.190 11.988 −2.102 1.00 41.38 C ATOM 2141 CG PHE B 120 15.342 12.284 −3.568 1.00 44.79 C ATOM 2142 CD1 PHE B 120 16.433 11.791 −4.276 1.00 46.25 C ATOM 2143 CE1 PHE B 120 16.573 12.041 −5.639 1.00 48.01 C ATOM 2144 CZ PHE B 120 15.597 12.780 −6.311 1.00 48.10 C ATOM 2145 CE2 PHE B 120 14.491 13.269 −5.614 1.00 48.86 C ATOM 2146 CD2 PHE B 120 14.363 13.008 −4.251 1.00 47.10 C ATOM 2147 C PHE B 120 15.235 14.411 −1.339 1.00 38.45 C ATOM 2148 O PHE B 120 14.098 14.642 −0.939 1.00 39.71 O ATOM 2149 N SER B 121 16.001 15.338 −1.908 1.00 38.75 N ATOM 2150 CA SER B 121 15.503 16.687 −2.222 1.00 35.73 C ATOM 2151 CB SER B 121 16.336 17.720 −1.482 1.00 41.04 C ATOM 2152 OG SER B 121 16.075 19.038 −1.979 1.00 32.57 O ATOM 2153 C SER B 121 15.630 16.928 −3.713 1.00 36.73 C ATOM 2154 O SER B 121 16.697 16.644 −4.245 1.00 37.53 O ATOM 2155 N PRO B 122 14.549 17.421 −4.414 1.00 35.00 N ATOM 2156 CA PRO B 122 14.686 17.884 −5.794 1.00 31.41 C ATOM 2157 CB PRO B 122 13.251 18.193 −6.211 1.00 33.87 C ATOM 2158 CG PRO B 122 12.549 18.466 −4.956 1.00 36.13 C ATOM 2159 CD PRO B 122 13.128 17.460 −4.018 1.00 31.71 C ATOM 2160 C PRO B 122 15.605 19.080 −6.037 1.00 34.20 C ATOM 2161 O PRO B 122 15.924 19.376 −7.206 1.00 28.62 O ATOM 2162 N ASN B 123 16.063 19.713 −4.952 1.00 35.06 N ATOM 2163 CA ASN B 123 17.077 20.740 −5.053 1.00 35.87 C ATOM 2164 CB ASN B 123 17.094 21.655 −3.821 1.00 36.31 C ATOM 2165 CG ASN B 123 18.043 22.880 −3.984 1.00 33.87 C ATOM 2166 OD1 ASN B 123 18.656 23.093 −5.032 1.00 32.22 O ATOM 2167 ND2 ASN B 123 18.121 23.693 −2.943 1.00 35.68 N ATOM 2168 C ASN B 123 18.448 20.112 −5.270 1.00 34.15 C ATOM 2169 O ASN B 123 18.928 19.291 −4.469 1.00 33.65 O ATOM 2170 N LEU B 124 19.039 20.510 −6.383 1.00 33.29 N ATOM 2171 CA LEU B 124 20.394 20.196 −6.723 1.00 37.26 C ATOM 2172 CB LEU B 124 20.804 21.083 −7.895 1.00 35.44 C ATOM 2173 CG LEU B 124 22.203 20.963 −8.484 1.00 40.34 C ATOM 2174 CD1 LEU B 124 22.338 19.636 −9.207 1.00 35.24 C ATOM 2175 CD2 LEU B 124 22.360 22.114 −9.433 1.00 38.11 C ATOM 2176 C LEU B 124 21.341 20.364 −5.524 1.00 36.68 C ATOM 2177 O LEU B 124 22.267 19.587 −5.378 1.00 38.26 O ATOM 2178 N TRP B 125 21.088 21.354 −4.662 1.00 37.81 N ATOM 2179 CA TRP B 125 21.878 21.556 −3.442 1.00 41.99 C ATOM 2180 CB TRP B 125 22.371 22.993 −3.331 1.00 44.52 C ATOM 2181 CG TRP B 125 23.266 23.394 −4.426 1.00 48.30 C ATOM 2182 CD1 TRP B 125 24.609 23.183 −4.507 1.00 48.48 C ATOM 2183 NE1 TRP B 125 25.100 23.701 −5.680 1.00 46.89 N ATOM 2184 CE2 TRP B 125 24.065 24.261 −6.381 1.00 48.31 C ATOM 2185 CD2 TRP B 125 22.892 24.093 −5.611 1.00 48.46 C ATOM 2186 CE3 TRP B 125 21.675 24.579 −6.110 1.00 51.01 C ATOM 2187 CZ3 TRP B 125 21.674 25.222 −7.336 1.00 47.38 C ATOM 2188 CH2 TRP B 125 22.857 25.380 −8.074 1.00 47.99 C ATOM 2189 CZ2 TRP B 125 24.062 24.917 −7.611 1.00 47.47 C ATOM 2190 C TRP B 125 21.117 21.240 −2.181 1.00 41.23 C ATOM 2191 O TRP B 125 21.540 21.611 −1.091 1.00 44.51 O ATOM 2192 N GLY B 126 20.007 20.538 −2.321 1.00 40.47 N ATOM 2193 CA GLY B 126 19.175 20.183 −1.183 1.00 40.35 C ATOM 2194 C GLY B 126 19.900 19.357 −0.144 1.00 41.68 C ATOM 2195 O GLY B 126 20.904 18.705 −0.452 1.00 41.73 O ATOM 2196 N LEU B 127 19.384 19.378 1.086 1.00 41.78 N ATOM 2197 CA LEU B 127 19.928 18.578 2.187 1.00 43.54 C ATOM 2198 CB LEU B 127 19.885 19.371 3.502 1.00 45.56 C ATOM 2199 CG LEU B 127 20.829 20.562 3.715 1.00 45.47 C ATOM 2200 CD1 LEU B 127 20.761 21.056 5.145 1.00 47.06 C ATOM 2201 CD2 LEU B 127 22.269 20.227 3.361 1.00 52.41 C ATOM 2202 C LEU B 127 19.169 17.251 2.317 1.00 46.47 C ATOM 2203 O LEU B 127 17.932 17.223 2.246 1.00 45.51 O ATOM 2204 N GLU B 128 19.914 16.151 2.486 1.00 49.01 N ATOM 2205 CA GLU B 128 19.358 14.785 2.392 1.00 50.26 C ATOM 2206 CB GLU B 128 19.662 14.201 1.002 1.00 50.78 C ATOM 2207 CG GLU B 128 19.339 15.167 −0.175 1.00 52.96 C ATOM 2208 CD GLU B 128 19.395 14.518 −1.561 1.00 52.08 C ATOM 2209 OE1 GLU B 128 20.089 13.484 −1.727 1.00 54.11 O ATOM 2210 OE2 GLU B 128 18.733 15.050 −2.500 1.00 44.98 O ATOM 2211 C GLU B 128 19.870 13.866 3.541 1.00 51.60 C ATOM 2212 O GLU B 128 21.053 13.901 3.882 1.00 51.94 O ATOM 2213 N PHE B 129 18.984 13.064 4.143 1.00 50.16 N ATOM 2214 CA PHE B 129 19.301 12.410 5.428 1.00 50.35 C ATOM 2215 CB PHE B 129 18.616 13.148 6.579 1.00 49.69 C ATOM 2216 CG PHE B 129 19.000 14.602 6.689 1.00 53.84 C ATOM 2217 CD1 PHE B 129 18.143 15.602 6.218 1.00 53.48 C ATOM 2218 CE1 PHE B 129 18.497 16.963 6.321 1.00 50.73 C ATOM 2219 CZ PHE B 129 19.718 17.324 6.879 1.00 51.56 C ATOM 2220 CE2 PHE B 129 20.589 16.329 7.349 1.00 56.53 C ATOM 2221 CD2 PHE B 129 20.223 14.982 7.253 1.00 53.44 C ATOM 2222 C PHE B 129 18.985 10.907 5.487 1.00 52.61 C ATOM 2223 O PHE B 129 17.967 10.449 4.950 1.00 51.12 O ATOM 2224 N GLN B 130 19.849 10.151 6.172 1.00 56.51 N ATOM 2225 CA GLN B 130 19.828 8.674 6.124 1.00 59.82 C ATOM 2226 CB GLN B 130 21.247 8.116 5.889 1.00 60.33 C ATOM 2227 CG GLN B 130 22.020 8.753 4.713 1.00 61.86 C ATOM 2228 CD GLN B 130 23.338 8.053 4.385 1.00 60.72 C ATOM 2229 OE1 GLN B 130 23.752 7.113 5.069 1.00 69.64 O ATOM 2230 NE2 GLN B 130 23.997 8.508 3.322 1.00 59.67 N ATOM 2231 C GLN B 130 19.170 7.969 7.328 1.00 60.84 C ATOM 2232 O GLN B 130 19.206 8.461 8.465 1.00 59.63 O ATOM 2233 N ALA B 131 18.610 6.790 7.038 1.00 63.58 N ATOM 2234 CA ALA B 131 17.841 5.932 7.965 1.00 64.07 C ATOM 2235 CB ALA B 131 17.808 4.489 7.434 1.00 64.33 C ATOM 2236 C ALA B 131 18.239 5.947 9.453 1.00 63.60 C ATOM 2237 O ALA B 131 17.463 6.390 10.298 1.00 64.85 O ATOM 2238 N ASN B 132 19.426 5.437 9.765 1.00 61.85 N ATOM 2239 CA ASN B 132 19.939 5.450 11.134 1.00 58.11 C ATOM 2240 CB ASN B 132 19.985 4.033 11.716 1.00 57.70 C ATOM 2241 CG ASN B 132 19.258 3.917 13.056 1.00 57.57 C ATOM 2242 OD1 ASN B 132 19.863 4.027 14.125 1.00 52.75 O ATOM 2243 ND2 ASN B 132 17.953 3.688 12.998 1.00 56.67 N ATOM 2244 C ASN B 132 21.325 6.091 11.097 1.00 56.55 C ATOM 2245 O ASN B 132 22.347 5.409 11.243 1.00 54.32 O ATOM 2246 N LYS B 133 21.343 7.408 10.876 1.00 52.59 N ATOM 2247 CA LYS B 133 22.584 8.143 10.583 1.00 51.69 C ATOM 2248 CB LYS B 133 22.726 8.277 9.055 1.00 52.35 C ATOM 2249 CG LYS B 133 23.788 9.235 8.509 1.00 54.30 C ATOM 2250 CD LYS B 133 25.209 8.685 8.590 1.00 55.71 C ATOM 2251 CE LYS B 133 26.123 9.361 7.560 1.00 56.13 C ATOM 2252 NZ LYS B 133 26.218 10.847 7.729 1.00 55.26 N ATOM 2253 C LYS B 133 22.690 9.507 11.316 1.00 50.35 C ATOM 2254 O LYS B 133 21.680 10.157 11.581 1.00 45.66 O ATOM 2255 N ASP B 134 23.925 9.906 11.646 1.00 50.68 N ATOM 2256 CA ASP B 134 24.219 11.149 12.375 1.00 51.33 C ATOM 2257 CB ASP B 134 25.246 10.914 13.497 1.00 53.85 C ATOM 2258 CG ASP B 134 24.881 9.760 14.403 1.00 54.97 C ATOM 2259 OD1 ASP B 134 23.787 9.792 15.001 1.00 61.14 O ATOM 2260 OD2 ASP B 134 25.692 8.818 14.521 1.00 63.22 O ATOM 2261 C ASP B 134 24.781 12.214 11.446 1.00 51.63 C ATOM 2262 O ASP B 134 25.579 11.910 10.546 1.00 50.16 O ATOM 2263 N TYR B 135 24.368 13.464 11.678 1.00 51.47 N ATOM 2264 CA TYR B 135 24.844 14.617 10.903 1.00 50.95 C ATOM 2265 CB TYR B 135 23.765 15.107 9.945 1.00 51.81 C ATOM 2266 CG TYR B 135 23.375 14.080 8.901 1.00 53.87 C ATOM 2267 CD1 TYR B 135 22.302 13.228 9.120 1.00 55.22 C ATOM 2268 CE1 TYR B 135 21.930 12.280 8.175 1.00 55.50 C ATOM 2269 CZ TYR B 135 22.633 12.174 6.991 1.00 55.59 C ATOM 2270 OH TYR B 135 22.241 11.219 6.075 1.00 55.74 O ATOM 2271 CE2 TYR B 135 23.716 13.008 6.738 1.00 55.39 C ATOM 2272 CD2 TYR B 135 24.082 13.961 7.697 1.00 50.04 C ATOM 2273 C TYR B 135 25.222 15.724 11.857 1.00 50.07 C ATOM 2274 O TYR B 135 24.666 15.811 12.959 1.00 47.79 O ATOM 2275 N TYR B 136 26.169 16.559 11.444 1.00 52.35 N ATOM 2276 CA TYR B 136 26.726 17.566 12.352 1.00 53.64 C ATOM 2277 CB TYR B 136 28.187 17.242 12.691 1.00 56.73 C ATOM 2278 CG TYR B 136 28.423 15.870 13.310 1.00 60.71 C ATOM 2279 CD1 TYR B 136 28.328 14.701 12.541 1.00 63.40 C ATOM 2280 CE1 TYR B 136 28.547 13.453 13.099 1.00 63.12 C ATOM 2281 CZ TYR B 136 28.892 13.353 14.431 1.00 61.25 C ATOM 2282 OH TYR B 136 29.120 12.116 14.984 1.00 61.58 O ATOM 2283 CE2 TYR B 136 29.008 14.494 15.216 1.00 64.20 C ATOM 2284 CD2 TYR B 136 28.772 15.743 14.654 1.00 59.76 C ATOM 2285 C TYR B 136 26.636 18.985 11.820 1.00 52.48 C ATOM 2286 O TYR B 136 26.701 19.225 10.613 1.00 52.71 O ATOM 2287 N ILE B 137 26.509 19.926 12.750 1.00 51.25 N ATOM 2288 CA ILE B 137 26.430 21.344 12.443 1.00 48.75 C ATOM 2289 CB ILE B 137 24.975 21.849 12.481 1.00 51.09 C ATOM 2290 CG1 ILE B 137 24.223 21.481 11.180 1.00 50.13 C ATOM 2291 CD1 ILE B 137 22.704 21.633 11.274 1.00 47.53 C ATOM 2292 CG2 ILE B 137 24.941 23.358 12.811 1.00 40.73 C ATOM 2293 C ILE B 137 27.240 22.060 13.510 1.00 48.65 C ATOM 2294 O ILE B 137 26.978 21.897 14.709 1.00 46.02 O ATOM 2295 N ILE B 138 28.208 22.864 13.067 1.00 46.40 N ATOM 2296 CA ILE B 138 29.125 23.546 13.969 1.00 44.96 C ATOM 2297 CB ILE B 138 30.534 22.873 13.957 1.00 46.61 C ATOM 2298 CG1 ILE B 138 31.170 22.955 12.558 1.00 44.58 C ATOM 2299 CD1 ILE B 138 32.693 22.657 12.515 1.00 36.53 C ATOM 2300 CG2 ILE B 138 30.468 21.423 14.466 1.00 48.73 C ATOM 2301 C ILE B 138 29.285 24.999 13.548 1.00 46.45 C ATOM 2302 O ILE B 138 28.681 25.433 12.583 1.00 45.73 O ATOM 2303 N SER B 139 30.093 25.756 14.283 1.00 46.68 N ATOM 2304 CA SER B 139 30.615 27.033 13.767 1.00 50.66 C ATOM 2305 CB SER B 139 29.706 28.215 14.146 1.00 51.05 C ATOM 2306 OG SER B 139 30.290 29.441 13.717 1.00 52.58 O ATOM 2307 C SER B 139 32.023 27.264 14.314 1.00 50.78 C ATOM 2308 O SER B 139 32.239 27.119 15.520 1.00 51.39 O ATOM 2309 N THR B 140 32.964 27.625 13.438 1.00 50.11 N ATOM 2310 CA THR B 140 34.352 27.920 13.864 1.00 54.13 C ATOM 2311 CB THR B 140 35.409 27.282 12.924 1.00 52.12 C ATOM 2312 OG1 THR B 140 35.051 27.513 11.560 1.00 51.29 O ATOM 2313 CG2 THR B 140 35.493 25.775 13.164 1.00 56.06 C ATOM 2314 C THR B 140 34.629 29.421 14.072 1.00 53.66 C ATOM 2315 O THR B 140 35.762 29.833 14.319 1.00 54.84 O ATOM 2316 N SER B 141 33.568 30.220 13.978 1.00 53.68 N ATOM 2317 CA SER B 141 33.640 31.661 14.128 1.00 52.39 C ATOM 2318 CB SER B 141 32.400 32.311 13.503 1.00 54.33 C ATOM 2319 OG SER B 141 32.157 31.779 12.205 1.00 47.17 O ATOM 2320 C SER B 141 33.722 31.968 15.609 1.00 54.75 C ATOM 2321 O SER B 141 33.090 31.288 16.428 1.00 57.16 O ATOM 2322 N ASN B 142 34.509 32.969 15.975 1.00 52.29 N ATOM 2323 CA ASN B 142 34.741 33.204 17.392 1.00 51.16 C ATOM 2324 CB ASN B 142 36.220 33.539 17.661 1.00 50.07 C ATOM 2325 CG ASN B 142 36.473 34.996 17.869 1.00 55.16 C ATOM 2326 OD1 ASN B 142 36.678 35.743 16.915 1.00 61.85 O ATOM 2327 ND2 ASN B 142 36.509 35.414 19.136 1.00 51.49 N ATOM 2328 C ASN B 142 33.736 34.157 18.063 1.00 51.20 C ATOM 2329 O ASN B 142 33.895 34.521 19.238 1.00 51.08 O ATOM 2330 N GLY B 143 32.719 34.570 17.299 1.00 50.47 N ATOM 2331 CA GLY B 143 31.643 35.424 17.795 1.00 50.52 C ATOM 2332 C GLY B 143 31.764 36.925 17.590 1.00 51.28 C ATOM 2333 O GLY B 143 30.825 37.669 17.903 1.00 50.26 O ATOM 2334 N SER B 144 32.898 37.376 17.056 1.00 53.07 N ATOM 2335 CA SER B 144 33.265 38.799 17.086 1.00 55.66 C ATOM 2336 CB SER B 144 34.725 38.939 17.504 1.00 55.64 C ATOM 2337 OG SER B 144 35.557 38.164 16.662 1.00 55.12 O ATOM 2338 C SER B 144 33.037 39.605 15.805 1.00 57.74 C ATOM 2339 O SER B 144 32.699 40.803 15.873 1.00 58.24 O ATOM 2340 N LEU B 145 33.237 38.964 14.651 1.00 58.51 N ATOM 2341 CA LEU B 145 33.204 39.638 13.329 1.00 59.93 C ATOM 2342 CB LEU B 145 32.877 41.138 13.436 1.00 59.99 C ATOM 2343 CG LEU B 145 32.790 42.022 12.187 1.00 58.59 C ATOM 2344 CD1 LEU B 145 31.717 41.539 11.235 1.00 56.85 C ATOM 2345 CD2 LEU B 145 32.557 43.492 12.576 1.00 60.03 C ATOM 2346 C LEU B 145 34.515 39.443 12.583 1.00 60.20 C ATOM 2347 O LEU B 145 34.543 38.819 11.524 1.00 60.65 O ATOM 2348 N GLU B 146 35.604 39.974 13.134 1.00 61.34 N ATOM 2349 CA GLU B 146 36.928 39.772 12.538 1.00 62.60 C ATOM 2350 CB GLU B 146 37.998 40.590 13.266 1.00 61.85 C ATOM 2351 CG GLU B 146 38.123 42.030 12.766 1.00 64.43 C ATOM 2352 CD GLU B 146 37.060 42.965 13.338 1.00 67.41 C ATOM 2353 OE1 GLU B 146 37.408 43.791 14.212 1.00 68.51 O ATOM 2354 OE2 GLU B 146 35.884 42.880 12.916 1.00 67.92 O ATOM 2355 C GLU B 146 37.292 38.287 12.520 1.00 62.26 C ATOM 2356 O GLU B 146 38.134 37.850 11.723 1.00 62.28 O ATOM 2357 N GLY B 147 36.635 37.522 13.393 1.00 60.53 N ATOM 2358 CA GLY B 147 36.785 36.077 13.424 1.00 58.38 C ATOM 2359 C GLY B 147 35.703 35.336 12.662 1.00 57.21 C ATOM 2360 O GLY B 147 35.808 34.128 12.464 1.00 56.76 O ATOM 2361 N LEU B 148 34.675 36.069 12.229 1.00 57.52 N ATOM 2362 CA LEU B 148 33.487 35.517 11.552 1.00 55.98 C ATOM 2363 CB LEU B 148 32.674 36.661 10.914 1.00 56.73 C ATOM 2364 OG LEU B 148 31.380 36.448 10.111 1.00 54.78 C ATOM 2365 CD1 LEU B 148 30.401 35.463 10.759 1.00 47.97 C ATOM 2366 CD2 LEU B 148 30.710 37.791 9.842 1.00 53.84 C ATOM 2367 C LEU B 148 33.817 34.432 10.524 1.00 56.07 C ATOM 2368 O LEU B 148 33.181 33.388 10.489 1.00 55.33 O ATOM 2369 N ASP B 149 34.832 34.674 9.704 1.00 57.37 N ATOM 2370 CA ASP B 149 35.228 33.712 8.675 1.00 57.71 C ATOM 2371 CB ASP B 149 35.433 34.427 7.333 1.00 58.37 C ATOM 2372 CG ASP B 149 35.787 35.901 7.504 1.00 59.20 C ATOM 2373 OD1 ASP B 149 36.457 36.258 8.508 1.00 58.54 O ATOM 2374 OD2 ASP B 149 35.383 36.700 6.635 1.00 60.63 O ATOM 2375 C ASP B 149 36.466 32.893 9.080 1.00 58.10 C ATOM 2376 O ASP B 149 37.213 32.410 8.220 1.00 57.61 O ATOM 2377 N ASN B 150 36.680 32.742 10.390 1.00 56.91 N ATOM 2378 CA ASN B 150 37.712 31.834 10.874 1.00 56.84 C ATOM 2379 CB ASN B 150 37.912 31.931 12.396 1.00 55.39 C ATOM 2380 CG ASN B 150 38.659 33.192 12.799 1.00 54.03 C ATOM 2381 OD1 ASN B 150 39.183 33.914 11.946 1.00 53.83 O ATOM 2382 ND2 ASN B 150 38.698 33.473 14.099 1.00 56.00 N ATOM 2383 C ASN B 150 37.367 30.430 10.447 1.00 57.87 C ATOM 2384 O ASN B 150 36.336 29.880 10.840 1.00 58.19 O ATOM 2385 N GLN B 151 38.222 29.876 9.599 1.00 57.57 N ATOM 2386 CA GLN B 151 38.005 28.551 9.045 1.00 58.65 C ATOM 2387 CB GLN B 151 38.760 28.417 7.716 1.00 59.29 C ATOM 2388 CG GLN B 151 38.337 29.449 6.648 1.00 55.33 C ATOM 2389 CD GLN B 151 37.597 28.832 5.475 1.00 61.37 C ATOM 2390 OE1 GLN B 151 38.109 27.918 4.824 1.00 63.82 O ATOM 2391 NE2 GLN B 151 36.394 29.340 5.184 1.00 50.29 N ATOM 2392 C GLN B 151 38.365 27.428 10.036 1.00 59.36 C ATOM 2393 O GLN B 151 38.176 26.237 9.730 1.00 58.04 O ATOM 2394 N GLU B 152 38.862 27.810 11.223 1.00 59.43 N ATOM 2395 CA GLU B 152 39.181 26.833 12.272 1.00 60.25 C ATOM 2396 CB GLU B 152 40.602 26.256 12.078 1.00 61.48 C ATOM 2397 CG GLU B 152 41.747 27.124 12.625 1.00 66.64 C ATOM 2398 CD GLU B 152 42.467 27.885 11.504 1.00 68.50 C ATOM 2399 OE1 GLU B 152 43.153 27.227 10.670 1.00 70.55 O ATOM 2400 OE2 GLU B 152 42.360 29.142 11.471 1.00 70.22 O ATOM 2401 C GLU B 152 38.979 27.296 13.735 1.00 59.91 C ATOM 2402 O GLU B 152 39.092 28.489 14.055 1.00 57.60 O ATOM 2403 N GLY B 153 38.670 26.328 14.603 1.00 59.88 N ATOM 2404 CA GLY B 153 38.611 26.530 16.052 1.00 61.08 C ATOM 2405 C GLY B 153 37.320 27.083 16.638 1.00 62.49 C ATOM 2406 O GLY B 153 36.298 26.389 16.676 1.00 61.87 O ATOM 2407 N GLY B 154 37.397 28.340 17.090 1.00 63.05 N ATOM 2408 CA GLY B 154 36.402 29.036 17.933 1.00 62.98 C ATOM 2409 C GLY B 154 34.981 28.521 18.070 1.00 62.97 C ATOM 2410 O GLY B 154 34.373 28.096 17.087 1.00 64.66 O ATOM 2411 N VAL B 155 34.452 28.571 19.295 1.00 61.10 N ATOM 2412 CA VAL B 155 33.051 28.238 19.574 1.00 57.44 C ATOM 2413 CB VAL B 155 32.086 29.191 18.770 1.00 59.75 C ATOM 2414 CG1 VAL B 155 30.869 28.479 18.148 1.00 53.52 C ATOM 2415 CG2 VAL B 155 31.694 30.398 19.640 1.00 59.92 C ATOM 2416 C VAL B 155 32.774 26.725 19.473 1.00 56.32 C ATOM 2417 O VAL B 155 32.358 26.102 20.454 1.00 55.79 O ATOM 2418 N CYS B 156 33.067 26.126 18.319 1.00 54.93 N ATOM 2419 CA CYS B 156 33.049 24.667 18.173 1.00 54.61 C ATOM 2420 CB CYS B 156 33.494 24.270 16.754 1.00 52.18 C ATOM 2421 SG CYS B 156 33.580 22.483 16.410 1.00 54.42 S ATOM 2422 C CYS B 156 33.909 23.990 19.278 1.00 54.64 C ATOM 2423 O CYS B 156 33.407 23.164 20.052 1.00 54.63 O ATOM 2424 N GLN B 157 35.187 24.360 19.371 1.00 55.54 N ATOM 2425 CA GLN B 157 36.065 23.825 20.426 1.00 56.56 C ATOM 2426 CB GLN B 157 37.535 23.863 19.983 1.00 56.95 C ATOM 2427 C GLN B 157 35.892 24.528 21.791 1.00 56.30 C ATOM 2428 O GLN B 157 35.845 23.877 22.843 1.00 57.99 O ATOM 2429 N THR B 158 35.780 25.856 21.755 1.00 54.56 N ATOM 2430 CA THR B 158 35.832 26.703 22.947 1.00 51.87 C ATOM 2431 CB THR B 158 36.082 28.197 22.528 1.00 53.75 C ATOM 2432 OG1 THR B 158 37.496 28.431 22.411 1.00 49.36 O ATOM 2433 CG2 THR B 158 35.470 29.201 23.512 1.00 52.72 C ATOM 2434 C THR B 158 34.632 26.566 23.900 1.00 51.82 C ATOM 2435 O THR B 158 34.800 26.579 25.128 1.00 52.22 O ATOM 2436 N ARG B 159 33.441 26.403 23.335 1.00 49.63 N ATOM 2437 CA ARG B 159 32.187 26.495 24.078 1.00 49.75 C ATOM 2438 CB ARG B 159 31.544 27.873 23.850 1.00 47.71 C ATOM 2439 C ARG B 159 31.223 25.388 23.657 1.00 50.64 C ATOM 2440 O ARG B 159 30.016 25.478 23.906 1.00 52.26 O ATOM 2441 N ALA B 160 31.780 24.338 23.045 1.00 49.93 N ATOM 2442 CA ALA B 160 31.031 23.199 22.492 1.00 48.16 C ATOM 2443 CB ALA B 160 30.681 22.213 23.589 1.00 47.09 C ATOM 2444 C ALA B 160 29.781 23.593 21.693 1.00 47.13 C ATOM 2445 O ALA B 160 28.729 22.967 21.837 1.00 46.20 O ATOM 2446 N MET B 161 29.897 24.650 20.888 1.00 48.64 N ATOM 2447 CA MET B 161 28.791 25.123 20.060 1.00 50.67 C ATOM 2448 CB MET B 161 28.928 26.603 19.706 1.00 52.39 C ATOM 2449 CG MET B 161 28.155 27.506 20.613 1.00 51.45 C ATOM 2450 SD MET B 161 27.427 28.867 19.687 1.00 55.07 S ATOM 2451 CE MET B 161 26.010 29.168 20.740 1.00 54.49 C ATOM 2452 C MET B 161 28.658 24.300 18.803 1.00 49.34 C ATOM 2453 O MET B 161 29.151 24.659 17.730 1.00 48.03 O ATOM 2454 N LYS B 162 27.994 23.170 18.953 1.00 49.25 N ATOM 2455 CA LYS B 162 27.692 22.303 17.820 1.00 48.55 C ATOM 2456 CB LYS B 162 28.860 21.354 17.556 1.00 51.62 C ATOM 2457 CG LYS B 162 29.575 20.893 18.800 1.00 49.28 C ATOM 2458 CD LYS B 162 31.087 20.929 18.634 1.00 50.58 C ATOM 2459 CE LYS B 162 31.753 20.166 19.772 1.00 50.05 C ATOM 2460 NZ LYS B 162 33.254 20.284 19.818 1.00 49.37 N ATOM 2461 C LYS B 162 26.373 21.547 18.060 1.00 49.72 C ATOM 2462 O LYS B 162 25.916 21.410 19.222 1.00 43.36 O ATOM 2463 N ILE B 163 25.736 21.121 16.963 1.00 47.99 N ATOM 2464 CA ILE B 163 24.568 20.251 17.040 1.00 47.17 C ATOM 2465 CB ILE B 163 23.306 20.835 16.329 1.00 46.99 C ATOM 2466 CG1 ILE B 163 22.952 22.213 16.880 1.00 46.43 C ATOM 2467 CD1 ILE B 163 21.965 22.944 16.019 1.00 56.53 C ATOM 2468 CG2 ILE B 163 22.082 19.898 16.490 1.00 43.12 C ATOM 2469 C ILE B 163 24.929 18.931 16.392 1.00 47.16 C ATOM 2470 O ILE B 163 25.505 18.905 15.299 1.00 47.77 O ATOM 2471 N LEU B 164 24.586 17.844 17.085 1.00 47.94 N ATOM 2472 CA LEU B 164 24.639 16.492 16.538 1.00 47.40 C ATOM 2473 CB LEU B 164 25.458 15.602 17.485 1.00 48.90 C ATOM 2474 CG LEU B 164 25.515 14.084 17.312 1.00 48.11 C ATOM 2475 CD1 LEU B 164 25.891 13.674 15.901 1.00 52.59 C ATOM 2476 CD2 LEU B 164 26.497 13.532 18.324 1.00 46.10 C ATOM 2477 C LEU B 164 23.210 15.947 16.335 1.00 48.56 C ATOM 2478 O LEU B 164 22.455 15.805 17.301 1.00 47.48 O ATOM 2479 N MET B 165 22.836 15.666 15.078 1.00 49.17 N ATOM 2480 CA MET B 165 21.500 15.120 14.757 1.00 48.85 C ATOM 2481 CB MET B 165 20.840 15.899 13.620 1.00 48.68 C ATOM 2482 CG MET B 165 20.442 17.324 14.038 1.00 51.96 C ATOM 2483 SD MET B 165 20.732 18.576 12.780 1.00 52.67 S ATOM 2484 CE MET B 165 22.520 18.375 12.593 1.00 54.06 C ATOM 2485 C MET B 165 21.509 13.624 14.460 1.00 47.92 C ATOM 2486 O MET B 165 22.112 13.162 13.481 1.00 43.94 O ATOM 2487 N LYS B 166 20.820 12.893 15.332 1.00 49.57 N ATOM 2488 CA LYS B 166 20.791 11.437 15.337 1.00 50.86 C ATOM 2489 CB LYS B 166 21.118 10.881 16.748 1.00 50.14 C ATOM 2490 CG LYS B 166 22.499 11.269 17.311 1.00 44.29 C ATOM 2491 CD LYS B 166 22.993 10.265 18.367 1.00 51.13 C ATOM 2492 CE LYS B 166 24.398 9.728 18.020 1.00 44.96 C ATOM 2493 NZ LYS B 166 25.262 9.450 19.224 1.00 51.45 N ATOM 2494 C LYS B 166 19.437 10.891 14.869 1.00 52.27 C ATOM 2495 O LYS B 166 18.388 11.185 15.452 1.00 49.95 O ATOM 2496 N VAL B 167 19.466 10.116 13.793 1.00 53.68 N ATOM 2497 CA VAL B 167 18.484 9.043 13.659 1.00 55.69 C ATOM 2498 CB VAL B 167 17.754 8.987 12.300 1.00 53.78 C ATOM 2499 CG1 VAL B 167 16.393 8.309 12.485 1.00 51.87 C ATOM 2500 CG2 VAL B 167 17.564 10.378 11.706 1.00 60.81 C ATOM 2501 C VAL B 167 19.221 7.728 13.947 1.00 56.53 C ATOM 2502 O VAL B 167 20.288 7.731 14.582 1.00 55.95 O ATOM 2503 O HOH C 1 −1.068 19.700 −2.247 1.00 20.00 O ATOM 2504 O HOH D 2 15.644 38.458 −11.327 1.00 20.00 O ATOM 2505 O HOH D 3 −8.095 49.449 −9.306 1.00 20.00 O ATOM 2506 O HOH D 4 14.879 14.522 19.283 1.00 20.00 O ATOM 2507 O HOH D 5 19.086 43.782 7.312 1.00 20.00 O ATOM 2508 O HOH D 6 3.762 36.483 −0.689 1.00 20.00 O ATOM 2509 O HOH D 7 5.977 28.240 −23.712 1.00 20.00 O ATOM 2510 O HOH D 9 38.280 30.933 15.129 1.00 20.00 O ATOM 2511 O HOH D 10 −2.614 8.973 −12.882 1.00 20.00 O ATOM 2512 O HOH D 11 33.557 12.755 6.451 1.00 20.00 O ATOM 2513 O HOH D 12 13.880 42.897 11.851 1.00 20.00 O ATOM 2514 O HOH D 13 19.942 29.901 −7.927 1.00 20.00 O ATOM 2515 O HOH D 14 20.613 48.185 26.172 1.00 20.00 O ATOM 2516 O HOH D 15 23.384 36.996 17.915 1.00 20.00 O ATOM 2517 O HOH D 16 12.029 8.173 11.014 1.00 20.00 O ATOM 2518 O HOH D 18 17.554 21.123 −23.737 1.00 20.00 O ATOM 2519 O HOH D 19 34.755 13.969 18.956 1.00 20.00 O ATOM 2520 O HOH D 20 19.454 17.871 −19.578 1.00 20.00 O ATOM 2521 O HOH D 21 16.241 30.564 5.560 1.00 20.00 O ATOM 2522 O HOH D 22 4.906 11.442 0.110 1.00 20.00 O ATOM 2523 O HOH D 23 0.407 21.483 −3.061 1.00 20.00 O ATOM 2524 O HOH D 24 11.613 15.180 −2.107 1.00 20.00 O ATOM 2525 O HOH D 25 3.322 26.535 2.926 1.00 20.00 O ATOM 2526 O HOH D 26 0.515 33.846 2.133 1.00 20.00 O ATOM 2527 O HOH D 27 20.755 10.411 1.428 1.00 20.00 O ATOM 2528 O HOH D 28 17.637 11.370 −10.183 1.00 20.00 O ATOM 2529 O HOH D 29 25.321 5.436 7.341 1.00 20.00 O ATOM 2530 O HOH D 30 12.205 9.020 −7.002 1.00 20.00 O ATOM 2531 O HOH D 31 10.319 15.291 −12.878 1.00 20.00 O ATOM 2532 O HOH D 32 13.474 26.530 21.387 1.00 20.00 O ATOM 2533 O HOH D 33 −5.385 36.132 3.825 1.00 20.00 O ATOM 2534 O HOH D 34 −12.238 40.692 −6.393 1.00 20.00 O ATOM 2535 O HOH D 35 −7.910 35.441 3.507 1.00 20.00 O ATOM 2536 O HOH D 36 16.595 21.733 4.395 1.00 20.00 O ATOM 2537 O HOH D 37 6.286 16.055 −2.458 1.00 20.00 O ATOM 2538 O HOH D 38 5.079 15.735 −7.772 1.00 20.00 O ATOM 2539 O HOH D 39 0.584 7.759 −10.414 1.00 20.00 O ATOM 2540 O HOH D 40 11.416 24.606 13.912 1.00 20.00 O ATOM 2541 O HOH D 43 9.303 12.604 −3.017 1.00 20.00 O ATOM 2542 O HOH D 45 28.991 19.384 1.268 1.00 20.00 O ATOM 2543 O HOH D 46 21.356 43.725 10.404 1.00 20.00 O ATOM 2544 O HOH D 49 −12.300 34.162 −0.864 1.00 20.00 O END
[0076]
TABLE 2
Crystallographic Statistics for the EphB4-ephrinB2 Complex
Resolution (Å) 1
20-2.0 (2.1-2.0)
Wavelength (Å)
0.98
Space Group
P4 1
Unit Cell Dimensions (Å)
a = b = 81.09 81.09 c = 50.95
Completeness (%)
99.6 (99.9)
R sym (%) 2
3.9 (20.8)
l/σ
4.8
Mean Redundancy
4.7
No. Reflections
19,785
R cryst (%) 3
22.6 (26.5)
R free (%) 4
29.5 (30.0)
R.m.s. deviations
Bond length (Å)
0.02
Bond angle (°)
1.7
Average B factor (Å 2 )
56.6
Number of atoms
Protein
4,992
1 Number in parentheses is for the highest shell.
2 R sym = Σ|I − <I>|/ΣI, where I is the observed intensity and <I> is the average intensity of multiple symmetry-related observations of that reflection.
3 R cryst = Σ||F obs | − |F calc ||/Σ|F obs |, where F obs and F calc are the observed and calculated structure factors. R sym = Σ|I − <I>|/ΣI, where I is the observed intensity and <I> is the average intensity of multiple symmetry-related observations of that reflection.
4 R free = Σ||F obs | − |F calc ||/Σ|F obs | for 10% of the data not used at any stage of structural refinement.
[0077]
TABLE 3
Effects of EphB4 mutation on binding to Alexa-532-TNYL-RAW
EphB4 mutant
Kd, nM
WT
5 ± 0.9
L95R
ND*
T147F
25 ± 5.6
R148S
4.5 ± 0.7
K149Q
23 ± 8
R150V
6.1 ± 0.8
RKR148-150SQV
21 ± 6
A186S
16 ± 4
*FP window is not significant to accurately determine Kd
[0078]
TABLE 4
Binding of peptide (TNYL-RAW) and human ephrinB2 to the human EphB4
ephrin-binding domain and EphB4 mutants. Experiments were performed at
25° C. in 50 mM Tris pH 7.8, 150 mM NaCl, 1 mM CaCl 2 .
All values represent the average of at least two experiments.
Kd
ΔG
ΔH
TΔS
Receptor
Ligand
(nM)
(kcal mol−1)
(kcal mol−1)
(kcal mol−1)
EphB4 (wt)
ephrinB2
40 ± 20
−10.2 ± 0.3
3.3 ± 0.1
13.4 ± 0.4
EphB4
ephrinB2
20 ± 10
−10.6 ± 0.4
3.7 ± 0.2
14.4 ± 0.3
(K149Q)
EphB4
ephrinB2
1900 ± 1100
−7.8 ± 0.3
5.2 ± 0.7
13.0 ± 0.8
(L95R)
EphB4 (wt)
TNYL-RAW
71 ± 14
−9.8 ± 0.1
−14.7 ± 0.2
−4.9 ± 0.2
EphB4
TNYL-RAW
160 ± 120
−9.4 ± 0.5
−12.5 ± 1.2
−3.2 ± 1.3
(K149Q)
EphB4
TNYL-RAW
35900 ± 5000
−6.1 ± 0.1
−12.0 ± 0.3
−5.8 ± 0.4
(L95R)
EXAMPLES
[0079] Aspects of the present teachings may be further understood in light of the following examples, which should not be construed as limiting the scope of the present teachings in any way.
Example 1
Construct Design, Expression and Purification of EphB4
[0080] Twelve sequential 4 amino acid truncations in human EphB4 were designed based on EphB4-EphB2 sequence alignment in the region C-terminal to the last β-strand in the EphB2 structure. The resulting fragments were cloned into the insect cell expression vector pBAC6 (Novagen, Wis.) under control of the heterologous GP64 signal peptide and containing a N-terminal six histidine tag. Constructs were sequence verified, and baculovirus was generated using homologous recombination into Sapphire Baculovirus DNA (Orbigen, Calif.) using the manufacturers protocol. After 3 rounds of viral amplification, a small scale expression screen was conducted for all constructs in both Sf9 and Hi5 insect cells. Briefly, 5×10 6 cells were infected with baculovirus at an MOI of 2 in 38 mm tissue culture dishes; cells were harvested at 48 hours post infection and supernatant containing secreted EphB4 was concentrated 10-fold and buffer exchanged into 50 mM Tris pH 7.8, 400 mM NaCl, and 5 mM imidazole using an Amicon Ultra 5K concentrator (Millipore, MS). The secreted protein was bound to Ni-NTA magnetic beads (Qiagen, CA), washed with 50 mM Tris pH 7.8, 400 mM NaCl, 20 mM Imidazole buffer and eluted with 50 mM Tris pH 7.8, 400 mM NaCl, 250 mM Imidazole. Based on analysis of immobilized metal affinity chromatography (IMAC) elutes, the EphB4 (17-196) construct was identified as the highest expressor at ˜6 mg/L in Hi5 insect cells. Large scale expression was conducted using Wave Bioreactors (Wave Biotech LLC, NJ) at a MOI of 2 for 48 hours in Hi5 insect cells. Media containing secreted EphB4 was concentrated and buffer exchanged using a Hydrosart Crossflow filter (Sartorius, NY). Following IMAC purification on ProBond resin (Invitrogen, CA) as described above, EphB4 was concentrated to 5 mg/ml and loaded on a Superdex 75 16/60 column (GE HealthCare, N.Y.). A small amount of aggregated material was removed by preparative size exclusion chromatography, while most of the sample eluted in a single peak corresponding to an EphB4 (17-196) monomer. The complete removal of the GP64 secretion sequence and protein identity were confirmed by MALDI analysis.
[0081] The wtEphB4 construct was used as a template for the generation of site specific mutants. The human ephrinB2 (extracellular domain; residues 25-187) was designed based on the previously published EphB2-ephrinB2 structure and cloned into a modified pFastBac1 vector containing a GP67 leader peptide. Recombinant baculovirus was generated using the Bac-to-Bac system (Invitrogen, CA). Briefly, large scale expression of ephrinB2 was carried out using Wave Bioreactors on a 5 L scale at an MOI of 5 for 48 hr. resulting in 10 mg of ephrinB2 per liter of Hi-5 insect cells (Invitrogen, CA). Media containing secreted ephrinB2 protein was concentrated and buffer exchanged using a Hydrostart Crossflow Filter (Sartorius Edgewood, N.Y.). The ligand was purified by immobilized metal affinity chromatography (IMAC), and cleaved overnight with TEV protease. Material was further re-purified by IMAC chromatography to remove the protease and an N-terminal fragment containing the histidine tag. The EphB4-ephrinB2 complex was formed with a 1.5-fold molar excess of ephrinB2 overnight at 4° C. in buffer containing 50 mM Tris, pH 7.8, 100 mM NaCl, and 10 mM Imidazole. The complex was purified by IMAC chromatography, followed by size exclusion chromatography to remove trace aggregates (Phenomenex S2000).
Example 2
Crystallization, Data Collection, and Structure Solution
[0082] The EphB4-ephrinB2 complex was concentrated to 20 mg/mL and crystallized by sitting drop vapor diffusion at 20° C. against a precipitant of 2.2 M ammonium sulfate and 100 mM tris, pH 7.8. Crystals formed in the P4 1 spacegroup and contained one monomer of receptor and one monomer of ligand in the asymmetric unit. Data were collected at the Advance Photon Source (Argonne, IL) on beamline GM/CA-CAT. Images were processed and reduced using HKL2000 (31). The structure was solved by molecular replacement with MolRep (CCP4i), using the EphB2-ephrinB2 structure (PDB: 1 KGY) as a search model (10,32). The structure was refined by a rigid body refinement, followed by model building in 0 and iterative refinements with refmac (32,33). The structure exhibits good geometry with no Ramachandran outliers.
Example 3
Isothermal Titration Calorimetry
[0083] All mutants and ligands were dialyzed into buffer containing 50 mM Tris-Cl (pH 7.8), 150 mM NaCl, and 1 mM CaCl 2 prior to use in isothermal titration calorimetry (ITC) experiments. All experiments were performed with a Microcal MCS ITC at 25° C. Titrations were completed as described in Example 4. EphB4 (wild-type or mutant) was present in the sample cell at a concentration of 12 to 15 μM and the injection syringe contained either 127 μM ephrinB2 or 200 μM TNYL-RAW. Titrations of TNYL-RAW with the L95R mutant of EphB4 were performed with 2 mM TNYL-RAW in the injection syringe and 15 μM EphB4 (L95R) in the sample cell. Data for these titrations were fit assuming a stoichiometry of 1 and at least 60% saturation at the final peptide concentration as described (19,34).
Example 4
[0084] Isothermal titration calorimetry and ELISA experiments: EphB4 and ephrin-B2 were either dialyzed or buffer exchanged into 50 mM Tris-Cl (pH 7.8 at 25° C.), 150 mM NaCl, 1 mM CaCl 2 , prior to use in calorimetry experiments. Peptides were dissolved into the same buffer used for the dialysis of EphB4. The concentration of EphB4, ephrin-B2 and the peptides was determined by measuring the A 280 and using the theoretical extinction coefficient (Gill and von Hippel, 1989). ITC experiments were performed with a Microcal MCS ITC at 25° C. Following an initial injection of 2 μl, titrations were performed by making 20 13 μl injections of peptide into EphB4 in the sample cell to produce an approximate final 2:1 ratio of injectant to sample in the cell. For most titrations the sample cell contained 15 μM EphB4 and the injection syringe contained a 200 μM solution of the peptide. Titrations with ephrin-B2 contained 13 μM EphB4 in the sample cell and 290 μM ephrin-B2 in the syringe. Prior to loading the sample cell, EphB4 was centrifuged at 18,000 g for 5 min at 4° C. to remove aggregates and degassed for 5 minutes at room temperature. Corrections for heats of dilution for the peptides and ephrin-B2 were determined by performing titrations of peptide or ephrin-B2 solutions into buffer. Dilution data were fit to a line and subtracted from the corresponding titration data. Titration data were analyzed using Origin ITC software (Version 5.0, Microcal Software Inc.) and curves were fit to a single binding site model (Wiseman et al., 1989). The low affinity of the TNYL peptide and the limited availability of EphB4 (17-196) precluded accurate determination of the K d for this interaction by ITC. A lower limit for the binding constant was determined by performing a titration in which the sample cell contained 30 μM EphB4 and the injection syringe contained a 1.45 mM solution of the peptide, producing a final ratio of peptide to EphB4 of 10:1. The data was fit assuming a stoichiometry of 1 and at least 60% saturation of binding at the final peptide concentration (Turnbull and Daranas, 2003).
[0085] The ability of peptides to compete the binding of mouse ephrin-B2 alkaline phosphatase to immobilized mouse EphB4-Fc-His (R&D Systems) was measured by ELISA as previously described (Koolpe et al., 2005).
Example 5
[0086] This Example illustrates fluorescence polarization (FP) assays using a fluorescently-labeled reporter peptide to measure binding of various ligands to the EphB4-LBD.
[0087] We have evaluated TMR and Alexa-532 labeled peptides, and experimentally confirmed the preference of Alexa-532-TNYL-RAW peptide for the assay because of the better dynamic range. We have also evaluated mutants predicted to have altered binding affinity to the TNYL-RAW peptide based on structural observations. The dose-response curve in FIG. 6A shows the wild-type EphB4 and EphB4 K149Q mutant signal upon binding to labeled TNYL-RAW peptide. AK149Q mutant has a greater dynamic range and slightly lower affinity for the labeled peptide than wtEphB4. In competition experiments, the affinity for the TNYL-RAW peptide is 170 nM, which is slightly lower than for wtEphB4 (100 nM) ( FIG. 7 ). Without being bound by a particular theory, a better dynamic range is likely a result of the interaction of this specific mutant with the Alexa-532 fluorophore of the reporter peptide. These characteristics make it an attractive tool for high throughput screening. The assay windows are approximately 6-fold for wtEphB4 and 12-fold for the EphB4 (K149Q) mutant. In addition we have validated the assay by studying binding of an L95R mutant, which was shown to have Kdephrin-B2=2 uM by ITC analysis. We have not detected a significant signal in FP analysis to accurately calculate KdAlexa-TNYL-RAW ( FIG. 6B ). This analysis also further validates the use of labeled TNYL-RAW peptide as a surrogate ligand for studies of ephrin-B2-EphB4 binding.
[0088] In this and other examples involving Alexa-532-TNYL-RAW peptide, A serial dilution of EphB4 was prepared in Assay Buffer (50 mM Tris pH 7.8, 150 mM NaCl, 1 mM CalCl2, 0.1% Pluronic 124). TNYL-RAW-Alexa-532 labeled peptide was prepared as a 100 μM stock solution in the Assay Buffer and a 300 nM working solution was made fresh prior to the measurements by dilution in the assay buffer. 5 μL of serially diluted EphB4 (9 nM-2362 nM concentration range) was combined with 5 μL of labeled peptide (final concentration 75 nM) in the final volume of 20 μL (Assay plate, 384 well flat bottom, black polystyrene, non-binding surface, Corning, cat #3654) in the absence and presence of 200 μM TNYL-RAW as a control for non-specific binding. The mixture was allowed to equilibrate for 30 min at room temperature, and measurements were performed with a Tecan Genios Pro (Tecan Instruments) using 535 nm excitation and 580 nm emission wavelength. All experimental data were analyzed using Prism 4.0 software (GraphPad Software Inc., San Diego, Calif.) and Kd values were generated by fitting the experimental data using a one-site binding hyperbola nonlinear regression model or equation 8.10 (.www.invitrogen.com/downloads/FP8.pdf).
[0089] In these experiments, the human EphB4 (17-196) ligand binding domain was cloned into the insect cell expression vector pBAC6 (Novagen, San Diego, Calif.) under control of the heterologous GP64 signal peptide and containing an N-terminal six histidine tag. The construct was sequence verified, and baculovirus was generated with homologous recombination into Sapphire Baculovirus DNA (Orbigen, San Diego, Calif.) following the manufacturer's protocol (10). The wtEphB4 construct was used as a template for generation of site specific mutants.
[0090] Large-scale expression was conducted with Wave Bioreactors (Wave Biotech LLC, Somerset, N.J.) at an MOI of 2 for 48 hr in Hi5 insect cells. Media containing secreted EphB4 (17-196) was concentrated and buffer exchanged with a Hydrosart Crossflow filter (Sartorius, Edgewood, N.Y.). Following immobilized metal affinity chromatography (IMAC) purification on ProBond resin (Invitrogen, Carlsbad, Calif.), EphB4 was concentrated to 5 mg/ml and loaded on a Superdex 75 16/60 column (GE HealthCare, Chicago, Ill.). A small amount of aggregated material was removed by preparative size exclusion chromatography, while most of the sample eluted in a single peak corresponding to an EphB4 (17-196) monomer. The complete removal of the GP64 secretion sequence and protein identity were confirmed by MALDI analysis.
[0091] The TNYL-RAW peptide was labeled with Alexa-532 (Biopeptides Inc., San Diego, Calif.). All peptides are purified to >95% purity, and supplied with rigorous analytical specifications, including HPLC and MS analysis.
Example 6
[0092] This Example illustrates that the fluorescence polarization assay (Example 5) is tolerant of organic solvents.
[0093] In these experiments, dimethylsulfoxide (DMSO) was added in various concentrations to a solution comprising Eph4 and Alexa-532-TNYL-RAW peptide, and FP was measured. As shown in FIG. 8 , the FP assay is tolerant to 5% DMSO (filled diamonds in FIG. 8 ) as indicated by analysis of EphB4 binding in the presence of various concentrations of DMSO. We have also been successful in the crystallization of EphB4 with the TNYL-RAW peptide in the presence of 5% DMSO, which is indicative of excellent tolerance of this specific interaction to DMSO.
Example 7
[0094] This Example illustrates determination of Z-factor at protein concentrations representing upper and lower plateaus of the dose response curve for the EphB4 K149Q mutant ( FIG. 6A ). The calculated Z-factor for 108 samples, each at 2 different protein concentrations, is 0.715 ( FIG. 9 ). The range of Z-factor between 0.5 and 1 is considered to be representative of a high quality assay.
Example 8
[0095] This Example illustrates thermodynamic characterization of TNYL-RAW peptide binding to EphB4-ligand binding domain (EphB4-LBD).
[0096] In these experiments, we monitored the binding of EphB4-LBD to ephrin-B2 and peptide ligands using isothermal titration calorimetry (ITC). The interaction between EphB4 (17-196) and ephrin-B2 yielded a Kd of 40 nM and a ΔHo of +3.3 kcal mol-1. This is slightly lower than the affinity reported for the interaction between the entire mouse EphB4 extracellular domain and mouse or human ephrin-B2. Without being limited by theory, we hypothesize that the difference may be explained by the existence of a third low affinity Eph-ephrin interface located outside the ephrin-binding domain (Smith, F. M., et al., J. Biol. Chem. 279: 9522-9531, 2004. In addition, N- and C-terminal truncations of the peptide, as well as targeted mutations in the center of the peptide, were synthesized in order to biophysically validate individual effects of the peptide upon EphB4 binding. Table 5 presents data of a thermodynamic analysis of wtEphB4 and mutant EphB4 binding to ephrin-B2 and TNYL-RAW and related peptides. The table shows the results of isothermal titration calorimetry (ITC) analysis. The Kd values reported from this method compare well with the Kd values determined from the FP assays ( FIGS. 6 and 7 ). Three regions of interactions proved critical for receptor binding: The N-terminal Tyr, the Phe/IIe amino acids in the center of the peptide, and the high-affinity C-terminal RAW sequence. The N- and C-terminal truncations appear detrimental due to the loss of stability at the D-E (N-terminal) and J-K (C-terminal) loops, while the Phe/IIe mutations resulted in a loss of stability at an imperative disulfide bridge critical to EphB4 LBD stability.
TABLE 5 ΔG (kcal TΔS (kcal Receptor Ligand Kd (nM) mol−1) ΔH (koal mol−1) mol−1) EphB4 (wt) ephrin-B2 40 ± 20 −10.2 ± 0.3 3.3 ± 0.1 13.4 ± 0.4 EphB4 ephrin-B2 20 ± 10 −10.5 ± 0.4 3.6 ± 0.1 14.1 ± 0.4 (K149Q) EphB4 ephrin-B2 1900 ± 1100 −7.8 ± 0.3 5.2 ± 0.7 13.0 ± 0.8 (L95R) EphB4 (wt) TNYL-RAW 71 ± 14 −9.8 ± 0.1 −14.7 ± 0.2 −4.9 ± 0.2 EphB4 TNYL-RAW 250 ± 50 −9.0 ± 0.1 −11.7 ± 0.2 −2.7 ± 0.2 (K149Q) EphB4 (wt) NYLF-RAW 65 ± 7 −9.8 ± 0.1 −15.5 ± 0.1 −5.7 ± 0.1 EphB4 (wt) YLFS-RAW 80 ± 36 −9.7 ± 0.2 −13.8 ± 0.5 −4.1 ± 0.4 EphB4 (wt) LFSP-RAW 3,500 ± 680 −7.4 ± 0.1 −5.3 ± 0.5 2.1 ± 0.4 EphB4 (wt) TNYL ≧140,000 ND −9.6 ± 0.3 ND EphB4 (wt) LFSP-RAW(F to ≧500,000 ND −7.9 ± 0.9 ND A) EphB4 (wt) LFSP-RAW(I to 60,000 ± 20,000 −5.7 ± 0.1 −2.7 ± 0.3 3.0 ± 0.4, A)
[0097] Results
[0098] Anti-EphB4-ephrinB2 therapeutic development can be accomplished by providing the three dimensional crystal structure of the EphB4-ephrinB2 complex at a high resolution. EphB4 specificity can also be probed using the three dimensional crystal structure. In addition, site-directed mutagenesis and biophysical analyses were conducted to investigate the role of several residues within the ligand binding cavity of EphB4 in contributing to the binding of both ephrinB2 and the antagonistic TNYL-RAW peptide. These results allow the development of predictive models for structure-based drug design of small molecule compounds for use as therapeutics and to probe the biology of EphB4-ephrinB2 bi-directional signaling.
[0099] Overall Structure
[0100] EphB4 and ephrinB2 were co-concentrated to 20 mg/mL and crystallized by sitting drop vapor diffusion against a precipitant of 2.2 M ammonium sulfate and 100 mM Tris, pH 7.8 at 20° C. The co-crystal structure was refined to 2.0 Å resolution with an R-factor of 22.6% and a free R factor of 29.5% (Table 1). Unlike crystals of the of the EphB2-ephrinB2 complex, which consisted of a heterotetramer, crystals of the EphB4-ephrinB2 complex consist of a heterodimer. Previously, formation of ephrinB2-EphB2 tetramers was observed for a concentration range around 1 mM using size exclusion chromatography analysis (SEC), while analytical ultracentrifugation demonstrated that the EphB2-ephrinB2 complex was a heterodimer at concentrations in the low micromolar range (10). The SEC analysis of the of the present invention provides the EphB4-ephrinB2 complex in a concentration range up to 500 μM indicating that the EphB4-ephrinB2 complex exsists as a heterodimer (data not shown). The overall structure of the EphB4-ephrinB2 complex is similar to that of the EphB2-ephrinB2 complex, with an r.m.s. deviation of 5.0 Å over 316 equivalent Cα positions. Significant deviation is evident, however, throughout the structure of the loop regions compared with the EphB4-TNYL-RAW and EphB2-ephrinB2 structures, with r.m.s. deviations of 1.8 and 5.3 Å, respectively in the J-K loop. The ephrinB2 ligand deviates minimally between previously described apo and receptor-bound structures, shifting only 0.91 and 0.90 Å respectively (10, 17).
[0101] EphB4-EphrinB2 Interface
[0102] Although the overall shape of the EphB4-ephrinB2 interaction interface is in good agreement with that previously described in the EphB2-ephrinB2 structure, marked differences exist within the receptor loops that frame the ligand binding channel. The EphB4 J-K loop assumes a distinct position compared to previously described crystal structures, and is situated directly above the ligand G-H loop and 15 Å from the D-E loop ( FIG. 2 ). The corresponding J-K loop from the EphB2-ephrinB2 structure, on the other hand, is shifted 6.4 Å from the D-E loop, and therefore maintains a more compact binding cavity. In fact, the J-K loops differ in position by up to 10 Å from furthest positions between the two ephrinB2-bound complex structures. Not surprisingly, the J-K loop shows remarkable flexibility in each structure described, also shifting in position by up to 20 Å from furthest positions between the EphB4-TNYL-RAW structure and the EphB4-ephrinB2 structure. Furthermore, crystallization trials with the apo form of EphB4 failed to produce diffracting crystals, likely because of the inherent flexibility of the J-K and D-E loops. A feature unique to EphB4 is a three residue insert in the J-K loop, which is absent in all other Eph receptors. It has been speculated that this insert contributes to the ligand binding specificity inherent to the EphB4 receptor (35). Indeed, two of the three residues (Pro-151, Gly-152, Ala-153) form the tip of the J-K loop, and make contacts with the ligand: Pro-151 R(R. receptor; L, ligand) forms a hydrophobic contact with Phe-120L, while Gly-152R makes a main-chain to side-chain polar contact with Glu-152L. In addition, the G-H and D-E loops, which form two walls of the ligand binding cleft, also shift in order to accommodate the ligand. The G-H loop is shifted by over 4.5 Å between the EphB4 and EphB2-bound ephrinB2 structures, while the D-E loop only deviates by 1.5 Å between the two structures.
[0103] The high affinity EphB4-ephrinB2 heterodimer is formed by insertion of the solvent exposed ligand G-H loop into the upper convex and hydrophobic surface of the EphB4 receptor, positioned above receptor strands E and M. Hydrophobic contacts drive receptor-ligand binding in this region. Ligand residues Phe-120, Pro-122, Trp-125 and Leu-127 participate in van der Waals interactions with receptor residues lining the receptor binding cavity in the D-E, G-H and J-K loops ( FIG. 4 ). Phe-120L forms hydrophobic interactions with Leu-95R (see below), Leu-100R, and Pro-101R, while Leu-124L interacts with Thr-147R from the receptor J-K loop. Meanwhile, Trp-125L extends to the surface of the receptor, in-between the J-K and G-H loops, participating in hydrophobic interactions with residues Leu-48R, Glu-50R, Val-159R, Leu-188R, and Ala-186R. In addition, Pro-122L, similar to all previous crystal structures, maintains its position by participating in a direct interaction with the receptor Cys61-Cys-184 disulfide bridge. Few polar contacts are formed at the receptor-ligand dimer interface. Ser-121 L forms a side-chain side-chain hydrogen bond with Glu-59R as well as a main-chain side-chain hydrogen bond with Lys-149R, while Asn-123L forms a hydrogen bond with the main-chain oxygen of Leu-48R. Additionally, Lys-149R extends to the body of the ephrinB2 G-H loop, forming side-chain side-chain hydrogen bonds with Glu-128L, and side-chain main-chain hydrogen bonds with Ser-121L and Asn-123L, wich are both part of the high affinity ligand FSPN sequence ( FIG. 3 ). The introduction of this new interaction at the EphB4-ephrinB2 interface is certain to contribute to the high affinity of this receptor-ligand complex.
[0104] Similar to the EphB2-ephrinB2 structure, a second portion of the high affinity heterodimerization interface exists immediately adjacent to the ligand binding cavity, formed by ligand strands C, G. and F. and receptor strands B-C, E, and D. This region of the complex deviates minimally from the corresponding structure of in the EphB2-ephrinB2 complex, with a maximum of 2.1 Å from furthest atoms, and is predominantly characterized by backbone-backbone, backbone-sidechain, and sidechain sidechain hydrogen bonds. In particular, sidechain-sidechain interactions between Glu-59R (Glu-68 in EphB2)-Gln-118L and Ser-121 L, Asp-29R (Glu-40 in EphB2)-Lys-112L, and Glu-43 (Glu-52, EphB2)-Lys 116L provide the binding potential characteristic of this low nanomolar interaction. Sidechain-mainchain interactions between Ser-55 and Lys-116L, and Glu-44R and Lys-60R complete the binding network in this region.
[0105] EphB4 Specificity
[0106] Sequence comparison and structural analysis of the EphB4 and EphB2 receptors suggested that one residue in EphB4 is particularly important in determining the specificity of the EphB4-ephrinB2 interaction: Leu-95. The corresponding residue in EphB2, Arg-103, is strictly conserved across both A and B subclasses, and deviates only in the EphB4 receptor. Arg-103R participates in hydrogen bonds with residues from the high affinity ephrin G-H loop, including Ser-121L and Glu-128L, and is situated in proximity to Phe-120L, a residue critical for receptor binding. However, superposition of Arg to Leu-95 in the EphB4-ephrinB2 structure suggests that a steric clash would result between an arginine at position 95R and Phe-120L. The corresponding Leu-95R, on the other hand, is able to form a 3.2 Å van der Waals interaction with Phe-120L due to its position within the ligand binding cavity. Thus, Arg-95R would also sterically clash with the phenylalanine from the TNYL-RAW peptide in the EphB4-TNYL-RAW structure (19), while the smaller Leu-95R forms favorable contacts with the peptide. Interestingly, the highly conserved Phe-120L is shifted in position by ˜90° as compared to previous complex structures (8, 10, 19) ( FIG. 5 ) and is buried within the hydrophobic cleft of the receptor, unlike its position in the EphB2-ephrinB2 complex structure, where it is directed towards the surface. In addition, the position of Arg-103R requires the J-K loop of the EphB2 receptor to extend away from the ligand G-H loop and towards the receptor D-E loop to avoid steric interference with residues lining the ephrin-B2 G-H loop. The smaller Leu-95R, together with the Phe-120L, allows the J-K loop of EphB4 to adopt a novel position directly above the ligand G-H loop.
[0107] Biophysical Characterization of EphB4 Specificity: Enthalpic vs. Entropic Contributions
[0108] A series of site-specific mutations was generated by changing residues lining the EphB4 G-H and J-K loops to the corresponding residues found in EphB2 (Table 3). The EphB4 mutants were rank-ordered based on their binding to fluorescently labeled Alexa-532-TNYL-RAW peptide. Fluorescence Polarization (FP) analysis corroborated the prediction that Leu-95 is a critical determinant for binding of the TNYL-RAW peptide because the Leu95Arg mutant did not exhibit significant binding of the peptide in our assay. EphB4 mutants Thr147Phe, Ala186Ser and Lys149Gln showed approximately 4-5 fold reduction in binding affinity of the fluorescently labeled peptide. The reduction in affinity due to mutation of these residues is consistent with what would be expected based on the structural information. A Thr-147-Phe mutation would impose steric constraints between the receptor J-K loop and the ephrinB2 G-H loop, as well as with Leu-95R due to the position of the receptor J-K loop. Interestingly, EphB4 possesses an alanine at position 186, which is conserved across the A-subclass while other B-subclass receptors have a conserved Ser. Ala-186R forms a van der Waals interaction with the main chain carbon of Asn-123 of the high affinity ligand G-H loop. A Ser at position 186 of EphB4 would cause a polar redistribution at the heterodimerization interface with ephrinB2 and result in the displacement of the receptor G-H loop due to a steric clash with Thr-93L and potential displacement of the ephrinB2 G-H loop. Finally, Lys-149R forms interactions at the dimer interface with ephrinB2 residues Ser-121L, Asn-123L and Gln-128L. Mutation to Gln should not result in steric interference with the ligand G-H loop, but could result in a slight readjustment of the J-K loop in order to accommodate the bulkier Gln side chain.
[0109] Based on the structural information and preliminary binding characterization, two EphB4 mutants, Leu95Arg and Lys149Gln, were chosen for detailed thermodynamic analysis of their binding to both ephrinB2 and the TNYL-RAW peptide ligand using isothermal titration calorimetry (ITC). As reported previously, EphB4 binds to ephrinB2 with an affinity of 40 nM and a ΔH obs of 3.3 kcal mol −1 (19). Mutation of EphB4 Lys-149 to Gln has no effect on the binding affinity or enthalpy of ephrinB2 binding (Table 4). In contrast, mutation of EphB4 Leu-95 to Arg reduces the binding affinity of ephrinB2 by nearly two orders of magnitude. Binding of ephrinB2 to all forms of EphB4 is endothermic, and the binding of ephrinB2 is more endothermic with the L95R mutation in EphB4 (5.2 kcal mol −1 versus 3.3 kcal mol −1 for wild-type EphB4). Preliminary experiments carried out in a buffer with different enthalpy of ionization showed a similar enthalpy change to that reported here. For example, binding of ephrinB2 to EphB4 (K149Q) results in a ΔH obs of 3.9 (±0.1) kcal mol −1 in phosphate (ΔH ion =0.8 kcal mol −1 ) compared to the ΔH obs of 3.7 (+0.2) kcal mol −1 value obtained in Tris (ΔH ion =11.34 kcal mol −1 ) (Table 4). Thus, the protonation/deprotonation is not coupled to ephrinB2 binding under the conditions of the ITC experiments.
[0110] Binding of the TNYL-RAW peptide to the wild-type, Lys149Gln, and Leu95Arg forms of EphB4 was also monitored by ITC. TNYL-RAW binds to EphB4 with an affinity of 70 nM and a ΔH obs of −14.7 kcal mol −1 (19). In contrast to the different effects of mutations in EphB4 on the interaction of EphB4 with ephrinB2, mutation of EphB4 of either Lys-149 to Gln or Leu-95 to Arg reduces the affinity of the EphB4-TNYL-RAW interaction (three-fold and 500-fold, respectively; Table 4). Binding of the TNYL-RAW peptide to all three forms of EphB4 is characterized by an exothermic enthalpy.
[0111] Thus, thermodynamic analysis reveals that TNYL-RAW binding to the EphB4 ligand binding domain is an enthalpically driven process, while ephrinB2 binding to EphB4 is an entropically driven process. The differences in the binding thermodynamics are consistent with the available structural information. Burial of the hydrophobic ligand G-H loop within the hydrophobic receptor binding cleft could entropically drive the interaction through the release of water, increasing the solvent entropy. In addition, the ephrinB2 ligand G-H loop is quite rigid, both in apo and receptor-bound structures, minimizing massive conformational entropy losses. The small loss of conformational entropy counteracts the heterodimerization process by ordering the otherwise flexible receptor J-K, D-E, and G-H loops. Unlike ephrinB2, however, the free peptide ligand loses significant conformational degrees of freedom upon EphB4 binding, resulting in an entropy loss. This is compensated by an enthalpic gain due to the formation of favorable interactions, both polar and nonpolar, at the receptor-peptide interface.
[0112] It should be noted that we produced the ephrinB2 extracellular domain in insect cells in a glycosylated form, while the ephrins used for previous crystal structure determinations were produced in E. coli and therefore not glycosylated. A conserved glycosylation site exists in ephrinB2 at residue Asn-39, in proximity of the low affinity tetramerization interface. Consistent with its possible glycosylation, Asn-39 is located near the surface of the protein and its side chain extends toward the surface of the complex. Although the carbohydrate was not observed in our electron density map, most likely because it was disordered, there is a theoretical possibility that a sugar at this location could interfere with the formation of receptor-ligand tetramers in the crystal lattice. However, previous reports have suggested that carbohydrate moieties would play more a favorable than an unfavorable role in tetramerization (36).
OTHER EMBODIMENTS
[0113] The detailed description set-forth above is provided to aid those skilled in the art in practicing the present invention. However, the invention described and claimed herein is not to be limited in scope by the specific embodiments herein disclosed because these embodiments are intended as illustration of several aspects of the invention. Any equivalent embodiments are intended to be within the scope of this invention. Indeed, various modifications of the invention in addition to those shown and described herein will become apparent to those skilled in the art from the foregoing description which do not depart from the spirit or scope of the present inventive discovery. Such modifications are also intended to fall within the scope of the appended claims.
REFERENCES CITED
[0114] Citation of a reference herein shall not be construed as an admission that such is prior art to the present invention. Specifically intended to be within the scope of the present invention, and incorporated herein by reference in its entirety, is the following publication: Chrencik, J. E., Brooun, A., Kraus, M. L., Recht, M. I., Kolatkar, A. R., Han, G. W., Seifert, J. M., Widmer, H., Auer, M., Kuhn, P. Structural and Biophysical Characterization of the EphB4-EphrinB2 Protein-Protein Interaction and Receptor Specificity. (2006) J. Biol. Chem. 281:28185-28192.
[0115] Publications referred to herein include:
1. Dodelet, V. C., and Pasquale, E. B. (2000) Oncogene 19, 5614-5619 2. Pasquale, E. B. (2005) Nat Rev Mol Cell Biol 6, 462-475 3. Wilkinson, D. G. (2001) Nat Rev Neurosci 2, 155-164 4. Wilkinson, D. G. (2000) Int Rev Cytol 196, 177-244 5. Blits-Huizing a, C. T., Nelersa, C. M., Malhotra, A., and Liebl, D. J. (2004) IUBMB Life 56, 257-265 6. Gale, N. W., Holland, S. J., Valenzuela, D. M., Flenniken, A., Pan, L., Ryan, T. E., Henkemeyer, M., Strebhardt, K., Hirai, H., Wilkinson, D. G., Pawson, T., Davis, S., and Yancopoulos, G. D. (1996) Neuron 17, 9-19 7. Committee, E. N. (1997) Cell 90, 403-404 8. Himanen, J. P., Chumley, M. J., Lackmann, M., Li, C., Barton, W. A., Jeffrey, P. D., Vearing, C., Geleick, D., Feldheim, D. A., Boyd, A. W., Henkemeyer, M., and Nikolov, D. B. (2004) Nat Neurosci 7, 501-509 9. Takemoto, M., Fukuda, T., Sonoda, R., Murakami, F., Tanaka, H., and Yamamoto, N. (2002) Eur J Neurosci 16, 1168-1172 10. Himanen, J. P., Rajashankar, K. R., Lackmann, M., Cowan, C. A., Henkemeyer, M., and Nikolov, D. B. (2001) Nature 414, 933-938 11. Hopkins, A. L., Mason, J. S., and Overington, J. P. (2006) Curr Opin Struct Biol 16, 127-136 12. Holland, S. J., Gale, N. W., Mbamalu, G., Yancopoulos, G. D., Henkemeyer, M., and Pawson, T. (1996) Nature 383, 722-725 13. Schmucker, D., and Zipursky, S. L. (2001) Cell 105, 701-704 14. Kalo, M. S., and Pasquale, E. B. (1999) Biochemistry 38, 14396-14408 15. Davy, A., Gale, N. W., Murray, E. W., Klinghoffer, R. A., Soriano, P., Feuerstein, C., and Robbins, S. M. (1999) Genes Dev 13, 3125-3135 16. Chin-Sang, I. D., George, S. E., Ding, M., Moseley, S. L., Lynch, A. S., and Chisholm, A. D. (1999) Cell 99, 781-790 17. Toth, J., Cutforth, T., Gelinas, A. D., Bethoney, K. A., Bard, J., and Harrison, C. J. (2001) Dev Cell 1, 83-92 18. Himanen, J. P., Henkemeyer, M., and Nikolov, D. B. (1998) Nature 396, 486-491 19. Chrencik, J. E., Brooun, A., Recht, M. I., Kraus, M. L., Koolpe, M., Kolatkar, A. R., Bruce, R. H., Martiny-Baron, G., Widmer, H., Pasquale, E. B., and Kuhn, P. (2006) Structure 14, 321-330 20. Nakamoto, M., and Bergemann, A. D. (2002) Microsc Res Tech 59, 58-67 21. Liu, W., Ahmad, S. A., Jung, Y. D., Reinmuth, N., Fan, F., Bucana, C. D., and Ellis, L. M. (2002) Cancer 94, 934-939 22. Berclaz, G., Karamitopoulou, E., Mazzucchelli, L., Rohrbach, V., Dreher, E., Ziemiecki, A., and Andres, A. C. (2003) Ann Oncol 14, 220-226 23. Andres, A. C., Reid, H. H., Zurcher, G., Blaschke, R. J., Albrecht, D., and Ziemiecki, A. (1994) Oncogene 9, 1461-1467 24. Nikolova, Z., Djonov, V., Zuercher, G., Andres, A. C., and Ziemiecki, A. (1998) J Cell Sci 111 (Pt 18), 2741-2751 25. Munarini, N., Jager, R., Abderhalden, S., Zuercher, G., Rohrbach, V., Loercher, S., Pfanner-Meyer, B., Andres, A. C., and Ziemiecki, A. (2002) J Cell Sci 115, 25-37 26. Berclaz, G., Andres, A. C., Albrecht, D., Dreher, E., Ziemiecki, A., Gusterson, B. A., and Crompton, M. R. (1996) Biochem Biophys Res Commun 226, 869-875 27. Noren, N. K., Lu, M., Freeman, A. L., Koolpe, M., and Pasquale, E. B. (2004) Proc Natl Acad Sci USA 101, 5583-5588 28. Kertesz, N., Krasnoperov, V., Reddy, R., Leshanski, L., Kumar, S. R., Zozulya, S., and Gill, P. S. (2006) Blood 107, 2330-2338 29. Martiny-Baron, G., Korff, T., Schaffner, F., Esser, N., Eggstein, S., Marme, D., and Augustin, H. G. (2004) Neoplasia 6, 248-257 30. Koolpe, M., Burgess, R., Dail, M., and Pasquale, E. B. (2005) J Biol Chem 280, 17301-17311 31. Otwinowski, Z., Minor, W. (1997) Processing of x - ray diffraction data collected in oscillation mode . Methods in Enzymology, Macromolecular Crystallography, part A (Sweet, C. W. C. R. M., Ed.), 276, Academic Press, New York 32. CCP4. (1994) Acta Crystallogr D Biol Crystallogr 50, 760-763 33. Jones, T. A., Zou, J. Y., Cowan, S. W., and Kjeldgaard. (1991) Acta Crystallogr A 47 (Pt 2), 110-119 34. Turnbull, W. B., and Daranas, A. H. (2003) J Am Chem Soc 125, 14859-14866 35. Nikolov, D. B., Li, C., Barton, W. A., and Himanen, J. P. (2005) Biochemistry 44, 10947-10953 36. Himanen, J. P., and Nikolov, D. B. (2002) Acta Crystallogr D Biol Crystallogr 58, 533-535 37. Day, B., To, C., Himanen, J. P., Smith, F. M., Nikolov, D. B., Boyd, A. W., and Lackmann, M. (2005) J Biol Chem 280, 26526-26532 38. Smith, F. M., Vearing, C., Lackmann, M., Treutlein, H., Himanen, J., Chen, K., Saul, A., Nikolov, D., and Boyd, A. W. (2004) J Biol Chem 279, 9522-9531
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The invention relates to the three-dimensional structure of a crystal of an EphB4 receptor complexed with a ligand. The three-dimensional structure of a Receptor-Ligand Complex is disclosed. The receptor-ligand crystal structure, wherein the ligand is an inhibitor molecule, is useful for providing structural information that may be integrated into drug screening and drug design processes. Thus, the invention also relates to methods for utilizing the crystal structure of the Receptor-Ligand Complex for identifying, designing, selecting, or testing inhibitors of the EphB4 receptor protein, such inhibitors being useful as therapeutics for the treatment or modulation of i) diseases; ii) disease symptoms; or iii) the effect of other physiological events mediated by the receptor.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to the field of apparatus for orienting containers, especially prior to the application of labels to the containers. More specifically, the invention relates to an in-line apparatus for rotating a container and for stopping the container from rotating when an ear or other protrusion on the can reaches a specific, pre-selected angular orientation. This apparatus is especially useful in connection with labeling equipment for such containers where it is desired to orient the container relative to a label so that the ear or other protrusion registers with a corresponding opening in the label.
[0003] 2. Description of the Prior Art
[0004] The art of labeling equipment is highly developed and the patent literature includes many patents directed to virtually every facet of labeling apparatus and methods. In a patent search directed to the present invention, the following US patents were identified: U.S. Pat. No. 3,241,578 (Heisler '578); U.S. Pat. No. 3,848,394 (Heisler '394); U.S. Pat. No. 4,344,522 (Heisler '522); U.S. Pat. No. 4,383,601 (Heisler '601); U.S. Pat. No. 3,209,512 (Ferguson); U.S. Pat. No. 3,289,810 (Iannucci) and U.S. Pat. No. 3,462,912 (Anderson).
SUMMARY OF THE INVENTION
[0005] The present invention is concerned with apparatus for orienting containers which have at least one ear on a side of the container. In particular, the invention is concerned with such apparatus preferably in combination with labeling equipment for applying a label to the oriented container so that an opening in a label registers with the at least one ear on the container.
[0006] Apparatus according to the preferred embodiment of the invention comprises a star wheel with pockets which permit relatively free rotation of containers positioned within the pockets, an ear bump associated with each pocket in the star wheel and a releasable container hold down to prevent containers in the star wheel pockets from tilting while they are being oriented. The apparatus can further comprise a labeling station for applying labels to the containers when they have been oriented so that at least one opening in the label registers with the at least one ear on each container.
[0007] Accordingly, it is an object of the present invention to provide an apparatus which is capable of consistently orienting containers relative to at least one ear on each container, prior to the application thereto of a label.
[0008] It is a further object of the invention to provide such an apparatus which can be incorporated into existing labeling stations with a minimum amount of disruption to the components of the labeler.
[0009] It is yet another object of the invention to provide such an apparatus which is especially suited to containers with a pair of ears for supporting a bail handle, for example.
[0010] These and other objects and advantages of the present invention will no doubt become apparent to those skilled in the art after having read this detailed description of the invention including the following description of the preferred embodiment which is illustrated by the various drawing figures.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a top view of container orienting and labeling apparatus according to the present invention.
[0012] FIG. 2 is a partial cross-sectional view of the apparatus shown in FIG. 1 , taken along the line 2 - 2 of FIG. 1 .
[0013] FIG. 3 is a view of the star wheel portion of the station showing portions of container retainer devices.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0014] Referring to FIG. 1 , a container orienting label applicator station is indicated generally at 10 . Labels 12 from a roll (not shown) are supplied to a label cutter station, indicated generally at 14 , after passing through label guide rollers 16 . Cut labels 18 are transferred from a rotary cutter 20 in the cutter station 14 to a vacuum label drum 22 . Adhesive is applied to each label 18 by a glue roller 23 . Containers C are advanced, from left to right in FIG. 1 , on a conveyor belt 24 or some other conveyance. First, individual containers C enter successive pockets 25 defined by an upper star wheel 26 and a lower star wheel 28 ( FIG. 2 ) which are rotated in the direction indicated by the arrow on the star wheel 26 ( FIG. 1 ). As each container C exits one of the pockets 25 of the star wheels 26 and 28 , it passes between the vacuum label drum 22 and a roll-on pad 30 where an individual label 18 is transferred from the label drum 22 to the container C. The labeled containers C then exit the label applicator station 10 . This much of the label applicator station 10 illustrated in FIGS. 1 and 2 is largely conventional and will not be described further, except in the context of the container orienting features of the present invention.
[0015] The label applicator station 10 includes apparatus for orienting containers C. The containers C, as shown in the drawing, each have a pair of opposed ears E which may support a wire bail (not shown) in a known manner, as is the case with a conventional container known in some circles as a paint can. These containers typically have a one gallon capacity. The ears E on these containers C present some interesting challenges when it comes to applying a label to the containers. As is explained below, the present invention includes apparatus that will rotate an eared container to a predetermined angular orientation and deliver it into the labeling section of a label machine so that a label can be applied to the eared container. In one embodiment, the labels and the vacuum drum on which they are supported have openings that register with the ears when the label is applied to the container.
[0016] The container orienting apparatus includes a stop 32 associated with each pocket 25 and a roll pad 34 that cooperates with one of the pockets 25 . The roll pad 34 has a surface 36 that is grippy in the sense that it is resilient and has a relatively high coefficient of friction. The grippy surface 36 is positioned so that a side wall of a container C carried in the pocket 25 that is closest to the roll pad 34 engages the surface 36 and, when the star wheels 26 and 28 are rotating, this engagement between the container C and the stationary grippy surface 36 causes the container C to rotate in the pocket 25 until such rotation brings an ear E of the container C into contact with the stop 32 . At this point, the stop 32 resists further rotation of the container C to the extent that static friction between the side wall of the container C and the surface 36 is overcome and the container C stops rotating relative to the star wheel pocket 25 and begins rotating relative to the surface 36 . The container C is now oriented for delivery to and engagement by and between the vacuum label drum 22 and the roll-on pad 30 so that the ears E will register with corresponding recesses in the face of the vacuum label drum and with corresponding recesses in the cut labels 18 supported on the vacuum label drum 22 .
[0017] When an ear E on a container C in a pocket 25 strikes the stop 32 and the container begins to slide along the grippy surface 36 of the roll pad 34 , the container will be subjected to a number of forces that will try to lift it out of and/or skew it within the pocket 25 . To prevent this, a container retainer 38 ( FIG. 2 ) is associated with each pocket 25 . The retainer 38 , preferably, is supported for reciprocating movement between an extended position as shown in FIG. 2 where it is operable to hold a container C against the conveyor 24 and a retracted position (not shown) in which it is inoperable to hold the container C against the conveyor 24 . Each of the retainers 38 is preferably supported for reciprocating movement with a piston rod of a compressed air piston assembly associated with each pocket 25 . An air switch operated, for example, by cam can be used to move the retainer 38 to the extended position and back again, in a desired timed sequence. It is preferred that the retainer 38 for a given pocket be extended into a first position just as, or immediately after, a container C enters the given pocket. It is also preferred that the retainer 38 remain in that position until and after the time that an ear E on the container C engages the stop 32 and until the container C moves past the grippy surface 36 of the roll pad 34 to a slippy surface 40 ( FIG. 1 ) of the roll pad 34 . At this instant, the retainer 38 is retracted and the container slides along the slippy surface 40 , with an ear E abutted against the stop 32 until the container passes the slippy surface 40 and the container C is delivered to and engaged by and between the vacuum label drum 22 and the roll-on pad 30 so that the ears E will register with corresponding recesses 42 in the face of the vacuum label drum 22 and with corresponding recesses (not shown) in the cut labels 18 supported on the vacuum label drum 22 .
[0018] It will be appreciated that the star wheels 26 and 28 are synchronized with the other components of the container orienting label applicator station 10 and, specifically, with the vacuum drum 22 and the label cutter 14 . As a consequence, the leading edge of each pre-cut label 18 is applied to each container C at the same angular position relative to the star wheels 26 and 28 and to one of the ears E on the container C. The container orienting apparatus described above is operable to rotate each container C to position the ear E at a predetermined angular orientation relative to the star wheel pockets 25 and to maintain that orientation while the container C is delivered to the vacuum label drum 22 .
[0019] During set-up of the apparatus 40 , it may be determined that the containers C are being consistently rotated to the same angular orientation which is not the predetermined or desired angular orientation. In a preferred embodiment, as shown in FIG. 1 , the stop 32 is mounted for sliding movement in a slot indicated at 44 in FIG. 3 . A fastener 46 is operable to lock the stop 32 into a desired location along the slot 44 and, by varying the position of the stop 32 , one can fine tune the angular orientation of the ear E elative to one of the star wheel pockets 25 .
[0020] Referring now to FIG. 3 , some details of the actuator for the container retainer 38 are shown. A linear actuator 48 (one for each star wheel pocket 25 ) is mounted on top of a lower, outer, actuator support ring 50 which is partially broken away. The container retainers 38 are mounted below the support ring 50 , between it and the upper star wheel 26 . Good results have been achieved with a linear actuator 48 that is retracted or extended under the influence of compressed air delivered through a hose 52 or a hose 54 , respectively. Compressed air is selectively delivered to the actuator 48 through hose 52 or hose 54 , according to the condition of an air valve 56 which is mounted on an inner, upper support ring 58 . The support rings 50 and 58 are mounted together with the star wheels 26 and 28 for rotation together therewith about the central axis of the star wheels 26 and 28 and the support rings 50 and 58 . The air valve 56 receives compressed air through a hose 62 which gets compressed air from a central post (not shown) through a rotating connector (not shown) and, when the valve 56 is in a first condition, it delivers compressed air through hose 52 , causing the actuator 48 and the container retainer 38 to retract away from a container C in the corresponding pocket 25 of the star wheels 26 and 28 . When the valve 56 is in a second condition, it delivers compressed air through hose 54 , causing the actuator 48 and the container retainer 38 to extend towards a container C in the corresponding pocket 25 of the star wheels 26 and 28 , to retain the container C in the star wheel pocket 25 and on the conveyor 24 .
[0021] The condition of the valve 56 is determined by the angular position of the support ring 58 relative to a fixed cam plate 60 that is supported on a center cam support 62 . A cam follower 64 is supported on a valve lever 66 which is pivotally mounted, as at 68 , for movement between a first position, shown in FIG. 3 , where it causes the valve 56 to deliver compressed air through the hose 52 to retract the associated container retainer 38 and a second position (not shown) in which the valve lever 66 has rotated counter clockwise about the pivot mount 68 from the position shown in FIG. 3 to a second position (not shown) in which it has depressed valve button 70 . With the valve button 70 depressed, the valve 56 will direct compressed air to hose 54 causing the associated container retainer 38 to extend to a position where it will be operable to hold the associated container against the conveyor 24 and keep it in the pocket 25 of the star wheels 26 and 28 . The cam follower 64 cooperates with the cam plate 60 and, specifically, a cam bump 72 , to move the valve lever 66 from the first position to the second position. A spring (not shown) associated with the valve button 70 returns the valve lever 66 to the first position when the cam follower 64 clears the cam bump 72 as the support ring 58 rotates around the fixed, non-rotating cam plate 60 .
[0022] Although the present invention has been described in terms of specific embodiments, it is anticipated that alterations and modifications thereof will no doubt become apparent to those skilled in the art. It is intended that the appended claims be interpreted as covering all such alterations and modifications as fall within the true spirit and scope of the invention.
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Apparatus for orienting containers which have at least one ear on a side of the container is disclosed. Such apparatus is especially suited for use in combination with labeling equipment for applying a label to the oriented container so that at least one opening in a label registers with the at least one ear on the container. The apparatus comprises a star wheel with pockets which permit relatively free rotation of containers positioned within the pockets, an ear bump associated with each pocket in the star wheel and a releasable container hold down to prevent containers in the star wheel pockets from tilting while they are being oriented.
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BACKGROUND OF THE INVENTION
The invention relates to a lamp, in particular for elongate lighting means with caps at both ends, having a lamp housing and a lamp cover provided to restrict dazzle.
Lamps having a lamp cover provided to restrict dazzle are known in the most diverse embodiments, with the lamp cover usually consisting of a molding matched to the special lamp design or of a plurality of special moldings assembled to form a cover.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a lamp having a lamp cover which can be manufactured in an easily variable design in a particularly economic manner, which is characterized by low weight and which moreover allows a simple and problem-free changing of the lighting means.
This object is satisfied in accordance with the invention essentially in that the lamp cover comprises at least one areal element which has a pre-selectable light transmission and is made of elastic material which extends between the end walls of the lamp housing and is fixable in complementary recesses in the end walls via coupling lugs after an elastic deformation resulting in a shortening and a subsequent relaxation.
The areal element or each areal element is here preferably positively latched in the end walls through its own stress.
Since the areal elements consist of elastic material, they can be bent simply, with the length of the respective element being shortened by the bending so that it is possible to insert the coupling lugs provided at the end sides into the corresponding recesses in the faces of the lamp housing without problem. The coupling lugs enter into the corresponding recesses by a simple release of the areal elements initially held in the bent or curved state, are preferably positively received there, and latch and thus hold the areal element in the desired defined position by its own stress.
It is particularly advantageous in connection with this basic principle that both cubic planar covers and convexly or concavely arched covers can be created by the selection of the planar length of the areal elements, with it only being necessary to pre-set the desired dimension of the respective arching by pre-setting the corresponding length dimension.
With respect to the variability of the design in accordance with the invention and its different application purposes, it is of advantage that, for example, only one lower areal cover element, or one lower areal cover combined with one lateral cover element or combined with two lateral cover elements, can be associated with the respective lighting means so that the respectively desired radiation characteristics or relationships can be taken into account. Since each areal element represents a unit which can be independently latched to the respective face areas of the lamp housing, the respectively required selection can be made without problem.
The stability of the shape of a light means cover consisting of a plurality of areal elements can preferably be further improved by latches being provided formed between the individual areal elements, e.g. by punched-out openings at one element and spigots at the other element.
An unintentional release of the lamp cover, such as cannot be excluded, for example, with simply clamped covers, is precluded with certainty in the solution in accordance with the invention due to the permanently active own stress after the completed assembly of the areal elements.
As a rule, only the central cover has to be removed to change the respective lighting means, which is possible in a simple manner by it being bent in a direction which shortens the areal element and uncouples it from the lamp housing.
BRIEF DESCRIPTION OF THE INVENTION
Further particularly advantageous embodiments and features of the invention are explained in more detail with reference to the drawing, in which:
FIG. 1 is a schematic perspective representation of an embodiment of a lamp having a lamp cover in accordance with the invention;
FIG. 2 is a schematic longitudinally sectioned view of a lamp housing having a planar lamp cover;
FIG. 3 is a schematic longitudinally sectioned view of a lamp cover having a convexly arched lamp cover;
FIG. 4 is a schematic longitudinally sectioned view of a lamp cover having a concavely arched lamp cover;
FIG. 5 is a schematic bottom view of a lamp having a cubic planar lamp cover;
FIG. 6 is a schematic bottom view of a lamp having convexly arched areal elements of a lamp cover;
FIG. 7 is a schematic bottom view of a lamp having concavely executed areal elements of a lamp cover;
FIG. 8 is a perspective representation of the design of the lamp cover in accordance with FIG. 5;
FIG. 9 is a perspective representation of the design of a lamp cover in accordance with FIG. 6; and
FIG. 10 is a perspective representation of the design of a lamp cover in accordance with FIG. 7 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a lamp 1 intended for ceiling mounting having a lamp housing 2 and a lamp cover 3 spaced from and surrounding the elongate lighting means with caps at both ends which extends between the two end walls 8 , 9 of the lamp housing 2 . The lamp housing 2 furthermore receives a reflector 4 , for example a reflector curved in a twin paraboloid manner. It has to be noted here that reflectors of the most varied kind and housing designs of a varied kind can generally be used in connection with a lamp in accordance with the invention.
The schematic sectioned view in accordance with FIG. 2 shows a box-like lamp housing 2 having end walls 8 , 9 between which an elongate lighting means 15 and an areal element 5 acting as a lamp cover 3 extend.
This light-transmitting, light-scattering and elastically formed areal element 5 preferably consists of a suitable plastic and is latched in the end walls 8 , 9 of the lamp housing 2 in corresponding recesses 11 via coupling lugs molded at the end side. This is done by the areal element 5 —as shown by a chain line—first being deformed by bending and thus being shortened in length, whereupon its coupling lugs 10 can be arranged in front of the recesses 11 in the end walls 8 , 9 and then released for relaxation so that the coupling lugs 10 engage into the recesses 11 and thus fix the areal element 5 in place securely and exactly positioned by the return of the areal element 5 into its extended shape. In the case of FIG. 2, the length of the areal element 5 is selected such that it assumes a planar form in the fixed position.
FIG. 3 shows an embodiment in which the length of the areal element 5 is selected to be greater than the distance between the two end walls 8 , 9 of the lamp housing 2 . Since in this case the length of the areal element 5 means that it cannot relax in a planar manner after coupling with the lamp housing 2 , a concavely arched structure of the cover 3 is achieved due to the residual stress of the areal element 5 .
FIG. 4 shows a basic arrangement corresponding to FIG. 3 with a correspondingly dimensioned areal element 5 ; however, in this case, the arching of the areal element has been carried out in the opposite direction so that a concavely arched cover structure results in the latched state of the areal element 5 .
Since the lamp cover in accordance with the invention consists of individual areal elements, the number of the areal elements to be used in an individual case and also their relative positions can be freely selected depending on the desired radiation characteristics, with, in the event of different relative positions, only correspondingly matching recesses 11 also having to be provided in the end walls of the lamp housing.
FIG. 5 shows a bottom view of a lamp in which the lamp cover is executed in a cubic planar manner; i.e. a central areal element 5 is arranged between two lateral areal elements 6 , 7 . Additional latches 12 on opposite sides, which can be realized for example by punched-out openings and spigots engaging into these, can be provided between the central areal element 5 and the lateral areal elements 6 , 7 to increase the overall stability and for the exact definition of the mutual spacings. In this way, exact gaps 13 extending in a defined manner can be achieved between adjacent areal elements.
The principle of convex and concave stressing of areal elements was already explained in connection with FIGS. 3 and 4. This principle cannot only be used for an individual areal element, but it can also be realized in connection with box-like lamp covers such as is shown schematically in FIGS. 6 and 7.
FIG. 6 shows a central areal element 5 whose two longitudinal sides are convexly shaped and which extends in at least substantially planar manner between the two faces 8 and 9 of the housing 2 . Lateral areal elements 6 , 7 are associated with this central areal element 5 and are stressed in the lamp housing 2 due to their selected length dimension such that the required matching to the contour of the central areal element is obtained. Inter-engaging latched connections 12 can also be provided here between the areal elements.
The embodiment in accordance with FIG. 7 differs from the embodiment of FIG. 6 in that the central areal element 5 has concavely extending side boundaries and in that the lateral elements 6 , 7 are stressed in a curved manner towards the center and in this way match the shape of the central areal element 5 .
The perspective representations in accordance with FIGS. 8, 9 and 10 show the lamp housings, which are respectively shown in a bottom view in FIGS. 5, 6 , and 7 , in their three-dimensional form, with it having to be noted here that the curvatures of the lateral areal elements 6 , 7 are created in the embodiment in accordance with FIGS. 9 and 10 by the stress of the elements, which are planar per se, in the end walls of the lamp housing.
The coupling lugs 10 shown in the drawings, and naturally their complementary recesses 11 in the end walls of the respective lighting housing, can basically be designed in the most varied way. It is only necessary to ensure that the coupling lugs 10 can be inserted into the corresponding recesses by deformation of the respective areal element and that these lugs 10 engage into the corresponding recesses after the release of the areal elements, which are initially curved during mounting, such that a removal of the areal elements is only possible when these elements are again directly deformed or bent, such as will be the case when it becomes necessary to change a lighting means.
Substantial advantages of the lamp cover in accordance with the invention lie in their low weight, the simplicity of their production by punching, cutting or lasering, the variability with respect to their dimensions and shape, the avoidance of additional fastening elements such as clamps and the like, and in that the most varied radiation characteristics of a lamp can be achieved by the selection of the shape, the number and the position of the individual areal elements.
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A lamp has a light housing and a light cover intended to restrict dazzle, wherein the lamp cover comprises at least one areal element having a pre-selectable light transmission and made of elastic material which extends between the end walls of the lamp housing and is fixable in complementary recesses in the face walls via coupling lugs after an elastic deformation resulting in a shortening and a subsequent relaxation.
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FIELD OF THE INVENTION
This invention relates to a control method of brightness of a screen used for a projection display and a control apparatus of the same.
BACKGROUND OF THE INVENTION
A typical conventional projection display is disclosed, for example, in U.S. Pat. No. 4,040,047 entitled "Erasable Thermo-Optic Storage Display of a Transmitted Image" distributed on Aug. 2, 1977. This apparatus does not control the input power of an illumination light source in response to brightness of the screen. For this reason, screen brightness might drop due to the change with time of the illumination light source or a projection light source.
The prior art apparatus described above is not free from a drawbacks in that since brightness of the light source fluctuates due to the change with time of the projection light source and due to the change of ambient conditions, screen brightness is not constant and a stable screen image cannot be obtained. More specifically, brightness of a Xenon lamp (hereunder, Xe lamp), which is this kind, drops with the passage of time and the image becomes somewhat darker and difficult to watch with the passage of a few months after the start of use. Therefore, it has been customary to replace the Xe lamp by new one at this stage by judging that the life of the lamp is reached.
The prior art apparatus is not at all considered at this point but replaced the Xe lamp with a new one within a short period by judging that the service life is over. Therefore, the lamp is not utilized fully and a stable screen image in brightness cannot be obtained.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a control method of brightness of a screen used for a projection display and control apparatus of the same which can use a light source for a long period and can provide a stable screen image in conjunction with brightness.
To accomplish the object described above, the present invention provides a control method of brightness of a screen used for a projection display which comprises detecting brightness of a screen based on the luminous flux projected on the screen from a light source, feeding back its detection signal, comparing a set value of brightness of the screen with the actually measured value detected, and regulating the input power to be supplied to the light source in such a direction that the difference between them becomes zero.
The present invention provides also a control method of brightness of a screen used for a projection display which comprises setting in advance the relationship between the magnitude of the input power to be supplied to the light source, its supply time and brightness of the light source to such a relationship that brightness becomes substantially constant, measuring actually the supply time of the input power to the light source and regulating the input power so that brightness becomes substantially constant on the basis of the relationship set in advance.
Furthermore, the present invention provides a control apparatus of brightness of a screen used for a projection display which comprises a light source, a screen on which a luminous flux emitted from the light source is modulated and displayed as a screen image brightness detection means for detecting brightness of this screen and input power control means to which the actually measured value detected by the brightness detection means is fed back, which compares it with a set value of screen brightness set in advance and which regulates the magnitude of the input power to be supplied to the light source in such a direction that the difference between them becomes zero.
The present invention provides also a control apparatus of brightness of a screen used for a projection display which comprises a light source, a screen on which a luminous flux emitted from the light source is modulated and displayed as a screen image, time measurement means for measuring actually the supply time of an input power to the light source, and input power control means to which the relationship between the magnitude of the input power to be supplied to the light source, its supply time and brightness of the light source is set so that brightness of the light source becomes substantially constant, which receives the signal from the time measurement means and which regulates the magnitude of the input power so that brightness of the light source becomes substantially constant, on the basis of the relationship set in advance.
In the control apparatus described above, the input power control means is preferably the one that changes and regulates an input current to the light source.
In the control apparatus described above, the input power control means includes, for example, a change-over switch for connecting individually the input side of the light source to a plurality of terminals for mutually different impressed voltage and a switch for switching the change-over switch upon receiving the signal from the time measurement means.
In the control apparatus described above, the input power control means includes, for example, a function generator which is connected to the time measurement means and to which the inverse function of the correlation of the supply time of the input power to the light source and brightness of the light source is set, and a multiplier which is disposed between the light source and a power source and outputs a signal regulating the magnitude of the input power upon receiving the signal from the function generator.
In the control apparatus described above, the input power control means includes, for example, a function generator which is connected to the time measurement means and to which the inverse function of the correlation of the supply time of the input power to the light source and brightness of the light source is set, and an amplifier which receives the signal from the function generator and regulates a power source voltage.
In the control apparatus described above, the time measurement means includes the one that detects the voltage applied to the power source and measures its supply time, or the one that measures an A.C. input of a D.C. amplifier for the light source.
In the control apparatus described above, it is advisable to dispose an alarm which operates at a time after the passage of a predetermined time from the point of time at which the magnitude of the input power to the light source attains a set maximum value.
In the control apparatus described above, a brightness sensor or an illumination sensor can be utilized as the brightness detection means.
In the control apparatus described above, examples of the light source include a Xe lamp, an Ar lamp, a mercury lamp and a halogen lamp.
The control apparatus described above preferably includes means for comparing the magnitude of the input power regulated by the input power control means with the magnitude of the actual input power supplied to the light source and for regulating the magnitude of the input power.
In accordance with the present invention, brightness of the screen is detected and fed back by the brightness detection means so that the input power control means operates in such a direction as to increase brightness of the light source. Accordingly, the drop of brightness of the light source with the passage of time is prevented by increasing the input power and brightness of the screen can be kept substantially constant.
Brightness of the light source drops with the passage of time while keeping the correlation with the magnitude of the input power to the light source and the time of use. Therefore, if such a correlation is in advance determined for the light source, the use time of the light source can be measured by the time measurement means without detecting brightness of the screen in practice, the magnitude of the input power can be regulated on the basis of the correlation determined in advance and brightness of the light source can be made substantially constant.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a structural view showing a control apparatus in accordance with one embodiment of the present invention;
FIG. 2 is a characteristic diagram showing the relation between brightness of a light source and a use time;
FIG. 3 is a structural view of the principal portions when control is effected in the same way as in the embodiment shown in FIG. 1 by use of a micro-computer;
FIG. 4 is a flowchart when brightness of the screen of a projection display is controlled by use of the apparatus shown in FIG. 3;
FIG. 5 is a structural view showing another embodiment of the present invention;
FIG. 6 is an explanatory view useful for explaining the change-over operation of a switch shown in FIG. 5;
FIG. 7 is a structural view showing still another embodiment of the present invention;
FIG. 8 is a structural view of the principal portions when control is effected in the same way as in the embodiment shown in FIG. 7 by use of a micro-computer;
FIG. 9 is a flowchart when brightness of the screen of a projection display is controlled by use of the apparatus shown in FIG. 8;
FIG. 10 is a structural view showing still another embodiment of the present invention; and
FIG. 11 is a structural view showing still another embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a system which detects brightness of a screen and controls brightness of the screen of a projection display. Incidentally, the system of FIG. 1 may be of the type which detects illumination of the screen by use of an illumination detector. Though the brightness detector 1 is shown disposed near the screen 2 in the drawing, it may be disposed within the reach range of angles θ, θ' of luminous fluxes. The operation and construction of the system will be hereinafter explained. The innermost loop 3 is a current control loop. This current control loop 3 consists of a projection light source 4, a D.C. amplifier 5 for a light source and a current detection resistor 6 (R I ). The current feedback control of this loop 3 is such that a current instruction 8 given from a brightness control loop 7 and a current feedback value 9 are processed by an adder 10 so that a light source current corresponding to the current instruction 8 flows. Incidentally, examples of the light source include a Xe lamp, an Ar lamp, a mercury lamp and a halogen lamp.
To control the light source current is substantially equal to the control of the input power to the light source 4. For, as the property peculiar to a discharge tube, the terminal voltage of the projection light source 4 is constant irrelevantly to a passing current. In other words, the following equation is given:
PT=Vt·It=K·It (1)
where:
Pt: input power,
Vt: terminal voltage,
It: passing current,
K: constant.
Accordingly, output brightness of the projection light source 4 can be controlled by controlling the input current. The brightness instruction 11 is generated by a potentiometer 12 or a brightness instruction variable resistor. This brightness instruction 11 and the output 13 of the brightness detector 1 on the screen 2, that is, screen brightness, are processed by the adder 14 and the processed result is applied to the brightness controller 15 to output the current instruction 8 described above.
If screen brightness or the brightness detection value drops, the brightness controller 15 increases the current instruction 8 to thereby increase the input current to the light source 4. This increase in the current results in the increase in the input power to the light source 4 and therefore operates so as to increase brightness of the light source 4. In accordance with the operation described above, brightness constant control can be made on the basis of the brightness instruction 11. The predetermined luminous flux from the projection light source 4 which has predetermined brightness passes through a projection lens 16 and an optical screen modulator 17 and strikes the screen 2 so that the picture corresponding to a modulation signal 18 is displayed on the screen 2.
The drop of brightness of the light source 4 will be explained with reference to FIG. 2. This diagram shows the characteristics of the projection light source 4. Brightness of the projection light source drops with the passage of its use time. Symbols I 1 , I 2 , I 3 and I 4 represent the magnitudes of the input current to the light source and symbols X L1 , X L2 , X L3 and X L4 represent brightness corresponding to the input currents I 1 , I 2 , I 3 and I 4 , respectively. Generally, brightness of a discharge tube drops as described above and its cause resides in that scattering materials of an electrode occurring with discharge adhere to the inside of the discharge tube and impede the passage of the rays of light. For this reason, brightness drops monotonously.
When brightness of the light source 4 drops, brightness of the screen 2 drops, too. This drop is detected by the brightness detector 1 and the input current to the light source 4, that is, the input power, is increased to prevent the drop of brightness of the light source 4 so as to keep brightness of the screen 2 substantially constant. This is attained by the embodiment shown in FIG. 1.
FIG. 3 is a structural view showing the principal portions of an apparatus performing substantially the same control as that of the embodiment shown in FIG. 1 by use of a micro-computer. In the drawing, reference numeral 19 represents a digital controller equipped with a micro-computer (MPU) and memories (ME); 50 is an analog input AI; 51 is an analog output AO; 52 is an analog/digital converter (AD); 53 is a digital/analog converter (DA); and 20 is a data input portion. The processing of this digital controller 19 is shown in the flowchart of FIG. 4.
The brightness instruction 11 is inputted to the digital controller 19 through AI and AD at step 21. The brightness detection output 13 from the brightness detector 1, that is, practical brightness of the screen, is inputted at step 22. The difference between the brightness instruction input value and the practical brightness value is calculated at step 23. Whether or not this difference is above a predetermined reference value is judged at step 24. This reference value is set so that screen brightness falls within an allowable range. If the difference described above is above the reference value, brightness of the light source must be increased. Therefore, the value of a new current instruction 8, that is, a new input power value, is calculated at step 25. This calculation can be conducted on the basis of the characteristics shown in FIG. 2. The input power instruction thus determined is output at step 26 to the adder 10 through DA and AO. If the difference is below the reference value, on the other hand, the input power need not be changed.
FIG. 5 shows a control system for measuring actually the supply time of the input power to the light source. A use time meter 27 for measuring this supply time detects the voltage 28 applied to the light source 4 and measures the application time. The input power control apparatus in this embodiment includes change-over switches 29, 30, 31, 32 for individually connecting the input side of the light source 4 to a plurality of terminals having mutually different impressed voltages and a switch 35 for receiving the signal 33 from the use time meter 27 and outputting the signal 34 which changes over the change-over switches 29, 30, 31, 32. As shown in FIG. 6, the change-over operation of the switches is made in such a manner as to increase the current instruction 8 with the use time. Due to this switching operation, brightness of the light source reaches a mean value X LA (1 m) and good screen brightness with less fluctuation can be obtained.
FIG. 7 shows another embodiment of the present invention. The input power control apparatus of this embodiment is equipped with a function generator 36 which is connected to the use time meter 27 and to which the inverse function of the correlation (FIG. 2) between the supply time of the input power to the light source and brightness of the light source 4 is set and with a multiplier 37 which is disposed between the light source 4 and its power source, receives the signal from the function generator 36 and outputs a signal for regulating the magnitude of the input power, that is, the current instruction 8. The control of this embodiment can be regarded as the one that changes continuously the current instruction 8.
FIG. 8 is a structural view showing the principal portions of an apparatus for making the control equivalent to that of the embodiment shown in FIG. 7 by use of a micro-computer. The processing of the digital controller 19 of this micro-computer is shown in the flowchart of FIG. 9. A voltage Vi which is a detection voltage of the voltage 28 is inputted to the digital controller 19 through AD at step 38. This Vi is compared with a Vset which is set in advance, at step 39. If Vi>Vset, brightness of the light source need not be increased and the procedure flows to step 40. When a light source use time T is reached at the pre-set voltage at step 40, the procedure then flows to step 41. A new input power value is calculated at this step 41. This calculation is based on the characteristic curve shown in FIG. 2. The input power instruction thus determined is output to the adder 10 through DA and AD at step 42. If Vi<Vset at step 39, on the other hand, the increase of the input power must be made at step 41 immediately.
FIG. 10 shows another embodiment of the present invention. This embodiment is the system which does not measure the voltage of the projection light source 4 for the measurement of the use time of the light source 4 but measures the application time of the A.C. input 43 to the D.C. amplifier 5 for the light source. In other words, a main power switch 44 and a rectifier 45 are disposed next to the A.C. input 43. This measurement method is more economical.
Furthermore, an alarm lamp 46 requiring the replacement of the projection light source 4 is disposed. If the time lapsed after the application of the maximum current to the projection light source 4 exceeds a predetermined time, the alarm lamp 4 indicates that the life of the projection light source 4 is up. Accordingly, if the light source 4 is replaced beforehand, a stable projection light source 4 free from interruption can be obtained.
In FIG. 11, there is shown disposed an amplifier 47 which changes the power source voltage for a brightness instruction resistor in accordance with the use time in place of the multiplier 37 shown in FIG. 7, and its action and effect is the same as that of FIG. 7.
In accordance with the control method of brightness of a screen of the present invention, brightness of the light source can be kept substantially constant by increasing the input power to the light source even when brightness of the light source drops with the passage of time. Accordingly, brightness of the screen, too, can be kept substantially constant and a projection display providing a stable picture in connection with brightness can be obtained. Moreover, the life of the light source can be extended.
The control method described above can be practiced easily in accordance with the control apparatus of brightness of the screen.
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Brightness of a screen is detected on the basis of a luminous flux projected from a light source to the screen. This detection signal is fed back and a set value of brightness of the screen is compared with the detection signal. The magnitude of input power to the light source is controlled so that the comparison value becomes zero.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Prov. Ser. 61/525,366 filed Aug. 19, 2011 which is hereby incorporated by reference herein in its entirety.
BACKGROUND OF THE INVENTION
[0002] The field of intralumenal therapy for the treatment of vascular disease states has for many years focused on the use of many different types of therapeutic devices. While it is currently unforeseeable that one particular device will be suitable to treat all types of vascular disease states it may however be possible to reduce the number of devices used for some disease states while at the same time improve patient outcomes at a reduced cost. To identify potential opportunities to improve the efficiency and efficacy of the devices and procedures it is important for one to understand the state of the art relative to some of the more common disease states.
[0003] One cerebrovascular disease state is ischemia resulting from reduced or blocked arterial blood flow. The arterial blockage may be due to thrombus, plaque, foreign objects or a combination thereof. Generally, soft thrombus created elsewhere in the body (for example due to atrial fibrillation) that lodges in the distal cerebrovasculature may be disrupted or dissolved using mechanical devices and or thrombolytic drugs. While guidewires are typically used to disrupt the thrombus, some sophisticated thrombectomy devices have been proposed. For instance U.S. Pat. No. 4,762,130 to Fogarty et al., entitled, “Catheter with Corkscrew-Like Balloon”, U.S. Pat. No. 4,998,919 of Schepp-Pesh et al., entitled, “Thrombectomy Apparatus”, U.S. Pat. No. 5,417,703 to Brown et al., entitled “Thrombectomy Devices and Methods of Using Same”, and U.S. Pat. No. 6,663,650 to Sepetka et al., entitled, “Systems, Methods and Devices for Removing Obstructions from a Blood Vessel” discloses devices such as catheter based corkscrew balloons, baskets or filter wires and helical coiled retrievers. Commercial and prototype versions of these devices have shown only marginal improvements over guidewires due to an inability to adequately grasp the thrombus or to gain vascular access distal to the thrombus(i.e. distal advancement of the device pushes the thrombus distally).
[0004] To remove foreign objects from a body lumen, a number of catheter based retrieval devices have been proposed such as a spring jaw medical instrument disclosed in U.S. Pat. No. 5,782,747 entitled, “Spring Based Multi-purpose Medical Instrument.” That apparatus, used for capturing an intravascular object, has a variety of jaw structures including a configuration having opposing serrated surfaces for crushing an object and a configuration having a closed loop jaw suitable for grasping an object. Proposed devices for the removal of foreign objects such as embolic coils and stents are disclosed in U.S. Pat. No. 6,989,020 to Jones et al., entitled, “Embolic Coil Retrieval System” which includes biased jaw members having major and minor teeth positioned along the outer edge of the jaw members. Additional retrieval devices are described in U.S. Pat. No. 6,673,100 to Diaz et al., entitled, “Method and Device for Retrieving Embolic Coils” wherein the system includes an outwardly biased jaw member having an acutely angled latch member for grasping coils.
SUMMARY OF THE INVENTION
[0005] In accordance with one aspect of the present invention there is provided a medical device system for removing an object from a body lumen of a mammal. The retrieval system includes a catheter or sheath having proximal and distal ends and a lumen extending therethrough and a retrieval device comprising an elongate flexible member having a capture member coupled to its distal end. The retrieval device is slidably positioned within the catheter lumen. The capture member of the retrieval device has first and second arms that are resiliently biased in an open configuration. The capture member further includes an engagement member extending between the first and second arms. The engagement member includes a plurality of retaining elements positioned along the length of the engagement member which are resiliently biased and generally extend in a direction towards the first or second arms when unconstrained. The capture member of the retrieval device is operable between an unconstrained configuration in which the arms are open and a constrained configuration where the arms are generally closed or collapsed. In the constrained configuration the arms are brought into contact with the retaining elements of the engagement member causing the retaining elements to collapse. During delivery to a target site, the retrieval device is positioned within the lumen of the catheter thereby placing the capture member in a constrained configuration. Upon exiting the catheter lumen, the resilient arms of the capture member are unconstrained and move to an open configuration exposing the engagement member and allowing the retaining elements to take there biased configuration. To capture an object the capture member is positioned such that a portion of the object is between a capture arm and retaining element. The catheter may then be advanced to collapse the capture arms thus securing the object between the arm and engagement member. The retrieval system may then be removed along with the object.
[0006] In accordance with another aspect of the present invention there is provided a retrieval system comprising biocompatible resilient materials. Suitable resilient materials include metal alloys such as nitinol, titanium, stainless steel and cobalt chromium and any alloys thereof Additional suitable materials include polymers such as polyimides, polyamides, fluoropolymers, polyetheretherketone (PEEK) and shape memory polymers. These materials may be formed into desired shapes by a variety of methods which are appropriate to the materials be in utilized such as laser cutting, injection molding, welding, electrochemical machining, machining, photo-etching and casting.
[0007] In accordance with still another aspect of the present invention there is provided a retrieval system having a capture member that includes radiopaque materials to provide visibility under fluoroscopy. The radiopaque materials may take the form of markers (including coils, rivets and radiopaque shrink tubing) positioned on portions of the capture member. The capture member may include a radiopaque coating utilizing radiopaque materials. Suitable radiopaque materials include gold, tantalum, tungsten, platinum, iodinated or barium containing compounds or mixtures and alloys thereof. Coatings may be applied using known techniques such as electro deposition, sputtering, dipping, printing and spray methods.
[0008] In accordance with another aspect of the present invention there is provided a method of retrieving an object, such as an embolic coil or stent from the body. The method comprises the steps of positioning a catheter at a preselected site within a body lumen, providing an elongate flexible retrieval device deliverable through the lumen of said catheter, advancing the retrieval device such that the distal capture member exist the catheter lumen and expands, positioning the capture member to engage the object, advancing the catheter relative to the retrieval device to secure the object and removing the retrieval system and object from the body.
[0009] A more detailed explanation of the invention is provided in the following description and claims, and is illustrated in the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a partial cross-sectional view of a retrieval system according to an embodiment of the present invention.
[0011] FIG. 2 is an enlarged partial cross-sectional view of the distal end of the retrieval system according to an embodiment of the present invention.
[0012] FIG. 3A is a partial perspective view of the distal portion of a deployed retrieval system according to an embodiment of the present invention.
[0013] FIG. 3B is a partial perspective view of the distal portion of a deployed retrieval system according to another embodiment of the present invention.
[0014] FIGS. 4 through 7 are partial cross-sectional views illustrating a method of using a retrieval system within a vessel at a target site to remove an object according to an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0015] FIG. 1 illustrates a retrieval system 10 suitable for use in removing foreign objects such as embolic coils and stents. Retrieval system 10 includes a catheter 20 formed of a polymeric material as is known in the art, having distal end 22 , proximal end 24 and lumen 25 extending therethrough. Catheter hub 26 , having a luer connector is coupled to proximal end 24 . While not shown, the construction of catheter 20 may utilize known catheter technologies that incorporate braiding and or coiling using metallic or non-metallic reinforcing filamentous materials to provide high strength while maintaining catheter flexibility. The incorporation of lubricious hydrophilic and or hydrophobic materials on the inner and or outer surface of the catheter is considered to be within the scope of known catheter construction techniques and suitable for use in a retrieval system according to embodiments of the present invention. Positioned within catheter 20 is an elongate flexible retrieval device 30 having distal end 32 and proximal end 34 . Retrieval device 30 includes a pushable flexible member 36 extending from proximal end 34 to distal end 32 . Flexible member 36 preferably takes the form of a wire having a distal taper similar to that of guidewires. Suitable materials include stainless steels, nitinol and polymers. Preferably a flexible coil 38 is positioned over the distal portion of flexible member 36 to aid in delivery. Capture member 40 is coupled to coil 38 at distal end 32 typically through soldering, welding or gluing.
[0016] FIG. 2 provides an enlarged view of the distal end of retrieval system 10 where capture member 40 is shown to include capture arms 42 and 44 that extend outwardly from the longitudinal axis of retrieval device 30 . Capture arms 42 and 44 are formed of a resilient material and biased in an open configuration. Capture member 40 may be formed from a tube of nitinol that has been partially split wherein each half of the split tube is shaped to become a capture arm. Engagement member 46 having shaft 47 , proximal end 48 , distal end 49 and distal tip 50 is coupled to capture member 40 at proximal end 48 and is positioned between capture arms 42 and 44 . Engagement member 46 includes a number of retaining elements represented by retaining elements 52 , 54 , 56 and 58 . Retaining elements of engagement member 46 extend from shaft 47 in an angled direction towards the capture arms. For instance, representative retaining elements 52 and 54 on one side of shaft 47 are angled towards capture arm 42 while representative retaining elements 56 and 58 on the opposite side of shaft 47 are angled towards capture arm 44 . The orientation of the retaining elements relative to the capture arms is depicted in the perspective view of FIG. 3A .
[0017] As shown in FIG. 3A , arms 42 and 44 are generally spaced apart when capture member 40 is in an unconstrained configuration. The distance between arms 42 and 44 may range from 1.5 mm to 5 mm for devices designed for use in neurovascular applications, however, may range from 1.5 mm to 50 mm for devices designed for use in other body lumens. The lengths of arms 42 and 44 are also dependant upon a particular design for a particular application but typically range from 3 mm to 50 mm. Representative retaining elements 52 and 54 are spaced apart on the same side of engagement member 46 as previously discussed. The length, angle and spacing distance for retaining elements is dependant upon the designed device and dimensions of the object to be removed but may typically range from length of 1 mm to 20 mm, an angle of 5 to 85 degrees and a spacing distance of 0.010 inches to 0.080 inches. Capture member 40 of retrieval device 30 is operable between an unconstrained configuration in which arms 42 and 44 are open and a constrained configuration, such as within a catheter lumen, where the arms are generally closed or collapsed. In the constrained configuration, arms 42 and 44 are brought into contact with retaining elements 52 , 54 56 and 58 of engagement member 46 causing the retaining elements to collapse. In the constrained configuration the collapsed retaining elements are shielded by collapsed arms 42 and 44 .
[0018] FIG. 3B illustrates a retrieval device according to another embodiment. While many portions of retrieval device 130 are similar to previously described retrieval device 30 , engagement member 146 does not have retaining elements that project towards the capture arms. Engagement member 146 includes a plurality of retaining elements 152 , 154 and 156 that take the form of grooves or recessed areas in shaft 147 .
[0019] Preferably, the retrieval devices of embodiments of the present invention comprise a biocompatible resilient material. Suitable resilient materials include metal alloys such as nitinol, titanium, stainless steel. Additional suitable materials include polymers such as polyimides, polyamides, fluoropolymers, polyetheretherketone (PEEK) and shape memory polymers. These materials may be formed into desired shapes by a variety of methods which are appropriate to the materials be in utilized such as laser cutting, thermal heat treating, vacuum deposition, electro-deposition, vapor deposition, chemical etching, photo etching, electro etching, stamping, injection molding, casting or any combination thereof. In addition, the biased resiliency of these materials allow a retrieval device with a normally expanded configuration to have a collapsed, small diameter configuration when constrained within a delivery catheter suitable for delivery to a target site and upon being deployed at a target site return to its expanded configuration.
[0020] A method of removing a foreign object such as an embolic coil using retrieval system 10 is illustrated in FIGS. 4 , 5 , 6 and 7 . Catheter 20 is introduced into vessel 200 and distal end 22 is positioned adjacent a target site such as embolic coil 202 . Retrieval device 30 is then introduced into and advanced through the catheter with the arms 42 and 44 in a constrained collapsed configuration as illustrated in FIG. 4 . As shown in FIG. 5 , when capture member 40 exits the lumen of catheter 20 , arms 42 and 44 move to an open unconstrained configuration. The capture member is then manipulated to cause the retaining elements of engagement member 46 to sufficiently engage a portion of embolic coil 202 . Catheter 20 is then advanced relative to retrieval device 30 such that distal end 22 causes arms 42 and 44 to collapse thereby securing a portion of coil 202 as illustrated in FIG. 6 . FIG. 7 depicts retrieval system 10 , along with secured coil 202 , being retracted from the target site and subsequently removed from the body.
[0021] Novel devices, systems and methods have been disclosed to remove foreign objects from a body lumen of a mammal. Although preferred embodiments of the invention have been described, it should be understood that various modifications including the substitution of elements or components which perform substantially the same function in the same way to achieve substantially the same result may be made by those skilled in the art without departing from the scope of the claims which follow.
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Devices, systems and methods are provided for performing intra-lumenal medical procedures in a desired area of the body. Retrieval devices and methods of performing medical procedures to remove foreign objects to re-establish the intravascular flow of blood are provided.
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BACKGROUND OF THE INVENTION
[0001] The application claims priority to German Application No. 10 2004 018 461.5, which was filed on Apr. 16, 2004.
[0002] The invention relates to a sliding roof system comprising at least one guide rail, a carriage shiftable in the guide rail, and a cover support adapted for attachment to a cover and coupled with the carriage.
[0003] Sliding roof systems for vehicles are generally known. These sliding roof systems are capable of shifting at least one cover (made from sheet metal, plastics or glass, for instance) between a closed position and an open position. In the closed position, an opening in a vehicle roof will be closed. When the cover is in the open position, the opening will be at least partially exposed.
[0004] All sliding roof systems in which the cover is shifted outwardly, such that the cover lies on an outer surface of the vehicle roof in the open position, share a common feature regarding travel and height. It is desirable to provide as much outward travel as possible in combination with an overall height of the sliding roof system that is as small as possible. With a multitude of systems, the travel is directly provided by slotted pieces that are attached to a guide rail or a carriage. In this configuration, the travel is smaller than the height of the guide rail. In order to obtain a particularly large travel, the guide rail has to be constructed to have an increased height, which in turn results in a reduced headroom in an interior of the vehicle. Constructions are also known in which a lifting motion, which is predefined by a slotted piece, is translated by means of levers into a larger travel of the cover. These systems, however, are relatively complicated.
[0005] It is the objective of the present invention to provide a sliding roof system of the type initially mentioned, in which a particularly large travel can be achieved with low effort.
SUMMARY OF THE INVENTION
[0006] In order to meet this objective, a sliding roof system includes a first lifting lever that has one end connected to a cover support and another end connected to a carriage with two guide pieces that are movable within slots. This type of connection is referred to as a “slotted piece guide.” The first lifting lever produces a desired large lifting motion because the first lifting lever is directly coupled with the carriage with a slotted piece guide connection. This provides a particularly simple construction, which can be manufactured at favorable costs, and with low tolerances. The term “slotted piece guide” means in this context the engaging of a movable element in a slotted piece.
[0007] According to a preferred embodiment of the invention, the sliding roof system includes a second lifting lever that has one end connected to the cover support and another end connected with two guide pieces to the carriage in a slotted piece guide connection. In this way it is possible to have full control over the lifting motion of the cover just by the movement of the carriage and without any intermediate levers or complicated transmissions.
[0008] Advantageous designs of the invention will be apparent from the sub-claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a schematic, perspective view of a vehicle roof with a sliding roof system according to the invention.
[0010] FIG. 2 is a schematic view of a guide rail in which components of a sliding roof system according to a first embodiment of the invention are arranged with a cover being in a closed position.
[0011] FIG. 3 is a view corresponding to that of FIG. 2 , with the cover being in a ventilation position.
[0012] FIG. 4 is a view corresponding to that of FIG. 2 , with the cover being in a fully raised position extending outwardly.
[0013] FIG. 5 shows in a view corresponding to that of FIG. 2 , a sliding roof system according to a second embodiment of the invention.
[0014] FIG. 6 shows in a view corresponding to that of FIG. 4 , the sliding roof system according to the second embodiment.
[0015] FIG. 7 shows in a view corresponding to that of FIG. 2 , a sliding roof system according to a third embodiment of the invention.
[0016] FIG. 8 shows in a view corresponding to that of FIG. 4 , the sliding roof system according to the third embodiment.
[0017] FIG. 9 shows in a view corresponding to that of FIG. 3 , a sliding roof system according to a forth embodiment.
[0018] FIG. 10 shows the sliding roof system of FIG. 9 , in a fully open position.
[0019] FIG. 11 is a schematic side view of a sliding roof system according to a fifth embodiment, with the cover being in an open position.
[0020] FIG. 12 is a schematic side view of the sliding roof system of FIG. 11 , with the cover being in a ventilation position.
[0021] FIG. 13 shows a further side view of the sliding roof system of FIG. 11 , with the cover being in an outwardly raised position.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0022] FIG. 1 shows a vehicle roof 5 with an opening 7 . Associated with the opening 7 is a cover 9 that can be moved between a closed position in which the cover 9 closes the opening 7 , and an open position that at least partially exposes the opening 7 . Associated with the cover 9 is a sliding roof system, the essential components of which include two guide rails 10 , first and second lifting levers 12 , 14 , and two cover supports 16 . The cover supports 16 are configured as separate components that are fixedly mounted to the cover 9 . Nevertheless, the cover supports 16 may also be constituted by inlay parts, which are embedded in the cover 9 , or constituted by fastening tabs that are formed in one piece with the cover 9 , etc.
[0023] The two guide rails 10 extend along longitudinal edges of opening 7 , i.e., extend along a longitudinal direction of travel of a vehicle, from front to rear. Usually the guide rails 10 are formed by a section made of an aluminum alloy. A carriage 18 (see FIG. 2 ) is movably arranged in each guide rail 10 . Coupled to the carriage 18 is a drive mechanism (not shown), such as a metal cable that is resistant to bending and tension for example, and which is driven by a drive motor (not shown). The carriage 18 is typically made from a plastic material.
[0024] In the first embodiment, the carriage 18 has the first and second lifting levers 12 , 14 coupled to the carriage 18 . The first lifting lever 12 is a front lifting lever and the second lifting lever 14 is a rear lifting lever. Slotted piece guides are used to couple the first and second lifting levers 12 , 14 with the carriage 18 . These are formed by a plurality of lifting slots in the carriage 18 that are engaged by pins provided on the first and second lifting levers 12 , 14 . The carriage 18 has a first lifting slot 20 , which (related to the direction of travel of the vehicle) is arranged on a front end of the carriage 18 . As seen from the front to the rear, the first lifting slot 20 initially runs obliquely to the rear in a downward direction and then extends generally to the rear, further slightly falling away. A second lifting slot 22 is arranged on the carriage 18 roughly in the middle, with a front edge of the second lifting slot 22 lying above and ahead of a rear end of the first lifting slot 20 . Starting from a front end, the second lifting slot 22 extends approximately in a straight line to the rear with a slight inclination. A short transition portion is provided in the middle, where the second lifting slot 22 extends so as to be horizontal. A third lifting slot 24 starts underneath a rear end of the second lifting slot 22 , initially extends horizontally to the rear, then ascends in an upward direction, subsequently extends horizontally again to the rear, and finally extends in an obliquely downward direction to the rear.
[0025] The first lifting lever 12 is connected with the first lifting slot 20 and the second lifting slot 22 by the first and second pins 26 , 27 . The second pin 27 is arranged on a rear end of the first lifting lever 12 , and the first pin 26 is arranged on the first lifting lever 12 at a distance from the second pin 27 further to the front. The distance between the first and second pins 26 , 27 , however, is smaller than half the length of the first lifting lever 12 . The end of the first lifting lever 12 that is opposite to the second pin 27 is connected with the cover support 16 by a first bolt 30 .
[0026] The second lifting lever 14 is connected with the third lifting slot 24 by means of third and fourth pins 28 , 29 . The third pin 28 is arranged on a front end of the second lifting lever 14 , and the fourth pin 29 is situated behind a front end of the second lifting lever 14 . The distance between the third and fourth pins 28 , 29 is smaller than half the length of the second lifting lever 14 . At a rear end opposite to the third pin 28 , the second lifting lever 14 is connected with the cover support 16 by a second bolt 31 .
[0027] The cover support 16 provides support for the cover 9 , and is provided with a guide tab 34 at a front end. Attached to a lower end of the guide tab 34 is a guide pin 36 . The guide pin 36 engages into a guiding slot 38 . Starting from a front end of the guide rail 10 , the guiding slot 38 initially extends obliquely upwards to the rear and then in a straight line along the guide rail 10 .
[0028] FIG. 2 shows the carriage 18 in a position that corresponds to the closed position of cover support 16 and cover 9 . The carriage 18 is shifted to the front to the full extent, so that the fourth pin 29 is situated at a rear end of the third lifting slot 24 and the first and second pins 26 , 27 are situated at the rear end of the first lifting slot 20 and second lifting slot 22 , respectively. The guide pin 36 of the cover support 16 is at the front, lower end of the guiding slot 38 . In this position, the cover support 16 and the cover 9 are locked in the closed position. Movement in a vertical direction is prevented by the first and second lifting levers 12 , 14 , which due to being coupled to the carriage 18 , cannot perform a vertical movement. A movement of the cover support 16 in the longitudinal direction is prevented by the guide pin 36 , which is retained in the guiding slot 38 .
[0029] When cover 9 is being opened, the carriage 18 is shifted from the position shown in FIG. 2 to the rear to the position shown in FIG. 3 . This causes the rear end of the second lifting lever 14 , which is connected with the cover support 16 , to be swiveled upwards, because the fourth pin 29 moves upward in the third lifting slot 24 , while the third pin 28 moves downward in the third lifting slot 24 . Thus, the second lifting lever 14 performs a swiveling motion about a point lying between third and fourth pins 28 , 29 , such that the rear end of the cover support 16 is lifted.
[0030] The first lifting lever 12 only performs a slight lifting motion because the second pin 27 goes down slightly during shifting of the carriage 18 , while at the same time the first pin 26 goes up slightly. The resulting, short travel of the front end of the first lifting lever 12 , is transferred via the first bolt 30 to the cover support 16 which performs a corresponding lifting motion in the region of the front end. This causes the guide pin 36 in the guiding slot 38 to be slightly lifted, whereby the cover support 16 is shifted to the rear by a small amount. The position shown in FIG. 3 is usually termed a ventilation position because it is mainly a rear edge of cover 9 which is lifted, so that a ventilation of vehicle interior space is achieved by a gap at the rear edge.
[0031] To further open the cover 9 , the carriage 18 is further shifted to the rear. In so doing, the second lifting lever 14 essentially remains in a position shown in FIG. 3 , while the front end of the first lifting lever 12 is lifted further. This can be in particular traced back to the fact that the first pin 26 is markedly shifted upwards by the front end of the first lifting slot 20 . In addition, the second pin 27 further goes down in the second lifting slot 22 . It is by this lifting motion at the front end of the cover support 16 that the guide pin 36 is further lifted, until the guide pin 36 enters the horizontally extending portion of the guiding slot 38 . The cover support 16 together with the cover 9 can now be shifted to the rear by the carriage 18 , so that the opening 7 is fully exposed in the vehicle roof 5 .
[0032] If the cover 9 is to be closed again, the carriage 18 is shifted to the front, whereupon the reversed motion sequence of the first and second lifting levers 12 , 14 will occur, until cover 9 has arrived in the closed position again.
[0033] A particular advantage of the sliding roof system according to the invention is that the lifting motion can be produced with very few components. Two lifting levers are used, which are directly coupled with both the carriage 18 and the cover support 16 . Intermediate levers or transmission levers are not required. As the lifting slots are arranged at advantage, in particular as the lifting slots overlap each other, the carriage 18 can be configured to have a short length, seen in the direction of shifting. Despite a very small overall height, a comparably large travel of the cover 9 is produced due to the transmission achieved with the first and second lifting levers 12 , 14 .
[0034] In FIGS. 5 and 6 there is shown a sliding roof system according to a second embodiment. For the components known from the first embodiment the same reference numerals are used, and insofar reference is made to the above explanations.
[0035] The difference from the first embodiment is that the carriage 18 is configured to include two parts and has a front carriage part 18 a and a rear carriage part 18 b. The front and rear carriage parts 18 a, 18 b are connected with each other by a joint 19 comprising a ball joint or pivot joint. The joint 19 allows use of a guide rail with a varying curvature, to which the carriage 18 can adapt.
[0036] In FIGS. 7 and 8 there is shown a sliding roof system according to a third embodiment. For the components known from the first embodiment the same reference numerals are used, and insofar reference is made to the above explanations.
[0037] The difference from the first embodiment is that the cover 9 of the third embodiment can only be put to a ventilation position (see FIG. 8 ) and cannot be completely moved to the rear. In this configuration, the first lifting lever at the front may be omitted; there is merely provided the second lifting lever 14 at the rear. Accordingly, the carriage 18 is provided with one lifting slot only, namely the third lifting slot 24 at the rear, known from the first embodiment. This third lifting slot 24 is also known from the rear carriage part 18 b of the second embodiment.
[0038] In FIGS. 9 and 10 there is shown a sliding roof system according to a fourth embodiment. For the components known from the first embodiment the same reference numerals are used, and insofar reference is made to the above explanations.
[0039] The sliding roof system according to the fourth embodiment is a combination of the first and third embodiments. The fourth embodiment includes a first cover 9 that can be moved from a ventilation position (see FIG. 9 ) to a fully open position (see FIG. 10 ). As seen in the direction of travel, there is additionally provided behind cover 9 a second cover 9 ′, which from a fully closed position can only be put to a ventilation position (see FIG. 9 ). In case the first cover 9 is raised outwardly beyond the ventilation position and then moved to the rear, the second cover 9 ′ will return to the closed position (see FIG. 10 ) again, so that the first cover 9 can pass over the second cover 9 ′.
[0040] For controlling the first 9 and second 9 ′ covers there are provided separate drive mechanisms (not shown) that can be signaled in an appropriate manner. It is also conceivable to use one drive mechanism only, which is coupled with the carriage 18 for the first and second covers 9 , 9 ′ in a suitable way, so that, during opening the first cover 9 , the second cover 9 ′ performs the desired movement to the ventilation position and back again.
[0041] FIGS. 11 to 13 show a sliding roof system according to a fifth embodiment. In the basic construction, the fifth embodiment corresponds to the first embodiment, so that essentially only the differences of the fifth embodiment in relation to the first embodiment will be described in the following.
[0042] The sliding roof system according to the fifth embodiment differs from that according to the first embodiment in that a guiding lever 40 is provided instead of the guide tab 34 fixedly attached to the cover support 16 . One end of the guiding lever 40 is pivotally connected with the cover support 16 by a joint 42 . A side of the guiding lever 40 facing away from the joint 42 is connected with the guiding slot 38 (shown in FIGS. 11-13 at its center axis) through first and second guide pins 36 , 37 . In the embodiment shown, two portions of the guiding lever 40 include an angle of about 140°. Other values are also possible depending on the constructional circumstances.
[0043] When the cover 9 is in the closed position ( FIG. 11 ), the guiding lever 40 retains the front end of the cover support 16 in a lowered position. It is in this position of the guiding lever 40 that the guide pin 36 , attached to the end of the guiding lever 40 that faces away from the cover support 16 , is situated in the upper, approximately horizontally extending portion of the guiding slot 38 . The second guide pin 37 , which is arranged approximately in the middle of the guiding lever 40 , is situated at the lower, front end of the guiding slot 38 .
[0044] When the cover 9 is in the ventilation position ( FIG. 12 ), the cover 9 has been shifted as a whole by a certain amount to the rear (to the right in the Figures) in relation to the closed position. Thereby the second guide pin 37 of the guiding lever 40 has moved upwards by a small amount in the guiding slot 38 , while the first guide pin 36 has merely traveled to the right approximately on a constant level. Thereby the guiding lever 40 has been pivoted in a clockwise direction about the first guide pin 36 (in addition to the translational movement), so that the joint 42 , and with this the front edge of the cover 9 , has been shifted in upward direction. Thus, the cover 9 has been lifted away from a seal against which the cover 9 rests at a front edge.
[0045] When the cover 9 is in a position where the cover 9 is fully raised outwardly ( FIG. 13 ), the cover 9 has been shifted to the right and beyond the ventilation position. Thereby the second guide pin 37 also arrives at the horizontal portion of the guiding slot 38 . This causes the guiding lever 40 to pivot about the first guide pin 36 even farther, so that the front edge of the cover 9 will be raised outwards to the maximum extent.
[0046] The particular advantage of the fifth embodiment is the compact design. The first embodiment requires elongation of the guiding slot at a front end as far as underneath a level which is defined by the guide rail proper. This portion, clearly seen in FIGS. 2 to 4 , results in a large overall height and may lead to a restriction of the headroom in the interior of the vehicle. With the fifth embodiment the guiding lever 40 acts as a transmission mechanism. The guiding slot 38 has a comparably small height, because the guiding slot 38 is fully housed within the profile of the guide rail 10 ; a portion protruding downward is not necessary. By the guiding lever 40 , the small height of the guiding slot 38 is translated to a larger travel of the front portion of cover 9 .
[0047] Although a preferred embodiment of this invention has been disclosed, a worker of ordinary skill in this art would recognize that certain modifications would come within the scope of this invention. For that reason, the following claims should be studied to determine the true scope and content of this invention.
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A sliding roof system includes at least one guide rail, a carriage shiftable in the guide rail, and a cover support coupled with the carriage. The cover support is adapted to be attached to a cover that is movable to open and close a roof opening. A first lifting lever has one end connected to the cover support and another end connected to the carriage with guide pieces received within slots formed in the carriage.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The field of invention relates to show drying apparatus, and more particularly pertains to a new and improved shoe drying support apparatus wherein the same is directed to the positioning of tennis shoes and the like within a clothes dryer.
2. Description of the Prior Art
Structure for positioning shoes and the like within a dryer is addressed in U.S. Pat. No. 4,702,016, wherein the use of a magnetic plate is arranged to secure shoes to be dried in adjacency to a shoe drying drum, wherein the shoe is fixedly positioned relative to the interior surface of the drum.
U.S. Pat. No. 3,840,998 to Marcussen sets forth a basket for positioning within a dryer structure.
U.S. Pat. Nos. 4,908,957 and 5,016,364 are examples of structure arranged to effect drying of shoes and the like.
The instant invention attempts to overcome deficiencies of the prior art by providing the shoes to be tumbled within a clothes drum when positioned within a securing basket and in this respect, the present invention substantially fulfills this need.
SUMMARY OF THE INVENTION
In view of the foregoing disadvantages inherent in the known types of shoe drying apparatus now present in the prior art, the present invention provides a shoe drying support apparatus wherein the same is arranged to secure fabric shoes within a clothes dryer to effect their drying and tumbling within the clothes dryer drum. As such, the general purpose of the present invention, which will be described subsequently in greater detail, is to provide a new and improved shoe drying support apparatus which has all the advantages of the prior art shoe drying apparatus and none of the disadvantages.
To attain this, the present invention provides a mesh tubular basket arranged for mounting about a support tube and secured at each end of the mesh basket by strap members to position canvas type shoes and the like within a clothes dryer during a drying procedure. The support tube is arranged with a spring-biased sleeve, having a collar member to secure the sleeve if desired in a biased orientation against an interior wall of a drying machine drum.
My invention resides not in any one of these features per se, but rather in the particular combination of all of them herein disclosed and claimed and it is distinguished from the prior art in this particular combination of all of its structures for the functions specified.
There has thus been outlined, rather broadly, the more important features of the invention in order that the detailed description thereof that follows may be better understood, and in order that the present contribution to the art may be better appreciated. There are, of course, additional features of the invention that will be described hereinafter and which will form the subject matter of the claims appended hereto. Those skilled in the art will appreciate that the conception, upon which this disclosure is based, may readily be utilized as a basis for the designing of other structures, methods and systems for carrying out the several purposes of the present invention. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the present invention.
Further, the purpose of the foregoing abstract is to enable the U.S. Patent and Trademark Office and the public generally, and especially the scientists, engineers and practitioners in the art who are not familiar with patent or legal terms or phraseology, to determine quickly from a cursory inspection the nature and essence of the technical disclosure of the application. The abstract is neither intended to define the invention of the application, which is measured by the claims, nor is it intended to be limiting as to the scope of the invention in any way.
It is therefore an object of the present invention to provide a new and improved shoe drying support apparatus which has all the advantages of the prior art shoe drying apparatus and none of the disadvantages.
It is another object of the present invention to provide a new and improved shoe drying support apparatus which may be easily and efficiently manufactured and marketed.
It is a further object of the present invention to provide a new and improved shoe drying support apparatus which is of a durable and reliable construction.
An even further object of the present invention is to provide a new and improved shoe drying support apparatus which is susceptible of a low cost of manufacture with regard to both materials and labor, and which accordingly is then susceptible of low prices of sale to the consuming public, thereby making such shoe drying support apparatus economically available to the buying public.
Still yet another object of the present invention is to provide a new and improved shoe drying support apparatus which provides in the apparatus and methods of the prior art some of the advantages thereof, while simultaneously overcoming some of the disadvantages normally associated therewith.
These together with other objects of the invention, along with the various features of novelty which characterize the invention, are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and the specific objects attained by its uses, reference should be had to the accompanying drawings and descriptive matter in which there is illustrated preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood and objects other than those set forth above will become apparent when consideration is given to the following detailed description thereof. Such description makes reference to the annexed drawings wherein:
FIG. 1 is an isometric illustration of the invention in use.
FIG. 2 is an enlarged isometric illustration of the invention.
FIG. 3 is an isometric illustration of the invention in a partially exploded view.
FIG. 4 is an isometric view, partially in section, indicating the spring-biased construction of the outer sleeve.
FIG. 5 is an enlarged isometric illustration of section 5 as set forth in FIG. 4.
FIG. 6 is an orthographic view, taken along the lines 6--6 of FIG. 4 in the direction indicated by the arrows.
FIG. 7 is an isometric illustration of the invention employing a deodorizing dispenser structure.
FIG. 8 is an enlarged orthographic view of section 8 as set forth in FIG. 7.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference now to the drawings, and in particular to FIGS. 1 to 8 thereof, a new and improved shoe drying support apparatus embodying the principles and concepts of the present invention and generally designated by the reference numeral 10 will be described.
More specifically, the shoe drying support apparatus 10 of the instant invention essentially comprises the invention arranged for positioning within a clothes dryer 11, and more specifically, within a clothes dryer drum 12. To this end, a mounting tube 15 is provided, having a first end, including a first end resilient cap 14 mounted thereon for frictional engagement within the drum 12. The mounting tube includes a mounting tube second end terminating in a mounting tube abutment wall 16 (see FIGS. 4 and 5). The abutment wall 16 is spaced from a locking collar 17, with the locking collar including a collar conical internally threaded surface 20 arranged for threaded engagement and securing of an outer sleeve 21, and more specifically, the outer sleeve first end having a sleeve externally threaded cylindrical first end surface 23. In this manner, the conical threads are arranged to lock the sleeve in a predetermined orientation along the mounting tube 13 (see FIG. 6). The outer sleeve 21 accordingly includes an outer sleeve cavity 19 oriented between the abutment wall 16 and an outer sleeve resilient cap 22 positioned at a second end of the outer sleeve 21, with a biasing spring 18 positioned within the cavity 19 to effect biasing of the outer sleeve 21 exteriorly of the abutment wall in a projecting manner to effect engagement within the clothes dryer drum 12. In this manner, the locking sleeve 17 need not be employed as the spring-biased engagement of the outer sleeve resilient cap 22, as well as the engagement of the mounting tube first end resilient 14, may position the structure within the drum 12. If additional tension is desired, the locking collar 17 and the outer sleeve first end are slid along the mounting tube 13 to provide for enhanced pressure engagement of the mounting tube 13 within the drum 12.
First and second lock sleeve 24 and 25 are mounted to the mounting tube 13 in a spaced relationship between the locking collar 17 and the mounting tube first end. Securing the locking sleeves are respective first and second fasteners 26 and 27 directed through the locking sleeves for engagement with the mounting tube 13 for fixed positioning of the respective first and second lock sleeves 24 and 25. A tubular net 28 is directed between the first and second lock sleeves 24 and 25, wherein the tubular end includes a tubular net first end 29 arranged for positioning over the sleeve 24, with a first securement strap 31 positioned over the net first end 29 and the lock sleeve 24. The tubular net includes a tubular net second end 30 positioned over the second sleeve 25 utilizing a second securement strap 32 securing the net second end about the second sleeve 25. The first and second securement straps 31 and 32 are secured to respective first and second hook and loop fastener ends for ease of securement of the straps about the respective first and second sleeves 24 and 25. Alternative fastening of the straps may be employed such as snap fasteners, resilient straps, and the like. In this manner, once the net first and second ends 29 and 30 are mounted to respective first and second sleeves 24 and 25, the sleeves may be extended in a spacing away from one another or towards one another to provide for volumetric reshaping of the net structure dependent upon the type of shoes and the nature of other garments within the associated clothes dryer drum 12.
The FIGS. 7 and 8 indicate the use of a container housing 33 mounted to the mounting tube 13 within the tubular net 28. The container housing 33 includes a cap 34 removably mounted relative to the container housing 33 employing threaded engagement and the like. A matrix of cap apertures 35 are directed through the cap 34 to provide for the selective metering and dispensing of a deodorizing powder 36 from within the container housing 33 that is dispensed during the tumbling and rotation of the clothes dryer drum 12 to provide for enhanced freshness and deodorizing of the shoes within the clothes dryer drum.
It is understood that the shoes to be dried, such as indicated in FIG. 1, are initially positioned within the net structure prior to its securement relative to the associated sleeves 24 and 25, wherein in this manner, associated socks and the like that are to be separated relative to other clothes within the drum structure may be also positioned within the net during a drying procedure.
As to the manner of usage and operation of the instant invention, the same should be apparent from the above disclosure, and accordingly no further discussion relative to the manner of usage and operation of the instant invention shall be provided.
With respect to the above description then, it is to be realized that the optimum dimensional relationships for the parts of the invention, to include variations in size, materials, shape, form, function and manner of operation, assembly and use, are deemed readily apparent and obvious to one skilled in the art, and all equivalent relationships to those illustrated in the drawings and described in the specification are intended to be encompassed by the present invention.
Therefore, the foregoing is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention.
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A mesh tubular basket is arranged for mounting about a support tube and secured at each end of the mesh basket by strap members to position canvas type shoes and the like within a clothes dryer during a drying procedure. The support tube is arranged with a spring-biased sleeve, having a collar member to secure the sleeve if desired in a biased orientation against an interior wall of a drying machine drum.
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FIELD OF THE INVENTION
The present invention relates to electronic postage meters, and more particularly, to an electronic postage meter reset circuit for microprocessor-based electronic postage meter systems.
BACKGROUND OF THE INVENTION
Electronic postage meter systems have been developed, as for example, the systems disclosed in U.S. Pat. No. 3,978,457 for MICROCOMPUTERIZED ELECTRONIC POSTAGE METER SYSTEM, and in European Patent Application, Application No. 80400603.9, filed May 5, 1980 for ELECTRONIC POSTAGE METER HAVING IMPROVED SECURITY AND FAULT TOLERANCE FEATURES. Electronic postage meters have also been developed employing plural computing systems. Such a system is shown in U.S. Pat. No. 4,301,507 for ELECTRONIC POSTAGE METER HAVING PLURAL COMPUTING SYSTEMS.
The accounting circuits of electronic postage meters include non-volatile memory capability to store postage accounting information. This information may include the amount of postage remaining in the meter for subsequent printing or the total amount of postage printed by the meter. Other types of accounting or operating data may also be stored in the non-volatile memory. The non-volatile memory function in the electronic accounting circuits have replaced the function served in previous mechanical type postage meters by mechanical accounting registers. Postage meters with mechanical accounting registers are not subject to many problems encountered by electronic postage meters. Conditions cannot normally occur in mechanical type postage meters that prevent the accounting for a printing cycle or which result in the loss of data stored in the registers.
Conditions can occur in electronic postage meters where information stored in electronic accounting circuits can be permanently lost. Conditions such as a total power failure or fluctuation in voltage can cause the microprocessor associated with the meter to operate erratically and either cause a loss of data or the storage of spurious data in the non-volatile memory. The loss of data or the storage of spurious data may result in the loss of information representing the postage funds stored in the meter. Since data of this type changes with the printing of postage and is not stored elsewhere outside of the meter, there is no way to recover or reconstruct the lost information. In such a situation, a user may suffer a loss of postage funds.
To minimize the likelihood of a loss of information stored in the electronic accounting circuits, efforts have been expended to insure the high reliability of electronic postage meters. Some systems for protecting the critical information stored in meters are disclosed in the above-noted patents as well as in U.S. Pat. No. 4,285,050 for ELECTRONIC POSTAGE METER OPERATING VOLTAGE VARIATION SENSING SYSTEM and in U.S. patent application Ser. No. 306,979 filed Oct. 5, 1981, for MEMORY PROTECTION CIRCUIT FOR AN ELECTRONIC POSTAGE METER, and assigned to Pitney Bowes Inc. These systems provide protection against unpredictable circuit operation even if the microprocessor manfunctions at low voltage levels, as for example, where the microprocessor turns off below a predetermined voltage level and thereafter, within a lower voltage range, turns on again and becomes capable of outputting data.
SUMMARY OF THE INVENTION
The present invention provides a reset circuit which helps insure proper operation of an electronic postage meter. The reset circuit operates in conjunction with a non-volatile memory protection circuit. The combined operation of the reset circuit of the present invention and the non-volatile memory protection circuit controls the reset line of the electronic postage meter computing means and the write enable terminal of the non-volatile memory. The reset circuit and the non-volatile memory protection circuit operate to insure proper function of the electronic postage meter during power-up and power-down of the meter as when the meter power switch is turned on and off. The circuits further protect the electronic postage meter from improper operation where spurious data might be written into the non-volatile memory.
The present invention enables the reset circuit to operate in conjunction with voltages applied to the non-volatile memory to insure that the microprocessor reset is not released enabling the microprocessor to commence operation, until after the non-volatile memory voltage is at its proper level. The reset circuit operates in a manner which insures that the reset terminal is maintained active to hold the microprocessor in the reset state while the voltage levels build so that the microprocessor will be enabled to write data into the meter's non-volatile memory only after the memory is properly powered. The reset circuit of the present invention may also operate to simultaneously apply an active reset signal to the microprocessor when the necessary voltages to write into the non-volatile memory falls below a predetermined level.
When a power reduction occurs causing the electronic postage meter to go into a power down routine, the reset circuit will cause the reset to go active putting the microprocessor into a known state after the completion of the power down routine when the non-volatile memory write voltage falls below a predetermined level. During a power-up condition, the reset circuit of the present invention causes the reset terminal to be active until after the voltages have stabilized on the electronic postage meter non-volatile memory. The reset circuit of the present invention may be adapted to simultaneously control plural reset terminals of plural computing systems. For example, the reset terminal of both an accounting module microprocessor and another microprocessor in the system, such as the microprocessor associated with the printing module, may be simultaneously controlled by the reset circuit of the present invention.
In accordance with the present invention, a reset circuit is provided for an electronic postage meter of the type having printing means for printing postage, accounting means coupled to said printing means for accounting for postage printed by the printing means and non-volatile memory means coupled to the accounting means for storing data when the accounting means is not energized by a source of operating power. The reset circuit includes controlling means coupled to the non-volatile memory means and the accounting means. The controlling means controls the sequence of enabling the non-volatile memory means to operate and the enabling the accounting means to be conditioned to write data into the non-volatile memory. The controlling means is operable to enable the non-volatile memory to have data written into memory locations and thereafter enabling the accounting means to write data into the non-volatile memory.
DETAILED DESCRIPTION OF THE DRAWINGS
A complete understanding of the present invention may be obtained from the following detailed description thereof, when taken in conjunction with the accompanying drawings, in which:
FIG. 1 is an interconnection diagram of FIGS. 1a and 1b; and
FIGS. 1a and 1b, when taken together, are a schematic circuit diagram, partly in block form, of an electronic postage meter reset circuit embodying the present invention.
DETAILED DESCRIPTION
Reference is now being made to FIG. 1. A postage memter 12 includes an accounting module 14 having microprocessor and non-volatile memory such as a General Instrument Corporation ER3400 type electronically alterable read only memory. The General Instrument ER3400 is described in a General Instrument Corporation manual dated November 1977, entitled EAROM and designated by a number 12-11775-1; a printing module 16 having microprocessor and motor control circuits; and a control module 18 having a microprocessor and control circuits. The detail of construction and operation of the system may be in accordance with the postage meter system and the mechanical apparatus shown in the above-noted U.S. Pat. No. 4,301,507 for ELECTRONIC POSTAGE METER HAVING PLURAL COMPUTING SYSTEMS and in U.S. Pat. No. 4,287,825 for PRINTING CONTROL SYSTEM.
Postage meter 12 includes a series of opto-interrupters 20, 22, 24, 26 and 28. The opto-interrupters are used to sense the mechanical position of the parts of the meter. For example, the opto-interrupters can be employed to sense the position of the shutter bar which is used to inhibit operation of the meter under certain circumstances, the position of the digit wheels, the home position of the print drum, the position of the bank selector for the print wheels, the position of the interposer, or any other movable mechanical component within the meter. These opto-interrupters are coupled to the printing module 16 which monitors and controls the position of the mechanical components of the meter.
The printing module 16 is connected to the accounting module 14 via a serial data bus 30 and communicates by means of an ecoplex technique described in the above-noted U.S. Pat. No. 4,301,507 for ELECTRONIC POSTAGE METER HAVING PLURAL COMMPUTING SYSTEMS. Both ends of the bus are buffered by an optics buffer, not shown, which is energized by the power supply +5 volt line to be hereafter described. Similarly, the control module 18 is connected to the accounting module 14 via a serial data bus 32 and also communicates by means of the ecoplex technique. Optics buffers, not shown, are provided to buffer the bus. It should be recognized that the particular architecture of the postage meter system is not critical to the present invention. Plural or single microprocessor arrangements may be each be employed with the present invention.
A source of operating voltage, such as 110 volts 60 Hertz supply, is applied across meter input terminals 34. The voltage is applied to a linear +10.8 volt power supply 36. The output from the +10.8 volt linear power supply 36 is supplied to a first +8 volt linear regulated power supply 38 and to a second +5 volt linear regulated power supply 40. The +8 volt power supply is used to power a display 42 which is operatively coupled via a bus 44 to the control module 18. The output from the power supply 40 is directly coupled to the control module 18 and is operated to energize the control module microprocessor.
The AC operating voltage at terminals 34 is also applied to a silicon controlled rectifier type, 24 volt power supply 46. The regulated output from the power supply 46 is applied to the print wheel bank stepper motor 48 and the print wheel stepper motor 50 associated with the printing module 16. The 24 volt DC power supply is coupled by an AC choke 52 to capacitor 54. The internal capacitance within the 24 volt power supply 46 provides sufficient energy storage to continue to properly energizing a switching regulator 56 should an AC power failure occur at terminals 34. In such an event, the accounting module microprocessor 58 transfers information from the postage meter volatile memory (which may be internal or external to the microprocessor) via a data bus 60 to a NMOS non-volatile memory 62. The switching regulator 56, in conjunction with a transformer 68 with related circuitry, provides regulated output voltages used to energize the accounting module.
A +5 volts is developed and applied to the accounting module microprocessor 58, to NMOS non-volatile memory 62, to the optic buffers (not shown) for the serial data bus 30 connected between the accounting and the printing modules, to the printing module 16, and to the opto-interrupters 20-28. A -30 volts is also developed and is similarly applied via a NPN transistor 64 to the NMOS non-volatile 62. The -30 volts is required in conjunction with a -12 volts which is also developed and applied to the NMOS non-volatile memory 62 and the +5 volts to enable the non-volatile memory to have data written into the device.
The switching regulator 56 functions to selectively apply the 24 volts developed across a capacitor 54 to the junction of a diode 66 and poled transformer primary winding 68. The frequency at which the regulator 56 operates or switches is determined by a capacitor 70 which controls the operating frequency of the supply. Primary winding 68 is further coupled to ground by a capacitor 72. Diode 66 and capacitor 72 form a complete circuit in parallel with the primary winding 68. The circuit path is through a point of fixed referenced potential, here shown as ground.
During quiescent operation, a +5 volts is developed across capacitor 72. This voltage is sensed and coupled via a series connected variable resistor 74 and a fixed resistor 76 to an input terminal on the switching regulator 56. The feedback path controls the supply to maintain a constant voltage across capacitor 72. For the component value shown, a voltage variation of approximately 10 millivolts can occur across a capacitor 72. A step-up secondary winding 78 oppositely poled to the primary winding is electromagnetically coupled via a permalloy core 80 to the primary winding 68. The secondary winding 78 is connected to ground at one end and has its opposite end coupled via a diode 82 which operates in conjunction with a capacitor 84 and a current limiting resistor 86 to develop a -30 volts across a zener diode 88. A tap 90 on the secondary winding is connected to a diode 92 which operates in conjunction with a capacitor 94 and a current limiting resistor 96 to develop a -12 volts across a zener diode 98.
Because of the filtering provided by capacitor 72 and the inductance of the primary winding 68, the noise introduced by switching transients in the primary circuit is minimized. In a like manner, the capacitor is 84 and 94 and the inductance of the secondary winding 78, provide further filtering which also minimizes the noise introduced by swtitching transients. The operation of the power supply is described in greater detail in U.S. patent application Ser. No. 306,805 filed Sept. 29, 1981, for POWER SUPPLY SYSTEM and assigned to Pitney Bowes Inc.
A circuit is provided to insure that the NMOS non-volatile memory 62 is not energized by the -30 volts necessary for a writing operating after a predetermined voltage condition in the power down sequence has been reached. This circuit operates in conjunction with a second circuit adapted to insure a proper reset is applied in a predetermined relationship to the application and the removal of the -30 volts from the non-volatile memory. The system insures that even if data is put onto the data bus 60 by the microprocessor 58, no data will be written into the NMOS non-volatile memory 62. This is particularly important because it has been noted in the aforementioned U.S. patent application Ser. No. 306,979 for MEMORY PROTECTION CIRCUIT FOR AN ELECTRONIC POSTAGE METER that although the microprocessor may be designed to turn off and not output data at a determined voltage level, it has been discovered that such microprocessors may become active again even at lower voltages notwithstanding the signal applied to the microprocessor reset terminal.
The -30 volts supply to non-volatile 62 is passed through the collector-emitter current path of the NPN transistor 64. The collector electrode of the transistor is coupled via the resistor 100 to the +5 volts developed at capacitor 72. The voltage developed at the collector electrode of transistor 100 controls the voltage applied to the based electrode of a transistor 102 whose collector electrode is connected to the reset terminal 104 of the microprocessor 58 of the accounting module 14 and to the reset terminal 106 of the microprocessor for the printing module 16. Base bias for the transistor 64 is obtained from a PNP transistor 108. The emitter electrode of the transistor 108 is connected by a 10 volt zener diode 110 to the 24 volt power supply 46. A resistor 112 provides a ground return for the base electrode of transistor 108. Resistors 114 and 116 are connected to the base electrode of transistor 64. A capacitor 118 is provided to further filter transients.
The base electrode of transistor 102 is coupled to the collector electrode of transistor 64 by a resistor 120 and to the +5 volts developed at capacitor 72 by a resistor 122. A capacitor 124 is connected across the collector-emitter electrode current path of transistor 102. The collector electrode is further connected by a resistor 126 to the +5 volts developed at capacitor 72. It should be noted that although the transistor 102 is shown connected to the reset terminals 106 and 104 of the microprocessors, respectively, associated with the printing module 16 and the accounting module 14, the arrangement is only by way of example. The reset system can be employed with either single microprocessor or plural microprocessor electronic postage meter systems.
When the AC line voltage at terminals 34 fails, and the 24 volts power supply 46 output voltage begins to drop and fall below a predetermined level, such as 19 volts, a low voltage detector 128 with about 2 volts of hysterisis senses the falling voltage and initiates an interrupt signal to an interrupt or restart terminal 130 on the accounting module microprocessor 58. The routine may be initiated by a system such as that disclosed in the aforementioned U.S. Pat. No. 4,285,050 for ELECTRONIC POSTAGE METER OPERATING VOLTAGE VARIATION SENSING SYSTEM. The interrupt routine completes all pending accounting functions and transfers all register readings from the internal microprocessor RAM to the external non-volatile memory 62. It then goes into a wait loop which is terminated by a microprocessor reset or the return of normal voltage, indicated by a voltage greater than 21 volts at low voltage sensor 128. When the AC line voltage line drops to a level such that the 10 volts zener diode 110 is no longer operating in a breakdown mode, current flow through the collector-emitter of transistor 108 ceases. As a result, transistor 64 is biased out of conduction. This causes the +5 volts which is applied via resistor 100 to the collector electrode of transistor 64 to be applied to the NMOS non-volatile memory -30 volt terminal 132. It should be noted that the -30 volts is required in conjunction with a -12 volts (which is also developed and applied to the NMOS non-volatile memory 62 -12 volts terminal 134) to have data written into the memory. Thus, rather than a negative voltage being applied to the microprocessor NMOS non-volatile memory -30 volt terminal 132, a positive voltage is applied and information cannot be written into the memory.
Simultaneous with the application of the +5 volts to the NMOS non-volatile memory -30 volt terminal 132, the +5 volts is likewise applied via resistors 100, 120 and 122 to the base electrode of transistor 102. This biases transistor 102 into conduction causing capacitor 124 to quickly discharge through the collector-emitter electrode current path of transistor 102 thereby applying a reset signal to the reset terminals 104 and 106 of the accounting module microprocessor 58 and the printing module microprocessor by coupling these terminals to ground. The activation of the reset terminal places the microprocessor in a known condition. Nevertheless, the +5 volts applied to the NMOS non-volatile memory terminal 132 insures that no information can be written into the non-volatile memory 62 during the remainder of the power down cycle. This is because, as peviously noted, a -30 volts must be applied to terminal 132 to enable a WRITE operation in the NMOS non-volatile memory 62. The microprocessors reset terminal will have a reset signal applied (a ground level potential) as power decays until the voltage at the base electrodes of transistor 102 falls below the level necessary to forward bias the base-emitter junction, usually approximately 7/10ths of a volt for many devices.
For the various supplies and component value shown, by the time the output voltage of the +24 supply 46 decays to approximately +7.5 volts, the +5 volts developed at capacitor 72 will begin to drop. By this time however, the 10 volt zener diode 110 will have been turned off for a voltage change of approximately 21/2 volts and terminal 132 will have had a positive voltage applied to it. Thus, when the output voltage from the +24 volts supply drops to approximately +10 volts, a positive potential is applied to the NMOS non-volatile memory -30 volts write enable terminal 132, and no data can be written by microprocessor 58 into the non-volatile memory 62. This situation continues until the voltage falls below the range of uncertain operating voltage levels wherein the microprocessor 58 may operate despite a reset signal being applied to the reset terminal 106. Protection against writing into the NMOS non-volatile memory 62 is afforded by control over the conductivity of the collector-emitter electrode current path of transistor 64.
During a power-up routine as the voltages begin to build, the voltage from the +24 volts power supply 46 begins to charge up its capacitors including capacitor 54 as it builds toward the 24 volt output. When the voltage builds to a sufficient level, zener diode 110 will breakdown and begin to conduct. This establishes a current flow through the collector-emitter electrode current path or transistor 108 which in turn biases transistor 64 into conduction. As a result, the -30 volts is coupled via resistor 120 to the base electrode of transistor 122 biasing the transistor out of conduction. Up to this point in time, howver, transistor 102 is biased into conduction as the voltage builds by the +5 volts applied to its base electrodes via resistors 100, 120 and 122. This prevents a charge from building up on capacitor 124 thereby causing a solid reset signal to be applied to the reset terminals 104 and 106. When the -30 volts is applied to the NMOS non-volatile memory terminal 132, transistor 102 is biased out of conduction. This allows capacitor 124 to begin charging from the +5 volts supply through resistor 126. When the capacitor is charged to a suitable level, the reset signal is removed from the reset terminals 104 and 106 of the microprocessors, and the microprocessors begin executing instructions. It should be noted that the time delay due to charging the capacitor 124 and controlling the bias of transistor 102 from the -30 volts supply insures that the -30 volts potential is applied and has stablized on the NMOS non-volatile memory -30 volt terminal 132 prior to the microprocessor reset terminals being released to enable the microprocessor to commence operation. Moreover, when the power begins to fall, the reset terminals 104 and 106 of the microprocessors are rendered active putting the microprocessors in the reset condition simultaneous with the removal of the -30 volts supply from the NMOS non-volatile memory terminal 132.
The sequence of operation of the electronic postage meter reset circuit shown in FIGS. 1a and 1b is set forth in the following table of Sequence of Operations.
__________________________________________________________________________Sequence of Operations Micropro- Low Voltage Non-VolatileState 24 V Supply +5 V Supply cessor Reset Sense Memory (NVM)__________________________________________________________________________Power-Up1 0-7.5 <5 Indeterminate Low Disabled2 7.5-10 V +5 Reset Low Disabled3 10-21 V +5 Wait* Low Enabled Loop4 21-24 V +5 Read NVM Normal Enabled Then OperatePower-Down4 24-19 V +5 Operate Normal Enabled5 19-10 V +5 Write NVM Low Enabled Then Wait** Loop2 10-7.5 +5 Reset Low Disabled1 7.5-0 <5 Indeterminate Low Disabled__________________________________________________________________________ *Can go to either state 2, 4 or 5 if line voltage fluctuates widely. **Can go to either state 2 or 3 if line voltage fluctuates widely.
It is known and understood for the purpose of the present application that the term postage meter refers to the general class of device for the imprinting of a defined unit value for governmental or private carrier delivery of parcels, envelopes or other like application for unit value printing. Thus, although the term postage meter is utilized, it is both known and employed in the trade as a general term for devices utilized in conjunction with services other than those exclusive employed by governmental postage and tax services. For example, private, parcel and freight services purchase and employ such meters as a means to provide unit value printing and accounting for individual parcels.
Having described the invention in conjunction with the specific embodiment thereof, it is to be understood that further modification may suggest itself to those skilled in the art. The scope of the present invention is not to be limited to the embodiment disclosed but to be interpreted as set forth in the appended claim.
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A reset circuit for an electronic postage meter controls the operation of the reset line of the meter's computing system. The reset circuit operates in conjunction with a non-volatile memory protection circuit. The inter-relation of the reset circuit and non-volatile memory protection circuit protects against the possible loss of postage funds due to spurious data being written into the non-volatile memory. The reset circuit operation is controlled in part by the voltage levels applied to the non-volatile memory. This insures that the reset to the electronic postage meter computing system is released during power-up of the meter after proper voltage levels have applied to the user's non-volatile memory and reestablished during low power or power-down conditions.
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GOVERNMENT INTEREST
[0001] This invention may be made, used, and licensed by or for the United States Government without payment to me of any royalty.
BACKGROUND OF THE INVENTION
[0002] Military vehicles frequently travel cross-country as part of exercises and/or actual battle conditions. When so engaged they frequently encounter obstacles which must be surmounted. One example of a problem frequently encountered by military forces is the hedgerows located across countrysides in many places in the world. Such hedgerows are the result of local farmers removing stones from fields and placing the stones at the edge of their fields, this removes the stones from interfering with normal farming operations. In addition frequently brush, brambles or other low growing shrubs are added or row naturally to create a barrier for cattle and other livestock on the farm. Such hedgerows frequently will remain undisturbed for many years and become dense and impenetrable not only to persons and cattle but also to vehicles. Further, in the case of military vehicles, as they traverse over a hedgerow the underside of the vehicle, that is most vulnerable, will be momentarily exposed to an enemy. This allows an enemy combatant an open shot at the underside and therefore the most vulnerable part of the vehicle endangering the vehicle occupants and compromising the mission.
[0003] In World War II the allies discovered that in traversing the countryside the hedgerows they encountered constituted a substantial obstacle even to tanks and many vehicles were disabled by the enemy when they attempted to climb over the hedgerows. As a solution to this problem, a device known as “Culin hedgerow cutter” was developed by a soldier and proved successful at removing hedgerows as a vehicular obstacle.
[0004] However, the device, which was developed while allowing breaching of the hedges, left a tangled mass of debris. Because the device merely cut the brush and pushed aside whenever stones were present the resulting pile of debris made it difficult for soldiers on foot to follow behind a vehicle pushing the cutter. One of the purposes of military vehicles, particularly large armored vehicles is to provide a cleared pathway and shelter for soldiers moving on foot around the vehicle. Thus the prior art cutter and similar devices do not provide a suitable pathway for infantry soldiers who were following the vehicle.
[0005] One example of a commercial brush clearing apparatus is found in U.S. Pat. No. 4,180,108. This invention relates to a blade designed to be pushed ahead of a tractor to clear brush and trees. The device has a planar cutting assembly in the form of a triangular blade structure wherein opposite surfaces of the blade present a cutting edge with the third side of the blade being mounted on the front of a tractor. The device is disposed essentially horizontal to the ground with the cutting edges outboard. The cutting edges have a plurality of teeth and the blade further has a beveled portion adjacent the leading edge of each tooth to provide a self-clearing function.
[0006] Both the prior art devices described above result in a path which is cleared of standing brush and the like but which will still in an uneven and tangled mass for traverse by individuals on foot.
[0007] The hedgerow clearing device of the present invention not only cuts any brush which forms a part of hedgerow or similar obstacle but it will also move rocks ad other solid debris that may be present. Because of the invention's structure, it also levels the debris formed to a state that can be more easily traversed by foot soldiers. This will result in less stress on the troops and a faster traverse of a particular obstacle decreasing the soldier's exposure time to enemy fire and increasing their chance of survival.
SUMMARY OF THE INVENTION
[0008] The present invention is a hedge-breaching device designed to be mounted on a military vehicle, either combat or tactical. The device has at least two and possibly more, brackets which are be attached to corresponding mounting points or bosses on a particular vehicle. From each of the brackets an arm extends outward from the front of the vehicle with a first section of the arm being disposed at the level of the bosses and extending approximately parallel to the ground over which the vehicle is traveling. At the end of the first section distal the vehicle, a second section of the arm is attached to the first section at an oblique angle. The second section will depend downward towards the ambient terrain. A third section of the arm will extend outward from the second section parallel to the ground but at a position relatively closer to the ground than the first arm. The level of the third section above the terrain can be thought of as the working height.
[0009] A dentate cutting bar is attached to the free ends of the arm's third section. To provide a cutting means which can be pushed into and through a hedgerow. A leveling roller is attached to and depends from the first section of the arms and between the vehicle and the dentate cutting bar. After the brush has been cleared the roller will flatten the brush resulting in a pathway of a more uniform texture and height providing a pathway more amenable to persons on foot.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] Referring to the accompanying drawing:
[0011] FIG. 1 s a perspective view of one embodiment of this invention;
[0012] FIG. 2 is a perspective view of a tactical vehicle bumper suitable for use with this invention; and
[0013] The Prior Art Figure is perspective view of the World War II device.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0014] Referring to the accompanying drawing wherein like numerals referred to like parts, the prior art figure shows a device having a pair of mounting brackets located at the rear of the device which can be attached to corresponding bosses extending outward from the front of a vehicle. The particular device shown is constructed so as to be readily attached to the front of a Sherman tank that had such attachment means mounted on the front of the vehicle. The device as shown is a relatively flat plate with a plurality of teeth extending parallel to the direction of vehicle travel and arms which extend outward from each side and the middle of the device to provide structure and strengthen the teeth along which they are positioned. Such a device when mounted on the front of a Sherman tank was fully capable of pushing through the type of hedgerow found in the European countryside and provided a quick and easy means to breach this type of obstacle. However, the device was not designed to level or otherwise dress the debris created by the device and the result was a path that was difficult for the infantry to follow.
[0015] Turning to FIG. 1 , the front portion of a tracked combat vehicle 10 is shown with a pair of mounting bosses, 12 containing threaded apertures 14 , mounted on the front portion of the vehicle. Since both combat and tactical vehicles used by the military require substantial ground clearance to avoid becoming mired or damaged when moving cross-country, the bosses 12 will be mounted at a substantial distance above the terrain (not shown) the vehicle 10 is traversing. As shown, a pair of brackets 16 having corresponding apertures 18 suitable for receiving threaded fasteners 20 is provided for attaching a hedgerow breacher generally 22 to the mounting bosses 12 on vehicle 10 . Extending outward from the brackets is a pair of arms 24 . As shown, each arm 24 has a first section 26 attached to the bracket 16 such as by welding the first section to the bracket. The first section 26 extends perpendicular to the face of the bracket 16 and substantially parallel to the terrain over which the vehicle is moving. The first section 26 has a second end distal the end attached to the brackets, the distal end being attached to a second section 28 of the arm 24 , which extends at an oblique angle to the first section 26 so that the second section 28 depends downwardly towards the ambient terrain. At the end of the second section 28 opposite the first section 26 , a third section 30 is mounted at an oblique angle to the second section 28 similar to the angle between the first and second sections so the third section 30 extends outwardly parallel to the terrain.
[0016] At the end of the third section 30 , a dentate cutting bar 32 having a plurality of teeth 34 is attached rigidly across the arms 24 . The result is a cutting device disposed at a distance from the vehicle, which will remove brush, small trees, and rocks.
[0017] As shown in the drawing, the hedge-breaching device of this invention can be constructed with additional structural members designed to increase rigidity and provide stability. The device as shown has two reinforcement bars 36 or members that are disposed perpendicular to and between the first and second sections of the arms 24 . Also shown are two additional reinforcement structures 38 or members shaped similarly to the arms 24 . The reinforcement arms 38 are disposed between the bracket arms 24 , to provide additional rigidity and are attached to the other rigidifying members 36 . The result is a large open mesh arrangement. This type of structure with its openness allows brush and shrubs that are cut, and rocks that are dislodged to flow over the cutting bar and through the openings between the various members. The second sections 28 of the bracket arms 24 and reinforcement arms 38 form a ramp structure that will resist the upward motion of debris as it leaves the relatively flat surface of the third sections and cutting bar. This serves to keep the load on the third sections from building up and the resulting debris will be forced though the openings between the arms in furrows. Thus, rather than merely pushing or crushing the debris it will be moved and channeled to a semblance of uniformly. The resulting sized and furrowed debris will be more amenable to treatment by the leveling mechanism, described hereinafter.
[0018] The hedge-clearing device as shown has a pair of bosses 40 mounted on and extending downward towards the terrain from the first or upper section 26 of the arms 24 . As shown, two link chains 42 extend or hang downward from the bosses 40 to a point close to the ground. On the ends of the chain 42 opposite the bosses 40 , a heavy roller 44 is rotatably mounted on the ends of the chains closest to the ground. The roller 44 will contact debris which has passes through the mesh structure of the cutting bar and will level the resulting furrowed material into a path more amenable to traverse by individuals on foot. This will be particularly good for soldiers who are generally carrying substantial additional weight in the form of equipment and supplies.
[0019] FIG. 2 shows a bumper 12 which can be attached or would be attached to a tactical vehicle such as a truck with bosses similar to those shown on the combat vehicle of FIG. 1 . The device of this invention mounts to such a truck in the same manner as it would be mounted on a combat vehicle.
[0020] Various alterations and modifications will become apparent to those skilled in the art without departing from the scope and spear this invention and is understood that this invention is limited only by the appended claims.
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A hedge-breaching device for military vehicles has shaped arms holding a dentate cutting blade. The hedge breacher has an open mesh structure which will cause the debris to be deposited in furrows as the breacher moves forward and further has a leveling device that will dress the debris so as to provide a somewhat leveler terrain over which a person on foot can move easily.
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CROSS REFERENCE
This application is a continuation-in-part of my earlier filed U.S. application for Expansion Fit Interior Storm Window Assembly bearing Ser. No. 841,939 and filed on Mar. 20, 1986, which in turn is a continuation of my copending application Ser. No. 634,463, filed July 25, 1984, and entitled Expansion Fit Interior Storm Window Assembly, now abandoned.
BACKGROUND OF THE INVENTION
The present invention relates to a unitary storm window assembly which is readily installed in an existing window opening. More specifically, the present invention relates to a unitary storm window held in place through a bias frictional fit and which is installed and removed in its entirety, that is, as an integral unit.
Heretofore, numerous so called "quick attachable" windows have existed which can be installed to an existing window opening containing an existing window and pane therein and are represented by the following patents.
U.S. Pat. No. 961,726 to Mayr relates to a double sliding sash window wherein an upper and a lower inner sash is slidable upon an outer upper and lower sash.
U.S. Pat. No. 1,123,088 to Bryant relates to providing an improved form of friction shoe for holding a screen or sash in a raised or lowered position.
U.S. Pat. No. 1,525,002 to Sembower relates to a pivoted and sliding window in which spring metal weather strips are interposed between the sliding stiles and the sides of a frame.
U.S. Pat. No. 1,740,960 to Roberge relates to detachable windows and screens as well as detachable guides for holding the same in place.
U.S. Pat. No. 1,858,109 to Pauli relates to an automobile window which partially closes a regular window opening whereby an operator's arm can be extended from an automobile to give manual signals.
U.S. Pat. No. 2,402,112 to Gee relates to a combined storm and screen window installation having an interchangeable sash which can be removed and is held in place by side channel irons.
U.S. Pat. No. 2,504,510 to Ernest relates to a device adapted to prevent the rattling of slidable windows as in an automobile.
U.S. Pat. No. 2,846,734 to Zitomer relates to an interior storm window which is applied to an existing window opening through guide members which are screwed to the frame of the existing window.
U.S. Pat. No. 3,095,617 to Bruno relates to an anti-bellying means for securing storm sashes to their adjacent frames.
U.S. Pat. No. 4,364,198 to Netti relates to a storm window unit having a bottom latch which window is added to an existing track.
Canadian Pat. No. 872,571 relates to a replaceable sash which is removably mounted in a window frame and which is secured to an existing opening.
German Pat. No. 26 21 254 relates to a replaceable window which is inserted in an existing opening.
While often relating to windows such as replaceable windows, none of the above documents relate to a unitary interior storm window assembly having side channels which interlock with a window perimeter frame and which assembly is frictionally fit in a sidewall jamb but is readily removable therefrom.
SUMMARY OF THE INVENTION
It is therefore an aspect of the present invention to provide a unitary interior window assembly.
It is a further aspect of the present invention to provide a unitary interior window assembly, as above, wherein said unitary window assembly is readily removable or insertable in its entirety.
It is a still further aspect of the present invention to provide a unitary window assembly, as above, wherein said unitary window assembly frictionally engages an existing window opening and hence requires no external fasteners, window tracks, window guides, and the like.
It is yet further aspect of the present invention to provide a unitary interior window assembly, as above, wherein side channels interlockingly engage a window perimeter frame.
It is yet an additional aspect of the present invention to provide a unitary interior window assembly, as above, wherein leaf springs urge at least one said side channel outward to create said frictional fit with the sidewall of an existing window opening.
These and other aspects of the present invention will become apparent from the following detailed description.
In general, a unitary interior storm window assembly comprising; a window pane, a perimeter frame, said window pane residing in said perimeter frame, at least one side channel, said side channel having interlocking tabs thereon, said side channel interlockingly connected to said perimeter frame so that a unitary window assembly is formed.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be more fully understood from the following detailed description thereof when considered in connection with the accompanying drawing wherein the invention is illustrated by way of example and in which:
FIG. 1 is a front elevation view, broken away in part, of a storm window assembly according to the present invention.
FIG. 2 is a side section view taken substantially through a plane indicated by section line 2--2 in FIG. 1 of the invention.
FIG. 3 is a partial perspective view of the end portion of the side channel of the invention.
FIG. 4 is a front elevation view of another embodiment of a unitary storm window according to the present invention.
FIG. 5 is a side section view taken substantially through line 5--5 of FIG. 4.
FIG. 6 is a side section view taken substantially through line 6--6 of FIG. 4.
FIG. 7 is a top elevation view taken on line 7--7 of FIG. 4.
FIG. 8 is an enlarged fragmentated view of the lower right portion of FIG. 4 showing the latch mechanism.
DETAILED DESCRIPTION
Referring to the drawings, and more particularly to FIG. 1, there is shown an expansion fit interior storm window assembly generally referred to by reference numeral 10 according to the present invention. A window pane 11 made of glass or other suitable clear material is encased in a rigid perimeter frame 12. Suitable insulation 13 such as felt insulation is fastened to perimeter frame 12 by adhesive along the bottom edge 14 to seal against air leaking between frame 12 and existing window sill 22.
A "U" shaped top channel 15 extends the complete width and is permanently attached to the building existing window frame top 20 by screws 19 through channel bottom 18. Top channel 15 has insulation 16 provided on the inside of one leg 17 as shown in FIG. 2 to seal against air passing around perimeter frame 12 when inserted therein.
Side channels 25 are also U-shaped and tightly enclose perimeter frame 12 within legs 26. A leaf spring 30 is clamped to the interior of side channel 25 on bottom 27 as shown in a broken away perspective view in FIG. 3. Additional leaf springs may similarly be attached to the middle portion of side channels 25 by cutting a slot in bottom 27. Insulation 29 such as felt is applied to the outside of side channel bottom 27 by a suitable adhesive. A tab 28 is formed in side channels 25 to aid in gripping them when installing and removing the assembly and pressing against the bias of leaf springs 30. The side channels 25 will thus expand against existing window frame sides 21 in tight frictional engagement due to the outward bias of leaf springs 30. Tabs 28 are indented at 31 to permit inserting side channels 25 in top channel 15.
The assembly 10 is safely held within the existing building window frame and is prevented from falling out by top channel 15 and frictional engagement by side channels 25 with existing window frame sides 21. To further prevent the assembly from popping out under severe wind conditions, a latch 33 is attached to perimeter frame bottom 35 and tongue 36 is provided to engage a hole 34 formed in window sill 22.
Perimeter frame 12, top channel 15 and side channels 25 are preferably made of aluminum but obviously can be made of other suitable materials such as extruded polyvinyl chloride. Leaf springs 30 are made of metal but likewise can be made of suitable plastic material having spring characteristics.
In installing the assembly 10, side channels 25 are inserted on perimeter frame 12 and pressed together by gripping tabs 28 and pressing inward against the bias of springs 30. The assembly is then inserted into top channel 15 and the existing window frame. Side channels 25 are released and they are expanded to frictionally engage window frame sides 21. Side channels 25 and perimeter frame 12 are then pulled downward to tightly engage window sill 22. Existing building window frames are frequently not constructed square but are often irregular in inside dimensions. However, it can be seen that the assembly of the present invention can conform to an irregular shape by perimeter frame 12 being slidably adjustable and interfitting within the top channel 15 and side channels 25. Thus, the storm window can be adjusted or tilted within top channel 15 and side channels 25 to conform to the existing window frame and still remain sealed and insulated against air leaks around the edges. In removing the assembly, simply grip tabs 28, push side channels 25 inward together and withdraw downward and out from top channel 15. This easy and simple procedure of installing and removing the assembly 10 of this invention can be accomplished within minimum effort and skill by most any person.
The invention has been described in great detail sufficient to enable one of ordinary skill in the art of interior storm windows to make and use the same. Obviously, modifications and alterations of the preferred embodiment will occur to others upon a reading and understanding of the specification. It is my intention to include all such modifications and alterations as part of my invention insofar as they come within the scope of the appended claims.
According to another aspect of the present invention, a unitary window assembly is generally indicated by the numeral 100. As will be explained hereinbelow in greater detail, unitary window assembly 100 resides within the interior portion of a building or a home and engages the sidewall or jamb of an existing window opening generally indicated by the number 105. Although the present aspect will be discussed with regard to a storm window, it is to be understood that in lieu of a window pane, a screen, or the like, can also be utilized.
Referring to FIG. 1, window pane (or screen) 111 is surrounded by a perimeter frame 115. The perimeter frame comprises side frame portions 116, top frame portion 117 and bottom frame portion 118. The various perimeter frame portions can be mitered in any conventional manner and held together by a suitable fastener such as a screw. The perimeter frame can be of any conventional material known to the art and to the literature such as extruded aluminum, polyvinyl chloride, and the like. Desirably, the perimeter frame contains sealing material 121 so that a waterproof seal is generally made between the frame and the glass pane. Typically, a compression fit is also formed. Seal material 121 can be any conventional material known to the art as well as to the literature and hence can be rubber, plastic, and the like with a specific example being marine glazing. The sealant material is generally resilient and thus due to the pressure exerted upon it by the perimeter frame forms a compression fit as well as resiliently grasps the window pane.
An important aspect of the present embodiment is that an interlocking member 124 exists at or near the end of the perimeter frame. As best seen in FIG. 7, frame interlocking member 124 contains flange 125 thereon. A flange is generally located on each end of the "U" shaped outer periphery of the perimeter frame. Flange 125 extends outward from the plane of the perimeter flange and has an angular projection 127. The projection extends at an angle towards the frame periphery. That is, an acute angle is generally formed between angular projection surface 127 and the frame side. Interlocking member 124 generally exists on at least one side frame portion 116 and desirably on both frame side portions. A similar interlocking connection can also exist on top perimeter frame portion 117.
The unitary window assembly of the present invention is removably and frictionably attached to an existing window opening. That is, it can be readily applied and maintained in position and yet readily and quickly detached from any existing conventional building or home window. The positioning and location of the unitary window assembly 100 of the present invention is within the generally flat, unobstructed jamb portion thereof. By unobstructed it is meant that the place of engagement or residence of the unitary window assembly is free from, that is, outside of any window tracks, guides, and the like and thus resides upon the side jamb area of the opening which is typically flat.
To prevent the window from topping over, a top channel 130 is fastened to the upper portion of the existing window opening as a safety precaution. The top channel can be "U" shaped to permit quick insertion as well as removal of the unitary window assembly. Top channel 130 has a forward extending front edge lip 132 as best seen in FIG. 5. Naturally, the depth of the top channel is sufficient so that when the window is fully seated and rests upon its base, top perimeter frame 117 is securely engaged by top channel 130.
Side channels 140 can generally be of any shape so long as they are slidably and interlockingly connected to the angular projections of side perimeter frame portions 116. As shown in FIG. 7, they can be "U" shaped and have a pair of sidewalls 142. The innermost portion of side channels 140, with respect to the window pane, have inner locking tabs 144 thereon desirably located on each sidewall 142. The interlocking tabs have flanges 145 extending therefrom including an angular projection 147. Angular projections 147 matingly and slidably engage side perimeter frame interlocking member 124. Desirably, an acute angle is formed between the angular projection surface 147 and the sidewall. The interlocking engagement between side channels 140 and the perimeter side frame portion 116 forms a unitary window assembly in that the entire window is held together. That is, even when taken out from an existing open window aperture, the window assembly 100 has no loose parts but will stay together in a fixed relationship as if the entire assembly were integral. In order to assist gripping the window assembly as well as the initial installation of side channels 140 to side perimeter frame portion 116, hand grip tabs 148 project from the side channels.
Since the window assembly of the present invention desirably acts as a storm window, the perimeter thereof desirably has weather stripping or insulation attached thereto. Any conventional weather stripping known to the art and to the literature can be utilized. Accordingly, weather stripping such as wool pile exists in end recess 149 of side channels 140. The weather stripping can be attached thereto in any conventional manner such as through the use of an adhesive. Desirably the weather stripping is a type which does not lose its resiliency under compression for extended periods of time.
It is an important feature of the present invention that at least one of the side channels and preferably both of the side channels are bias against the sidewall jamb of the existing window opening. That is, a bias engagement between unitary window assembly side channels 140 and the existing window opening jamb is desired in order that a frictional fit exists. The bias engagement can be created by the existence of leaf springs 150. One end of leaf spring 150 is generally fixedly attached to a portion of side perimeter recess 129 and the remaining end 155 is desirably moveably attached. Leaf springs 150 are often bowed to create a spring-like effect. Attachment of fixed end 151 can be according to any conventional manner. For example, fixed end 151 of the leaf spring can have a wide neck portion which is wider than the recess opening, and thus fixed end 151 can be inserted into recess 129 and turned such that wide neck cuts into the lips of the recess. Remaining spring end 155 can have a narrow neck such that this end is moveable or slidable within recess 129. Generally, any number of springs 150 can exist such that the entire side channels form a bias engagement with the window opening sidewall or jamb. The bias force of the spring is generally sufficient such that a snug and secure engagement occurs between side channels 140 and the existing window opening sidewalls. The net result is a frictional engagement or fit. That is, the sole source of engagement between unitary window assembly 100 and the sidewalls of the existing window opening is through a pressure or bias engagement. Window tracks, guides, mechanical engagements such as fasteners and the like are not required and not desired. In effect, an obstruction free engagement, that is a frictional fit is achieved.
The installation of the unitary window assembly of the present invention is as follows: Hand tabs 148 on each of the side channels are grasped and the window assembly is carried to an appropriate existing window opening for installation. Unitary window top perimeter frame portion 117 is then pushed upwardly into top channel 130. With the side channels 140 of the unitary window construction forced inward, window assembly 100 is slid into place into the obstruction free, generally flat jambs of an existing window opening 105. Upon release of grip tabs 148, leaf springs 150 will bias side channels 140 into engagement with the jambs of the existing window opening. Since a plurality of springs or bias means exist, should the window opening be irregular, for example wider on top than on the bottom, the springs will accordingly urge the upper portion of the side channels outward to a wider extent. A snug and secure frictional engagement is thus made. Through the use of weather stripping, an essentially air tight engagement is made. The storm window through bottom perimeter frame 118 will reside upon an appropriate surface such as a sill of the existing window opening. The storm window can remain in place throughout a winter season. When it is desired that the detachably unitary window assembly be removed, hand grip tabs 148 are grasped and forced inward. The bottom portion of the window assembly 100 is then pulled outward and downward. No removal of fasteners or the like is required. Since window assembly 100 is unitary, the entire window is removed and no parts of the window assembly such as guideways, tracks, cover flanges, sealing flanges, or the like remain with the sole exception of top channel 130. Upon removal of the unitary frictionally fit unitary window assembly from the obstruction free sidewall jamb, no permanent deformation is created nor must any guides, trackways, or other accessories be removed.
Should a mechanical engagement between the unitary window assembly with the existing window opening sidewall be desired, window assembly 100 can have side latches 160 thereon or bottom latches (not shown), or both. As best seen in FIG. 8, these latches can be any conventional latch such as a spring loaded latch having a projection 162 extending through aperture 163 of the side channels. A corresponding recess can exist in the existing window opening jamb so as to matingly receive bottom latch projection 162. In order to create a weather tight seal, recess 165 can exist on the bottom portion of the latch assembly. The weather stripping can be of any suitable material such as discussed hereinabove.
While in accordance with the Patent Statutes, a best mode and preferred embodiment have been set forth in detail, the scope of the invention is not limited thereby, but rather by the scope of the attached claims.
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A unitary removable storm window assembly contains a window pane, a perimeter frame, and at least one side channel. The storm window assembly is unitary in that the side channel is interlockable with the perimeter frame so that the various components are fixed in relationship to one another even when the window is not in use, that is not installed. The storm window assembly contains at least one spring for urging the side channel away from the window perimeter. Thus, when placed within the jambs of an existing building or home window opening, the unitary window assembly is frictionally retained therein by the channels. The engagement is thus free from securing guides, tracks, and the like, and the entire window assembly is readily removable as a unitary structure within a matter of seconds.
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FIELD OF THE INVENTION
[0001] This invention relates to headliners for use in the interiors of motorized vehicles such as automobiles and trucks. More particularly, it relates to headliners that include shaped projections that extend from a flat surface and are able to absorb and disperse the energy from a collision. The headliners according to the invention are readily adaptable to fit all types of vehicle contours and are useful on roof portions and support beams, and other areas where a passenger's body part may contact a part of the vehicle during the course of a collision.
BACKGROUND OF THE INVENTION
[0002] Headliners for motor vehicles are mounted inside the passenger compartment and against the sheet metal roof of the vehicle to provide an aesthetic covering for the sheet metal. Historically, headliners have been constructed of a single layer. However, more recently, headliners comprising multiple layers laminated together have been proposed in response to increased requirements of safety measures for vehicle passengers in the event of an impact. Federal regulations have become increasingly stringent, especially regarding energy absorption of passenger head impact. For example, the Laboratory Test Procedure for FMVSS 201 requires that future passenger cars and other light vehicles achieve a head impact energy absorption performance requirements HIC(d) which shall not exceed a value of 1000, when calculated in accordance with the following formula: HIC(d)=0.75446 (Free Motion Headform HIC)+164 HIC, wherein HIC is calculated by the following formula:
HIC = [ 1 t 2 - t 1 ∫ t 1 t 2 a t ] 2.5 ( t 2 - t 1 )
[0003] in which t 1 and t 2 are any two points in time during the impact event separated by no more than a 36 millisecond time period, and a is the resultant acceleration at the head center of gravity (c.g.).
[0004] These new standards require that the structure above the vehicle beltline (bottom of vehicle glass) subject to occupant head impact be modified to meet these standards. Many materials have been evaluated for impact energy absorption, but have been found to be too bulky and/or expensive for use in the confines of a modern vehicle interior where maximizing available open space is desirable. An additional criterion is the retention of a high level of sound absorption to provide a quiet environment inside a motor vehicle.
[0005] A wide variety of materials have been employed in vehicles for minimizing head injuries in the event of an accident. Previously, a variety of open and closed cell foam materials have been employed for areas such as the instrument panel. In order to provide head impact absorption in contemporary vehicles, padded visors have been employed as shown in U.S. Pat. No. 4,958,878 for protecting the occupants in the front windshield area. In more recent years, headliners for vehicles have been integrally molded and have a thicknesses which vary depending upon the area of the headliner, where the thickness of headliners is thicker in areas where absorption and diffusion of impact energy may be important. With such increased thickness, however, the cost of manufacturing the headliner through a molding process increases, as does the complexity of the size and shapes of the molds employed, thus complicating the manufacturing process and increasing the need for quality control measures. Further, modem vehicles do not allow space for a significant additional conventional padding or cushioning materials in view of the trend towards more compact interior designs and in some cases highly angled windshields.
[0006] U.S. Pat. No. 4,131,702, for example, describes a self-supporting molded headliner formed of a layered composite arrangement of polyethylene foam panels laminated on both sides to a reinforcing layer of rigid paperboard. Similarly, U.S. Pat. No. 5,503,903 depicts a headliner including front and back sheets of wood fibers and polypropylene laminated with an intermediate corrugated sheet. U.S. Pat. No. 4,020,207 depicts a multiple-layer structure comprising two sheets of polyethylene foam bonded with a reinforcing polymer-containing layer.
[0007] U.S. Pat. No. 5,879,802 teaches a vehicle panel material comprising a mixture of recycled, reground thermo-formable material and reprocessed headliner material which includes fibrous bats with polyester fibers, glass fibers and a thermo-setting resin. The method of manufacturing such material includes the steps of shredding thermo-formable material into strips; shredding headliner material comprising thermo-formable fibrous bats, glass fibers and thermo-setting resin; mixing and carding the thermo-formable material and headliner material into a mat; heating the mat to at least partially melt the thermo-formable material; and shaping the mat into a vehicle panel.
[0008] U.S. Pat. No. 5,884,962 discloses an impact absorption member comprising a sheet of crushable material having curvilinear projections having a width, height, length and spacing selected for different impact absorption characteristics. In a preferred embodiment of the invention, the projections are sinusoidal, and the material comprises a mixture of recycled, reground thermo-formable material and reprocessed fibrous bats including polyester fibers, glass fibers, and a thermo-setting resin. In the preferred embodiment of the invention, the member constitutes an elongated arch-shaped base having integrally superimposed thereon the curvilinear projections.
[0009] U.S. Pat. No. 6,036,227 sets forth an energy absorption material for covering a rigid vehicle support surface to provide impact protection for a vehicle occupant's head comprising a sheet of material formed into a waveform comprising a plurality of regular corrugations which have identical crests and valleys connected by inclined sidewalls. The material thickness of the crests and valleys is the same and thicker than that of the sidewall material. The crests and valleys are curved such that the inside radius of each of the crests is smaller than the inside radius of each of the valleys, so that the sidewalls adjacent a valley are laterally closer than the sidewalls adjacent a crest. The corrugations have a pitch equal to their height. This construction provides a deformation mode of the material in which the crests and valleys deform by bending and the sidewalls deform by buckling. The material can contain a plurality of perforations, covering 7%-15% of the area for sound absorption.
[0010] U.S. Pat. No. 6,070,902 teaches a vehicle interior headliner system useful in a vehicle having side windows and a roof panel. The headliner system includes a headliner attachable to the roof panel by a self-locating attachment system configured for blind attachment of the headliner to the roof panel. At least one inflatable bladder is secured to the headliner by the self-locating attachment system for deployment along the side windows. At least one inflator assembly is secured to the headliner for inflating the bladder. The self-locating attachment system includes a conical retainer and a floating fastener for blind attachment in a variety of applications.
[0011] U.S. Pat. No. 6,120,090 sets forth a headliner for motor vehicles which includes first and second sheets of material in juxtaposition to each other and adapted for positioning in a mold having two mold portions. The material of at least one of the sheets is fluid deformable with respect to another of the sheets, and is attachable to the material of the other of the sheets by the mold portions at sufficient locations to outline a potential duct between the sheets. The potential duct is adapted to receive fluid between the sheets for forming an actual duct. When fluid is received between the sheets, the material of the at least one sheet is deformed with respect to the material of the other of the sheets to define the actual duct. In one embodiment of the headliner, at least one head impact block is disposed in the duct. The headliner may also include at least one substantially air-impermeable layer disposed within the duct and attached to at least one of the first and second sheets. The layer preferably includes a polymer powder.
[0012] All of the foregoing U.S. patents are herein incorporated in their entirety by reference thereto.
[0013] Another known headliner construction includes top and bottom sheets attached together to form a duct in the rear portion of the headliner. The top sheet includes a corrugated cardboard layer sandwiched between two perforated polymer layers that allow moisture to pass therethrough. Furthermore, the top sheet is preformed by compression molding before being attached to the bottom sheet. Since space is limited, it is desirable to develop a material that can meet these stringent energy absorption standards and still provide sufficient sound isolation characteristics.
SUMMARY OF THE INVENTION
[0014] The present invention provides a construct useful as a headliner in a motorized vehicle that includes a substantially planar first base portion having an upper surface and a lower surface, and a plurality of absorption projections disposed on the upper surface of the base portion. The absorption projections each are shaped in the form of a geometric solid having an axis. The absorption projections may include a second base portion and a topmost portion, and the absorption projections extend from the upper surface such that their axes are oriented substantially perpendicularly to the plane of the base portion, The absorption projections include a hollow interior portion in a preferred form of the invention. Although the invention is described in terms of automotive headliners, the constructs of the invention are anticipated as being useful in other articles of manufacture which are designed for human head contact, including without limitation, motorcycle helmets, aircraft helmets, and sports helmets.
[0015] Another form of the present invention is a method of molding an automobile headliner that includes a substantially planar first base portion having an upper surface and a lower surface, and a plurality of absorption projections disposed on the upper surface of said base portion. The absorption projections each are shaped in the form of a geometric solid having an axis. The absorption projections include a second base portion and a topmost portion, and the absorption projections extend from the upper surface such that their axes are oriented substantially perpendicularly to the plane of the base portion, The absorption projections include a hollow interior portion in a preferred form of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The above and further advantages of the invention may be better understood by referring to the following detailed description in conjunction with the accompanying drawings in which corresponding numerals in the different figures refer to the corresponding parts in which:
[0017] [0017]FIG. 1 is a perspective view of a section of a headliner construct according to one form of the invention;
[0018] [0018]FIG. 2 a is a top view of a section of a headliner construct according to one form of the invention;
[0019] [0019]FIG. 2 b is a side view of a section of a headliner construct according to one form of the invention;
[0020] [0020]FIG. 2 c is a end view of a section of a headliner construct according to one form of the invention;
[0021] [0021]FIG. 2 d is a top view of a section of a headliner construct according to an alternate form of the invention;
[0022] [0022]FIG. 2 e is an underside view of a section of a headliner construct according to one form of the invention;
[0023] [0023]FIG. 3 is a perspective view of a section of a headliner construct according to an alternate form of the invention;
[0024] [0024]FIG. 4 a is a top view of a section of a headliner construct according to an alternate form of the invention;
[0025] [0025]FIG. 4 b is an end view of a section of a headliner construct according to an alternate form of the invention;
[0026] [0026]FIG. 4 c is a section A-A view of a section of a headliner construct according to an alternate form of the invention;
[0027] [0027]FIG. 4 d is an underside view of a section of a headliner construct according to an alternate form of the invention.
[0028] [0028]FIG. 5 a is a perspective view of a section of a headliner construct according to an alternate form of the invention;
[0029] [0029]FIG. 5 b is a top view of a section of a headliner construct according to an alternate form of the invention;
[0030] [0030]FIG. 5 c is a side view of a section of a headliner construct according to one form of the invention;
[0031] [0031]FIG. 5 d is a end view of a section of a headliner construct according to one form of the invention; and
[0032] [0032]FIG. 6 is a graph depicting the performance of an object in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0033] While the making and using of various embodiments of the present invention are discussed herein in terms of an automobile headliner and a method for making one, it should be appreciated that the present invention provides many applicable inventive concepts that can be embodied in a wide variety of specific contexts. The specific embodiments discussed herein are merely illustrative of specific ways to make and use the invention and are not meant to limit the scope of the invention in any manner.
[0034] Although the embodiments herein depicted in the various drawings show a construct according to the invention having absorption projections of uniform shape and dimension, the subject matter of the present invention contemplates headliner constructs comprising an assortment of absorption projections having different geometrical shapes. For example, a headliner construct according to the invention may include a row of truncated cones adjacent to a row of truncated pyramids. Alternatively, headliner constructs according to the present invention may include a row of rectangular solids adjacent to a row of truncated pyramids or a row of truncated cones. The various absorption projections selected may be present in a mixed array or present in a regularly repeating pattern. One non-delimitive example is shown in FIG. 5 in which a preferred embodiment of the invention is depicted as a headliner construct comprising two differently sized rectangular solids having different length dimensions arranged in a regular array.
[0035] Referring to the drawings and initially to FIG. 1 there is shown a section of a headliner construct 10 according to one form of the invention. Such a construct comprises a base portion 14 , which exists substantially in the shape of a planar sheet and can be thought of for purposes of defining the present invention as having a length dimension L, a width dimension W, and a thickness dimension T, although it may be rare that in actual practice that a rectangular construct would be employed since the head space in the interior of a motor vehicle is not exactly rectangular; however, it is nevertheless advantageous for defining the invention to consider a rectangular section of the disclosed construct.
[0036] In accordance with the invention, the base portion includes one or more absorption projections 12 which extend upwardly from the plane of the base portion. It is preferred that the projections are shaped in the form of geometric solids, such as cones, conical sections, pyramids, truncated pyramids, rectangular solids, rectangles, cubes, spheres, spheroids, ellipses, truncated ellipses, rhombohedral solids, truncated rhombohedral solids, etc. In one form of the invention, it is preferred that the absorption projections comprise a hollow interior portion 18 which assists in the absorption and dispersal of the energy from an impact, and such feature is conveniently achieved in a preferred manufacturing process of the constructs of the invention described elsewhere herein.
[0037] In the cases where it is desired to employ a truncated geometric solid, such as a truncated pyramid or truncated cone, as shown in FIG. 1, such truncated solid will preferably comprise a flat top portion 20 , and a hole 22 as shown in FIG. 1, which hole extends through the entire construct, including the base portion 14 .
[0038] One variable in a headliner construct according to the invention is the size of the hole 22 at the top flat surface portion 20 . It is preferred that when such hole is circular as in the cases where a truncated cone or cylindrically shaped absorption projection is selected, the diameter of the hole is preferably any value in the range of between about 0.10 and about 1.0 centimeters, including every hundredth centimeter there between. More preferably, the diameter of the hole is in the range of between about 0.2 and about 0.5 centimeters. It is most preferred that when the hole is circular that the diameter of the hole is about 0.3 centimeters.
[0039] In FIG. 2 a is shown a top view of a section of a headliner construct according to one form of the invention having a length dimension L and a width dimension W. In this figure, the absorption projections 12 are shown in a square array that is 8 absorption projections long and 6 absorption projections wide. However, the absorption projections 12 may also be in a staggered configuration as shown in FIG. 2 d , which principle is equally applicable to cases when other geometric solids are employed in the stead of truncated cones, which truncated cones shown in the embodiment of FIG. 1. In embodiments in which the absorption projections of the invention are arranged in rows that are not staggered, as shown in FIG. 2 a , the variable S 1 is used to refer to the distance between individual adjacent absorption projections from adjacent rows. It is preferred that this distance is between about 0.1 and about 2.0 centimeters, including every hundredth centimeter therebetween. It is more preferred that this distance is between about 0.5 and about 1.0 centimeters, including every hundredth centimeter therebetween, with about 0.75 centimeters being most preferable.
[0040] The shape of the portion of the absorption projection that contacts the base portion 14 is that of a circle as viewed from above when truncated cones are selected. Such circle represents the outer perimeter of the base of the cone at the point where it extends upwardly from the base portion 14 . Each one in a plurality of such circles have a centerpoint, and the centerpoints of adsorption projections in adjacent rows are separated by a definite distance when the absorption projections of the invention are arranged in rows which are not staggered, as shown in FIG. 2 a . The variable C is used to refer to the distance between the centerpoints of individual adjacent absorption projections from adjacent rows. It is preferred that this distance is between about 1.0 and about 4.0 centimeters, including every hundredth centimeter therebetween. It is more preferred that this distance is between about 1.5 and about 3.2 centimeters, including every hundredth centimeter therebetween, with about 2.0 centimeters being most preferable.
[0041] The shape of the portion of a given absorption projection which contacts the base portion 14 determines the amount of the surface area of the base portion which is to be occupied by the absorption projection. In the case where the shape of the portion of a given absorption projection which contacts the base portion 14 is circular, such absorption projection has a base diameter indicated by D in FIG. 2 a . It is preferred that this diameter is between about 0.5 and about 3.0 centimeters, including every hundredth centimeter therebetween in the case of a circular absorption projection. It is more preferred that this diameter is between about 1.0 and about 2.0 centimeters, including every hundredth centimeter therebetween, with about 1.5 centimeters being most preferable.
[0042] In the present application “absorption projection density” means the number of absorption projections that occupy a base portion 14 according to the invention in terms of absorption projections per square centimeter. It is preferred that the absorption projection density is between about 0.05 and about 1.0 absorption projections per square centimeter, in the case of a circular absorption projection. It is more preferred that this density is between about 0.10 and about 0.50 absorption projections per square centimeter, with about 0.36 absorption projections per square centimeter being most preferable.
[0043] When truncated cones are selected, the cones will appear circular as viewed from above at both the point where the lower portion of the cone contacts the base portion 14 and the outer perimeter of the upper portion 20 of the truncated cone. It is preferred that the diameter of the perimeter of the upper portion 20 of the truncated cone is between about 0.50 and about 2.5 centimeters, including every hundredth centimeter therebetween in the case of a circular absorption projection. It is more preferred that this diameter is between about 0.75 and about 2.0 centimeters, including every hundredth centimeter therebetween, with about 1.0 centimeters being most preferable.
[0044] The base portion 14 may take on any shape required by the particular application in which a headliner according to the invention will be used. Thus, it is quite often the case that a headliner construct according to the invention will not exist in the form of a rectangular sheet with its absorption projections, but will rather take on the shape of the headspace it is intended to cover. In any event, the base portion of a construct according to the invention will have a definite thickness as represented by T in FIG. 2 c . It is preferred that the thickness T is between about 0.10 and about 2.0 centimeters, including every hundredth centimeter therebetween. It is more preferred that the thickness T is between about 0.20 and about 1.75 centimeters, including every hundredth centimeter therebetween, with about 1.50 centimeters being most preferable.
[0045] Another variable in a headliner construct according to the invention is the thickness of the wall portion of the absorption projection as represented by Y in FIG. 2 c . In the cases where the absorption projection is selected to exist in the shape of a cylinder or truncated cone, it is preferred that the thickness Y is between about 0.10 and about 1.0 centimeters, including every hundredth centimeter therebetween. It is more preferred that the thickness Y is between about 0.20 and about 0.75 centimeters, including every hundredth centimeter therebetween, with about 0.40 centimeters being most preferable.
[0046] During the manufacture of a headliner construct according to the invention, indentations are formed on the opposite side of the base portion from which the absorption projections protrude thus causing holes 24 to appear thereon, as shown in FIG. 2 e.
[0047] [0047]FIG. 3 shows a perspective view of a section of a headliner construct according to an alternative embodiment of the invention in which the absorption projections are truncated pyramids. In FIG. 3, there is a base portion 14 , from whose surface project outwardly a plurality of absorption projections 12 each having an upper surface 20 having holes 22 disposed therethrough. The construct has a length dimension L a width dimension W, and a thickness dimension T.
[0048] In FIG. 4 a is shown a top view of a section of a headliner construct according to one form of the invention having a length dimension L and a width dimension W. In this figure, the absorption projections 12 are shown in a square array which is 6 absorption projections long and 4 absorption projections wide. However, the absorption projections 12 may also be in a staggered configuration as was shown in the case of the truncated cones in FIG. 2 d . In embodiments in which the absorption projections of the invention are arranged in rows that are not staggered, as shown in FIG. 4 a , the variable S 1 is used to refer to the distance between individual adjacent absorption projections from adjacent rows. It is preferred that this distance is between about 0.10 and about 2.0 centimeters, including every hundredth centimeter therebetween. It is more preferred that this distance is between about 0.20 and about 1.5 centimeters, including every hundredth centimeter therebetween, with about 0.75 centimeters being most preferable.
[0049] The shape of the portion of the absorption projection that contacts the base portion 14 is that of a square as viewed from above when truncated pyramids are selected. Such square represents the outer perimeter of the base of the pyramid at the point where it extends upwardly from the base portion 14 . Each one in a plurality of such squares have a centerpoint, and the centerpoints of adsorption projections in adjacent rows are separated by a definite distance when the absorption projections of the invention are arranged in rows which are not staggered, as shown in FIG. 3 a . The variable C is used to refer to the distance between the centerpoints of individual adjacent absorption projections from adjacent rows. It is preferred that this distance is between about 0.10 and about 1.0 centimeters, including every hundredth centimeter therebetween. It is more preferred that this distance is between about 0.20 and about 0.50 centimeters, including every hundredth centimeter therebetween, with about 0.30 centimeters being most preferable.
[0050] The shape of the portion of a given absorption projection which contacts the base portion 14 determines the amount of the surface area of the base portion which is to be occupied by the absorption projection. In the case where the shape of the portion of a given absorption projection which contacts the base portion 14 is a square, such absorption projection has a base dimension indicated by D in FIG. 4 a . It is preferred that this dimension is between about 0.20 and about 4.0 centimeters, including every hundredth centimeter therebetween in the case of a pyramidal absorption projection. It is more preferred that this dimension is between about 1.0 and about 3.0 centimeters, including every hundredth centimeter therebetween, with about 1.5 centimeters being most preferable.
[0051] In the case of pyramidal absorption projections, it is preferred that the absorption projection density is between about 0.1 and about 1.0 absorption projections per square centimeter. It is more preferred that this density is between about 0.20 and about 0.50 absorption projections per square centimeter, with about 0.37 absorption projections per square centimeter being most preferable.
[0052] When truncated pyramids are selected, the pyramids will appear as a square as viewed from above at both the point where the lower portion of the pyramid contacts the base portion 14 , and at the outer perimeter of the upper portion 20 of the truncated pyramids. It is preferred that the length dimension of the perimeter of the upper portion 20 of the truncated pyramid is between about 0.2 and about 3.5 centimeters, including every hundredth centimeter therebetween in the case of a circular absorption projection. It is more preferred that this dimension is between about 0.5 and about 2.5 centimeters, including every hundredth centimeter therebetween, with about 1.5 centimeters being most preferable. In the case when the upper surface 20 of a truncated pyramid exists in the shape of a rectangle, these same preferred dimensions are applicable, and refer to the length dimension of such rectangle.
[0053] The base portion 14 may take on any shape required by the particular application in which a headliner according to the invention is will be used. Thus, it is quite often the case that a headliner construct according to the invention will not exist in the form of a rectangular sheet with its absorption projections, but will rather take on the shape of the headspace it is intended to cover. In any event, the base portion of a construct according to this embodiment of invention will have a definite thickness as represented by T in FIG. 4 b . It is preferred that the thickness T is between about 0.10 and about 2.0 centimeters, including every hundredth centimeter therebetween. It is more preferred that the thickness T is between about 0.20 and about 1.75 centimeters, including every hundredth centimeter therebetween, with about 1.50 centimeters being most preferable.
[0054] A construct according to the invention in which square pyramids are employed as the absorption projections also has an overall height measurement, as represented by H in FIG. 4 b . It is preferred that the height H is between about 0.50 and about 3.00 centimeters, including every hundredth centimeter therebetween. It is more preferred that the height H is between about 1.00 and about 2.50 centimeters, including every hundredth centimeter therebetween, with about 2.00 centimeters being most preferable.
[0055] A construct according to the invention in which pyramids are employed as the absorption projections also has as one of its variables of construction the dimensions of the length B and width G of the holes in the planar base portion when viewed from the underside, as shown in FIG. 4 d . In the case where B and G are equal, the absorption projection exists in the shape of a square pyramid. It is preferred that the width G is between about 0.50 and about 3.00 centimeters, including every hundredth centimeter therebetween. It is more preferred that the width G is between about 0.75 and about 2.00 centimeters, including every hundredth centimeter therebetween, with about 1.75 centimeters being most preferable.
[0056] It is preferred that the length B is between about 0.50 and about 3.00 centimeters, including every hundredth centimeter therebetween. It is more preferred that the length B is between about 0.75 and about 2.00 centimeters, including every hundredth centimeter therebetween, with about 1.75 centimeters being most preferable.
[0057] Another variable in a headliner construct according to the invention is the size of the hole 22 at the top flat surface portion 20 . In cases where the hole is not circular as in the cases where an absorption projection having a pyramidal or rectangular solid is selected, the hole will be either be square or rectangular in dimension, although other shapes are contemplated herein, such as ellipses, ovals, rhombuses, hexagons, trapezoids, etc. When the hole is a square polygon such as a square or rectangle, the dimensions of length Z and width Q from FIGS. 4 a and 4 c serve to define the dimensions of the hole 22 at the top surface 20 of the absorption projections. In the case where Z and Q are equal, the hole at the top portion 20 of the absorption projection exists in the shape of a square. It is preferred that the length Z is between 0.10 and 1.00 centimeters, including every hundredth centimeter therebetween. It is more preferred that the length Z is between about 0.20 and about 0.75 centimeters, including every hundredth centimeter therebetween, with about 0.30 centimeters being most preferable. It is preferred that the width Q is between about 0.10 and 1.00 centimeters, including every hundredth centimeter therebetween. It is more preferred that the width Q is between about 0.20 and about 0.75 centimeters, including every hundredth centimeter therebetween, with about 0.30 centimeters being most preferable.
[0058] A further variable in a headliner construct according to the invention is the thickness of the wall portion of the absorption projection as represented by Y in FIG. 4 c . In the cases where the absorption projection is selected to exist in the shape of a pyramid, it is preferred that the thickness Y is between about 0.10 and about 1.00 centimeters, including every hundredth centimeter therebetween. It is more preferred that the thickness Y is between about 0.20 and about 0.75 centimeters, including every hundredth centimeter therebetween, with about 0.40 centimeters being most preferable.
[0059] Although the embodiments herein depicted in the various drawings show a construct according to the invention having absorption projections of uniform shape and dimension, the present invention contemplates headliner constructs comprising an assortment of absorption projections having different geometrical shapes. For example, a headliner construct according to the invention may include a row of truncated cones adjacent to a row truncated pyramids. Alternatively, headliner construct according to the invention may include a row of rectangular solids adjacent to a row truncated pyramids or a row of truncated cones. The various absorption projections selected may be present in a mixed array or arranged in a regularly repeating pattern.
[0060] One non-delimitive example is shown in FIG. 5A, in which a preferred embodiment of the invention is depicted having a headliner construct comprising two differently sized solids having different length dimensions arranged in a regular array. This embodiment utilizes projections 26 and 28 that are essentially quadrilateral in shape such that they are either substantially cubes or rectangles. In the case of substantially rectangular projections 26 and 28 the relative ratio of the lengths of the sides can be varied as necessary to maximize the impact protection and to allow for finished headliner to be fitted to the appropriate shape for installation. As shown in FIG. 5A, the size of all of the projections 26 and 28 need not be identical. The number and width of channels 30 and 32 are also a variable in the construction of this embodiment of the present invention. The width of both channels 30 and 32 is typically about 1.3 centimeters. The thickness and width of the projections may be varied as desired to meet the design requirements for a specific headliner application, with the longest legs of the rectangles typically ranging from about 0.2 to 2.0 centimeters.
[0061] The height of the projections 34 that is shown in FIGS. 5C and 5D is also variable depending on the application for which the finished headliner is to be used. The thickness of the foam 36 that forms the headliner is typically about 30 mm thick, but can be varied as desired.
[0062] The graph in FIG. 6 depicts the beneficial results obtained with the present invention. The axes of the graph are acceleration, in units of multiples of the force of gravity (G's) and displacement, measured in millimeters. The baseline case, I, which does not include the advantages of the present invention, has an HIC (d) value of 1600. Plot II is data obtained for a 25 mm thickness of GECET® foam having a density of 3.0 pounds per cubic foot (pcf) in a pattern similar to that depicted in FIG. 5. where the approximate width and length of the top of projections 26 are about 23 mm and 10 mm respectively, and the approximate width and length of the top of projections 28 are about 60 mm and 10 mm respectively. The width of the channels 30 and 32 is approximately 10 mm.
[0063] Plots III, IV and V are for similarly patterned GECET® foam to that used in plot II, wherein the thicknesses 36 and densities are 25 mm and 2.5 pef (III), 30 mm and 2.5 pcf (IV), and 35 mm and 3.0 pcf (V). The HIC(d) values for the four samples are 890(II), 874 (III), 717 (IV) and 622(V), which are well below the value of 1000 mandated by FMVSS 201.
[0064] The preferred materials of construction of a headliner according to the present invention include all materials known in the prior art which have been used as cushioning materials in headliners used in motor vehicles and others, including foams such as polyolefin foams such as polyethylene foams, polypropylene foams, polystyrene foams, polyurethane foams, polyurea foams, etc. Such materials include without limitation various foamed materials such as: polyurethanes, foamed polystyrenes, foamed polyolefins such as polypropylene and polyethylene, including copolymers thereof. Especially preferred materials are the resins known as GECET® resins ARCEL® resins and RMER® resins. Any foamed material is suitable for providing a construct according to the invention.
[0065] A finished headliner construct according to the invention, includes indents on the opposite side of the base portion from which the absorption projections protrude which appear in the form of holes 24 , as is shown in FIGS. 2 e and 4 d.
[0066] In order to produce a headliner construct according to the present invention one may use a thermoforming process using a sheet of foam as a starting material as such thermoforming is known to those skilled in the art. In cases where truncated cones, pyramids, cylinders, etc. are selected, a die may be used to cut the holes in the formed sheets either prior to or after thermoforming. Alternatively, the foam may be produced by introducing the pre-set foam composition into a mold, as such is known to those skilled in the art.
[0067] Consideration must be given to the fact that although this invention has been described and disclosed in relation to certain preferred embodiments, obvious equivalent modifications and alterations thereof will become apparent to one of ordinary skill in this art upon reading and understanding this specification and the claims appended hereto. Accordingly, the presently disclosed invention is intended to cover all such modifications and alterations, and is limited only by the scope of the claims that follow.
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Provided herein are headliners for use in motorized vehicles. The headliners are of such construction that head impact encountered during a collision is greatly reduced over headliners of prior art. A headliner according to the invention comprises a substantially-planar first base portion having an upper surface and a lower surface, and a plurality of absorption projections disposed on said upper surface of said base portion. The absorption projections each are shaped in the form of a geometric solid having an axis. The absorption projections include a second base portion and a topmost portion, and the absorption projections extend from the upper surface such that their axes are oriented substantially perpendicularly to the plane of the base portion.
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FIELD OF THE INVENTION
The present invention relates to a continuous method of eliminating excess nitrite in diazotisation solutions, which method is controlled by an electrochemical controlled variable.
BACKGROUND OF THE INVENTION
The usual procedure for the preparation of azo dyes is to diazotise the amine employed as diazo component in a first step and then, in a second step, to react the diazotised amine with the appropriate coupling component. The diazotisation is normally carried out in a mineral acid solution by adding an excess of nitrite, e.g. sodium nitrite. When diazotisation is complete, the excess nitrite must be removed before the azo coupling takes place. This removal is usually effected by adding a small amount of non-diazotised amine or by adding urea or amidosulfonic acid (sulfamic acid). For diazotisation on an industrial scale the rapidly acting sulfamic acid is normally added. However, the drawback of this procedure is that if an excess of sulfamic acid is added, especially where diazonium salts containing strongly negative substituents are obtained, it may result in secondary reactions, e.g. in the reaction of the sulfamic acid with the diazonium salt so that the amine is formed again by rediazotisation (q.v. H. R. Schweizer, Kunstliche Organische Farbstoffe und ihre Zwischenprodukte, Springer Verlag 1964, page 182). To avoid this yield-diminishing secondary reaction it is necessary to add the sulfamic acid as accurately as possible in an amount just sufficient to destroy the excess nitrite. Especially in continuous reactions, monitoring the concentration of nitrite in the diazotisation solution by the widely employed spot test on potassium iodide starch paper has not proved at all suitable Hence it is the object of the present invention to provide a method that permits continuous monitoring of the nitrite concentration and a smooth controlled addition of agent for removing nitrite.
SUMMARY OF THE INVENTION
It has now been found that it is possible to determine the concentration of nitrite in diazotisation solutions in simple manner by means of an electrochemical method of analysis, wherein the current-voltage characteristic of suitable electrodes can be utilised directly as controlled variable for regulating the addition of agent for removing nitrate.
Accordingly, the present invention relates to an automatically controlled continuous method of eliminating excess nitrite in diazotisation solutions of aromatic amines, which comprises controlling the addition of the agent employed for eliminating the nitrite ions by means of an electrochemically controlled variable.
DESCRIPTION OF THE INVENTION
Suitable electrochemical methods of analysis are primarily potentiometric, voltrametric or polarographic methods. Among these methods, it is preferred to use the potentiometric method. This method comprises monitoring the change in the redox potential of the diazotisation solution as a function of the nitrite concentration using electrodes of known construction, and subsequently regulating the addition of agent for removing nitrite.
The electrochemical methods of analysis referred to above are known per se and are described e.g. in Kirk-Othmer, Encyclopedia of Chemical Technology, Vol. 2 (1978), page 616 ff. and Vol. 8 (1979), page 662 ff.; Rompps Chemie-Lexikon, Vol. 2 (1981), page 1081 ff. and the literature cited therein. Examples of suitable indicator electrodes are platinum, silver/silver chloride, platinum/calomel or gold/calomel electrodes. A platinum/glass single rod electrode is particularly suitable for use in the process of this invention.
The method of the invention is normally carried out in a voltage range from about 50 to 700 mV, with control being effected within an interval of about 2-10 mV in the range of maximum sharpness of the voltage curve (end point) for the control system.
If the voltage falls to values below this interval, then the addition of agent for removing nitrite is discontinued. If the voltage rises to values above this range, then addition of agent for removing nitrite is recommended. The great advantage of measuring redox potentials resides in the substantially instantaneous indication allied to simple use of the fluctuations of the potential for automatic control purposes. A process control computer is conveniently employed as control means for regulating the pump which adds the agent for removing nitrite.
The excess nitrite is removed with customary agents, preferably sulfamic acid, which is conveniently added in the form of a 0.5 to 1 molar aqueous solution. Urea or p-nitroaniline may also suitably be used; but nitroaniline is only suitable if the shade of the dye will not thereby be adversely affected.
A further advantage of using sulfamic acid is that, when added intermittently and at a constant rate, it keeps the electrode clean. This kind of addition, in which a small excess of sulfamic acid is briefly present in the diazotisation solution, can be readily made by on/off feed-back control. In this context, a constant rate of addition shall be understood as meaning that a constant amount of sulfamic acid solution is added to the diazotisation solution per unit of time, provided the metering pump is switched on (position: on), i.e. that the voltage has risen to values above the interval. In addition to the potentiometric method preferably employed in this invention, suitable electrochemical methods are--as mentioned at the outset--e.g. the polarographic or voltametric method. This last mentioned method is carried out for example using two platinum electrodes which are polarised by a constant current. If excess nitrite is present, the electrodes are depolarised, which is reflected in a sharp drop in voltage. This drop in voltage is utilised to regulate the pump or valve by means of which the requisite amount of agent for removing nitrite is added to the diazotisation solution. The control system is here to adjusted to a point on the sharp drop in voltage that corresponds more or less to the equivalence point.
DESCRIPTION OF THE DRAWING
The procedure is for example (see drawing) that the diazo component (RNH 2` ) is diazotised continuously with sodium nitrite in a tube reactor R and the nitrite-containing diazotisation solution is subsequently passed into a stirred vessel K. The addition of sulfamic acid, controlled by the potential, is made simultaneously from the storage vessel B. The stirred vessel K is equipped with an electrode E (platinum/glass single rod electrode). The fluctuations in potential measured by means of this electrode are processed by the process control computer C which, via a corresponding control signal, regulates the pump P which pumps the aqueous solution of sulfamic acid into the stirred vessel. The reaction of nitrous acid with the sulfamic acid then takes places at a temperature in the range from 10° to 50° C., although higher temperatures may also be chosen according to the stability of the diazonium salt. As substantial amounts of nitrogen are evolved, it is advisable to carry out the process in an open vessel, especially as the diazonium salt solutions have a tendency to foam fairly strongly. The residence time of the diazotisation solution in the stirred vessel is about 1 to 30, usually 3 to 10, minutes. Diazonium salt solution (RN 2 +) which is free from nitrite is drawn off continuously from the stirred vessel and, if necessary, subsequently clarified by filtration and then coupled to a suitable coupling component. The method is susceptible of application to all amines which can be diazotised in acid aqueous media.
A suitable, fully electronic, microprocessor-controlled device for controlling a pump or other device in response to a fluctuating electrical signal is the Capax 5SO (Camille Bauer AG, Wohnen, Switzerland).
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In particular, the method of the present invention can be used for the preparation of azo dyes, preferably for the continuous preparation of azo dyes. The preferred utility is as part of an on-line control of a computer-integrated, automated process for the preparation of azo dyes.
Examples of suitable diazo components are: amiline and derivatives thereof such as 4-nitroaniline, 3-nitroaniline, 2-chloro-4-nitroaniline, 4-chloro-2-nitroaniline, 2,6-dichloro-4-nitroaniline, 4-aminoacetanilide, 2,4-dinitroaniline, 2-cyano-4-nitroaniline, 4-cyanoaniline, 4-chloroaniline, 2,4,5-trichloroaniline, 2,5-dimethoxyaniline, o-anisidine, p-anisidine, o-phenetidine, p-phenetidine, o-toluidine, p-toluidine, 4-nitro-2-aminoanisole, 2-nitro-4-aminoanisole, p-phenoxyaniline, or also 4-methylsulfonylaniline, 4-amino-2, 4-dichlorobenzophenone, 4'-amino-2,4-dinitro-benzophenone, 2-nitroaniline, 2-chloro-4, 6-dinitroaniline, 2, 5-dichloroaniline, 3, 3'-dichlorobenzidine, 5-nitro-2-amino-anisole, 3-nitro-4-aminotoluole, 2, 4-dichloroaniline, 3-nitro-4-aminoanisole, 2-aminoanisole-4-sulfodietylamide, 5-chloro-2-aminotoluene, 4-chloro-2-aminotoluene, 4-nitro-2-aminotoluene, 5-nitor-2-aminotoluene, 4-nitro-2-aminoanisole, 3, 3-dimethoxybenzidine, 3, 3'-dimethyoxy-6, 6'-dichlorobenzidine, 2-amino-4-chlorophenol, 2-aminophenol-4-sulfamide, 2-aminophenol-5-sulfamide, 2-aminophenol-4-sulfomethylamide, 3-amino-4-hydroxyphenylmethylsulfone, 2-amino-5 -nitrophenylmethylsulfone, 4-amino-3-nitrophenylmethylsulfone, 2-(N-methyl-N-cyclohexylsulfamoyl)aniline, 2-amino-4, 2', 4'-trichlorodiphenyl ether and 4-aminoazobenzene; α- or β-napthylamine, and derivatives thereof, such as 2-naphtylamine-6, 8-disulfonic acid, 1-naphthylamine-3, 6, 8-trisulfonic acid, 4-naphthylamino-5-hydroxy-1, 7-disulfonic acid or 2-naphthylamino-7-hydroxy-6-sulfonic acid; Examples of further heterocylic amines are: 3-amino-1,2, 4-triazole, 2-aminothiazole, benzthiazoles such as 2-aminobezthiazole, 2-amino-4-chlorobenzthiazole, 2-amino-4-cyanobenzthiazole, 2-amino-4, 6-dinitrobenzthiazole, 2-amino-4-methoxy-6-nitrobenzthiazole, 2-amino-6-methoxyl-1, 3-benzonthiazole or aminobenztriazoles, which may also be appropriately substituted.
The invention is illustrated by the following Example, in which percentages are by weight.
EXAMPLE:
A mixture of 4158.25 g of 4-aminoactanilide (89.0%) and 2588.25 g of aniline (100%) is diazotised continuously in a tube reactor in a hydrochloric acid solution. A 0.5 to 10% excess of nitrite is employed, based on the theoretically required amount. The diazotisation solution containing excess nitrite is introduced into a straight-through reactor, in which the redox potential is measured continuously by means of a platinum/argental single rod electrode. As a function of the potential, an aqueous solution of sulfamic acid is introduced into the straight-through reactor. This addition is made by means of a pump, regulated by a process control computer which switches the pump on and off as required. The addition of sulfamic acid is made such that the potential of the diazo solution is kept within a 10 -30 mV interval in the range of the end point, e.g. from 590 mV to 610 mV. The reaction between the nitrous acid and the sulfamic acid proceeds at room temperature (20°-25° C.) and the adiabatic rise in temperature is about 1° C. The residence time in the straight-through vessel is not less than 3 minutes. It is expedient to ensure that nitrogen evolved in the course of there reaction can escape from the vessel. This method ensures that the diazo solution leaves the straight-through reactor free from nitrite and can then be further processed in known manner to azo dyes.
Even after prolonged operation, no toxic deposits can be observed on the electrode. Comparably good results are obtained by using a platinum/glass electrode instead of the platinum/argental electrode.
Excess nitrite is also removed by the same method from diazotisation solutions of the following amines: 2-chloro-4-nitroaniline, 4-chloro-2-nitroaniline, 4-aminoazobenzene and 3-amino-1, 2, 4-triazole.
By repeating the procedure of this Example, but using the voltametric or polarographic method instead of the potentiometric method, and/or by using urea and/or 4-nitroaniline instead of sulfamic acid, it is also possible to monitor the nitrite ion concentration of diazotisation solutions and to control the amount of agent for removing nitrite.
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The invention relates to an automatically controlled continuous method of eliminating excess nitrite in diazotization solutions of aromatic amines, which comprises controlling the addition of the agent employed for eliminating the nitrite ions by means of an electrochemically controlled variable.
The process permits a smooth monitoring of the nitrite ion concentration in diazotization solutions. It is advantageous that the determination of the electrochemical controlled variable is almost instantaneous and that the addition of agent for removing nitrite ions can be controlled in simple manner via the fluctuations in the potential.
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This application is a divisional of co-pending application Ser. No. 11/633,996 filed Dec. 4, 2006, which is a non-provisional application based on provisional patent application Ser. No. 60/752,283.
FIELD OF THE INVENTION
The present invention pertains to a wear assembly for securing a wear member to an excavating bucket or the like.
BACKGROUND OF THE INVENTION
Wear members in the form of adapters, shrouds, and the like are ordinarily secured to the front edge of an excavating bucket. Such wear members are commonly subjected to harsh conditions and heavy loading. Accordingly, the wear members wear out over a period of time and need to be replaced. The wear members are made to withstand the rigors of a digging operation and still be capable of replacement when worn. Whisler-style locking arrangements have long been in use for mechanically attaching wear members to the lip of a bucket. Such locks generally consist of a wedge and a C-shaped clamp or spool. While the wedge is typically hammered into the assembly, U.S. Pat. Nos. 4,433,496 and 5,964,547 disclose arrangements wherein the wedge is drawn into place under pressure from a screw. U.S. Patent Application Publication No. 2004/0216336 discloses a lock where the wedge is a conical threaded member that is turned to drive the wedge into and out of the assembly.
FIG. 19 discloses one example of a conventional Whisler shroud 21 attached to a lip 16 . As seen in the drawing, the lip includes a digging edge 25 , an inner surface 27 and an outer surface 29 . A hole 31 , which is elongated axially, extends through the lip at a location rearward of the digging edge. Hole 31 has a generally straight front wall 33 and a rear wall 35 that includes a step 37 . The step includes a tapered surface 39 that tapers away from inner surface 27 as it extends rearward away from digging edge 25 .
Shroud 21 wraps around the front end 25 of lip 16 with an inner leg 41 extending along inner surface 27 and an outer leg 43 extending along outer surface 29 . Inner leg 41 includes an through-hole 47 which generally aligns with hole 31 when the shroud 21 is put on the lip. The hole 31 and opening 47 collectively define a passage 49 into which is received a lock 51 adapted to releasably hold the shroud 21 to the lip 16 . Through-hole 47 includes a step 53 adjacent wear surface 55 of inner leg 41 . As with step 37 in hole 31 , step 53 includes a tapered surface 57 that tapers away from inner surface 27 as it extends rearward away from the digging edge 25 . In this way, tapered surfaces 39 , 57 diverge rearwardly at generally equal inclinations relative to a central axis of the lip 16 .
Lock 51 includes a wedge 61 and a clamp or spool 63 . Spool 63 has C-shaped configuration with a generally vertical body 65 and two axially extending arms 67 , 69 . Upper arm 67 is adapted to fit within step 53 , while lower arm 69 is adapted to fit within step 37 . Each arm 67 , 69 is formed with an inclined inner wall 71 , 73 that conforms and sets against a respective tapered surface 39 , 57 . The front surface of body 65 defines a ramp surface 75 that is inclined forward (relative to vertical) as it extends downward in passage 49 . Wedge 61 has front and rear converging walls 81 , 83 . Converging wall 83 abuts ramp surface 75 during installation and use in order to produce a tight fit of lock 51 in passage 49 . As shown in FIG. 19 , converging wall 83 and ramp surface 75 are formed with interlocking ridges 85 to ensure a stable and sure contact between the surfaces.
For installation, shroud 21 is first fit on lip 16 so that through-hole 47 generally aligns with hole 31 . Spool 63 is then placed within the defined passage 49 with arms 67 , 69 inserted into steps 37 , 53 . On account of the incline of tapered wall 57 and inner wall 71 , the spool tends to slide forward and downward through passage 49 if not held in place. As a result, the spool at times can slip through the lip and fall to the ground requiring the worker to retrieve it from under the bucket. This can be a difficult process particularly if installation is being done at night. In addition, crawling under the bucket can place the worker in a potentially hazardous position.
The spool 63 must therefore be held in place while the wedge 61 is inserted into the assembly. In order to withstand the rigors of the digging operation, the wedge must be fit very tightly into passage 49 . A large hammer is required to install the wedge into the assembly, which places the worker in a potentially hazardous position for injury from pieces that may fly off during hammering.
As wedge 61 is forced into passage 49 , arms 67 , 69 are pushed rearward over tapered walls 39 , 57 . This causes shroud 21 to be pulled tight against digging edge 25 and inner leg 41 to be pinched against lip 16 . This tight fit is intended to resist heavy and diverse loading that may be applied to the wear member. The large forces applied to the spool arms can result in spreading of the arms. Such spreading reduces the grip of the lock on the wear member and can at times lead to failure of the lock.
SUMMARY OF THE INVENTION
The present invention pertains to an improved wear assembly for securing wear members to excavating equipment or the like.
The present invention regards a lock assembly for securing a wear member to a base. For example, the inventive lock is useful in securing a shroud or other wear member to a lip of an excavating bucket to avoid problems experienced in the prior art.
In one aspect of the invention, an improved spool is used with a wedge to hold the wear member in place. The spool is formed with at least one laterally extending arm at its upper end in lieu of an axial arm such as used in a conventional C-shaped spool. In this way, the spool can be easily supported in the assembly as the wedge is installed. The spool does not fall through the opening and no special care is needed to prevent it from falling. As a result, installation of the wear assembly is easier and less hazardous. In addition, the lateral support reduces the risk that the spool will suffer spreading.
In a preferred construction, an upper lateral arm extends outward from each side of a spool body to generally define a T-shaped configuration. The spoof with upper lateral arms can be used with a variety of lower arms, such as an axial arm, lower lateral arms or other supports adapted to engage a lower leg or lower portion of the lip. In any of the combinations, the inner walls of the upper and lower arms are preferably inclined outward in a rearward direction to apply the rearward pinching force generally provided in Whisler-style locks.
Similarly, in another aspect of the invention, the wear member is formed with an opening having at least one spool support for receiving and holding a spool with a lateral arm. Preferably, the wear member is formed with a side recess as the spool support to each side of the lock-receiving opening. As noted above, this new construction enables the wear member to be assembled on the lip or other equipment more easily and with less risk to the user.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an axial cross-sectional view of a wear assembly in accordance with the present invention secured to a lip of a bucket.
FIG. 2 is an enlarged, partial cross-sectional view of the wear assembly.
FIG. 3 is a partial top view of the wear assembly.
FIG. 4 is a perspective view of the wear assembly with an axial cross-section.
FIG. 5 is a side view of a spool in accordance with the present invention.
FIG. 6 is a front perspective view of the spool.
FIG. 7 is a rear perspective view of the spool.
FIG. 8 is a perspective view of a wedge in accordance with the present invention.
FIG. 9 is a perspective view of a lock assembly in accordance with the present invention.
FIG. 10 is a perspective view of a wear member in accordance with the present invention.
FIG. 11 is an enlarged, partial perspective view of the through-hole in the wear member.
FIG. 12 is an upper perspective view of an alternative wear assembly of the present invention without the wedge.
FIG. 13 is a bottom perspective view of the alternative wear assembly without the wedge.
FIG. 14 is an exploded perspective view of the alternative wear assembly without the wedge.
FIG. 15 is a perspective view of the alternative wear assembly with the spool partially installed into the wear assembly.
FIG. 16 is a perspective view of the alternative wear member.
FIG. 17 is a bottom perspective view of a portion of a lip adapted to be used with the alternative wear assembly.
FIG. 18 is an axial cross-sectional view of a second alternative wear assembly in accordance with the present invention.
FIG. 19 is an axial cross-sectional view of a wear assembly of the prior art.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention pertains to a wear assembly 100 in which a wear member 102 is releasably attached to excavating equipment 103 ( FIGS. 1-4 ). In this application, wear member 102 is described in terms of a shroud that is attached to a lip of an excavating bucket. However, wear member 102 could be in the form of other kinds of products (e.g., adapters, wings, etc.) attached to other equipment. Moreover, relative terms such as forward, rearward, up or down are used for convenience of explanation with reference to the drawings; other orientations are possible.
In one embodiment ( FIGS. 1-4 ), shroud 102 fits on a conventional lip 16 . Although the lip in FIG. 1 is slightly different than in FIG. 19 , for convenience, the same numbers are used to identify the lip and its features. The particular lip construction is not critical for the invention, and an assembly in accordance with the present invention can be used with a wide range of lips.
Lock 104 includes a wedge 106 and a spool or clamp 108 to releasably secure shroud 102 to lip 16 ( FIGS. 1-9 ). Spool 108 includes a body 110 , at least one and preferably two upper arms 112 , and a lower arm 114 . Lower arm 114 is formed in the same manner as lower arm 69 in a conventional spool; i.e., lower arm 114 extends axially rearward from body 110 . Lower arm 114 also has an inclined inner surface 116 that sets against tapered wall 39 formed in the lip. However, unlike a conventional spool, spool 108 includes at least one laterally extending upper arm 112 to engage shroud 102 . In the preferred construction, an upper lateral arm 112 extends outward from each side 118 of body 110 in a transverse direction so as to define a generally T-shaped configuration with body 110 .
In the preferred construction, wedge 106 has a rounded, conical shape with a helical thread 120 formed on its exterior surface 122 , preferably in the form of a helical groove. The wedge is formed generally in accordance with the wedge disclosed in co-pending U.S. Patent Application Publication No. 2004/0216336 and U.S. patent application Ser. No. 10/824,490, which are both incorporated herein by reference. Spool 108 includes a front ramp surface 126 , inclined to vertical, to abut exterior surface 122 of wedge 106 . Ramp surface 126 preferably includes a trough 128 with a concave surface that generally conforms to the curve of wedge 106 , but other concave configurations could be used to provide the desired support to the wedge. Other shaped ramp surfaces may also be used so long as the abutment of the wedge and spool is sufficient and stable in the assembly during use. The trough may extend substantially along the entire length of body 110 or only part way. In either case, a thread formation 130 is provided on ramp surface 126 , and in this embodiment, within trough 128 , to mate with thread 120 of wedge 106 . Thread formation 130 may extend the entire length of trough 128 as shown or along only a part of the length.
Wear member 102 is formed with a front working end 134 , an inner leg 136 and an outer leg 138 ( FIGS. 1-4 and 10 - 11 ). As with known shrouds, inner leg 136 is preferably longer than outer leg 138 , but other arrangements could be used (see, e.g., FIG. 18 where the legs are the same length). Inner leg 136 includes a through-hole 140 that generally aligns with hole 31 in lip 16 to collectively define a passage 141 . However, unlike conventional shrouds 21 , through-hole 140 includes at least one and preferably two spool supports 142 extending along sides 144 ( FIGS. 10 and 11 ). In a preferred construction, spool supports 142 are recesses or steps that extend partially through inner leg 136 within through-hole 140 . In the preferred construction, each spool support or recess 142 includes a bearing surface 146 and a stop 148 in a generally V-shaped configuration, though other shapes could be used. Bearing surface 146 is preferably inclined away from lip 16 as it extends rearward away from digging edge 25 but other configurations could be used. The inclination of bearing surface 146 relative to the lip is preferably the same as tapered or inclined wall 39 in lip 16 , albeit in the opposite direction. Stop 148 is preferably inclined away from the lip in the forward direction. As one example, bearing surface 146 sets about 18 degrees relative to lip 16 , and about 90 degrees relative to stop 148 ; although a wide variation of each angle could be used.
Each lateral arm 112 of spool 108 is received into a corresponding spool support or recess 142 of shroud 102 ( FIGS. 1-4 ). In the preferred construction, each upper arm 112 includes a bearing surface 152 and a stop 154 to complement and engage bearing surface 146 and stop 148 of the recess 142 into which it is received ( FIGS. 3 , 4 , 10 and 11 ). Bearing surface 152 is inclined to generally conform to the inclination of bearing surface 146 in shroud 102 , and stop 154 to generally conform to the inclination of stop 148 , although other shapes are possible. When spool 108 is installed into passage 141 , bearing surface 152 of spool 108 sets against bearing surface 146 of shroud 102 , and stop 154 against stop 148 . The engagement of surfaces 146 , 152 and 148 , 154 prevent the spool from falling through the passage 141 . The V-shaped configuration of bearing surfaces 146 , 152 and stops 148 , 154 also hold spool 108 in place as wedge 106 is inserted.
To install lock 104 , spool 108 is first placed into passage 141 such that lower arm 114 is set in step 37 and upper arms 112 are set in spool supports or recesses 142 . The recesses 142 hold the spool in its proper position for receiving the wedge without any additional holding by a worker or anything else. As a result, the spool no longer falls through the lip to the ground. Additionally, workers are not forced into hazardous conditions when installing the locks.
Following insertion of spool 108 , wedge 106 is installed into passage 141 between front wall 33 of hole 31 and ramp surface 126 of spool 108 . In the preferred construction, wedge 106 includes a tool engaging structure 156 such as a socket for a wrench. Thread formation 120 of wedge 106 is engaged with thread formation 130 of spool 108 , and the wedge rotated about its axis 158 to draw the wedge into passage 141 . As the wedge is driven into the opening, spool 108 is pushed rearward such that bearing surfaces 152 press against bearing surfaces 146 , and inner surface 116 presses against tapered wall 39 . The upper and lower arms 112 , 114 of spool 108 , then, function to push shroud 102 rearward into a tight fit with lip 16 and to pinch inner leg 136 against the inner surface 27 of lip 16 for a secure attachment of the wear member to the bucket. The positioning of the upper arms 112 closer to the vertical axis of the spool also reduces the tendency for the upper and lower arms to spread apart during use; that is, this new orientation of the upper arms reduces the couple tending to spread the arms in conventional spools such that upper and lower arms 112 , 114 of spool 108 experience less deformation in use.
Spool 108 preferably includes a cavity 160 in trough 128 ( FIG. 6 ). A retainer 162 preferably formed of a rubber, foam or other elastomer is fit within the cavity to press outward against the exterior surface 122 of wedge 106 . The retainer provides resistance to prevent loosening of the wedge as the bucket is used in digging operations. Of course, other retainers could also be used to prevent loosening.
In an alternative embodiment ( FIGS. 12-17 ), spool 108 a is formed with lower lateral arms 114 a as well as upper lateral arms 112 a . The lip 16 a is, then, formed with lower spool supports 37 a ( FIG. 17 ) rather than the conventional axial step 37 ( FIG. 19 ). Upper lateral arms 112 a can retain the same structure as arms 112 . Spool 108 a is turned ninety degrees for installation into passage 141 a ( FIGS. 14 and 15 ). Specifically, spool 108 a is initially turned so that lower lateral arms 114 a extend generally parallel to the rearward extension of inner leg 136 a of wear member 102 a , i.e., forward and rearward relative to passage 141 a . In this way, the spool can be inserted into passage 141 a until the lower arms can be set in side steps 37 a . Side steps 37 a are formed in the outer surface of lip 16 to have the same construction as side steps 142 described above for shroud 102 . Shroud 102 a is formed with asymmetrical side steps or recesses 142 a , 142 a ′ to accommodate turning of spool 108 a when placing lower arms 114 a into side steps 37 a ( FIGS. 12 , 14 and 15 ). Specifically, step 142 a preferably has a longer axial shape than step 142 a ′, and no stop, to accommodate the swinging of the front upper lateral support 112 a (during installation) into step 142 a . Step 142 a ′ has a bearing surface and stop essentially the same as steps 142 .
Other modifications can also be made to the lip, lock or wear member. As examples only, the lower leg of the wear member can be extended and provided with a recess(s) for receiving the lower arm(s) or the spool instead of the lip structure ( FIG. 18 ), such as in U.S. Patent Application Publication No. 2004/0216334, which is incorporated herein by reference. The shapes of the upper and lower spool supports along with the configuration of the bearing surfaces and stops could be altered. A hammered wedge could be used with a spool in accordance with the present invention instead of a rotating wedge. A wedge driven by a separate screw member or composed of multiple parts that apply an expansion force could also be used with a spool utilizing the novel lateral arms. Additionally, various inserts (such as between the front wall of the hole in the lip and the wedge) could be included in the through-holes to improve the locking or wear of the assembly.
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In a wear assembly for securing wear members to excavating equipment, a spool is used with a wedge to hold the wear member in place. The spool is formed with at least one laterally extending arm at its upper end in lieu of an axial arm such as used in a conventional C-shaped spool. In this way, the spool can be easily supported in the assembly as the wedge is installed. The spool does not fall through the opening and no special care is needed to prevent it from falling. The spool also holds itself in place when the wedge is driven into the passage. As a result, installation of the wear assembly is easier and less hazardous. In addition, the lateral support reduces the risk that the spool will suffer spreading.
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BACKGROUND OF THE INVENTION
This invention relates generally to a means for supporting a limb of a person receiving medical treatment. More particularly, the present invention provides a medical support board that inhibits movement of a patient's limb. Two specific applications of the medical support board, and not limiting ones, is as a support to inhibit movement of a patient's limb while receiving an intravenous medicament or during defibrillation. A general application, and again not a limiting one, is for emergency situations wherein the medical support board can be rapidly attached and detached and is removably adherable to materials underlying the support board to inhibit movement of the patient's limb. The underlying materials may be carpets, blankets, the patient's clothing or the like.
In emergency situations, such as those that face emergency personnel, for example, members of a rescue squad, there is a need for a medical support board that is convenient for use in a variety of circumstances. The variety of circumstances that can face emergency personnel are too numerous to list or even imagine but the following are illustrative:
a. A patient requiring an intravenous medicament thus requiring the elbow joint, forearm and/or wrist and hand being rigidly supported;
b. A patient requiring transportation to a medical facility and requiring the limb to be stabilized relative to the body;
c. A multiple injury incident wherein a plurality of injured persons require rapid and effective treatment; and
d. A situation wherein a person may be unconscious, disorderly or violent, uncooperative, or requires cardioversion or defibrillation during cardiac arrest. These circumstances are but a few of the variety that can face emergency personnel; however, it can be seen from these few circumstances that the following are minimum requirements for the medical support board:
a. Because of the limited storage space on typical rescue vehicles there is a requirement for a multi-purpose device that can be used for as many situations as possible and can be disassembled for storage in as limited a space as possible;
b. Because of the emergency situation the device must be capable of being attached and detached rapidly and effectively;
c. Because of the possibility of having to treat more than one person it is necessary that the device be effectively attached and remain attached securely while the attendant is attending another person;
d. Because of the necessity of transporting a patient to a hospital or other facility the device must be capable of being secured so that the limb will be stabilized relative to the body;
e. Because there are situations wherein the patient is violent, disorderly or needs defibrillation the device needs to be capable of being rapidly and securely attached to a stationary surface to prevent the arm from moving and dislodging the I.V. or to further prevent aggravation of an injury.
f. Because there are situations wherein an injury may require a plurality of straps placed in a variety of locations on the limb the device must be capable of having a plurality of straps attachable anywhere on the device.
The prior art discloses boards and strap assembles in various configurations, however, none of them meet the minimum requirements for those devices.
SUMMARY OF THE INVENTION
The present invention overcomes the disadvantages of prior support boards by providing a medical support board and strap assembly that can be rapidly attached and detached, is easily disassembled for storage in a small area and is further attachable to underlying material to inhibit movement of the limb relative to the body. There is provided a rigid support board and a plurality of straps to tightly encircle the limb and the support board. The support board is padded on the side that is disposed next to the limb while the opposite side is provided with a strip of adherent or adhesive material which may extend along the length of the board. The straps are of a sufficient length to encircle and overlap and injured person's limb and the support board. The straps are constructed with adherent material placed on both sides of the strap so that when overlapped the overlapped sections adhere to each other.
Accordingly, an object of the present invention is the provision of a medical support board that is adherable to a material underlying the board to inhibit movement of the board and limb relative to the body of the patient.
Another object of the present invention is the provision of a medical support board and strap assembly that can be rapidly attached and detached to and from the material underlying the board and from the patient's limb.
A further object of the present invention is the provision of a medical support board and strap assembly having a plurality of straps removably attachable to the support board at any position on the board and is thus adaptable for a variety of uses.
Still another object of the present invention is the provision of a medical support board and strap assembly that is simple and thus inexpensive and which is easily disassembled for compact storage.
Other objects, advantages and novel features of the present invention will become apparent from the following detailed description of the invention in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a pictorial view of the present invention securing a persons arm to the board and the board adhering to an underlying material.
FIG. 2 is a bottom view of the support board showing two straps in an open position.
FIG. 3 is a top view of the support board showing the board and two straps, one of which is unattached from the board.
FIG. 4 is a pictorial view of an alternate use of the present invention.
FIG. 5 is a cross sectional view of the support board.
FIG. 6 shows the present invention disassembled and connected together for storage.
FIG. 7 shows two boards constructed according to the present invention used as a splint.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The medical support board and strap assembly of the present invention will now be described in connection with FIGS. 1 through 6. FIG. 1 is a pictorial view of the present invention with a person's arm supported thereon. The arm is held on the support board 10 by straps 12 and 14. It is noted that while the description hereinafter discusses the use of the present invention in relation to an arm however, legs are also applicable. It is also noted that throughout this description only two straps will be shown, however, it is understood that more than two straps can be used and may be necessary in certain situations. FIGS. 1 and 4 show the concept of the support board adhering to a cloth or fabric material 16 underlying the board, which may be a carpet, a blanket, clothing of the patient, etc., these materials being susceptible of adhering to the adhering material 18 employed in the present invention. Any adherent material may be used, however, the preferable type of adherent material is materially commonly known as hook material. Hook material, which is manufactured by several manufacturers, is sometimes known as Velcro material, after the name of one of its manufacturers, Velcro Manufacturing Co. This material is known and described, for example, in U.S. Pat. No. 3,640,273, which issued Feb. 8, 1972 to Tommy D. Ray. Strip 18 on the bottom side 20 of board 10 is the monofilament type hooks of the "Velcro" fastener. These monofilament type hooks adhere to cloth or fabric materials such as carpets, blankets, clothing, etc., that in most instances are disposed beneath or on a patient.
The straps 12 and 14 are made of any strong flexible material, such as a woven synthetic type material such as that used for seatbelts. The straps 12 and 14 are also provided with a "Velcro" fastener. The outwardly facing sides 22 and 24 of the straps 12 and 14 are provided with the monofilament hooks of the "Velcro" fastener. The inwardly facing sides 26 and 28 of the straps 12 and 14 are provided with the "Velcro" type pad. The inwardly facing sides 26 and 28 may have the "Velcro" type pad attached the entire length of straps 12 and 14 or any intermediate length. A preferable embodiment is shown in FIG. 5 wherein the adherent material does not extend the length of the straps 12 and 14. A space 27 is provided, free of adherent material to allow the board 10 to be easily adjustable on the patient's limb. The principal purpose of the inwardly facing strips 26 and 28 is to provide an adherent "Velcro" type pad to adhere to the monofilament "Velcro" type hooks disposed on the overlapping outwardly facing sides 22 and 24 of straps 12 and 14 respectively. As can be seen from FIG. 2, the outwardly facing sides 22 and 24 being provided with the monofilament "Velcro" type hooks add to the adhering strength of the adhering strip 18 disposed on board 10 by providing additional area of monofilament "Velcro" type hooks that are adherable to an underlying material 17.
FIG. 3 shows the concept of the easy removal of the straps 12 and 14. The straps being easily detached and attached can be disposed at any position on the board 10 and any number of straps may be disposed, limited of course to the available area provided by the length of the board 10 and the width of the straps.
FIG. 4 shows the medical support board being used as an arm restraint for the application of an intravenous medicament. The board 10 is shown with an underlying material 16 to which the adherent strip 18 FIG. 2 is adhered. As can be seen from FIGS. 2, 3 and 4 and a consideration of an emergency situation, such as a heart attack where time is of the essence, the board 10 has major advantages and is used as follows: The board 10 with straps attached as in FIG. 2 can be placed upon a surface 16 to which it will adhere and the patient's arm placed thereon and the straps 12 and 14 rapidly secured. The I.V. 30 is then administered and taped by a strip of tape 32, all within a matter of seconds. The attendant can then move on to further treatment procedures, for example, defibrillation. The application of the high voltage pulse in defibrillation procedures causes the limbs of even an unconscious patient to spasm violently. Because of the high voltage, the attendants do not hold the limbs of the person being difibrillated and this causes a danger of the I.V. being pulled out or the I.V. needle or catheter being broken off or crimped in the person's vein. By catheter is meant a flexible hollow tube usually of a plastic material in which is inserted into the patient by means of a pointed steel shank initially inserted into the tube hollow. The steel shank is thereafter withdrawn from the patient through the tube, leaving the tube, unsupported in the patient. Since the tube is flexible it is subject to crimping to which will ceast the flow of fluid. The strip 18 disposed on the underside 20 of board 10 prevents the arm being moved, either involuntarily or voluntarily by the patient. At the same time, however, the attendant can free the board 10 from the underlying material 16 rapidly by an upward motion so the patient can be transported. During transportation, the board 10 can be adhered to another material such as a blanket underlying the patient and the board or it may be adhered to the patient' s clothing.
FIG. 5 shows a cross-sectional view of the preferable embodiment of the support board. The board 10 consists of a rigid member 34 with a section of padding 38 to cushion the limb with a washable plastic covering 38 surrounding the member 34 and padding 36. The adherent strip 18 is permanently attached to the underside of board 10.
FIG. 6 shows the board 10 and straps 12 and 14 disassembled and placed in a storage condition. The adherent strips disposed on either side of the straps 12 and 14 allow the placing together of the board 10 and strips 12 and 14 for easy and compact storage. Furthermore, the monofilament "Velcro" type hooks extending from strap 14 in FIG. 6 allows the board to be stored in an easily accessible position within the rescue vehicle. For example, a strip of adherent material placed in a convenient location would hold the board 10 and straps 12 and 14 securely.
FIG. 7 illustrates the use of the support boards of the present invention as a limb splint. In the FIG. 7 embodiment, two support boards such as illustrated in FIGS. 2 and 3 herein are used with a single pan of straps 12, 14 to support a broken limb. The adherent strip on the underside of the boards function as previously described.
Thus, a new and novel medical support board is provided that is rapidly attachable and detachable is adaptable for a variety of uses and is attachable to a material underlying the injured person.
Although the invention has been described and illustrated in detail, it is to be clearly understood that the same is by way of illustration and example only and is not to be taken by way of limitation, the spirit and scope of the invention being limited only to the terms of the appended claims.
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A medical support board to inhibit movement of a patient's limb is provided. The support board is provided with an adherent strip applied to its reverse side. The adherent strip is a removably adherable to materials underlying the support board such as carpets, blankets or the clothing of the patient. The adherent strip adherring to an underlying material inhibits movement of the patient's limb relative to the body. Straps are provided to secure the limb to the support board and are fastened by means of adherent strips.
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CROSS REFERENCE TO RELATED APPLICATIONS
This invention is related to subject matter disclosed in copending U.S. application Ser. Nos. 800,635, 800,641, now U.S. Pat. No. 4,156,699, 800,644, now U.S. Pat. No. 4,165,422, 800,645, now U.S. Pat. No. 4,156,773, 800,646 now U.S. Pat. No. 4,140,675, 800,647, now U.S. Pat. No. 4,154,771, 800,648, now U.S. Pat. No. 4,156,772, 800,656, now U.S. Pat. No. 4,156,770 filed May 26, 1977, respectively; Ser. Nos. 807,990, now U.S. Pat. No. 4,156,771, 808,021, now U.S. Pat. No. 4,158,728, both filed June 20, 1977; and Ser. No. 907,589 filed May 19, 1978. All of the aforesaid applications are assigned to the assignee of this application, and all of the subject matter disclosed and referenced therein is incorporated herein in its entirety by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to linear, branched, and/or cross-linked urethane-coupled block polymers of quinone-coupled polyphenylene oxides. The polymers are prepared by contacting polyfunctional isocyanates with quinone-coupled polyphenylene oxides having an average hydroxyl group per molecule value greater than zero including 2.0 or less.
2. Description of the Prior Art
Self-condensation reactions of certain phenols employing oxygen in combination with an effective oxidative coupling catalyst system to form prior art polyphenylene oxides, i.e., polyphenylene oxides having an average hydroxyl group per molecule of 1.0 or less, are described in various U.S. patent applications including Hay's U.S. Pat. Nos. 3,306,879; 3,914,266; 4,028,341, a continuation-in-part of Ser. No. 441,295, filed Feb. 11, 1974, now abandoned; and Olander's U.S. Pat. Nos. 3,956,442; 3,965,069; 3,972,851 and 4,054,553.
Block polymers of prior art polyphenylene oxides employing simple bifunctional coupling compounds such as diacyl halides, diisocyanates, bis(haloaryl)sulfones, etc., are described in White's U.S. Pat. Nos. 3,793,564; 3,770,850; 3,809,729 and 3,875,256.
DESCRIPTION OF THE INVENTION
This invention embodies new linear, branched, and/or cross-linked urethane-coupled polymers of quinone-coupled polyphenylene oxides. The polymers are prepared by contacting polyfunctional isocyanates with quinone-coupled polyphenylene oxides having an average hydroxyl group per molecule value greater than zero including 2.0 or less.
In general, illustrative of the broad group of urethane-coupled block polymers of quinone-coupled polyphenylene oxides that are included within the scope of this invention are those described, among others, by the following model segmented polymer structures: ##STR1## The above illustrative model structures include polyfunctional quinone-coupled polyphenylene oxide units represented by --B--, polyfunctional coupling agents units represented by --Z-- and ##STR2## etc., and monofunctional polyphenylene oxide units represented by --A, which units are described in greater detail hereafter.
In general, the expression "polyfunctional polyphenylene oxides" as employed herein and in the claims includes quinone-coupled polyphenylene oxides having an average hydroxyl group per molecule greater than zero including 2.0 or less. These polyphenylene oxides--which can be prepared by the methods described in U.S. applications Ser. Nos. 800,635 and 800,646--are described by the formula (II) set out hereafter: ##STR3## wherein independently each --OEO-- is a divalent quinone residue, E is a divalent arene radical, either a or b is at least equal to 1, the sum of a plus b is preferably at least equal to 10, more preferably 40 to 170, the sum of r and s being a number average of from about 0.001 to about 2.0, and R is hydrogen, a hydrocarbon radical, a halohydrocarbon radical, a hydrocarbonoxy radical or a halohydrocarbonoxy radical. The polyfunctional polyphenylene oxide units of the block polymers can be conceptualized by the structure of formula (II) above wherein the hydrogen atoms are disassociated from the polyhydroxy groups of the quinone-coupled polyphenylene oxide, e.g. where r and s are equal to zero. When r and s are zero the difunctional radical of formula (II) can be described as a quinone-coupled polyphenoxy radical or a divalent phenoxy radical, and for brevity can be abbreviated as a polymer segment of the formula --B--.
In general, the expression "monofunctional polyphenylene oxides" as employed herein and in the claims includes polyphenylene oxides having an average hydroxyl group per molecule value greater than zero including 1.0 less. These polyphenylene oxides--which can be prepared by any of the methods of the prior art--are described by formula (III) set out hereafter: ##STR4## wherein independently each R is the same as in formula (II) above, n is a number of at least 1, preferably 10, and more preferably 40 to 170, and m being a number average of from 0.001 to about 1.0. The monofunctional polyphenylene oxide units of the block polymers can be conceptualized by the structure of formula (III) above wherein the hydrogen atom is disassociated from the monohydroxy group of the polyphenylene oxide, e.g. where m is zero. When m is zero, the difunctional radical of formula (III) can be described as a phenoxy radical or a monovalent phenoxy residue, and for brevity can be abbreviated as a polymer segment of the formula --A.
In general, the expression "polyfunctional coupling agent" as employed herein and in the claims includes any polyfunctional isocyanate having at least two isocyanate coupling reaction sites. The term "polyfunctional isocyanate" includes, among others, any di- or tri-functional isocyanates illustrated by the formula:
R"--(NCO).sub.c, (IV)
where c is a number at least equal to 2, and R" is C 2-8 alkylene, e.g., ethylene, propylene, isopropylene, the various isomeric butylenes, the various isomeric pentylenes, the various isomeric hexylenes (including cyclohexylenes) the isomeric heptylenes, the isomeric octylenes, phenylene, biphenylene, i.e., ##STR5## e.g., 2,2'-, 2,3'-, 2,4'-, 3,3'-, 3,4'- and 4,4'- biphenylene; bis(phenylene)-C 1-8 alkane, i.e., ##STR6## where R a is C 1-8 alkylene or alkylidene, e.g., methylene, ethylidene, isopropylidene, butylidene, etc. and the various other examples given above for R"; biphenylene oxide, i.e., ##STR7## poly (C 2-8 oxyalkylene), having an average of 2 to 10 repeating units, i.e., --(R b --O) p where p is 2-10 and R b is alkylene, examples of which are given above for R", and the above-mentioned groups containing a phenylene or biphenylene group, e.g., the various phenylenes, biphenylenes, bis(phenylene)-C 1-8 alkanes, and (biphenylene) oxides, wherein, one up to the total number of aromatic hydrogens have been replaced with halogen, preferably chlorine, and/or C 1-8 groups.
Illustrative of specific examples of a portion of presently preferred polyfunctional isocyanates that can be employed are:
polymethylene diisocyanates, e.g.,
ethylene diisocyanate,
trimethylene diisocyanate,
tetramethylene diisocyanate,
hexamethylene diisocyanate,
octamethylene diisocyanate, etc.;
alkylene diisocyanates e.g.,
propylene-1,2-diisocyanate,
butylene-1,2-diisocyanate,
butylene-1,3-diisocyanate,
butylene-2,3-diisocyanate, etc.;
alkylidene diisocyanates, e.g.,
ethylidene diisocyanate,
propylidene diisocyanate,
isopropylidene diisocyanate, etc.;
cycloalkylene diisocyanates, e.g.,
cyclopentylene-1,3-diisocyanate,
cyclohexylene-1,2-diisocyanate,
cyclohexylene-1,3-diisocyanate,
cyclohexylene-1,4-diisocyanate, etc.;
aromatic diisocyanates, e.g.,
o-phenylene diisocyanate,
m-phenylene diisocyanate,
p-phenylene diisocyanate,
1-chloro-2,4-phenylene diisocyanate,
4-chloro-1,3-phenylene diisocyanate,
4,6-dichloro-1,3-phenylene diisocyanate,
2,4,6-tribromo-1,3-phenylene diisocyanate,
2,4,6-trichloro-1,3-phenylene diisocyanate,
tetrachloro-1,3-phenylene diisocyanate,
methylene-4,4'-bis(phenyl isocyanate),
2,4-tolylene diisocyanate,
2,6-tolylene diisocyanate,
3,3'-dimethyl-4,4'-biphenylene diisocyanate,
methylene-4,4'-bis(2-methylphenyl isocyanate),
2,2', 5,5'-tetramethyl-4,4'-biphenylene diisocyanate,
1-chloro-2,4-phenylene diisocyanate,
4chloro-1,3-phenylene diisocyanate,
4,6-dichloro-1,3-phenylene diisocyanate,
2,4,6-tribromo-1,3-phenylene diisocyanate,
2,4,6-trichloro-1,3-phenylene diisocyanate,
tetrachloro-1,3-phenylene diisocyanate, etc.
The polyfunctional isocyanate coupling agent residue of the polymers can be conceptualized by the structure ##STR8## wherein c is a number equal to 2 or 3, etc., R" being as defined above, and for brevity can be abbreviated in the polymer models in FIG. I as a polymer segment of the formulas --Z--, or ##STR9## etc.
In general, the process of preparing urethane-coupled block polymers of quinone-coupled polyphenylene oxides comprises contacting polyfunctional polyphenylene oxides and polyfunctional coupling agents in the presence of an aqueous solution of a water soluble base and a catalytic phase transfer agent. Any amount of functional (reactive) polyphenylene oxide and coupling agent can be employed, e.g. from 1/1000 to 1000 times the stoichiometric requirements required to couple all of the reactive polyphenylene oxide.
Any water soluble base can be employed, however preferably is an aqueous solution of a water soluble base, e.g. an aqueous alkaline metal or alkaline earth metal hydroxide or carbonate solution. Specific examples include aqueous solutions of potassium hydroxide, sodium hydroxide, sodium monocarbonate, barium carbonate, etc. Any amount of water soluble base (WSB) can be employed. Generally effective mole proportions of WSB relative to the amount of coupling agent that are employed are coupling agent:water soluble base proportions of from about 1:100 to about 50:1 and more frequently from about 1:10 to about 10:1.
Any catalytic phase transfer agent can be employed, however, preferably is a phase transfer agent selected from the group consisting of quaternary ammonium, quaternary phosphonium, and tertiary sulfonium compounds or mixtures thereof. These catalytic phase transfer agents can be described by the formulas: ##STR10## wherein each R' is independently selected from aliphatic hydrocarbon radicals having from about 1 to about 30 carbon atoms, preferably from about 2 to about 15 carbon atoms, each X - is selected from the group consisting of Cl - , Br - , F - , CH 3 SO 3 - , CH 3 CO 2 - , CF 3 CO 2 - or OH - , and each Y -- is selected from the group consisting of SO 4 -- , CO 3 -- , or C 2 O 4 -- . Any amount of catalytic phase transfer agent (PTA) can be employed, however generally effective molar proportions of PTA relative to the amount of water soluble base are within the range of from about 1:10 to about 1:1000 and more frequently within the range of from 1:100 to 1:1000.
The coupling reactions can be carried out at any temperature. Preferably temperatures within the range of from 0° to 150° C. or even higher, and more preferably from 50° C. to 100° are employed.
In order that those skilled in the art may better understand my invention, the following example is given which is illustrative of the best mode of practicing my invention.
EXAMPLE I
(A) Polymer Preparation, and (B) Catalyst Deactivation
A 2.5 gallon stainless steel reactor equipped with an air-driven paddle stirrer, oxygen inlet tube, and water-cooled coil and jacket was charged with 150 g. 2,6-xylenol, 2.3 liters of toluene. 1.5 g. of Adogen® 464, i.e. trialkyl(C 8-10 )methyl ammonium chloride, 3.4 g. N,N'-di-t-butylethylenediamine (DBEDA), 47.5 g. dimethyl-n-butylamine (DMBA), 15 g. di-n-butylamine (DBA), and 4.2 ml. of a catalyst stock solution formed by dissolving 19.30 g. of cuprous oxide in 500 ml. of a chilled 47.2% aqueous hydrobromic acid solution. Oxygen was bubbled through the reaction medium at a rate of 8.3 moles per hour and the mixture was stirred vigorously. 1350 g. of 2.6-xylenol in 1.5 liters of toluene was pumped into the reactor while the reaction temperature was maintained at 25°±1° C. over a 30-minute period. The temperature was then allowed to rise to 35°±1° C. After the desired reaction product viscosity was obtained the reactor was purged of oxygen by passing nitrogen instead of oxygen through the reaction medium and a 38% aqueous solution of a trisodium salt of EDTA, i.e. ethylenediamine tetraacetic acid was added to deactivate the catalyst system. Summarily, the reaction parameters relative to molar ratios of 2,6-xylenol: Cu:DBEDA:DMBA:Br:DBA were as follows: 1124:1:1:8:43:3.2:10.5.
______________________________________Summary of Reaction Parameters andProperties of Poly(2,6-dimethyl-1,4-phenylene oxide) React. React. OHRun TMDQ Temp. Time [η] Absorbance GPCNo. (%) (°C.) (min.) (dl./g.) @3610cm.sup.-1 --M.sub.w /--M.sub.n______________________________________1 0.91 25-35 103 0.37 0.182 --______________________________________
(C) Quinone Coupling
The reaction mixture as described in sections (A) and (B) above with a steady nitrogen sweep was heated to 50° C. and maintained at 50°-55° C. until the deep orange TMDQ color disappeared leaving a very light green solution. Methanol was added to the reaction mixture to precipitate the polymer. The polymer was collected on a filter, washed with methanol, and dried in a circulating air oven at 90° C.
______________________________________Summary of Reaction Parameters andProperties ofQuinone-Coupled Poly(2,6-dimethyl-1,4-phenylene oxide) React. React. OHRun TMDQ Temp. Time [η] Absorbance GPCNo. (%) (°C.) (min.) (dl./g.) @3610cm.sup.-1 --M.sub.w /--M.sub.n______________________________________1 <0.001 50-55 ˜90 0.31 0.301 3.43______________________________________
(D) Coupling With Toluene 2,4-Diisocyanate
A solution containing 10 g. of quinone-coupled polyphenylene oxide prepared as in part (C) above and 30 ml. monochlorobenzene was added to a 300 ml. Waring blender, kept under a nitrogen atmosphere and contacted with 0.5% Adogen® 464 and 1.3 ml. of a 50% aqueous sodium hydroxide solution. The mixture was stirred in the blender at maximum speed (high fluid shear stress reaction conditions) and 0.19 g. of toluene 2,4-diisocyanate was added over a four minute period. Stirring was continued an additional 2-3 minutes. Toluene was added and the polymer was precipitated by acidification with concentrated HCl and the addition of methanol. The polymer was filtered and dried in vacuo at 60° C. overnight.
The intrinsic viscosity of the polymer before coupling was 0.31 dl./g. and after coupling was 0.47 dl./g.
The diisocyanate coupled quinone-coupled polyphenylene oxide phenolic hydroxyl absorbance at 3610 cm. -1 (in carbon disulfide) was 0.026 absorbance units for a 2.5% solution in a 1.0 cm. cell.
As illustrated by the foregoing example, polyfunctional isocyanates can be reacted with quinone-coupled polyphenylene oxides under widely varying reaction conditions to form urethane-coupled quinone-coupled polyphenylene oxides. Preferred urethane coupled polymers prepared in accordance with our process are linear polymers wherein the polymers are essentially linear polymers and more preferably are essentially linear polymers wherein all available hydroxyl components have been end-capped so that the hydroxyl content of the resulting polymer is essentially nil.
The urethane-coupled quinone-coupled polyphenylene oxides of our process can have any intrinsic viscosity and any weight average molecular weight M w . Presently preferred polymers of our process generally have an M w value of 10,000 to 120,000, more preferably 30,000 to 60,000, having generally corresponding intrinsic viscosities of 0.17 to 1.7, and 0.4 to 0.7, respectively.
The polymers of this invention can be combined with other fillers, modifying agents, etc., such as dyes, pigments, stabilizers, flame retardant additives with beneficial results.
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Linear, branched and/or cross-linked urethane-coupled block polymers of quinone-coupled polyphenylene oxides are described. The polymers are prepared by contacting polyfunctional isocyanates with quinone-coupled polyphenylene oxides having an average hydroxyl group per molecule value greater than zero including 2.0 or less. The polymers either alone or in combination with other polymers can be formed into useful articles of manufacture by conventional molding, extruding, etc., processing techniques.
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FIELD OF THE INVENTION
The present invention is generally directed to food processors and particularly to a novel hand-held food processor for cutting, slicing, shredding or grating of food, such as vegetables, fruits and cheeses containing novel foodcutting devices and to a consumer and/or commercial product containing the same.
BACKGROUND OF THE INVENTION
In many households, the use of knives and graters to cut, slice, grate and shred food has become obsolute over the last 15 years. Full-size food processors have provided a viable alternative to manual food preparation. Food processors have been an effective means of reducing the time needed to perform such foodcutting operations.
However, full size processors have fallen out of favor with consumers for several reasons. They are complicated, combersome, difficult to clean and, as a result, the full-size food processor has been relegated to infrequent use.
More recently, so-called mini-processors have been developed to overcome the deficiencies of their predecessors and to reclaim the shrinking food processor market. Such devices have been scaled down in size and reduced in cost. While they are somewhat easier to use, and less cumbersome, they are not substantially easier to set-up or clean and have therefore not satisfied the needs of the marketplace.
Of critical importance to the enduring success of a food processor is that it must possess the simplicity, convenience and stand-by readiness of a knife along with the speed, accuracy and versatility of a multi-purpose cutter. In addition, it must be easier to store and easier to clean than ordinary food processors.
Applicants have developed a food processor which can readily be held in the hand and moved to any desired location in an efficient manner. In addition, the food processor, in a preferred form of the invention, has a self-contained power supply that makes it portable. The food processor of the present invention includes novel cutting blade assemblies which make accurate cuts of food and are easy to load and clean.
It is therefore an object of the invention to provide a hand-held food processor which is easy to operate and easy to use and clean.
It is another object of the preferred form of the invention to provide a food processor which has a self-contained power source and which is therefore not dependent on being connected to an electrical outlet during operation.
It is a further object of the invention to provide novel cutting devices which are easily inserted into the food processor and which efficiently cut and eject food from the food processor.
It is a still further object of the invention to provide a consumer kit containing the food processor and cutting devices in a surface mountable storage unit.
SUMMARY OF THE INVENTION
The present invention is directed to a hand-held food processor for cutting, slicing, shredding or grating of food, such as vegetables, fruits and cheeses which includes a power supply means which is preferably contained solely within the food processor to enable operation without having the food processor attached to an electrical outlet during operation.
The food processor also includes a food cutting means which is operatively connected to the power supply means and a food delivery means which is operatively connected to the food cutting means for conveying uncut food to the food cutting means.
In a preferred form of the invention, the food cutting means has an arcuate cross-sectional shape which is at least partially rotatable in at least one direction about an axis. It includes at least one arcuate blade section positioned about the axis of rotation. In a preferred form of the invention, there are provided at least two arcuate blade sections eccentrically positioned about the axis of rotation.
Each blade section has a guiding or non-cutting edge and a cutting edge such that the guiding edge of one blade section and the cutting edge of a contiguous blade section define a cutting zone.
The guiding edge acts to position the food to be cut and is spaced apart from the corresponding cutting edge of the cutting zone a distance which corresponds to the thickness of the desired cut.
The unique geometry of the blade section, especially the cutting edge, allows the cut or excised portion of the food product to easily move along the arcuate interior surface of the cutting edge blade section during rotation of the cutting device. As a result, the cutting edge is easily able to slide entirely through the food product without fracturing or splitting the food product.
The food processor also includes food delivery means which is preferably in the form of a tube or chute which can be easily loaded with food to be cut at a location remote from the cutting edge. Preferably the food containing means are retained in a correspondingly shaped portion of the food processor and preferably movable collar means are provided which facilitate releasably retaining the food cutting means in the food processor.
The food processor kit of the present invention includes a surface-mountable (e.g. wall mountable) case which comprises a first section for housing the food processor and a second, adjacent section for housing at least one cutting device which is removably insertable into the food processor. The typical food processor kit may include a plurality of cutting devices for cutting thin slices, thick slices and crinkle cuts (e.g. for french fries), section cut slices, as well as cutting devices which grate and shred. The kit is provided with spaced-apart cavities for housing the respective cutting devices in the second section.
The kit is also provided with a lid hinged at one end for covering the second section. The inside surface of the lid may be provided with at least one food preparation means adapted to divide a bulky food, such as a potato, into smaller portions which are readily insertable into the food delivery section of the food processor.
In a preferred form of the invention, the food preparation means comprises a frame and an array of cutting edges connected between portions of the frame. The cutting edges define a plurality of open-ended chambers. When the cutting edges are forced against the bulky food product or vice versa, the food product is divided into sections which move through the open-ended chambers creating a plurality of elongated food portions of a desired cross-sectional dimension which can then be inserted into the food delivery means.
In operation, the food processor is removed from the kit and a suitable cutting means (slicer, grate, etc) inserted into the food cutting chamber. The cutter is secured in place preferably by a collar means releasably secured to the front end of the chamberr remote from the end of the chamber in which the cutting means is releasably secured to the rotation means of the motor.
A bulky food product such as a carrot is inserted into the food delivery means and then the food processor is actuated by depressing a momentary switch on the housing or vice versa. The carrot is cut and ejected out of the opening in the front end of the chamber into a bowl, receptacle, or onto a surface as desired.
BRIEF DESCRIPTION OF THE DRAWINGS
The folowing drawings in which like reference characters indicate like parts are illustrative of embodiments of the invention and are not intended to limit the invention as encompassed by the claims of the application.
FIG. 1 is a top plan view of the food processor kit showing the food processor in the first section and a lid in the closed position covering the second section;
FIG. 2 is a top plan view of the food processor kit of FIG. 1 showing the lid in the open position exposing the second section for housing the cutting devices and showing food preparation devices on the interior surface of the lid;
FIG. 3 is a side view of the food processor kit shown in FIG. 2;
FIG. 4 is a side view of the food processor of the invention ready for use with a schematic representation of the power supply means and cutting means;
FIG. 5 is a top plan view of the food processor shown in FIG. 4;
FIG. 6 is a detailed cross-sectional view of the food processor shown in FIG. 4;
FIG. 6A is a cross-sectional view taken through line A--A of FIG. 6;
FIG. 6B is a cross-sectional view taken through line B--B of FIG. 6;
FIG. 7 is a plan view of one bayonet attachment device for attaching the collar to the food cutting chamber shown in FIG. 6B;
FIG. 8 is an enlarged cross-sectional view of the bearing means between the collar and cutting device.
FIG. 9 is a side view of the cutting device with a schematic representation of the means by which the cutting device is connected to the rotation means of the power supply means;
FIG. 10 is an enlarged cross-sectional view of the means of bearing the cutting device against the power supply means;
FIG. 11 is a side view of the food processor of FIG. 4 with electrical means for connection to an electrical outlet;
FIGS. 12A-12E are respective views of embodiments of the cutting devices of the present invention;
FIGS. 13A-13C are cross-sectional views showing in sequence how a food product is sliced using the cutting device shown in FIG. 12A.
FIGS. 14A through 14C are cross-sectional views showing in sequence how a food product is sliced using a known cutting device.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawings and first to FIGS. 1-3, the food processor kit 2 of the present invention includes a case 4 having a first section 6 for housing a food processor 8 and a second section 10 for storing at least one cutting device 12 which also constitutes part of the present invention.
The case 4 has attached at one end 14 a lid 16 by hinges 18 or other conventional attachment means. The lid 16 is movable from a closed position shown in FIG. 1, covering the second section 10 of the case 4, to an open position shown in FIG. 2 exposing the second section 10 and the interior surface 20 of the lid 16. The lid 16 may be secured in the closed position by press fitting a pair of projections 13 into corresponding slots 15.
The case 4 may be provided with openings 32 for mounting the case 4 on a flat surface such as a wall. When the case 4 is opened and the lid 16 is moved to expose the second section 10, the wall-mounted case 4 will have the appearance shown in FIG. 2.
The food processor 8 is stored in the first section 6 of the case 4 within a cavity 22 shown in FIG. 3. The food processor 8 is held in the cavity 22 by a conventional bracket 24 and by a conventional bracket 33. The bracket 24 may be provided with conventional contacts 26 and an outlet mounted transformer (not shown) to recharge the batteries to provide for the recharging of the power supply unit. In addition, there may be provided an L.E.D. 28 for indicating when the food processor 8 is in the recharging mode.
The second section 10 of the case 4 may be provided with at least one cavity 30 for storing the cutting devices 12. The cavities 30 have a shape complimentary to the shape of the cutting device 12, as for example, a conical shape as shown in FIG. 3. Each cavity 30 may be provided with a plurality of projections 34 and slots 36 for securing a corresponding portion of the frame 42 of the cutting devices 12.
The interior surface 20 of the lid 16 is adapted to store at least one food preparation device 40 which is employed to reduce the width of uncut foods into portions which are readily insertable into the food delivery means of the food processor 8.
The food preparation device 40 shown in FIG. 2 is readily suited for sectioning bulky foods that are relatively stable on a flat surface such as a table (e.g. a potato). The device 40a is particularly suited for bulky foods that tend to move or are unstable on a flat surface (e.g. a cucumber). The devices 40 and 40a include a frame 43 and an array of cutting edges 44 which form a plurality of open-ended chambers 46. Each of the chambers 46 has a maximum cross-sectional dimension less than the cross-sectional dimension of the interior surface of the food delivery means. The food preparation device 40a is preferably provided with centrally positioned cutting edges 48 which may be larger than the cutting edges 44.
In operation, the food preparation device 40 is placed upon a bulky food product which is stable on a flat surface (e.g. a potato) and forced downward so that the cutting edges 44 make a complete cut through the potato dividing the potato into a plurality of elongated spears corresponding to the shape of the chambers 46.
The device 40a is used for bulky foods which are unstable on a flat surface (e.g. a cucumber). The cucumber is placed upon the sharpened edges of the device 40a and forced downward so that one end of the cucumber is partially cut and engaged by the centrally positioned cutting edges 48. The device 40a is then turned over and pressed downward until the cutting edges 44 and 48 cut entirely through the cucumber producing a plurality of spears.
Each of the spears produced by the devices 40 and 40a has a maximum cross-sectional dimension less than the cross-sectional interior dimension of the food delivery means of the food processor 8. The spears are then ready to be inserted into the food delivery means and cut, sliced, grated or shred depending on the particular cutting device 12 which is inserted and secured within the food processor 8.
The food preparation devices 40 and 40a are held in the lid 16 by conventional brackets 50 as shown in FIG. 3.
Referring to FIGS. 4-6A, the food processor 8 of the present invention includes a substantially cylindrical housing 52 which is adapted to be comfortably held by the hand of the user. The housing 52 encases a power supply means 54 which is operated by a switch 56 (e.g. a momentary switch). One end 53 of the housing 52 opens into the rear end 58 of a food cutting chamber 60 in which is secured one of the cutting devices 12 having one or more cutting edges 114 as shown in FIG. 4.
The chamber 60 is conical in cross section and tapers outwardly, and has an opening 62 intermediate its end for receiving uncut food through a food deliver means 64. Rotation of the correspondingly conically shaped cutting device 12 within the chamber 60, as illustrated in FIG. 4, causes each cutting edge 114 of the device 12, as hereinafter more fully explained, to completely cut through a portion of the uncut food to produce the desired slices, cuts, etc. The slices of food exit out of the larger open end 66 of the chamber 60. The cutting device 12 is secured within the chamber 60 by a collar 65 which is removably attached to the food processor 8 at the end of the chamber 66.
The food processor 8 has a power supply means 54 which preferably operates on rechargeable batteries. The rechargeable or so-called "cordless" embodiment of the invention enables the user to operate the food processor 8 in any desired location without interference from a permanent electrical outlet cord. However, the present invention is also readily adaptable to the use of a permanent outlet cord.
As shown in FIGS. 6 and 6A, the cordless embodiment has a power supply means 54 which includes rechargeable batteries 68, recharging contacts 70, a motor 72, a gear reduction device 74 and a drive gear means 76 which is adapted to engage and rotate the cutting device 12 within the chamber 60.
The batteries 68 are the standard rechargeable type (e.g. AA standard charge rated 0.5 A/hr) each having a voltage rating of, for example, 1.2 volts. Typically four such batteries 68 are employed. The rear of the housing 55 is provided with an L.E.D. contact 28 which provides a conductive bridge between the recharge contacts 70 and the batteries 68 when the batteries 68 are being recharged in the case 4 through charge terminals 26 and transformer (not shown).
The batteries 68 are connected to the motor 72 which rotates a spindle 78. The motor 72 converts electrical power into a mechanical force for rotating the cutting device 12 via a spindle 80. The motor 72 may be selected from standard motors such as, for example, a Johnson HC 610 G/6337. The speed at which the spindle 80 rotates in most cases is reduced by a planetary gear reducer 74, typically having a 33:1 reduction capacity. The gear reducer 74 has the spindle 80 connected to a hub 82 which is adapted to removably attach to the rear end of the cutting device 12 as seen in FIG. 6.
The power supply means 54 can be adapted to provide a clockwise or counterclockwise rotational movement, or an oscillating or reciprocating linear movement through the use, for example, of a cam means (not shown) positioned between the gear reducer 74 and the cutting device 12.
Between the gear reducer 74 and the cutting device 12 and positioned in the rear end 58 of the chamber 60 is a bearing means 84 for locating one end of the cutting device 12 in the chamber 60 and which also acts as a water resistant seal for the power supply means 54. As shown in FIGS. 6 and 10, the bearing means 84 has an extension 86 which allows the end 87 of the cutting device 12 to be aligned in place via projections 89.
The collar 65 in the illustrative embodiment is releasably secured within the opposed open end 66 of the chamber 60. The collar 65 has at least one notch 88 which is removably engaged by a corresponding projection 90 on the inner surface of the chamber 60. The collar 65 can therefore be easily press-fitted into place about the open end 66 of the chamber 60 by inserting the projection 90 into the notch 88 and rotating the collar as shown in FIG. 7. The collar 65 is prevented from being loosened by the rotation of the cutting device 12.
As shown in FIG. 6B, a preferred embodiment of the invention employs three notch 88/projection 90 pairs, the first located at the top of the open end 66 of the chamber 60 and the second and third pairs spaced around the periphery of the open end 66. The distance between the first pair and either of the second and third pairs being dimensioned differently than the distance between the second and third pairs of notches 88/projections 90. This arrangement is preferred so that the collar 65 is always in proper orientation when placed over the open end 66 of the chamber 60.
The collar 65 is also provided with a curvilinear bearing face 92 which serves to locate the collar 65 against the cutting device 12 while allowing the cutting device 12 to freely rotate during cutting operations. As shown in FIG. 8 the bearing face 92 has a curvilinear cross-section which provides a fixed position and guidance for the end of the cutting device 12.
The food delivery means 64 as shown best in FIG. 6 includes an open ended tube or chute 94 rigidly affixed to the food cutting chamber 60. The angle of the chute 94 with respect to the surface of the cutting device 12 may be more or less than 90° but is preferably about 90° for most cutting applications. Preferably the length of the chute 94 exceeds the length of the fingers for safety reasons. The chute 94 has a top open end 96 and a bottom open end 98 which provides a pathway for movement of uncut food into the food cutting chamber 60. By the practice of this invention described herein, food is pulled downward by the arcuate blade construction and conically shaped curling device 12 resulting in a self feeding of the food into the chamber 60. Food which does not readily move down the chute 94 may be urged downward by exerting pressure thereon with a plunger 100. The plunger 100 has a cross-sectional dimension slightly less than the interior cross-sectional dimension of the cute 94 so that its movement within the chute 94 is unimpeded.
The plunger 100 has a flat bottom end 102 which contacts and forces the uncut food downward into the food cutting chamber 60. The opposed end 104 of the plunger 100 is provided with a suitable hand gripping surface 106.
Referring to FIGS. 6, 9, and 12A-12E, the cutting device 12 constituting a part of the present invention, preferably includes a frame 42 comprising opposed frame sections 108 and 110 having attached therebetween at least one blade section 112 which is either integral or mounted to the frame sections 108 and 110 in a customary manner. The frame sections 108 and 110 can be made out of rigid plastic or can be made of stainless steel as with the blade section 112. In the latter embodiment the cutting device 12 can be made as a single piece construction. As illustrated the cutting device 12 is conical in cross section and tapered outwardly from the frame section 108 to the frame section 110.
The cutting device 12 is rotatable within the chamber 60 and about a central axis A as shown in FIG. 9 by engagement with and the movement of the hub 82. In a preferred form of the invention, a plurality of blade sections 112 are employed. Each blade section 112 has a cutting edge 114 and a remote guiding edge 116. Each blade section 112 is, preferably, eccentrically positioned about the axis A of rotation such that the guiding edge 116 of one blade section 112 and the cutting edge 114 of a contiguous blade section define a cutting zone 118 where the uncut food from the chute 94 is cut and falls into the chamber 60. As illustrated the blade sections 112 and 114 extend between and the excised preferably to the frame sections 108 and 110.
As shown in FIG. 12A the depth of cut is determined by distance "X" between the cutting edge 114 and the guiding edge 116 comprising the cutting zone 118.
As shown best in FIGS. 6 and 9 the rear frame section 108 of the cutting device 12 has a cavity 120 having a shape complimentary to the shape of hub 82. The cavity contains slots 122 which are placed between radially extending projections 124 of the hub 82 so that rotation of the hub 82 causes the cutting device 12 to rotate about axis A.
The distance "X" may be chosen in accordance with the thickness of any desired cut typically in the range of about 5 millimeters for thick slices and 2 millimeters for thin slices.
As shown specifically in FIG. 12A the cutting device 12 may be provided with cutting zones 118 capable of cutting different thicknesses. For example, the distance of X may be set at five millimeters to cut thick slices and the distance "Y" may be set at two millimeters for thin slices to produce alternating thick and thin slices.
As shown in FIG. 12B, the cutting edges 114 may be of irregular shape to produce decorative slices such as crinkle cuts. FIG. 12C shows a plurality of vertical slices of food product passing through cutting zone 118 to provide, for example, french fries. FIGS. 12D and 12E shown single blade sections 112 for grating and shredding, respectively.
The cutting devices 12 shown in FIGS. 12A-12C offer significant advantages over cutters customarily used for food processors. The unique geometry of the cutting devices 12 and particularly the smooth arcuate surface in the region proximate to the cutting edge 114 enables the blade section 112 to cut completely through the food without fracturing or splitting the uncut product.
Referring to FIGS. 13A-13C, the cutting edge 114 engages one side of the uncut food which is in the food cutting position within the chute 94. Once the initial cut is made the partially cut food makes an unimpeded pass along the interior surface of the blade section 112 thereby minimizing friction during the cut and requiring less power.
In contradistinction, prior art cutting devices shown in FIGS. 14A to 14B have non-eccentric blade sections. Only the cutting edge is raised and not the entire blade section. As a result, the top of the cut food product is forced downward as it contacts the rear portion of the cutting edge causing pressure at the cutting point (see specifically FIGS. 14B and 14C). The pressure may be of sufficient magnitude to cause the food to deform, fracture or split before the blade makes a complete pass, as well as increasing friction and requiring more power.
In use the food processor 8 is removed from the case 4, the collar 65 is removed and the desired cutting device 12 (e.g. the device of FIG. 9) is inserted into the chamber 60. The collar 65 is secured to the front of the chamber 60 causing the cutting device 12 to engage the hub 82 for rotation by the power supply means 54. Holding the food processor 8 with one hand and depressing the switch 56 activates the cutting device 12. Food may be placed in the chute 94 with the other hand and delivered to the device 12 for slicing, cutting etc., whereupon the slices tumble into the interior of the device 12 and exit from the forward end 66 of the chamber 60. When the desired amount of the food has been sliced, the switch 56 is released.
Replacing the device 12 (FIG. 9) with another device 12 (e.g FIG. 12B) is accomplished by removing the collar 65 and changing devices 12. Cleaning can be accomplished by disengaging the chamber 60 and chute 94 from the housing 52 and washing such components along with one or more devices 12 which have been removed from the chamber 60.
Other features which would be apparent to those skilled in the art and not specifically recited in the disclosure are within the scope of the present invention.
For example, the food processor 8 may be adapted for use without rechargeable batteries by replacing the batteries with an electrical connection between an outlet cord and the motor. Such a device would have the appearance of the food processor 8 shown in FIG. 11.
In addition, the switch 56 may be placed in any location of the housing 52, preferably in a place easily accessible to the user's fingers.
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A hand-holdable food processor for cutting, slicing, shredding or grating vegetables, fruit, cheese and the like. The food processor is operable in various orientations while being held by hand and has a power supply, food cutting means for cutting, slicing, shredding or grating operatively engaging the power supply and a food delivery means extending from the processor for momentary storage and feeding of food to the food cutting means. A food cutting device also is disclosed which includes one or more blade sections eccentrically positioned about the axis of a food processor.
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FIELD OF THE INVENTION
[0001] The present invention relates to a non-invasive device Nadi Tarangini useful for quantitative detection of arterial nadi pulse waveform. More particularly, the present invention relates to an apparatus for obtaining the complete spectrum of the Nadi (arterial pulse) as a time series and application of advanced machine learning algorithms to identify the pulse patterns. According to the present invention, three diaphragm-based strain gauge elements are to be placed at the exact pick up positions (known as Vata, Pitta and Kapha positions) at the root of thumb on a hand wrist, which experience the pressure exerted by the radial artery and give equivalent electrical output. Each electrical output, coupled with the excitation of the strain gauge at the transmitter, is then digitized using a digitizer, having an interface with the personal computer at the USB port. This pressure is tiny in pressure units is captured in accurate, reproducible and noise-free waveforms to perform accurate diagnosis. A very small air gap is introduced between each of the sensing elements and the skin of person for capturing the exact values. The typical physiological properties such as rhythm, self-similar nature, and chaotic nature present in the pulse are extracted using rigorous machine learning algorithms. Subsequently the six pulse waveforms obtained through our invention (three waveforms on each hand) are classified as various types and sub-types of nadi patterns, primarily defined in the Ayurvedic literature.
[0002] The system of the present invention is intended to eliminate all the human errors in the Nadi-Nidan performed manually by Ayurvedic practitioner and the diagnostics could be performed based on accurate and quantitative information. The invention could also eliminate any subjectiveness in the diagnostics.
BACKGROUND AND PRIOR ART
[0003] Ayurveda (Indian Traditional Medical science) believes that the function of entire human body is governed by three humors: Vata, Pitta and Kapha, collectively called as Tridosha. The equilibrium of these three doshas maintains the proper functioning of every aspect of physiology. Any imbalance in the proportion causes a disorder. The imbalance causes the vessels carrying the blood to contract or expand with respect to its normal position. This contraction/expansion of vessels results in modulation of blood flow, which is called as Nadi. In brief, Nadi dictates the mode of blood circulation, which no doubt is governed by the physiological state of the individual. This makes Nadi-Nidan [meaning diagnosing a disease by sensing the blood flow] as a first step and in most cases the only diagnostic tool for patient diagnosis, according to Ayurveda.
[0004] There are around 74000 locations in human body where the Nadi pulses can be obtained, out of which only two positions are in proximity. However, the standard position according to Ayurvedic practitioners is at the root of thumb on the wrist as shown in FIG. 1 . The three fingers of an Ayurvedic practitioner's hand, 1 in FIG. 1 , namely the index finger, 2 in FIG. 1 , the middle finger, 3 in FIG. 1 , and the ring finger, 4 in FIG. 1 , are placed at the root of thumb of a patient's hand, 5 in FIG. 1 , and the pulses can be sensed at the fingertip. Each finger senses Vata prakriti, 6 in FIG. 1 , Pitta prakriti, 7 in FIG. 1 , and Kapha prakriti, 8 in FIG. 1 , respectively. The general characteristics of these pulses are given in the Table 1.
[0005] All the pulses sensed at the fingertip have been traditionally further classified as Sukshma, Tikshna, Kathina and Sama as major types and Vegavati (fast), Manda (slow), Khol (deep) as few of the subtypes and their combinations. The above classification is mainly based on the excursion and pulse movements. The nature of these pulses can be expressed in terms of the parameters such as frequency, depth, power, rhythm. All these parameters are sensed at the predetermined pick-up points on each of the fingertips. Any change in these characteristics represents the kind of disorder.
[0006] Some of the previous related references include U.S. Pat. No. 6,432,060, US 20031009105, U.S. Pat. No. 6,364,842, U.S. Pat. No. 5,623,933, U.S. Pat. No. 5,755,229, U.S. Pat. No. 5,832,924, U.S. Pat. No. 5,938,618, U.S. Pat. No. 6,155,983, U.S. Pat. No. 6,159,166, U.S. Pat. No. 6,261,235, U.S. Pat. No. 6,364,842, U.S. Pat. No. 6,767,329, U.S. Pat. No. 6,293,915, U.S. Pat. No. 6,730,040, U.S. Pat. No. 7,074,193, U.S. Pat. No. 7,192,402 and U.S. Pat. No. 7,195,596. Some of these approaches capture pulse waveforms from fingertips instead of wrist positions. Some approaches apply pressure on the position using compressed air to take the pulse, which changes the pulse reading. It is also difficult to tell if the Nadi obtained using these methods is complete or not.
[0007] The drawbacks of the hitherto reported prior art can be summarized as follows:
The above description itself dictates that the skill involved in the Nadi-Nidan comes through lot of practice and experience. Again, the information content is only qualitative and no quantitative conclusions can be drawn at the outset. Also there is subjectiveness in the reported processes. In most of the previous attempts disclosed, the methodology involves application of some constant pressure (to obtain maximum amplitude) on the radial artery. But, it is known that Nadi-Nidan does not support any such external pressure on the artery, since it affects the blood circulation and hence the Nadi itself. Further, for any diagnostic method, it is essential to know the completeness as well as inaccuracies (in the present case, the noise content of the waveform), which is not mentioned. Most of the previous attempts disclosed just present the pulse waveforms or compute the pulse rate, but no further processing is presented towards diagnosis.
[0012] Thus, the inventors of the present invention realized that there exists a need to develop a system based on Ayurveda, which would overcome all these problems. Hence it was thought desirable to have a system, which can give Nadi pulses as a time-series data and yet simple to use. In the present disclosure all the limitations have been removed, hence the waveforms obtained from the present embodiment are used for diagnosis based on quantitative information. Further, all the major types and subtypes of the Nadi pulses have been identified, which supports the accuracy of the waveforms obtainable from the present disclosure.
[0013] The system of the present invention is intended to provide a convenient, inexpensive, painless, and noninvasive methodology to eliminate all the human errors in the Nadi-Nidan performed manually by Ayurvedic practitioner and the diagnostics could be performed based on accurate and quantitative information. The invention could also eliminate any subjectiveness in the diagnostics.
OBJECTS OF THE INVENTION
[0014] Thus, the main object of the present invention is to provide a convenient, inexpensive, painless, and non-invasive Computer-aided device which will eliminate all the human errors in the Nadi-Nidan performed manually by Ayurvedic practitioner for diagnostics of disorders and human health parameters.
[0015] Another object of the invention is to provide a device which is easy-to-use and quick in response system, which removes the subjectiveness by performing based on accurate and quantitative information.
[0016] Yet another object of the invention is to provide a device which can give nadi pulses as a time-series data and yet simple to use.
[0017] Still another object of the invention is to provide a device wherein various machine learning algorithms have been applied on the nadi waveforms to classify the major types and subtypes of the nadi pulses, which supports the accuracy of the waveforms obtainable from the present disclosure.
SUMMARY OF THE INVENTION
[0018] The methodology adapted in the present invention involves the placement of the pressure sensing element at the exact pick-up point of the fingertip, where nadi pulses are sensed and the analog pressure signal generated therein is digitized. The waveforms are then analyzed using modern machine learning techniques and are then classified into various types and sub-types of nadi defined in Ayuniedic literature.
[0019] The definitions of the terms used in the present invention are given here as under:
“Ayurveda”—Ayurveda is a Sanskrit word derived from two roots: ayur, which means life; and veda, which means knowledge. It has its roots in ancient vedic literature. Ayurveda, a system of diet, healing and health maintenance, is probably the oldest science of life, just like the science of Yoga. “Nadi”—refers to pulse
[0022] The starting point for many people into the ancient scientific art of Ayurveda is the relationship of the three Doshas: Vata, Pitta and Kapha.
[0023] Ayurveda sees life as a harmonic flow, a dynamic balance of those three fundamental forces:
Vata (wind, air) the principle of movement and impulse Pitta (bile, fire) the principle of assimilation and transformation Kapha (mucus, water) the principle of stability
[0027] These forces act in everyone. When they are in balance they bring well-being and health, in imbalance they lead to feeling unwell and later disease. Everybody is unique and Ayurveda respects this uniqueness. That is why there are individual constitution types, Doshas, in the body.
[0028] Out of the three basic forces seven categories of individuals can be formed:
1. Wind dominated individuals (vata) 2. Bile dominated individuals (pitta) 3. Mucus dominated individuals (kapha) 4. Wind and Bile dominated individuals (vata and pitta) 5. Wind and Mucus dominated individuals (vata and kapha) 6. Bile and mucus dominated individuals (pitta and kapha) 7. Wind, bile and mucus dominated individuals (vata and pitta and kapha in equal proportion) “vegavati”—if the pulse rate is very high, and the movement is higher, then the pulse is detected as Vegavati pulse “manda”—if the pulse rate is low with very less movements in Tidal and Dicrotic waves, then the pulse is detected as Mande pulse “sukshma”—if the pulse has very low slopes with wide widths of Tidal and Dicrotic waves, then the pulse is detected as Sukshma pulse “tikshna”—if the pulse has sharp slopes at the Percussion wave, then the pulse is detected as Tikshna pulse. It promotes sharpness and rapidity of comprehension. “kathina”—if the shapes at the Tidal and Dicrotic waves look like equilateral triangle, then the pulse is detected as Kathina pulse. It increases strength, rigidity. “sama”—if the pulse shows equivalent behaviour in all the three doshas, then the pulse is detected as Sama pulse.
[0042] As mentioned earlier, the Nadi pulses are sensed by the three fingertips of the Ayurvedic practitioner at the root of thumb on wrist, which actually measure the pressure exerted by the artery. This pressure is in fact very tiny (−0.00124 Pa to +0.00124 Pa) in pressure units. In the present invention similar methodology is used. Three pressure sensing elements (of pressure range of 3 inch H 2 O to 5 inch H 2 O) coupled with three transmitters (one for each one sensing element), which can amplify the electrical signal, are placed at the predetermined locations instead of the three fingertips, which generate three electrical signals proportional to the pressure experienced by the three pressure sensing elements. Each of the three electrical signals is then digitized using the digitizer, having an interface with the personal computer at the USB port. The data can be obtained on the computer for a predetermined length of time, for any change in the signal value, by using the data acquisition software, which controls the digitization as well. The minimum change in the signal, which can be measured, depends solely on the resolution of the ADC. The three such pulse data are stored against one time information on one hand. Similar pulse data are obtained for the second hand of the person.
[0043] The data obtained in this way is usually corrupted because of implicit and explicit electronic and electrical disturbances, called as noise, which modulates the information content. The noise level obtained in the present system developed is almost zero, after proper shielding. Hence the Nadi obtained is in pure form and any digital filtering on the signal obtained from the digitizer, of any kind, is not required.
[0044] Once the pulse data is stored on computer, Pitch Synchronous Wavelet Transform is applied on each pulse data series to extract the average properties. Then important physiological properties are computed using various feature extraction methods such as Fourier analysis, Chaos analysis, Variability analysis. Finally, types and sub-types of pulses are detected based on these parameters.
[0045] Accordingly, the present invention provides a non-invasive device Nadi Tarangini, useful for quantitative detection of arterial ‘nadi’ pulse waveform, wherein the said assembly comprising:
[a] at least three circuits of diaphragm based pressure sensors [ 1 in FIG. 2 ] placed side by side at the three predetermined exact pick up points on the wrist of a user [ 6 , 7 , 8 in FIG. 1 ] for sensing the ‘nadi’ pulses; [b] at least one strip of neoprene [ 5 in FIG. 3 ] provided at the bottom of the said pressure sensors; [c] the said strip provided with at least three holes [ 3 in FIG. 3 ] to introduce air gaps having thickness in the range of 1 to 5 mm for capturing the arterial pulsations; [d] providing at least one transducer [ 1 in FIG. 2 ] corresponding to each of the said pressure sensor provided above along with a DC power source [ 4 in FIG. 4 ] for converting the pressure signal into an equivalent electrical signal; [e] providing at least one digitizer [ 5 in FIG. 4 ] for converting the electrical signal obtained in step [d] above into digital form, using at least one Analog to Digital Converter (ADC) [ 5 in FIG. 4 ], along with a shielding arrangement [ 7 in FIG. 5 ] for minimizing the noise; [f] providing a computing device [ 7 in FIG. 2 ] connected to the said digitizer for obtaining the visual display of the pulse pressure waveform.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
[0052] FIG. 1 shows the positioning of the fingertips of an Ayurvedic practitioner on patient's hand for sensing the pulse at three positions Vata, Pitta and Kapha.
[0053] FIG. 2 provides the schematic drawing of the present invention.
[0054] FIG. 3 shows the arrangement of neoprene sheet to introduce air gap between sensors and the patient's skin.
[0055] FIG. 4 is the electrical line diagram according to the present invention.
[0056] FIG. 5 is the circuit diagram for one of the sensing elements of the system according to the present invention (same circuitry is done for other two sensors).
[0057] FIG. 6 shows a sample pulse data for small duration from our database for three pick-up positions.
[0058] FIG. 7 shows a sample dosha waveform (of three) indicating the important time domain features.
[0059] FIG. 8 shows an example of Vegavati pulse
[0060] FIG. 9 shows an example of Manda pulse
[0061] FIG. 10 describes the steps involved in computation of average values to capture the essence of pulse data series using Pitch Synchronous Wavelet Transform (PSWT)
[0062] FIG. 11 shows an example of Tikshna Nadi
[0063] FIG. 12 shows an example of Kathina Nadi
[0064] FIG. 13 shows an example of Sama Nadi
[0065] FIG. 14 shows an example of Sukshma Nadi
[0066] FIG. 15 shows the variations in multifractal spectra of vata data series of persons in three age-groups.
[0067] FIG. 16 shows a sample arrhythmic pulse where every third beat is missing, and is captured by the variability of pulse intervals.
[0068] FIG. 17 shows the comparison between normal and fever pitta pulse through recurrence plot analysis.
[0069] FIG. 18 displays a flowchart indicating important steps in our approach of diagnosing a patient using data from our embodiment using rigorous machine learning algorithms.
[0070] FIG. 19 shows an example of pulse of person 32 at three predefined positions vata, pitta and kapha.
[0071] FIG. 20 shows and example of Vata pulse of person 32 for 1 minute.
[0072] FIG. 21 shows and example of Fourier transform of the vata pulse of person 32 .
[0073] FIG. 22 shows an example of the detected peaks of vata pulse of person 32 .
[0074] FIG. 23 shows an example of folding the vata pulse of person 32 , so that all the peaks are together.
[0075] FIG. 24 shows and example of average vata pulse of person 32 showing the essence of the entire time series.
[0076] FIG. 25 shows an example of the multifractal spectrum of vata pulse of person 32 .
[0077] FIG. 26 shows an example of the pulse rate variability indicating the time differences between the peaks of vata pulse of person 32 .
[0078] FIG. 27 shows an example of the recurrence plot of vata pulse of person 32 .
DETAILED DESCRIPTION OF THE INVENTION
[0079] Time series analysis and Machine learning are useful tools to understand the underlying dynamics of the physiological system. In general, a time-series can be obtained by digitizing the analog signal from the pressure sensing element and the transducer, at the desired sampling rate and for desired time, by using a digitizer (analog to digital converter, ADC). ADC has an interface with personal computer (PC) which can transfer and store the data series, called as time series, on the disk. The time series obtained by this way can then be analyzed using various machine learning algorithms to extract the dynamic features of the underlying system. A similar methodology is adapted in the present invention to acquire the Nadi pulses quantitatively.
[0080] In the present invention, mounted over a neoprene sheet, 3 in FIG. 2 , three pressure sensing elements, 1 in FIG. 2 , coupled with transmitters, 4 in FIG. 2 , which can amplify the electrical signal, are placed at the three predetermined locations, 6 , 7 , 8 in FIG. 1 , in place of the fingertips of the Ayurvedic practitioner. The pressure sensing elements along with the neoprene sheet have to be properly adjusted on the patient's wrist considering the variable size of patient's wrist, skin differences, and such that all the three diaphragms, 2 in FIG. 4 , of the three sensing elements exactly come in contact with the patient's nadi at the three predetermined locations on the wrist. The sensor leads, 2 in FIG. 2 , are properly shielded. Each of the pressure sensing elements is supplied with the excitation voltage by using the DC power source, 5 in FIG. 2 , through the transmitter. This arrangement generates an electrical signal proportional to the pressure experienced by the pressure sensing element, which is then digitized using the digitizer (ADC), 6 in FIG. 2 , having an interface with the personal computer (PC), 7 in FIG. 2 , at the USB port.
[0081] The data can be obtained on the computer for a predetermined length of time, for any change in the signal value, by using the data acquisition software, which controls the digitization as well. The minimum change in the signal, which can be measured, depends solely on the resolution of the digitizer.
[0082] The data obtained in this way is usually corrupted because of implicit and explicit electronic and electrical disturbances, called as noise, which modulates the information content. The noise level obtained in the present system developed is almost zero, after proper shielding. Hence the nadi obtained is in purer form and any digital filtering on the signal obtained from the digitizer, of any kind, is not required.
[0083] The waveforms obtained from the present invention contain typical physiological properties such as rhythm, self-similar nature, and chaotic nature. Rigorous machine learning algorithms are used to classify these waveforms, primarily defined in the Ayurvedic literature, as various types and sub-types of nadi patterns. The waveforms are accurate, complete, reproducible and noise-free to perform accurate diagnosis.
[0084] The methodology adapted involves:
(a) placement of each of the three pressure sensing elements at the exact pick-up points by the three fingertips (of Ayurvedic practitioner) respectively, where Nadi pulses are sensed and the analog pressure signal generated therein is digitized after removing the DC component; (b) introducing an arrangement for an air gap between each of the sensors and the skin using a neoprene sheet with three holes; (c) connecting at least up to one transmitter to each of the sensor which is further connected to the DC voltage supply from the other side; (d) connecting at least one digitizer for converting the electrical signal as obtained from step (d) into digital form using at least one Analog to Digital Converter (ADC) for capturing the rapid changes in input signal, along with a shielding of filtering arrangement for minimizing the noise; (e) recording and storing different parameters from the digital signals of primary and secondary peaks as obtained from step (d) into a storage device; (f) designing dedicated programs in the storage device for optimizing a performance criterion of classification of pulse patterns; (g) observing and interpreting the results obtained from above steps by analysis of pulse waveforms for detecting various disorders.
[0092] The detailed description of the system adapted is as follows.
FIG. 4 explains the electrical line diagram of the present invention. Each of the diaphragm, 2 in FIG. 4 , based pressure sensing elements, 1 in FIG. 4 , is supplied with the excitation voltage by using the DC power source, 4 in FIG. 4 , through the transmitters, 3 in FIG. 4 . Each output of the pressure sensing element is obtained from the transmitter through the corresponding connecting leads, 7 in FIG. 4 . The output is further connected to the ADC, 5 in FIG. 4 for digitization and finally stored in computer, 6 in FIG. 4 . The details of the circuitry adapted for each sensing element in the present invention are disclosed in FIG. 5 . The Wheatstone bridge, 1 in FIG. 5 , of the pressure sensing element receives the constant excitation voltage from reference voltage generator, 9 in FIG. 5 , through the connecting bus. The variable resistor, 2 in FIG. 5 , of the bridge recognizes the pressure changes from the Nadi pulses. This output is amplified through a series of amplifiers, 3 in FIG. 5 , and is given to the base of the NPN-type transistor, 4 in FIG. 5 . The output is obtained from the emitter terminal, which is proportional to the amplified pressure signal from the bridge. The current output is converted into voltage, 8 in FIG. 5 , by using a resistor, 5 in FIG. 5 , which goes for digitization. The diode, 6 in FIG. 5 , allows the unidirectional current flow. All the connecting wires, 7 in FIG. 5 , were properly shielded and grounded which eliminate any external interference, noise. FIG. 3 shows the arrangement of neoprene sheet, 5 in FIG. 3 , to introduce air gap between sensors and the person's skin. The dimensions of each sensor are 8.5 mm×6.5 mm. A very tiny diaphragm, 1 in FIG. 3 , is at the center of the sensor, 2 in FIG. 3 , which has to be exactly placed at pre-defined position on wrist. Three holes, 3 in FIG. 3 , are made into the neoprene sheet (of thickness 1 to 5 mm) for introducing air gaps, 4 in FIG. 3 . The size of each hole is such that each sensor just rests on the sheet covering its respective hole. Digitizer and data acquisition software: The analog signal obtained from the transmitter is freed from the DC component and is then subjected to the digitization by using an ADC. Bandwidth of the ADC is high enough to capture the rapid changes in the input signal from the transmitter. An ADC of accuracy 12-bit was used for our invention. The ADC is interfaced to the personal computer at the USB port. The software, LabVIEW, supports the abovementioned ADC device, which enables the operations of ADC through personal computer itself. The software acquires the digitized data of Nadi pulses for a prefixed time and saves the digitized pulse wave on the disk. FIG. 6 gives a normalized sample pulse data from our database. The three colors indicate three different doshas captured at pre-defined positions on wrist. The three dosha waveforms almost follow each other, but they show different nature. The information hidden in these data are captured using various algorithms. FIG. 7 shows a zoomed version of a pulse cycle from FIG. 6 of one dosha, indicating the important time domain features. In our database, the details in Percussion wave, 1 in FIG. 7 , Tidal wave, 2 in FIG. 7 , Valley, 3 in FIG. 7 , and Dicrotic wave, 4 in FIG. 7 , show different behavior for different patients and thus can be identified by learning the behavior. Also the points-representation of pulse data, 5 in FIG. 7 , gives the idea of the complete picture of pulse and that no extra information is available.
[0098] Hence the pulse time series, thus extracted consists of complete and noise-free spectra of the Nadi pulse. This is the unique feature of the present invention.
[0099] In an embodiment of the present invention, the parameters used are selected from the group comprising age, gender, profession, skin and atmospheric conditions.
[0100] In another embodiment of the present invention, the chaotic nature is determined in terms of strange attractor properties and the chaotic properties being captured in terms of Recurrence Quantification analysis parameters which are capable of capturing various disorders including fever, back-pain, arrhythmia and heart disorders.
[0101] In still another embodiment of the present invention, the variable resistor of the Wheatstone bridge is capable of recognizing the pressure changes at nadi pulses.
[0102] In yet another embodiment of the present invention, the device being capable of detecting arterial pulse pressure in the range of (−) 0.00124 Pa to (+) 0.00124 Pa.
[0103] In a further embodiment of the present invention, the type of nadi is selected from the group consisting of Sukshma, Tikshna, Kathina and Sama, their sub-types and combinations thereof, wherein the pressure points of the user are vata, pitta and kapha.
[0104] In another embodiment of the present invention, the pressure at the sensors is in the range of 7.5 to 13 cm H 2 0 pressure for capturing accurate pressure readings.
[0105] In still another embodiment of the present invention, the thickness of neoprene sheet used is in the range of 1 to 5 mm.
[0106] In yet another embodiment of the present invention, the three sensing elements are mounted exactly on the three holes made [ 4 in FIG. 3 ] in a neoprene sheet with thickness in the range of 1 to 5 mm to introduce three air gaps between the sensors and the patient's skin so as to capture the tiny pressure very accurately.
[0107] In another embodiment of the present invention, the storage device is preferably a computer having at least one USB port.
[0108] In still another embodiment of the present invention, the waveform produced comprises domain features of percussion wave, tidal wave, valley and dicrotic wave.
[0109] In a further embodiment of the present invention, is provided a method for quantitative detection of arterial nadi pulse waveform of an individual using the claimed device Nadi Tarangini, wherein the said method comprising the steps of placing the said device at predetermined position for at least up to 60 seconds followed by acquiring and recording different parameters forming complete noiseless nadi waveform peaks characterized by typical physiological properties selected from the group comprising rhythm, self-similar nature, chaotic nature and then interpreting the results obtained for identifying possible disorders in a user.
[0110] In a further embodiment of the present invention, the sub-type of nadi is selected from the group consisting of Manda and Vegavati, wherein the pressure points of the user are vata, pitta and kapha.
[0111] In a further embodiment of the present invention, the pulse rate is quantitatively computed from the Fourier spectrum of the pulse.
[0112] In another embodiment of the present invention, the peaks include both main and secondary types and varies with change on different parameters.
[0113] In yet another embodiment of the present invention, the rhythm used is Pitch Synchronous Wavelet Transform, wherein the wavelet coefficients being capable of extracting the average values of the pulse to capture the essence of the whole data series.
[0114] In still another embodiment of the present invention, the self-similar nature of the waveform is determined by multifractal spectrum being capable of distinguishing various pulse patterns of different age groups of users.
[0115] In yet another embodiment of the present invention, the variations between consecutive pulse beats is captured by Pulse Variability, to capture the arrhythmic behavior present in the pulse.
[0116] In still another embodiment of the present invention, the chaotic properties in the pulse data are captured in terms of descriptor from Recurrence Plot to describe large and small-scale structures to detect disorders including fever.
EXAMPLES
[0117] The following examples are given by way of illustration and therefore should not be construed to limit the scope of the present invention.
Example 1
[0118] The Nadi pulses were recorded using our embodiment by placing the three pressure sensing elements, mounted on neoprene sheet, exactly at the three predetermined locations ( 6 , 7 , 8 in FIG. 1 ) on patient's left hand wrist, in place of the fingertips of the Ayurvedic practitioner. The three predetermined locations are vata position, pitta position and kapha position on the patient's wrist. The sampling rate of the acquisition was 500 Hz, which was enough to capture all the details. The data was collected for 1 to 5 minutes. All the three signals were individually digitized using the ADC ( 5 in FIG. 4 ) and were stored in the pulse database as vata pulse data, pitta pulse data and kapha pulse data respectively. Same procedure was followed for the patient's right hand wrist to get three more data. Therefore in the pulse database, 6 pulse signals (from vata, pitta and kapha positions on both the hands) were stored for each patient. Also the patient's information such as age, gender, profession was recorded in the database. The complete database contains information and pulse signals of 42 patients suffering from different disorders including fever, arrhythmic disorder. Each of the signals show variations in the parameters Amplitudes, Frequency, Rhythm, Depth and Power, and therefore carry different patterns with different information. We studied and analyzed all the pulse signals collectively using different machine learning algorithms to provide a non-invasive, easy-to-use and quick in response diagnostic device Nadi Tarangini, which eliminated all the human errors in the Nadi-Nidan performed manually by Ayurvedic practitioner for diagnostics. The important steps are briefly explained here (and shown in FIG. 1 ), and the details involved are given in the subsequent examples. Firstly, the Fourier coefficients are computed for a pulse signal of a patient (any one out of total 6 pulses, as the pulse rate is the same in all of them for the considered patients). The pulse rate is computed from the fundamental frequency in the Fourier spectrum. In order to check the reproducibility of our embodiment Nadi Tarangini, the pulse signals of a single person were recorded at different times in a morning session, and their correlation dimensions were computed to verify. As the length of each pulse signal is very high, we compute the average pulse values using the Pitch Synchronous Wavelet Transform to capture the essence of pulse. This averaged pulse can also further be used for the detection purpose. Using the above mentioned parameters and average pulse for all the 6 pulse signals for a patient, the four major types of Nadi (i.e. Sukshma, Tikshna, Kathina and Sama), the sub-types of Nadi (i.e. Manda and Vegavati) and their combinations were obtained. The detection was done using the classifier Support Vector Machine (SVM). Firstly, the classifier was trained using the parameters from first 31 patients and then tested for remaining 11 patients. Also, the pulses of patients showed different behavior prominently in three age-groups (i.e. “age below 25”, “age 25 to 50” and “age above 50”) and this behavior was captured using the multifractal analysis based on nonlinear dynamics and SVM. The arrhythmic behavior in pulse signal was captured using the variations in the pulse intervals using Pulse Rate Variability analysis and SVM. Finally, the chaos theory based Recurrence Plot analysis (based on recurrence quantification descriptors % recurrence, % determinism, entropy and % laminarity) was used to easily detect the disorders in the pulse signals using SVM.
[0119] As an example, we show these steps and calculations for a sample pulse of person 34 . FIG. 19 shows the complete pulse captured for 1 minute with sampling rate 500 Hz. Therefore, for the 3 doshas (at three predefined positions vata, pitta and kapha), the total no. of points are 3×60 (sec)×500 (Hz)=3×30,000=90,000. Only vata pulse is shown in the FIG. 20 , which contains 30,000 points for 1 minute. Fourier Transform of vata pulse is computed, which gives 30,000 Fourier coefficients. Only the first 1500 coefficients (excluding the first one, which provides the average value) are plotted, for visibility, in FIG. 21 . It can be noted that the first peak is at frequency 80.57 (=81), 1 in FIG. 21 , which is the pulse rate of the person 34 . The manually counted pulse rate is also 81. The correlation dimensions of the three doshas individually are 1.76, 1.71 and 1.75 respectively. For computing the average vata pulse, first the peaks in the vata pulse are computed as shown in FIG. 22 , where the ‘red *’ points indicate peaks. Then the vata pulse is folded in such a manner that all the peaks are together as shown in FIG. 23 . The wavelet transform of this folded vata pulse finally provides the average pulse as shown in FIG. 24 . Also, it can be seen that the pulse movements are high, thus the sub-type of vata pulse is vegavati. The shapes at the Tidal and Dicrotic waves look like equilateral triangle, thus the vata pulse is also a Kathina pulse. Further, all the three doshas show equivalent behavior and thus the pulse is sama pulse. Then the multifractal analysis of vata pulse provides the multifractal spectrum as shown in FIG. 25 , which captures the self-similarity. The peaks computed above are then used for pulse rate variability. In the considered vata pulse, there are 81 peaks, and thus 80 differences between them. These differences are all close enough as shown in FIG. 26 , and thus the considered vata pulse is not arrhythmic. Finally the recurrence plot of vata pulse (only first 8,000 points out of 30,000 are shown for better visibility) in FIG. 27 shows the small- and large-scale structures in the vata pulse. The recurrence quantification descriptors using embedding dimension 7 , time delay 1 and radius 0.3 are recurrence=5,579, laminarity=−2.182 and determinism=95. We finally used all the above results in the form of parameters for the diagnosis of person 34 by passing them to the classifier. The classifier SVM finally provides the outputs such as person 34 is of type sama kathina vegavati, person 34 does not have arrhythmic disorder.
Example 2
[0120] Pulse rate: The pulses were obtained by placing the sensor at the predetermined position for 1 to 5 minutes. Immediately after the Nadi was taken, the pulse rate was measured manually for every acquisition. The pulse rate is computed using the fundamental frequency in the Fourier spectrum of any one dosha of the 6 pulse data of the patient. The comparison of pulse rate measured from a pulse time series and that manually measured for few of the patients is given in Table 2.
Example 3
[0121] Reproducibility: The Nadi pulses were acquired of person 2 (age 27) at 7 different timings throughout a morning session (8:30 am, 9:15 am, 10:00 am, 10:45 am, 11.30 am, 12.15 pm and 1.10 pm) using our invention described in above description. Apart from the person's physic, Nadi is sensitive to mental status, stresses, thoughts, etc. Because of which the nature of the pulse essentially changes. For the above mentioned 7 timings, the person was asked to relax for 5 minutes before taking the pulse. Chaos analysis was carried on all the pulse data of the 7 timings, and it was observed that the Correlation Dimensions and Largest Lyapunov exponents [reference—D. Kugiumtzis, B. Lillekjendlie, and N. Christophersen. Chaotic time series part I: Estimation of some invariant properties in state space. Modeling, Identification and Control, 15(4):205-224, 1994] of the particular dosha remain almost constant, even though the shape of pulse changes slightly. The correlation dimensions of the pulses for vata, pitta and kapha of left hand are given in Table 3. Since the correlation dimensions (and largest Lyapunov exponents) throughout the morning session remained constant, it shows that the pulses obtained are completely reproducible, but the pulse shape may change slightly.
Example 4
[0122] Computing essence of the pulse data: Each pulse data series is given to the Pitch Synchronous Wavelet Transform algorithm [reference—Evangelista, G. 1993 . “Pitch Synchronous Wavelet Representations of Speech and Music Signals.” IEEE Transactions on Signal Processing 41(12):3313-3330] to extract the average values of the pulse, which capture the essence of the whole data series as shown in FIG. 10 . The same procedure is carried for the other two dosha data series also. The Pitch Synchronous Wavelet Transform first finds the peaks in the time series, 1 in FIG. 10 , folds the time series in such a manner that all the peaks come together, 2 in FIG. 10 , and then takes the wavelet transform, 3 in FIG. 10 , in z-direction, 4 in FIG. 10 . The final outcome gives the average values throughout the pulse data series.
Example 5
[0123] Identification of types of Nadi: The types of Nadi are identified using supervised classification. Firstly, various parameters such as Amplitudes, Frequency, Rhythm, Depth and Power are computed for all the pulse waveforms available in the database. The true Nadi types are also provided by the Ayurvedic practitioner in qualitative terms. Support Vector Machine (SVM) [reference—Vladimir N. Vapnik. The Nature of Statistical Learning Theory . Springer, New York, N.Y., USA, 1995] is used as the classifier. SVM rigorously based on statistical learning theory simultaneously minimizes the training and test errors, and produces a unique globally optimal solution. The parameters extracted from person 1 through person 31 , along with their known Nadi types, are used for training the SVM. Then, the parameters of person 32 through person 42 are tested. The output labels of SVM (quantitatively determined labels using said method) are compared with the true Nadi types (qualitatively recorded labels from the database, provided by Ayurvedic practitioner). The comparison is given in Table 4. We could classify the pulses into the Nadi types as Sukshma, Sama, Kathina, Tikshna and their combinations with good accuracy.
Example 6
[0124] Identification of sub-types of Nadi: The pulse data are preliminary classified as Vegavati or Manda depending upon the pulse rate and the movement of the pulse. As shown in FIG. 8 , if the pulse rate is very high, and the movement is higher, 1 in FIG. 8 , then the pulse is detected as Vegavati pulse. On the other hand, as shown in FIG. 9 , if the pulse rate is low with very less movements, 1 in FIG. 9 , in Tidal and Dicrotic waves, then the pulse is detected as Manda pulse.
Example 7
[0125] Identification of Tikshna Nadi: FIG. 11 shows vata pulse waveform of person 41 as an example of Tikshna Nadi, where the slopes at the peaks of Percussion wave are found to be very sharp, 1 in FIG. 11 .
Example 8
[0126] Identification of Kathina Nadi: FIG. 12 shows kapha pulse waveform of person 38 as an example of Kathina Nadi, where the shapes at the Tidal and Dicrotic waves look like equilateral triangle, 1 in FIG. 12 .
Example 9
[0127] Identification of Sama Nadi: FIG. 13 shows all three pulse waveforms of person 40 as an example of Sama Nadi, where the pulse shows equivalent behaviour in all the three doshas.
Example 10
[0128] Identification of Sukshma Nadi: FIG. 14 shows vata pulse of person 36 as an example of Kathina Nadi, where the pulse has very low slopes with wide widths of Tidal and Dicrotic waves, 1 in FIG. 14 .
Example 11
[0129] Identification of special pulses: Pulse Rate Variability, Multifractal spectrum analysis and Recurrence Plot methodologies are used for capturing the special cases of pulses in all the doshas.
A Multifractal spectrum [reference—J. F. Muzy, E. Bacry and A. Arneodo, The multifractal formalism revisited with wavelets . Int. J. Bif. Chaos 4 (1994) 245-302] captures the self-similarity of the pulse series, which is an essential property of a physiological time series. 22 normal pulses are separated into three age-groups namely “age below 25”, “age 25 to 50” and “age above 50” and their multifractal spectra are observed. In FIG. 15 , multifractal spectrum of one randomly chosen normal pulse from each age-group is shown. As shown in FIG. 15 , the multifractal spectrum moves towards top-up corner, as the age increases. Therefore, as explained in Example 5, a classifier can be trained to classify a pulse into once of the three age-groups. Pulse variability [reference—L. Li and Z. Wang. Study on interval variability of arterial pulse. In The 1st Joint BMES/EMBS Conference, page 223, 1999] captures the variations between consecutive pulse beats, rather than simply the pulse rate. Firstly, the pulse peaks are detected and the difference between these peaks forms the pulse variability data. We use this pulse variability data to capture the missing pulse beats, if any, and thus the data is very useful to capture the arrhythmic behavior present in the pulse as shown in FIG. 16 . In a normal pulse data, the differences between in pulse peaks vary in a very close range. In the considered pulse data, every third beat is missing, 1 in FIG. 16 ; therefore the differences between the peaks are varying and thus can be detected as an arrhythmic pulse data. The chaotic properties in the pulse data can be captured in terms of Recurrence Plot (RP) [reference—J. P. Zbilut, C. L. Webber Jr.: Embeddings and delays as derived from quantification of recurrence plots, Physics Letters A, 171(3-4), 199-203 (1992)], whose quantification analysis describes large and small-scale structures through a set of descriptors. These descriptors are subsequently used to detect various disorders (e.g. fever) by training a classifier as explained in Example 5. FIG. 17 shows an example of recurrence plot of fever Pitta pulse, 2 in FIG. 17 , which shows very different behavior than the recurrence plot of a normal pitta pulse, 1 in FIG. 17 , and hence is identified using the descriptors.
TABLES
[0133] Table 1: Characteristics of three humors (Vata, Pitta and Kapha) defined in Ayurveda.
[0134] Table 2: Comparison of the pulse rate.
[0135] Table 3: Comparison of the correlation dimensions (CD) of the pulses (from morning session) of person 2 for checking reproducibility.
[0136] Table 4: Identification of Nadi pulses using machine learning algorithms.
[0000]
TABLE 1
Characteristics of three humors (Vata, Pitta and Kapha)
defined in Ayurveda.
VATA PULSE
PITTA PULSE
KAPHA PULSE
Characteristics
Fast, feeble,
Prominent, strong,
Deep, slow, broad
cold, light,
high amplitude,
wavy, thick, cool,
thin, disappears
hot, forceful, lifts
warm, regular
on pressure
up the palpating
fingers.
Location
Best felt under
Best felt under
Best felt under
the index finger
the middle
the ring
finger
finger
Gati
Moves like a
Moves like a frog
Moves like a
[Movement]
cobra
swimming swan
[0000]
TABLE 2
Comparison of the pulse rate.
PULSE RATE IN THE
ACQUIRED DATA USING
PULSE RATE
AGE
FOURIER ANALYSIS
MANUALLY
GROUP
PERSON
(rounded to nearest integer)
MEASURED
Below 25
Person 1
68
69
25 to 50
Person 2
78
76
25 to 50
Person 3
79
78
25 to 50
Person 4
75
75
Above 50
Person 5
82
82
Above 50
Person 6
111
112
25 to 50
Person 7
74
78
Above 50
Person 8
81
81
Below 25
Person 9
68
69
25 to 50
Person 10
82
80
Below 25
Person 11
66
66
[0000]
TABLE 3
Comparison of the correlation dimensions (CD) of the pulses
(from morning session) of person 2 for checking reproducibility.
CD OF
CD OF
CD OF
TIMING
VATA PULSE
PITTA PULSE
KAPHA PULSE
8.30 am
1.4945
1.7466
1.5924
9.15 am
1.5046
1.8286
1.6728
10.00 am
1.4962
1.8649
1.6340
10.45 am
1.5427
1.7723
1.6776
11.30 am
1.5024
1.8343
1.6826
12.15 pm
1.4667
1.8502
1.6785
1.10 pm
1.5118
1.7363
1.7016
[0000]
TABLE 4
Identification of Nadi pulses using machine learning algorithms
TRUE NADI LABEL
PROVIDED BY
NADI LABEL OUTPUT
AYURVEDIC
SR. NO.
NAME
FROM SVM
PRACTITIONER
1
Person 32
Sukshma Sama Kathina
Sama Kathina (Manda)
(Manda)
2
Person 33
Sukshma Sama
Sukshma Sama
3
Person 34
Sama Kathina (Vegvati)
Sama Kathin (Vegvati)
4
Person 35
Sukshma Kathina
Sukshma Kathina
5
Person 36
Sukshma (Manda)
Sukshma (Manda)
6
Person 37
Sukshma Sama
Sukshma Sama
7
Person 38
Kathina (Vegvati)
Kathina (Vegvati)
8
Person 39
Sama Kathina (Manda)
Kathina (Manda)
9
Person 40
Sama (Manda)
Sama (Manda)
10
Person 41
Tikshna
Tikshna
11
Person 42
Sukshma Sama
Sukshma Sama
(Vegavati)
ADVANTAGES:
[0137] 1. Data Acquisition Methodology Using Air-Gap.
An air gap is introduced between each of the three sensors and the skin at wrist using a neoprene sheet with three holes. The dimensions of a sensor are 9×7 mm and the tiny diaphragm is at the center. The neoprene sheet is of thickness 1 to 5 mm. The three holes on this sheet which are of dimensions 7×5 cm are such that the sensors just fit around them. This arrangement helps to pick up the pressure exerted by the artery accurately.
[0139] 2. Accurate, Complete Waveforms: Physiological Properties.
The waveforms obtained from our embodiment are accurate and complete (contain all the information), reproducible and thus contain the typical physiological properties such as rhythm, chaotic nature, self-similarity.
[0141] 3. Pulse Patterns.
The waveforms obtained from our system show patterns which resemble the nadis defined in the Ayurvedic literature such as Sama, Kathina, Tikshna, Sukshma.
[0143] 4. Diagnosis based on Ayuvedic Concepts.
Rigorous machine learning algorithms are applied to classify the pulse waveforms obtained from our system to diagnose a patient for various disorders and health parameters.
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The present invention discloses the procedure for obtaining complete spectrum of the Nadi pulses, as a time series and capable of detecting the major types and the subtypes of the Nadi pulses. The device of this invention involves three diaphragm elements equipped with strain gauge, three transmitters cum amplifiers, and a digitizer for quantifying analog signal. The system acquires the data with 12-bit accuracy with practically no electronic and/or external interfering noise. The pertaining proofs are given which clearly shows the capability of delivering the accurate spectrums, with repeatability of the pulses from the invented system. ‘Nadi-Nidan’ is a prominent method in Ayurveda (Ayurveda is a Sanskrit word derived from ‘Ayus’ and ‘vid’, meaning life and knowledge respectively. It is a holistic science encompassing mental, physical and spiritual health), which is known to dictate all the salient features of a human body. Nadi-Nidan is a specialty of ‘Vaidyas’ (Ayurvedic physicians) and hence the present system would enable the diagnosis accurately, quantitatively and independent of any human errors.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 09/603,485, filed Jun. 23, 2000, now abandoned.
This application is related to Korean Patent Application No. 1999-24469 filed Jun. 26, 1999, and takes priority from that date.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an organic anti-reflective coating (“ARC”) material which allows the stable formation of ultrafine patterns suitable for 64 M, 256 M, 1 G, 4 G and 16 G DRAM semiconductor devices. More particularly, the present invention relates to an organic anti-reflective coating material that contains a chromophore with high absorbance at the wavelengths useful for submicrolithography. A layer of said anti-reflection material can prevent back reflection of light from lower layers or a surface of the semiconductor ship, as well as eliminate the standing waves in the photoresist layer, during a submicrolithographic process using a 193 nm ArF laser light sources. Also, the present invention is concerned with an anti-reflective coating composition comprising such a material, an anti-reflective coating therefrom and a preparation method thereof
2. Description of the Prior Art
During a submicrolithographic process, one of the most important processes for fabricating highly integrated semiconductor devices, there inevitably occur standing waves and reflective notching of the waves due to the optical properties of lower layers coated on the wafer and to changes in the thickness of the photosensitive film applied thereon. In addition, the submicrolithographic process generally suffers from a problem of the CD (critical dimension) being altered by the diffracted light and reflected light from the lower layers.
To overcome these problems, it has been proposed to introduce a film, called an anti-reflective coating, between the substrate and the photosensitive film to prevent light reflection from the lower layer. Largely, anti-reflective coatings are classified into “organic” and “inorganic” by the materials used and into “absorbing” and “interfering” by the operation mechanisms.
An inorganic anti-reflective coating is used mainly in the process of ultrafine-pattern formation using i-line radiation with a wavelength of 365 nm. TiN and amorphous carbon have been widely used in light-absorbing coatings, and SiON has been used in light-interfering coatings. The SiON anti-reflective coatings are also adopted for submicrolithographic processes that use KrF light sources.
Recently, extensive and intensive research has been and continues to be directed to the application of organic anti-reflective coatings for such submicrolithography. In view of the present development status, organic anti-reflective coatings, if they are to be useful, must satisfy the following fundamental requirements:
First, during the pattern formation process, the photoresist must not be peeled from the substrate by dissolving in the solvent used in the organic anti-reflective coating. For this reason, the organic anti-reflective coating needs to be designed to form a cross-linked structure, and must not produce chemicals as a by-product.
Second, acid or amine compounds must not migrate in or out of the anti-reflective coating. This is because there is a tendency for undercutting at the lower side of the pattern if an acid migrates, and for footing if a base such as an amine migrates.
Third, the anti-reflective coating must have a faster etching speed compared to the photoresist layer so that the etching process can be performed efficiently by utilizing the photoresist layer as a mask.
Finally, the organic anti-reflective coatings should be as thin as possible while playing an excellent role in preventing light reflection.
As various as anti-reflective coatings are, those which are satisfactorily applicable for submicrolithographic processes using ArF light have thus far not been found. As for inorganic anti-reflective coatings, there have been reported no materials which can control interference at the ArF wavelength, that is, 193 nm. In contrast, active research has been undertaken to develop organic materials into superb anti-reflective coatings. In fact, in most cases of submicrolithography, the coating of photosensitive layers is necessarily followed by organic anti-reflective coatings that prevent the standing waves and reflective notching occurring upon light exposure, and that eliminate the influence of the back diffraction and reflection of light from lower layers. Accordingly, the development of such an anti-reflective coating material showing high absorption properties against specific wavelengths is one of the hottest and most urgent issues in the art.
SUMMARY OF THE INVENTION
The present invention overcomes the problems encountered in the prior art and provides a novel organic compound that can be used as an anti-reflective coating useful for submicrolithography processes using 193 nm ArF laser.
The present invention provides a method for preparing an organic compound that prevents the diffusion and reflection caused by light exposure in submicrolithography.
The present invention further provides an anti-reflective coating composition containing such a diffusion/reflection-preventive compound and a preparation method therefor.
The present invention also provides an anti-reflective coating formed from such a composition and a preparing method thereof.
The polymers of the present invention comprise a monomer with a phenyl group having high absorbance at 193 nm, so that the polymer resin absorbs 193 nm wavelength light. A cross-linking mechanism using a ring opening reaction is introduced into preferred polymer resins of the invention by adding another monomer having an epoxy structure, so that a cross-linking reaction takes place when coatings of the polymer resins are “hard baked”, i.e., heated at a temperature of 100-300° C. for 10-1,000 seconds. Accordingly, a great improvement can be effected in the formation, tightness and dissolution properties of the anti-reflective coatings using polymers of the present invention. Particularly, maximal cross-linking reaction efficiency and storage stability are realized by the present invention. The anti-reflective coating resins of the present invention have superior solubility in all hydrocarbon solvents, in order to form a coating composition, yet are of such high solvent resistance after hard baking that they are not dissolved in any solvent at all. These advantages allow the resins to be coated without any problem to form an anti-reflective coating which prevents undercutting and footing problems when images are formed on the overlying photosensitive layer. Furthermore, coatings made of the acrylate polymers of the invention are higher in etch rate than the photosensitive film coatings, thereby improving the etch selection ratio therebetween.
DETAILED DESCRIPTION OF THE INVENTION
Polymer resins according to the present invention are represented by the following general formula 1:
wherein,
R a , R b , R c and R d each represents hydrogen or methyl group;
R 1 represents hydrogen, hydroxy, a substituted or unsubstituted, straight or branched C 1 -C 5 alkyl, cycloalkyl, alkoxyalkyl or cycloalkoxyalkyl;
w, x, y and z each represents a mole fraction of 0.01-0.99; and n 1 , n 2 and n 3 each represents an integer of 1 to 4;
and by the following general formula 2:
wherein,
R a , R b , and R c each represents hydrogen or methyl group;
R 1 represents hydrogen, hydroxy, substituted or unsubstituted, straight or branched C 1 -C 5 alkyl, cycloalkyl, alkoxyalkyl or cycloalkoxyalkyl;
x, y and z each represents mole fraction of 0.01-0.99; and n 1 and n 2 each represents an integer of 1 to 4.
The polymer resins of the present invention are particularly suitable for use as organic anti-reflective coatings because they comprise a (toluene-4-sulfonyloxy)alkyl acrylate monomer, in which the phenyl group readily absorbs wavelength of 193 nm. Preferred monomers comprise a monomer of the following chemical formula 3:
wherein,
R is hydrogen or methyl group; n is an integer of 2 or 3.
The polymers represented by general formula 1 can be prepared in accordance with the reaction equation 1 set forth below, wherein (toluene-4-sulfonyloxy)alkyl acrylate type monomers, hydroxyalkyl acrylate-type monomers, methyl acrylate-type monomers and glycidyl methacrylate-type monomers are polymerized with the aid of an initiator in a solvent. Each of the monomers has a mole fraction ranging from 0.01 to 0.99.
wherein,
R a , R b , R c and R d each represents hydrogen or methyl group;
R 1 represents hydrogen, hydroxy, straight or branched C 1 -C 5 alkyl, cycloalkyl, alkoxyalkyl or cycloalkoxyalkyl; and n 1 , n 2 and n 3 each represents an integer of 1 to 4.
The polymers represented by general formula 2 above can be prepared in accordance with the reaction equation 2 set forth below, wherein, (toluene-4-sulfonyloxy)alkyl acrylate type monomers, hydroxyalkyl acrylate-type monomers and methyl acrylate-type monomers are polymerized with the aid of an initiator in a solvent. Each of the monomers has a mole fraction ranging from 0.01 to 0.99.
wherein,
R a , R b , and R c each represents hydrogen or methyl group;
R 1 represents hydrogen, hydroxy, a substituted or unsubstituted, straight or branched C 1 -C 5 alkyl, cycloalkyl, alkoxyalkyl or cycloalkoxyalkyl; and n 1 and n 2 represents an integer of 1 to 4.
Conventional radical initiators, preferably 2,2-azobisisobutyronitrile (AIBN), acetylperoxide, laurylperoxide or t-butylperoxide, may be used for initiating the polymerization reaction forming the polymers of general formulas 1 and 2. Also, conventional solvents may be used for the polymerization, preferably tetrahydrofuran, toluene, benzene, methylethylketone or dioxane. Preferably, the polymerization for the polymers of the general formulas 1 and 2 is carried out at 50-80° C.
Semiconductor devices of the present invention may be prepared as described below. The copolymer of general formula 1 or formula 2 may be dissolved in a suitable solvent alone, or with a cross-linker additive selected from acrolein, diethylacetal and melamine-type cross linkers, at an amount of 0.1 to 30% by weight. The solution is filtered and coated on a wafer and then hard-baked to form a cross-linked anti-reflective coating. Semiconductor devices can then be fabricated therefrom in the conventional manner.
Conventional organic solvents may be used in preparing the anti-reflective coating composition, with preference given to ethyl 3-ethoxypropionate, methyl 3-methoxy propionate, cyclohexanone or propyleneglycol methyletheracetate. The solvent is preferably used at an amount of 200 to 5000% by weight based on the weight of the anti-reflective coating resin copolymer used.
It has been found that the anti-reflective coatings of the present invention exhibit high performance in photolithography processes for forming ultrafine-patterns using 193 nm ArF radiation. The same was also true of where 248 nm KrF, 157 nm F 2 laser, E-beams, EUV (extremely ultraviolet) and ion beams are used as light sources.
A better understanding of the present invention may be obtained from following examples, which are set forth to illustrate, but are not to be construed to limit, the present invention.
EXAMPLE I
Synthesis of 2-(toluene-4-sulfonyloxy)ethyl acrylate monomer
To 0.35 mole of triethylamine was added 0.35 mole p-toluene sulfonylchloride followed by 0.3 mole of 2-hydroxyethyl acrylate The reaction mixture was stirred for over 24 hours with cooling, and monitored by TLC. The reaction mixture was neutralized with 1N sulfuric acid and washed with deionized water. The aqueous layer was extracted, and the organic layer were combined, dried over MgSO 4 to yield compound of chemical formula 1. The yield was 90-95%.
EXAMPLE II
Synthesis of 2-(toluene-4-sulfonyloxy)ethyl methacrylate monomer
To 0.35 mole of triethylamine was added 0.35 mole of p-toluene sulfonylchloride followed by 0.3 mole of 2-hydroxyethyl methacrylate. The reaction mixture was stirred for over 24 hours with cooling and monitored by TLC. The reaction mixture was neutralized with 1N sulfuric acid and washed with deionized water. The aqueous layer was extracted, and the organic layers were combined, dried over MgSO 4 to yield compound of chemical formula 2. The yield was 90-95%.
EXAMPLE III
Synthesis of 3-(toluene-4-sulfonloxy)propyl acrylate monomer
To 0.35 mole of triethylamine was added 0.35 mole of p-toluene sulfonylchloride followed by 0.3 mole of 3-hydroxypropyl acrylate. The reaction mixture was stirred for 24 hours with cooling and monitored by TLC. The reaction mixture was neutralized with 1N sulfuric acid and washed with deionized water. The aqueous layer was extracted, and the organic layers were combined and dried over MgSO 4 to provide compound of chemical formula 3. The yield was 90-95%.
EXAMPLE IV
Synthesis of 3-(toluene-4-sulfonyloxy)propyl methacrylate monomer
To 0.35 mole of triethylamine was added 0.35 mole of p-toluene sulfonylchloride followed by 0.3 mole of 3-hydroxypropyl methacrylate. The reaction mixture was stirred for over 24 hours with cooling, and the reaction was monitored by TLC. The reaction mixture was neutralized with 1N sulfuric acid and washed with deionized water. The aqueous layer was extracted, and the organic layers were combined and dried over MgSO 4 to provide compound of chemical formula 4. The yield was 90-95%.
EXAMPLE V
Synthesis of poly [2-(toluene-4-sulfonyloxyl)ethyl acrylate/2-hydroxyethyl acrylate/-methyl methacrylate/-glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.25 mole of 2-hydroxyethyl acrylate, 0.1 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of 2,2-azobisisobutyronitrile (AIBN). The reaction mixture was heated to 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxyl)ethyl acrylate-/2-hydroxyethyl acrylate/-methyl methacrylate/-glycidyl methacrylate] represented by the following chemical formula 5, at a yield of 65-70%.
EXAMPLE VI
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/2-hydroxyethyl methacrylate/-methyl methacrylate/-glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.33 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.2 mole of 2-hydroxyethyl methacrylate, 0.15 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethylether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/2-hydroxyethyl methacrylate/-methyl methacrylate/-glycidyl methacrylate] represented by the following chemical formula 6, at a yield of 65-70%.
EXAMPLE VII
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/3-hydroxypropyl acrylate/-methyl methacrylate/-glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.25 mole of 3-hydroxypropyl acrylate, 0.1 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/3-hydroxypropyl acrylate/-methyl methacrylate/-glycidyl methacrylate] represented by the following chemical formula 7, at a yield of 65-70%.
EXAMPLE VIII
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/3-hydroxypropyl methacrylate-/methyl methacrylate-/glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.23 mole of 3-hydroxypropyl methacrylate, 0.1 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/3-hydroxypropyl methacrylate-/methyl methaclylate-/glycidyl methacrylate] represented by the following chemical formula 8, at a yield of 65-70%.
EXAMPLE IX
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/4-hydroxybutyl acrylate/-methyl methacrylate/-glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.2 mole of 4-hydroxybutyl acrylate, 0.1 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, and 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/4-hydroxybutyl acrylate/-methyl methacrylate/-glycidyl methacrylate] represented by the following chemical formula 9, at a yield of 65-70%.
EXAMPLE X
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/2-hydroxyethyl acrylate/-methyl methacrylate/-glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.25 mole of 2-hydroxyethyl acrylate, 0.15 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of 2,2-azobisisobutyronitrile (AIBN). The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexan, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/2-hydroxyethyl acrylate/-methyl methacrylate/-glycidyl methacrylate] represented by the following chemical formula 10, at a yield of 65-70%.
EXAMPLE XI
Synthesis of the poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/2-hydroxyethyl methacrylate-/methyl acrylate-/glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.2 mole of 2-hydroxyethyl methacrylate, 0.15 mole of methyl acrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethylether or n-hexane, filtered and dried to provide poly [2-toluene-4-sulfonyloxy)ethyl methacrylate/2-hydroxyethyl methacrylate-/methyl acrylate-/glycidyl methacrylate] represented by the following chemical formula 11, at a yield of 65-70%.
EXAMPLE XII
Synthesis of poly [2-(toluene-4-sulfonyloxy) ethyl methacrylate/3-hydroxypropyl acrylate-/methyl methacrylate-/glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.25 mole of 3-hydroxypropyl acrylate, 0.15 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/3-hydroxypropyl acrylate-/methyl methacrylate-/glycidyl methacrylate] represented by the following chemical formula 12, at a yield of 65-70%.
EXAMPLE XIII
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/3-hydroxypropyl methacrylate-/methyl methacrylate-/glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.22 mole of 3-hydroxypropyl methacrylate, 0.15 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/3-hydroxypropyl methacrylate-/methyl methacrylate-/glycidyl methacrylate] represented by the following chemical formula 13, at a yield of 65-70%.
EXAMPLE XIV
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/4-hydroxybutyl acrylate-/methyl methacrylate-/glycidyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.2 mole of 4-hydroxybutyl acrylate, 0.1 mole of methyl methacrylate, 0.3 mole of glycidyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/4-hydroxybutyl acrylate-/methyl methacrylate-/glycidyl methacrylate] represented by the following chemical formula 14, at a yield of 65-70%.
EXAMPLE XV
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/2-hydroxyethyl acrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.3 mole of 2-hydroxyethyl acrylate, 0.25 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/2-hydroxyethyl acrylate-/methyl methacrylate] represented by the following chemical formula 15, at a yield of 65-70%.
EXAMPLE XVI
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/2-hydroxyethyl methacrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.33 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.35 mole of 2-hydroxyethyl methacrylate, 0.25 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/2-hydroxyethyl methacrylate/-methyl methacrylate] represented by the following chemical formula 16, at a yield of 65-70%.
EXAMPLE XVII
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/3-hydroxypropyl acrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.33 mole of 3-hydroxypropyl acrylate, 0.22 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/3-hydroxypropyl acrylate/-methyl methacrylate] represented by the following chemical formula 17, at a yield of 65-70%.
EXAMPLE XVIII
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/3-hydroxypropyl methacrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.33 mole of 3-hydroxypropyl methacrylate, 0.25 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/3-hydroxypropyl methacrylate-/methyl methacrylate] represented by the following chemical formula 18, at a yield of 65-70%.
EXAMPLE XIX
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/4-hydroxybutyl acrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl acrylate, 0.3 mole of 4-hydroxybutyl acrylate, 0.3 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/4-hydroxybutyl acrylate/-methyl methacrylate] represented by the following chemical formula 19, at a yield of 65-70%.
EXAMPLE XX
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/2-hydroxyethyl acrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.25 mole of 2-hydroxyethyl acrylate, 0.3 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to produce poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/2-hydroxyethyl acrylate-/methyl methacrylate] represented by the following chemical formula 20, at a yield of 65-70%.
EXAMPLE XXI
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/2-hydroxyethyl methacrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.32 mole of 2-hydroxyethyl methacrylate, 0.3 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/2-hydroxyethyl methacrylate/-methyl methacrylate] represented by the following chemical formula 21, at a yield of 65-70%.
EXAMPLE XXII
Synthesis of poly [2-(toluene-4-sulfonyloxy) ethyl methacrylate/3-hydroxypropyl acrylate/-methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.33 mole of 3-hydroxypropyl acrylate, 0.3 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/3-hydroxypropyl acrylate/-methyl methacrylate] represented by the following chemical formula 22, at a yield of 65-70%.
EXAMPLE XXIII
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/3-hydroxypropyl methacrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy)ethyl methacrylate, 0.3 mole of 3-hydroxypropyl methacrylate, 0.3 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to produce poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/3-hydroxypropyl methacrylate/-methylmeth acrylate] represented by the following chemical formula 23, at a yield of 65-70%.
EXAMPLE XXIV
Synthesis of poly [2-(toluene-4-sulfonyloxy)ethyl methacrylate/4-hydroxybutyl acrylate-/methyl methacrylate]
In a 500 ml round-bottom flask was placed 0.3 mole of 2-(toluene-4-sulfonyloxy) acrylate, 0.33 mole of 4-hydroxybutyl acrylate, 0.3 mole of methyl methacrylate, 300 g of tetrahydrofuran (THF), and 0.1 g-3 g of AIBN. The reaction mixture was heated at 60-75° C. for 5-20 hours. The product was precipitated in ethyl ether or n-hexane, filtered and dried to provide poly [2-(toluene-4-sulfonyloxy)ethyl acrylate/4-hydroxybutyl acrylate/-methyl methacrylate] represented by the following chemical formula 24, at a yield of 65-70%.
EXAMPLE XXV
Preparation of ARC
A polymer (resin) having a chemical structure of general formula 1, as obtained in each of Examples V-XIV polymer (resin), is dissolved in 200-5,000% (w/w) of propyleneglycolmethyletheracetate (PGMEA). This solution is filtered, coated on a wafer, and hard-baked (i.e. heated at 100-300° C. for 10-1,000 sec). A photosensitive material may be applied on the anti-reflective coating thus formed, and imaged to ultrafine patterns in the conventional manner.
EXAMPLE XXVI
Preparation of ARC
A polymer (resin) having a chemical structure of the general formula 2, as obtained in each of Examples XV-XXIV is dissolved in 200-5,000% (w/w) of propyleneglycolmethyletheracetate (PGMEA). This solution, alone or in combination with 0.1-30% by weight of at least one cross-linker selected from the group consisting of acroleindimethylacetal, acroleindiethylacetal and melamine type cross-linker is filtered, coated on a wafer, and hard-baked (i.e. heated at 100-300° C. for 10-1,000 sec). A photosensitive material may be applied on the anti-reflective coating thus formed, and imaged to ultrafine patterns in the conventional manner.
As described hereinbefore, anti-reflective coating of the present invention, for example, coatings formed from the polymer resins of chemical formulas 5 to 24, contain phenyl groups pendant from the polymeric backbone which exhibit superior absorbency at 193 nm wavelength. Thus, an anti-reflective coating of the present invention can play an excellent role in forming ultrafine patterns. For example, it can prevent the back-reflection of light from the wafer surface and lower layers as well as eliminate the standing waves in the photoresist layer itself during a submicrolithographic process using a 193 nm ArF laser. This results in the formation of ultrafine patterns suitable for 64 M, 256 M, 1 G, 4 G, and 16 G DRAM semiconductor devices and a great improvement in the production yield.
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The present invention relates to organic anti-reflective coating polymers suitable for use in a semiconductor device during a photolithograhy process for forming ultrafine patterns using 193 nm ArF beam radiation, and preparation method therefor. Anti-reflective coating polymers of the present invention contain a monomer having a pendant phenyl group having high absorbency at the 193 nm wavelength. When the polymers of the present invention are used in an anti-reflective coating in a photolithography process for forming ultrafine patterns, the polymers eliminate the standing waves caused by changes in the thickness of the overlying photosensitive film, by the spectroscopic property of lower layers on wafer and by changes in CD due to diffractive and reflective light originating from the lower layers. Use of the anti-reflective coating of the present invention results in the stable formation of ultrafine patters suitable for 64M, 256M, 1G, 4G and 16G DRAM semiconductor devices and a great improvement in the production yield.
The present invention also relates to anti-reflective coating compositions containing these polymers and to the anti-reflective coatings formed from these compositions, as well as preparation methods therefor.
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CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of application Ser. No. 916,445, filed June 19, 1978 now abandoned.
BACKGROUND OF THE INVENTION
This invention relates to the field of inspection and particularly to the field of ultrasonic inspection of materials.
Conventional ultrasonic inspection techniques utilize a narrow beam of longitudinal or transverse type ultrasonic waves which is injected into the part being inspected by contacting the transducer with the part or by contacting the transducer with a transmitting medium, such as water, which also contacts the part. Such contact transducers generally employ piezoelectric crystals.
More recently, electromagnetic acoustic transducers (EMATs) have been developed which are capable of injecting ultrasonic waves into the part without any physical contact with the part. Because of the non-contact feature of such transducers, they are particularly useful in many nondestructive testing applications. One such electromagnetic transducer utilizes a periodic meander coil placed in a magnetic field. When an RF signal is applied to the meander coil, an ultrasonic wave is created in the test part, as described in U.S. Pat. No. 3,850,028.
A later developed type of electromagnetic acoustic transducer does not utilize a periodic meander coil. Rather, this type of transducer includes a row or stack of individual, alternately oriented permanent magnets which create a static, periodic magnetic field. One side of a coil is placed in the periodic magnetic field so that a sheet of current moves transverse to the magnetic field when a pulse of current flows through the coil. This latter type of transducer can be used to create horizontal shear (SH) waves and Lamb waves in an electrically conductive part, as described in U.S. Pat. No. 4,127,035.
The various EMATs described above are built with a particular periodicity D (determined by the spacing of a meander coil or of a row of magnets) which defines the wavelength, λ, of the ultrasonic wave which the EMAT is designed to generate. The frequency, f, used to generate the ultrasonic wave is then determined from the dispersion relationship between the wavelength, λ, and the velocity, v, of the wave in the particular material of the part being tested. The frequency of the fundamental horizontals hear wave mode, n=0, for example is given by the relationship v=λf. The relationship is more complex for higher order modes and is based on dispersion curves characteristic of the mode type.
Unfortunately, however, electromagnetic transducers exhibit a low efficiency in operation as compared to piezoelectric transducers, which makes it difficult to use an EMAT to locate small defects. Consequently, methods and apparatus for increasing the operating efficiencies of electromagnetic transducers and other transducers which operate with reduced efficiency are needed in the art.
SUMMARY OF THE INVENTION
It is a general object of this invention to provide an improved method for generating ultrasonic waves.
A method for generating an ultrasonic wave in a material having a thickness t includes, according to the present invention, the steps of:
(a) positioning a transducer near a surface of the material, the transducer being selected to induce a higher than fundamental mode wave in the material, and
(b) driving the transducer with an AC signal at a frequency which is selected to be above the minimum cutoff frequency for the higher mode wave but is sufficiently close to the cutoff frequency to drive the transducer with at least a preselected increase in efficiency relative to the efficiency attainable with a fundamental mode wave.
In more particular embodiments, the transducer may be configured to generate a higher mode Lamb wave or a higher mode horizontal shear wave. Where a horizontal shear wave is induced, the cutoff frequency f c is defined as:
f.sub.c =v.sub.s n/2t
where
v s =the velocity of the horizontal shear wave,
n=the integral mode number of the horizontal shear wave.
The driven frequency may be selected according to the radiated power expression ##EQU1##
Examples of the more important features of this invention have thus been broadly outlined in order that the detailed description which follows may be better understood, and so that the contributions which this invention provides to the art may be better appreciated. There are, of course, additional features of the invention which will be described herein, and which are included wihin the subject matter of the claims appended hereto.
BRIEF DESCRIPTION OF THE DRAWINGS
Additional objects, features, and advantages of the present invention will become apparent by referring to the following detailed description of the preferred embodiments in connection with the accompanying drawings, wherein like reference numerals refer to like elements throughout all the FIGURES. In the drawings:
FIG. 1 is a perspective view of a meander coil transducer for generating Lamb waves in a plate;
FIG. 2 is a perspective view of a periodic magnet transducer with a transverse winding for generating Lamb waves in a plate;
FIG. 3 is a perspective view of a periodic magnet transducer with a longitudinal winding for generating horizontal shear waves (or torsional waves in a tube);
FIG. 4 is a schematic drawing illustrating the interaction between eddy currents and a multiply reflected shear wave in a plate;
FIG. 5 depicts the relationship between frequency and wavelength in a 0.05 inch thick Inconel alloy plate for three modes of horizontal shear and Lamb waves;
FIG. 6 is a schematic of a test apparatus for practicing the invention; and
FIG. 7 shows the amplitude of a wave obtained utilizing the test apparatus of FIG. 6.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIGS. 1-3 show different types of electromagnetic acoustic transducers (EMATs) suitable for practicing the present invention. A meander coil 2, for example, when placed between the poles of a magnet 4, can be used to generate a Lamb wave 6 in a plate 8, as shown in FIG. 1. The wavelength, λ, of wave 6 is determined by the periodicity D of the meander coil 2.
Periodicity in the transducer can also be obtained by using a stack 10 of magnets 12, as shown in FIGS. 2 and 3. If a coil 14 is wrapped transversely to the stack 10, as illustrated in FIG. 2, then a Lamb wave 6 will be generated in the plate 8. If a coil 16 is wrapped longitudinally around a stack 18 of magnets, then a horizontal shear wave (a torsional wave in a tube) 22 is generated, as shown for the tube 24 in FIG. 3.
Other configurations and arrangements of electromagnetic transducers, as well as other types of transducers, can be utilized for practicing the invention, provided only that they are capable of inducing forces in the test part which will generate modes of vibration higher than the fundamental mode, generally n=1, 2, 3, 4, or 5.
Although noncontact transducers, such as the EMATs illustrated in FIGS. 1-3, are desirable for use in nondestructive testing applications, the low efficiency which has been demonstrated by such transducers relative to other transducers designs has heretofore been a disadvantage which has limited the useful applications of noncontact transducers. It is an outstanding feature of this invention, however, to provide an improved method by which the efficiency of operation of an ultrasonic transducer may be increased.
The principle on which the invention is based is illustrated in FIG. 4 in a perspective cross sectional view of a plate 8. A higher mode wave is shown as a reverberating shear wave 26 (the fuundamental mode wave would propagate down the plate without reflecting from the plate boundaries). It consists of an initial shear wave which strikes the back surface of plate 8 at an incident angle 28 and is reflected at the same angle. The superposition of these two waves, and their subsequent reflections, become the higher mode shear wave 26, which propagates down the plate at an effective velocity slower than the velocity of the fundamental shear wave in the material, as a consequence of the greater distance traveled by the wave as it reflects from surface to surface.
Forces exerted in alternating directions in the material are created by eddy currents which are induced in the plate by the periodicity of an electromagnetic transducer, as shown by the lines 30, 32. When the transducer is operated near the minimum frequency (the cutoff frequency) at which the higher mode will propagate, a resonant condition is created due to the interaction between the forces 30, 32 and the higher mode wave. Consequently, a transducer of finite length will interact with the wave during a number of reflections and thereby may be used to build up a large amplitude ultrasonic wave. The higher mode wave generation will cease when the angle 28 reaches 90°, at which point the reverberating wave does not propagate down the plate and the frequency of operation corresponds to the cutoff frequency. This resonance effect is analogous to a similar effect known to occur with microwaves travelling in a waveguide.
Tests have been performed using a periodic magnet transducer, such as that shown in FIG. 3, to generate torsional waves in the 0.05 inch thick wall of a 0.875 inch diameter Inconel alloy tube. For the n=0 mode, (i.e. no reflections of the wave from the walls of the tube) the signal-to-noise ratio for direct transmission between two transducers was measured at 30 dB. When tests were run in the n=1 mode near the minimum cutoff frequency, the signal-to-noise ratio was found to increase to 56 dB. In addition to being excited with greater efficiency, the higher order mode was also found to be more sensitive to defects located near the tube surface, since most of the ultrasonic energy is concentrated in the near-surface region for higher mode waves.
FIG. 5 provides a graphic illustration of the dispersion curves in a 0.05 inch thick Inconel plate for the symmetric and antisymmetric Lamb waves, represented by curves 34 and 36 respectively, and the horizontally polarized shear (SH) wave represented by curves 38. The minimum cutoff frequency f c for a particular mode is the frequency at which the slope of the curve is zero, as shown at frequencies 40-46 for various higher order modes. For a horizontally polarized shear wave, the cutoff frequency f c can be calculated from the equation:
f.sub.c =v.sub.s n/2t, (1)
where:
v s =the velocity of a shear wave in the material,
n=mode number≧1, and
t=thickness of the part.
Again in the case of horizontal shear waves, the range of enhanced efficiency may be characterized by proceeding from the expression for the total power P n radiated by a transducer operating in a mode n:
P.sub.n ∝ω.sup.2 /Y.sub.2n (2)
where
Y.sub.2n =ρωv.sub.s βnt/ε.sub.n
is an admittance parameter defined as the ratio of power carried per unit r..m.s. of surface displacement, and ##EQU2## Substituting in (2) for Y 2n and βn: ##EQU3## Further substitution in (3) for k s elimination of constants yields: ##EQU4##
Relationship (4) indicates that the radiated power theoretically reaches a maximum at the cutoff frequency (ω c =nπv s /t) and diminishes for frequencies higher than the cutoff frequency. Below the cutoff frequency, the expression is imaginary. Thus, the power expression confirms that a particular amount of enhanced transducer efficiency may be achieved by operating the transducer in a higher order mode at a frequency above the cutoff frequency for that mode but sufficiently close to the cutoff frequency to raise the efficiency to the desired level. For example, if twice the unenhanced efficiency is desired, the ratio P u /P.sub.ω=∞ is set equal to (2) and relationship (4) may be utilized to yield an upper frequency f u ##EQU5## Thus, in order to achieve this particular efficiency enhancement, the transducer would be operated at a frequency between f c and 1.15 f c .
The frequency f c and approximations for f u for Lamb wave modes and for the tube (torsional) modes obey similar, but mathematically more complex, relationships. For a particular type of wave, the frequency of the RF signal can be varied to generate higher order modes and the change in the amplitude or efficiency of wave generation may be measured as the frequency is varied. A rapid drop in amplitude indicates that the cutoff frequency has been reached.
The sensitivity of the efficiency/frequency relationship changes rapidly in the region very close to the cutoff frequency. Since the cutoff frequency varies inversely as the thickness of the material, normal variations in the material thickness can cause problems in the interpretation of data. However, such problems can be minimized if care is taken not to operate the transducer too close to the cutoff frequency, taking into consideration the variation in thickness of the material being inspected.
FIG. 6 is a schematic of a typical apparatus which may be used to practice the invention. A Matec RF pulse generator 48 supplies an AC signal at a selected frequency to the coil of an EMAT transmitter 50, which is placed in side a metal tube 52 being tested. This signal creates an acoustic wave 54, which travels in the tube 52 outward from the transmitter 50. An EMAT receiver 56 is placed in the tube to detect the acoustic wave 54 as it travels past receiver 56 and to detect the reflections or echoes of the wave 54 as they travel past the receiver 56. Receiver 56 may be similar in construction to transmitter 54, or a different type of EMAT can be used. The signal detected by the receiver 56 is amplified in a low noise amplifier 58 and displayed in an oscilloscope 60 or another suitable display device. For purposes of demonstration in a particular test which was conducted, a small hole 62 was drilled in the wall of the tube 52 to represent a defect in the test.
FIG. 7 shows typical ultrasonic wave forms which will be displayed by the oscilloscope 60 when the transmitter 50 is operated at two different frequencies in the arrangement shown in FIG. 6. The ultrasonicwave 54 was excited by an RF tone burst, and the 61 μsec width (at the -40 dB level) of the wave 54 transmitted directly between transmitter 50 and receiver 56 corresponded to a wave packet of spatial length equal to 7 inches along the tube. For this example, defects spaced closer than 3.5 inches along the tube axis would begin to overlap in time. Resolution of defects more closely spaced than 3.5 inches may be readily accomplished, however, by utilizing shorter transducers at the cost of lower sensitivity. The present invention provides for the recovery of the loss of efficiency which is suffered in the attempt to gain this increased sensitivity.
Since the higher order modes travel with a lower group velocity near the cutoff frequency, a second advantage is also realized with the present invention. For a given spatial resolution, a higher mode ultrasonic pulse will have a greater temporal duration than the fundamental mode. This means that the higher mode wave can be detected in a filter with a narrow bandwidth, thereby reducing noise and further improving sensitivity as compared to traditional techniques which operate with fundamental mode waves.
In FIG. 7, the first signal 68 represents the electrical feed-through which occurs when the transmitter electronics are activated. The next signal 70, at approximately 50 μsec, represents the ultrasonic wave which has propagated directly between transmitter 50 and receiver 56. In a system using a transmit-receive switch and a single transducer for both transmission and reception, this signal would occur at the same time as the feed-through signal 68 and hence would reduce the complexity of the display. Signal 72 illustrates the echo reflection from defect 62 and is of primary interest because it indicates the existence and location of the defect in the tube. Finally, signal 74 represents a reflection from the end of the tube.
The dashed trace 76 is typical in amplitude of signals obtained according to the prior art practice of selecting a frequency which will generate and receive the fundamental mode, n=0. It would also be typical for signals of higher order modes, n≧1, when the transmitter is not operated at frequencies sufficiently near the cutoff frequency f c .
The solid trace 78 is typical of the amplitude of a signal obtained when a higher order mode is excited at a frequency near its cutoff, according to the present invention. For comparison, the peaks of the signals are shown as occurring at the same time although there normally would be a small horizontal shift between the two methods depending upon the frequencies used. Clearly, trace 78 provides a much higher signal-to-noise ratio than does trace 76. This improvement, which is obtained by utilizing the method of the present invention, increases the available sensitivity of ultrasonic inspection techniques utilizing electromagnetic acoustic transducers and enables the artisan to take advantage of the noncontact characteristics of EMATs in applications requiring a level of sensitivity which was not attainable utilizing previous inspection techniques.
Numerous variations and modifications may be made without departing from the present invention. Accordingly, it should be clearly understood that the form of the present invention described above and shown in the accompanying drawings is illustrative only and is not intended to limit the scope of the present invention.
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Disclosed is a method for generating an ultrasonic wave in a material, utilizing a transducer adapted to induce a higher than fundamental mode wave in the material and a signal generator adapted to drive the transducer at a frequency above the cutoff frequency below which the higher mode wave will not propagate. For a horizontal shear wave, optimal transducer efficiency is obtained by selecting a driven frequency between a minimum cutoff frequency f c =v s n/2t and an upper frequency sufficiently close to f c to drive the transducer with at least a preselected increase in efficiency.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to construction, and more particularly, to a decking assembly and a method to construct a deck.
[0003] 2. Description of the Related Art
[0004] Several designs for decking systems have been designed in the past. None of them, however, include clips with tabs that frictionally fit into corresponding slots on the edge of planks or in keyholes on the underside of planks.
[0005] No other decking system designed in the past is as well suited for installations where the area adjacent to the footprint of the deck is limited. The present invention provides a cutout feature on the edge of the plank to facilitate the clip engaging into the plank.
[0006] None of the existing decking systems have ridges and nubs on clips to more securely hold planks to deck frame assembly. Said ridges also provide a gap between the clip and plank that reduces the risk of rot or discoloration of the plank.
[0007] Applicant believes that the closest reference corresponds to U.S. Patent Application Publication No. 2006/0283122 by Roy Burgess, Et. Al. However, it differs from the present invention because the Burgess application does not provide a clip with multiple fasteners, does not provide a clip with ribs or nubs and does not provide periodic cutouts or keyholes in the plank to facilitate engagement of the clip to the plank.
[0008] Another reference teaching a decking technology is found in U.S. Pat. No. 6,651,398 issued to Karl Gregory. However, it differs from the present invention because the Gregory patent does not provide a clip with multiple fasteners, does not provide a clip with ribs or nubs and does not provide periodic cutouts or keyholes in the plank to facilitate engagement of the clip to the plank.
[0009] Other patents describing the closest subject matter provide for a number of more or less complicated features that fail to solve the problem in an efficient and economical way. None of these patents suggest the novel features of the present invention.
SUMMARY OF THE INVENTION
[0010] It is one of the main objects of this invention to provide a decking system comprising a plurality of adjoining planks, each having a first side and an opposing second side, a top surface and a bottom surface, at least one of said opposing sides of each deck member having a slot therein, a plurality of clips each having a trunk and a head sized and configured so that said trunk is disposed between adjoining planks and said head is disposed into said slot in side of said planks and a substrate onto which said clips are affixed. In an alternate embodiment said clips have one or more parallel bores that terminate on the upper end off center on the upper side of said head and on the lower end in the center of the bottom side of said trunk. In another alternate embodiment the edges of the head of said clips have tabs and the slot in said planks have a complimentary profile to receive said tabs. In yet another embodiment the slot on said plank has intermittent cutouts on the bottom side of said slot dimensioned to fit over the head of said clips. In another embodiment said clips have ridges and/or nubs on said trunk and/or the underside of said head. In another embodiment the head of said clip is made of metal and the trunk of said clip is made of plastic.
[0011] Another object of the present invention is to provide a decking system comprising a plurality of adjoining planks, each having a first side and an opposing second side, a top surface and a bottom surface, said bottom surface of each deck member having a keyhole slot therein, a plurality of clips each having a trunk and a head sized and configured so that said head is disposed into said keyhole slot and a substrate onto which said clips are affixed.
[0012] Another object of the present invention is to provide a decking system comprising a plurality of adjoining planks, each having a first side and an opposing second side, a top surface and a bottom surface, said bottom surface of each deck member having a slot therein, a plurality of clips each having a trunk and a head sized and configured so that said head is disposed into said slot and a substrate onto which said clips are affixed.
[0013] It is one of the objects of the present invention to provide a decking assembly and method of installing said decking assembly.
[0014] It is another object of this invention to provide a decking assembly that securely holds plank to the deck substrate.
[0015] It is still another object of the present invention to provide a decking assembly that reduces the visibility of decking hardware on the finished deck.
[0016] It is another object of this invention to provide a decking system that permits the easy replacement of individual planks.
[0017] It is an object of this invention to provide a decking system with a clip that reduces the occurrence of rot and discoloration of the plank.
[0018] It is an object of this invention to provide a decking system that can be installed in a confined area.
[0019] It is another object of this invention to provide a decking system that reduces the possibility of fasteners backing-out and thereby reduces a hazard to a user.
[0020] It is yet another object of this invention to provide such an assembly that is inexpensive to manufacture and maintain while retaining its effectiveness.
[0021] Further objects of the invention will be brought out in the following part of the specification, wherein detailed description is for the purpose of fully disclosing the invention without placing limitations thereon.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] With the above and other related objects in view, the invention consists in the details of construction and combination of parts as will be more fully understood from the following description, when read in conjunction with the accompanying drawings in which:
[0023] FIG. 1 shows an exploded perspective view of an embodiment of the present invention.
[0024] FIG. 2 is an elevation view of a series of clips and planks.
[0025] FIG. 3 is a cross section of a perspective view of an alternate embodiment of a deck clip.
[0026] FIG. 4 is a perspective view of a deck clip attached to a substrate.
[0027] FIG. 5 represents a perspective view of an alternate embodiment a clip.
[0028] FIG. 6 shows a perspective view of the bottom side of the clip shown in FIG. 5 .
[0029] FIG. 7 illustrates a perspective view of an alternate embodiment of a clip.
[0030] FIG. 8 shows a perspective view of the bottom side of the deck clip shown in FIG. 7 .
[0031] FIG. 9A is a perspective view of the bottom side of an alternate embodiment of a clip.
[0032] FIG. 9B is a perspective view of an alternate embodiment of a clip.
[0033] FIG. 10A is a perspective view of an alternate embodiment of a clip.
[0034] FIG. 10B is a perspective view of plank used with the clip shown in FIG. 10A .
[0035] FIG. 10C is a perspective view of an embodiment of a clip used with the plank shown in FIG. 10B .
[0036] FIG. 11A is a perspective view of an alternate embodiment of a clip.
[0037] FIG. 11B is a perspective view of plank used with the clip shown in FIG. 11A .
[0038] FIG. 11C is a perspective view of an embodiment of a clip used with the plank shown in FIG. 11B .
[0039] FIG. 12A is a perspective view of an alternate embodiment of a clip.
[0040] FIG. 12B is a perspective view of plank used with the clip shown in FIG. 12A .
[0041] FIG. 12C is a perspective view of an embodiment of a clip used with the plank shown in FIG. 12B .
[0042] FIG. 13 is a perspective view of the bottom side of an alternate embodiment of a plank.
[0043] FIG. 14 is a perspective view of the bottom side of an alternate embodiment of a plank.
[0044] FIG. 15 is a perspective view of an alternate embodiment of a clip.
[0045] FIG. 15A is a perspective view of an alternate embodiment of plank used with the clip shown in FIG. 15 .
[0046] FIG. 16 is a perspective view of the bottom side of an alternate embodiment of a plank.
[0047] FIG. 16A is a perspective view of an alternate embodiment of a clip.
[0048] FIG. 17 is a perspective view of the bottom side of an alternate embodiment of a plank.
[0049] FIG. 18 is a plan view of the bottom side of the plank shown in FIG. 17 .
[0050] FIG. 19 is a perspective view of the bottom side of an alternate embodiment of a clip.
[0051] FIG. 20 is a cross-section of a perspective view of the clip shown in FIG. 19 .
[0052] FIG. 21 shows a perspective view of the preferred embodiment of a clip.
[0053] FIG. 22 shows a cross sectional perspective view of the deck clip shown in FIG. 21 .
[0054] FIG. 23 shows a perspective view of an alternate embodiment of a deck clip.
[0055] FIG. 24 is an elevation view of a series of clips and planks.
[0056] FIG. 25 shows a perspective view of an alternate embodiment of a clip.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0057] Referring now to the drawings, where the present invention, a decking system, as shown in FIG. 1 is generally referred to with numeral 10 , it can be observed that it basically includes a plurality of clips 204 that attach planks 206 to a plurality of joists 202 which act as a substrate.
[0058] In a typical installation a deck frame assembly 200 is constructed to support planks 206 . The deck frame assembly 200 is comprised of, inter alia, a plurality of joists 202 that are attached at each end to a girder 210 by a fastener 208 to form a unitary frame. Said fastener 208 may be a nail, screw, bolt, hanger or other fastener or adhesive. A plurality of clips 204 are attached to the top side of said joists 202 . In the embodiment of the present invention shown in FIG. 1 said plank 206 slides onto the clips 204 to hold the plank 206 securely to the joists 202 . Clips 204 on a joist 202 are typically spaced apart a distance complimentary to the width of the planks 206 .
[0059] Said plank 206 , in this embodiment or any of the following embodiments, is typically is made of natural wood and also could be made of any of a wide variety of natural woods, engineered wood products, composite boards, synthetic boards, polymer boards, metal, stone, masonry, glass or any other suitable solid material.
[0060] FIG. 2 illustrates an embodiment of the present invention where end-clips 222 and clips 226 interface with planks 220 . The shape of the edge of the plank 220 is formed to complement the shape of the head of the end-clips 222 and clips 226 and firmly hold the plank to the deck frame assembly 200 as shown in FIG. 1 . In one possible configuration of the invention the end-clip 222 secures the plank 220 on the edge of the frame assembly 200 and the clips 226 are utilized between planks 220 . Both the end-clips 222 and the clips 226 are secured to a joist by a fastener 224 such as a screw, nail, bolt, adhesive or other fastener.
[0061] FIG. 3 shows a fastener 246 , in this example a screw, penetrating a clip through a bore 248 that passes through the head 240 and trunk 244 of the clip. Optionally, the top side of the bore 248 is countersunk to permit the head of the fastener 246 to be flush with the top surface of the head 240 .
[0062] Now referring to FIG. 4 where a clip 264 is shown attached to a joist 260 with a fastener 262 . Said clip 264 is oriented on said joist 260 to permit the longer dimension of a plank 206 (shown in FIG. 1 ) to be oriented perpendicular to the longer dimension of the joist 260 . Said fastener 262 may be a screw, nail, bolt, adhesive or other fastener.
[0063] Referring to FIG. 5 where an embodiment of a clip is shown that comprises, inter alia, a trunk 100 and a head 102 . Extending through the height of the trunk 100 and head 102 is a bore 104 . The bore 104 is dimensioned to receive a fastener, such as a screw, nail, bolt or other fastener. Optionally, there are ridges 106 formed integrally with the vertical surface on the side of the trunk 100 . Said ridges 106 act to maintain an airspace between the trunk 100 and a plank (not shown in FIG. 5 ). Said ridges 106 may also improve the frictional grip the trunk 100 has with plank (not shown in FIG. 5 ).
[0064] The clip shown in FIG. 5 , or any of the variations and embodiments of the clip, may be made out of a wide variety of rigid or semi-rigid materials. A preferred material for many applications is a single piece of synthetic polymer or metal. For some applications it may be preferable to fabricate the clip shown in FIG. 5 from multiple materials such as, for example, a synthetic trunk 100 and a metallic head 102 .
[0065] Now referring to FIG. 6 where the bottom side of the clip in FIG. 5 is shown. In this view said ridges 106 are shown in more detail. On the bottom side of said head 102 are optional nubs 108 . The nubs 108 promote airflow and grip between anything coming into contact with the head 102 . The interior of the trunk 100 may optionally have a cavity 112 to lighten the clip and reduce the material necessary to construct the clip. A rib 110 may span the width of the trunk 100 to add strength and rigidity to the clip. The rib 110 may also be traversed by a bore 104 dimensioned to accept a fastener as pass through the clip from the top to the bottom and into a substrate. Any of the various embodiments of the clips as shown in the following figures may optionally also include a cavity and rib similar to the cavity 112 and rib 110 as shown in FIG. 6 .
[0066] FIGS. 7 and 8 show an alternate embodiment of a clip that is comprised of, inter alia, a trunk 118 , a head 116 , tabs 114 , bores 120 , nubs 124 and ridges 122 . Said bores 120 pass through the head 116 and through the bottom surface 126 of the trunk 118 . Optionally, the upper end of the bore 120 me be counter sunk to permit a fastener to be flush to the surface of the head 116 . Each of the outer edges of the head 116 has a tab 114 to enhance the engagement of the tab 114 with a plank. The bottom surface of the head has raised nubs 124 and the side walls of the trunk has ridges 122 that, inter alia, hold a plank apart from the clip to provide drainage, airflow and an improved frictional grip.
[0067] FIG. 9A shows the bottom side of an embodiment of a clip comprising, inter alia, a trunk 164 , a head 166 and bores 162 . The trunk 164 has a bottom surface 160 where said bores 162 terminate. Said bores 162 are dimensioned to accept a fastener such as a screw, bolt, nail, adhesive or other fastener. For some decks it may be preferable for the clip to have a single bore instead of the two bores 162 shown in FIG. 9A . Any of the clips described above or below may have one or two bores dimensioned to accept a fastener.
[0068] Now referring to FIG. 9B where an alternate embodiment of a clip is shown comprising, inter alia, of a trunk 182 , a head 180 and a bore 184 . The bore 184 passes through the trunk 182 and head 180 . Said bore 184 is dimensioned to accept a fastener such as a screw, bolt, nail, adhesive or other fastener.
[0069] FIG. 10A shows an embodiment of a clip 300 comprised of, inter alia, a head 302 , a trunk 308 and a bore 304 . FIG. 10B shows a portion of a plank 310 with a slot 312 . The clip 300 in FIG. 10A is typically used in conjunction with the plank 310 with slot 312 shown in FIG. 10B . In typical use a fastener is placed through the bore 304 on the clip 300 to secure the clip 300 to a substrate such as the joist 260 in FIG. 4 . The edge of the head 302 engages into the slot 312 to hold the plank 310 to a joist. The height of the trunk 308 is dimensioned to position the head 302 at the same height as the slot 312 . FIG. 10C shows an embodiment of an end-clip comprising a trunk 400 , head 408 and bore 406 . The end clip shown in FIG. 10C can be used where a plank such as the example in FIG. 10B is only placed on one side of the end-clip and the head 408 engages slot 312 .
[0070] FIG. 11A shows an embodiment of a clip 330 comprised of, inter alia, a head 332 , a trunk 342 , a tab 334 , a tab 340 and bores 338 . FIG. 11B shows a portion of a plank 346 with a slot 348 . The clip 330 in FIG. 11A is typically used in conjunction with a plank 346 with a slot 348 shown in FIG. 11B . In typical use fasteners are placed through the bores 338 on the clip 330 to secure the clip 330 to a joist such as the joist 260 in FIG. 4 . The edge of the head 332 and the tab 340 engage into the slot 348 to hold the plank 346 to the joist. Tab 334 engages into another section of plank 346 . The height of the trunk 342 is dimensioned to position the head 332 , tab 334 and tab 340 at the same height as the slot 348 . FIG. 11C shows an embodiment of an end-clip comprising a trunk 434 , head 420 , tab 428 and bores 432 . The end-clip shown in FIG. 11C can be used where a plank such as the example in FIG. 11B is only placed on one side of the end-clip and the head 420 and tab 428 engage slot 348 .
[0071] FIG. 12A shows an embodiment of a clip 360 comprised of a head 364 , a trunk 372 , a tab 362 , a tab 370 and a bore 366 . FIG. 12B shows a portion of a plank 382 with a slot 380 . The clip 360 in FIG. 12A is typically used in conjunction with the plank 382 with slot 380 shown in FIG. 12B . In typical use a fastener is placed through the bore 366 on the clip 360 to secure the clip 360 to a joist such as the joist 260 in FIG. 4 . The edge of the head 364 and the tab 370 engage into the slot 380 to hold the plank 382 to the joist. Tab 362 engages into another piece of plank 346 . The height of the trunk 372 is dimensioned to position the head 364 , tab 362 and tab 370 at the same height as the slot 380 . FIG. 12C shows an embodiment of an end-clip comprising a trunk 450 , head 448 , tab 442 and bores 452 . The end clip shown in FIG. 12C can be used where a plank such as the example in FIG. 12B is only placed on one side of the end-clip and the head 448 and tab 442 engage slot 380 .
[0072] Referring to FIG. 13 , a perspective view of an alternate embodiment of a plank 474 is shown. On the bottom edge 470 is a keyhole 476 that is comprised of an edge 468 , an edge 464 , an edge 482 , an edge 477 , a tab 460 and a tab 462 . Said edges 468 , 464 , 482 , 477 have a height less than that of edge 478 of the plank 474 so that the depth of the keyhole 476 does not extend entirely through the plank 474 and the upper surface 472 remains intact. This embodiment can be best used with a clip such as the clips as shown in any one of FIG. 9B , 10 A, 16 A, 19 , 21 , 23 or 25 but other clip shapes may also work well in particular decking applications. In a typical installation of this embodiment of the plank 474 , clips such as the clip shown in FIG. 23 are fastened to joists similar to the configuration in FIG. 1 of joists 202 , clips 204 and girders 210 . Keyholes 476 are spaced periodically on the bottom edge 470 of the plank 474 at the same distance apart as the joists 202 are spaced apart. The clips 204 are fastened to the joists 202 along the top of the joists 202 . The clips 204 are spaced apart on a joist 202 sufficiently to permit a series planks 474 to be laid side by side in contact with the joists 202 . To secure a plank 474 to the joists 202 the wider part of the keyhole 476 is fit over the head 786 of the clip shown in FIG. 23 . The plank is then slid so that said tab 460 and tab 462 fit under the head 786 of the clip thereby preventing the plank 474 from lifting away from the joists 202 . To remove or replace any of the planks 474 the individual plank 474 can simply be slid to permit the clip to be removed from the keyhole 476 without the necessity of removing adjacent planks 474 .
[0073] Referring to FIG. 14 , a perspective view of an alternate embodiment of a plank 500 is shown. On the bottom edge 514 is a keyhole 506 that is comprised of an edge 508 , a tab 510 and a tab 512 . Said edge 508 has a height less than that of edge 502 so that the keyhole 506 does not extend entirely through the plank 500 and the upper surface 504 remains intact. This embodiment can be best used with a clip such as the rounded head clips as shown in any one of FIG. 9B , 16 A, 23 or 25 but other clip shapes may also work well in particular decking applications. In a typical installation of this embodiment of the plank 500 , clips such as the clip shown in FIG. 9B are fastened to joists similar to the configuration in FIG. 1 of joists 202 , clips 204 and girders 210 . Keyholes 506 are spaced periodically on the bottom edge 514 of the plank 500 at the same distance apart as the joists 202 are spaced apart. The clips 204 are fastened to the joist 202 along the top of the joist 202 . The clips 204 are spaced apart on a joist 202 sufficiently to permit a series of planks 500 to be laid side by side in contact with the joists 202 . To secure a plank 500 to the joists 202 the wider part of the keyhole 506 is fit over the head 180 of the clip shown in FIG. 9B . The plank is then slid so that said tab 510 and tab 512 fit under the head 180 of the clip thereby preventing the plank 500 from lifting away from the joists 202 . To remove or replace any of the planks 500 the individual plank 500 can simply be slid to permit the clip to be removed from the keyhole 506 without the necessity of removing adjacent planks 500 .
[0074] Another advantage of the keyhole design as shown in FIGS. 13 and 14 is that the plank may be installed where there is limited area around the deck because the plank need only be slid, for example, a few inches to engage a clip within the keyhole contrasted to sliding the plank the entire length of the plank as necessary for some of the other embodiments of this invention described herein.
[0075] Referring now to FIGS. 15 and 15A where yet another embodiment of a clip 558 and a plank 584 combination is shown. Said clip 558 is comprised of, inter alia, a trunk 560 , bores 566 , tab 556 , tab 550 , a head 564 and nubs 552 . Said bores 566 go through the head 564 and trunk 560 . Said bores are dimensioned to accept a fastener such as a bolt, screw, nail or other available fastener. Said bores 566 optionally have a countersink in the end near the head 564 to permit a fastener to fall flush to or below the surface of the head 564 . Said tabs 556 and 550 optionally have a series of nubs 552 comprised of protrusions on the upper edges of tabs 556 and 550 to create a gap and increase the strength of the connection when the clip 558 is engaged into a plank 584 . Optionally ridges may be formed into the trunk 560 similar in form the ridges 106 shown in FIG. 6 . In a preferred embodiment of the clip 558 the entire clip 558 is made out of a synthetic polymer or plastic. In another preferred embodiment the clip 558 could be made out of metal or a metal alloy. In yet another preferred embodiment the clip 558 has a head 564 of metal and the balance made of a polymer.
[0076] Said plank 584 has, inter alia, an upper surface 570 , slot 578 , tab 586 , roundover 572 , tab 582 and slot 580 . In a preferred embodiment at least two clips 558 are used to secure a plank 584 to a joist. A typical application of this embodiment is shown in FIG. 1 where the clip 204 and the plank 206 in FIG. 1 are replaced by clip 558 and plank 584 , respectively. Clips 558 are fastened to the joists 202 and the plank 584 is slid between clips 558 where tab 550 fits under tab 586 and edge 562 fits into slot 578 . Another clip 558 similarly fits into slot 580 and tab 582 on the opposite edge of the plank 584 . Said roundover 572 is primarily cosmetic and may optionally be present on the plank 584 . In a preferred embodiment said plank 584 is constructed of solid wood but may also be made of engineered wood, synthetic material, metal, masonry or other solid material.
[0077] FIGS. 16 and 16A show another alternate embodiment of a complimentary plank 624 and clip 628 . Said plank 624 is comprised of, inter alia, a bottom surface 622 , tab 620 , tab 614 , top surface 602 and slot 608 . Said slot 608 is formed along the length of the plank 624 . Said tab 620 and tab 614 partially cover the slot 608 . Said clip 628 is comprised of, inter alia, bores 640 , head 638 and trunk 630 . In the preferred application of the clip 628 , a series of clips 628 are fastened to joists similar to the joists 202 in FIG. 1 . The head 638 of the first clip 628 in the series of clips is slid into the slot 608 of the plank 624 and the trunk 630 is fit between tab 620 and tab 614 to secure the plank 624 to the joist 202 . The plank 624 is successively slid onto subsequent clips 628 to secure the plank 624 to the joists 202 . In one of the preferred embodiments the clip 628 is made of plastic but it could also be effective if made out of any rigid polymer, metal or other solid material or combination of solid materials.
[0078] Now referring to FIGS. 17 and 18 where an alternate embodiment of a plank 701 is shown that is comprised of, inter alia, a lower tab 704 , an upper tab 710 , a slot 708 and cutouts 702 . Said slot 708 is bounded by the lower tab 704 and the upper tab 710 . In the preferred embodiment the plank 701 is made from wood, engineered wood, polymer, metal or masonry but any other solid material could be utilized.
[0079] The plank 701 is used similar to the deck frame assembly 200 in FIG. 1 where clips 204 are fastened to joists 202 that are supported by girders 210 . In the preferred embodiment the plank 701 is secured by a clip (for example, the clips shown in any of FIG. 5 , 6 , 9 A, 9 B, 10 A, 16 A or 19 , but any clip with a head complimentary to the slot 708 could be used) to a joist 202 . Said cutouts 702 are positioned periodically on the lower tab 704 and are spaced apart the equal to the distance between the joists 202 . When installing the plank 701 the cutouts 702 are fit over the clips 204 and the bottom surface 700 of the plank 701 rests on to the joists 202 . The plank 701 is slid along the top of the joists 202 so that the head of the clips fit into the slot 708 between the upper tab 710 and lower tab 704 .
[0080] Referring to FIGS. 19 and 20 where an alternate embodiment of a clip 744 is shown comprising, inter alia, a trunk 742 , a tab 740 , a tab 746 , cutouts 748 and bores 750 . In this embodiment of the clip 744 the bores 750 are dimensioned to accept a fastener such as a screw, nail or bolt. Said bores 750 pass through the trunk 742 from the side of the trunk 742 under the tab 746 to the bottom surface of the trunk 754 . Said tab 746 has cutouts 748 adjacent to the bores 750 to permit passage of a fastener and a tool to secure the fastener. One of the advantages of the position of the bores 750 is to permit a plank, such as the plank 310 shown in FIG. 10B , to be laid onto a supporting joist before the clip 744 . In this installation method a plank, for example plank 310 , is laid onto a joist then a first clip 744 is inserted into the slot 312 and fastened to the joist. Then a second plank 310 is laid onto the joist and its slot 312 is pressed into the first clip 744 and a second clip 744 is inserted into the slot 312 on the side of plank 310 opposite the first clip 744 and the second clip 744 is then fastened to the joist to secure the second plank 310 . This method is repeated until the planks 310 cover the substrate. The installation method described above is similar to that shown and described below in FIG. 24 .
[0081] Now referring to FIGS. 21 and 22 where the preferred embodiment of a clip 768 is shown that comprises, inter alia, a bore 778 , a trunk 772 and a head 770 . Said trunk optionally includes a series of ridges 776 to provide an airspace between the clip 768 and any plank material. One of the distinguishing features of this clip 768 is that the bore 778 passes through the head 770 off of center and exits through the bottom side of the trunk 772 at or near its center. Similar to the clip 300 shown in FIG. 10A , clip 768 could have multiple bores 778 , each angled through the trunk 772 . Said bore 778 is dimensioned to accept a fastener 774 such as a screw, bolt, nail or other similar means. Optionally, the upper end of the bore 778 may have a countersink to permit the head of the fastener 774 to fall below the surface of the head 770 . In a preferred embodiment, this clip 768 is made of plastic or metal but could also be made of any durable, rigid material or combination of materials.
[0082] FIG. 23 is an alternate embodiment of a clip that comprises, inter alia, a trunk 782 , a bore 784 and a head 786 . The distinguishing feature that this clip demonstrates is the rounded shape of the head 786 as well as the angular edge 780 of the head 786 . The edge 780 may facilitate the clips engagement into the slot of any of the above-described planks. As in other clips described above, this clip may have more than one bore and/or have the bores at an angle not perpendicular to the surface of the head 786 .
[0083] FIG. 24 is an alternate embodiment of a clip that comprises, inter alia, a trunk 802 , a bore 806 and a head 800 . The distinguishing feature that this clip demonstrates is the rounded shape of the head 800 as well as the angular edge 804 of the head 800 . The edge 804 may facilitate the clips engagement into the slot of any of the above-described planks. As in other clips described above, this clip may have more than one bore and/or have the bores at an angle not perpendicular to the surface of the head 800 .
[0084] FIG. 24 is an illustration of an example of a method to install a deck comprising, inter alia, plank 790 , plank 791 , clip 793 , clip 794 , slot 795 , slot 796 , slot 797 and fasteners 792 . This method is one of the preferred methods used with clips that have bores at an angle not perpendicular to the surface of the head of the clip such as the clips shown in FIG. 19 or 21 .
[0085] In this installation method a plank 791 is laid onto a joist then the slot 795 is fit into a first clip 794 . Then a second clip 793 is fitted into slot 796 on plank 791 and fastened with fastener 792 to the joist below. Then the next plank 790 is laid onto the joist and its slot 797 is fitted into the second clip 793 . This method is repeated by laying subsequent planks and then clips until the deck is completed.
[0086] Generally, any of the various embodiments of the clips described above in this invention can have one or more bores, any of the shapes of the edges of their head, have ridges and/or nubs, bores can be perpendicular to the head or angular respective to the head and be made out of any of the described materials or combination of materials. Likewise, the planks can be made out of any solid material that can be shaped to have the planks slot interface with the clip.
[0087] The foregoing description conveys the best understanding of the objectives and advantages of the present invention. Different embodiments may be made of the inventive concept of this invention. It is to be understood that all matter disclosed herein is to be interpreted merely as illustrative, and not in a limiting sense.
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A decking system that consists of a clip that complements a slot in deck planks to securely fasten the deck planks to a substrate such as deck or floor joists, masonry, concrete, wood or any other substrate. Generally, the clips fit into slots cut or formed into the side deck surface boards or alternatively into a keyhole on the bottom of the plank. In one of the preferred embodiments a series of clips are fastened to the substrate with a fastener such as a screw. The clips mechanically grip the plank to secure the plank to the deck joists. Ridges and/or nubs on the clips reduce the occurrence of rot or discoloration of the planks.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention pertains to the field of urethane catalysts. More particularly, this invention relates to the use of certain dimethylamino polyalkyleneoxy isopropanols as catalysts for preparing polyurethane foam.
2. Description of Related Art
The use of a catalyst when preparing polyurethanes by reacting a polyisocyanate with an active hydrogen-containing compound, as measured by the Zerewitinoff method, such as a polyol, and other optional ingredients, is known. Catalysts are employed to promote at least two, and generally three, major reactions. These reactions must proceed simultaneously and at competitively balanced rates during the process in order to yield a polyurethane with desired physical characteristics.
One reaction is a chain extending isocyanate-hydroxyl reaction by which a hydroxyl-containing molecule is reacted with an isocyanate-containing molecule to form the urethane. The progress of this reaction increases the viscosity of the mixture and forms a polyurethane containing a secondary nitrogen atom in the urethane groups.
A second reaction is a cross-linking isocyanate-urethane reaction wherein an isocyanate-containing molecule reacts with the secondary nitrogen atom of the urethane group. The third reaction, which often is important, particularly when the preparation of flexible polyurethane foam is desired, comprises an isocyanate-water reaction wherein an isocyanate-terminated molecule is extended and by which carbon dioxide is generated to "blow" or assist in the "blowing" of the foam. The in-situ generation of carbon dioxide by this reaction plays an essential part in the preparation of "one-shot" flexible polyurethane foams.
In order to obtain a good urethane foam structure, these reactions must proceed simultaneously at optimum balanced rates relative to each other. For example, if the carbon dioxide evolution is too rapid in comparison with the chain extension reaction, the foam tends to collapse. Alternatively, if the chain extension reaction is too rapid in comparison with the reaction that generates carbon dioxide, foam rise will be restricted, thus resulting in a high-density foam with a high percentage of poorly defined cells. Finally, if crosslinking reactions, including the second reaction, do not keep pace with the first or third reactions, the foam may not be stable because of the absence of adequate cross-linking.
It has long been known that tertiary amines, such as trimethylamine, triethylamine, tetramethylpropanediamine, triethy lenediamine, dimethylethanolamine, methyltriethylenediamine, N-methylmorpholine, N-ethylmorpholine and the like are effective for catalyzing the cross-linking isocyanate-urethane reaction. Many of the tertiary amines also are effective for catalyzing the water-isocyanate reaction that causes carbon dioxide evolution. A variety of tertiary amine catalysts are disclosed in U.S. Pat. Nos. 3,476,933, 3,925,268, 3,127,436 and 3,243,389.
However, tertiary amines are only partially effective as catalysts for the chain extension reaction and thus normally are used in combination with other catalysts, typically an organic tin catalyst. For example, in the preparation of flexible foams, a one-step or "one-shot" process has long been used wherein triethylenediamine is employed for promoting the water-isocyanate reaction and the crosslinking reaction; while an organic tin compound is used in synergistic combination with the triethylenediamine to promote the chain extension reaction.
One problem with triethylenediamine and other similar materials is that they are solids and must be dissolved prior to use to avoid processing difficulties such as non-homogeneous reactions. Also, triethylenediamine and many of the other prior art amines impart a strong amine odor to the polyurethane foam. In addition to odor and handling problems, certain other tertiary amines are very high in relative volatility and present significant safety and toxicity problems.
U.S. Pat. No. 2,941,967 discloses a process for catalytically enhancing the reaction of an isocyanate with a polyol by including mono and diamino ethers, e.g., dimethyl-(2-methoxyethyl)-amine and bis-(3-dimethylaminopropyl)ether as a catalytic component.
U.S. Pat. Nos. 3,330,782 and 3,480,675 disclose using tertiary amine ethers as catalysts for the reaction of organic polyisocyanates with active hydrogen-containing compounds. In the '782 patent, beta-(N,N-dimethylamino) alkyl ethers are used as catalysts for the urethane reaction.
U.S. Pat. No. 3,622,542 and U.S. Pat. No. 4,495,081 disclose using N,N'-tetramethyl-2-hydroxy-1,3-diaminopropane as a catalyst for preparing polyurethane foams.
U.S. Pat. No. 3,632,707 uses a mixture of trimethylaminoethylpiperazine and dimethylamino ethanol as a catalyst for preparing flexible polyurethane foam from a polyether polyol using the "one shot" process.
U.S. Pat. No. 3,645,925 discloses an amine catalyst for a polyurethane reaction consisting of a 4,4'-dimorpholinodiethyl ether. Its use in combination with other tertiary amines also is disclosed.
U.S. Pat. No. 3,786,029 describes using amino-orthoesters, prepared by reacting amino alkanols, such as 1-methyl-2-(N,N-dimethylaminoethoxy) ethanol, with an orthoester, as catalysts for polyurethane formation.
U.S. Pat. Nos. 4,410,466 and 4,101,470 describe certain bis(dimethylaminopropyl)-amine derivatives which include ethers and alcohol-terminated compounds. These components are alleged to have catalytic activity for urethane synthesis.
U.S. Pat. Nos. 4,419,461 and 4,421,869 disclose using the combination (i.e. a partial salt) of 3-dimethylaminopropylamine and either a branched octanoic acid or phenol as a catalyst for preparing polyurethane foam.
U.S. Pat. No. 4,582,938 also relates to certain bis(dialkylaminoethyl) polyamine ethers useful as catalysts for urethane synthesis.
Included among the above catalysts useful for urethane synthesis are tertiary amines having active hydrogens, which thus are reactive with isocyanate groups. Such tertiary amines include triethanolamine; triisopropanolamine; N-methyldiethanolamine; N-ethyldiethanolamine; N,N-dimethylethanolamine and their reaction products with alkylene oxides such as propylene oxide and/or ethylene oxide. See, for example, U.S. Pat. Nos. 3,669,913; 3,793,237; 4,190,417 and 4,304,872.
Polyamines also have been used as the active hydrogen-containing reactant for preparing polyurethanes. U.S. Pat. No. 2,697,118 describes using N,N,N',N'-tetrakis-(2-hydroxypropyl)-ethylene diamine. U.S. Pat. No. 3,697,458 uses the propoxylated adduct of the reaction product of a dialkanolamine and an epihalohydrin. U.S. Pat. No. 3,330,782 discloses using the alkylene oxide adducts of trialkanolamines. U.S. Pat. No. 3,847,992 uses partially aminated polyoxyalkylene polyols containing primary hydroxyl groups and possibly some terminal secondary hydroxyl groups. See also U.S. Pat. Nos. 3,125,540; 3,383,351 and 3,404,105 and G.B. Patent No. 1,028,810.
DESCRIPTION OF THE INVENTION
The present invention is directed to a particular class of reactive polyurethane catalysts which exhibit an excellent balance between their promotion of the isocyanate-water reaction and their own reactivity with isocyanates. The catalysts of the invention primarily catalyze the reaction between isocyanate and water. Their reactivity with isocyanates is low enough that the catalysts are not consumed until substantially all of the water has been reacted with isocyanate for foaming the polyurethane. Thus, the catalysts of the present invention are able to satisfy their primary function, i.e., catalyzing the isocyanate-water reaction, and still react into the urethane molecule to reduce amine-odor problems.
The reactive dimethylamino polyalkyleneoxy isopropanol catalysts of this invention have the following structural formula: ##STR1## where X is at least 1 and Y is at least 1. Preferably, X is 1 to 5 and/or Y is 1 to 5, more preferably X is 1 to 3 and Y is 1 to 2, most preferably X is 1 to 2 and Y is 1.
These compounds may be prepared using a wide variety of known synthetic techniques. For example, the reactive polyurethane catalysts of this invention can be prepared by reacting dimethylethanolamine (DMEA) or an ethylene oxide adduct of dimethylethanolamine with propylene oxide. Suitable reactive polyurethane catalysts according to the present invention also can be prepared by reacting bis-2-(N,N'-dimethylamino) ethyl ether (DMEE) with propylene oxide. Reaction of an olefin oxide such as propylene oxide with a hydroxy-containing or amine-containing reactant as required for producing the above catalysts, are well known to those skilled in the art. Such reactions often are carried out under basic conditions using alkali metal hydroxides, oxides and hydrides and in some cases basic amines. Because one of the reactants is an amine, there may be no need to add additional alkali. The molar amounts of ethylene oxide and/or propylene oxide relative to the amine starting material, e.g., DMEA, are selected to provide the desired level of ethyleneoxy units and propyleneoxy units in the catalyst compound.
In order to facilitate recovery and purification of the catalytic compound, e.g. by distillation, it is helpful to limit the length of the alkyleneoxy sub-units. Thus, it is preferred that the catalyst have no more than about five mols of ethyleneoxy or propyleneoxy per mol of amine. Most preferably, the catalyst has one or two ethyleneoxy units and one propyleneoxy unit.
Two characteristic features of the catalysts of this invention are the presence of a terminal secondary hydroxyl group together with a dimethylamino-ethyleneoxy molecular sequence. It is this combination of structures which is believed to provide the catalysts of this invention with their unique combination of good catalytic activity with a suitably low level of reactivity.
Although not wishing to be bound to any particular theory, it is believed that aminoalcohols having primary hydroxyl groups are less effective as catalysts than the compounds of the present invention due to their higher level of reactivity with the isocyanates; while other aminoalcohols than those specifically disclosed herein but also having secondary alcohols are believed to be less effective as catalysts because they lack the dimethylamino-ethyleneoxy molecular sequence of the compounds of the present invention.
Because of their reduced reactivity, the catalysts of the present invention also can be expected to contribute to small improvements in foam properties. The low reactivity prevents these catalysts from interfering, to any significant extent, with the desired isocyanate-polyol chain extending reactions and the cross-linking reactions. Thus, these catalysts do not disturb the desired sequence of polymer growth by undesired competition reactions.
To prepare polyurethanes using the catalysts of the present invention, any polyisocyanate, generally an aromatic polyisocyanate, can be used. Suitable aromatic polyisocyanates include: m-phenylene diisocyanate, p-phenylene diisocyanate, polymethylene polyphenylisocyanate, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, dianisidine diisocyanate, bitolylene diisocyanate, naphthalene-1,4-diisocyanate, diphenylene-4,4'-diisocyanate, aliphatic-aromatic diisocyanates, such as xylylene-1,4-diisocyanate, xylylene-1,3-diisocyanate, bis(4-isocyanatophenyl) methane, bis(3-methyl-4-isocyanatophenyl) methane, and 4,4'-diphenylpropane diisocyanate.
Most preferred aromatic polyisocyanates are 2,4 and 2,6 tolylene diisocyanates and their mixtures and methylene-bridged polyphenyl polyisocyanate mixtures which have a functionality of from about 2 to about 4. Known processes for preparing such methylene-bridged polyphenyl polyisocyanates are described, for example, in U.S. Pat. Nos. 2,683,730; 2,950,263; 3,012,008; 3,344,162 and 3,362,979.
The hydroxyl-containing polyol component, i.e. the active hydrogen-containing compound, which reacts with the isocyanate may suitably be a polyester polyol or a polyether polyol having a functionality of at least about 2 and a hydroxyl number ranging from about 700 or higher to about 25, or lower. When it is desired to provide a flexible foam, the hydroxyl number is preferably in the range of from about 25 to 100. For rigid foams, the hydroxyl number is preferably in the range of from about 350 to 700. Semi-rigid foams of a desired flexibility are provided when the hydroxyl number is intermediate to the ranges just given. The catalysts of the present invention have particular utility for preparing flexible urethane foams from polyols containing predominantly, and preferably only, primary hydroxyls.
Hydroxyl number is defined as the number of milligrams of potassium hydroxide required for the complete hydrolysis of the fully acetylated derivative prepared from one gram of polyol. The hydroxyl number also is defined by the equation; ##EQU1## where OH equals the hydroxy number of the polyol; f equals the functionality of the polyol (i.e., the average number of hydroxyl groups per molecule of polyol); and M.W. equals the molecular weight (e.g. number average) of the polyol.
When the polyol is a polyester, it is preferred to use, a polyester resin having a relatively high hydroxyl value and a relatively low acid value made from the reaction of a polycarboxylic acid with a polyhydric alcohol. When a flexible urethane foam is desired, the polyester polyol should generally have an average functionality (i.e., the number of active hydrogens per molecule) of from about 2 to about 4 and a molecular weight of from about 2,000 to about 4,000. For rigid foams, the functionality of the polyester polyol component is normally from about 4 to about 7.
When the hydroxyl-containing component is a polyether polyol for use in flexible polyurethane foam, the polyol may be an alkylene oxide adduct of a polyhydric alcohol with a functionality of from about 2 to about 4. The polyester polyol will suitably have a molecular weight within the range of from about 2000 to about 7000. For flexible polyether polyurethane foams, the alkylene oxide is preferably propylene oxide or a mixture of propylene oxide and ethylene oxide.
For rigid polyether polyurethane foams, the polyol should typically have a functionality of from about 4 to about 7 and a molecular weight of from about 300 to about 1200. Polyols for rigid polyether polyurethane foams may be made in various ways including the addition of an alkylene oxide, as above, to a polyhydric alcohol with a functionality of from 4 to 7.
Also suitable as the active hydrogen-containing component are the so-called "polymer/polyols or graft polyols, such as those obtained by polymerizing ethyleneically unsaturated monomers in a suitable liquid polyol in the presence of a free radical catalyst. Reactants, reaction conditions and proportions for preparing such polymer/polyols are well-known to those skilled in the art. Suitable monomers for producing these polymer/polyols include for example, acrylonitrile, vinyl chloride, styrene, butadiene, vinylidine chloride and the like. Copolymers of acrylonitrile and styrene are particularly preferred.
Polyols suitable for producing the polymer/polymers include polyhydroxyalkanes; the polyoxyalkylene polyols and the like. As above, polyols employed for making polymer/polyols useful in the present invention may have a wide range of hydroxyl numbers. Generally, the hydroxyl numbers of the polyols used to prepare the polymer/polyols range from about 20 and lower to about 200 and higher, and preferably range from about 25 to about 150.
A more comprehensive discussion of polymer/polyols can be found inter alia in the Stanberger patents, U.S. Pat. Nos. 3,304,273; 3,383,351; and Reissue No. 28,715 (reissue of U.S. Pat. No. 3,383,351); the Stanberger British Patent No. 1,022,434; U.S. Pat. Nos. 3,652,639 and 3,823,201; U.S. Pat. No. 3,953,393; U.S. Pat. Nos. 4,119,586 and 4,148,840; and U.S. Pat. No. 4,282,331.
The amount of hydroxyl-containing polyol, i.e., active hydrogen compound, to be used relative to the isocyanate compound in both polyester-based and polyether-based polyurethane foams normally should be an amount such that the isocyanate groups are present in at least a molar equivalent amount, and preferably, in slight excess, compared with the free hydroxyl groups of the polyol. Preferably, the ingredients will be proportioned so as to provide from about 1.05 to about 1.5 mol equivalents of isocyanate groups per mol equivalent of hydroxyl groups. Normally, an amount of isocyanate is used to provide an isocyanate index in the range of above about 95 to 135, more usually about 100 to 120, wherein the isocyanate index is the percentage of the calculated stoichiometric amount of polyisocyanate needed to react with all of the active hydrogen-containing components in the formulation. For example, an isocyanate index of 110 indicates that 110% of the stoichiometric amount of the polyisocyanate needed to react with all active hydrogens in the formulation is used.
Water generally is used in an amount, based on the molar amount of the hydroxyl groups of the polyol compounds, within the range of from about 0.02 mol to below about 5.0 mols per mol equivalent of hydroxyl. Preferably between about 0.2 to 3.3 mols of water per mol of hydroxyl is used. Stated alternatively, between about 0.3 and 6.0 parts of water per hundred parts of the polyol normally are used when preparing flexible foam.
It also is within the scope of the present invention to utilize an extraneously added inert blowing agent such as a gas or gas-producing material. For example, halogenated low-boiling hydrocarbons, such as trichloromonofluoromethane and methylene chloride, carbon dioxide, nitrogen, etc., may be used. The inert blowing agent reduces the amount of excess isocyanate and water that is required in preparing flexible urethane foam. Selection of a proper blowing agent is well within the knowledge of those skilled in the art.
The catalysts of the present invention are useful in the preparation of rigid, semi-rigid or flexible polyester or polyether polyurethane foams. The catalysts have particular suitability for preparing flexible foams, especially using the one-shot technique well-known to those skilled in the art. Based on the combined weight of the hydroxyl-containing compound and the polyisocyanate, these catalysts are employed in an amount of from about 0.01 to about 10.0 weight percent. More generally, the amount of catalyst used is about 0.05 to 5.0 weight percent of the combined polyurethane reactants, and usually between about 0.1 to 1.0 weight percent.
The catalysts of this invention may be used either alone or in mixture with one or more other catalysts such as organic tin compounds or other polyurethane catalysts, such as other amine catalysts. The organic tin compounds particularly useful in making flexible foams from polyether feedstocks include stannous or stannic compounds, such as a stannous salt of a carboxylic acid, i.e., a stannous acylate; a trialkyltin oxide; a dialkyltin dihalide; a dialkyltin oxide, and the like, wherein the organic groups of the organic portion of the tin compound are hydrocarbon groups containing from 1 to 8 carbon atoms. For example, dibutyltin dilaurate, dibutyltin diacetate, diethyltin diacetate, dihexyltin diacetate, di-2-ethylhexyltin oxide, dioctyltin dioxide, stannous octoate, stannous oleate, etc., or a mixture thereof, may be used. Such co-catalysts are used in their conventional amounts.
Additional conventional polyurethane formulation ingredients also can be employed, such as, for example, foam stabilizers also known as silicone oils or emulsifiers. A wide variety of silicon-based surfactants are known in the art. For example, the foam stabilizer may be an organic silane or siloxane. See, for example, U.S. Pat. No. 3,194,773. Still other, additional ingredients that can be employed in the polyurethane formulation include dyes, pigments, fire retardants, anti-microbial agents and the like. Such ingredients are employed in preparing a polyurethane foam in their conventional minor amounts.
In preparing a flexible foam, the ingredients may be simultaneously, intimately mixed with each other by the so-called "one-shot" method to provide a foam by a one-step process. In the "one-shot" process, the polyol and polyisocyanate reactants, the catalysts, blowing agents, surfactants and other optional ingredients are mixed together in a conventional mixing head and the resulting mixture is dispensed into a mold. Usually, the foam is prepared as slab stock wherein the foaming mixture is discharged from the mixing head onto a continuously moving, generally open-topped and open-ended conveyor-type mold. As the conveyor advances, foam reactions cause the foam to expand upwardly. In this instance, water should comprise at least a part (e.g., 10 to 100%) of the blowing agent. The foregoing methods are well known to those skilled in the art.
When it is desired to prepare rigid foams, either the "one-shot" method or the so-called "quasi-prepolymer method" can be employed. In accordance with the "quasi-prepolymer method," a portion of the hydroxyl-containing component is reacted in the absence of a catalyst with the polyisocyanate component in proportions so as to provide from about 20 percent to about 40 percent of free isocyanate groups in the reaction product, based on the polyol. To prepare a foam, the remaining portion of the polyol is added and the two components are allowed to react in the presence of the catalytic system, such as those discussed above, and other appropriate additives.
The following examples are presented to illustrate and not limit the invention. Unless otherwise indicated, all parts and percentages are on a weight basis, and all temperatures are on the Centigrade scale.
EXAMPLE 1
This example illustrates a method for preparing catalysts of the present invention. To a 4-neck flask equipped with a stirrer, a condenser, a metering funnel, and an inlet for nitrogen, about 100 milliliters of either DMEA or DMEE are added. The reaction flask is purged and blanketed with nitrogen. Thereafter, about 20 mol percent of the stoichiometrically required amount of propylene oxide to yield one mole of propylene oxide per mole of dimethylamino reactant is added to the reaction flask through the metering funnel. The reaction mixture is heated to about 90° C. with stirring under the nitrogen atmosphere.
The heating bath then is removed and the remaining stoichiometric requirement of propylene oxide is slowly added at a rate to maintain a constant temperature. Once all of the propylene oxide is added to the reaction flask, any residual propylene oxide is consumed by increasing the temperature to about 125° C. for about 15 minutes. The reaction mixture then is fractionated by distillation under a vacuum and several distillate fractions are recovered. Each of the distillates is analyzed using gas chromatography for purity. Fractions. containing more than about 98% of the desired catalyst (i.e., the catalysts of formula (I) wherein X is 1 or 2 and Y is 1) are retained for polyurethane synthesis. The catalysts can be used for making polyurethane foam from either ether polyol or ester polyol reactants.
EXAMPLE 2
A series of polyurethanes were prepared from an ether polyol (Polyurax 10.01 available from BP Chemicals) and TDI 80 (tolylene diisocyanate available from Bayer, A. G.) and water. Based on 100 parts by weight of the ether, 107 (index) isocyanate, 4.5 parts water and 1.4 parts of a siloxane surfactant (SC-162 available from BP Chemicals) were used. A catalyst system comprising a combination of stannous octoate and an amine was used. Polyurethane foam was prepared using each amine at three different levels of addition; and at each amine level three different stannous octoate levels of addition were used. Thus, for each catalyst pair nine different catalyst concentrations were examined.
The cream time and rise time of the various formulations were measured and the density, air flow (porosity) and hardness at 40% compression were measured for each of the resulting foams. The results are presented in the Table below. As used herein, cream time is the elapsed time from the mixing of the polyisocyanate (TDI) with the other ingredients until a noticeable expansion of the foam mixture occurs. Rise time is the elapsed time from the mixing of the polyisocyanate (TDI) with the other ingredients until a visible blow-off of gas occurs at near full rise of the foam.
The DMEA-propylene oxide adduct (using equal molar amounts of the reactants) made in accordance with Example 1 is designated DMEA-PO; while the DMEE-propylene oxide adduct (using equal molar amounts of the reactants) made in accordance with Example 1 is designated DMEE-PO.
TABLE 1__________________________________________________________________________ ATMOS- HARDNESS AMINE STANNOUS PREMIX PHERIC ABS. CREAM RISE FOAM Air- 40% COM-AMINE AMOUNT OCTOATE TEMP. PRESSURE HUM. TIME TIME DENSITY flow PRESSIONTYPE (pbw) (pbw) (°C.) (mbar) (mmHg) (SEC) (SEC) (kg/m.sup.3) (scFm) (k__________________________________________________________________________ Pa)DMEA-PO 0.192 0.160 22.8 1026 6.7 14.0 96 22.6 7.6 3.60DMEA-PO 0.192 0.175 23.1 1026 6.7 12.5 90 22.4 7.1 3.50DMEA-PO 0.192 0.190 22.7 1026 6.7 12.5 90 22.2 7.0 3.50DMEA-PO 0.240 0.190 22.6 1022 7.1 12.0 87 22.0 7.3 3.30DMEA-PO 0.240 0.210 22.5 1022 7.1 12.0 83 21.7 5.9 3.40DMEA-PO 0.240 0.230 22.3 1022 7.1 12.0 81 21.3 4.3 3.60DMEA-PO 0.300 0.220 22.7 1020 6.9 11.5 77 21.4 4.8 3.60DMEA-PO 0.300 0.250 22.6 1020 6.9 11.0 75 21.2 3.2 3.60DMEA-PO 0.300 0.280 23.1 1020 6.9 11.0 72 20.8 1.6 3.70DMEE-PO 0.192 0.160 22.7 1026 6.7 14.0 99 22.5 7.7 3.50DMEE-PO 0.192 0.175 22.9 1026 6.7 13.0 95 22.5 7.3 3.60DMEE-PO 0.192 0.190 22.7 1026 6.7 13.0 93 22.4 6.7 3.70DMEE-PO 0.240 0.190 22.5 1023 6.9 12.5 89 21.8 6.0 3.40DMEE-PO 0.240 0.210 22.5 1023 6.9 12.5 85 21.4 5.3 3.60DMEE-PO 0.240 0.230 22.4 1023 6.9 12.0 83 21.4 4.2 3.60DMEE-PO 0.300 0.220 22.7 1020 6.9 11.5 82 21.8 5.8 3.40DMEE-PO 0.300 0.250 22.8 1020 6.9 11.0 76 21.2 3.0 3.70DMEE-PO 0.300 0.280 22.7 1020 6.9 11.5 74 21.1 2.2 3.60__________________________________________________________________________
EXAMPLE 3
Using the polyurethane formulation of Example 2, the catalyst system DMEA/Stannous Octoate and DMEA-PO/Stannous Octoate were compared. The foams were prepared under the same conditions of premix temperature (23.2° C.±0.3); barometric pressure (1026 mba) and absolute humidity (6.3 mm Hg). Preparation of DMEA-PO was in accordance with Example 1. The results are presented below in Table 2.
TABLE 2__________________________________________________________________________ AMINE STANNOUS CREAM RISE FOAM HARDNESSAMINE AMOUNT OCTOATE TIME TIME DENSITY Airflow 40% COMPRESSIONTYPE (pbw) (pbw) (SEC) (SEC) (kg/m.sup.3) (scfm) (k Pa)__________________________________________________________________________DMEA 0.320 0.160 10.0 95 22.4 7.5 3.60DMEA 0.320 0.175 11.0 90 22.0 7.0 3.60DMEA 0.320 0.190 11.5 87 22.0 6.8 3.60DMEA 0.400 0.190 11.5 84 22.0 7.0 3.50DMEA 0.400 0.210 11.5 80 21.9 6.3 3.40DMEA 0.400 0.230 11.0 77 21.6 4.8 3.80DMEA 0.500 0.220 10.5 73 21.9 5.8 3.60DMEA 0.500 0.250 10.5 70 21.3 4.2 3.60DMEA 0.500 0.280 10.0 67 21.2 2.1 3.90DMEA-PO 0.192 0.160 13.5 97 22.1 7.8 3.50DMEA-PO 0.192 0.175 13.5 94 21.7 7.6 3.40DMEA-PO 0.192 0.190 13.0 91 21.9 6.8 3.60DMEA-PO 0.240 0.190 12.5 88 21.6 7.5 3.40DMEA-PO 0.240 0.210 12.0 84 21.6 6.5 3.50DMEA-PO 0.240 0.230 12.0 81 21.3 4.5 3.70DMEA-PO 0.300 0.220 11.5 78 21.4 6.0 3.40DMEA-PO 0.300 0.250 11.5 75 21.2 4.1 3.60DMEA-PO 0.300 0.280 10.5 72 20.6 1.6 3.80__________________________________________________________________________
As the polyurethane catalyst, the propylene oxide adduct of DMEA tended to yield a foam having a slightly lower density (about 1% to 3% lower) than foams prepared using DMEA, when compared at the same level of stannous octoate and rise time. Furthermore, it appears that the cream times of the catalysts of the invention are longer than encountered using DMEA.
EXAMPLE 4
A series of polyurethanes were prepared from an ester polyol (Desmophen 2381M available from Bayer, A. G.) and TDI 80 (tolylene diisocyanate available from Bayer, A. G.) and water. Based on 100 parts by weight of the ester, 95 (index) isocyanate, 3.5 parts water and 1.0 parts of a siloxane surfactant (SE-232 available from BP Chemicals) were used. The cream time and rise time of the formulations were measured and the results are presented below in Table 3.
TABLE 3__________________________________________________________________________ AMINE STANNOUS CREAM RISEAMINE AMOUNT OCTOATE TIME TIMETYPE (pbw) (pbw) (SEC) (SEC)__________________________________________________________________________DMEA-PO 1.0 -- 12 68DMEA-PO 0.8 -- 15 76 DMEA-PO/DM-16D* 0.53/0.1 0.02 17.5 86DMEE-PO/DM-16D 0.61/0.1 0.02 16.0 90__________________________________________________________________________ *ARMEEN DM16D (Dimethylhexadecylamine) available from Akzo Chemicals.
While certain specific embodiments of the invention have been described with particularity herein, it will be recognized that various modifications thereof will occur to those skilled in the art, and it is to be understood that such modifications and variations are to be included within the purview of this application and the spirit and scope of the appended claims.
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Certain dimethylamino alkyleneoxy isopropanols obtained by propoxylation of dimethylamino alkanols and ethers is used as a catalyst for preparing polyurethane foam.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefits of U.S. provisional patent application Ser. No. 61/129,844 filed Jul. 23, 2008; which is hereby incorporated by reference.
TECHNICAL FIELD
[0002] The present invention relates to a portable plasma based diagnostic apparatus and diagnostic method. The present invention further relates to a portable plasma, atomic, ionic and photonic based diagnostic apparatus and diagnostic method.
BACKGROUND
[0003] The quality of health care is founded on complete and accurate information about the patient.
[0004] Presently, four main diagnostic modalities are used in hospitals: X-ray, including computed tomography, magnetic resonance imaging, radiopharmaceutical imaging and ultrasound.
[0005] Computed tomography (CT) is a medical imaging method employing tomography. Digital geometry processing is used to generate a three-dimensional image of the inside of an object from a large series of two-dimensional X-ray images taken around a single axis of rotation. CT produces a volume of data which can be manipulated, through a process known as windowing, in order to demonstrate various structures based on their ability to block the X-ray beam.
[0006] Magnetic resonance imaging (MRI) is a medical imaging technique primarily used in Radiology to visualize the structure and function of the body. It provides detailed images of the body in any plane. MRI provides much greater contrast between the different soft tissues of the body than does computed tomography (CT), making it especially useful in neurological, musculoskeletal, cardiovascular, and oncological imaging. Unlike CT it uses no ionizing radiation, but uses a (powerful) magnetic field to align the nuclear magnetization of (usually) hydrogen atoms in water in the body.
[0007] Radiopharmacology is the study and preparation of radiopharmaceuticals, which are radioactive pharmaceuticals. Radiopharmaceuticals are used in the field of nuclear medicine as tracers in the diagnosis and treatment.
[0008] Medical sonography (ultrasonography) is an ultrasound-based diagnostic medical imaging technique used to visualize muscles, tendons, and many internal organs, their size, structure and any pathological lesions with real time tomographic images. It is also used to visualize a fetus during routine and emergency prenatal care. Ultrasound is one of the most widely used diagnostic tools in modern medicine.
[0009] Increasing demand for medical diagnostics is being driven by the aging population and the rise in prevalence of age-related diseases such as cancer, Alzheimer's disease, stroke, heart failure, etc. These diseases represent the highest cost burden to healthcare systems in industrialized nations, and there is tremendous pressure to develop tests that can assist in earlier diagnosis and aid selection of the most appropriate treatments in order to reduce costs. Hospitals are looking to purchase cost-efficient and more specialized medical equipment that will require fewer medical staff and reduce patients' length of hospital stay.
[0010] Despite recent spectacular advances in medicine, mortality rates for the most prevalent cancers have not been significantly reduced. In terms of primary prevention, we do not as yet have at hand robust strategies for these metabolic disorders or diseases.
[0011] Thus, there is a need for a simple, portable, noninvasive, rapid, accurate, easy to use, inexpensive and safe diagnostic apparatus to help health care providers to diagnose automatically and in real-time risk or presence of health issues such as, for example, infection, cancer, malignancy diseases or metabolic disorder in order to allow health care providers to take decisions at faster rate and react quickly and appropriately to prognosis or disease risk.
SUMMARY
[0012] The present invention relates to a spectrometry plasma, atomic, ionic and photonic-based apparatus that provides in real time and automatically clinicians and healthcare providers with early patient diagnostic of infection, presence of cancer or malignancy diseases by recording the signature of his or her biological tissue (skin), saliva, blood or urine. It enables earlier diagnosis, infection, pre-symptomatic disease detection and disease prevention. It improves operational capabilities for prevention and helps health care providers to take decisions at faster rate and to react quickly and appropriately to symptomatic, pre-symptomatic malignancy diseases, infection or metabolic disorder.
[0013] The apparatus is based on a miniaturized atmospheric soft ionization source coupled to miniaturized mass spectrometer. The quantum transfer energy source is coupled to a fast mass spectrometer, for example time of flight, quadrupole or ion-trap, to produce fingerprinting and quantitative measurements of the patient's chemical and biological compounds. The apparatus provides both a quantitative and a qualitative analysis, generating identification of the substances of interest and diagnostic information regarding metabolic disorder, cancer or infectious (malignancy) disease risk possibilities.
[0014] The ion source combines selective ionization with selective fragmentation, which provides exceptional detection limits. Increased sensitivity and decreased background allow for low detection limits and false positives diminution. Using different quantum energy beam (plasma, atoms, photons, electrons or ions) as well as direct introduction of divers patient specimens (skin, blood, urine or saliva) strongly enhance structural elucidation, mass spectral chemical and biological information, and specificity. Spectra are highly reproducible and do not require sample pre-treatment, leading to speed of analysis. There is no matrix to complicate matters. Thus eliminating potential losses and excessive handling, which also limits contaminations that can invalidate results. Contaminations are also minimized by direct sample introduction. Eliminating sample preparation gives an added advantage, especially to medical healthcare providers. It also offers for simplicity, along with limited exposure.
[0015] An operating process provides secure control of the overall apparatus and simplifies its use by non expert personnel. Reference libraries and automated interpretation of the raw data provide quantification and identification of the chemical and biological compounds as well as diagnostic information regarding malignancy diseases or risk thereof from the patient's sample(s).
[0016] More specifically, in accordance with the present invention, there is provided a portable plasma based diagnostic apparatus, comprising:
a miniature atmospheric plasma source for producing energetic projectiles; a miniature high pressure environment mass analyzer; an atmospheric direct sample introduction interface for receiving a sample to be analyzed, the atmospheric direct sample introduction interface being positioned between the plasma source and the mass analyzer; a database containing a reference library of indicators with their associated mass spectra; a processor operatively connected to the plasma source, the mass analyzer and the database, the processor being so configured so as to:
obtain from the mass analyzer a sample mass spectrum of parent and fragment ions resulting form the collision between the energetic projectiles and the sample; compare the sample mass spectrum with mass spectra in the reference library in order to identify at least one indicator; and provide a report based on the at least one identified indicator.
[0025] In accordance with the present invention, there is also provided a plasma based diagnostic method, comprising:
projecting a beam of energetic projectiles at a sample to be analyzed; recording a sample mass spectrum of parent and fragment ions resulting form the collision between the energetic projectiles and the sample; comparing the sample mass spectrum with mass spectra of a reference library in order to identify at least one indicator; and providing a report based on the at least one identified indicator.
BRIEF DESCRIPTION OF THE FIGURES
[0030] Embodiments of the invention will be described by way of example only with reference to the accompanying drawings, in which:
[0031] FIG. 1 is a block diagram of a portable ion based diagnostic apparatus according to an illustrative embodiment of the present invention;
[0032] FIGS. 2A and 2B is a flow diagram of an example of an operating process that can be used by the apparatus of FIG. 1 ;
[0033] FIG. 3 is a flow diagram of an example of a background and surrounding environment analysis sub-process that may be used with the operating process of FIGS. 2A and 2B ; and
[0034] FIG. 4 , is a graph of an example of an analyte profile of a patient using high energy projectiles such as energetic helium atoms (˜20 eV), the analyte profile of the same patient using low energy projectiles such as energetic nitrogen atoms (˜8 eV) and a reference analyte profile of a healthy individual using high energy projectiles such as energetic helium atoms (˜20 eV).
DEFINITIONS
[0035] The detailed description and figures refer to the following terms which are herein defined:
Analyte: A sample being analyzed, the sample being solid, liquid or gaseous. Examples of analytes include biological tissue (skin), saliva, blood or urine. Other examples may include air or soil samples, etc. Analyte ion: Ions resulting from the collision between an energetic projectile and an analyte. These ions may be parent ion or various ions resulting from fragmentation. Analyte profile: The mass spectrum resulting from the collision between an energetic projectile and an analyte. Sample spectrum: The mass spectrum resulting from the collision between an energetic projectile and an analyte including the background spectrum. Parent ion pattern: The mass spectrum resulting from the collision between low energy projectiles and an analyte. This spectrum results from the loss of an electron in the analyte molecule. Fragmentation ion pattern: The mass spectrum resulting from the collision between high energy projectiles and an analyte. This spectrum results from the decomposition of the parent ion or its instability. Biomarkers: Specific molecules observed in infectious or carcinogenic diseases.
DETAILED DESCRIPTION
[0043] Generally stated, the non-limitative illustrative embodiment of the present invention provides a portable plasma, atomic, ionic, electronic and photonic based diagnostic apparatus that provides to clinicians and healthcare providers, in real time and automatically, early patient diagnostic of infection, metabolic disorder, presence of cancer or malignancy diseases by scanning, recording the chemical and/or biological signature(s) of his or her biological tissue (skin), saliva, blood or urine and automatically analyzing obtained spectra for various medical conditions.
[0044] Referring to FIG. 1 , there is shown a portable plasma, atomic, ionic, electronic and photonic based diagnostic apparatus 100 according to an illustrative example of the present invention. The diagnostic apparatus 100 generally comprises a continued or pulsed miniature atmospheric plasma source 102 , a direct sample introduction interface 104 , an analyzer chamber 106 , a processor 116 with an associated memory 118 , a database 120 , logs 122 , a user interface 124 , an input/output interface 126 and a power supply 128 . The analyzer chamber 106 includes a miniature vacuum pump 108 , a pressure gauge 109 , a high pressure ions detector 110 , ion extraction and transport lenses 112 , and a miniature high pressure environment mass analyzer 114
[0045] The plasma source 102 can have, for example, ca. 0.175 cm 3 as volume or less, with gas density of ca. 10 13 -10 15 particles/mm 3 and a downstream flow of ca. 10 16 -10 19 particles/sec. Depending on the selected application, the processor 116 adjusts the settings of the plasma source 102 , which produces the energetic projectile beam that transfers quantum energy to the analyte to form the free (radical) ions. The plasma source 102 may be based on technologies such as, for example, arc-discharge, chemical, Penning or Niers-Bernas ionization processes. As well, fast atom bombardment, lasers and ultraviolet lamps may also be used.
[0046] The direct sample introduction interface 104 consists in a free atmospheric interface between the plasma source 102 and the analyzer chamber 106 . The patient specimens, i.e. biological tissue (skin), blood drop, saliva or urine (wet cotton), which do not require pre-treatment, are directly introduced into the direct sample introduction interface 104 , perpendicularly to the energetic beam emitted by the plasma source 102 . The absence of pre-treatment has the benefit of minimizing sample waste and excessive handling, which causes losses. It also limits the risk of contamination that can invalidate results. In an alternative embodiment, the direct sample introduction interface 104 may be provided with a needle mechanism in order to automatically take a blood sample. It may be also provided with water or alcohol beams and a heat interface for contamination cleaning and sterilization.
[0047] Ions formed from the collisions of the energetic beam with the analyte directly introduced into the direct sample introduction interface 104 generate fingerprinting of the complex chemical and biological system of the patient, and are extracted and transferred through the ion extraction and transport lenses 112 to the mass analyzer 114 with associated high pressure ions detector 110 using a high differential electric field. The mass analyzer 114 , which is located within the analyzer chamber 106 , analyzes and records the parent and/or fragmentation ion patterns, which are reproducible for a given energy level and a given sample. The mass analyzer 114 may be based on technologies such as, for example, miniature high performance ion-traps, quadrupoles or time-of-flight (TOF), which may be operated in a high pressure environment, for example 10 −4 to 10 −1 mbar.
[0048] During a collision, an electron is ejected into continuum leading to ionization. The ejected electron can take a range of kinetic energies that is defined by the species, i.e. the nature of the analyte and the quantum transfer energy beam involved in the collision. The presence of fragment ions is governed by the excitation energy and the nature of the sample (i.e. analyte or patient specimens). The plasma source 102 allows precise control over fragmentation and yields very reproducible mass spectra. Parent and fragment ions are used for the identification of constituents in complex mixtures.
[0049] The analyzer chamber 106 consists in a small differential pumping chamber, for example ca. 1.6 I, which keeps the mass analyzer 114 at pressures of, for example 10 −4 to 10 −1 mbar, using the miniature vacuum pump 108 . The analyzer chamber 106 also includes the high pressure ions detector 110 and the ions extraction and transport lenses 112 , which are electrostatic lenses. The ion extraction and transport lenses 112 consist in two plate electrodes biased at high differential voltage used downstream of the direct sample introduction interface 104 to extract the analyte ions. Thin coaxial cylinders, on axis, downstream of the extraction electrodes are used to transport and focus the extracted analyte ions at the entrance of the mass analyzer 114 in order to determine the composition of the ion beam.
[0050] The peaks in the spectra recorded by the mass analyzer 114 correspond to different mass-dependent velocities (i.e. different mass-to-charge ratios (m/z)) of the ionized sample and are analyzed using a diagnostic process which will be further detailed below. The diagnostic process uses the mass spectrum of the parent and fragment ions, and their relative abundances, provided by the mass analyzer 114 for both the quantization and identification of the analyte composition of the sample in order to establish the patient's analyte profile.
[0051] To provide a diagnosis, the established analyte profile of the patient is compared to those of healthy people of the reference library, which is stored in the database 120 , in order to identify abnormal peaks. The peaks may be identified by first calculating the mass-to-charge ratios (m/z) and normalizing the spectrum with regard to the total ion currents. The background is then filtered out from the spectrum and peaks detected with an automatic peak detection process. The peak detection process allows for the evaluation of each peak for its contribution into the spectrum, i.e. the relative abundance of each peak in the spectrum. This process may also incorporates a spectral de-convolution sub-process which takes into account discrimination or interference between elements and isotope ratios.
[0052] The identified peaks are then used to search the reference library in order to determine a related biomarker. The reference library contains chemical and biological reference materials over a variety of concentrations, well below the limits of detection required. It also contains a chemical and biological database of diseases, along with an ability to create novel chemical and biological sub-libraries. The reference materials may be provided, for example, by federal, provincial and healthcare provider partners.
[0053] Optionally, the various test results, error conditions, alarm conditions, etc., may be recorded in logs 122 .
[0054] The user interface 124 may be used to automatically operate the diagnostic apparatus 100 , provide instructions to the user as to how to operate the diagnostic apparatus 100 and display various information such as, for example, user menus, alarms and diagnostic results.
[0055] The input/output interface 126 may be used to, for example, update the library, export logs or provide diagnostic results to a further system or storage medium.
[0056] The power supply 128 may be, for example, a battery (such as a 9, 12 or 24 Volts battery) to allow the diagnostic apparatus 100 to be portable. The power supply 128 may also be provided with the capability to be directly powered by a 110 or 220 Volts AC power source.
[0057] Referring now to FIGS. 2A and 2B , there is shown a flow diagram of an example of an operating process 200 that may be executed by the processor 116 of the diagnostic apparatus 100 of FIG. 1 . The steps of the process 200 are indicated by blocks 202 to 240 .
[0058] The process 200 starts at block 202 where the start-up sequence is initiated, namely the plasma source 102 is powered up and stabilized, the vacuum pump is activated 108 and once the pressure gauge 130 reads a pressure around 10 −2 mbar within the analyzer chamber 106 , the ions extraction and transport lenses 112 and mass analyzer 114 are powered up. It is to be understood that complimentary sub-processes may be executed at this point in order to verify the proper functioning of the various components of the diagnostic apparatus 100 .
[0059] At block 204 , the process 200 executes a background (i.e. the environment in which the diagnostic apparatus 100 is used) test in order to determine if there are any contaminants present. This allows the diagnostic apparatus 100 to be also used as an indoor air quality or environment monitor. The background test will be further detailed below.
[0060] Then, at block 206 , the process 200 verifies if the background test has passed. If it has failed, the diagnostic apparatus 100 analyses and identifies the chemical and biological contaminants of the environment and alerts the end users, then shutdowns at block 208 . If it has passed, the process proceeds to block 210 .
[0061] At block 210 , the masses of the various components present in the background are determined and, at block 212 , the process verifies if the peaks of the background spectrum are shifted in mass. If so, at block 214 , the shifts are computed and the mass analyzer 114 is calibrated, after which the process 200 returns to block 210 . If there is no shift in mass of the peaks, the process 200 proceeds to block 216
[0062] At block 216 , the user interface 124 indicates that the diagnostic apparatus 100 is ready.
[0063] Then, at block 218 , the process 200 asks for the patient's identification, either by reference to some identification number or by entering the patient's information using the user interface 124 . Once the patient has been identified, the process 200 then asks, at block 220 , for the type of analysis to be performed, i.e. skin, blood, urine or saliva.
[0064] At block 222 , the process 200 detects the presence of a sample in the direct sample introduction interface 104 and then starts to record the sample spectrum. Alternatively, the recording may be activated manually. The recorded spectrum may then be stored in the database 120 with the patient's identification and the logs 122 updated.
[0065] Then, at block 224 , the background spectrum recorded at start-up is subtracted from the recorded sample spectrum. The peaks of the resulting spectrum, the analyte profile, are analyzed and identified at block 226 . Following this, at block 228 , the identified peaks are compared to those of the analyte profiles of healthy patients stored in the database 120 in order to identify, at block 230 , abnormal peaks in the patient's biological and chemical fingerprint (i.e. analyte profile).
[0066] At block 232 , the process 200 searches through the reference library in order to identify one or more spectra for the given sample type, identified at block 220 , having similar peak and mass patterns, each pattern corresponding to a given condition. Each element of the peak and mass pattern, alone or in combination, corresponding to one or more biomarkers, which are associated with a probability of a condition being present.
[0067] At block 234 , the process 200 establishes a diagnostic using the one or more conditions identified at block 232 . This is accomplished taking into consideration each pattern's fit with the identified abnormal peaks as well as probabilities associated with each condition. Furthermore, if multiple types of samples have been analyzed, i.e. skin, blood, urine or saliva, then the results of each analysis can be combined to provide a more accurate diagnosis by enhancing structural elucidation, mass spectral or chemical information and increase sensitivity and specificity, and confirm or complete the pre-diagnosis. The diagnosis can take the form of, for example, a table with the detected masses or molecules, abnormal peaks, their abundance, their identified patterns with corresponding conditions and probabilities. The diagnosis may then be stored in the database 120 along with the patient's information and the logs 122 updated.
[0068] Basically, the mass spectrum for parent and fragment ions, and their relative abundance, is used for both the quantization and identification of the chemical and biological composition of a patient's sample. The obtained mass spectrum is first compared to those of healthy profiles in order to isolate abnormalities. The identified abnormalities are then compared to a library of known biomarkers. Each contribution into the spectrum is evaluated taking into account discrimination or interference between elements and isotope ratios. The abundance of resulting biomarkers then allows the generation of an appropriate diagnosis. The biomarkers may also be compared to those present in individuals having a similar profile.
[0069] The use of different beams (i.e. plasma, atoms, photons, electrons or ions), with different quantum energies, as well as different patient specimens (i.e. skin, blood, urine or saliva) strongly enhances structural elucidation, mass spectral, chemical or biological information, resulting in highly increased sensitivity, specificity and strongly confirms or completes a pre-diagnosis.
[0070] Referring to FIG. 4 , there is shown an example of a graph 400 of an analyte profile of a patient using high energy projectiles such as energetic helium atoms (˜20 eV) 403 , the analyte profile of the same patient using low energy projectiles such as energetic nitrogen atoms (˜8 eV) 402 and a reference analyte profile of a healthy individual using high energy projectiles such as energetic helium atoms (˜20 eV) 401 . It may be observed from the graph 400 that both the analyte profiles 402 and 403 of the patient show the presence of an abnormal peak 410 representing an unknown biomarker. The mass-to-charge ratio, intensity, and isotopic ratios of the peak 410 are then used to search in the reference library in order to identify the biomarker corresponding to the identified abnormal peak 410 , and to determine the contamination level or the disease stage.
[0071] Then, at block 236 , the process 200 asks if a new analysis is to be performed. If so, the process 200 proceeds to block 238 , if not, the process 200 ends.
[0072] At block 238 , the process 200 asks the user to clean the direct sample introduction interface 104 . In an alternative embodiment, the direct sample introduction interface 104 may be provided with a cleaning mechanism using, for example, alcohol, water or heat, which may be activated by the process 200 and automatically clean up any contamination due to the last analysis performed. The needle may also be changed automatically. The process 200 then proceeds to block 240 .
[0073] Finally, at block 240 , the process 200 asks if the new analysis is for the same patient. If so, the process 200 proceeds to block 220 where the sample type is selected, if not, it proceeds to block 218 where the information about the new patient is entered.
[0074] Referring now to FIG. 3 , there is shown a flow diagram of an example of a background analysis sub-process 300 that may be executed by process 200 at block 204 of FIG. 2A . The steps of the sub-process 300 are indicated by blocks 302 to 326 .
[0075] The sub-process 300 starts at block 302 where the background spectrum is recorded. Following which, at block 304 , the sub-process 300 verifies if the background is normal by comparing the recorded background spectrum with that of reference background spectra stored in the database 120 . If the background spectrum is normal, then the sub-process 300 proceeds to block 306 where the background test is set to “PASS”. The sub-process 300 then hands over control back to process 200 of FIG. 2A , which then proceeds to block 206 . If the background spectrum is not normal, then sub-process 300 proceeds to block 308 .
[0076] At block 308 , the sub-process 300 verifies if the background has been determined to be abnormal for the third time. If not, the sub-process 300 proceeds to block 310 where it pauses, for example by waiting for a few minutes (e.g. from 1 to 5 minutes) before proceeding back to block 302 for a new recording of the background spectrum. If the background has been determined to be abnormal for the third time, the sub-process 300 proceeds to block 312 where the presence of an irregular background is reported via the user interface 124 . A listing of the detected compounds and contaminants, as well as their proportions, may also be communicated. These may be identified by comparing the abnormal peaks found in the background spectrum with spectra stored in the reference database 120 .
[0077] At block 314 , the sub-process 300 asks the user to clean the direct sample introduction interface 104 . In an alternative embodiment, the direct sample introduction interface 104 may be provided with a cleaning mechanism using, for example, alcohol, water or heat, which may be activated by the sub-process 300 and automatically clean up any contamination due to the last analysis performed. The needle may also be changed automatically.
[0078] At block 316 , sub-process 300 pauses for a few minutes (e.g. 1 to 3 minutes) before proceeding to block 318 where the background spectrum is recorded.
[0079] Then, at block 320 , sub-process 300 verifies if the background spectrum is within an acceptable range of the reference background, for example 25%, and that no dangerous compounds or contaminants have been detected. If so, sub-process 300 proceeds to block 306 , if not, it proceeds to block 322 .
[0080] At block 322 , the sub-process 300 verifies if the background has been determined not to be within an acceptable range of the reference background for the third time. If not, the sub-process 300 proceeds to block 316 . If so, the sub-process 300 proceeds to block 324 where the presence of a contaminated environment is reported via the user interface 124 . A listing of the detected compounds and contaminants, as well as their proportions, may also be communicated. Furthermore, should the detected compounds and contaminants, or their proportions, are found to be dangerous, the sub-process 300 instructs the user to evacuate the contaminated zone and, in an alternative embodiment, may sound an alarm and/or communicate the danger to a further system using the input/output interface 126 . The sub-process 300 then proceeds to block 326 where the background analysis is set to “FAIL”. The sub-process 300 then hands over control back to process 200 of FIG. 2A , which then proceeds to block 206 .
[0081] It is to be understood that the number of repetitions of the background test at blocks 308 and 322 , as well as the waiting times at blocks 310 and 316 , as well as the range at block 320 may be adjusted.
[0082] It is also to be understood that the described diagnostic apparatus 100 can be used, provided that the appropriate spectra libraries are included in the database 120 , as a real-time analyzer of biological or chemical contaminated areas, for:
indoor air quality: detection of chemical and biological contaminants in hospitals, schools, private and public buildings, plants, malls, planes, trains, etc.; environmental assessments: soil, water or air contamination; mining industry: exploration and analysis of soil mineral content; food industry: analysis of the food composition and detection of contaminants in the production chain; homeland security: monitoring of restricted areas in airports, ports, etc.; and other fields such as forensics, pharmaceuticasl, cosmetics, etc.
[0089] It is to be understood that although reference has been made to the peak and mass patterns being used for the identification of biomarkers, they may also be used to identify an indicator which may be a biomarker, a chemical compound, a chemical element, a mineral, etc., depending on the application. Furthermore, depending on the application, the diagnosis may be a report listing contaminants, mineral composition, oil presence, etc.
[0090] Although the present invention has been described by way of a particular embodiment and examples thereof, it should be noted that it will be apparent to persons skilled in the art that modifications may be applied to the present particular embodiment without departing from the scope of the present invention.
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A portable plasma based diagnostic apparatus comprising a plasma source for producing energy projectiles atmospheric pressure, a mass analyzer, a sampling interface for receiving direct sample to be analyzed, the sampling interface being positioned between the plasma source and the mass analyzer, a database containing a library of biomarkers with their associated mass spectra, a processor operatively connected to the plasma source, the mass analyzer and the database. The processor is so configured so as to obtain from the mass analyzer a sample mass spectrum of parent and fragment ions resulting form the collision between the energetic projectiles and the sample, compare the sample mass spectrum with mass spectra in the reference library in order to identify at least one indicator and provide a report based on the at least one identified indicator.
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FIELD OF THE INVENTION
This invention relates to ergonomic knee braces.
BACKGROUND OF THE INVENTION
In the field of adjustable knee braces or supports, it is desirable that the brace include arrangements for limiting the movement of the lower leg relative to the upper leg both as to bending the knee or flexion, and as to extension of the lower leg relative to the upper leg. Various knee brace arrangements have been proposed, and these have included upper struts for extending along the thigh, and lower struts for extending along the lower leg or calf. These are normally provided both on the inside or medial side of the leg and also on the outer or lateral side of the leg; and the medial and lateral struts are normally padded, and provided with straps to hold them in place. Pivoting arrangements are provided for coupling the upper and lower struts, and stops are provided for limiting both extension and flexion of the knee.
The prior art patents in the field of knee braces include U.S. Pat. No. 5,672,152 granted Sep. 30, 1997; U.S. Pat. No. 5,921,946, granted Jul. 13, 1999; U.S. Pat. No. 4,817,588, granted Apr. 14, 1989, U.S. Pat. No. 4,953,543 granted Sep. 4, 1990, and U.S. Pat. No. 4,620,532 granted Nov. 4, 1986. Although many of the foregoing provided useful results, these prior art knee braces had shortcomings, in that they were unduly bulky, or were not simple to adjust, or did not have as many stop increments as would be desired, or were otherwise not ergonomically configured.
INVENTION SUMMARY
Accordingly, objects of the invention include providing a knee brace which is compact, easy to use, which has many points of adjustment and is otherwise ergonomically configured. Preferably the adjustments should be simple and natural so that there is no need to resort to collateral written instructions.
Initially, relative to an illustrative preferred embodiment of the present knee brace, the knee brace stop construction operates at the periphery of the pivot arrangements so that the number of stop increments is maximized for the size of the pivot discs. Secondly, the stops may be operated by simple inward pressure on a push button associated with the flexion stop or the extension stop, to release the stop, followed by rotation of the stop to virtually any desired angle, and then followed by release of the push button to permit locking of the stop in the new angular position. With this simplified ergonomic construction, the stop adjustments may be easily made while the brace is mounted on the leg; and the mode of accomplishing stop adjustments is substantially self evident, with the shifting of the stops resulting in the natural or expected angular change in flexion or extension stops.
In order to achieve the foregoing results in one illustrative embodiment, the pivoting assembly interconnecting the upper and lower struts includes, for both extension and flexion, at least one generally circular or arcuate catch plate with stop recesses facing or opening inward toward the center of the assembly, and a movable stop member pivoted at the center of the assembly and having an outwardly biased locking member for selectively engaging one of the stop recesses, and with the locking member attached to a release button which extends radially outward to the periphery of the pivot assembly.
Viewed from a different aspect, the pivoting assembly may include an outer cover or closure plate and an inner cover or closure plate; an arcuately configured array of locking steps; a movable stop member pivoted at the center of the assembly and having an outwardly biased locking member for selectively engaging at least one of the locking steps; and with the locking member attached to a release button which is located radially outward at the periphery of the pivot assembly.
Additional features may include the provision of angular indicia on the outer surface of the outer one of said cover or closure plates and the implementation of the movable stop assembly by an outer, radially extending flat support member adjacent the indicia, preferably with a window through which the angular indicia may be seen. Further, the movable stop assembly may extend over the edge of one of said plates into the space between the two cover plates to cooperate with the locking steps. This construction contributes to the relatively thin overall configuration of the pivoting assembly, which may be only about one-half inch or about 1.3 cm thick. Also, to provide adequate strength and compactness, the brace and it components are preferably made of high strength material such as steel, titanium, zinc alloys, or other high strength metals or high strength plastic.
It is further noted that, in the preferred design, two catch plates are provided, and each of the stop assemblies includes a pin which seats in corresponding recesses in each of the two catch plates, to provide a balanced locking configuration for resisting forces applied between the struts to limit flexion or extension. The inner and outer cover plates may also have complementary recesses to more positively secure the stops at the selected angular position.
Referring back to the overall construction as mentioned above, one strut extends from the knee pivot assembly up the upper leg or thigh, and the other strut extends from the pivot assembly down the lower leg. The pivot stop assembly is mounted on the end of a first one of these struts, and the second strut has stop surfaces on its end adjacent the stop assembly which engage the flexion and extension stops. Further, the catch plates as described above are mounted on opposite sides of this second strut, with the locking member of the movable stop assembly engaging locking steps on both of the two catch plates, so that a balanced positive stopping force is transmitted to the second strut when the stop surfaces on the end of the second strut engage the flexion stop or the extension stop.
Additional aspects of the knee brace may include the following:
(1) catch plates which have separate sets of notches for the flexion and extension stops, and a mechanical coupling between these two sets of notches;
(2) Color coded flexion and extension actuation buttons, with the degree indicia set forth in matching different colors;
(3) Apertures or holes in the actuation buttons to permit locking of the buttons against change.
Other objects, features and advantages of the invention will become apparent from a consideration of the drawings and from the detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a knee brace assembly illustrating the principles of the invention;
FIG. 2 is a plan view of one of the two knee braces included in the knee brace assembly of FIG. 1 ;
FIG. 3 is a side view of the knee brace of FIG. 2 ;
FIG. 4 is an enlarged plan view of a knee brace pivot and motion limiting assembly, illustrating the principles of the invention;
FIG. 5 is an enlarged perspective view of the pivot assembly;
FIG. 6 is an exploded view of the knee brace assembly illustrating the principles of the invention;
FIG. 7 is an enlarged view of the central pivot and stop assembly of the knee brace of FIGS. 1-6 , with the front cover removed;
FIG. 8 is an exploded view of the two movable stops and their associated adjustment buttons, and indication support members; and
FIG. 9 through 12 show various stop adjustment configurations for the knee brace.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
While the specification describes particular embodiments of the present invention, those of ordinary skill can devise variations of the present invention without departing from the inventive concept.
Referring more particularly to the drawings, FIG. 1 shows a leg brace 12 for the knee, including two struts extending up and down the leg from a central pivot assembly 14 . Extending along the upper leg is a strut 16 , and extending down the lower leg from the pivot assembly 14 is a lower strut 18 . These struts are sometimes referenced as femoral struts (as extending along the femur or upper leg bone) and tibial struts (extending along the tibia, or the principal lower leg bone). A pivot assembly on the other side of the knee is also provided with struts extending up and down the leg, but these are not visible in FIG. 1 .
To hold the struts in place on the leg are a series of straps 22 on the upper leg, and straps 24 on the lower leg. Suitable padding 26 is provided on the upper leg and the struts are normally secured to the padding 26 by appropriate Velcro® or hook and loop type material. Similar padding 28 underlies the strut 18 and straps 24 . The straps 22 extend through the loops 38 to hold the entire assembly together under active usage conditions.
The present invention is directed primarily to the pivot stop assemblies which interconnect the struts. For a post-operative patient, it is desirable to be able to limit the bending of the knee both in the extension direction when the patient is straightening his or her leg, and in the flexion direction where the patient is bending the leg at the knee as far as practical under the circumstances.
The showing of FIG. 1 is of the outside of the left leg. On the inside of the left leg is a similar assembly, to that shown in FIG. 1 , with two struts and a central pivot assembly. The two units are similar and both are held to the leg by the straps 22 and 24 . Most of the parts are common to the inner and outer assemblies, but with the struts and the cover plates being mirror images of one another.
To better understand the operation of the entire assembly, it is useful to refer briefly to the exploded view of FIG. 6 . In operation, the two struts 16 and 18 are pivoted relative to one another about center rivet 56 ; and strut 18 has two stop surfaces 32 and 34 . Adjustable stops are mounted to the hinge pivot assembly 14 on strut 16 and the adjustable stops engage stop surfaces 32 and 34 to limit pivoting of the knee in both the extension and the flexion directions.
FIG. 2 of the drawings shows the assembly 12 and the pivot assembly 14 with the straps 22 and 24 , and the padding 26 and 28 removed. Visible in FIG. 2 are the strap coupling members 36 which are secured to the struts, and the strap receiving openings 38 . FIG. 3 is a side view of the assembly of FIG. 2 . The central stop mechanism 14 will be described in greater detail hereinbelow.
Referring now to FIGS. 4 and 5 of the drawings, these are plan and perspective views, respectively of the central stop mechanism 14 which interconnects the struts 16 and 18 .
Now, considering FIG. 4 in detail, it includes the extension stop assembly 42 and the flexion stop assembly 44 . Visible on the cover plate 46 are degree indicia which may be read through the openings 48 and 50 on the stop assemblies 42 and 44 , respectively. To change the limits of motion, the push buttons 52 and 54 are depressed and the stop assemblies are rotated to the desired angular settings. Incidentally, the outermost surfaces of push buttons 52 and 54 are preferably knurled, ribbed or textured for non-slip engagement. Alternatively the stops may be coated with a frictional coating.
Concerning the angular settings, when the extension stop 42 is at zero degrees (0°), the patient is free to fully extend his lower leg. When the extension stop 42 is set to 90°, the lower leg is restrained from movement beyond 90° relative to the upper leg, so the lower leg cannot be straightened out.
Regarding the flexion stop 44 , when it is set to 120° the lower leg may be fully bent toward the upper leg. When the flexion stop is set to “lock”, then the lower leg is fully extended, and is blocked from any bending. If both stops 42 and 44 are set to 60° for example, the knee is held at 60° from fully open, and is restrained from movement in either direction.
Incidentally, the support members for the stops are both pivoted about the center 56 of the pivot assembly 14 , with the reference number 56 representing the head of a rivet extending through the assembly.
Consideration will now be given to the detailed construction of the pivotal stop mechanism, by reference to the exploded view of FIG. 6 . As mentioned above, one of the two struts 18 has the two stop surfaces 32 and 34 on its end, and is pivoted, with opening 62 receiving rivet 56 which extends through the entire assembly. The flat parts 64 and 66 are spacers and also serve the function of washers in facilitating rotation of the overlying parts. They may be formed of plastic such as nylon. The catch plates 68 and 70 have a series of inwardly opening recesses which receive outwardly biased locking pins as described below.
The inner cover plate 72 and the outer cover plate 74 may also be provided with inwardly directed recesses, matching those in the catch plates 68 and 70 . This provides supplemental restraint for the locking pins shown in detail in later figures of the drawings.
FIG. 7 is an enlarged view of the central mechanism with one of the cover plates removed. The stop assembly 44 has a locking pin 82 which moves inward with the push button 54 to change settings, but is spring biased outward to engage one of the recesses 84 . Similarly, the locking pin 86 associated with push button 52 , locks the stop 42 by engagement with a selected one of the catch plate recesses 84 .
FIG. 8 is an enlarged showing of the physical stop members 92 and 94 which engage the stop surfaces 32 and 34 as shown in FIG. 6 . Two small pairs of coil springs 96 and 98 serve to bias the push buttons 52 and 54 , and the associated locking pins 86 and 82 outward, into engagement with the catch plate 68 (see FIG. 7 ) and the other catch plate 70 (see FIG. 6 ).
Incidentally, the physical stops 92 and 94 may be formed of a high strength zinc alloy referenced as ZA-28, or other high strength material.
FIGS. 9 through 12 shows various adjustments of the stops, and the resultant permitted positions of the struts 16 and 18 . More specifically, FIG. 9 shows the extension stop 42 and the flexion stop 44 in their positions for full range of motion, with the extension stop 42 at 0° and the extension stop 44 at 120° (see FIG. 4 ). In FIG. 9 the struts (and the leg) are fully extended; while in FIG. 10 , the struts and the leg are bent to their extreme flexed position, with the two stops in the same positions for both FIG. 9 and FIG. 10 .
FIG. 11 is a similar pair of drawings with the extension stop at about 45° and the flexion stop at about 75° in both figures. In FIG. 11 the struts are extended as far as possible with this setting of stops 42 and 44 ; and in FIG. 12 the struts (and leg) are bent as far as permitted with this setting of the stops 42 and 44 .
An alternative embodiment of the stop mechanism may include a physical stop having a radially extending slot for receiving a locking pin associated with a push button; and a wire spring biasing the push button and locking pin radially outward relative to the stop support members.
Concerning another matter, with reference to FIG. 4 of the drawings, the push buttons 52 and their associated assemblies are preferably color coded to match colored angle indicia. Thus, push button 52 may be colored blue, with the associated degree indicia from “0” to “90” degrees being the same blue color; and push button 54 and associated indicia may be colored green.
It may be noted that the push buttons are provided with holes near the outer ends thereof. This permits the physician or technical assistant to thread wire or plastic ties through the openings to discourage re-setting or tampering with the angular settings, as shown at reference numerals 101 and 103 in FIGS. 11 and 12 of the drawings. Other elements for preventing or restricting actuation of the push buttons, including locking ties, may be employed; and these elements may be separate from or integral with and movable with respect to, the knee brace assembly.
It is to be understood that the foregoing detailed description discloses one preferred illustrative embodiment of the invention. Various changes and modifications may be made without departing from the spirit and scope of the invention. Thus, by way of example and not of limitation, instead of having catch plates with locking recesses, a series of outwardly extending rods or protrusions may be provided, with the stop buttons having an outwardly biased fork member for engaging the rods and thereby positioning the stop body or stop plate in the desired angular position. In addition, while the disclosed configuration of the stop supports 44 and 48 is preferred, the stop assemblies may be pivotally mounted within the cover plates as well as, or instead of, extending over the outer surface of the outer cover plate. With regard to another matter, the release push button may be integral with the physical stops. Also, the various parts may be replaced by their mechanical equivalents, such as rivets being replaced by threaded fasteners, or the like. Accordingly, the present invention is not limited to the precise embodiments described in detail hereinabove, and shown in the accompanied drawings.
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A knee brace is provided with push button actuatable stops, wherein the stops are biased outward into angular locking positions and inwardly directed pressure on the push buttons releases the stops and permits angular adjustment of the stops. A pair of catch plates with locking recesses facing inward, are provided, and outwardly biased locking pins engage the recesses in both catch plates. Each of the stop assemblies has an outwardly directed plate extending over the outer cover plate, and this plate is coupled to the physical stop member around the outer edge of the outer cover plate. The cover plate has angular indicia thereon, which may be viewed through windows in the outwardly extending plate portions of the stop assemblies.
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BACKGROUND OF THE INVENTION
This invention relates to an apparatus for automatically aligning logs to be fed into a block sawing machine. At log sawing it is of great importance that the logs prior to their feed into the sawing machine are aligned and positioned so that optimum results and wood yield are obtained. Heretofore logs substantially have been aligned manually by turning them to a position, which visually had been deemed most favorable for producing the greatest possible wood yield. This alignment work, however, has proved not only to involve high physical strain but also to require a very good judgement and long experience. Due to the physical strain, however, even the most experienced staff has difficulties in permanently making optimum judgements. Therefore, it has long been a desire that a more or less automatic machine should be available which aligns the logs and eliminates at least the heavy and difficult operations.
An automatic apparatus for aligning blocks, it is true, is known previously, but this apparatus does not work unless at least one side of the object to be aligned is sawed plane and, therefore, this known apparatus cannot be used for aligning logs.
The object of the present invention, therefore, is to provide an apparatus for aligning logs which apparatus is so constructed that it fully automatically aligns every log to be fed into a sawing machine and thereby not only eliminates the heavy and difficult operations, but also saves labour and simultaneously improves the yield and increases the efficiency.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is described in greater detail in the following, with reference to the accompanying drawings, in which
FIG. 1 is a schematic lateral view of a log aligning apparatus according to the invention,
FIG. 2 is a schematic view of a section substantially along the line II--II in FIG. 1,
FIG. 3 is a schematic view of a section substantially along the line III--III in FIG. 1,
FIG. 4 is a schematic view of a section substantially along the line IV--IV in FIG. 5,
FIG. 5 is an end view of what is shown in FIG. 4, and
FIG. 6 is a section substantially along the line V--V in FIG. 1.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to FIG. 1, a feed chain 1, which is located in a feed bench is provided with drivers 1a for feeding a log into a sawing machine 4. Said machine comprises at least two saw blades 4a, which are movable in lateral direction for being adjusted relative to the predetermined vertical longitudinal central plane of the sawing machine, which plane coincides with the vertical longitudinal central plane A of the feed bench. During the in-feed operation every log is retained by a log holder 2, which is located above the feed chain 1 and can be of any per se known design. The holder, therefore, is not described here. Prior to its feed into the sawing machine 4, however, the log must be aligned and positioned for rendering the optimum result and wood yield.
According to the present invention, therefore, the feed bench is equipped with a plurality of upwardly open V-shaped yokes 8, which are arranged symmetrically in relation to the vertical longitudinal central plane A of the bench and spaced from each other along the bench for receiving and carrying the log to be fed into the sawing machine 4. The yokes 8 are supported each by an arm 3, which can be lifted and lowered and is pivotally mounted in the feed bench at 11, and which via a joint 12 is connected rigidly to a pull rod 13 being common for all yokes 8 and coupled to a cylinder and piston 14. With the cylinder and piston 14, thus, the yokes can be lifted and lowered simultaneously. The feed bench further comprises a device 5, which as shown consists of two conveyors 5a arranged in V-shape and driven in the same direction for turning a log applied on said yokes 8 and said conveyors 5a. The turning device 5 is lifted and lowered in the same way as the yokes 8, i.e. by an arm 15, which is mounted on the feed bench at 16 and via a joint 17 rigidly connected to the pull rod 13 of the yokes. The turning device, thus, is liftable and lowerable simultaneously with the yokes 8.
The log aligning apparatus according to the invention further comprises a plurality of sensing members 6 and 7, which in spaced relationship are arranged in the feed bench and capable of sensing how a log supported by the yokes 8 and turning device 5 changes its centre in relation to the vertical central plane A of the feed bench while it is being turned through an entire revolution by said turning device 5. The sensing members 7, more precisely, are arranged to sense the change in lateral direction, and the sensing members 6 are arranged for sensing the change in vertical direction, i.e. whether the log curve faces upward or downward. Each of the sensing members 6,7 are coupled to a respective potentiometer 9 and 10, which are connected in series in a loop or circuit to a computer or similar device (not shown) for evaluation of information received from the sensing members 6,7. Thereafter on the basis of the evaluation result the computer causes the turning device 5 to turn the log to a position providing the optimum wood yield, in which position a curved log shall be located with the curve upward and with its centre in the central plane A of the feed bench.
Each sensing member 7, more precisely, comprises two sensing arms 7a, which are located symmetrically in relation to the central plane A of the feed bench and interconnected for simultaneous movement. Said sensing arms 7a are actuated toward each other by a force exerting device 18 acting at least on one sensing arm, which device causes the sensing arms 7a to tend to always move toward one another to a starting position, in which the resistance of the potentiometer connected to the respective sensing member 7 is the lowest, whereby at least one of said sensing arms 7a always is held abutting the log side. When the log is being turned, the sensing arms 7a in the case of a curved log are moved apart or away from each other when the log with its centre B moves from the vertical central plane A, and are moved toward each other when the log with its centre B moves toward said central plane. The movement or deflection of said sensing arms is transferred to the potentiometer 10 of the sensing member, in such a manner that this potentiometer increases its resistance when the sensing arms 7a are moved apart and decreases its resistance when the sensing arms 7a move toward each other. The lowest resistance, thus, is obtained when the log with its centre B passes the vertical central plane A of the feed bench.
The sensing member 6, which senses whether the log curve faces upward or downward, comprises two sensing arms 6a, which are located symmetrically in relation to the central plane of the feed bench and interconnected for simultaneous movement. The sensing arms 6a like the sensing arms 7a are actuated toward each other by a force exerting device 19, which acts at least on one sensing arm 6a and, thus, causes the sensing arms 6a to tend to always move toward each other to a starting position, in which the resistance of the potentiometer 10 connected to this sensing member is the lowest. The sensing arms have contact surfaces 7b inclined toward each other, against which the log is intended to abut. Upon turning of the log, it presses apart the sensing arms 6a when it with its centre B moves downward from above, and permits the sensing arms 6a to move toward each other when the log with its centre B moves upward from below. This movement or deflection of the sensing arms is transferred to the potentiometer 9 of the sensing member, so that the potentiometer increases its resistance when the sensing arms 6a are moved apart, and decreases its resistance when the sensing arms 6a move toward each other. The lowest resistance, thus, is obtained when the curve of the log faces upward, and the centre B is located in the vertical central plane A of the feed bench.
The potentiometers 9,10 of the sensing members 6,7 being connected in series, different resistance values are obtained during the revolution of the log and fed into the computer. But of these values it is only one, the lowest one, which indicates the optimum alignment position for the log. When the log has been turned through one revolution, thus, the computer knows how the log is to be aligned for yielding the optimum sawing result, and it permits the turning apparatus 5 to turn the log until the computer again records the lowest resistance value previously obtained. The computer then stops the turning of the log. The alignment of the log thereby is completed, and the log can be fed into the sawing machine 4, possibly subsequent to a necessary lowering of the yokes 8 and to a switch-in of the log holder 2.
Instead of the sensing members 6,7 described above and shown in the drawings, it is possible within the scope of the invention to use optical scanners, although this is not shown. Said optical scanners may be photocells arranged in vertical ramps in tightly spaced relationship for scanning in vertical direction, and in horizontal ramps for scanning in lateral direction. By recording in relation to predetermined reference planes the number of photocells switched on and off by the log while being turned through one revolution, it is, thus, possible to determine the optimum alignment position for the log to be fed in.
Each sensing member 7 and preferably also sensing member 6 advantageously can be pivotal about a pivot 20 located in the vertical central plane A as shown in FIGS. 4 and 3, whereby the two sensing arms in each sensing member 7,6 normally are held in abutment to the log. By recording in the potentiometer 10,9 the pivotal motion of the sensing arms about the pivot 20, thus, the deflection transferred to the potentiometer is reduced very substantially, especially in cases when one and/or the other sensing arm in a sensing member during the turning of the log meets a projection from a knot remainder on the log.
The principles, preferred embodiments and mode of operation of the present invention have been described in the foregoing specification. However, the invention which is intended to be protected is not to be construed as limited to the particular embodiments disclosed. The embodiments are to be regarded as illustrative rather than restrictive. Variations and changes may be made by others without departing from the spirit of the present invention. Accordingly, it is expressly intended that all such variations and changes which fall within the spirit and scope of the present invention as defined in the claims be embraced thereby.
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An apparatus for automatically aligning logs to be sawn in a sawing machine in a position for yielding an optimum sawing result, comprising an arrangement for carrying the log to be aligned in a predetermined vertical longitudinal plane through the sawing machine, and a device for turning the log. The apparatus further comprises sensing members, which are connected to an evaluation which, control unit and by external sensing the log by the sensing members, records changes of the log center in relation to the longitudinal plane during one revolution of the log. Thereafter, the unit on the basis of information received determines the optimum alignment position and permits the turning device to turn the log into this position.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims foreign priority benefits under 35 U.S.C. §119(a)-(d) to DE 10 2016 203 201.1 filed Feb. 29, 2016, which is herein incorporated by reference in its entirety.
BACKGROUND
[0002] In modern motor vehicles, airbags form part of the restraint systems which are present as standard equipment. The airbag may be a plastic bag which is connected to a gas generator which serves to inflate the airbag in an accident. The gas generator in turn is triggered via sensors which normally react to high acceleration values, as may be present in the event of accidents. For safety reasons, it is desirable that the inflation of the airbag takes place very rapidly, for example within 20-50 ms after the start of the accident. This may be achieved via pyrotechnical gas generators, and alternatively with cold gas generators or hybrid gas generators. In addition to front airbags which are accommodated in the steering wheel and/or in the dashboard in front of the driver or passenger, some vehicles are also provided with side airbags. Side airbags are deployed between the door cladding and the seat, and serve to protect the side of the occupant adjacent the door. The side airbag may be accommodated inside the seat, commonly in the seat backrest. For reasons including aesthetics, the side airbag may be concealed below a cover of the seat backrest which also covers the seat cushion. The cover may also be called an outer cover.
[0003] In the event of an accident, the airbag is forced through a tear seam of the outer cover provided therefor, deploying outwardly. Before deployment, the tear seam connects two parts of the outer cover. The tear seam is designed to tear in the presence of forces which act when the airbag is deployed. A concern is that the tear seam is located in a region which in spatial terms is relatively narrowly defined as regards the airbag, whilst said airbag attempts to expand in all directions. The latter is undesirable in that it may lead to the airbag being forced into the cushion body of the seat, for example, or a different region where it is ineffective in terms of safety. Even when the airbag is forced through the tear seam, an expansion in other directions may result in the expansion into the safety-relevant region between the door cladding and the seat being delayed, so that optimal protection of the occupant is no longer able to be ensured.
[0004] In order to counteract this, therefore, so-called force concentrators are used in order to deflect the expansion of the airbag in the direction of the tear seam and/or to concentrate the expansion force onto the tear seam. Such force concentrators normally predominantly surround the airbag and include a material having low expandability which counteracts the forces present during the expansion of the airbag. The force concentrator is opened in the direction of the tear seam, whereby a direction of expansion for the airbag is predetermined. In many cases, the ends of the force concentrator on opposing sides of the tear seam are connected (for example stitched) to the cover so that during the expansion they tear apart the cover at the tear seam and thus cause the tearing of the tear seam.
[0005] U.S. Pat. No. 6,045,151 A discloses a seat cushion sub-assembly comprising a cushion which is supported by a frame as well as a cover which surrounds this seat cushion sub-assembly and has at least one seam. An airbag is attached with an inflation unit to the frame and is partially covered by the cushion and the cover. A cover element covers the airbag in order to hold the airbag in a folded position. A seam of the cover is aligned with the airbag such that the airbag is able to tear this seam when deployed. An approximately tubular force concentrator surrounds the cover element and the airbag. The force concentrator includes a layered, flexible material which is able to resist the pressure of the airbag during inflation and is connected with two opposing ends to the cover, for example by stitching. When the airbag is inflated, the force is oriented in the direction of the seam by the force concentrator, so that said seam tears.
[0006] U.S. Pat. No. 5,967,603 A discloses a vehicle seat having a frame element, an airbag attached thereto and an outer cover which surrounds the frame element and the airbag and has a predetermined tear line. A force concentrator is connected to the outer cover in the vicinity of the predetermined tear line. The force concentrator has two parts made of material which is flexible but not expandable. Said parts have proximal ends which on opposing sides of the predetermined tear line are connected to the outer cover and extend therefrom below the outer cover in opposing directions to the distal ends. The two parts are fastened to one another at these distal ends by complementary fastening means, such that they form a sleeve enclosing the airbag and the frame member.
[0007] A device for a vehicle seat is disclosed in FR 2 940 212 A3, said device comprising at least one airbag module and a force concentrator which serves to deflect the airbag in a predetermined region. In this case, the force concentrator and the airbag module are arranged adjacent to a support structure and secured, for example, by a screw and nut. The force concentrator may include the same material as the airbag and has a predetermined tear seam, said force concentrator being secured by means of a hook and loop fastener in the vicinity of said tear seam to a foam block of the vehicle seat.
[0008] FR 2 978 712 B1 discloses a backrest of a vehicle seat having a side airbag. In this case, an airbag module and a force concentrator which are screwed to a support structure are also provided. The force concentrator which surrounds the airbag module in the manner of a jacket has two adjacent ends which are arranged in the vicinity of a predetermined tear seam of an outer sleeve of the vehicle seat. The aforementioned ends in this case are connected via rapid fasteners to the parts of the outer sleeve adjacent to the predetermined tear seam, wherein the rapid fasteners may be configured as hook and loop fasteners, hooks or buttons.
[0009] DE 10 2011 105 461 A1 discloses a vehicle seat having a structural part, a cushion body as well as a cover which covers the cushion body and which has two cover parts connected together in a tear seam. Moreover, an airbag module is received in an airbag pocket which serves as a force concentrator and which is fastened with its two ends in the region of the tear seam to the cover. In order to prevent the airbag from being forced into the cushion body, a protective strip made of flexible tear-resistant material is also fastened between the airbag pocket and the cover.
[0010] DE 10 2006 053 601 A1 discloses a vehicle seat device having a frame, a seat cushion arranged in the vicinity thereof as well as a cladding cover which has a seam on one side of the seat. Moreover, an airbag module is provided with an airbag. A housing, the airbag being able to expand therein and having a tear seam, is enclosed by a force concentrator with two panels. The ends of the panels are fastened to the seam of the cladding cover, whereby they exert a force on this seam when the airbag is triggered.
[0011] In view of the prior art set forth, the rapid and reliable deployment of an airbag accommodated inside a vehicle seat leaves further room for improvement.
SUMMARY
[0012] A vehicle seat part, in particular for a motor vehicle such as a truck or a passenger motor vehicle, is provided. The vehicle seat part forms in this case at least one part of a vehicle seat, for example a seat surface or a seat backrest. The vehicle seat part has a cover with a tear seam, an airbag module with an airbag, as well as a force concentrator at least partially surrounding the airbag, for deflecting an expansion force of the airbag toward the tear seam. The cover which may also be denoted as the outer cover, sleeve or cladding of the seat part, forms at least one part of the actual surface of the vehicle seat. The cover generally includes a layered, flexible material, for example fabric, leather, synthetic leather or the like. Embodiments are also expressly possible in which the cover includes a plurality of layers. The cover comprises a tear seam which may also be denoted as the predetermined tear seam. This seam is provided such that it tears according to plan when the airbag is triggered and thus opens up a through-opening for the airbag.
[0013] The term “seam” is not to be understood as limiting, in that it has to be a stitched connection, but here it could also theoretically be a connection produced in a different manner, for example bonded or welded, between two portions or parts of the cover, which is structurally weakened in comparison with the adjacent material, so that it tears according to plan in the event of a corresponding load.
[0014] The cover at least partially surrounds the airbag module and/or that said airbag module is arranged inside the cover or behind said cover. For reasons of comfort, the vehicle seat part generally also comprises a cushion body arranged inside the cover, for example made of foamed plastics material. In addition, sensors, heating elements or other components may also be arranged below the cover, i.e. on the vehicle seat, which however are not critical to this description.
[0015] Apart from the actual airbag, for example a gas generator and/or an airbag sleeve which simply serves for packaging the folded-up airbag and yields without any appreciable resistance when said airbag is triggered, may also form part of the airbag module. Alternatively, the gas generator may be arranged at some distance from the airbag, optionally even outside the seat part, and may be connected thereto via a connection line, whereby it would not be part of an airbag module in the narrower sense. Normally, however, the gas generator more or less directly adjoins the airbag. The gas generator may be configured as a pyrotechnical gas generator or as a hybrid gas generator in which gas is pyrotechnically released from a pressurized container. The airbag itself is configured in the known manner as a flexible tear-resistant bag and may include a plastics film or a textile material, for example a woven fabric, which in turn may be coated with a film.
[0016] The force concentrator, which may also be denoted as an expansion force concentrator, expansion guiding element or the like, serves to deflect the force and/or the pressure which the airbag creates when deployed, and the expansion associated therewith, in the direction of the tear seam. It could also be said that the function of the force concentrator is to concentrate this force in the region of the tear seam or to deflect the expansion of the airbag in the direction of the tear seam. To this end, the force concentrator which generally includes a material which is flexible but has relatively little elasticity, at least substantially surrounds the airbag. In a typical embodiment, the force concentrator is configured in the manner of a jacket or sleeve. It is possible that the force concentrator includes a material which may also be used for an airbag and/or includes the same material as the airbag.
[0017] The force concentrator has two end regions which are connected on opposing sides of the tear seam to the cover. The end regions may, for example, be ends of a strip of flexible material, the force concentrator consisting of said material. The one end region is connected relative to the tear seam on one side to the cover, whilst the other end region is connected on the opposing side to the cover. In a normal case, the tear seam connects two parts of the cover together so that each of the end regions is connected to just one of the two parts. Generally, the connection is provided in a region adjacent to the tear seam. The connection may be configured by a positive, non-positive and/or material connection. The connection does not have to be gas-tight but in any case it should be stronger than the connection represented by the tear seam. Thus it is ensured that when a force acts on the end region, this force acts via the aforementioned connection onto the cover and thus onto the tear seam, wherein the tear seam tears when a specific load is exceeded, whilst the connection between the end region and the cover ideally remains intact. It could be said that the cover is torn apart by the action of the force of the end regions of the force concentrator on the tear seam.
[0018] One end region may be connected to the cover only in a plurality of connecting portions spaced apart from one another along the tear seam. In other words, the at least one end region is not connected to the cover continuously along the tear seam but here there are connecting portions in which a connection is provided between the end region and the cover, and between two connecting portions in each case there is a portion without a connection, to a certain extent a “free”, “unconnected” or “connection-less” portion. This means that the force concentration and/or the tearing apart of the tear seam takes place through the end regions of the force concentrator, as described above, initially only and/or primarily on the connecting portions. In this case it is provided that the yielding of the tear seam has its starting point in these connecting portions but then continues to the further unconnected portions. As a result, it may be possible to ensure that the tear seam tears more or less at the same time at a plurality of points, whereby the tearing may take place as a whole more rapidly and/or more uniformly, which in turn overall has a positive effect on the expansion of the airbag.
[0019] Advantageously, both end regions are connected to the cover only in the connecting portions spaced apart from one another along the tear seam. In other words, in the direction of extension of the tear seam, there are connecting portions in which both end regions are connected to the cover, and between two connecting portions in each case a (connection-less) portion in which neither of the two end regions is connected to the cover. This embodiment is advantageous in that a relatively symmetrical force acts on the tear seam, i.e. a pulling force which is exerted by the one end region is applied toward one side and a pulling force which is exerted by the other end region is applied toward the other side. In one portion where there is no connection between the cover and the force concentrator, a considerably lower force is applied on the tear seam which also—at least in terms of order of magnitude—may be regarded as symmetrical.
[0020] In particular, the at least one end region may be connected in at least two connecting portions to the cover. There are two connecting portions, a portion being arranged therebetween where no connection is provided between the end region and the cover. The two connecting portions may be arranged in particular in the direction of extent of the tear seam at the two ends of the end region. Alternatively, however, three, four or more connecting portions may also be provided, which also may be determined according to the respective application.
[0021] According to a preferred embodiment, each of the two connecting portions extends over 20 to 40% of the at least one end region. Further preferably, each of the connecting portions may extend over 30-35% of the at least one end region. This naturally refers to the extent of the end region in the direction of the tear seam. When, therefore, the connecting portions in the direction of the tear seam begin and/or end at the end of the end regions, for example a first connecting portion may extend over 30% of the end region and a second connecting portion may also extend over 30%, wherein a connection-less portion extends therebetween over 40% of the end region. It might also be conceivable that each of the portions takes up exactly one third of the end region. If the extent of one of the connecting portions is less than 20%, this may potentially lead to no effective force concentration at this point and the tear seam not tearing primarily here but only secondarily due to the tearing at a different point. If one or even both connecting portions extends over more than 40% of the end region, the deployment dynamics of the airbag is potentially similar to that in a system where the end regions are connected over the entire length to the cover. In principle, however, embodiments are also possible and may be effective where the extent of at least one connecting portion is outside the cited region. It is also possible, for example, to provide two or more connecting portions having a different extent.
[0022] Irrespective of the number of connecting portions, it is preferred that these portions extend as a whole over at most 80% of the end regions. If an even larger part of the end regions is taken up by the connecting portions, the deployment dynamics are potentially similar to those in a connection over the entire length, i.e. the advantages according to the arrangement described herein may be reduced.
[0023] The connection of the end regions to the cover may be implemented in different ways. Thus this may be carried out, for example, by bonding or welding. Advantageously, the end regions are stitched to the cover. This connecting method is appropriate in that both the force concentrator and the cover normally include layered, flexible materials which may be stitched together relatively easily in terms of process technology. Moreover, a very strong connection may be implemented by a seam which preserves the flexibility of the connected materials and also permits displacements of the materials relative to one another.
[0024] According to one embodiment, at least one end region between two connecting portions has an indented region which is set back from the tear seam. In other words, whilst the contour of the end region in the connecting portions is normally in line with the path of the tear seam, the contour in the indented region is set back from the tear seam, i.e. the end region here is at a greater distance from the tear seam. This means at the same time that here there is also a greater distance from the other end region and/or that the force concentrator has a larger hole here. By this measure the concentration of force onto the connecting portions is assisted and in the region located therebetween only a relatively low force is exerted on the tear seam. If an indented region is not provided between two connecting portions and the end region here is located in the vicinity of the tear seam, this may have the result in some cases that in spite of the absence of a connection between the end region and the cover a considerable force acts on the tear seam and thus the concentration of force onto the connecting portions is impaired.
[0025] The arrangement described herein may be used, in principle, for all airbag systems which are accommodated in vehicle seats, such as for example seat cushion airbags arranged in the seat surface. Preferably, however, the vehicle seat part is configured as a seat backrest, the tear seam being arranged thereon at the side. “At the side” naturally refers here to the viewing direction of an occupant on the vehicle seat. The airbag in this case is thus a side airbag which is provided to be deployed between the seat and the side wall and/or the door cladding.
[0026] It is possible to produce the force concentrator from a single piece, for example from a layered strip made of plastics material which surrounds the airbag, and the edges thereof form the end regions. According to a further embodiment, the force concentrator may include two parts, in each case an end region being formed thereon, and which are connected together on a side remote from the tear seam. The two parts may, for example, be material strips, films or the like. The connection of the two parts may, for example, be implemented by stitching, bonding, welding or other appropriate techniques. The connection does not necessarily have to be seamless but larger holes could result in the airbag expanding therein which would impair the effectiveness of the force concentrator.
[0027] According to one embodiment, the airbag may be fastened to a frame part of the vehicle seat part arranged inside the cover. The frame part may form part of a frame of the vehicle seat part which substantially lends the vehicle seat part its mechanical stability and, for example, includes metal, for example steel. In the case of a seat backrest, the frame also serves for the pivotable connection to the seat surface which in turn is connected (in a manner adjustable in its position) to the vehicle floor. The frame part may, in particular, be a sheet metal shaped part. Normally the entire airbag module including the gas generator is fastened to the frame part. This also encompasses embodiments in which the airbag is indirectly fastened to the frame part via the gas generator. The fastening may take place, for example, by a screw connection.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] FIG. 1 shows a side view of a seat backrest according to the prior art.
[0029] FIG. 2 shows a sectional view along the cutting line II-II in FIG. 1 .
[0030] FIG. 3 shows a schematic view of a part of a seat backrest.
[0031] FIG. 4A shows a sectional view of the seat backrest along the cutting line IV-IV of FIG. 3 .
[0032] FIGS. 4B-4D show sectional views according to FIG. 4A which illustrate the sequence of an expansion process of an airbag.
DETAILED DESCRIPTION
[0033] In the various figures the same parts are always provided with the same reference numerals, which is why these parts are only described once.
[0034] FIG. 1 and FIG. 2 show a seat backrest 100 for a motor vehicle according to the prior art, wherein FIG. 1 is a side view and FIG. 2 is a sectional view. An airbag module 103 with an airbag 104 and a gas generator, not shown here, is located at the side of the seat backrest 100 below a cover 101 . The airbag module 103 is screwed to a frame part 105 which provides the seat backrest 100 with mechanical stability. The gas generator is located in the region of the screw connection. The airbag module 103 is surrounded by a jacket-like force concentrator 106 which has two end regions 106 . 1 , 106 . 2 . On opposing sides of a tear seam 102 of the cover 101 these end regions 106 . 1 , 106 . 2 are connected to said cover. The force concentrator 106 includes the same material as the airbag 104 , for example a synthetic fiber fabric which is coated with a silicone film. When the airbag 104 is triggered, an expansion thereof is limited and/or deflected by the force concentrator 106 surrounding it, and namely in the direction of the end regions 106 . 1 , 106 . 2 and the tear seam 102 .
[0035] FIG. 3 and FIG. 4 show the seat backrest 10 . FIG. 3 shows a schematic side view of a part of the seat backrest 10 , whilst FIG. 4 is a sectional view. The construction of the seat backrest 10 substantially corresponds to the seat backrest 100 of FIGS. 1 and 2 . Thus also in this case an airbag module 3 with an airbag 4 is screwed to a frame part 5 and is partially surrounded by a jacket-like force concentrator 6 . Also here, a gas generator, not shown, of the airbag module 3 is located in the region of the screw connection to the frame part 5 . Cushion bodies 7 , 8 made of foam are provided on both sides of the frame part 5 and the force concentrator 6 , said cushion bodies providing the seat backrest 10 with the required shape and resilience. Also here, a cover 1 is stretched over the aforementioned parts 3 - 8 , said cover having a tear seam 2 . The tear seam 2 in the present case is stitched but also other connection methods are possible. As may be identified by way of example in FIG. 3 in the side view, the force concentrator 6 in the drawing plane tapers from bottom to top, i.e. a dimension and/or extent transversely to the tear seam 2 is greater in a lower region than in an upper region. In FIG. 3 , for example, an upper edge in the drawing plane is smaller in its extent D 1 than the extent D 2 of the edge arranged below in the drawing plane. Thus the force concentrator 6 is able to be mounted in a particularly simple and easy manner. Naturally, the force concentrator 6 may also taper from top to bottom, viewed in the drawing plane.
[0036] The force concentrator 6 consists in the present case of two parts 6 . 7 , 6 . 8 ( FIG. 4A ) which are connected together on a side remote from the tear seam 2 by a connecting seam 6 . 9 . The force concentrator 6 has two end regions 6 . 1 , 6 . 2 which are connected to the cover 1 on opposing sides of the tear seam 2 , for example by stitching. However, the connection is only provided in partial regions, namely for example in two connecting portions 6 . 3 , 6 . 4 ( FIG. 3 ) which are arranged relative to the path of the tear seam 2 at the end of the end regions 6 . 1 , 6 . 2 and extend approximately in each case over a third of the end regions 6 . 1 , 6 . 2 . A connection-less portion 6 . 5 is located therebetween in which the end regions 6 . 1 , 6 . 2 are not connected to the cover 1 . Here they also have an indented region 6 . 6 which is set back relative to the tear seam as is visible in FIG. 3 .
[0037] If the airbag module 3 is triggered, the airbag 4 initially starts to expand inside the force concentrator 6 until it substantially fills the airbag as shown in FIG. 4B . Whilst the force of the airbag 4 is not sufficient in order to tear the force concentrator 6 itself, via the connection to the cover 1 provided in the connection portions 6 . 3 , 6 . 4 a tensile force is exerted on both sides of the tear seam 2 , resulting in the tear seam ultimately yielding and/or tearing, as shown in FIG. 4C . In this case the tearing initially takes place (at the same time or rapidly in succession) in the region of the connecting portions 6 . 3 , 6 . 4 and then continues into the connection-less region 6 . 3 located therebetween. Overall, this may lead to a more uniform and/or more rapid tearing of the tear seam 2 which accelerates the expansion of the airbag 4 . After the airbag 4 has been forced into the tear seam 2 , it expands unhindered outwardly as shown in FIG. 4D .
[0038] The disclosure has been described in an illustrative manner, and it is to be understood that the terminology which has been used is intended to be in the nature of words of description rather than of limitation. Many modifications and variations of the present disclosure are possible in light of the above teachings, and the disclosure may be practiced otherwise than as specifically described.
|
A vehicle seat part has a cover with a tear seam and an airbag module with an airbag and a force concentrator. The force concentrator partially surrounds the airbag. The concentrator has two end regions connected to the cover adjacent to and on opposing sides of the tear seam. One of the end regions is connected to the cover at a plurality of connecting portions spaced apart from one another.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates generally to assuring safe and efficient operation of a battery. More particularly, the invention relates to a system for continually assuring that a battery has a satisfactory state of health (SoH) while the battery is installed in its operating environment
[0002] A battery pack's SoH degrades with use and over time because individual cells in the battery pack lose their ability to store and deliver electrical energy with use and over time. But, the battery pack operating voltage range remains the same even with degradation in a battery's capacity. Thus, while a battery pack may appear ostensibly to be in satisfactory operational condition, the battery pack may, in fact, be on the verge of failure. In some instances such failure may produce problems beyond mere lack of performance of the battery pack. For example, because individual cells in the battery pack are not identical, the individual cells may degrade at a different rate with time and use. This may lead to a condition known as cell unbalance. A battery pack with degraded cells may still deliver a desired output. However, the degraded cell(s) may discharge or charge at a faster rate when compared with the other cells in the pack. Temperature of degraded cell(s) during operation may have more variance when compared with healthy cells and may lead to unsafe conditions such as thermal runaway.
[0003] Some battery packs are employed to deliver electrical power in applications where safety is of paramount importance. For example, numerous battery packs are used in modern “more electric aircraft” (MEA). To assure safe operation of such an aircraft, it would be desirable to provide a flight crew with a continuous report of the SOH and/or cell unbalance of battery packs on the aircraft so that the flight crew might take corrective action in the event of a report of a potential failure of a battery pack.
[0004] As can be seen, there is a need for system that enables safe use of battery packs in environments such as aircraft.
SUMMARY OF THE INVENTION
[0005] In one aspect of the present invention, a system for assuring safe use of a battery pack comprises: a switch connecting the battery pack to a DC power system; a display unit; a state of health (SoH) monitor connected to the battery pack, the SoH monitor including; a processor; and a memory block comprising a non-transitory computer-readable medium with instructions stored thereon, that when executed by the processor, performs the steps; a) instructs the SoH monitor to measure terminal voltage of the battery pack at a beginning of a current flow cycle; b) instructs the SoH monitor to measure terminal voltage of the battery pack after completion of the current flow cycle c) instructs the SoH monitor to successively re-measure terminal voltage of the battery pack after completion of the current flow cycle until one of the successively re-measured terminal voltages is equal to a previous one of the re-measured terminal voltage; d) instructs the SoH monitor to determine and record ampere-hours (Ah) passing through the battery pack during the time period between steps a) and c); e) instructs the SoH monitor to determine SoH of the battery pack as a function of a quotient of a difference between terminal voltages determined in steps a) and c) divided by the Ah determined in step d), and f) instructs the SoH monitor to send the SoH determined in step e) to the display unit for display as an updated SoH of the battery pack; wherein the switch is operable to disconnect the battery pack from the DC power system upon the display unit indicating SoH of the battery pack being below a predetermined value.
[0006] In another aspect of the present invention, apparatus for controlling electrical power distribution on an aircraft comprises. a starter motor for an engine of the aircraft; a DC power system connected to the starter motor; a battery pack; a first switch connecting the battery pack to the DC power system; a second switch for connecting the starter motor to an external power source; a state of heath (SoH) monitor connected to the battery pack; a display unit connected to the SoH monitor for displaying SoH of the battery pack; and a disconnect control unit configured to open the first switch and close the second switch in the event that displayed SoH of the battery pack is below a predetermined value.
[0007] In still another aspect of the present invention, a method for assuring safe use of a battery pack in a DC power system comprising the steps: determining terminal voltage change values for n cells of the battery pack during a current flow cycle; determining terminal voltage change value for the battery pack during the current flow cycle; dividing the battery pack voltage changes value by each of n cell voltage change values to develop terminal-voltage-change indices for the n cells; determining if the terminal-voltage-change indices for the n cells are equal; generating a cell-unbalance display in the event of inequality of any of the n terminal-voltage-change indices; disconnecting the battery pack from the DC power system in the event of said inequality.
[0008] These and other features, aspects and advantages of the present invention will become better understood with reference to the following drawings, description and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is block diagram of a system for assuring safe use of a battery in accordance with an exemplary embodiment of the invention;
[0010] FIG. 1A is a block diagram of a system for assuring safe use of a battery in accordance with a second exemplary embodiment of the invention;
[0011] FIG. 2 is a block diagram of a state of health (SoH) monitor of the system of FIG. 1 in accordance with an exemplary embodiment of the invention;
[0012] FIG. 3 is a plot of time versus battery voltage of a battery pack of the system of FIG. 1 in accordance with an exemplary embodiment of the invention;
[0013] FIG. 4 is an electrical equivalent 2-RC model of the battery pack of the system of FIG. 1 in accordance with an exemplary embodiment of the invention; and
[0014] FIG. 5 is a flow chart of a method for assuring safe use of a battery pack in accordance with an exemplary embodiment of the invention; and
[0015] FIG. 6 is a flow chart of a method for assuring safe use of a battery pack in accordance with another exemplary embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0016] The following detailed description is of the best currently contemplated modes of carrying out the invention. The description is not to be taken in a limiting sense, but is made merely for the purpose of illustrating the general principles of the invention, since the scope of the invention is best defined by the appended claims.
[0017] Various inventive features are described below that can each be used independently of one another or in combination with other features.
[0018] The present invention generally provides a system for assuring safe use of a battery pack. More particularly, the invention provides for monitoring and displaying of SoH while the battery pack is installed and operational to determine if continued use of the battery should be terminated. Still further, the invention provides for monitoring SoH of individual cells and cell unbalance of the battery pack to determine if the battery pack should be disconnected from a DC power system.
[0019] Referring now to FIG. 1 , an exemplary embodiment of a safety-control system 100 for a battery pack 102 is illustrated. The control system 100 may include a state-of-health monitor 104 (hereinafter SoH monitor 104 ) coupled to the battery pack 102 and to individual cells 108 of the battery pack 102 . A display unit 112 may be coupled to SoH monitor 104 . A disconnect control 114 may be connected to operate a disconnect contactor or switch 116 to disconnect the battery pack 102 from a DC power system 118 . If an unsafe condition within the battery pack 102 or the SoH of the battery pack 102 is below a predetermined value, the battery pack 102 may be disconnected from the DC power system 118 .
[0020] Referring now to FIG. 1A , an exemplary embodiment of battery-pack safety control system 200 is illustrated as it might be employed in an aircraft (not shown). The system 200 may differ from the system 100 in that a disconnect control 214 may be connected to operate both the switch 116 and a second switch 117 . When the switch 116 is open and the switch 117 is closed, the battery pack 102 may be disconnected from a starter motor 119 of an engine (not shown) of an aircraft. The starter motor 119 may then be powered from an external power source 121 in the event that SoH of the battery pack 102 is lower than a predetermined value.
[0021] The system 200 may be useful in an aircraft that may be employed in short-haul operations. The flight crew may observe, from the display unit 112 , that SoH of the battery pack 102 may be low, but still above a predetermined replacement limit. In that case, the flight crew may elect to use external power source 121 for driving a starter motor 119 of an auxiliary power unit (APU) of the aircraft instead of using the on-board battery pack 102 for such APU starting. In this manner, the flight crew may extend useful life of the battery pack 102 and avoid a need for a non-scheduled battery pack replacement. In other words, replacement of the low-SoH battery pack may be delayed until the aircraft is taken out of service for regularly scheduled maintenance.
[0022] Referring now to FIG. 2 , a block diagram illustrates an exemplary embodiment of the SoH monitor 104 . The SoH monitor 104 may include a measurement block 120 having a voltage sensor 122 , a current sensor 124 and a temperature sensor 126 . The measurement block 120 may be adapted to take on-line measurements from the battery pack 102 . The SoH monitor 104 may also include a computer 128 with a non-volatile memory 132 and a processor 136 .
[0023] Referring now to FIGS. 1 and 2 , it may be seen that individual cells 108 of the battery pack 102 may be connected to the SoH monitor 104 . More particularly, individual cells 108 may be connected to a cell measurement block 106 of the SoH monitor 104 . The cell measurement block 106 may include a plurality, n, of voltage sensors 140 coupled individually to each of n cells 108 .
[0024] In operation, the SoH monitor 104 may perform an SoH determination each time the battery pack 102 experiences completion of a cycle of current flow resulting from either charging or discharging. Such a cycle may include an initiation of current flow followed by a termination of the current flow. In some applications, the battery pack 102 may experience multiple cycles of current flow with relatively short time periods between cycles. For example, the battery pack 102 may provide power to a load for a period of five minutes and then after a lapse on only a few seconds the battery pack 102 may again provide power to a load for a five minute period. Such rapidly changing and repeating load powering may be considered to be a dynamic mode of operation.
[0025] Alternatively, the battery pack 102 may be installed in a vehicle such as an aircraft which may be parked at a terminal for a period of an hour or more, during which time the battery pack 102 may not be subjected to any cycles of current flow. In such a context, the battery pack 102 may be subjected to current flow cycles at intervals that may spaced apart in time by periods of hours. In other words, the current flow cycles may be separated in time by rest periods. Such a mode of operation may be referred to herein as a resting mode of operation.
[0026] The SoH monitor 104 may utilize a first SoH estimation technique for determining SoH for a cycle of current flow during a resting mode of operation of the battery pack 102 . The SoH monitor 104 may utilize a second SoH estimation technique when a cycle of current flow occurs in the context of a dynamic mode of operation of the battery pack 102 .
[0027] Referring now to FIG. 3 , a graph 300 illustrates a time versus battery voltage relationship for the battery pack 102 as it undergoes a cycle of current flow in a rested mode of operation. As the battery pack 102 discharges, changes in terminal voltage may be observed due to the following phenomena:
1. V d(res) —Instantaneous drop in voltage due to series ohmic resistance at the start of discharge; 2. V d(pol+dis1) —Drop in voltage due to combined effect of polarization and discharge phenomena; 3. V d(dis2) —Drop in voltage due to discharge phenomenon only; 4. V r(res) —Instantaneous rise in voltage due to series ohmic resistance at the end of discharge; and 5. V r(depol) —Rise in voltage due to depolarization phenomenon during rest period.
[0033] The term “V d(pol+dis1) ” may be resolved into two components “V d(pol) ” and “V d(dis1) ”. The components “V d(pol) ” may represent voltage drop due to polarization effect and “V d(dis1) ” may represent voltage drop due to charge delivering phenomenon during polarization period. Among the five phenomena listed above, only the “V d(dis1) ” and “V d(dis2) ” components represent terminal voltage lost due to charge delivering phenomenon. The other components are not associated with charge delivering phenomenon but still, they may affect a total change in terminal voltage.
[0034] Terminal voltage drop or gain per Ampere-Hour (Ah) delivered or received changes with battery health. Therefore, SoH function may be determined in accordance with the expression,
[0000]
SoH
=
f
(
Δ
V
bat
Ah
)
(
1
)
[0035] In this context, SoH is most accurately determined if the term “ΔV bat ” represents the change in terminal voltage due only to charge delivering phenomenon during discharge or charging operation. But, the total drop in terminal voltage during discharge operation is given by:
[0000] Δ V bat(total) =V d(res) +V d(pol) +( V d(dis1) +V d(dis2) )=Total Voltage Drop (2)
where V d(res) =Instantaneous drop in voltage due to series ohmic resistance; V d(pol) =Drop in voltage due to polarization effect; and V d(dis1) +V d(dis2) =Drop in voltage due to charge delivering phenomenon
[0039] As a practical matter, it may not be possible to separate and extract the voltage drop only due to charge delivering phenomenon (i.e. “V d(dis1) +V d(dis2) ”) in the above equation. Instead, the first two terms may be compensated for or cancelled out using rising voltage components that occur after discharge or charging operation.
[0040] There may be an instantaneous voltage rise “V r(res) ” in the battery terminal voltage at the end of discharge. This may be equal in magnitude and opposite in polarity to the instantaneous drop observed at the start of discharge operation. So, “V r(res) ” component can compensate “V d(res) ”.
[0000] V r(res) =−V d(res) (3)
[0041] Also, depolarization that occurs after the current flow cycle may compensate the polarization effect that occurs at a beginning of the current flow cycle. The battery pack 102 may get depolarized during a rest period to the same extent it is polarized during the current flow cycle, provided that the battery pack 102 is sufficiently rested after the current flow cycle. The voltage drop “V d(pol) ” due to polarization is equal to the voltage rise “V r(depol) ” during depolarization.
[0000] V r(depol) =−V d(pol) (4)
[0042] Net change in terminal voltage during discharge operation is given by,
[0000]
Δ
V
bat
=
V
d
(
res
)
+
V
d
(
pol
)
+
(
V
d
(
dis
1
)
+
V
d
(
dis
2
)
)
+
V
r
(
res
)
+
V
r
(
depol
)
(
5
)
Thus
SoH
=
f
(
Δ
V
bat
Ah
)
=
f
(
V
d
(
res
)
+
V
d
(
pol
)
+
V
d
(
dis
1
)
+
V
d
(
dis
2
)
+
V
r
(
res
)
+
V
r
(
depol
)
Ah
)
(
6
)
[0043] Using eq. (3) and (4), rewriting eq. (6),
[0000]
SoH
=
f
(
Δ
V
bat
Ah
)
=
f
(
V
d
(
dis
1
)
+
V
d
(
dis
2
)
Ah
)
(
7
)
[0044] It may be noted that accuracy of the rested-mode estimation technique described above may be dependent upon the occurrence of a sufficiently long rest period between successive current flow cycles. As explained hereinbelow and illustrated in FIG. 5 , such sufficiency of length of a rest period may be determined to exist when successive measurements of V r(depol) (See FIG. 3 ) at an end of a current flow cycle are equal to one another.
[0045] If the battery pack 102 is operated with only insufficient rest periods between successive current flow cycles, the second or dynamic-mode estimation technique may be performed. This dynamic-mode estimation may be performed in a manner similar to that described in US Patent Application Publication 2013/0138369, which publication is incorporated herein by reference in its entirety. In the dynamic-mode estimation technique, the computer 128 may employ a battery dynamic model 130 stored in the non-volatile memory 132 . The battery dynamic model 130 may include various values of parameters R s , C st , R st , C lt and R lt determined at various temperatures, terminal voltages and currents while the battery pack 102 is off line. The parameters may be elements of a battery model 133 illustrated in FIG. 4 .
[0046] The computer 128 may include a processor 134 adapted to receive the on-line measurements from the measurement block 120 and to calculate an open circuit voltage online, using an equation
[0000] V OC =V BAT +ΔV R +ΔV P (8)
[0000] where
[0047] V BAT =Battery terminal voltage;
[0048] ΔV R =Voltage drop due to battery resistance;
[0049] ΔV P —Voltage drop due to polarization phenomenon; and
[0050] wherein ΔV P is computed using an equation
[0000]
Δ
V
P
=
I
*
[
(
R
st
1
+
(
R
st
·
C
st
)
s
)
+
(
R
lt
1
+
(
R
lt
·
C
lt
)
s
)
]
(
9
)
[0000] in which values of R s , C st , R st , C lt and R lt are determined from the battery dynamic model 130 by comparing the on-line measurements to the battery dynamic model 130 .
[0051] Accuracy of a resultant calculation of Voc may be enhanced by recursive application of mathematical filtering within the processor 134 . In an exemplary embodiment of the invention the following adaptive filter equations may be employed:
State Estimate Equation (Time Update:
[0052]
[
SoC
(
k
)
V
ST
(
k
)
V
LT
(
k
)
]
=
[
1
0
0
0
1
-
(
dt
R
ST
(
k
-
1
)
*
C
ST
(
k
-
1
)
)
0
0
0
1
-
(
dt
R
LT
(
k
-
1
)
*
C
LT
(
k
-
1
)
)
]
[
SoC
(
k
-
1
)
V
ST
(
k
-
1
)
V
LT
(
k
-
1
)
]
+
[
-
d
t
Q
d
t
C
ST
(
k
-
1
d
t
C
LT
(
k
-
1
)
]
[
/
Bat
(
k
)
]
…
(
10
)
V
OC
(
k
)
-
=
V
OC
(
SoC
(
k
)
-
)
(
11
)
Output Equation
[0053] V Bat(k) =V OC ( SoC (k) )− V ST(k) −V LT(K) −└I Bat(k) *R ser ┘ (12)
State Correction Equation (Measurement Update):
[0054]
[
SoC
(
k
)
+
V
ST
(
k
)
+
V
LT
(
k
)
+
]
=
[
SoC
(
k
)
-
V
ST
(
k
)
-
V
LT
(
k
)
-
]
+
L
k
[
V
Bat
(
mes
)
-
V
Bat
(
k
)
]
(
13
)
V
OC
(
k
)
+
=
V
OC
(
SoC
(
k
)
+
)
(
14
)
Where:
[0000]
R ser is ohmic resistance of the battery pack;
Q is the full capacity of the battery;
L k is the filter gain matrix; and
V Bat(mes) is the measured battery voltage.
[0059] SoH of the battery pack 102 may then be determined in the manner described in US Patent Application Publication 2013/0138369 by employing the value of Voc determined in accordance with the dynamic-mode estimation technique described above.
[0060] Referring now to FIG. 5 , a flow chart illustrates an exemplary embodiment of a method 500 for assuring safe use of a battery pack. The method 500 may employ either or both of the rested-mode SoH estimation technique and the dynamic-mode SoH estimation technique. In a step 502 , terminal voltage of the battery pack may be measured at a beginning of a current flow cycle (e.g. the terminal voltage may be measured by the voltage sensor 122 of the SoH monitor 104 ). In a step 504 , an end-of-cycle terminal voltage of the battery pack may be measured at an end of the current flow cycle (e.g. V r(depol) of FIG. 3 may be measured by the voltage sensor 122 ). In a step 508 , the end-of-cycle terminal voltage may be re-measured (e.g. V r(depol) of FIG. 3 may be re-measured by the voltage sensor 122 ). In a step 510 . the end-of cycle terminal voltage of step 506 may be compared to the end-of-cycle terminal voltage of step 506 . If the measured voltage of step 508 is unequal to the measured voltage of step 506 , the steps 506 and 508 may be successively repeated until the voltages of steps 504 and 506 are found to be equal. Equality of voltage measurements of steps 506 and 508 may be indicative of passage of sufficient time to assure that the rested-mode of estimation may be properly employed.
[0061] In a step 510 , a determination may be made as to whether a new current flow cycle has begun prior to achieving re-measured terminal voltage equality in step 508 . In that event SoH of the battery pack may be estimated in step 512 in accordance with the dynamic-mode of SoH estimation. If, in step 508 , end-of-cycle terminal voltage of steps 504 and 506 are found to be equal, then SoH of the battery pack may be estimated in step 514 in accordance with the rested-mode of SoH estimation.
[0062] If step 514 is performed, then in a step 516 , rested-mode SoH estimations may be displayed at the nominal value determined in step 514 . If step 516 is performed, then in a step 518 , a dynamic mode estimation of SoH may be displayed with an adjusted value of the actual SoH determined in step 512 . Rested-mode estimations may have a higher likelihood of being accurate as compared to dynamic-mode SoH estimations. Thus, the dynamic-mode SoH estimation may be adjusted to account for a potential margin of error. For example, a adjusted dynamic-mode SoH value may be about 0.01% to about 0.015% lower than a nominal SoH value determined by the rested-mode estimation technique. In a step 520 , the battery pack may be disconnected from a DC power system if SoH of the battery pack is below a predetermined value.
[0063] Referring now to FIG. 6 , a flow chart illustrates another exemplary method 600 for assuring safe use of a battery. The method 600 may differ from the method 500 in that cell unbalance and SoH values of individual cells of the battery are monitored and displayed. In a step 602 , terminal voltage change for each of n cells may be determined during a current flow cycle (e.g., terminal voltage change may be measured with the n voltage sensors 140 of the cell measurement block 106 ). A step 604 may be performed simultaneously with step 602 . In the step 604 , terminal voltage change for the battery pack may be determined during the current flow cycle (e.g., terminal voltage change may be measured with the voltage sensor 122 of the measurement block 120 during the same current flow cycle for which terminal voltage change is measured in step 602 ).
[0064] In a step 606 , the voltage changes measured in steps 602 and 604 may be combined to develop a terminal-voltage-change index for each of the n cells in accordance with the expression:
[0000]
Δ
V
index
(
cn
)
=
Δ
V
pack
Δ
V
cn
(
15
)
[0065] In a step 608 , a determination may be made as to whether the terminal-voltage-change indices for all the n cells are equal. In a step 610 , a cell-unbalance display may be generated in the event of inequality of any of the n terminal-voltage-change indices. In the step 610 , the identity of one or more degraded cells may also be displayed. SoH for each of the n cells may be determined in accordance with the expression;
[0000]
SoH
cn
=
Δ
V
index
(
cn
)
×
SoH
pack
n
(
16
)
[0066] In a step 614 , SoH for each of the n cells may be displayed (e.g., the display unit 112 of FIG. 1 may be employed to display the SoH information from step 614 ). In step 616 , a disconnect alarm may be generated if a high unbalance is present (e.g., the display unit may provide a high unbalance display if cell unbalance exceeds about 0.1 volts to about 0.15 volts). In that event, a step 618 may be performed in which the battery pack may be disconnected from a DC power system.
[0067] Referring back to FIG. 1 , it may be seen that with such a collection of battery-related information on the display unit 112 , an observer of the display unit 112 may have an opportunity to make a real-time decision as to whether or not to allow the battery to continue performing its role. Consider, for example, the battery pack 102 being installed in an aircraft. The flight crew might elect to operate the disconnect control 114 if the display unit 112 showed that a cell unbalance condition exceeding about 0.1 to about 0.15 volts had developed. The battery pack 102 would then be disconnected from the DC power system 118 and a risk of overheating of the battery pack 102 might be precluded.
[0068] It should be understood, of course, that the foregoing relates to exemplary embodiments of the invention and that modifications may be made without departing from the spirit and scope of the invention as set forth in the following claims.
|
A system for assuring safe use of a battery pack includes a display unit and a state of health (SoH) monitor connected to the battery pack, the SoH monitor. The SoH monitor a) instructs the SoH monitor to measure terminal voltage of the battery pack at a beginning of a current flow cycle; b) instructs the SoH monitor to measure terminal voltage of the battery pack after completion of the current flow cycle; c) instructs the SoH monitor to successively re-measure terminal voltage of the battery pack after completion of the current flow cycle until one of the successively re-measured terminal voltages is equal to a previous one of the re-measured terminal voltage; d) instructs the SoH monitor to determine and record ampere-hours (Ah) passing through the battery pack during the time period between steps a) and c); e) instructs the SoH monitor to determine SoH of the battery pack as a function of a quotient of a difference between terminal voltages determined in steps a) and c) divided by the Ah determined in step d), and f) instructs the SoH monitor to send the SoH determined in step e) to the display unit for display as an updated SoH of the battery pack. A switch is operable to disconnect the battery pack from the DC power system upon the display unit indicating SoH of the battery pack being below a predetermined value
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CROSS-REFERENCE TO RELATED APPLICATIONS
This is a continuation of U.S. patent application Ser. No. 12/698,021, filed 1 Feb. 2010, which is a continuation-in-part of my co-pending U.S. patent application Ser. No. 11/532,882, filed 18 Sep. 2006, both of which are incorporated herein by reference.
U.S. patent application Ser. No. 11/532,882, filed 18 Sep. 2006, claims priority of my U.S. Provisional Patent Application No. 60/717,639, filed 16 Sep. 2005, for “MULTI ANGLE FUNCTIONING LED BULBS AND LAMPS,” which is incorporated herein by reference. Priority of U.S. Provisional Patent Application No. 60/717,639, filed 16 Sep. 2005, is hereby claimed.
My. U.S. patent application Ser. No. 11/057,691, filed 14 Feb. 2005, issued as U.S. Pat. No. 7,566,142 on 28 Jul. 2009, for “Changing color LEDs” is incorporated herein by reference; however, this is not a continuation-in-part of that patent application.
My U.S. Provisional Patent Application No. 60/544,409, filed 13 Feb. 2004 for “Changing Color LEDs” is incorporated herein by reference.
My U.S. patent application Ser. No. 10/730,744, filed 8 Dec. 2003 for “Loaded LED Bulbs for Incandescent/Fluorescent/Neon/Xenon/Halogen Bulbs Replacement in Load Sensitive Applications and more” is incorporated herein by reference; however, this is not a continuation-in-part of that patent application.
My U.S. patent application Ser. No. 10/408,768, filed 7 Apr. 2003 for “LED Products: Flashing LED Display and Decorative LEDs for Autos and Trucks” is incorporated herein by reference; however, this is not a continuation-in-part of that patent application.
My U.S. Provisional Patent Application Ser. No. 60/431,333, filed 6 Dec. 2002, is incorporated herein by reference.
U.S. patent application Ser. No. 10/123,542, filed 16 Apr. 2002, issued as U.S. Pat. No. 6,786,625 on 7 Sep. 2004, is incorporated herein by reference; however, this is not a continuation-in-part of that patent application.
My U.S. Provisional Patent Application Ser. No. 60/370,319, filed 5 Apr. 2002, is incorporated herein by reference.
My U.S. Provisional Patent Application Ser. No. 60/346,666, filed 8 Jan. 2002, is incorporated herein by reference.
My U.S. Provisional Patent Application Ser. No. 60/345,788, filed 31 Dec. 2001, is incorporated herein by reference.
U.S. patent application Ser. No. 09/578,813, filed 24 May 2000, issued as U.S. Pat. No. 6,371,636 on 16 Apr. 2002, is incorporated herein by reference; however, this is not a continuation-in-part of that patent application.
My U.S. Provisional Patent Application Ser. No. 60/135,797, filed 24 May 1999, is incorporated herein by reference.
Incorporated herein by reference are all of my US patent applications and patents, and all published versions thereof, including:
PUB. APP. NO. Title
20110018436 Loaded LED Bulbs for Incandescent/Fluorescent/Neon/Xenon/Halogen Bulbs Replacement in Load Sensitive Applications and more 20080037262 Loaded LED bulbs for incandescent/fluorescent/neon/xenon/halogen bulbs replacement in load sensitive applications and more 20050195597 Changing color LEDS 20040085781 LED products: flashing LED display and decorative LEDs for autos and trucks 20020191416 LED light module for vehicles
PAT. NO. Title
U.S. Pat. No. 7,871,178 LED Products: Flashing LED Display and Decoratice LEDs for Autos and Trucks U.S. Pat. No. 7,566,142 Changing color LEDS U.S. Pat. No. 6,786,625 LED light module for vehicles U.S. Pat. No. 6,371,636 LED light module for vehicles.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable
REFERENCE TO A “MICROFICHE APPENDIX”
Not applicable
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to light-emitting diodes (LEDs) and more particularly to versatile LEDs for use in a variety of applications.
2. Background
Incorporated herein by reference are the following:
PUB. APP. NO. Title
20110018436 Loaded LED Bulbs for Incandescent/Fluorescent/Neon/Xenon/Halogen Bulbs Replacement in Load Sensitive Applications and more 20080037262 Loaded LED bulbs for incandescent/fluorescent/neon/xenon/halogen bulbs replacement in load sensitive applications and more 20050195597 Changing color LEDS 20040085781 LED products: flashing LED display and decorative LEDs for autos and trucks 20020191416 LED light module for vehicles
PAT. NO. Title
U.S. Pat. No. 7,871,178 LED Products: Flashing LED Display and Decoratice LEDs for Autos and Trucks U.S. Pat. No. 7,566,142 Changing color LEDS U.S. Pat. No. 6,786,625 LED light module for vehicles U.S. Pat. No. 6,371,636 LED light module for vehicles. U.S. Pat. Nos. 7,040,790; 6,563,269; 6,585,385; 5,378,931; 5,748,459; 4,115,790 and 6,784,357.
U.S. Published Patent Application Nos: 2005/0213326; 2006/0082322; 2006/0192502; and 2006/0055012.
U.S. Pat. Nos. 6,634,771; 6,621,222; 6,598,996; 6,709,132; 6,902,308; 7,059,754; 7,011,430; 7,086,756; 6,523,978; 5,806,965; and 5,561,346.
U.S. Published Patent Application Nos: 2004/0114367; 2005/0174769; 2002/1091396; and 2002/0176253.
See also www.SpiderLite.com and Publication No. US 2005/0099810 A1.
SUMMARY OF THE INVENTION
The present invention includes versatile LEDs for use in a variety of applications. The present invention includes Multi Angle Functioning Led Bulbs and Lamps.
“Single bright” as used herein means LED lamps which typically shine at a single brightness when on, while “double bright” refers to LED lamps (such as those described in my prior patents) which shine at two different brightnesses when on (such as an LED lamp functioning as a tail light and a brake light).
PCB refers to printed circuit board. LED or Led refers to light-emitting diode.
The bulbs of the present invention can be used in the applications mentioned in my prior patents and patent applications.
BRIEF DESCRIPTION OF THE DRAWINGS
For a further understanding of the nature, objects, and advantages of the present invention, reference should be had to the following detailed description, read in conjunction with the following drawings, wherein like reference numerals denote like elements.
FIG. 1 shows a preferred embodiment of the present invention, and is a Single and Dual Bright Multi-Directional Automotive LED Bulb/Lamp side view assembled X pattern bayonet bulb.
FIG. 2 shows an alternate embodiment of the present invention, and is a Single and Dual bright automotive LED bulb pcb seat;
FIG. 3 shows an alternate embodiment of the present invention, and is a Single bright Multi Directional automotive LED bulb bayonet base;
FIG. 4 shows a partial perspective view of PCBs of the present invention, with LED bulbs pointing in different directions; and,
FIG. 5 shows an alternate embodiment of the present invention, and is an automotive LED replacement for tubular bulbs.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Although specific embodiments of the present invention will now be described with reference to the drawings, it should be understood that such embodiments are by way of example only, and merely illustrative of but a small number of the many possible specific embodiments which can represent applications of the principles of the present invention. Various changes and modifications obvious to one skilled in the art to which the present invention pertains are deemed to be within the spirit, scope and contemplation of the present invention as further defined in the appended claims.
1 Multi-Directional LED Bulbs and Lamps
LED bulbs and lamps with LEDs pointing to the sides, top, bottom, and even to the back in addition to the front are desirable to light up more or different parts of the lamp and or lens or to produce more total light in many applications. Various viewing angles and configurations are used to achieve the desired light pattern and brightness. If the correct viewing angle and number of LEDs are selected and placed at the proper locations, it is possible to emit light at the same or near same viewing angle of the incandescent bulb for that application. Restrictions and customizations are achieved by changing the variables of PCBs, LEDs and positioning during the manufacturing process. One group of examples are lollipop LED bulbs with one or more PCBs where LEDs face opposite directions in various or same colors that replace incandescent bulbs in fender top mounted turn signal and running lights on freight trucks. Typically they have amber lenses on front and red on rear facing, but it is also common for red and red. The LED colors, types, brightness, viewing angles and so forth as well as positioning are preferably all determined for specific applications. A second group of examples are single or multi directional LED bulbs for cab top lights in trucks. Another example is one or more PCB radial LED bulbs used for tail lights, running lights, marker lights, and much more where light is directed both directly to lens and also directed to reflector or housing. The embodiments are virtually limitless but examples are shown using 1 PCB, 2 PCBs, 3 PCBs, 4 PCBs and 5 PCB in a variety of arrangements, using various circuitries, positioning and configurations each for use in specific or universal applications. Applications are encompassing. Examples of some applications are flashlights, trucks, trailers, motor cycles, automobiles, marine, aviation, commercial, industrial, agricultural, government, rail, and home. These bulbs are different from prior art known to the inventor (LEDtronics bulbs) because prior art bulbs are limited to 2 stacked PCBs with LEDs on one side of one PCB pointing one way, and LEDs on one side of a second PCB, pointing out radially from the center, toward the sides. Six LEDs are each spaced 60 degrees apart in a circle, lying on their sides. The two PCBs are attached using “stanchions”, preferably three, to attach the two PCB's together. In contrast, the bulbs of the present invention use no stanchions to attach only 2 PCBs together nor do the LEDs necessarily mount upright on the top of a top PCB and down flat on a second PCB in a radial configuration nor are they limited to two PCBs. All bulbs of the present invention either operate in single brightness mode, dual brightness mode, or combination, or with split LEDs (as in the prior art to U.S. Pat. No. 6,371,636) or shared single brightness LEDs (for example, brake/tail LED bulbs in which some LEDs light up for tail and all light up for brake) or integrated dual element operation (as in U.S. Pat. No. 6,371,636) if dual action.
FIG. 1 shows an automotive LED bulb comprising a base 47 , printed circuit boards 50 and 53 in an X pattern, electrically connected to the base 47 ; the printed circuit boards 50 and 53 having two sides, and LEDs 44 , 51 operatively connected to the printed circuit boards 50 and 53 and on both sides of the printed circuit boards 50 , 53 . The sides of the printed circuit board have main surfaces and one or more LEDs 51 , 44 , and 43 pointing away from one of the main surfaces and in multiple directions. Base 47 fits in a standard automobile bulb socket. Further, LED bulb has a longitudinal axis, and the PCBs 50 , 53 have faces parallel to the longitudinal axis. The PCBs 50 , 53 have a first edge between the two sides, with LEDs on the first edge pointing in a direction parallel to the main surfaces.
FIG. 2 shows an automotive LED bulb 247 comprising a base which fits in a standard automobile socket, a printed circuit board 249 electrically connected to the base, the printed circuit board having two sides, LEDs 248 , 251 operatively connected to the printed circuit board on both sides of the printed circuit board and wherein the sides of the printed circuit board have main surfaces and one or more LEDs 251 on one side of the printed circuit board are parallel to the main surfaces.
FIG. 3 shows an automotive LED bulb 267 comprising a base 271 which fits in a standard automobile socket, a printed circuit board 262 electrically connected to the base, the printed circuit board having two sides, LEDs 268 , 269 operatively connected to the printed circuit board on both sides of the printed circuit board, wherein the sides of the printed circuit board have main surfaces and one or more front LEDs 269 on one side of the printed circuit board are parallel to the main surfaces, the PCBs have faces parallel to the longitudinal axis, and wherein the printed circuit board has a first end proximal the base and a distal end, and one or more LEDs 269 points toward the distal end and one or more LEDs 269 points toward the proximal end.
FIG. 3 shows an automotive LED bulb 267 comprising a base 271 which fits in a standard automobile bulb socket, at least two printed circuit boards electrically connected to the base, LEDs 268 , 269 operatively connected to the printed circuit boards, the bulb has a first end proximal the base and a second end distal from the base, one or more LEDs pointing to front point toward the second end, one or more LEDs 269 pointing to rear point toward the first end. Further, the bulb has a side between the first and second ends, and one or more LEDs 269 pointing to the side, LEDs 269 , 268 pointing in opposite directions and all around to sides and back, and LEDs 269 on one side of each PCB pointing in opposite directions.
FIG. 4 is a partial perspective view of PCBs 284 with LED bulbs 285 pointing in different directions.
FIG. 5 shows an automotive LED replacement automotive light bulb 290 for tubular bulbs, the replacement bulb having metal contacts 292 , 293 on both ends and LEDs 291 pointing in different directions.
The automotive LED replacement automotive light bulbs of the present invention preferably include a base which fits in a standard automobile bulb socket for one of the following standard automobile bulbs: 1156, 1157, 3156, 3157, 7440, 7443, 1895, 194, 5MM wedge base bulb.
Commercial embodiments of the present invention are sold by Jam Strait under model nos. 1156-HRR; 1156-HAR; 1156-HWR; 1156-HRWR; 1157-HRR; 1157-HAR; 1157-HWR; 1157-HRWR; 3157-HRR; 3157-HAR; 3157-HWR; 3157-HRWR; 7440-HRR; 7440-HAR; 7440-HWR; 7440-HRWR; 7443-HRR; 7443-HAR; 7443-HWR; 7443-HRWR; 1895-HRR; 1895-HAR; 1895-HWR; 1895-HRWR; 194-HRR; 194-HAR; 194-HWR; 194-HRWR; LDL-HRR; LDL-HAR; LDL-HWR; LDL-HRWR; 5MM-HRR; 5MM-HAR; 5MM-HWR; 5MM-HRWR; KC1; and KC2.
More information about LEDs and LED products can be found at www.jamstrait.com.
FIG. in
which it
Part No.
Description
first appears
43
LED bulb
1
44
Square LED bulb
1
46
Housing
1
47
Bayonet base
1
48
Contacts
1
49
Index pin
1
50
PCB
1
51
Square LED bulb
1
53
PCB
1
54
Insulator
1
247
Single and Dual bright LED bulb PCB seat
2
248
LED bulb
2
249
PCB
2
250
PCB
2
251
LED bulb
2
252
Connector
2
253
Optional rear LEDs
2
254
Closeup of FIG. 35
2
262
Circuit board
3
267
Single bright Multi Directional LED bulb bayonet base
3
268
LED bulb
3
269
LED bulb
3
270
index pin
3
271
Bayonet base
3
272
Contact
3
273
Bottom end
3
290
Multi Angle single pcb dome light LED bulb
5
291
LED bulb
5
292
contact
5
293
contact
5
294
Optional clear or colored tube/cover
5
297
Multi Angle Multi PCB dome light PCBs
4
All measurements disclosed herein are at standard temperature and pressure, at sea level on Earth, unless indicated otherwise.
The foregoing embodiments are presented by way of example only; the scope of the present invention is to be limited only by the following claims.
|
Automotive bulbs and including at least one printed circuit board electrically connected to a standard automotive bulb base, and a plurality of light emitting diodes (LEDs) arranged on the circuit board to project light in at least two opposite directions. In some embodiments, circuit boards are arranged in an X pattern, and the LEDs are arranged to project light in substantially all directions about the longitudinal axis of the automotive bulb.
| 5
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BACKGROUND OF THE INVENTION
This invention is directed generally to liquid separation within liquid containers such as underground wells and, more particularly, to a method and apparatus for removing substantially immiscible liquids, such as hydrocarbons or pollutants from a collecting well which contains both water and such immiscible liquids.
There are various known techniques for removing immiscible liquids (hereinafter generally referred to as "liquids" or "liquid product") from containment apparatus. One such method is to employ a "cone of depression" technique. As stated in U.S. Pat. No. 4,746,423, the use of a "cone of depression" for collecting hydrocarbons from an underground well containing an overlying immiscible liquid, usually a hydro-carbon product, from an underlying, conductive, heavier liquid in a two liquid body is well established. The technique requires a depression pump located at or near the bottom of a well to remove water in large enough quantities to actually lower the water table locally, and thereby cause underground liquids to drain toward the region in which the table is depressed. The lighter liquid products then collect within the well along with the water and typically as the water is pumped out by the depression pump, a skim pump located higher in the well, in the region atop the collected water where the lighter fluid products collect, is used to pump out the contaminants. Several examples of this technique and other removal schemes may be found in the patents listed below.
U.S. Pat. No. 4,273,650 to Solomon teaches a system using a cone of depression technique which employs a submergible, drawn down, electrically powered pump submerged at the bottom of a well. A water discharge control including the pump and the pump switch controls the flow of water from the well to establish and maintain by gravity flow a predetermined liquid level at a spaced distance below the static water table. In this way, a cone of depression is established. A combined pollutant pump and sensor apparatus including an electrically powered pollutant pump, a pump switch and sensors responsive to pollutant level to actuate the pump switch are supported in the well at the level of the apex of the cone of depression. The Solomon apparatus also includes sensors for sensing a low level water/pollutant interface and energizing the pollutant pump to pump pollutant into a tank while permitting the water/pollution interface to rise and also for sensing a high level water/pollutant interface and de-energizing the pollutant pump upon sensing the high level water/pollutant interface.
U.S. Pat. No. 4,469,170 to Farmer, Jr. teaches a skimmer which is designed to float in the two-liquid body contained in the well. The Farmer, Jr. skimming apparatus requires a float and, apparently, also requires a depression pump.
U.S. Pat. No. 4,746,423 to Moyer discloses a two pump skimmer system for recovery of lighter-than-water hydrocarbons from water wells. The pumps are located in individual chambers which are interconnected with the water chamber below the hydrocarbon chamber and with limited one-way flow into the water chamber. Both pumps are independently controlled by sensors in the upper chamber to assure that each pumps only the proper liquid.
U.S. Pat. No. 4,766,957 to McIntyre discloses a method and apparatus for gravitationally separating hydrocarbons and water discharged from a subterranean well. McIntyre teaches that a mixture of hydrocarbons and water flows into the interior of a well casing through perforations disposed adjacent the production zone. The water flows downwardly or is forcibly pumped downwardly to the water absorbing formation and is absorbed in such formation.
U.S. Pat. No. 4,770,243 to Fouillout, et al. shows a microprocessor controlled system for separating water from hydrocarbons. The Fouillout device is directed to the field of the production of petroleum from deposits in which water is mixed with hydrocarbons, and not to the skimming of contaminant hydrocarbons from a water producing well. Separation of the water from the hydrocarbons is accomplished at the bottom of the well in a packer.
U.S. Pat. No. 4,761,225 to Breslin discloses an apparatus for controlling the removal of liquid hydrocarbons from groundwater in a perforated well casing consisting of a plurality of pump chambers and a control system which is powered by compressed air.
The present invention has advantages over the prior art in that, it is believed that for the first time, it provides a highly dynamic, automatic microprocessor-controlled system which has a programmable operation capable of using a single sensor in combination with a float sensor to control both a skim pump and a depression pump, thereby promoting cooperation between the two pumps to result in hydrocarbon removal. The invention provides a microprocessor based controller for a "cone of depression" type removal system which heretofore has not been found in the prior art. In yet another aspect of the invention, a method and apparatus is provided to remove floating liquids using only an interface sensor and a microprocessor controlled skim pump, without employing a depression pump to create a cone of depression.
SUMMARY OF THE INVENTION
The present invention provides a method and apparatus for removing floating, substantially immiscible liquids such as hydrocarbons from containers or wells containing both liquids and water. In one aspect of the invention, a microprocessor control receives and processes input signals from a liquid sensor, an upper water interface sensor and a skim pump. The skim pump is located in the well proximate to the water interface. The liquid sensor is located proximate to the skim pump. The upper water interface sensor is located adjacent to and below the liquid sensor. The microprocessor control is initialized by setting certain parameters such as the initial conditions for pump output values. The microprocessor controls and operates the skim pump in response to the input signals.
In a further aspect of the invention, a depression pump is also included. The depression pump is located in the well below the skim pump. In one embodiment of the invention, the skim pump is not activated if the depression pump is running. If the depression pump is not running and liquids are sensed by the liquid sensor at the skim pump, the skim pump is activated. In appropriate applications, the skim pump may be operated so as to be inhibited at all times when the depression pump is operating. In other applications, the skim pump and depression pump may operate simultaneously. Collected water is discharged to a designated site outside of the well by the depression pump. The skim pump pumps liquid products into a product tank located outside of the well. The product tank also provides an input signal to the microprocessor control from a high tank level sensor which provides an indication as to the fluid level in the tank. The microprocessor control processes this signal in order to stop the skim pump in the event that the product tank is filled.
In a yet further aspect of the invention, status displays in the form of lights and electronic readouts are provided as well as external problem or troubleshooting outputs. Other optional features may be added, such as a lower water interface sensor, which also provides input signal data to the microprocessor control.
It is one object of the invention to provide a microprocessor controlled apparatus for removing hydrocarbons from wells containing both hydrocarbons and water.
It is yet another object of the invention to provide a unitary controller which controls both a skim pump and a depression pump using input signals from a single water interface sensor for controlling and coordinating operation of both pumps.
It is a further object of the invention to provide a hydrocarbon removal apparatus which operates so as to prevent water from being pumped through the skim pump.
It is still a further object of the invention to provide an apparatus for creating a cone of depression removal system which uses signals from a lower water interface sensor to inhibit the depression pump from pumping liquid product.
Other objects, features and advantages of the invention will become apparent to those skilled in the art through the description of the preferred embodiment, claims and drawings herein wherein like numerals designate like elements.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of one embodiment of the apparatus of the invention.
FIG. 2 is a block diagram of an alternate embodiment of the apparatus of the invention.
FIG. 3 is a high level flow chart illustrating generally the method of the invention.
FIG. 4 is a detailed flow chart of the control scheme of a depression pump as employed by one embodiment of the invention.
FIG. 5 is a detailed flow chart of the control scheme of a skim pump as employed by one embodiment of the invention.
FIG. 6 is a block diagram of a further alternative embodiment of the invention employing a modulating valve for regulating water discharge from the depression pump.
FIG. 7 is a flow chart of a method of optimizing liquid product removal as provided by the invention.
FIG. 8 illustrates an example of a control panel employed by one embodiment of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1, a block diagram of one embodiment of the invention is shown schematically. The liquid product removal apparatus of the invention 10 for a cone of depression scheme comprises a microprocessor control 12, skim pump 14, liquid sensor 22, upper water interface sensor 23, depression pump 16, skim pump power contactor 30, depression pump power contactor 32, skim pump time delay switch 34, and depression pump time delay switch 36. In another aspect, the invention provides an apparatus and method for removal of floating liquids which may be used in a system not requiring a cone of depression technique. In such a system, the basic apparatus needed for hydrocarbon removal is microprocessor control 12, skim pump 14 and liquid sensor 22. In such a system, as long as liquid sensor 22 provided a signal indicating the presence of floating liquid products, the skim pump would be activated by the microprocessor control unit to pump out the liquids. The skim pump time delay switch 34 may still be utilized to prevent short cycling of the skim pump.
The microprocessor control may advantageously be any suitable microprocessor device such as an 8 bit microprocessor or similar device. In one embodiment of the invention, an INTEL model 8751 8-bit microprocessor is employed. The microprocessor and associated elements including the contactors and switches are preferably located in a control enclosure or housing 5. Those skilled in the art will appreciate the fact that any number of similar programmable devices, computers or equivalent circuits may also be employed to provide the microprocessor control function. The microprocessor executes a control algorithm according to the invention as described herein. The invention will first be described in terms of its functional elements, followed by a description of the operation of the invention.
The skim pump time delay switch 34 may be used to set a first time delay used in operating the skim pump. Similarly, the depression switch 36 may also be set manually or automatically in order to set a second time delay used in the operation of the depression pump. Both timers 35 and 37 are advantageously implemented in the software control algorithm executed by the microprocessor control. The settings of the switches 34 and 36 are read into the microprocessor control 12 during a program logic cycle. The switches 34 and 36 may be, for example, DIP switches or equivalent devices. These parameters may also be provided in various ways such as by a digital device compatible with the microprocessor, such as a read only memory (ROM).
A first control output 50 of the microprocessor is connected to the depression power contactor 32. The depression power contactor operates in response to the output 50 in order to activate or deactivate the depression pump 16 through line 52. Similarly, a second microprocessor control output 54 is provided to skim pump power contactor 30 which activates or deactivates the skim pump 14 through line 56. Depression pump 16 may be any suitable depression pump as is commercially available and well-known by those skilled in the art. Similarly, skim pump 14 may be any suitable, commercially available skim pump for pumping hydrocarbons. Both skim pump 14 and depression pump 16 are supported by well-known means in well 40. The skim pump 14 is advantageously placed at a position in the well which is proximate to the water interface. Depression pump 16 is located below skim pump 14 nearer to the bottom of the well where it is totally submerged in water and does not come into contact with hydrocarbon fluid product.
Liquid sensor 22 and upper water interface sensor 23 may advantageously be housed together in upper probe 21. Liquid sensor 22 senses the presence of liquids. The liquid sensor may advantageously be a float switch. Other types of sensors could be used including sensors responsive to capacitance, optical refraction or thermal conductivity. Such devices are well-known in the art. The liquid sensor 22 provides a sensing signal transmitted on line 60 to a first input of the microprocessor control. Upper water interface sensor 23 is located adjacent to liquid sensor 22 and provides a water interface sensing signal on line 62 to a second input of the microprocessor control. An optional lower water interface sensor 24 of the same type as the upper water interface sensor may be included. If used, the lower water interface sensor 24 is preferably disposed between the skim pump and the depression pump intakes. Lower water interface sensor 24 also provides a sensing signal to a third input of the microprocessor control on line 64. The upper and lower water interface sensors may preferably be well-known conductivity sensors or equivalent devices. Other devices which may be used include float sensors which are buoyant in water, but not in hydrocarbon products.
The depression pump 16 discharges water through conduit 66 to an appropriate discharge location 17. The skim pump 14 discharges hydrocarbon product into product tank 18 through conduit 68. The product tank 18 includes a high tank level sensor 20 which senses the tank level. A tank level sensing signal is presented by the high tank level sensor to a fourth input of the microprocessor control through line 70.
Referring now to FIG. 2, an alternate embodiment of the apparatus which comprises the invention is shown. In the embodiment shown in FIG. 2, optional features have been added to the system shown in FIG. 1. These additional features include a communications bus 80, status display 82, external problem indicators 84, option select switches 86, and current sensors 90 and 92.
The communications bus 80 may comprise any communication lines suitable for interfacing the microprocessor control with an external computer, such as a personal computer or main frame computer. Utilizing such a communications bus, an operator can easily monitor the well operation or modify a program in the microprocessor control to accommodate local special conditions. Optional select switches 86 may be provided for programming optional features such as engaging or ignoring the lower water interface sensor. Current sensor 90 provides a current sensing signal corresponding to the driving current in the skim pump referenced to a predetermined set point. If the current exceeds the predetermined set point, the microprocessor control processes the signal as indicating that the skim pump is pumping. Similarly, current sensor 92 measures the depression pump current and provides a signal on line 96 which corresponds to a measurement of whether or not the current in the depression pump exceeds a predetermined set point indicating that the depression pump is pumping. The signals from the optional current sensors may be used for monitoring operation of the well and are not employed in the preferred embodiment to effect the operation of the control system. Other optional features may be included to assure proper set up at a given well location. For example, jumpers may be supplied in the interface connectors (not shown) for the liquid sensor, upper water interface sensor, lower water interface sensor, and high tank level sensor to supply a continuity signal to the microprocessor controller when each of these devices is properly plugged into the control enclosure.
Status display 82 may include a digital display to show the operating time of current operation which may, advantageously, optionally alternate with a display elapsed time from previous operations. Status lights may also be included in the display for indicating current conditions of sensors and the controller cycle. Some of the status displays may advantageously be driven directly by the input lines to the microprocessor control instead of being driven by the microprocessor. A watch dog timer 110 may also be included to provide a reset signal to the microprocessor control in the event of a processor malfunction such as the program counter jumping to execute a non-program, a memory overflow, endless loop condition, etc. This reset signal is supplied by lines 112. When the microprocessor is properly executing its program, it will periodically reset the watch dog timer.
OPERATION OF THE INVENTION
Having described the elements of the invention and their relationship to each other, it is believed that the features and advantages of the invention can be better appreciated through a detailed description of the operation and method of the invention as provided herein below.
Referring now to FIG. 3, a high level flow chart illustrating generallY the method of the invention is shown. Those skilled in the art will appreciate that the precise order of events shown in FIG. 3 is not critical to the operation of the invention, but that many alternative configurations are possible to implement the principles of the invention. However, for the sake of illustrating the invention, the flow chart used in FIG. 3 will be used with the understanding that it is intended for illustration of the invention and not by way of limitation of the invention. At step 200, the system is turned on (or reset, as by the watchdog timer, depending upon the condition in which the process is being entered). The process then proceeds to step 210 wherein the microprocessor and variables, including initial values of outputs, flags and counters are set up and initialized.
At step 212, the microprocessor internal real time clock is updated from a an internal microprocessor timer and the microprocessor oscillator. Next, at step 214 the microprocessor control reads and processes the various inputs as provided from the liquid sensor, upper water interface sensor, lower water interface sensor, high tank level sensor, and other external lines. After step 214, the microprocessor control proceeds to cycle through the depression pump logic at step 216 which is explained in more detail hereinbelow with reference to FIG. 4. Upon exiting the depression pump logic sequence at 216, the skim pump logic sequence is entered at step 218. The skim pump logic sequence is explained in more detail with reference to FIG. 5 herein. Upon completing the skim pump logic cycle at step 218, the processor optionally executes step 220 wherein outputs are provided to the display panel and problem indication devices 84. The microprocessor control continues to cycle through steps 212 through 220 until the system is turned off or reset.
Referring now to FIG. 4, a more detailed flow chart of the control scheme of the depression pump as employed by one embodiment of the invention is shown. If the option select switches 86 are set to utilize the low water interface sensor, optional step 222 will be included in the computer algorithm being executed by the microprocessor. Otherwise the depression pump control scheme will begin at step 224. Assuming that the low water interface sensor option is selected, block 222 utilizes the input on line 64 in order to determine whether or not a low water interface is being sensed by the low water interface sensor 24. If the low water interface sensor is on, indicating that the water interface is at or above the low water sensor, the process flow continues to step 224. If the low water sensor is off, indicating that the water interface is below the low water sensor, the low water sensor output signal on line 64 will carry a corresponding electrical signal to the microprocessor control allowing the computer algorithm to proceed to step 232. At step 224, the microprocessor checks the timer for the depression pump cycle. If the timer has been set to zero, indicating the depression pump is currently off, the process proceeds to step 226. If the timer holds a value other than 0 the timer is incremented at step 228 and control then proceeds to step 230. Assuming the branch to step 230 is followed, the internal depression time is compared to the time delay set by depression pump switch 36 at step 230. If the timer is over the limit, control proceeds to step 232. At step 232, the timer is set equal to 0 which indicates that the pump has been turned off. Note that step 232 may also be entered from optional step 222 if the low water interface sensor is in the "off" condition. Step 232 is exited and control proceeds to step 234 wherein the depression pump is turned off by the microprocessor control operating through the depression pump contactor 32.
Assuming that the "yes" branch from step 224 is executed, the processor then executes step 226 wherein the signal from the upper water interface sensor is read and processed by the microprocessor control to determine whether or not the water interface is at or above the high water sensor. If the signal from the upper water interface sensor 23 on line 60 indicates an "on" condition, this indicates that the water interface is at or above the upper water interface sensor and the process proceeds to step 236 wherein the timer is incremented and started. If the upper water interface sensor proVides a signal on line 60 indicating an "off" condition, that is, indicating that the water interface is below the upper water level sensor, the process branches to step 234, wherein the depression pump is kept off by the microprocessor control supplying an appropriate control signal to the depression pump power contactor 32. Step 240 is entered either via step 236 or the "no" branch of step 230. At step 240, the microprocessor control supplies an appropriate signal to the depression pump power contactor via lines 50 to turn the depression pump on. Following the above described control process, the depression pump will always run if the upper water sensor indicates that the water interface level is at or above the level of the upper water sensor. Further, the depression pump will run until the time delay as set by the depression pump switch 36 has elapsed. If the lower water interface sensor is used, it will override the time delay and assure that the depression pump does not run when the water interface is below the lower water interface sensor level.
Referring now to FIG. 5, a flow chart showing the control scheme for the skim pump is shown. Decision step 242 is entered when step 216 has been completed. At step 242, the microprocessor control determines whether the skim pump is currently running. If the skim pump stops, the processor determines whether the depression pump has run since the skim pump stopped. This step is not essential to the operation of the skim pump but is useful in preventing short cycling of the skim pump. If the skim pump is running or the depression pump has run since the skim pump stopped running, the process proceeds to step 244 which determines whether or not the depression pump is off.
In an alternate embodiment of the invention wherein the optional step 244 is eliminated from the logic flow shown in FIG. 5, the depression pump and the skim pump may operate concurrently. In such an alternate embodiment, step 242 would be replaced by an alternate step 242 to determine the status of the upper water interface sensor. If the upper water interface sensor was on for a few seconds, control would proceed to step 262. If the upper water interface sensor was off, control would proceed to step 246.
Assuming step 244 is executed and the depression pump is not running, control then proceeds to decision block 246 wherein the microprocessor determines from the signal on line 60 whether or not the liquid sensor 22 is on. If the liquid sensor is on, it indicates the presence of hydrocarbon product. The liquid sensor may be, for example, a float switch. If the liquid sensor is on, process flow continues to step 248. At step 248, the signal on status line 70 is processed by the microprocessor control to determine whether or not the product tank 18 is full as indicated by the high tank level sensor 20. If the tank is not full, process flow continues to step 250 wherein the skim pump's current status is checked by the microprocessor control. If the skim pump is not running, the skim pump hold-off timer is checked at step 252. If the skim pump timer is set to 0, the timer is incremented at step 264 starting the timing process, and the skim pump is kept off at step 266 prior to exiting the control algorithm. If the skim pump timer is not equal to 0, the skim pump hold-off timer is incremented at step 254. At step 256, the skim pump hold-off timer is compared against the time limit as set by skim pump time delay switch 34. If the hold-off timer is over the limit, the timer is set to 0 and the skim pump is turned on. If the timer is under the limit, the skim pump is kept off at step 266 prior to exiting the routine. If any of the conditions at steps 242, 244, and 246 are determined to be negative, the skim pump hold timer is set to 0 at step 262 and the skim pump is turned off. If the product tank is full as determined at 248, the process also flows through steps 262 and 266 and then exits. Using the above control algorithm, the skim pump timer will not be activated during a predetermined time delay period which is initiated by the liquid sensor turning on. Further, the skim pump will not operate when the depression pump is running.
Referring now to FIG. 6, a block diagram of yet a further alternate embodiment of the invention is shown. The difference between the embodiment shown in FIG. 6 and the embodiment shown in FIG. 1 is substantiallY in the introduction of modulating valve 400 and optional solenoid valve 402 which controls the water discharge from the depression pump. Only those elements significant to this alternate embodiment are shown and it will be understood that other elements as depicted in FIG. 1 may be used in combination with the system shown in FIG. 6 as necessary. In the scheme shown in FIG. 6, the depression pump is controlled only by the low water sensor and the water line 66 is controlled at the surface by a modulating control valve or motor controlled throttling valve 400. The valve 400 slowly opens when water is sensed at the upper water sensor 23 and slowly closes when water falls below the upper water sensor. The rate of opening and closing the valve may advantageously be set so as to control the water interface 58 at a substantially static level. The speed of opening and closing the modulating valve may be optimized using an algorithm executed by the microprocessor based on historical experience in the well being pumped. Optionally, a solenoid valve 402 may advantageously be added across the modulating valve. When using the solenoid valve, when the power is first turned on, the solenoid valve opens and the modulating valve does not move until the water interface falls below the upper water sensor. At that point, the solenoid valve may be inactivated and the modulating valve is used for the duration for the operation of the pump 16.
Referring now to FIG. 7, a flow chart of another feature of the method of the invention is shown. As detailed in FIG. 7, the invention provides a computer algorithm executed by the microprocessor control for optimizing and dynamically changing the on-off cycle for the depression pump based upon prior experience data for a holding container, such as a well. At step 400, a series of initial recovery times for the water interface 58 are measured and stored in memory. The recovery time is defined as the time it takes for the water interface to return to the skim pump level as measured from the time the depression pump is turned off. The control then executes step 402 for calculating the optimum pump-on time initially based upon the measured initial recovery times found at step 400 and the optimum total cycle time for the depression pump as supplied by the manufacturer or as determined by the operator. Subsequent cycles through the algorithm will incorporate measurements of currently measured recovery times. The optimum pump-on time will usually be set to avoid short cycling of the skim pump. A tYpical total pump-on plus recovery time is about 15 minutes. The optimum pump-on time will vary from well to well. Once the optimum pump-on time has been calculated, the microprocessor adjusts the depression pump cycle time at step 404. At step 408 the current recovery time is monitored. The cycle then returns to step 402 and repeats while continuing to add to and use the historical data being accumulated for the well which includes the initial and current recovery times and the depression pump optimum total cycle time.
FIG. 8 shows an example of a control panel provided by one embodiment of the invention. The control panel 300 is used to interface with operators running the system. The panel 300 comprises a printed circuit board 302 upon which are mounted switches 34 and 36, numerical display indicators 301 and front panel 303. Front panel 303 is divided into a plurality of segments including a SENSOR segment comprising indicators 310, 312 and 314, a first SKIM PUMP segment comprising indicators 316 and 318, a second SKIM PUMP segment comprising indicators 336, 338 and switch 339, a DEPRESSION PUMP segment comprising indicators 332 and 334 and switch 335, and a PROBLEM SEGMENT including indicators 322, 324, 326, and 328 and switch 330.
The front panel 303 is positioned on the printed circuit board so as to align the DEPRESSION HOLD-ON nomenclature over depression switch 36 and the SKIM HOLD-OFF nomenclature over depression switch 34. Similarly, the nomenclature designating ERROR and ELAPSED CYCLE TIME is positioned under display indicators 301. Indicators 301 may comprise a plurality of seven segment numerical display devices or similar read-out devices. In one embodiment of the invention, two elements are used to display error indications and four elements are used to display elapsed time for the current and previous operating cycles. Indicators 304, 306 and 308 indicate the presence or absence of power to the system. In the SENSORS segment of the display, indicator 310 is designated as FLOAT, indicator 312 is designated HIGH WATER and indicator 314 is designated LOW WATER. When the indicators are lit, it is a signal to the operator that the named device or function is in the "on" condition or that the function named is "true".
A typical device will be provided with both audio and visual alarms, therefore, in the PROBLEM segment of the control panel, the operator may turn off the audio alarm by positioning switch 330 in the SILENCE mode. As can be seen in FIG. 8, problem indication lights 322, 324, 326 and 328 are provided. Similarly, indicator lights are provided to indicate microprocessor control and running of the skim pump by lights 336 and 338 and depression pump by lights 332 and 334. Also, the operator may override automatic control of either the skim pump or the depression pump through utilizing switches 339 and 335, respectively.
This invention has been described herein in considerable detail in order to comply with the Patent Statutes and to provide those skilled in the art with the information needed to apply the novel principles and to construct and use such specialized components as are required. However, it is to be understood that the invention can be carried out by specifically different equipment and devices, and that various modifications, both as to the equipment details and operating procedures, can be accomplished without departing from the scope of the invention itself.
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The present invention provides a method and apparatus for removing floating, substantially immiscible liquids such as hydrocarbons from containers or wells containing both floating liquids and water. In one aspect of the invention, a microprocessor control receives and processes input signals from a liquid sensor, an upper water interface sensor and a skim pump. The skim pump is located in the well proximate to the water interface. The liquid sensor is located proximate to the skim pump. The upper water interface sensor is located adjacent to and below the liquid sensor. The microprocessor control is initialized by setting certain parameters such as the initial conditions for pump output values. The microprocessor controls and operates the skim pump in response to the input signals so as to operate the skim pump in a manner responsive to the input signals.
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BACKGROUND
[0001] In many wellbore applications, sand laden fluids are filtered to return a clean fluid to the surface or to dehydrate a slurry at a desired location in a wellbore. The filtering is performed by a filtering media created from a wire wrapped or wire mesh structure. This type of filtering media is susceptible to plugging over a period time which can cause premature job failure.
[0002] Attempts have been made to reduce plugging by using powered tools associated with the filtering media. For example, screens have been designed with rotatable sleeves to help reduce plugging. Other screens utilize movable components that can be actuated to close off the screen during certain operations. However, such devices have limited effectiveness. Additionally, these devices tend to be complex, expensive devices requiring a power source for operation.
SUMMARY
[0003] In general, the present invention provides a system and method of filtering in a wellbore during various well related operations. A well screen is combined with a tool string for movement downhole into a wellbore. The well screen may be flexed via pressure differentials created across the well screen. For example, pressure inputs create pressure differentials able to flex the well screen between a normal mode and one or more deflection modes. Examples of deflection modes comprise a radially inward deflection mode and/or a radially outward deflection mode. Once the actuating pressure differential is diminished, the well screen automatically returns to the normal mode. The flexing of the well screen is used for adjusting flow gap size and for removing accumulated materials to unplug the well screen for continued use, thereby avoiding premature job failure.
BRIEF DESCRIPTION OF THE DRAWINGS
[0004] Certain embodiments of the invention will hereafter be described with reference to the accompanying drawings, wherein like reference numerals denote like elements, and:
[0005] FIG. 1 is a front elevation view of a wellbore assembly disposed in a wellbore, according to an embodiment of the present invention;
[0006] FIG. 2 is an isometric view of a well screen, according to an embodiment of the present invention;
[0007] FIG. 3 is a side view of the well screen illustrated in FIG. 2 , according to an embodiment of the present invention;
[0008] FIG. 4 is a cross-sectional view of a well screen mounted on a support structure, according to an embodiment of the present invention;
[0009] FIG. 5 illustrates an enlarged portion of the embodiment illustrated in FIG. 4 ;
[0010] FIG. 6 is a schematic illustration of a well screen in a normal deflection mode, according to an embodiment of the present invention;
[0011] FIG. 7 is a schematic illustration of a well screen in a radially inward deflection mode, according to an embodiment of the present invention;
[0012] FIG. 8 is a schematic illustration of a well screen in a radially outward deflection mode, according to an embodiment of the present invention; and
[0013] FIG. 9 is a flowchart illustrating utilization of a compliant well screen, according to an embodiment of the present invention.
DETAILED DESCRIPTION
[0014] In the following description, numerous details are set forth to provide an understanding of the present invention. However, it will be understood by those of ordinary skill in the art that the present invention may be practiced without these details and that numerous variations or modifications from the described embodiments may be possible.
[0015] The present invention generally relates to a system and methodology for filtering particulates from a fluid stream at a location within a wellbore. A compliant well screen is moved downhole into a wellbore for use in one or more well related operations. The well screen is compliant and cooperates with the overall system in a manner that enables removal of or prevention of plugging along the well screen. The well screen also can be used to facilitate downhole operations, such as the dehydration of a slurry in the wellbore. The compliant well screen is flexed between different modes of deflection via differential pressures across the well screen. For example, the pressure inputs resulting from the differential pressures across the well screen can be used to flex the well screen between a normal or intermediate mode and, for example, a radially inward mode of deflection or a radially outward mode of deflection.
[0016] Referring generally to FIG. 1 , a system 20 is illustrated according to an embodiment of the present invention. In the particular embodiment illustrated, system 20 comprises a wellbore assembly 22 disposed in a well 24 that comprises a wellbore 26 drilled into a formation 28 . Formation 28 may hold desirable production fluids, such as oil. Wellbore assembly 22 extends downwardly into wellbore 26 from, for example, a wellhead 30 that may be positioned along a surface 32 , such as the surface of the earth or a seabed floor. The wellbore 26 may comprise open hole sections, e.g. open hole section 34 , cased sections lined by a casing 36 , or a combination of cased sections and open hole sections. Additionally, wellbore 26 may be formed as a vertical wellbore or a deviated, e.g. horizontal, wellbore. In the embodiment illustrated in FIG. 1 , wellbore 26 comprises a vertical section 38 and a deviated section 40 which is illustrated as generally horizontal. One or more packers 42 also may be used with or included as part of wellbore assembly 22 to seal off desired sections of wellbore 26 .
[0017] In the example illustrated, wellbore assembly 22 further comprises a well screen 44 that is carried downhole into wellbore 26 on a tool string 46 . Well screen 44 is a compliant well screen that may be moved between a plurality of deflection modes via pressure differentials created between an exterior region 48 surrounding well screen 44 and an interior region 50 within well screen 44 and tool string 46 . Tool string 46 may be formed in a variety of configurations and with a variety of components depending on the specific well application for which it is designed. In some operations, for example, tool string 46 comprises a bottom hole assembly 52 coupled to a tubing 54 . However, other components and component arrangements can be used with well screen 44 to facilitate a variety of well related operations.
[0018] One embodiment of well screen 44 is illustrated in FIG. 2 . In this embodiment, well screen 44 is generally tubular in shape and able to undergo deflections away from a normal mode, such deflections being radially inward and/or radially outward deflections depending on the pressure inputs applied to the well screen. The illustrated well screen 44 comprises a first well screen end 56 and a second well screen end 58 . Well screen ends 56 and 58 are substantially rigid in the sense that the ends do not flex outwardly or inwardly when pressure differentials are applied between exterior region 48 and interior region 50 . Extending between well screen ends 56 and 58 are a plurality of elongate members 60 separated by slots 62 . The elongate members 60 extend in a longitudinal direction generally aligned with the axis of well screen 44 .
[0019] The slots 62 provide gaps for fluid flow across well screen 44 from exterior region 48 to interior region 50 or from interior region 50 to exterior region 48 . The gap size of slots 62 controls the size of particulars that are filtered from the flow of fluid. However, this gap size is adjusted as the compliant well screen 44 is transitioned between different deflection modes via flexing of elongate members 60 in, for example, a radially inward direction or a radially outward direction between screen ends 56 and 58 .
[0020] As further illustrated in FIG. 3 , elongate members 60 may be formed as beams that extend in a generally linear and parallel arrangement between well screen ends 56 and 58 . Each elongate member or beam 60 has linear ends 64 , 66 affixed to well screen ends 56 , 58 , respectively. Thus, the linear ends 64 , 66 of elongate members 60 are substantially fixed with respect to movement in a radial direction. However, the portion of elongate members 60 between ends 64 , 66 can be flexed in a radially inward or a radially outward direction to change the gap size of slots 62 . In the embodiment illustrated the design of elongate members 60 and slots 62 ensures the gap size is never reduced to zero. In other words, at least some fluid flow is allowed across well screen 44 between interior region 50 and exterior region 48 even when the well screen 44 is transitioned to a maximum deflection. It should also be noted that the amount of deflection, the pressure differential required to cause deflection, and the shape or pattern of deflection can be controlled by changing the length or cross-section of elongate members 60 . Additionally, these compliancy characteristics also can be controlled by selecting the appropriate material composition of elongate members 60 for a given application. For example, a variety of steels, other metals, phenolics, composites and non-metallic materials can be used in the construction of well screen 44 .
[0021] Well system 20 also may comprise a support structure 68 positioned to limit deflection of compliant well screen 44 . One example of support structure 68 is illustrated in FIG. 4 . In this embodiment, support structure 68 is positioned along an interior of well screen 44 to limit deflection of well screen 44 in a radially inward direction. However, alternate or additional support structures also can be located along an exterior of well screen 44 to limit deflection of well screen 44 in a radially outward direction. Additionally, support structure 68 may have a variety of other configurations that enable the limiting of well screen deflection.
[0022] In the specific example illustrated, support structure 68 comprises a tubular member having a plurality of radial openings 70 to accommodate fluid flow between exterior region 48 and interior region 50 . Support structure 68 further comprises standard connection ends 72 and 74 that allow support structure 68 to be coupled to tool string 46 . By way of example, standard connection ends 72 and 74 may comprise threaded connection ends or flange-style connection ends. Support structure 68 also comprises a tubular midsection 76 sized to fit within compliant well screen 44 so as to limit the radially inward deflection of well screen 44 .
[0023] As best illustrated in FIG. 5 , support structure 68 may further comprise a plurality of support elements 78 positioned to block radially inward movement of well screen 44 at a predetermined limit. For example, support elements 78 may be sized to insure the maximum deflection of well screen 44 remains within the elastic limits of the elongate members 60 . The maximum deflection within the elastic regime of elongate members 60 is a function of material choice as well as length of elongate members 60 .
[0024] In the embodiment illustrated, support elements 78 are mounted to tubular midsection 76 and are interchangeable to enable adjustment of the maximum deflection limitation. By way of example, each support element 78 may comprise a cap 80 of predetermined thickness. The cap 80 is mounted to tubular midsection 76 by a fastener 82 , such as a threaded fastener received in a threaded opening 84 formed in tubular midsection 76 of support structure 68 . Accordingly, the maximum deflection limitation can be changed by unthreading each threaded fastener 82 , removing each corresponding cap 80 , and reattaching the same or different threaded fasteners 82 with alternate caps 80 of a different thickness.
[0025] In some embodiments, the compliant well screen 44 can deflect in both an expanding mode and a collapsing mode to remove accumulation and prevent plugging of well screen 44 . The ability to deflect well screen 44 also facilitates a variety of well operations, such as dehydration of slurry in the wellbore during, for example, a gravel packing operation. The prevention of plugging is accomplished without employing any powered control mechanism downhole. Instead, elongate members 60 of well screen 44 are flexed upon application of sufficient pressure inputs created by internal and/or external pressure differentials formed along the well screen 44 . The application of pressure differentials also alters slots 62 which, in turn, changes the gap size through which fluid flows through well screen 44 . Pressure differentials may be generated by, for example, flow, mechanical crushing or drag resulting from movement of the bottom hole assembly 52 , mechanical radial force from a tool having a sliding sleeve, or other mechanisms or procedures for developing pressure differentials.
[0026] Until the pressure differential between exterior region 48 and interior region 50 is sufficiently great, elongate members 60 remain in an intermediate or normal mode, as illustrated schematically in FIG. 6 . In this illustration, the orientation of the pressure differential is indicated by a plurality of arrows 86 . The pressure differential acts on elongate members 60 which have ends 64 , 66 held radially stationary by well screen ends 56 , 58 as represented by triangles 88 in FIG. 6 .
[0027] Once the predetermined differential pressure is reached as a result of fluid flow from the exterior annulus region 48 to the interior region 50 within the tool string, the elongate members or beams 60 collapse, as illustrated schematically in FIG. 7 . The beams 60 collapse until the flexing is limited by support structure 68 . As described above, the deflection is limited such that elongate members 60 remain in their elastic state and thus remain free to return to the intermediate mode illustrated in FIG. 6 after sufficient reduction of the pressure differential. This radially inward mode of deflection does not completely remove the gaps created by slots 62 and thus allows some liquid flow therethrough. The retained gaps enable slurry, for example, to continue to dehydrate over a given period of time.
[0028] The radially inward deflection mode also forces the elongate members 60 into closer proximity with each other, thereby crushing particles that are within the gaps or slots 62 between elongate members 60 . Upon sufficient reduction or removal of the pressure differential across well screen 44 , the well screen 44 returns to its intermediate deflection mode. Fluid flow can then be directed into interior region 50 within tool string 46 to create an outward flow of fluid through well screen 44 from interior region 50 to exterior region 48 . The fluid flow can be directed to interior region 50 via flow through coiled tubing or jointed pipe of system 20 , for example. This backflow can be used to create a pressure differential able to transition the well screen to a radially outward deflection mode in which elongate members 60 are bowed radially outwardly, as illustrated schematically in FIG. 8 . The outward flexing of well screen 44 increases the gap size by opening slots 62 and further facilitates the washing away of any remaining debris previously trapped in the gaps between elongate members 60 . Upon removal or reduction of the pressure differential, well screen 44 returns to its intermediate deflection mode.
[0029] The ability to flex well screen 44 between radially inward and/or outward deflection modes and to control the gap size between elongate members 60 effectively allows well screen 44 to breathe by removing plugging proppant or other materials. Furthermore, the well screen gap size can be adjusted to an optimum size during usage of well screen 44 simply by using internal and external differential pressures across well screen 44 . One result is an increase in running time for well screen 44 which, in turn, facilitates the performance and efficiency of well operations by reducing the running in and out of the wellbore to change screen assemblies.
[0030] In some well applications, the deflection due to expansion is controlled by pressure drop because flow to the interior of tool string 46 can either leave through well screen 44 or through the bottom of bottom hole assembly 52 . In these embodiments, flushing at a predetermined, controlled rate provides the pressure differential needed to expand well screen 44 to the radially outward deflection mode.
[0031] Well system 20 can be designed for a variety of well related operations that can benefit from the ability to use simple pressure differentials in controlling gap size for conducting flow through the well screen 44 and in preventing plugging of the well screen 44 . As illustrated by the flowchart of FIG. 9 , the compliant well screen 44 can benefit a variety of well related operations. In operation, the compliant well screen 44 is initially connected to a tool string 46 designed for a specific well operation or operations, as indicated by block 90 in FIG. 9 . The compliant well screen 44 is then run downhole into wellbore 26 on tool string 46 , as indicated by block 92 . Once well screen 44 is positioned at a desired location within wellbore 26 , the well screen is utilized in the desired well operation, as indicated by block 94 .
[0032] The utilization of compliant well screen 44 may be incorporated into a variety of well operations. For example, compliant well screen 44 can be used in a producing well or to facilitate the return of clean fluid to a surface location in a gravel packing operation. Compliant well screen 44 also can be used to facilitate a fracturing operation or a well stimulation operation. Additionally, compliant well screen 44 can be used in a clean-out operation or to facilitate the reverse circulation of fluid through a bottom hole assembly. Furthermore, the well screen 44 can be flexed to create a desired gap size and/or to remove accumulation along the well screen while the well screen is moved along wellbore 26 . For example, well screen 44 can be flexed to prevent plugging and/or to adjust gap size as the well screen is run in hole, pulled out of hole, or moved between wellbore zones.
[0033] In any of these operations, well screen 44 is flexed via a created pressure differential to remove accumulation and prevent plugging and/or to adjust the gap size between elongate members 60 , as indicated by block 96 . During or after flexing of compliant well screen 44 to a desired deflection mode or modes, the well operation is continued without any need to pull well screen 44 from the wellbore, as represented by block 98 . Accordingly, no separately powered tools are required to clean the well screen, and well screen 44 can be operated with simple pressure differentials between an exterior and an interior of the well screen.
[0034] It should be noted that well system 20 may have a variety of configurations and components for use in many types of well operations. Additionally, the diameter, length, shape and materials of well screen 44 can be adjusted to accommodate system requirements, environmental factors or other design considerations.
[0035] Accordingly, although only a few embodiments of the present invention have been described in detail above, those of ordinary skill in the art will readily appreciate that many modifications are possible without materially departing from the teachings of this invention. Accordingly, such modifications are intended to be included within the scope of this invention as defined in the claims.
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A system and method is provided for filtering in a wellbore during various well related operations while limiting the potential for plugging. A well screen is used for filtering particulates from a fluid at a wellbore location. To remove accumulated material and avoid plugging, the well screen may be flexed via pressure differentials created across the well screen. The flexing of the well screen breaks free the accumulated materials, thereby avoiding premature job failure.
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FIELD OF THE INVENTION
The present invention is a system for accessing applications from even the most basic Instant Message (IM) enabled mobile device. The system utilizes the IM infrastructure of a mobile device to deliver application interfaces and manage the user experience.
BACKGROUND OF THE INVENTION
The growth of wireless technologies has produced a range of choices for mobile connectivity. This growth has been one enabler in the expansion of personal mobile devices such as advanced mobile phones, personal digital assistants (PDAs), and other diminutive devices. The plethora of devices and connectivity options has created an opportunity for new communication ideas and services. Even existing resources can be better utilized by exploiting the new wireless technology, middleware, and protocols. The increase in connectivity options has allowed users to keep their “always-on” devices always on their person. It appears that this trend will shift the concept of “personal computing” from desktop personal computers (PCs), and laptops, to mobile devices.
Concurrent with this wireless technologies growth has been the growth of instant messaging (IM). IM is a popular communication application that began on the desktop and quickly migrated to mobile devices, helped along by the ease in porting the small footprint client. The popularity of IM is due to its simplicity, wide usage, and quick response. Users are able to hold simultaneous disjoint text-based exchanges with multiple users or contacts. IM systems create a fluid communication environment that encourages many exchanges with multiple contacts by publishing their presence or availability. When a contact starts using their IM client, and thus available for receiving messages, the IM system notifies all other users interested in the contact. Users now aware of the presence of the contact simply send messages to the contact's IM identity. So the IM system not only manages the messages between users, it takes care of detecting and notifying users of each other's availability or presence.
IM clients can be found on mobile phones, wireless PDAs, pager devices, etc. Furthermore, IM enjoys healthy attention from service providers such as AOL (America Online) and MSN (Microsoft Network) as well as the open standards community like the JABBER organization. This results in a constant expansion of the IM paradigm and the underlying technology (for example, secure and enterprise versions). Early IM systems consisted of buddy lists (presence notification), chat (text messages), and chat rooms. More recent developments include file and media exchange, as well as streaming media.
The popularity of IM makes it a natural interface for communication applications. For example, presence-based voice calls are notable because they drop the dialing step, reducing the uncertainty of connecting with the party of interest. IM has also been used to add communication features to existing applications by associating an IM channel with application usage. Network gaming is one example of adding a separate or an integrated IM communication channel to enhance the dynamics of group play. Work-related collaboration is another natural progression for IM use, both in the session staging as well as the interaction phase.
The present invention extends IM beyond communications and into the general application space. There exist prior art systems that have put application interfaces on IM clients. Typically such systems provide a messaging server that interfaces to an application server using a server-side natural language processor to replace the elements of the application's interface. These systems translate phrases and abbreviated text into the appropriate query and command statements. The inclusion of a natural language interface creates an added layer of application abstraction requiring the user to learn a new model for using an application. The burden on the user grows with the number of applications added to the system. These systems are well suited for query-like application interfaces (i.e. Structured Query Language, SQL) for use with an online helpdesk or in information queries. Additional prior art systems include an “application buddy” that uses presence information and search algorithms to deliver general message alerts to a user.
In addition, prior art remote desktop systems exist that deliver the full desktop interface to networked devices. For example, Microsoft Corporation's Remote Desktop Protocol is a protocol for transporting mouse, keyboard, and display rendering information for Windows-based applications. It demands high bandwidth to a client that may have a smaller footprint but is physically a PC. This system is suited for locally networked PCs running Microsoft technology. Any deviation from this configuration introduces latency and detracts from the user interface experience. The number of devices and services that support the system also limits usage.
Many mobile application delivery systems are designed to deliver content to different devices, making the necessary content conversion or protocol translation. Standards, such as J2ME (Sun Microsystems, Java 2 Enterprise Edition), provide support for writing mobile device independent applications, including the user interface. There exist prior art proprietary systems that provide coverage for many devices that may be used to access resources. The breadth of support requires a complex infrastructure and maintenance. As mobile communications and devices continue to expand in the number of protocols and devices, these systems must incorporate the changes and resolve any conflicts and inconsistencies. By attempting to deliver device and technology independence they assume the burden of integrating new technologies and requirements while maintaining performance expectations.
There exists a need in the prior art to extend IM beyond communications, that is, to utilize it as an application interface. Moreover, this interface should provide a universal interface to represent disparate applications on unmodified IM clients. The present invention addresses these needs by providing an instant messaging user interface. This aspect of the invention is referenced herein as IMUI. IMUI leverages existing infrastructure, devices, client interfaces, and applications to provide ubiquitous access to computing services.
SUMMARY OF THE INVENTION
The present invention uses IM as a universal user interface. In particular, IM is extended beyond communications to provide control for remote applications. The means for using and controlling applications is known as a user interface. The user interface for an IM client is typically crude (in contrast to the Web), however, the present invention transforms that interface and combines it with an applications server to attain an application interface that leverages IM.
The invention uses the IM infrastructure to connect a user to an application's interface. This is accomplished no matter what type of device is being used. The invention maps user messages directly to an application's collection of commands. The list of IM buddies is actually a list of the menu items for an application or a group of applications. By constantly updating the Buddy List based on user behavior, the user can trigger the applications to perform desired operations. Unlike prior art systems that rely on a query system and resulting required customization, the present invention manages the display of an application's interfaces as IM buddies on the user's device. In this way the present invention maps presence and availability to functionality. By actively managing the availability of application interfaces for the user, and conveying the user's availability to applications, the invention enables a new presence-based dynamic to applications.
A further embodiment of the invention transforms IM into an interface of generality approaching graphical user interfaces (GUI). To simplify the use of GUI's, the underlying software architecture separates GUI management from the application code. Essentially, by having a message exchange between the GUI window management code and the application, two separate processes could be run to perform an application. Thus, in a typical GUI application interface the GUI menu items are encoded into messages sent to the application code when the user makes a selection. The application code knows the full palette of menu items but would have minimal knowledge of the underlying GUI code that generates and mages their presentation. This approach allows an application to be run on a remote separate machine and accept GUI messages for the user's machine.
This embodiment exploits this distributed structure to allow the user to send applications messages that may be on a remote system. The messages are related to the user interface (UI) messages in the menus. An application can define a set of instant messaging UI messages (IMUI) specifically to serve IM users. Furthermore, since application management on a desktop UI is similar, the invention allows the user to mimic the capabilities found on a desktop.
The invention exploits the typical features of IM provided by IM services. The invention creates and manages a group of IM identities specifically to serve as proxies for applications. These identities are then added to the Buddy list of actual IM users. Each of these new entities will be referred to as a buddy app (BAPP). Buddy list inclusion allows the BAPP to interact with users. A server, like a window management system, manages the application proxies to make BAPP appear, disappear, change appearance, change status, send messages, accept messages, etc. The server utilizes the IM behavioral model to produce the desired application interface to the IM user.
The real IM user sees a set of IM identities including the BAPPs that represent applications. The server is responsible for the presentation of applications' related IM identities. The server determines which identities should be presented to a user and the appearance. The message exchanges between IM user and the Bapp result in changes in the application buddies.
In a further embodiment of the invention, there is a special buddy to be available that acts like the Main BAPP. One can imagine it similar to a shell or command program, a program to launch other programs and manage files. By sending the main BAPP messages, the user can request applications, file operations, or services and receive appropriate responses. After an application is spawned, its BAPPs (one or more) are displayed as an IM buddy. The user can send messages to the application via the BAPPs. For example, (assuming the classic drop menu application scheme) by sending a “new” message to the “File” BAPP the user can create a new application document. The application sends a message response via the BAPP; the user can edit the message and send the modified text back to the application or issue a new message.
BRIEF DESCRIPTION OF THE DRAWINGS
Various embodiments of the present invention will now be described in detail in conjunction with the annexed drawings, in which:
FIG. 1 illustrates an example of the IMUI of the present invention using JABBER wherein the depicted buddies represent Desktop and three available printers;
FIG. 2 illustrates an embodiment of the invention when used with a standard IM client, such as AOL IM;
FIG. 3 is illustrates an embodiment of the invention in which chat with Desktop buddy is employed to issue directory commands;
FIG. 4 illustrates IMUI modules in the App Server in an embodiment of the invention; and,
FIG. 5 illustrates an embodiment of the invention utilizing IMUI with an MSExcel spreadsheet.
DETAILED DESCRIPTION
In an embodiment of the invention an IMUI (Instant Messaging User Interface) system is provided for mapping GUI-based applications onto a canonical IM client. The system produces a direct transformation of an application GUI to an IM user interface model with minimal functional deviations. Even important productivity features such as macros and keyboard shortcuts are transferred into the IM realm. In this embodiment IMUI does not replace the application usage model with yet another, instead, it leverages user knowledge and expertise by retaining the GUI elements and behavior within a messaging format. The same application is used but is essentially obtained from chat sessions in an IM client.
This invention is particularly applicable to a user who alternates, as needed, between desktop application usage and a more limited experience on a mobile device. If this user were seated in his office, then the desktop computer is likely the best platform for using his favorite applications. If the scenario parameters change in any way, then IMUI is a compelling alternative. By way of example, should the user walk next door to a colleague's office, applications may no longer be accessible or may require reconfiguration (i.e., file accessibility, work state, licensing, etc). Should the user leave the building, more challenges arise, like an absence of computers and network access.
FIGS. 1 and 2 , illustrate how IMUI 204 provides access to applications via the IM client of any well-known messaging system such as JABBER. Such a messaging system is employed over gateways 208 , to service providers such as AOL IM (illustrated as item 210 ), ICQ, Yahoo IM, MSN, etc. The embodiment of the invention depicted in FIG. 2 illustrates the IMUI components distributed across an enhanced JABBER server 206 and a J2EE application server 202 . By building upon widely available IM services and middleware standards this embodiment functions independent of network transport.
I. The IMUI User Interface Management Model
In one embodiment of the invention, IMUI maps application GUI elements such as menus and text boxes to automated IM identities. The system controls a pool of synthetic IM users (SIMU) or dynamically registers new user identities as necessary to provide service. IMUI logs SIMUs in or out of the IM server and configures the buddy associations. All messages to SIMUs are consumed by IMUI and routed to the appropriate application. IMUI accepts from (real) users messages formatted to reference an application GUI element. FIG. 1 is an example of such a message that shows a simple IMUI session in a JABBER client. As illustrated, the buddy list represents applications 102 and resources such as Desktop 104 and printers 106 . IMUI allows users to have a choice in how an application is represented in an IM client. As illustrated, top-level menus can be mapped to buddy groups (e.g. “Printers” 106 ) while submenu items 108 , 110 , 112 are mapped to the group members. Another option is to represent an application user interface with a single IM identity. The difference between the two options appears in the length of the GUI message. A shorter message is used when a message is sent to a submenu buddy because there is less need for disambiguation. For example, to open a file in a single buddy application the user may send the message “file open ‘filename’.” In an application with a buddy group per top-level menu the user may send the message “open ‘filename’” to the File buddy.
A. UI Management
The buddy name displayed on a user's IM client is either the unique IM handle or a nickname chosen by the user. This common IM feature allows a user to assign a nickname to replace the sometimes-cryptic unique handle. The nickname is strictly aesthetic; it can be changed at any time. Buddy lists are normally stored on the IM server for retrieval when the user logs in from an IM client. IMUI leverages this server scheme to automate the process of dynamic buddy list naming.
Logging SIMUs in and out of an IM server is not sufficient for rendering a user interface on a canonical IM client. In the IMUI system of this embodiment of the invention, a SIMU has three attributes. In addition to the unique IM handle, it has an association list, and a name (technically a nickname).
IMUI changes the SIMU nickname in a user's buddy list to correspond to a resource or application. By renaming a SIMU, IMUI can change an application's appearance on the IM client. This is useful when it is appropriate to display application or resource state information. For example, a telnet application may originally have a buddy name ‘telnet” but later include the host name.
An association list is the set of users that include a given SIMU in their buddy list.
This parameter allows a SIMU to be a reusable, pooled resource. A SIMU can be obtained from the pool and assigned to a user by changing the buddy lists of both the SIMU and the user. The SIMU is returned to the pool after the user terminates the application (SIMU) or logs out. The freed SIMU can be reused for another IMUI purpose.
In an additional embodiment of the invention, the IMUI has buddy list editing capability for all users, both real and synthetic. In this case, the IM server supports server-side buddy list changes. By way of example the IMUI may use a modified JABBER server that features an interface for roster (buddy list) management.
B. The Überbuddy
In an additional embodiment of the invention the IMUI defines a single, system-wide IM buddy, an “Überbuddy,” that is logged in at all times and captures user presence information for the system. The information is used by the IMUI to provide presence-driven service to the user. In this embodiment the Überbuddy is normally named “Desktop” in buddy lists because it also accepts service request messages from users. The Desktop buddy provides basic file and printer services and allows user applications to be spawned. By way of example, FIG. 3 illustrates this embodiment of the invention in which an IMUI chat with the Desktop buddy is employed to issue directory commands. Desktop is analogous to an operating system shell prompt like MSDOS and BASH. In additional embodiments, users may have applications pre-deployed on their IM client or launched based on a context-driven algorithm.
C. Minimalist Desktop
In an embodiment of the invention, the services of the Desktop buddy and other IMUI applications are referred to herein as the “Minimalist Desktop.” This name reflects an attempt by this embodiment of the invention to project a desktop PC application and resource model to IM users. That is, the IMUI design goal is to provide the choices and functionality of a desktop environment but on mobile devices. The Desktop buddy is typically accompanied with File and Printer groups. These two resources are user and context dependent. IMUI provides small-footprint servers for distributed file and printer access. Each server is user configured to expose local files systems and printer resources to the main IMUI server. IMUI can then provide access to these resources to the user over an IM client. The Desktop and resource buddies also share session context to streamline basic file and printer operations. For example, a user may perform a directory operation with either the Desktop buddy or the File buddy. Assuming the file listing was performed with Desktop and the user wishes to print the second file in the directory with the first printer buddy, the user may issue the print command through Desktop only using indices for the file and printer choices. This is possible because Desktop, the Überbuddy, is aware of the file listing order and the printer buddy order.
Desktop is the only native IMUI application. All other applications are external and integrated into the IMUI system. Currently, context sharing is limited to the Desktop, File, and Printer buddies. Further discussion of the Desktop buddy and the underlying IMUI infrastructure is found below.
II. GUI-Emulating API
The chat window of an IM client is a natural interface to applications with text-based terminal user interfaces. Difficulty arises when one considers the various classes of graphical user interfaces used by web and desktop applications. Menus, buttons, entry boxes, selection lists, etc., are part of the normal palette of interface elements in GUI applications. A user manipulates these GUI elements with text input, mouse clicks, dragging, etc. The activity is sent to the application, which interprets the element choice and user action. To support these applications in a messaging user interface model (IM chat), a transformation of the GUI elements to an IM paradigm-compatible form needs to be defined.
In an embodiment of the invention the IMUI accepts GUI manipulation expressions from an IM user to manipulate applications. Therefore, the system must capture application GUI design specifications to render on IM clients and for message parsing. Applications are controlled at the Application Program Interface (API) level, requiring IMUI to also incorporate application programming interface information. Therefore, each application has a particular GUI and API specification.
An embodiment of the invention will now be described which relates to the complementary GUI and API specifications in IMUI and the invention's methods for utilizing the information. In particular, this description will contain the general approach to GUI design capture and the available sources of design specification information.
A. GUI Design Capture
Contemporary computer systems and software development tools help programmers reduce the complexity of their applications by providing an independent server for GUI management. Systems such as X Windows Protocol and Microsoft Windows provide libraries for defining a GUI and managing user manipulation of the interface. The application programmer need only supply instructions for handling messages representing user activity and GUI state information.
Many development tools allow user interface design and viewing before any application code is written. The specification for the design is stored in a text file and processed by the development system for linkage with the application code. For example, a developer using the Microsoft Windows development environment can use the Microsoft Visual tools to design the user interface and save the description in a text resource file (*.rc file). Another example is Tcl/TK, a popular system and development environment, originally from the UNIX world, which also supports GUI applications. Tcl/TK is script-based so it naturally keeps user interface layout information in a script file (*.tcl file). In both examples the GUI specification can be kept in a text file separate from the application code.
B. Application Domain APIs
Application server component architectures such as J2EE and Microsoft's .NET contain a collection of technologies exposed through APIs (including protocols and services). Each API represents a domain of applications that can be invoked by the application server. However, each application defines a unique set of commands for application operation. For example, one API available on some application servers is COM. This API covers many Microsoft Windows applications. An application accessible over COM, such as Microsoft Excel, defines a set of application-specific commands. To load a spreadsheet, or perform any other operation possible from the Excel user interface, a script of Excel COM API calls can be generated to produce the desired behavior.
There are many other APIs, protocols, and programming abstractions available for application integration. Additional examples of APIs and their application domains include HTTP (Web), EJB (J2EE), SOAP (Web Services), SQL (Database), etc. In an embodiment of the invention IMUI's application server component is built upon the Weblogic application server (developed by BEA Systems, Inc., and hereby included by reference). This server supports many of the previously mentioned APIs. The set of APIs supported on the IMUI system determine the space of application domains available to users on their IM clients.
In additional embodiments of the invention the IMUI also incorporates the telnet protocol to extend the application server native API set. Telnet enables access to the large set of shell or command-line applications. Also, the terminal interface is naturally matched to the IM chat mechanism.
C. GUI-API Symmetry
An application model (user model) can be defined as the GUI or the front-end. The API or back-end is for developers and may be subject to different design goals. Depending on the functional symmetry between an application's API and GUI, a complete substitution of the GUI by an application server manipulating the API is possible. Due to this symmetry one embodiment of the invention creates a back-end application model that emulates the GUI. In fact, the model may be expressed simply with scripts of API calls that emulate GUI commands. If a script-level implementation is not sufficient the native programming tools of the application server can be used.
In IMUI the application GUI specification is captured by parsing the GUI text resource file using the development environment's grammar. The parsed specification can be converted into a software representation (e.g., Enterprise JavaBeans (EJB)) or a XML description or some combination of the two. For each GUI element a set of API instructions is generated to emulate user manipulation. To support a range of UI elements, naming and state variables are introduced.
The following are some examples of GUI elements and corresponding backend approaches to emulation in a messaging environment:
Commands (menu, button): one or more API calls to emulate a menu selection or button depress. Text Input (entry box): named variables are created for these interface elements commonly used in forms. State selection (drop list, radio button, check box): named variables are created with values constrained to the selection choices.
Some additional application interface issues are address below:
Object selection (point or region): a dynamic list of named objects is maintained to invoke API calls upon selection. Output from the application is returned from API calls and can be stored in state variables or sent to the user as a response message.
The GUI specification also holds common labor saving application UI features such as keyboard shortcuts and macros. By including macros and keyboard shortcuts IMUI retains most of the user interface options. More importantly, keyboard shortcuts and macros are text-based UI features compatible with the IM paradigm while also familiar and beneficial to users. Keyboard shortcuts are sometimes the interface of choice for many users and, therefore, may define the user's mental model of an application. Macros are application scripts that perform a series of application steps with a single command. They are potentially the most powerful mechanism in the IMUI system. Application macros streamline the syntactic matching between the IM chat interface and the backend application execution. Also, they can be used from both the GUI and the IM interfaces.
For information elements such as text entry and selection lists the system keeps corresponding state variables. They become part of the parameters used in commands when menu items or buttons are emulated.
The GUI/API information can be further utilized to help the user recall the application interface. In an embodiment -of the invention illustrated in FIG. 4 , the depicted APP Server 402 comprises an IMUI Query System 408 , a command review system analogous to the “help” feature of UNIX shells, thereby allowing the user to review the message syntax and features of an application interface. Users can refresh their application usage knowledge without needing keen recall of GUI commands and format. This system reduces the mental burden on the user when using a variety of applications via IM.
Also depicted in FIG. 4 is the IMUI Session Table 404 which keeps tracks of who the user 406 is and what applications/resources 410 are active/available/open. The IM session manager 412 sends the appropriate commands related to a buddy to the associated application/resources. An example of such a command related to an Excel spreadsheet is illustrated in FIG. 5 .
In FIG. 5 the left window 502 depicts a buddy list displayed with this embodiment of the invention. In the illustrated example, an Excel program is running d:\bea81\mortgage.xls. The right window 504 shows the IM “chat” with “d:\bea81\mortgage.xls” that is invoked when the appropriate entry on the buddy list is selected. In this example a ListNames Excel command is issued to the Excel program. This command results in a listing of all non-hidden names defined on the worksheet which appears in the right window 504 .
III. IMUI Framework Design and Implementation
The framework design of an embodiment of the present invention will now be discussed. The main goal of this design is to enable the integration of a wide class of applications for access via IM. Other priorities include the wise use of resources to maximize request throughput.
The three components of this embodiment, as illustrated in FIG. 4 , include the enhanced JABBER server, the IMUI Session Manager gateway and the IMUI system application server components. The client software is not included because the system is designed for use with an unmodified client.
A. Enhanced JABBER Server
In the depicted embodiment the messaging server is built upon the open source jabberd server. The jabberd server uses the Extensible Messaging and Presence Protocol (XMPP) and provides a gateway to AOL and other IM systems. Currently available clients include Exodus and, via gateways, the AOL, MSN, and Yahoo IM clients.
The server has been extended to include a pool of IM accounts for receiving messages from users destined for applications. These accounts are SIMUs, the IMUI buddies deployed to represent applications to IM users. The server also supports dynamic roster changes for both SIMUs and real user accounts. These administrative extensions enable the dynamic naming and associations necessary for UI management on an unmodified client. A privileged external entity (IMUI) is allowed to make these roster and SIMU changes.
B. IMUI Session Manager Gateway
The IMUI Session Manager gateway is separate from the enhanced JABBER server to isolate the general IM client traffic from the IMUI system traffic. Instant messaging is inherently stateless which means that messages have no access to the conversation history. Messaging servers are efficient traffic handlers because they are free of history or state. However, IMUI must handle state information to manage the UI rendering and application state. The gateway is bracketed by messages from the enhanced JABBER server and the application responses and administrative commands from the IMUI system. These are two distinct message traffic patterns requiring different implementation strategies. The gateway converts the XMPP messages for the IMUI system and sends the results via JMS. The IMUI system issues commands to the gateway to manage SIMUs and to shuttle messages between applications and users.
C. IMUI System
In this embodiment of the invention the IMUI system must monitor the presence of registered users, create application buddies as needed, and facilitate access to the backend application resources. Again, it should be noted that the messaging server could have been augmented to handle the IMUI functionality but since messaging servers are not designed to handle state or perform functions such as load balancing, resource pooling, and stateful transactions, these features would need to be created. Therefore, the system was implemented using BEA Weblogic, a J2EE compliant application server. Some of the highly utilized Weblogic services include message queues, database pooling, Microsoft COM access, servlets, and EJBs.
When a user logs into the messaging server, IMUI creates a user session object that stores key value pairs that represent application defaults, buddy mappings and current transaction information. The user state information is found each time a message is received by looking up the IM handle of the user sending the message. Each user key and value set is stored as a row in a database and is accessed via entity EJBs. State replication is avoided since many buddies can access the user state simultaneously without major coherency problems.
The buddy abstraction serves to manage access to applications based on the incoming message. Conversations can take place across multiple messages by providing stateful application resources that are managed for the user. Messages to the user can be produced independent of an initial user request by the asynchronous message handling subsystem.
1. The Buddy System
Each buddy that appears on an IMUI screen is an actual IM handle that has been renamed (nicknamed) to represent an application. The Überbuddy receives presence notifications from the server and messages from users requesting service from the IMUI system. It is “aware” of the existence of the other buddies because it is part of the session management system. It manages the user's session until the user logs out, causing the acquisition and release of SIMUs as needed.
User initiated messages are routed to the appropriate buddy application object based on the target of the incoming message. The IM handle of the message recipient is used to look up the target buddy in the user session record. The target buddy object is retrieved to service the request. The buddy parses the incoming text message and invokes the appropriate backend process to handle the user request. The backend process handles application specific data.
In addition to the Überbuddy, there are four other types of buddies:
Stateless synchronous—responses are synchronous, shared application resources Stateful synchronous—responses are synchronous, dedicated application resources Stateless asynchronous—not user-initiated; asynchronous messages from backend processes, shared application resources Stateful asynchronous—not user-initiated; asynchronous messages from backend processes, dedicated application resources
Stateless synchronous applications only send responses to user requests. This buddy can be shared between users since the application does not need to keep invocation specific information between messages. Any framework related defaults or administrative data is stored and maintained by the session manager.
Stateful synchronous applications send responses to user requests but the application instance needs users specific information and, therefore, cannot be shared between users. An example would be access to an Excel spreadsheet. When the buddy is created, it represents a specific spreadsheet that is accessible by a single user. As depicted in FIG. 5 the spreadsheet is opened and is dedicated to the session of the user.
Asynchronous message handlers are created for a specific user and buddy. The telnet buddy (terminal emulation to host machines) is an example of an application that needs asynchronous services. Such services watch for requests to return messages (i.e. a command line prompt) and map the messages back to the IMUI buddy that should display the message to the user. Although the telnet session's output is in response to a user request, there is no time limit on when replies might be received. Another example would be a buddy set up to send notifications of voicemail messages. The voicemail listener is an asynchronous service to send messages back to the user as necessary.
2. Proprietary IM Modifications
Some proprietary messaging systems do not facilitate the creation and change of user accounts programmatically. Therefore, the IM client-rendering model has been modified to allow all application access via a single Desktop buddy. In a single buddy interface all messages are sent through one chat window. Message destination is based on a “default” application context. To change the default application for receiving messages (i.e. change the target application from telnet to a printer), an additional set of commands are introduced. These commands allow the user to switch context from one application to another. The available applications can be listed as well to keep the user informed. The single buddy interface is also necessary when using limited IM clients such as pagers or wireless phones with limited text displays.
3. Resource Access Wrappers
Application resources exist on a variety of platforms and languages. Access to such resources is accomplished via wrappers that encode protocol and functionality information. By way of examples, IMUI applications may include Excel via COM; Dictionary.com via HTTP; SSH (secure telnet), file access and printer access via Remote Method Invocation (RMI); and directory access via Lightweight Directory Access Protocol (LDAP).
4. Resource Servers
Files and printers are location dependent resources. An enterprise may be composed of multiple physical locations sharing a common network. Printers in such an enterprise perform the same function yet are distinguished by physical location (and capabilities), both within a site and across facilities. A user may move about the various sites and need to print documents to the nearest printer. In an additional embodiment of the invention the IMUI utilizes printer servers, e.g., small footprint servers running the Java Print Service. Such printer servers perform service discovery and are distributed to map enterprise printers to their physical locations.
Similarly, users may access more than one file system. In addition to a home directory on a network file system a user may utilize files on their PC's. Other directories on networked machines may be of value to the user (i.e. shared project directories). IMUI uses local file servers to support retrieval of such files for the user via IMUI.
IMUI combines file and printer servers to allow a user to print their various files to the various printers. The servers are sent the print requests and handle the file transport outside of the IMUI server.
IV. Prototype Examples
As noted above, the “Minimalist Desktop” concept of the present inventions seeks to provide applications and resources commonly found on a desktop environment to IM users. In plain language, it is a recreation of a productive office application palette in the most diminutive package and enhanced by presence information. The expectation is that this new technology configuration will alter mobile application usage behavior. IMUI is designed to deliver applications beyond information query and access. The native GUI support allows the system to span application classes like Microsoft Office, the web, web services, etc.
In various embodiments of the invention IMUI provides the technological service of access and control of applications and information normally physically anchored in an office. The combination of access and usage of applications should lead to new usage behaviors and scenarios. For example, Excel spreadsheets, once built, hold financial models and information that can be useful even without display of the full worksheet. As illustrated in FIG. 5 , an Excel application buddy is loaded with a mortgage spreadsheet model. The user chats with the buddy to list all named cells in the mortgage model. The user can get/set those cells to values of interest and the spreadsheet is updated automatically (as expected). The user can then display a named cell, range of cells, or a region in the chat window. The user can also print or email the spreadsheet or a chart by executing a named macro. It is anticipated that IMUI users will change their spreadsheet designs to include more macros for common tasks and procedures. The motivation will in part be due to facilitating productivity in IMUI scenarios.
Presence information can be used to enhance any IMUI scenario. FIG. 5 shows the set of printers 506 selected by the Uberbuddy for the user upon presence detection. The set of printers could have been based on the user's location (possibly derived from the presence information). Of course, the user can add and remove printers as desired. For instance, the user may request a remote printer at a commercial document printer. Ideally, traveling to deliver a presentation could only require taking along a mobile phone with IM service and stopping by a local printing establishment near the destination.
Presence notification can also be used to provide the user with an indication of application state. A package-tracking buddy can perform the polling of package tracking websites and change presence state upon arrival of the package. An office phone buddy can indicate the ringing of the office phone whenever the user is out of audible range. The user might even wish to choose different answering options based on the caller id. For example, choosing a “just a minute I'm down the hall” message to keep the caller from hanging up.
The ability of the present invention to map an array of various IMUI specific visual icons to better reflect the state of various applications and/or resources is not limited to the above examples. The well-known IM ability to map different icons with buddies can be utilized in this invention in numerous ways. By way of example, the invention enables an individual to select an icon representing his mood to indicate his “state” for receiving phone calls. Use of animated icons, as are well-known in IM messaging, are also contemplated by the invention.
The telnet buddy can be seen as both an application and an application class. By providing access to shell-based applications on remote hosts, it delivers a class of applications to the user.
IMUI broadens the utility of telnet by facilitating sharing of telnet sessions. The IMUI session manager can allow users to share or swap telnet sessions by sending a request to the Desktop buddy. A useful application of this feature is remote technician access to networked systems. For example, a communications device on a network may need servicing by a technician. The technician may only need command line access to the device to issue commands, run scripts, etc. The customer need only log onto the network and transfer the session to the technician to initiate the repair operation. In sharing telnet sessions it would be rational to add message filtering to restrict certain messages from a telnet session borrower (i.e. password changes). If access to IMUI is allowed from unsecured external IM systems then it is recommended that the telnet buddy be restricted to hosts within a computer network demilitarized zone (DMZ).
IMUI is also useful in requests for graphical display service. A telnet session can be used to configure X-Windows for a local display. Since many corporate network access rules allow for outgoing connections it is possible to display an enterprise X-Windows application on an external machine.
Of course, other application buddies can be shared. A possible out growth of this sharing option is “application operators.” Similar to telephone operators, application operators are contacted to request applications on demand. This situation is likely during mobile device usage in a public environment. A customer might request a partially filtered list of airline flight times from a travel website. Once the application is transferred the customer can leisurely analyze and prune the list to serve their particular travel and budget needs.
V. Additional Features
Inherent in the current invention are the features that relate to built-in facilities in the application server and in the messaging server. Accordingly, access to IMUI via IM gateways is insecure using the popular free services. The invention contemplates attaining enhanced security by utilizing enterprise versions of these services. Additional embodiments of the invention further address issues of security within the architecture of IMUI. Building security and authentication features into IMUI are addressed in these embodiments.
Further embodiments of the invention include adding new application classes to IMUI. For example, supporting X-Windows applications within IMUI is useful because it allows users to benefit from the large software base. Not all applications can be used. For example, Xclock is a highly unlikely candidate for incorporation into IMUI.
While the invention has been described with reference to the preferred embodiment thereof, it will be appreciated by those of ordinary skill in the art that modifications can be made to the structure and elements of the invention without departing from the spirit and scope of the invention as a whole.
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The present invention is a system for accessing applications from even the most basic Instant Message (IM) enabled mobile device. The system utilizes the IM infrastructure of a mobile device to deliver application interfaces and manage the user experience. The invention is particularly applicable to applications with graphical user interfaces (GUI), even typical desktop or web applications. The system performs a direct transformation of application user interfaces into an IM messaging model with minimal functional distortions. The users own application knowledge and experience is leveraged, reducing application customization in the system architecture. The system also incorporates presence-driven mechanisms in the architecture.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. provisional patent application No. 61/119,065 filed Dec. 2, 2008, which is hereby incorporated by reference in its entirety herein.
BACKGROUND OF THE INVENTION
Field of the Invention
[0002] The present invention relates generally to airborne rocket and missile launching systems and, more particularly, to an aerodynamically optimized rotating launcher.
SUMMARY OF THE INVENTION
[0003] The rotating launcher disclosed is an airborne rocket and missile launching system designed to reduce drag.
[0004] In an embodiment, the rotating launcher system includes: a plurality of rocket or missile housing tubes arranged in a circular pattern within a carousel, a set of frames, a cylindrical protective skin, an aerodynamically optimized nose cone with a bore, and an optional door covering the bore, enabling rockets or missiles to exit the launcher. The rotating launcher system may also include an aerodynamically optimized tail cone with a bore, and an optional door covering the bore, enabling exhaust from the rockets or missiles to exit the launcher. The rotating launcher system also includes an integral controller for an indexing motor, and an indexing motor enabling the bores of the nose and tail cones to align with different rockets or missiles in the carousel by either rotating the nose and tail cones, or by rotating the carousel itself.
[0005] In the first configuration for the rotating launcher, an arming signal sent to the integral controller causes the doors over the bores of the nose and tail cones to open and create a clear path for the rocket or missile to exit the launcher. A subsequent firing signal causes the rocket or missile to fire and exit the launcher. Upon exit of the rocket or missile, the integral controller sends a signal to the indexing motor causing it to rotate the nose and tail cones by equal amounts either clockwise or counter-clockwise in order to align the bores of the nose and tail cones with another rocket or missile in the carousel. If the controller receives another firing signal it will repeat the launching sequence. If the controller receives a disarming signal, it will send a signal to the door actuators to close the optional doors covering the bores of the nose and tail cones, if applicable. In this configuration, the carousel is rigidly mounted, and the nose and tail cones are directly coupled together and to the indexing motor by coupled shafts and free to rotate about the longitudinal axis of the launcher based on the indexed position of the motor.
[0006] In a second configuration of the rotating launcher, the overall arming, firing and disarming sequences are the same as the first configuration, but the circular carousel housing the rockets or missiles is rotated instead of the nose and tail cones. In this configuration, the nose and tail cones are rigidly mounted and the carousel is coupled to the indexing motor and is free to rotate about the launcher's longitudinal axis based on the indexed position of the motor.
BRIEF DESCRIPTION OF THE FIGURES
[0007] Embodiments of the present invention will now be described more fully with reference to the accompanying drawings where like reference numbers indicate similar structure.
[0008] FIG. 1 is a representation of an embodiment of a rotating launcher with the nose and tail cone launch doors closed.
[0009] FIG. 2 is a representation of the rotating launcher of FIG. 1 with the nose and tail cone launch doors opened.
[0010] FIG. 3 is a wire frame representation of the rotating launcher of FIG. 1 with internal components visible.
[0011] FIG. 4 is a wire frame representation of the rotating launcher of FIG. 1 with a shaded view of the indexing motor and shafts.
[0012] FIG. 5 is a wire frame representation of the rotating launcher of FIG. 1 with a shaded view of the carousel frames and tubes.
[0013] FIG. 6 is a representation of the rotating launcher of FIG. 1 with the nose cone removed and rockets or missiles visible.
[0014] FIG. 7 is a representation of the rotating launcher of FIG. 1 with the nose and tail cones indexed to an initial position, the nose and tail cone doors opened, and a rocket or missile being fired out of the launcher.
[0015] FIG. 8 is a representation of the rotating launcher of FIG. 1 with the nose and tail cones indexed to an alternate position, the nose and tail cone doors opened, and a rocket or missile armed and ready to fire.
[0016] FIG. 9 is a flow chart showing the signaling and control sequence for the rotating launcher.
[0017] FIG. 10 is a close up view of a portion of the rotating launcher of FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
[0018] FIG. 1 shows a schematic representation of a rotating launcher 100 in accordance with an embodiment of the present invention. Rotating launcher 100 is an airborne rocket or missile launcher designed to reduce drag. Rotating launcher 100 includes a nose cone 101 , skin 102 and a tail cone 103 designed with such a shape as to reduce aerodynamic drag. Nose and tail cones 101 / 103 have tapered outer surfaces to create the aerodynamic shape. Skin 102 is rigidly mounted to an airframe (not shown). Nose cone 101 and tail cone 103 each have a bore 201 , 202 , shown in FIG. 2 , coaxial to one another, and running parallel to the longitudinal axis 404 of the launcher, in order to enable a rocket or missile to exit launcher 100 . Bores 201 , 202 may be covered by a nose cone door 301 and a tail cone door 302 to further optimize the rotating launcher. Thus, as shown in FIG. 1 , the doors are closed during flight when the rockets or missiles are not needed. The nose cone door 301 and tail cone door 302 have the ability to open mid-flight to expose bores 201 , 202 , as shown in FIG. 2 , in order to create a clear path for the rocket or missile to exit launcher 100 . Although the figures show a single bore in each of the nose and tail cones, one skilled in the art would recognize that multiple bores may be utilized. For example, multiple concentric circles of launcher tubes may be utilized and separate bores may be aligned with each of the circles instead of a larger single bore. Further, bores may be provided 180 degrees apart and the nose or tail cone may rotate 180 degrees instead of 360 degrees.
[0019] The rockets or missiles 601 , shown in FIG. 6 , are housed inside of tubes 501 , shown in FIG. 5 , which are preferably arranged in a circular pattern about and the longitudinal axis of the launcher and equidistant from the longitudinal axis of the launcher. Additionally, the bore 201 in nose cone 101 , the bore 202 in tail cone 103 , and all of the tubes 501 are preferably equidistant from the longitudinal axis of launcher 100 .
[0020] In an embodiment, as illustrated in FIG. 4 , an indexing motor 401 is rigidly mounted to one of frames 502 . Nose cone 101 and tail cone 103 are free to rotate about the launcher's longitudinal axis 404 . Tubes 501 and frames 502 together form the carousel housing the rockets or missiles, and are rigidly mounted to skin 102 . Nose cone 101 is coupled to the rotating shaft of indexing motor 401 through shaft 402 and tail cone 103 is coupled to the rotating shaft of indexing motor 401 through shaft 403 such that any rotation of indexing motor 401 to any position causes nose cone 101 and tail cone 103 to rotate by equal amounts. Nose cone 101 and tail cone 103 may be coupled to shafts 402 / 403 using fasteners such as bolts, welding, or any other coupling known to those skilled in the art. Nose and tail cones 101 / 103 may be removably coupled to shafts 403 / 403 . Nose and tail cones 101 / 103 are rotatable relative to the carousel. In one embodiment shown in FIG. 10 , a portion of nose cone 101 overlaps skin 102 of the carousel. Skin 102 includes a flange 110 such that there is a smooth transition between nose cone 101 and skin 102 , as shown in FIG. 10 . Nose cone 101 may also abut skin 102 , or other suitable configurations may be used such that nose cone 101 is rotatable relative to skin 102 . The configuration shown in FIG. 10 may also be used between skin 102 and tail cone 103 . Indexing motor 401 has the ability to rotate nose cone 101 and tail cone 103 through shafts 402 and 403 in such a way as to align bore 201 in nose cone 101 and bore 202 in tail cone 103 with any one of tubes 501 . Indexing motor 401 may be a stepper motor, a brushless DC motor with position sensors, or other suitable motors known to those skilled in the art.
[0021] Once bores 201 , 202 in nose cone 101 and tail cone 103 are aligned with any one of tubes 501 , launcher 100 is ready to fire. Once fired, rocket or missile 601 , exits the launcher through nose cone 101 as seen in FIG. 7 . Once rocket or missile 601 exits the launcher, indexing motor 401 rotates nose cone 101 and tail cone 103 to align bores 201 , 202 of nose cone 101 and tail cone 103 with any one of the other tubes 501 , as shown in FIG. 8 . Once rotation is complete and if the launcher is disarmed, optional nose cone door 301 and optional tail cone door 302 may be closed in order to minimize drag. Alternatively, nose cone door 301 and tail cone door 302 may stay open to enable the next rocket or missile to launch.
[0022] In another embodiment, indexing motor 401 is coupled to one of frames 502 such that rotation of indexing motor 401 causes a corresponding rotation of the frame 502 . Indexing motor 401 may be coupled to one of frames 502 using fasteners, for example, or by other means known to those skilled in the art. Nose cone 101 and tail cone 103 are rigidly mounted to skin 102 such that nose cone 101 and tail cone 103 do not rotate relative to skin 102 . Nose cone 101 and tail cone 103 are also preferably coupled to indexing motor 401 through shafts 402 , 403 such that rotation of indexing motor 401 does not rotate nose cone 101 and tail cone 103 . Tubes 501 and frames 502 are coupled to each other and are free to rotate as a set (i.e., the carousel) about the launcher's longitudinal axis 404 . Due to indexing motor being mounted to one of frames 502 , any rotation of indexing motor 401 to any position causes tubes 501 and frames 502 to rotate by equal amounts. Indexing motor 401 has the ability to rotate tubes 501 and frames 502 in such as way as to align the bore 201 in nose cone 101 and the bore 202 in tail cone 103 with any one of the tubes 501 . Thus, similar to the embodiment described above, an aircraft (not shown) with launcher 100 attached to it can fly with reduced drag compared to a launcher without nose cone 101 or tail cone 103 . The aircraft can fly with the optional doors 301 , 302 closed. When a missile or rocket 601 needs to be fired, doors 301 , 302 are opened and the missile or rocket 601 is fired, leaving one of the tubes 501 empty. Indexing motor 401 is then rotated, thereby rotating tubes 501 and frames 502 such that one of the tubes 501 with a missile or rocket therein is aligned with bores 201 , 202 .
[0023] FIG. 9 illustrates the signaling and control sequence for the rotating launcher. An arming signal 902 is sent to the integral controller to open the optional doors over the bores of the nose and tail cones to create a clear path for the rocket or missile to exit the launcher. A subsequent firing signal 904 causes the rocket or missile to fire and exit the launcher. Upon exit of the rocket or missile, the integral controller sends a signal 906 to the indexing motor causing it to rotate the nose and tail cones by equal amounts either clockwise or counter-clockwise in order to align the bores of the nose and tail cones with another rocket or missile in the carousel. If the controller receives another firing signal it will repeat the launching sequence. If the controller receives a disarming signal 908 , it will send a signal to the door actuators to close the optional doors covering the bores of the nose and tail cones, if applicable.
[0024] The parts of the launcher system may be made of suitable materials known to those skilled in the art, for example, aluminum, carbon-fiber, and high temperature composite material. As would be understood by those skilled in the art, material selection may be made based on weight, strength, and other relevant characteristics of the material. In a non-limiting example, the skin of the system may be may be made of carbon fiber, the nose and tail cones may be made of carbon fiber and high temperature composite material, the frames may be made of aluminum, the shafts may be made of aluminum or steel, and the launcher tubes may be made of high temperature composite material.
[0025] While the particular rotating launcher implementations as herein disclosed and shown through the figures are fully capable of obtaining the objects and providing the advantages a rotating launcher system, they are merely illustrative of the presently preferred embodiments of the invention, and as such, no limitations are intended to the details of construction or design herein shown. Further, while the embodiments have been described with a nose cone and a tail cone, one skilled in the art would recognize that a rotating launcher system with only one of a nose cone or tail cone may be utilized. Similarly, although the particular rotating launcher has been shown with five tubes to hold five missiles, it would be understood that a rotating launcher with more or less tubes and missiles is within the scope of this invention.
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A rotating launcher system includes a plurality of rocket or missile housing tubes arranged in a circular pattern within a carousel, a set of frames, a cylindrical protective skin, an aerodynamically optimized nose cone with a bore, and an optional door covering the bore, enabling rockets or missiles to exit the launcher. The rotating launcher system may also include an aerodynamically optimized tail cone with a bore, and an optional door covering the bore, enabling exhaust from the rockets or missiles to exit the launcher. The rotating launcher system also includes an integral controller for an indexing motor, and an indexing motor enabling the bores of the nose and tail cones to align with different rockets or missiles in the carousel by either rotating the nose and tail cones, or by rotating the carousel.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a U.S. national stage entry under 35 U.S.C. §371 of International Application No. PCT/EP2012/068677 filed Sep. 21, 2012, which claims priority to French Application No. 1102901 filed on Sep. 23, 2011, the whole content of these applications being incorporated herein by reference for all purposes.
TECHNICAL FIELD
The present invention deals with a method for determining the interfacial tension existing between two fluid phases, under temperature and pressure conditions in which at least one of the two fluid phases is in the supercritical state (the two fluid phases being able for example to be an aqueous phase and a phase based on CO 2 in the supercritical state). The invention also relates to devices suitable for the implementation of this method, as well as a screening procedure comprising one or more steps of measuring interfacial tensions under supercritical conditions employing the aforementioned determining method.
BACKGROUND ART
For the purposes of conciseness, in the subsequent description, the temperature and pressure conditions under which one and/or the other of two fluid phases present is in the supercritical state will be referred to by the generic term “supercritical conditions”. Thus, two fluid phases termed “in supercritical conditions” or “under supercritical conditions” in the present description comprise (1) a first phase in the supercritical state and (2) a second phase, in contact with the first, and where said second phase is in the liquid, gaseous or supercritical state (generally liquid or gaseous). Two fluid phases termed “under supercritical conditions” according to the present description are therefore not necessarily both in the supercritical state. Stated otherwise, two phases having critical temperatures of T 1 and T 2 and critical pressures P 1 and P 2 respectively, the phases will be considered to be “under supercritical conditions” within the meaning of the present description if, and only if:
the temperature is greater than T 1 and the pressure is greater than P 1 ; and/or the temperature is greater than T 2 and the pressure is greater than P 2 .
The aforementioned interfacial tension under supercritical conditions exists between two non-miscible fluid phases under the supercritical conditions of measurement. Unless explicitly specified to the contrary, the expression “non-miscible fluid phases” refers, in the present description, to two phases in the liquid, gaseous or supercritical state and which are not miscible under the conditions of implementation of the method (it being understood that the two phases could optionally be miscible under other conditions).
Access to the knowledge of the value of interfacial tensions between two fluid phases under supercritical conditions is of importance, in numerous technological sectors. This parameter may indeed turn out to be critical in particular in certain physico/chemical methods employing a phase in the supercritical state, or else liable to lead in the course of their implementation to supercritical conditions. Inter alia, access to the value of the interfacial tension is of interest for processes employing CO 2 in the supercritical state, which can be used for example in syntheses or methods not employing any organic solvents; in petroleum recovery methods; or else for the capture and storage of CO 2 .
The determination of an interfacial tension between two fluid phases under supercritical conditions is known as being relatively complex to implement. In fact, it generally requires heavyweight apparatus, in particular having regard to the high pressures which are employed. Moreover the procedures which have been proposed to date for the measurement of interfacial tensions in a supercritical medium generally involve long durations of measurement, as well as relatively significant volumes, with associated risks for the operators (supercritical conditions involving risks of explosion or of leakages which increase with the duration and the quantities). In addition to these safety problems, the proposed methods are often limited to the analysis of certain specific fluids and the conditions of analysis have to be adapted for each fluid pair studied.
The scant procedures which have currently been proposed for the measurement of interfacial tensions under supercritical conditions, prone to the aforementioned drawbacks, typically implement high-pressure visualization cells, within which the interfacial tension is determined according to the so-called “pending drop” (or “hanging drop”) technique, where the measurement is performed by analyzing the shape adopted by a drop of a dense phase suspended within a less dense phase. For further details in this regard, reference may in particular be made to U.S. Pat. No. 5,653,250 or else to the article by Adkins et al. In the Journal of Colloid and Interface Science , vol. 346, p. 455 (2010).
SUMMARY OF THE INVENTION
An aim of the present invention is to provide a procedure making it possible to determine the interfacial tension between two fluid phases under supercritical conditions, while circumventing the aforementioned problems encountered with the procedures described hitherto. The invention is in particular aimed at providing a procedure making it possible to determine, in a manner which is at one and the same time reliable, simple and as inexpensive as possible, the value of interfacial tension between two fluid phases under supercritical conditions.
For this purpose, the present invention proposes a procedure in which the two fluid phases are made to flow under supercritical conditions in contact with one another, in co-current and typically with a coaxial flow, within a flow system of small dimensions, and where the nature of the flow obtained for various flow rates of the two fluid phases is observed. As a function of the respective flow rates of the two fluid phases, the co-current flow takes place either in the form of a continuous jet of one of the fluid phases within the other (for certain flow rate pairs), or in the form of drops of one of the fluid phases within the other (for the other pairs of flow rates). According to the procedure of the invention, the interfacial tension is determined by establishing at least one limit value of flow rate where the transition between the jet flow and the flow of drop type takes place (jet/drop transition).
More precisely, according to a first aspect the subject of the invention is a method for determining at least one value of interfacial tension between two non-miscible fluid phases, under supercritical conditions, which comprises the following successive steps:
(E1) a first fluid phase, termed the inner phase, is made to flow in a first, so-called inner, flow member with a first flow rate termed D 1 , and a second fluid phase, termed the outer phase, is made to flow in a second, so-called outer, flow member with a second flow rate termed D 2
where the flux of the first fluid phase conveyed by the inner member discharges through an exit of the first flow member into the internal volume of the outer flow member within the flux of the second fluid phase; and the temperature and the pressure in the zone of contact between the first and the second fluid phase are such that at least the first and/or the second fluid phase is in the supercritical state,
whereby, there is formed, downstream of the discharge of the inner flow member into the outer flow member, as a function of the respective values of the flow rates D 1 and D 2 and of their ratio:
EITHER drops of the inner phase in the outer phase; OR a continuous jet of the inner phase in the outer phase;
and then (E2) the flow rate of the inner phase and/or of the outer phase is varied so as to modify the flow profile, namely:
IN THE CASE WHERE THE FLOW RATES D 1 AND D 2 STEP (E1) LEAD TO DROPS OF THE INNER PHASE IN THE OUTER PHASE: the flow rate of the inner phase and/or of the outer phase is modified until the formation of a continuous jet of the inner phase in the outer phase is obtained; and IN THE CASE WHERE THE FLOW RATES D 1 AND D 2 STEP (E1) LEAD TO A JET OF THE INNER PHASE IN THE OUTER PHASE: the flow rate of the inner phase and/or of the outer phase is modified until the formation of drops of the inner phase in the outer phase is obtained;
and a so-called transition pair of values of the flow rates of the inner and outer phases is identified, on the basis of which the modification of the flow profile takes place (from drops to jet or from jet to drops); and then (E3) on the basis of the transition pair identified in step (E2), the value of interfacial tension between the two fluid phases, inner and outer, is calculated;
or else the transition pair obtained in step (E2) is compared with the transition pair for another system of fluid phases in the critical phase determined under the same conditions, whereby a relative indication between the values of interfacial tension of the two systems is obtained.
The two phases placed in presence in the aforementioned steps (E1) and (E2) are non-miscible: this term is understood in its broadest acceptation in the present description, namely that it refers to two fluids suitable for forming, by mixing, a two-phase system under the conditions implemented, and making it possible to observe the jet/drop transition defined hereinabove.
The implementation of steps (E1) to (E3) hereinabove turns out to be particularly easy, and it makes it possible in particular to carry out, at lesser cost and in a reduced time, reliable and reproducible measurements of the interfacial tensions between various fluids under supercritical conditions.
Moreover, in the most general case, the flow devices to be employed in steps (E1) and (E2) exhibit another advantage, namely that of not requiring any particular technical complexity. In particular, although more elaborate embodiments are conceivable, the inner and outer flow members employed according to the invention can typically be reduced to two coaxial cylindrical tubes. Alternatively, it may involve micro- or milli-fluidic chips, advantageously of glass or glass/silicon.
Furthermore, and more fundamentally, steps (E1) and (E2) turn out to be suitable for an implementation within flow devices of small dimensions, typically within coaxial capillary tubes. Thus, the inner and outer flow members employed according to the invention can be two coaxial capillary tubes, thereby making it possible in particular to reduce the quantities of phases placed in presence under supercritical conditions, this being manifested, inter alia, in terms of speed of data acquisition and of decreased risks related to the implementation of supercritical conditions.
According to one interesting embodiment where the possibility of reducing the size of the device is well exploited, the outer diameter of the inner flow member is between 10 micrometers and 2 millimeters, for example between 20 and 200 micrometers. The inner diameter of the outer flow member can for its part advantageously be between 50 micrometers and 4 millimeters, for example between 100 and 500 micrometers, it being understood that, by definition, this inner diameter of the outer flow member remains greater than that of the outer diameter of the inner flow member. The difference between the inner diameter of the outer flow member and outer diameter of the inner flow member remains preferably between 5 micrometers and 2 millimeters, for example between 10 and 500 micrometers, and a ratio of the inner diameter of the outer flow member to the outer diameter of the inner flow member is between 1.1 and 10, preferably between 1.3 and 5.
The nature of the flow members employed according to the invention has to be adapted to the implementation of the supercritical conditions of steps (E1) and (E2). In most cases, and in particular when steps (E1) and (E2) implement CO 2 in the supercritical state, it is possible to use by way of flow members capillary tubes based on fused silica, which make it possible to achieve flows under pressures exceeding 75 bars and typically of up to at least 100 bars or indeed up to 200 bars. Advantageously, according to an embodiment which corresponds to that of the here-appended example, the inner and outer flow members are polyimide-sheathed fused silica capillaries, connected by connection technology elements consisting of PEEK (polyether ethyl ketone) plastic. Particularly well-suited flow members are for example the capillary tubes of the type of those marketed by the company Polymicro Technologies under the name “Flexible Fused silica capillary tubing”.
In particular when the flow devices exhibit reduced dimensions, for example with diameters in the aforementioned ranges, each of the flow rates of the fluid phases within the flow members in steps (E1) and (E2), and in particular each of the flow rates D 1 and D 2 of step (E1) can preferably be between 10 microliters per hour and 1000 ml per hour, preferably between 100 microliters per hour and 100 ml per hour.
In practice, whatever the dimensions of the device employed, the experimental conditions of step (E1) and of step (E2) may advantageously be identical, with the exception of the values of the flow rates of the fluid phases.
According to an interesting embodiment of steps (E1) and (E2), the so-called outer flow rate of the outer fluid phase can be held fixed (at the value D 2 ) in steps (E1) and (E2), whilst solely the so-called inner flow rate of the inner fluid phase is varied in step (E2). Conversely, according to another possible embodiment, it is the inner flow rate which can be held fixed (at the value D 1 ), whilst the outer flow rate is variable in step (E2). Alternatively, according to another conceivable although trickier mode, it is possible to vary the two flow rates jointly, simultaneously or not, in step (E2).
The identification of the nature of the flow in steps (E1) and (E2), namely the existence of drops or of a jet, can typically be carried out by employing an outer flow member which is at least locally transparent for a laser radiation on at least one portion of the outer flow member, said portion being situated downstream of the discharge of the inner flow member into the outer flow member. To identify the nature of the flow, this transparent zone of the flow member is placed between an emitter of said laser radiation and a receiver of said laser radiation (typically a photodiode), thus leading to two types of signals received by the receiver making it possible to distinguish the two types of flow, namely (i) a substantially continuous signal in the case of a jet (the laser beam is permanently crossed by a phase of like type); and (ii) a discontinuous signal in the case of the drops (the laser beam is crossed in succession by drops of the internal phase and then by the external carrier phase between the traversal of each drop).
The determination of the value of the interfacial tension in step (E3) can for its part be carried out according to any suitable procedure adapted on the basis of the knowledge of the pair of transition flow rates which is established in step (E2) and of the physical characteristics of the flow devices employed and of the fluid phases present.
Thus, for example, when steps (E1) and (E2) are carried out with a flow rate of the outer fluid phase fixed at the value of D 2 , the value of the interfacial tension can be established on the basis of the transition flow rate of the inner fluid phase, of the inner diameter of the outer flow member, and of the viscosities of the inner and outer fluid phases, typically by employing the following equation:
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According to an embodiment making it possible to further refine the measurement of the interfacial tension, the value of the interfacial tension between two like fluid phases under the same supercritical conditions can be determined several times in succession, for example by carrying out steps (E1) to (E3) several times at fixed outer flow rate and by varying the inner flow rate in step (E2), and by fixing at each cycle of step (E1) to (E3) a distinct value for the outer flow rate (namely with a flow rate D 2 for the first cycle, a flow rate D′ 2 ≠D 2 for the second cycle, a flow rate D″ 2 also distinct from D 2 and D′ 2 in the case of a third cycle, etc.).
It should be noted that, on account of its great simplicity of implementation, the method of the invention exhibits very great modularity and can be implemented in a very great number of applications. The method makes it possible in particular to carry out with a high acquisition rate successive measurements relating to phases of distinct natures without having to adapt the experimental conditions and the measurement conditions between each of the acquisitions.
In contradistinction to the techniques proposed hitherto, the procedure proposed according to the present invention makes it possible furthermore to determine the value of the interfacial tension of a very great number of pairs of fluid phases, without having to adapt case by case the nature of the analysis to be carried out when the physical or chemical nature of one and/or of the other of the fluid phases is modified. It can moreover be carried out according to a continuous mode and the nature of one and or the other of the two phases can be modified over time during this continuous process, thereby exhibiting a further advantage of the method.
According to a very particular embodiment, the placing in contact of the fluid phases in steps (E1) and (E2) is carried out in the presence of a surfactant. In this case, steps (E1) to (E3) can typically be implemented several times in succession under similar conditions but with variable quantities of surfactant, making it possible to vary the drop formation time, and to determine, on the basis of a curve of the evolution of the interfacial tension value as a function of the drop formation time, a characteristic time of the surfactant, corresponding to the transition between a zone where the interfacial tension value remains substantially constant as a function of the formation time, and an adjacent zone, where this interfacial tension value increases as this formation time decreases.
The method of the invention can be employed to determine the interfacial tension existing between two fluid phases in any physico/chemical method employing a phase in the supercritical state, or else liable to lead in the course of their implementation to supercritical conditions. In this case, the first fluid phase comprises supercritical CO 2 or another fluid in the supercritical state. It can in particular be used to measure the interfacial tension in processes employing CO 2 in the supercritical state or any other supercritical fluid, for example in synthesis reactions carried out in emulsion in supercritical CO 2 ; in methods of extraction using supercritical CO 2 including in particular petroleum recovery methods; or else in methods for capturing and storing CO 2 where the CO 2 is employed in the supercritical state.
According to another aspect, the subject of the present invention is also an installation suitable for the implementation of the aforementioned method comprising steps (E1) to (E3). This installation typically comprises:
an inner flow member and an outer flow member, which are preferably coaxial, the inner flow member discharging into the internal volume of the outer flow member; means for feeding with two fluid phases, respectively in the two flow members, suitable for conditions where one of the phases is in the supercritical state; means for controlling the temperature and pressure within the installation, suitable for bringing at least the internal space of the outer flow member into supercritical conditions of temperature and pressure for at least one of the fluid phases; means for varying the flow rate of at least one of the fluid phases; and means for observing the nature of the flow downstream of the discharge of the inner flow member into the outer flow member.
According to yet another aspect, the subject of the invention is finally a method for screening various pairs of fluid phases, in which these various pairs are prepared, at least one value of interfacial tension relating to each of these pairs is determined, according to the aforementioned steps (E1) to (E3), and at least one preferred pair is identified, from among said several screened pairs.
According to a particular mode of implementation, this mode of screening is employed by conducting steps (E1) and (E2) in succession, under the same conditions, firstly with a first pair of fluid phases, and then for a second pair of fluid phases, and then by comparing in step (E3) the results obtained in the two cases, whereby the two pairs are compared the one with respect to the other.
This screening method is in particular suitable for the implementation of the following variants:
it is possible to prepare the various pairs by adding at least one substance to at least one of the phases, for example a surfactant and/or a polymer and/or a solid particle and/or a mixture of several compounds, for example an oil or crude petroleum; and it is possible to prepare the various pairs by modifying at least one condition of at least one phase, for example its pH.
According to a particular embodiment of the screening method of the invention, at least one of the pairs employed comprises crude petroleum, preferably within supercritical CO 2 .
BRIEF DESCRIPTION OF DRAWINGS
The invention will now be described in greater detail hereinafter, with reference to the appended drawings and to the example hereinafter, where:
FIG. 1 is a side view, illustrating an installation allowing the implementation of a method for determining the interfacial tension between two fluid phases, in accordance with the invention;
FIGS. 2, 4 and 5 are side views, analogous to FIG. 1 , illustrating various steps for implementing this method;
FIG. 3 is a graph, illustrating the variations of the signal of a photodiode as a function of time;
FIG. 6 represents various flow regimes of jet or drop type observed within the framework of the example;
FIG. 7 is a phase diagram obtained within the framework of the example, showing the evolution of the flow regime under the effect of the variation of the flow rates.
FIG. 8 is the side view of FIG. 1 modified to add feeders and controllers.
DETAILED DESCRIPTION OF THE INVENTION
In FIG. 1 , there is illustrated an installation in accordance with the invention, which comprises two flow members, respectively an inner flow member 2 and an outer flow member 4 . In this illustrative example, these flow members 2 and 4 are capillaries, made in particular of fused silica, knowing that other flow members are conceivable.
The two capillaries 2 and 4 illustrated in the figure are coaxial, and thus possess a common main axis, denoted A. Moreover D i refers to the external diameter of the inner capillary 2 , namely that this diameter includes the walls of the capillaries. Furthermore D e denotes the internal diameter of the outer capillary 4 , namely that conversely this value of diameter does not include the walls of this capillary 4 .
In an advantageous manner, D i is between 10 microns (or micrometers) and 2 millimeters, preferably between 10 microns and 200 microns, whilst D e is between 50 microns and 4 millimeters, preferably between 100 microns and 500 microns. Furthermore, the ratio D e /D i is advantageously between 1.1 and 10, preferably between 1.3 and 5.
The discharge of the inner capillary 2 , in the internal volume of the outer capillary 4 , is denoted 2 ′. Immediately downstream of this discharge 2 ′, there is provided a laser emitter 6 , on a first side of the capillary 4 , which is associated with a photodiode 8 , placed opposite this emitter 6 . This emitter and this photodiode are able to deliver a signal, making it possible to obtain information on the formation of drops as well as on the frequency of this formation.
The installation described hereinabove, with reference to FIG. 1 , allows the implementation of a method in accordance with the invention, aimed at determining the interfacial tension between two fluid phases. For this purpose, the capillaries 2 and 4 are placed in communication with means of supply of two non-miscible phases to be tested. These supply means, which are of conventional type, are not represented in the FIGS. 1-5 , but are shown as feeders 10 , 20 in FIG. 8 , wherein feeder 10 is employed with flow controller 12 and temperature and pressure controller 14 and feeder 20 is employed with flow controller 22 and temperature and pressure controller 24 . In a customary manner, this may for example entail syringe plungers and microfluidic connection technologies.
According to a possible embodiment, illustrated in the figures, the outer flow rate, denoted Q e ( 1 ), of the fluid phase (Le) flowing in the outer capillary is fixed. In an advantageous manner, this outer flow rate value is between 10 microliters/hour and 1000 ml/hour, preferably between 100 microliters/hour and 100 ml/hour. Moreover, very low values are given to the inner flow rate, denoted Q i , of the fluid phase (Li) flowing in the inner capillary and to the outer flow rate Q e of the fluid phase (Le) flowing in the outer capillary. Under these conditions, the placing in contact of these two non-miscible fluid phases leads to the formation of drops G which consist of the inner fluid phase, in a carrier phase P formed by the outer fluid phase (see FIG. 2 ).
Next, for this same outer flow rate Q e ( 1 ), the value of the flow rate Q i , is increased progressively according to a predetermined time-dependent function Q i =f(t). The signal emitted by the photodiode is then observed, as a function of time.
At the start of the flow of the two fluid phases, corresponding to the formation of drops, the signal is periodic, namely it oscillates between two values, respectively s 1 and s 2 (see FIG. 3 ). The value s 1 corresponds to the position, in which the laser and the photodiode are separated both by the inner fluid phase and the outer fluid phase ( FIG. 4 ), whilst the signal s 2 corresponds to the position, for which this laser and this photodiode are separated solely by the outer fluid phase ( FIG. 2 ).
Above a certain flow rate value Q i , it is noted that the drops initially produced are replaced by a continuous jet J of the inner fluid phase in the outer fluid phase ( FIG. 5 ). From the moment this threshold value is attained, the signal emitted by the photodiode stabilizes at the value s 1 , since the laser and the photodiode are permanently separated both by the inner fluid phase and by the outer fluid phase.
The instant, denoted t( 1 ), corresponding to the appearance of the continuous jet is identified on the basis of the curve of FIG. 3 . Given that, as seen hereinabove, the variation in flow rate Q i is known as a function of time, it is possible to ascertain the flow rate value Q i ( 1 ) corresponding to this instant t( 1 ) of formation of the jet. Knowing the value of the outer flow rate Q e ( 1 ), as well as the value of the internal flow rate Q i ( 1 ) for which the continuous jet appears, it is possible to deduce therefrom the value of the interfacial tension γ( 1 ) between the two fluid phases.
For this purpose, the following equation is used:
Kax
3
E
(
x
,
λ
)
=
CF
(
x
,
λ
)
where
C
=
5
+
7
18
24
7
-
1
,
E
(
x
,
λ
)
=
-
4
x
+
(
8
-
4
λ
-
1
)
x
3
+
4
(
λ
-
1
-
1
)
x
3
,
F
(
x
,
λ
)
=
x
4
(
4
-
λ
-
1
+
4
ln
(
x
)
)
+
x
6
(
-
8
+
4
λ
-
1
)
+
x
8
(
4
-
3
λ
-
1
-
(
4
-
4
λ
-
1
)
ln
(
x
)
)
,
λ
=
η
i
η
e
,
α
=
(
1
+
λ
-
1
Q
i
Q
e
)
,
and
x
=
2
rj
De
=
α
-
1
λ
-
1
+
α
-
1
.
Solving equation (1) hereinabove makes it possible to ascertain the value of Ka, and then that of γ using the following equation:
Ka
=
Δ
PD
e
2
4
L
γ
,
with
Δ
P
L
=
128
η
e
Q
e
π
D
e
4
(
1
-
x
2
)
the
pressure
gradient
As is apparent from the foregoing, it is possible to deduce this interfacial tension value by knowing solely the values of the fixed outer fluid phase flow rate Qe, of the transition inner fluid phase flow rate Qi, of the diameter De of the outer capillary, as well as of the viscosities η i and η e of the inner and outer fluid phases. This value can therefore be known in a simple and fast manner.
It is possible to repeat the operation described hereinabove, fixing the external flow rate Q e at different values, denoted Q e ( 2 ) to Q 2 (n), each time. This makes it possible to ascertain corresponding values of internal flow rate, denoted Q i ( 2 ) to Q i (n), for which the transition between the drops and the jet takes place. For each group of values Q i (j) and Q e (j), where j varies from 1 to n, it is also possible to deduce n interfacial tension values denoted γ( 1 ) to γ(n). The values of inner flow rate Q i are typically between 10 microliters/hour and 1000 ml/hour, in particular between 100 microliters/hour and 100 ml/hour.
By way of variant, for a fixed outer flow rate, it is possible to choose a very high initial value of inner flow rate, such that the placing in contact of the two fluid phases leads to the formation of a jet.
Thereafter, this inner flow rate value is decreased progressively until drops are obtained. In a manner similar to what was described hereinabove, the inner flow rate sought corresponds to that for which the transition between jet and drops is identified, and not between drops and jet as in the first embodiment illustrated in FIG. 2 .
By way of variant, it is possible to envision fixing, not the outer flow rate, but the inner flow rate so that, in this case, the outer flow rate is then varied. This may be beneficial for reducing the errors in the measurements, in particular by carrying out firstly a first series of measurements with fixed outer flow rate, and then a second series with fixed inner flow rate, for the same fluid phases. It is then possible, in an advantageous manner, to average the values obtained during these two series of measurements.
According to an advantageous variant of the invention, it is possible to carry out a screening of various pairs of fluid phases, by using the method for determining surface tension, such as described hereinabove.
For this purpose, the flow capillaries 2 and 4 are linked up with means for adding at least one substance to at least one fluid phase, and/or with means making it possible to modify the conditions of the flow of at least one of these fluid phases. The adding means make it possible to add, to one and/or the other of the fluid phases, various types of substances such as a surfactant, a polymer, solid particles, salts, acids, or bases or mixtures of one or more substances, for example of crude petroleum or an oil. The means for modifying the flow conditions are for example able to vary the pH, the temperature, or else the pressure.
A pair of so-called base fluid phases is thereafter prepared, whose surface tension is determined in accordance with the method described hereinabove. Next, the base pair is modified, by adding at least one substance to at least one fluid phase, and/or modifying at least one condition of at least one of these base fluid phases.
The various surface tensions, relating to the various fluid phase pairs thus prepared, are then determined. Finally, one or more preferred fluid phase pairs is or are determined, for example those exhibiting the lowest surface tension.
According to the invention, it is possible to measure various values of interfacial tension as a function of the rate of formation of the drops, thereby making it possible to determine the rate of adsorption of a surfactant at the interface between the fluid phases, namely the dynamic interfacial tension. Accordingly, use is made of the installation described previously and a surfactant agent, whose properties it is desired to determine, is introduced into the flowing phases. This surfactant is added, in a customary manner, to one and/or the other of the fluid phases.
An illustrative mode of implementation of the procedure usable to determine the properties of a surfactant according to the invention will now be described in greater detail.
Typically, firstly in a first step, an outer flow rate Q e is fixed at a very low value, denoted Q e ( 1 ), thereby making it possible to ensure that the surfactant has the time required to be adsorbed at the interface between the two fluid phases, and then the inner fluid phase is made to flow at a very low initial flow rate, which is increased progressively according to the scheme described hereinabove. The inner flow rate value, beyond which the drops are transformed into a continuous jet, is denoted Q i ( 1 ). The frequency of formation of these drops is denoted ω 1 which is very small on account of the very low flow rate value Q e ( 1 ). This frequency of formation is measured for example by the laser emitter 6 , associated with the photodiode 8 . Finally, the value γ 1 of the interfacial tension is calculated according to the aforementioned equation, on the basis of the value Q e ( 1 ) and Q i ( 1 ) hereinabove.
In a second step, the outer flow rate is fixed at a value Q e ( 2 ) greater than that Q e ( 1 ) hereinabove. Consequently, the frequency ω 2 of formation of the drops will be greater than that ω 1 , mentioned hereinabove. Next, in a manner analogous to the first step, the flow rate Q i , is made to vary, until a value Q i ( 2 ) is identified corresponding to the transition between the drops and the continuous jet. This makes it possible to obtain a second value of interfacial tension, denoted γ 2 .
These two steps are thereafter repeated, in an iterative manner, for n flow rate values, thereby making it possible to obtain n values of frequency of formation of drops, as well as n values of interfacial tension.
The curve obtained for the variation of the interfacial tension γ as a function of the drop formation time t, which corresponds to the inverse of the frequency ω, typically divides into two main zones, namely:
a first zone I, corresponding to high formation times and consequently to low production frequencies, for which the value of the interfacial tension γ is substantially constant. Stated otherwise, in this portion of curve, the drops form slowly enough to allow the surfactant to be adsorbed at the interface between the two fluid phases. a second zone II, corresponding to higher formation frequencies, namely shorter formation times. As the minimum formation time t n is approached, an increase in the interfacial tension γ is noted. Stated otherwise, the more the drops form at high frequencies, the less time the surfactant has to be adsorbed and, consequently, the more the interfacial tension increases.
At the intersection between the zones I and II, a transition point corresponds to the minimum characteristic time denoted t K , required for the adsorption of the surfactant at the interface between the two fluid phases. Stated otherwise, the time is a value characteristic of the surfactant studied, in the sense that it corresponds to the minimum duration required for this surfactant to be adsorbed at the interface between the two fluid phases.
By using the procedure which has just been described, it is possible to implement a method for screening various surfactant agents. For this purpose, two base non-miscible fluid phases are used, which are made to flow in the capillaries 2 and 4 . Next, various surfactant agents are added to them in succession, whose characteristic times t K are measured, according to the steps described hereinabove. The preferred surfactant agent or agents corresponds or correspond in particular to those whose characteristic times are less than the characteristic times of the application.
The invention will be yet further illustrated hereinafter, in the light of the exemplary embodiment which follows, where the procedure described hereinabove with reference to the figures has been implemented by using as immiscible fluid phases respectively liquid water and CO 2 in the supercritical state (implemented at a pressure of 165 bar (165.10 5 Pa) and at a temperature of 50° C., and as flow members two fused silica coaxial capillary tubes marketed by the company Polymicro Technologies under the name “Flexible Fused silica capillary tubing”, having the following diameters respectively:
outer capillary: inner diameter: 250 microns inner capillary: inner diameter: 100 microns
outer diameter: 150 microns
EXAMPLE
Determination of the Surface Tension in the Presence of Surfactant in a Water/Supercritical CO 2 Mixture
Water and supercritical CO 2 were injected at co-current into the two flow members, under the aforementioned temperature and pressure conditions, while varying their respective flow rates. Supercritical CO 2 was injected through the internal capillary tube, within the liquid water conveyed by the external tube and playing the role of carrier phase.
As a function of the flow rates, various flow regimes are observed, namely a so-called jet regime (or ‘Jetting’), where the supercritical CO 2 flows in the form of a jet on exiting the internal capillary, and a so-called drop regime (or ‘Dripping’), where the CO 2 forms drops on exiting the internal capillary, as illustrated in the appended FIG. 6 .
Note that FIG. 6 is very illustrative of the notion of “drop” regime and “jet” regime such as it is employed in the present description. In this regard, it will be noted that the notion of drop or of jet within the meaning of the present invention is given with reference to the behavior at the level of the exit of the inner flow member. On the basis of the observation of the various regimes obtained, a dynamic phase diagram charting the nature of the regime as a function of the fluxes of the internal phase and of the external phase given as abscissa and as ordinate respectively, as illustrated in the appended FIG. 7 .
Similar measurements were performed with various surfactants added to the medium, which modify the dynamic phase diagram obtained in the absence of surfactant.
A first surfactant employed within this framework was cetyl trimethylammonium bromide (CTAB), added in an amount of 2% by mass to the liquid aqueous phase.
The addition of this surfactant modifies the values of the flow rates leading to the jet/drop transition. The value of the surface tension does in fact decrease on account of the addition of the surfactant.
The procedure of the invention can be obtained so as to establish the complete phase diagram or else solely to determine the flow rates which lead to the transition.
On the basis of these flow rate values, with the aid of the aforementioned equations, it is possible to infer the value of the surface tension.
The procedure of the invention was also used to inter-compare various solvents. For this purpose, it is possible to calculate the value of the surface tension for each of the solvents, but, more simply, within the framework of this example, the same conditions were simply retained while using various surfactants, thereby making it possible, by direct comparison and without calculation, to identify the effect of each of the surfactants employed.
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The invention concerns a method whereby: (E1) an inner liquid phase is made to flow in an inner flow member, and an outer liquid phase in an outer flow member, the flow of the inner liquid phase opening within the flow of the second liquid phase; and the temperature and pressure in the contact area between the first and second liquid phases being such that the first and/or second liquid phase is in the supercritical state, (E2) the flow rate of the inner phase and/or outer phase is varied in such a way as to modify the flow profile, and a torque is identified from values of the flow rates of the inner and outer phases, called transition flow rates, from which the modification in the flow profile occurs (from drops to a jet; or from a jet to drops); (E3) from the transition torque identified in step (E2), the value of the interfacial tension between the two inner and outer liquid phases is calculated, or the result obtained is compared to that obtained for another torque in the conditions of steps (E1) and (E2).
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional application of U.S. patent application Ser. No. 10/501,279, filed Jul. 9, 2004, which is a nationalization of PCT Application Serial No. PCT/GB2003/00072, filed Jan. 10, 2003, which claims priority to United Kingdom Patent Application No. 0200438.0, filed Jan. 10, 2002, which are incorporated herein by specific reference.
BACKGROUND OF THE INVENTION
1. The Field of the Invention
The invention relates to liquid metal electrolyte systems and is especially, though not exclusively, applicable to improving the efficiency and reducing the operating costs of modern-day aluminium reduction cells.
2. The Relevant Technology
The invention will be exemplified, and will subsequently be described and illustrated in this present specification, with reference to aluminium reduction or smelting.
Modern aluminium production plants consume huge amounts of electricity.
Virtually all of them operate by reducing alumina in electrolysis cells or, as they are called, pots. In practise a commercial aluminium smelting plant will consist of several hundred such pots and will operate on a continuous production basis.
There are two remarkable features of this process. First, it has remained virtually unchanged for over a century since it was first successfully developed (and indeed it is still universally known as the Hall-Héroult process after the two scientists who first independently discovered it). Second, the amount of energy consumed by the process is quite staggering.
It has been estimated that the modern-day production of aluminium consumes about two percent of all electricity generated worldwide (!) and yet much of this energy is absorbed in overcoming resistive losses in the poorly conductive highly resistive electrolyte layer of each individual smelting cell. The primary electrical driving current can be of low voltage but must be of relatively enormous amperage in order for the process to work, given these drawbacks, and it follows that any modification which enables that current, the electrolyte thickness, or both, to be reduced at all would indeed produce reductions in energy consumption which could truly be described as significant in relation to those needed without the modification today.
Efforts have been made, naturally, to overcome this problem but the main limiting factor is that, if the electrolyte thickness is reduced beyond a certain critical level, instabilities begin to occur at the interface between the liquid electrolyte and the liquid aluminium. These instabilities, which manifest themselves as a sloshing of the liquids within the cell, have been the subject of intensive research for some 20 years or more. In effect, these are interfacial gravity waves, modified by the external magnetic fields which pervade the cell and when a certain stability threshold is exceeded, these waves can grow by absorbing energy from the ambient electric and magnetic fields.
The good news is that the wave period is measured in minutes and its growth rate in hours, and so the problem ought to be susceptible to some controlled solution. The real problem is that once such a wave takes hold, it can disrupt the electrolysis to such an extent that the cell must be withdrawn from operation. In an extreme case, it could destroy the entire cell.
Previously proposed means for trying to eliminate these instabilities include:
Placing baffles in the aluminium to break up the long-wavelength waves whilst relying on friction to dissipate the short-wavelength components. Have a sloping cathode block so that the aluminium continually drains away. Destroy the standing waves by placing hydraulic energy absorbers at the edges of the cell. Tilt the anode in harmony with the wave so that the electrolyte layer remains almost uniform and thus one eliminates the perturbation in current.
The first of these prior proposals remains simplistically attractive but both it and the second one are limited by the need to find, in practical environments, a material which survives the chemically aggressive environment in a smelting cell. The second option has another difficulty in that thin aluminium layers will not properly wet the cathode and this cannot easily or cheaply be overcome. Whilst the third option is self-explanatory, the most recent research has concentrated on the final one but as far as is known, no practical embodiment has yet emerged.
Furthermore, a paper published by Elsevier Science dated 12 Nov. 2001 by authors A. Lukyanov, G. El and S. Molokov, is deemed to be relevant to the present application as it defines the general background of the mechanism of instability, however primarily in the context of determining the reflection coefficient rather than proposing a practical solution for controlling instability in a cell as is one of the objectives of the present application.
In summary, despite the length of time the problem has been around, and the importance of modern aluminium production to the progress of industrialised society as a whole in an era when, paradoxically, conservation of energy is becoming more urgent than ever, instability of aluminium reduction cells remains the central and unsolved problem in the industry at large.
The Inventive Concept
The applicants are proposing a modification of existing current-driven liquid metal electrolyte systems (of which an aluminium reduction cell is the obvious but not limiting example) which starts from a point quite different from any of those outlined above—but which could, we believe, be used in any appropriate combination with some, all, or any of the prior proposals outlined above.
In essence, we impose on such a system an additional, external, magnetic field whose design and operating parameters are so chosen as to enable the electrolyte thickness to be reduced significantly in relation to those needed without the modification. By doing this, we address the very source of the instability, which happens due to the interaction of the currents induced by the interface motion with the external magnetic field.
Based on our understanding of the fundamental mechanism governing the instability, we believe it to be possible that, with appropriately designed coils, a ring current around the cell inducing an automating magnetic field will stabilise the cell to an appreciable if not total extent.
Thus, rather than trying to understand fully all the processes happening inside the cell we effectively suppress the fluctuations by imposing a suitably powerful and time-dependent magnetic field around it. A modern aluminium (or any other metal) reduction cell is a complex and highly optimised device. There are a multitude of supple physical and chemical processes occurring within such a cell and many of them will inevitably interact. A small change in any one parameter could well have quite unexpected consequences and these may or may not be either inter-related or predictable at all. The size alone of the primary driving current makes it almost impractical to try to make relatively small adjustments to any one aspect of cell operation—for example, the “anode-tilt” approach exemplified in the fourth prior proposal outlined previously—with any real guarantee of even partial success.
We by contrast take an overview and we believe that, with appropriate design and with the ability to adjust the controlling parameters (i.e. field amplitude, frequency, and constant background) we are more likely to achieve real suppression of instability in a practical format within the foreseeable future.
In a subsidiary aspect, the magnetic field applied is essentially a vertical magnetic field. In this direction, significant effect on instability in liquid metal electrolyte occurs which allows the thickness of electrolyte itself to be reduced below levels at which conventionally instability would occur.
In a further subsidiary aspect, the magnetic field is dependent on an amplitude and frequency whose values are approximated through wave reflection analysis on an infinite wall. This is advantageous as it allows an appropriate magnetic field to be rapidly determined rather than relying on the skilled man to determine an adequate field through more extensive analysis.
BRIEF DESCRIPTION OF THE DRAWINGS
Various embodiments of the present invention will now be discussed with reference to the appended drawings. It is appreciated that these drawings depict only typical embodiments of the invention and are therefore not to be considered limiting of its scope.
FIG. 1 shows diagrammatically an example of a modern Hall-Héroult cell;
FIG. 2 presents the electrolysis zone of the cell schematically;
FIG. 3 shows graphically the existing and the modified instability levels occurring in respectively an unmodified and a modified cell in accordance with the invention; and
FIG. 4 shows, again in schematic form, one possible set-up embodying the invention.
FIG. 5 shows, a schematic diagram of a two-layer system.
FIG. 6 shows, a schematic diagram of wave reflection on an infinite plane wall.
FIG. 7 shows graphically the amplitude of interfacial wave for two electrolyte thicknesses when no alternating field is applied.
FIG. 8 shows graphically the amplitude of interfacial wave for a reduced electrolyte thickness cell with and without the alternating magnetic field.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
An example of a modern Hall-Héroult cell generally referenced 1 is shown in FIG. 1 . Cell 1 comprises covers 2 , carbon anodes 3 , molten salt electrolyte 4 , molten aluminium 5 , collector bars 6 , carbon lining 7 and a carbon bus 8 . All of these components may be of standard kind, modified or substituted if necessary by other relevant components or groups of components by the person skilled in the art without any recourse to inventive thought.
The current used in the electrolysis enters the electrolyte zone vertically through the anode and is collected by the cathode at the bottom. The thickness of both layers, electrolyte and aluminium, is very small in comparison with the horizontal dimensions. Schematically, the electrolysis zone can be presented as shown in FIG. 2 .
The major part of the consumed energy is wasted in the form of resistive losses in the poorly conductive electrolyte, layer 2 in FIG. 2 . But, when the depth of electrolyte is reduced below some critical level or the current exceeds some critical value, the cell becomes unstable. In other words, the waves at the interface between the two liquids start growing. The increment of the resulting instability is shown in FIG. 3 (curve 1 ).
It is proposed to apply an external, alternating magnetic field and to regulate the currents induced by this field so as to control or even suppress instability. The sketch of a possible set-up is shown in FIG. 4 . In this figure a ring current around the cell induces an alternating magnetic field. In practice, the alternating magnetic field may be created, for example, by coils surrounding the cell or other means carefully selected by the person skilled in the art. The result of simulations for the circular cell, which exemplifies the most unstable case, is presented by curve 2 in FIG. 3 . One can see that the instability disappears. Analysis of a more realistic, rectangular cell shows that the method works successfully in this case as well ( FIG. 8 ). It is believed that the method may be adapted by the person skilled in the art for any cell geometry.
Description of the Underlying Theory and Exemplary Results
In the following description, flow stabilization by an alternating magnetic field is presented, and the effect of suppression of instabilities is demonstrated on an example of a two-layer system in a rectangular geometry.
A) Mathematical Model of the MHD-Modified Interfacial Gravity Wave Dynamics in a Closed Domain
Consider the system of two electrically conducting liquids (liquid metal and electrolyte) carrying electric current of density J and exposed to a magnetic field B presented in FIG. 5 .
In the equilibrium state,
J=J 0 =(0,0,− J 0 ), B =( B ox, B oy, B oz ), ∇×[ J o ×B o ]=0. (1)
Here (x,y,z) are Cartesian co-ordinates. The last relationship implies that the vertical component of the magnetic field B 0z can be arbitrary (given by the external circuit).
Let the thickness of the liquid metal layer in the equilibrium state be H 1 and that of the electrolyte be H 2 . Any deviation of the interface from the equilibrium state (which is inevitably present in a real cell) induces the redistribution of the current (and, consequently, of the magnetic field). This process is accompanied by the wave motion of the two-layer liquid system. In the absence of the electric current, the system is stable (the amplitude of the initial perturbation of the interface does not grow in the process of the wave propagation). Eventually, because of the natural dissipation in the system, the wave would fade out. In contrast, when the current is on, interaction of the current perturbation with the external magnetic field can enhance the wave motion and lead to the uncontrolled growth of the interfacial wave amplitude.
The dynamics of the two-layer system is governed by the following equations:
ρ i [ ∂ u i ∂ t + ( u i · ∇ ) u i ] + ∇ ( P i + ρ i gz ) = F i - D i ( 2 a ) ∇ · u i = 0 , ∇ · J i = 0 , ∇ · B = 0 , ( 2 b - d )
where i=1, 2 is the layer number of FIG. 5 ; ρ i is the density; u i is the fluid velocity, P i is the hydrodynamic pressure, J i is the electric current density in the layer (which includes variations induced by the wave motion), B is the total magnetic field (which includes the field induced by the external circuit), t is time, F i =J i ×B is the Lorentz force, D i is dissipation describing energy losses in the layer. The dissipation term is taken in the conventional form for shallow-water equations, i.e. D i =ν i u i , where ν i is the dissipation coefficient.
The boundary conditions for the two-layer liquid system placed into the poorly conducting bath are:
( u i ·n ) bath =0; (3)
( J 1,2 ·n ) sidewalls =0; ( J 1 ·n ) bottom =−J 0 ; ( J 1 ·n−J 2 ·n ) interface =0, (4a-c)
where n is the unit vector normal to a particular surface.
The current boundary conditions (4) imply the following ranking of conductivities: σ sidewalls σ 2 σ bottom σ 1 , which is characteristic for industrial aluminium reduction cells (typically, σ 1 =3.3·10 6 (Om·m) −1 , σ 2 =200 (Om·m) −1, , σ bottom =2.10 4 (Om·m) −1, , σ sidewalls ≈0).
The system of Equations (2), together with the boundary conditions (3), (4) fully defines the motion of the two-layer system.
In the following, the deviation of the interface z=h(x,y,t) from the equilibrium state at z=0 will be discussed. The system of governing equations (2) can be significantly simplified if two small parameters are introduced as suggested by the actual physical and engineering conditions in the aluminium reduction cells, i.e.
ε=H 1 /L<<1, the shallow water parameter. Here L is the horizontal dimension of the cell. Typically, ε∝0.01. δ=max h/H 1 <<1, where max h is the amplitude of the interfacial wave. That means that we are interested in the dynamics of the small-amplitude perturbations, which is perfect for the stability analysis.
Implementation of these two parameters means that to the first order in δ the motion of interface is essentially two-dimensional and the following relationships are valid:
u i ( x,y,z,t )≈δν i ( x,y,t ), h ( x,y,z,t )≈δη( x,y,t ), F i ( x,y,z,t )≈δ f i ( x,y,t ), (5)
where ν i , η, f i are new, unknown, O(1) functions. These are the normalised velocity, and the perturbations of the interface and the Lorentz force, respectively.
Taking into account the shallow-water, small amplitude approximation (5), the analysis of the original equations (2)-(4) shows that to the first order in δ the following conclusions can be made:
the current perturbation induced by the interface motion is horizontal, i.e. J≈J 0 +j (x,y,t) (here and elsewhere subscript || denotes a component of a vector in the (x,y)-plane), the Lorentz force acting on the liquid metal depends only on the vertical component of the external magnetic field: f 1 ≈j×B 0Z , The Lorentz force acting on electrolyte is much less than that on the liquid metal, i.e. |f 2 f 1 |.
As a result, one can conclude that by controlling the vertical component of the magnetic field B 0Z (which is given by the external circuit) it may be possible to control the force inducing the unstable motion of the interface. One such a possibility is to superpose a certain alternating magnetic field onto the external, stationary field.
Therefore, the following form of the vertical component of the field is considered:
B oz =B o b ( x,y,t ),
where B 0Z is a constant, while function b(x, y, t) can be arbitrary. In previous studies, the magnetic field has been supposed to be stationary (i.e. independent on time) and fixed.
Under all assumptions made above the system governing motion of the interface assumes the form
∂ 2 η ∂ t 2 - c 2 ∇ 2 η = c 2 ∇ ϕ · [ ∇ × b ( x , y , t ) e z ] - v 1 ∂ η ∂ t , ( 6 ) ∇ 2 ϕ = - β η . ( 7 )
Here
∇ ≡ e x ∂ ∂ x + e y ∂ ∂ y ; c = ( ρ 1 - ρ 2 ) g [ ρ 1 / H 1 + ρ 2 / H 2 ] - 1
is the speed of the interfacial gravity waves in the absence of the external magnetic field, φ(x,y,t)=σ 1 B 0 g −1 (ρ 1 −ρ 2 ) −1 φ(x,y,t) is the normalised electric potential (i.e. j || =−σ 1 ∇φ), and β=J 0 B 0 /[H 1 H 2 (ρ 1 −ρ 2 )g].
It should be noted that natural dissipation in the cells plays crucial role in the stability of the existent set-ups. Typical value of the non-dimensional parameter β in this case is ˜20. Without dissipation the stable operation is only possible for small values of β≈1 which are totally impractical.
The boundary conditions (3), (4) yield:
∂ ϕ ∂ n = 0 , ∂ η ∂ n = - b ( x , y , t ) ∂ ϕ ∂ τ at Γ ( 8 a , b )
Here the function Γ(x, y)=0 defines the shape of the boundary (horizontal geometry of the cell); ∂/∂n and ∂/∂τ stand for normal and tangential derivatives to Γ=0, respectively.
Analysis of the system of Equations (6)-(8) by the skilled man in the art in the simplest case, when b≡1 (uniform, constant magnetic field), has revealed the mechanism underlying the interfacial instability. Essentially, it has been shown that the instability (if it occurs) is inspired at the boundaries of the cell by the wave reflection with the reflection coefficient greater than 1. Earlier studies missed this very point of the instability mechanism for a uniform external magnetic field. For this type of fields the first term in the right-hand side of Equation (6) vanishes, and Equation (6) becomes essentially decoupled from Equation (7). It is the boundary condition (8b) that is responsible for the development of the instability. And here is the remedy: there is an arbitrary function b(x, y, t), which is essentially the externally applied magnetic field, in this boundary condition.
Derivation from this underlying theory enables the preferred inventive external magnetic field b(x, y, t) to be found which leads to the attenuation or even suppression of instability.
Below results are presented for the simplest case of spatially uniform alternating magnetic field
b= 1 +b 0 cos(ω 0 t+θ 0 ) (9)
Here b 0 is the normalised amplitude, ω 0 is the frequency, and θ 0 is the initial phase of the controlling external magnetic field which is to be obtained.
For a realistic geometry of the cell the problem defined by Equations (6)-(8) must be solved numerically. For calculations in the specific case of a rectangular cell as presented hereafter, second order central differences may be used throughout. Equation (6) may be discredited using an explicit scheme in time. A fast Poisson solver may be used to solve Equation (7).
For calculations 32 points per unit length may be used. The scheme has been successfully tested on several benchmark problems to ensure both high accuracy and the absence of numerical dispersion. Other methods of determining advantageous magnetic field types may be employed and will be selected by the person skilled in the art from known alternatives.
An approximation for parameters b 0 and ω 0 can be advantageously obtained from the corresponding problem of a reflection from an infinite plane wall (see Sec. B). Starting from these initial estimates the frequency and the amplitude are either increased or decreased to minimize the increment of instability. The parameters are adjusted iteratively until stability of the interface is achieved.
B) Approximate Determination of the Amplitude and Frequency of the External Magnetic Field: Reflection From the Infinite Plane Wall
One example of reflection analysis from an infinite plane wall is presented in this section.
Both the amplitude and frequency of the controlling parameters of the external magnetic field are estimated using the simplest model of the reflection of the plane wave from the infinite boundary in the absence of dissipation as shown in FIG. 6 .
In a previous study of this kind where b was assumed ≡1, the reflection coefficient μ was found to be greater than 1 for some angles of incidence. In other words, the wave was being amplified at the boundary. It is clear that in the presence of the alternating magnetic field b(t) given by Equation (9) one obtains μ=μ(b 0 ,ω 0 ). Now we are going to find such controlling parameters b 0 and ω 0 that the reflection coefficient μ≦1. To achieve this it is convenient to represent the problem of the reflection of the plane wave from the wall in the form of the integral equation for the y-Fourier component of η(x, y, t).
The dependent variables in the reflection problem are represented in the form
η={tilde over (η)}( x,t )exp( ik y y ), φ={tilde over (φ)}( x,t )exp ( ik y y ),
where k y is the wave number of the incident wave.
The Fourier-transform with respect to x leads to the following integral equation for the function {tilde over (η)}(x,t) at the boundary:
x
=
0
:
∂
η
~
∂
x
=
-
ⅈ
b
(
t
)
∫
-
∞
0
η
~
(
x
′
,
t
)
exp
(
k
y
x
′
)
ⅆ
x
′
(
10
)
while function {tilde over (η)}(x,t) satisfies equation
∂ 2 η ~ ∂ t 2 - c 2 ∂ 2 η ~ ∂ x 2 + k y 2 c 2 η ~ = 0. ( 11 )
Applying further the Fourier transform over t i.e. {tilde over (η)}(x,t)=∫η ω exp(−iωt)dω, gives the solution of Eq. (11) as follows:
η ω =C 1 (ω)exp( ik x x )+ C 2 (ω)exp(− ik x x ), (12)
where
k x = ω 2 / c 2 - k y 2 ,
and C 1 (ω), C 2 (ω) are spectral powers of incident and reflected waves. Substituting Equation (12) into Equation (10) yields a functional equation, which links spectral powers of the reflected wave and the incident one, namely
k
x
(
ω
)
{
C
1
(
ω
)
-
C
2
(
ω
)
}
+
{
C
1
(
ω
)
k
y
+
ⅈ
k
x
(
ω
)
+
C
2
(
ω
)
k
y
-
ⅈ
k
x
(
ω
)
}
+
b
0
{
C
1
(
ω
±
ω
0
)
k
y
+
ⅈ
k
x
(
ω
±
ω
0
)
+
C
2
(
ω
±
ω
0
)
k
y
-
ⅈ
k
x
(
ω
±
ω
0
)
}
=
0.
(
13
)
Equation (13) can be solved iteratively assuming the spectral power of the incident wave is given, for instance C 1 (ω)=1. This gives the values of b 0 and ω 0 , which can be used as a starting point in our analysis of the instability in the rectangular cell with dissipation. Further, these parameters must be tuned using developed numerical code to achieve stability.
It is worth noting that Equation (10) can be used to solve a more general, inverse problem. That is, if one prescribes the spectral power of both the incident and the reflected waves, then one can obtain necessary time dependence of the controlling magnetic field b(t) rather than assuming any parametric form of the type (9) a priori.
C) Control of Instability in a Rectangular Cell
The stabilizing effect of an alternating magnetic field in a rectangular cell will be demonstrated on the following example. Let the geometrical parameters of the cell be: the length L 1 =9.8 m, the width L 2 =3.4 m, the thickness of electrolyte layer H 2 =5 cm and the thickness of aluminium layer H 1 =5 cm. The total current passing through the cell is I c =175 kA. The constant external magnetic field has been taken to be B 0 =3.10 −3 T. These conditions correspond to a stable process of the aluminium production, which is confirmed by computer simulations and corresponds to horizontal curve in FIG. 7 .
If one reduces the thickness of electrolyte layer by 5%, i.e. H 2 =4.75, the cell becomes very unstable. Such resulting instability is shown in the growing curve of FIG. 7 . As is seen, the growth rate is rather significant and after 30 minutes short-circuits occur.
FIG. 8 shows a stabilized cell with reduced thickness of an aluminium layer by an alternating field.
Operation of the cell with the same (reduced) electrolyte layer thickness but with application of an alternating magnetic field is given by Equation (9) where b 0 =0.66, ω 0 =20 rad.sec −1 , θ 0 =0 is shown in FIG. 8 .
The proper frequency ω 0 and the amplitude b 0 have been found according to our method described in section B) and tuned to achieve stability. Starting values were not far away from those that give stable operation, i.e b 0 approx ≈1.66, ω 0 approx ≈40 rad·sec −1 . Note that b 0 is normalised with B 0 =3.10 −3 T.
As a result the cell becomes stable as FIG. 8 shows. As will be shown in the following section, this result is particularly encouraging in terms of actual energy savings.
D) Reduction of the Energy Consumption
Let's calculate energy losses in the electrolyte layer per one millimeter under the parameters listed above. The conductivity of molten electrolyte is σ c =200 (Om·m) -1 . Then in each millimeter of the electrolyte layer (ΔL=1 mm) energy losses due to Joule dissipation are: W e =I c 2 ΔL/(σ e L 1 L 2 )=4.6 kWatt. Since the inventive magnetic field application has permitted the electrolyte layer's thickness of being reduced by W e =I c 2 ΔL/(σ e L 1 L 2 )=4.6 kWatt ΔH 2 =2.5 mm, it follows that the electric energy consumption may be reduced by ΔW e =11.5 kWatt. On the other hand, to create the stabilising external, alternating magnetic field by a coil, one needs to spend no more than W s =57 Watt, provided the coil has 300 loops of copper wire of 0.5 cm in diameter.
So, the ratio is just W s /ΔW e =0.5%. That is, the energy expenses for the production of the controlling magnetic field are very small in comparison with the resulting savings.
Two-layer systems carrying electric current in the presence of a magnetic field can be stabilized by the application of an external alternating magnetic field. Calculations for a typical geometry of an industrial aluminium reduction cell in the presence of a uniform field show that the energy losses required for stabilization are minimal.
Similar calculations may be performed for cells of various shapes and even for spatially non-uniform magnetic fields. The person skilled in the art will adapt the preceding broad underlying theory for each specific case while the current scope of the invention is defined in the claims which now follow.
|
A method of stabilizing an electrolysis cell with a boundary, a liquid metal layer and an electrolyte layer having specific operational and geometric parameters, and comprises the steps of determining amplitude and frequency values for a desired external, time-varying and/or alternating magnetic field through wave reflection analysis on a theoretical wall whose parameters are representative of the cell wall's parameters; and imposing on said cell an external, time-varying and/or alternating magnetic field having substantially the same amplitude and frequency values determined in the wave reflection analysis so that the resultant magnetic field imposed on the cell tends to parametrically and dynamically desynchronize the occurrence of resonance instability near the cell's walls.
| 2
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a method for excavation from the top down, usually known as "undercut". More particularly the invention relates to an undercut excavation method using posts which are adapted to support concrete floors that become a roof for the next lower cut or excavation level.
2. Discussion of the Prior Art
The excavation method of the present invention is particularly well suited to excavation of material having poor structural cohesion, such as overburden tills below proposed highrise buildings or of badly fractured or unstable mine rock. The so called "undercut-and-fill" mining method is especially well adapted for the purposes of the present invention. There are many descriptions of the conventional undercut-and-fill mining method in the mining literature, however, probably one of the best is to be found in the article entitled: "Undercut-and-Fill Mining at the Frood-Stobie Mine of the International Nickel Company of Canada, Limited" by J. A. Pigott and R. J. Hall published in The Canadian Mining and Metallurgical Bulletin for June, 1961, Montreal, pp. 420-424.
It is also already known to mine ore by an undercut-and-fill method while providing concrete floors that serve as a roof for the subsequent cut on a lower level. For example, in an article entitled "Kosaka Mine and Smelter" published in the Mining Magazine--November 1984, page 404, a method called underhand cut and fill using an "artificial roof" is disclosed. According to this method, the cross-cuts are back-filled by first installing a layer of reinforcing steel mesh near the floor, followed by pumping in a 500-600 mm thickness of a comparatively weak concrete mix and, when it is dry, backfilling with a mixture of sand, volcano ash and 3.5% cement. When alternate cross-cuts have been completed across the length of the mining block, the intermediate 4 meter wide ribs of ore are also extracted, so that the entire slice of ore is replaced by a continuous layer of reinforced concrete topped by loosely cemented fill. Then, when mining of the next lower cut is undertaken, the concrete which has been placed on the floor of the level above, now forms an artificial roof. However, because of such ground conditions, timber sets are installed at 1 meter intervals under such artificial roof to support the same when excavating the lower cut.
The main problem with the above method is that when mining is carried out under the artificial concrete roof, initially there is no support provided for this roof, and until such support is provided by means of timber sets that are needed at intervals as close as 1 meter apart, workers are exposed to safety hazards from potential fall of the roof and of materials above such roof during the temporary periods of unsupport. Another problem is the requirement of providing supporting timber sets at 1 meter intervals. Due to this, the excavated work area becomes congested with supports, thus restricting the excavation rate to small equipment with limited movement, at high unit cost. Also, short ramps (two meters or less) are required to prevent damage to posts and to limit the unsupported spans.
The cost component is an important consideration in mining operations and can dictate the economic viability of several known ore bodies which are presently considered for mining by the undercut-and-fill method. The novel method of the present invention, which lends itself to an efficient, high productivity mechanized excavation will be particularly suitable for such ore bodies.
In the area of civil engineering, the excavation from the top down is presently carried out with the use of sheet piles at great cost. The method of the present invention will again provide a relatively inexpensive and entirely viable replacement for such known practice.
SUMMARY OF THE INVENTION
It is, therefore, an object of the present invention to provide an improved excavating method which is safer, more productive and readily adaptable to mechanization. Another object of the invention is an undercut or undercut-and-fill mining method which is particularly suitable for fractured or unstable rock or for recovering crown or sill pillars and pillars left between cut-and-fill stopes, and entire higher grade ore bodies. Another object is to provide a mining method which gives essentially 100% ore recovery in one pass and allows mining in any desired direction on each lift. Further objects and advantages of the invention will become evident to those skilled in the art from the following description of the invention.
The excavation method of the present invention essentially comprises inserting posts into the ground, pouring a concrete floor on said ground to be supported by said posts, and excavating beneath said concrete floor which now serves as a roof. The posts can be inserted into the ground by any desired means. For example, holes of predetermined size and length can be drilled in the ground and then posts which, for example, can be made of concrete, may be inserted into the holes and positioned therein so as to support the concrete floor that will be poured onto the ground. Alternatively, steel posts could be driven into the ground to a predetermined depth and positioned in a predetermined pattern to provide a support for a concrete floor of a size and shape required for the excavation thereunder.
Then, once the excavation on one elevation level is completed, new posts are inserted into the ground of said first excavation and a concrete floor is poured on said ground to be supported by said new posts and then excavation is continued on a new lower level under said concrete floor which now serves as a roof for the new lower excavation level. In a preferred embodiment, the new posts that are inserted into the ground on the first excavation level are positioned in plan beside the posts that were previously inserted into the ground at the higher level and additional posts are installed on top of the new posts, extending up to and engaging the concrete roof over the first excavation to provide further support for the said roof. Then, when the new concrete floor is poured after installing the new posts, the concrete ties the ends of all these posts when it solidifies and provides a system of double-post support for the concrete roof.
Thus, in a preferred embodiment of the invention there is provided an efficient method of multilevel undercut excavation which comprises:
(a) drilling holes of a predetermined size and length into the ground under which excavation is to take place;
(b) inserting posts in said holes;
(c) pouring a concrete floor onto said ground to be supported by said posts and allowing the concrete to solidify;
(d) excavating beneath the concrete floor which now serves as a roof for the excavation at the lower level;
(e) drilling holes again into the ground at the lower level so excavated and inserting posts in said holes;
(f) installing additional posts on top of the posts inserted at the lower level, extending up to and engaging the concrete roof to provide further support for said roof;
(g) pouring a concrete floor onto the ground of said lower level and allowing the concrete to solidify, thereby tying the ends of the posts; and
(h) continuing downward excavation in this manner from level to level until the desired number of levels has been excavated.
Again, in the preferred embodiment of the invention the additional posts inserted in the holes on each lower level, are installed beside the posts already supporting the concrete roof at that level, so as to facilitate tying the ends of all these posts together with concrete when it is poured to form the new floor. Preferably all the posts are made of reinforced concrete, however, one could use a variety of posts, for example, the posts which are inserted into the holes could be made of concrete whereas additional supporting posts could be made of timber or steel. Preferably reinforced concrete is also used for the floors/roofs formed during the excavation, which allows positioning the posts at greater grid spaced distances and provides greater space for excavation beneath such floors.
The above described excavation method can be advantageously used for civil engineering excavations or for undercut mining. In the latter case it is also desirable to drill small (e.g. 5 cm) "helper" holes around the posts and blast the same to pre-break ore around the posts. This also de-stresses the area and facilitates further undercut excavation. Also concrete reinforcing means are preferably provided. For example, rebar and screen are laid on top of a layer (e.g. 200-300 mm) of broken ore before pouring the concrete. Rebar and screen are also extended vertically between and around the posts so that the inserted post cannot punch the concrete floor or alternatively the concrete floor cannot slide down the post without shearing off the rebar, screen and concrete.
Also, in mining operations, the present invention provides a particularly advantageous undercut-and-fill method, which comprises:
(a) cutting initial drifts in an underground mine to form rooms in a conventional manner and recovering the mined material from said rooms;
(b) drilling holes of a predetermined size and length in the sill of each room and inserting posts in said holes;
(c) pouring a concrete floor in said rooms to be supported by said posts;
(d) back-filling the rooms with a suitable fill;
(e) once a complete lift is so mined, repeating this mining procedure on a lower level where the concrete floor now serves as a roof supported by the said posts; and
(f) continuing mining in this manner from level to level in the downward direction until the ore body is mined.
Again in a preferred embodiment, additional posts are installed at each level under the first level, between the concrete floor of said level and the concrete roof of the preceding level, to provide further support for said roof. These additional posts are preferably installed in plumb on top of the posts inserted into holes drilled into the sill of each mine level under the concrete roof formed above, so that when the new concrete floor is poured, it ties the ends of all these posts. Also, preferably, the additional posts are positioned adjacent to the original posts supported by the concrete roof so as to facilitate tying them all together and provide a double-post system for supporting the concrete roof at each level.
The holes are drilled in the sill at predetermined grid spaced intervals and the post grid spacing as well as floor post concrete tie-in is so engineered as to provide a safe and economical mining operation. Also, the floor is suitably designed with rebars and screen within the concrete, so that the additional post which engages the roof cannot puncture the same. Again, at least some of the posts and even all the posts could be made of reinforced concrete although some could be made of steel or timber or similar materials.
The actual undercutting is usually done by the drill and blast method, although, again, other excavation methods could be used depending on the ore being mined. If mining is done in a soft ore, such as coal or potash or the like, where mechanized excavation systems are currently used, the method of this invention can readily be adapted to such mechanized methods. In harder rock, normally drill and blast techniques are employed and again the present method is suitable to be used therewith. As previously described with reference to the undercut mining, small blast holes can be drilled around the previously inserted concrete posts in such a way that the blast would break the ore around the posts prior to pouring the concrete floors and also de-stress the ground below, but without producing substantial damage to the posts. Such de-stressing removes the danger of rock burst which often occurs in highly stressed rock formations. Additional de-stress holes may be drilled in the walks or even further below the rooms being excavated, if required.
The method in accordance with the present invention produces in a single pass essentially 100% extraction of the ore from the mined areas where only the posts are left as pillars before the empty rooms are back-filled with a suitable filling material. The second post, as already mentioned, is preferably positioned adjacent to the first post in plumb on top of the post on the level below and tightly fitted under the post on the level above. In this manner, this second post which is never subjected to blasting damage, provides a solid support for the concrete roof above and the back-filled room over said roof. It reinforces the entire system and allows a safe and stable mining operation. However, if required due to some specific ground conditions, additional posts could be placed within the system at different levels to provide even greater support for the roof. For additional safety, the concrete posts can be provided with stress monitoring devices, so that loading on these posts can be monitored by mining crews and unexpected loads can be identified and supported by additional posts, if required.
For a typical mining environment, one can design a 0.2-0.3 m concrete floor suitably reinforced with rebar and mesh, being supported by 0.5 m diameter reinforced concrete posts on an 8 m by 8 m grid pattern for a 5 m cut. However, this typical design is by no means limitative and other suitable designs can be provided. In this regard, the novel method is very flexible and adaptable to any given mining environment and rock formation.
It should be noted that the initial posts are capable of supporting the roof on their own, allowing a number of rooms to be excavated simultaneously. As excavation continues, at each succeeding cut one will install the posts in holes bored in plumb aside the posts from the preceding lift. Additional posts will then be raised above these posts up to the roof. Each additional precast post so raised, in effect, more than doubles the factor of safety since it will never be subjected to blasting or other excavation abuse. Pouring of successive reinforced concrete floors will tie all these posts together and improve the overall strength. A suitable layer of broken ore can be left on the sill prior to pouring the concrete floor; this helps prevent blast damage to the concrete floor when mining proceeds under the floor which has become a roof. Also individual concrete pours are normally tied together with rebars and screens to form a continuous concrete floor slab tying together the various posts.
Advancing down vertically from cut to cut may be accomplished by progressively increasing the height of an access cut corridor and providing a ramp to the lower cut elevation. Ultimate design and spacing of the double post grid will depend on horizontal and vertical pressures exerted by the materials being excavated as well as the weight of the several floors formed on the upper excavated levels, including the backfilled material supported thereby. Also, the concrete floors must be designed to transmit these pressures to the posts taking into account the friction and shear effects of the fill and the concrete floors.
The excavation rate of the undercut-and-fill method of the present invention is very high. Volumes as large as 320 cubic meters per shift can be excavated in any one direction beneath the concrete floor. The method is also very flexible in allowing excavation or filling at several working places at once. Each trend can open up three rooms for excavation, left, right, and straight ahead, allowing for greater flexibility than traditional methods which can proceed only in a straight line. Such spacious design, allows for excavation to be mechanized using loaders, scooptrams and drill jumbos for quick and efficient operation. Mining functions, such as drilling, loading of blast holes, mucking of broken material, drilling post holes, pouring concrete floors, etc. can all be spaced out to optimize the excavation cycles.
Such a method is dramatically more economic than conventional undercut-and-fill mining method mainly because of its continuous work cycle. There are minimum work interruptions because numerous rooms can be opened up as the concrete posts are designed to support a large open area. There is also no need for the usual roof support means such as screens, rock bolts and the like.
Safety is also enhanced as personnel are never exposed to falls of material.
The method is also very cost effective for civil engineering excavation purposes. Supports during excavation become temporary or permanent floors and pillars depending on the design requirements. The method is particularly suitable for excavating underground parkades for multi story basement highrises where other techniques are not very suitable.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be described, by way of example, with reference to the accompanying drawings in which:
FIG. 1 is a perspective view of an excavation according to the method of the present invention;
FIG. 2 is a plan view of the same excavation showing the positioning of the posts;
FIG. 3 is a section view of such excavation;
FIG. 4 is a side view of a two-drift mining section showing the positioning of the post holes and of the "helper" or blast holes;
FIG. 5 is a side section view of the same arrangement showing the blasting around the posts and the two-drift sections filled;
FIG. 6 is a plan view of a grid of post undercut mining level with a ramp from one level to the other;
FIG. 7 is a section view of the same grid; and
FIG. 8 is a section view of undercut post mining section with a raise bore for supplying various equipment.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the drawings, in FIG. 1 ground 10 represents any surface from which the excavation according to the present invention proceeds in the downward direction. In this ground 10, which can be on the surface of the earth or in an underground mine, holes such as hole 12 are drilled using, for example, Ingersol Rand's DTH drills, cluster drills or rotary drills. For example, 0.5 m diameter and 5 m deep holes would be drilled at a distance of 8 meters from one another in the longitudinal direction L and in width W and concrete posts 14 of about 0.45 m diameter and approximately 5 m in length would be inserted into said holes. These concrete posts are preferably made of reinforced concrete using rebars or the like as reinforcing elements. Once this is accomplished, a concrete floor 16, having a thickness 0.2-0.3 m, is poured on the ground which is preferably provided with a layer of broken rock or ore. The concrete is also preferably reinforced with screens and rebars as is known in the art to give it greater strength.
Once the concrete floor has solidified, excavation proceeds thereunder, for example, in the direction of arrow E. This excavation can be done by any suitable means and it will be obvious that during such excavation the floor 16 will serve as a solid roof for the excavated space thereunder. In such manner, excavation at level A can proceed safely and efficiently. Also the 8 m×8 m spacings allow for heavy excavation machinery to be used such as LHDs for mucking, 15 ton trucks to truck ore or dump fill, a single or double boom hydraulic jumbo for drilling, a boom truck for mechanized post handling and so on.
As the excavation at level A proceeds, further holes are drilled of the same size and height as holes 12. In plan these holes are drilled off-plumb and immediately adjacent to the existing concrete posts 14. Then concrete posts 24 are inserted into said holes. Again these posts 24 are identical to posts 14, previously inserted into the ground at level A. On top of posts 24, additional posts 18, shown in broken lines, are stood-up and blocked between the ground 20 of level A and the floor/roof 16. These filler posts 18 are similar to posts 14 and 24 but slightly shorter in length so that they can tightly fit between the top of post 24 and the floor/roof 16 and provide extra support for the floor/roof 16. Once all these posts 14, 18 and 24 are properly positioned and secured, concrete floor 26 is poured to tie-in the posts at the bottom 20, thus solidifying the entire structure. Rebar and screen is preferably installed between the various posts to provide further reinforcement when the concrete is poured.
Once level A is thus excavated or mined, it may be back-filled with appropriate filling material. For example a 5% cement-rock fill could be used. Since according to the present invention several rooms can be opened at a time, the pouring of concrete floors, drilling of holes, placing of posts and back-filling of rooms will not slow down the drill-blast-muck-fill cycles of the mining operation. Slinger trucks may be used for tight back-filling with cemented rock fill, but paste fill or cemented sand could also be employed for back-filling.
In mining, when drill-and-blast is used for the excavation, for example, at level A, then original posts 14 could be slightly damaged, although they will always be solid enough to support floor/roof 16 at least initially. Then, when posts 18 are placed, they are never subjected to the blasting operation and are always undamaged and provide solid support for the floor/roof 16.
The same procedure is then repeated at level B where, as the excavation proceeds, holes 12 are drilled in plumb below posts 14 and posts 28 are inserted therein. Then posts 25, shown in broken lines, are stood at level B on top of posts 28 and secured between said posts 28 and the roof 26 providing additional support for said roof 26. These posts 25 are again undamaged by any excavating operation and will, therefore, provide safe support for the floor above even when it is back-filled. Again once posts 24, 25 and 28 are properly positioned and secured, concrete floor 27 is poured to tie their ends with concrete and solidify the entire structure. The same procedure may then be repeated for level C and any additional levels in the downward direction. As mentioned previously, a layer 22 of broken rock or ore is preferably provided prior to pouring the concrete floor 27.
FIG. 2 illustrates, in plan view, the positioning of the double posts in accordance with the preferred embodiment of the present invention at every excavated level. Post 14 is installed into the drilled post hole 12 and post 18 is raised beside post 14 for additional support. Concrete roof/floor 16 is shown in broken lines. Distance L normally corresponds to distance W and, in this preferred embodiment, it is 8 meters. However, post sizes and spacings will be selected to conform with existing rock mechanics and mining practices.
In FIG. 3, the section view of the same arrangement is illustrated. Each level A, B, C is 5 meters high, corresponding to the length of posts 14, 24 and 28. Additional posts 18 and 25 which are stood-up beside posts 14 and 24 are again shown in broken lines. All numerals in this FIG. 3 refer to the same items as in FIG. 1.
FIG. 4 illustrates a two 5 m×5 m drifts in a mine where the usual 0.5 m diameter by 5 m deep holes 29 are drilled under each drift. Then several (6 or 8) 5 cm helper holes 31 are drilled around holes 29 approximately to the same depth as holes 29.
FIG. 5 shows the following procedures, namely posts 33 are inserted into holes 29 and holes 31 are blasted to break the area around the posts 33 in the ground below Drift 1 and Drift 2, without damaging said posts 33. The primary purpose for so breaking the ground around posts 33 is to avoid excessive blast vibration transmitted through unbroken rock to the post from subsequent drill and blast mining, which may cause blast damage to the post. Moreover, the subsequent mining blast holes can then be drilled further away from the posts, thus preventing blasting damage when ore is mined around the posts.
Also, there is provided a layer 35 of broken ore on the ground prior to pouring the concrete floor 37 thereon. Rebars and screens may be used to reinforce the concrete. Then, Drift 1 and Drift 2 may be sequentially filled with a suitable filler material 39, such as a 5% cement-rock fill.
FIG. 6 illustrates, in plan view, a grid of post undercut mining level in accordance with a preferred embodiment of the present invention. Posts 30, 32 are respectively posts installed into a drilled hole and posts raised at their side for additional roof support. These posts can be at any mining level and according to this embodiment are installed 8 m apart. A 5 m wide ramp 34 is provided to give access from one level to the next lower level. As shown in FIG. 7, this ramp 34 is also provided with a concrete floor, for example 0.3 m thick. Such ramps can be permanent or temporary depending on the mining sequence.
In FIG. 8, there is shown a multilevel mining arrangement having a raise bore hole 36. In this embodiment a steel lined 4 m diameter raise bore hole is provided through which various mining equipment is supplied. The raise bore machine 40 is used to lower cages 42, 44 with service vehicles, drill jumbos and the like.
Again in this embodiment the double-post system of the present invention, with posts 30, 32 supporting concrete roofs of levels A, B, C, D and E would be very suitable. As the upper levels A, B, C, D are mined, they are then back-filled as in the conventional undercut-and-fill mining method. According to this embodiment, each level is 5 m high which essentially corresponds to the length of the inserted posts 30. Posts 32, shown in broken lines, are the additional roof supporting posts which are stood-up beside inserted posts 30.
The key to the undercut post excavation method of the present invention are the posts used to support continuous concrete roofs. These posts must be designed to provide adequate compressive strength to support the concrete roof. When concrete posts are used, in accordance with the preferred embodiment of the present invention, they are normally manufactured on surface and then lowered to the mine as required. For 0.45 m diameter posts, reinforced concrete is used, in the form of 7 cm×7 cm mesh on outside and a suitable number of vertical rebars on the inside. The load capacity of such posts is about 500 tons per post or when 2 posts at each location are used, 1000 tons per location which is entirely sufficient to support an 8 m×8 m×0.3 m concrete roof plus the back-fill over said roof. The posting or inserting of such posts into pre-drilled holes is a relatively quick and mechanized operation. A Hiab boom mounted on a mobile truck can be used to insert three or more posts per hour.
It should be pointed out that only a preferred embodiment of the invention has been illustrated and discussed above by way of example and it should be understood that the invention can be adapted to many various conditions and practised in many different ways without departing from the spirit thereof and the scope of the following claims.
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An excavation method is provided, which is particularly suitable as an undercut-and-fill mining method, wherein posts are inserted into the ground and are used to support a concrete floor of the upper level which serves as a roof for the lower excavation level. Excavation beneath such roof is thereby safely carried out. Also, for mining operations, the excavation is very efficient since it removes essentially 100% of the ore in a single pass. The posts are preferably made of concrete and are inserted into holes drilled in the ground. For greater safety a double post system can be used, which involves placing a second post beside the first and tying them all together with the concrete used to make the floor/roof at any given level of excavation.
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BACKGROUND-FIELD OF INVENTION
[0001] This invention relates to a novel method comprising a mixture of liquid or powdered Sodium Hychloride (bleach), Distilled H2O (water), Acedic Acid (vinegar), Sodium Bicarbonate (baking soda) and Glue Size which will remove foxing stains from paper and celluloid items.
DISCUSSION OF PRIOR ART
[0002] Foxing is a pattern of spotting or speckling stains that mar many archival works found in old books, vintage paper or sometimes cloth, usually brown or yellowish brown in tone and often more or less circular in shape. Its cause is not fully understood but generally it is believed a slow process caused by fungal or mold microorganisms enabled by impurities in paper and storage conditions that are damp and warm enough to facilitate the process.
[0003] Filamentous fungi are known to damage and destroy paper and celluloid items in two principal ways. First, they utilize the paper cellulose as a carbon source, weakening and eventually destroying the paper fibers. Fungi also live on the trace metals found in paper or often in the inks on the paper.
[0004] Four strains of fungi are commonly found to cause foxing and each fungi is characterized by the production of different colored stains. Fungus Alternaria Solani produces a dense black stain, Fusarium Oxysporum, a pinkish stain, Penicillium Notatum, a light green stain and Chaetomium Globosum, a brownish grey stain.
[0005] These stains can sometimes be extracted with harsh solvents but there are few effective solvents that do not dissolve the ink or damage the paper fibers and many stains resist solvent extraction effectively. Treatment for foxing is difficult at best and often simply impractical.
[0006] Developing new solvent systems is time consuming and requires a great deal of trial and error, since the chemical structure of the pigment stains is not generally known.
[0007] Mechanical stain removal is also problematic in that it is not selective between ink and stain; often produces abrasion of the paper fibers, markedly deteriorating the paper; and is extraordinarily tedious, thus an inexpensive safe and effective method is needed to remove foxing stains and is in great demand.
[0008] The use of unsafe and damaging treatments to remove foxing stains is well established in the art of restoration and conservation. Typical topical chemicals used in the art are Ethylene Oxide (also known as EO, EtO, ETO, anprolene, dihydrooxirene, 1,2-epoxyethane, oxacyclopropane, oxane, oxidoethane an oxirane), Sodium Hychloride (household bleach), Chloramine-T, Calcium Hypochlorite, Chloramine Gas, Hydrogen Peroxide, Sodium Borohydride, Chlorine Dioxide, Chlorhexidine Gluconate, Magnesium Oxide, Potassium Permanganate and Lithium Aluminum Hydride.
[0009] All of these dangerous chemicals seriously degrade the cellulose in the paper and may lead to wrinkling of pages or bleeding of text or illustrations. These chemicals when used also introduce acidic residue salts that will contribute to additional damage in time and are difficult to use and quite expensive to purchase.
[0010] Some typical foxing removal procedures and guidelines found in the art are as follows:
a) Timothy Barrett, Japanese Papermaking, Tokyo & New York: Weatherhill; b) Anne F. Clapp, Curatorial Care of Works of Art on paper. New York: Nick Lyons Books, 1987 c) Carl Schraubstadter, Care and Repair of Japanese Prints, Cornwall: Idlewild, 1948
[0014] To remove foxing stains by bleaching, Schraubstadter recommends chlorine bleach or what is the same, common household bleach (Sodium Hypoclorite) which is extremely alkaline and therefore easily damages the paper fibers. Furthermore, if not rinsed sufficiently, chemical residues remain on the paper, causing future damage and decomposition.
[0015] Further bleaching methods published in the art are with Chloramine-T, Sodium Peroxide Or Sodium Borohydride in water with Lithium Aluminum Hydride in non-aqueous solvents. Another published bleaching method is to use commercial grade Hydrogen Peroxide. The Hydrogen Peroxide can be diluted in a ration of 1:1 or more. After applying the Hydrogen Peroxide the paper must be washed in a solution of Calcium Hydroxide mixed in distilled water. This agent supposedly removes traces of acidic substances from the paper or celluloid item.
[0016] Unfortunately, these methods and formulations as well as others have many disadvantages such as toxicity, flammability and are expensive. They are also shown to damage the paper for which they were intended to save. Thus, a need exists for an inexpensive, safe and reliable method that is specifically designed to control and remove the unique problems associated with foxing stains on paper and celluloid items.
OBJECTS AND ADVANTAGES
[0017] Accordingly, several objects and advantages of our invention are:
a) to provide a novel method designed to control and remove foxing stains from paper and celluloid items. b) to provide a novel method designed not to harm or destroy the paper or celluloid item, text or artwork on the paper or celluloid items while controlling or removing the foxing stains. c) to provide a novel method that control and removes foxing stains and leaves no residue which will harm the paper or cellulose items. d) to provide a novel method that is safe to use by humans while applying it to paper and celluloid items. e) to provide a novel method that is low cost to manufacture and to use.
DETAILED DESCRIPTION OF THE INVENTION
[0023] In the present invention, the foregoing difficulties are obviated in that there are a provided a low cost, easily dispersed method consisting of inexpensive commercially available ingredients. In accordance with the invention, the method is as follows:
1) Soak the paper or celluloid item completely in a warm bath of distilled water; 2) Remove the paper or celluloid item and blot all excess water; 3) Soak the paper or celluloid item completely in a warm bath of household bleach, less than 5% concentration; 4) Soak and rinse the paper or celluloid item completely with warm distilled water; 5) Remove the paper or celluloid item and blot all excess water; 6) Soak the paper or celluloid item completely in a warm bath of vinegar, no less than 75% concentration; 7) Soak and rinse the paper or celluloid completely item in a bath of cold distilled water; 8) Remove the paper or celluloid item and blot all excess water; 9) Soak the paper or celluloid item completely in a bath of sodium bicarbonate (baking soda) and distilled water; 10) Soak and rinse the paper or celluloid item completely with distilled room temperature water; 11) Remove the paper or celluloid item and blot all excess water; 12) Soak the paper or celluloid item completely in a bath of glue size. 13) Soak and rinse the paper or celluloid item completely in a bath of cold distilled water; 14) Remove the paper or celluloid item and blot all excess water. 15) Air Dry the paper or celluloid item without the use of a heat blower.
CONCLUSION, RAMIFICATION AND SCOPE OF THE INVENTION
[0039] Accordingly, the reader will see that this intricate detailed step method of removing foxing stains provides that:
[0040] It will specifically control and kill the growth of filamentous fungi and mold microorganisms that attack paper and celluloid items:
[0041] It will not harm or destroy the paper or celluloid items:
[0042] It will not leave a harmful residue or film on the paper or celluloid items:
[0043] It will not harm humans while being applied to paper and celluloid items:
[0044] It will be a low cost archival method to conserve and protect valuable paper and celluloid items.
[0045] Those skilled in the art will have no difficulty in determining suitable proportions of the above method to be used. The invention has been described as applied to preferred embodiments and it will be understood that various substitutions and changes may be effected without departing from the spirit and scope of the novel concepts and principals of this invention.
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A method to safely remove foxing stains from paper and celluloid items using distilled water, sodium hychloride, acedic acid, sodium bicarbonate and glue size.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation-in-part of Ser. No. 10/084,011, filed Feb. 25, 2002, and entitled “Wireless Community Alerting System”.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This invention relates generally to electronic messaging systems, and more particularly, to a pager-based community alerting system for informing subscribers of immediate or impending conditions so that an appropriate response may be made.
[0004] 2. Discussion of the Prior Art
[0005] The prior art includes a large number of patents and publications relating to emergency warning systems whereby members of the public can be alerted to such events as dangerous weather conditions, terrorist activities, environmental hazards and the like. The Lemelson et al. U.S. Pat. No. 6,084,510 describes a danger warning and emergency response system having an extensive listing of prior art relating to such systems. The apparatus of the Lemelson '510 patent is intended to provide emergency information to large multitudes of persons who may be in harms way. Given the fact that the implementation described in the '510 patent calls for satellites, pilotless aircraft, a downlink to a command center having one or more computers for analyzing received information from the satellites to arrive at a “danger index” as well as a ground base radio broadcasting system, the implementation cost would price the system out of reach of most subscribers.
[0006] The prior art is also replete with systems specifically designed for warning citizens of impending natural disasters, such as tornadoes, hurricanes, heavy snow and ice storms in an affected geographical area. For example, the Uber et al. U.S. Pat. No. 4,633,515 describes an emergency broadcast alert system that comprises a radio receiver referred to as a “scanner” that is designed to lock onto a broadcasted signal in the presence of noise. The receiver then repeatedly scans within a predetermined frequency band, looking for a transmitted signal from the National Weather Service and the receiver then provides an audible alarm so that one would, therefore, have to resort to broadcast television or radio to find out the storm path and expected time of arrival in a given geographical area. Thus, while the Uber system is relatively inexpensive, it lacks a capability to promptly advise a listener of important information relating to a potentially dangerous storm.
[0007] U.S. Pat. No. 6,177,873 to Cragun also describes a weather warning system that includes a communication link for receiving transmitted alerts (weather warnings/watches). It also includes a user interface that allows for selection of different geographic areas so that weather conditions affecting areas other than those of interest are filtered out. For proper operation, it is essential that the system be preprogrammed to identify geographical areas and weather intensity parameters. The ability to program the system may exceed the capabilities of many end-users.
[0008] Thus, a need exists for a subscriber-based alerting system that is inexpensive to implement and, thus, well within the budget of most persons occupying houses, apartments and other residential units as well as commercial and government establishments and that requires little or no manual involvement, yet is both versatile and reliable in operation.
SUMMARY OF THE INVENTION
[0009] According to the present invention, an electronic messaging system for both emergency and non-emergency events affecting different communities or subscriber groupings comprises a monitoring center for accepting and verifying alerts from authorized agencies. The monitoring center may be coupled through a public switched telephone network or dedicated data network to at least one paging provider network having the ability to broadcast a radio-frequency carrier suitably modulated with information, including addressing data and message data, based upon paging data input from the monitoring center pertaining to an alert. A plurality of physical units are installed in residential, commercial, and government buildings. Each includes a receiver, tunable to the carrier frequency of a paging provider network, a demodulator for recovering the address data and message data sent by the paging terminal, a microprocessor coupled to receive the addressing and message data, where the microprocessor further includes a memory that stores a list of codes pertinent to a particular end user physical unit. The physical units also include a plurality of visual and audible signaling devices that become activated between an off-state, an on-state, or a blinking-state only when received addressing data matches an entry in the physical unit's stored code list. The physical units may also include an alphanumeric display to convey verbiage pertaining to a particular alert.
[0010] In accordance with a further feature of the invention, a graphics icon may be associated with each of the visual indicating devices to readily convey in a non-lingual manner the nature of the alert being sent to occupants viewing the physical unit. For example, the icon may comprise a funnel cloud to represent a tornado warning or an automobile to indicate parking restrictions.
[0011] Various other features and advantages of the invention will become apparent to those skilled in the art from the following detailed description of a preferred embodiment, especially when considered in conjunction with the accompanying drawings in which like numerals in the several views refer to corresponding parts.
DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 is a general block diagram of the electronic messaging system comprising a preferred embodiment of the present invention;
[0013] [0013]FIG. 2 is a block diagram of each of the physical units (PU) illustrated in FIG. 1;
[0014] [0014]FIG. 3 is a schematic diagram of the Status & Message Display Module shown in FIG. 2;
[0015] [0015]FIG. 4 is a front perspective view of a physical unit showing the layout of visual signaling devices thereon;
[0016] [0016]FIG. 5 shows a series of icons used on the unit of FIG. 4;
[0017] [0017]FIG. 6 is a functional flow diagram helpful in understanding the software algorithms used in implementing the system of FIG. 1; and
[0018] [0018]FIG. 7 is an overlay for a physical unit incorporating the current Homeland Security Advisory System for indication of a level of terrorist threat.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0019] Referring first to FIG. 1, there is illustrated a system block diagram of the electronic messaging system of the present invention. It comprises a monitoring center 10 that is coupled by a communications link 12 to a paging provider network 14 having transmission equipment for broadcasting information to one or more physical units 16 . Virtually many thousands, millions or an unlimited number of physical units 16 may be incorporated into the messaging system contemplated.
[0020] The monitoring center 10 incorporates a computing and communications networking equipment and an operator who may receive a variety of alerts from authorized public and/or private agencies or individuals. The operator at the monitoring center determines the legitimacy of the alert in question. He/she may then contact the paging provider network, sending an alpha and/or numeric message, via a public switched telephone network or data network to the paging transmitter 14 of a licensed paging service provider. The paging transmitter receives, processes, stores and forwards information input by the monitoring center 10 staff who has validated the call by determining the authenticity of the calling agency or individual. An RF transmission system owned by the paging company is often comprised of a plurality of transmitters capable of accepting data from the telephone lines. It should be understood, however, that instead of telephone lines, the communication link 12 may also comprise an RF link, data network or satellite transmission. Upon decoding the alert data, the transmitter translates the paging data into a signal that modulates an RF carrier signal of a desired frequency.
[0021] The physical units 16 are modified versions of commercially available receivers, which can be leased from a paging service provider or purchased through various retailers, and are adapted to receive messages transmitted to it from the pager terminal 14 .
[0022] Once the paging transmitter 14 receives a page message from the monitoring center 10 , it processes, stores and forwards the information to another paging transmitter through its communications network and/or ultimately on to the physical unit(s) 16 . The processing step involves encoding the paging data for transmission through the carrier paging system. Typically, an encoder accepts the incoming paging message, validates the pager address and “encodes” the address and page data into the appropriate paging signaling protocol. Once the page is encoded, it is sent to the RF link system, which includes the link transmitter and link receiver. A link transmitter sends the page to a link receiver, which is located at another paging terminal site along the channel. The transmitters of the paging terminal(s) then broadcast the page across the coverage area on the specified carrier frequency.
[0023] Once data is received from the encoder, the paging protocol employed at the paging transmitter 14 organizes the message into frames of data, which is a specified sized packet of data bits. One popular paging protocol developed by the Motorola Company is referred to as FLEX®. In it there are a total of 128 frames and it takes exactly four minutes to transmit all 128 frames. The FLEX protocol provides a variety of common services, such as message routing, encryption, data compression to enable applications to send messages reliably, securely and efficiently over the communication channel comprising one or more paging terminal(s) 14 to the physical units 16 . Other protocols are also available.
[0024] Turning next to FIG. 2, there is shown a block diagram of each of the plurality of physical units 16 . The heart of the physical unit 16 is a receiver module 18 coupled to receive the encoded messages transmitted by the pager transmitter 14 . Without limitation, the receiver 18 may be a Motorola Type LS350, which is operatively coupled to a microprocessor 20 , preferably a microchip Type TMP86FS41 Flash-based 8-bit CMOS microcontroller. While this microcontroller is not the only commercially available unit that can be used, its architecture provides a 16-bit wide instruction word with separate 8-bit wide data buses. A two-stage instruction pipeline allows all instructions to execute in a single cycle except for programmed branches. It incorporates a large register set that can be used to achieve very high performance. As such, it is well suited to use in home appliances, consumer electronics and hand-held electronics. Because of its wide application, it has a relatively low cost, making it a good choice for use in the present invention.
[0025] The microprocessor-based controller 20 is connected in controlling relation to a status & message display module 22 . FIG. 3 is a schematic diagram of the status & message display driver 22 and it preferably comprises a microcontroller 24 that is connected to data lines 26 and 28 by way of a data interface comprising NPN transistor switches 30 and 32 , respectively.
[0026] The microcontroller 24 , preferably a PIC 16F62 microcontroller, is especially designed to function as a display driver and its outputs are connected through current limiting resistors, as at 34 , to visual signaling devices, here shown as LEDs 36 - 48 . Ten of these LEDs ( 36 - 45 ) are used to convey alert message information to an observer while the remaining three ( 46 - 48 ) provide information as to the operating status of the system. One of the status indicators 46 is illuminated as long as alternating current power is being applied to the physical unit. A second indicator, 47 , may be used to indicate the charge status of the back-up battery used in the system and the remaining status indicator 48 may be used to indicate that the system is disabled because, for example, a subscriber has not paid the monthly charge for the alerting service. An alpha readout 49 could also be included in addition to the visual signaling devices to provide further information to the end user.
[0027] Certain emergency conditions may require immediate action on the part of a subscriber. For example, a tornado warning may take place at a time that a subscriber is sleeping or otherwise out of visual contact with the physical unit. For this reason, an audible signaling device termed a siren is also included in the physical unit as represented by block 50 in FIG. 2. The issuance of an audible signal by the system results in the subscriber moving to a position to visually examine the physical unit's display panel to become advised of the nature of the alert.
[0028] To provide a more observable visual indication that a physical unit has received an alert message, a “visual enhancer” in the form of a flashing light bar, star or other pattern is provided as represented by block 52 in FIG. 2. In implementing block 52 , the same type of display driver as is implemented in the Status & Message display 22 can be used. Upon receipt of an alarm-enable, the PIC 16 F62 microcontroller executes a program causing a plurality of light-emitting diodes that are physically arranged in a desired pattern to blink on and off either in synchronism or sequentially so as to create the illusion of movement. A subscriber noticing the flashing pattern would then approach the physical unit and view the particular alert message(s) being displayed by the visual signaling devices (LEDs) 36 - 45 . The microcontroller 20 is also coupled to a set of contacts to control the operation of remotely located devices such as, but not limited to horns, light flashers, and vibrating devices as represented by block 54 in FIG. 2. Thus, in a commercial or industrial installation, an audible/visual signaling device located in a building remote from the physical unit itself can be actuated by an appropriate message picked up by the receiver 18 and processed by the microcontroller 20 . The sounding or flashing device has its own power source that becomes connected to it when a “remote set” signal from microcontroller 20 actuates appropriate relay contacts (not shown). Those relay contacts become reset or reopened upon receipt of a remote-rst signal from the microcontroller 20 .
[0029] It has also been found expedient to provide a historical memory in the physical unit itself for recording the time and date and type of alert events received by the physical unit in question. The historical memory is represented by block 56 and preferably may comprise an Electrically Erasable PROM memory such as a Type 24LC16B device. It has 16 kilobits, organized as eight blocks of 256×8-bit memory. Those skilled in the art will appreciate, however, that other commercially available memory devices can be used as well.
[0030] With continued reference to FIG. 2, provision is made for manually resetting a physical unit following receipt of an alert message. The only end user input/control for the physical unit is a push-button momentary contact switch which when depressed causes a signal to be applied to the reset (RST) input to the receiver 18 and a /RST input to microcontroller 20 and selected inputs of the status & message display 22 , the audible alarm 50 and the remote switch 54 .
[0031] The central power module 57 (FIG. 2) comprises a full wave rectifier for converting AC line power to a DC voltage as well as conventional integrated circuit voltage regulators for providing the requisite operating voltages for the receiver 18 , the CPU 20 and the circuits 22 , 52 , 54 and 56 shown in the system block diagram of FIG. 2. The central power 57 also includes a DC battery backup, which takes over in the event of AC line power failure. A 9 volt battery fits into a compartment that is wired so as to render the compartment polarity insensitive. As such, it matters not which way the battery is inserted in the compartment. This avoids system malfunction in the event of an AC power failure if a subscriber had improperly inserted the battery into a battery compartment that has not been so wired as to be polarity insensitive.
[0032] Referring to FIG. 4, there is shown a front perspective view of a physical unit 16 showing the layout of visual and audible signaling devices thereon. It comprises a box-like housing 56 in which printed circuit boards (not shown) carrying the circuitry depicted in the block diagram of FIG. 2 reside. The alert message visual signaling devices 36 - 45 may be arranged in a horizontal row while the status visual indicators 46 , 47 and 48 may be grouped separately and may be arranged in a vertical pattern on the housing 56 . The audible alarm (siren) 50 is disposed behind the top cover with an aperture through which the sound is emitted. The reset button 60 for the system reset block 62 in FIG. 2 also projects through an aperture formed in the housing 56 and is an integral part of the top overlay so as to be accessible to the subscriber.
[0033] The “visual enhancer” light array, as at 62 , may also be provided. The on/off state of the individual LEDs is controlled by the microprocessor 20 , which is adapted to send a signal over line 64 in FIG. 2 to the block 52 labeled Alarm Display. The LEDs in the array 62 are shown as being arranged in a star-shaped pattern, but other patterns may be used as well. By causing the array 76 to blink on and off at a desired rate, the fact that a message has been received by the physical unit 16 can readily be discerned whereby the subscriber can then more closely examine the physical unit and note which one(s) of the message indicators 36 - 45 has (have) been activated.
[0034] To render the nature of an alert condition more understandable, in accordance with the present invention, a suitable icon is associated with and possibly overlaid upon each of the message indicators. FIG. 5 illustrates only a few of the possible icons that may be applied over their associated LEDs so as to become illuminated when a particular alert event is being transmitted to the physical unit. In FIG. 5, icon A can be associated with, say, LED 36 in FIG. 3 to thereby indicate receipt of a tornado alert from the paging station. Icon B in FIG. 5 can be made overlay the LED 37 in FIG. 3, which then becomes illuminated when the alert condition being transmitted is a severe thunderstorm. Likewise, icon C may be associated with LED 38 to signal a snowstorm or blizzard. Icon D in FIG. 5 can be positioned over LED 39 to indicate a school closing alert. By controlling the LED 39 , it can be made to blink to indicate a two-hour delay or it may remain on steadily to indicate an all day closing. Similarly, icon E representing a school bus may overlay the LED 40 to signal that buses are running late.
[0035] Those skilled in the art will recognize that the icons presented in FIG. 4 are somewhat arbitrary and are provided only as an example of how a particular alert being transmitted to the unit 16 is to be interpreted. Further information on the severity or urgency of a particular alert can be conveyed by a judicious choice of LED color for the message indicators.
[0036] Assume that an authorized individual or agency wishes to issue an alert to all subscribers residing in a given geographical area. The address code broadcast by the paging station may be based upon postal zip codes, which consume only five (or nine depending on the degree of localization desired) digits out of the total number of digits used. This leaves ample capacity for storing additional code digits for further defining particular subscriber physical units and alert types to which given physical unit 16 can be responsive.
[0037] The present invention also has the capability to issue and display multiple types of alerts simultaneously. For example, in the case of a snow storm in a particular area, an alert for the storm itself, and a school closing occasioned by the storm can be simultaneously displayed. The capability also exists for one physical unit 16 to be located in multiple physical or logical zones. For example, one physical unit could be part of weather zone 1 and school zone 1 . A different physical unit could also be a part of weather zone 1 but reside in school zone 2 . It is also possible to program a physical unit residing in weather zone 1 to respond to alerts for both weather zone 1 and weather zone 7 , even if weather zone 7 is physically separate by geographical distance. Logical groups of common interest can also be alerted simultaneously, regardless of their geographic distance from one another. For example, members of the armed forces could reside in geographically disperse areas but could be considered as one logical group.
[0038] Having described the apparatus involved in implementing the present invention, consideration will next be given to its mode of operation. In this regard, reference is made to the flow diagram of FIG. 6, which is illustrative of the algorithm executed by the hardware. Referring to block 66 , an event occurs or a condition develops that requires the notification of an individual or group of individuals or a group of people having physical units 16 and subscribing to the alerting service. An authorized party, such as the Federal Department of Homeland Security, the National Weather Service, the State Patrol, a school district superintendent or a city official initially determines at decision block 68 whether the event is of a nature requiring notification to subscribers. If so, the authorized individual contacts the monitoring center 10 by a voice telephone call, fax message, e-mail, etc. (block 70 ). Notification in all cases will consist of the type of event or condition that exists, which may be an emergency or non-emergency. The notification will also specify the physical or logical area to be covered. Examples of an emergency event may include severe weather conditions, an environmental disaster or the like. A non-emergency event may be the existence of a lawn sprinkling ban to conserve water, delayed school openings and periodic system tests that are regularly scheduled and issued automatically by the monitoring center for the purpose of performing a non-intrusive end to end test of the system. System tests can be performed on a per physical unit basis, a group by group basis, or globally to include all units.
[0039] A determination is made at decision block 72 to verify that the caller is authorized to initiate the type of alert to be issued. If the caller does not have the proper level of authorization, he is so advised and no alert is issued (block 74 ).
[0040] If, on the other hand, the individual calling the monitoring center is authorized to issue a particular alert, the monitoring center dials the appropriate pager number(s), or accesses the paging service provide via a data network (block 76 ). It should be recalled at this point that all of the physical units 16 contain paging receivers 18 that are preprogrammed to respond to the same CAP code. All of the physical units will, therefore, receive all messages sent from the paging station 14 that are associated with that paging telephone number, whether it is intended that those particular physical units are to respond or not. The determination as to whether or not a particular physical unit should respond is made by comparing the incoming signal data stream and the database, which resides in the physical unit, looking for a match as a result of the comparison.
[0041] A test is made at decision block 78 as to whether the monitoring center has received a pager tone or data connection confirmation and, if not, control loops back over line 80 causing the monitoring center to redial the pager number or reconnect the data network until the test at decision block 78 is satisfied. At this point, the monitoring center inputs the appropriate data such as, but not limited to a 16 decimal digit code (block 82 ). This code represents a combination of whether or not one or more of the physical units 16 should respond to the input code and the manner in which the response is to be made. To include a single physical unit, the unit's unique address would be sent along with the data stream instructing the unit as to how to respond. To address multiple units simultaneously, the use of “wild card” characters would be used to indicate all users of a particular sub group. For example, if the address data of each unit was nine characters long, wild card characters in place of digits six through nine would alert all units matching the first five digits irrespective of what the last four digits were. The use of wild card characters for all nine digits would equate to all units, therefore all unit would respond to the following string of data which would convey exactly how the physical unit should respond.
[0042] It is to be recalled at this point that all of the physical units 16 are preprogrammed with a list of one or more codes to which they will respond. All physical units are also preprogrammed with instructions as to how they should respond to a given code that matches one on their list, e.g., visual signal only, audible signal only, both visual and audible signals, whether the remote contacts should be actuated, etc. Furthermore, multiple codes can be stacked on an individual physical unit meaning, for example, that a visual indication indicative of severe weather and sound can be turned on simultaneously when a test light also has been turned on.
[0043] A test is made at decision block 84 to determine whether the physical units receive the code from the paging transmitter and, if not, control again passes over line 80 causing the monitoring center to again redial the pager number. If, however, the code was properly received, the subscriber unit responds appropriately to the notification. The subscriber's attention is captured by the flashing “visual enhancer” 62 and by the individual visual signaling LEDs and/or sound output. Their focus is then brought to the individual light(s) that are illuminated. The screening which overlays the individual lights bearing the icons serves to indicate what the particular light represents. Additional information may be communicated via an alpha display screen 49 as well.
[0044] If the subscriber desires to cancel the notification, he or she can depress the user interface button 60 and if the physical unit's programming allows, shut off the light and/or sound. It is be understood, however, that certain notifications are not able to be reset by the end-user and will require cancellation from the monitoring center via the same process used in which they were individually actuated, it being understood that a different code is employed to terminate a notification.
[0045] The present invention is readily adaptable for use as a part of the Federal Government's Homeland Security Advisory System (HSAS) to disseminate information regarding the risk of terrorist attacks to federal, state and local authorities as well as to members of the public. The HSAS includes five levels of potential risk. Referring to FIG. 7, in addition to the icons described previously, there are provided five additional colored overlays adapted to be back-lit by underlying LED devices. The color coding of green, blue, yellow, orange and red correspond to the colors used in the HSAS. In addition, the colored icons include the words “low”, “guarded”, “elevated”, “high” and “severe” in accordance with the HSAS standards. In adopting the overlay of FIG. 7, the icons in row 90 will overlay the LED lights 36 - 45 shown in FIG. 4 and the bar 92 would be used as the attention attractor rather than the star-shaped configuration shown in FIG. 4. Five additional LEDs would be added to the physical unit 16 to back light the HSAS status indicators shown in row 94 . The three overlays shown in the vertical column 96 will overlay the LEDs 46 , 47 and 48 to provide an indication of whether AC power, battery backup or a disabled state of the unit is active, all as previously described. Finally, if the physical unit incorporates an alpha/numeric LCD display, a cutout may be provided in the overlay 89 allowing messages to show through. The area labeled “PRESS” overlays the “RESET” button in FIG. 4.
[0046] From what has been heretofore described, it should be apparent how messages can be formatted and sent to the physical units for causing a selected one of the threat level indicators in row 94 to be illuminated as the alert level is issued by the Department of Homeland Security.
[0047] This invention has been described herein in considerable detail in order to comply with the patent statutes and to provide those skilled in the art with the information needed to apply the novel principles and to construct and use such specialized components as are required. However, it is to be understood that the invention can be carried out by specifically different equipment and devices, and that various modifications, both as to the equipment and operating procedures, can be accomplished without departing from the scope of the invention itself.
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A pager-based alert system includes a monitor center that is in telephonic or data communication with a paging station allowing the command center to send multi-digit code words where selected digits comprise an address for selecting one or more of a plurality of physical units (paging receivers) and to direct the receiver to output visible and/or audible signals indicative of a particular alert condition. By providing the physical unit with graphic icons overlaying the visual indicators, an observer can readily determine the nature of the alert condition so that appropriate remedial action can be taken.
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BACKGROUND
I. Field
The following description relates generally to recharging a variety of batteries, and more particularly to a universal battery charger.
II. Background
The evolving market for battery-powered electronic imaging devices, cellular phones, computers, peripherals, and other electronic devices has grown incredibly. As each new generation of these products is introduced, devices with more capabilities and better specifications, with lower weight and smaller size, are joining the cordless brigade. For example, audio/video capture systems such as camcorders are becoming more and more portable—even while increasing in resolution and fidelity.
Manufacturing electronic devices smaller and making them battery-powered, however, does not necessarily make them completely portable. Because of battery capacity, equipment run-times are normally less than desired. Battery charging typically require more time than the use of the battery. Moreover, each device typically has required its own dedicated battery and matched charger. Thus, for example, even if a consumer purchases a camcorder and a camera from the same manufacturer, each of these devices will undoubtedly require its own specific battery as well as matched charger.
Presently, there exists several dozen unique battery form factors for cameras. Cellular phones account for another several dozen different battery configurations- some with three or four separate power ratings. Camcorder makers have attempted to standardize on a few battery form factors, but these too come in multiple power ratings. Countless varieties of other individual types of battery cells are commonly used in photographic equipment, games, appliances and other applications.
One of the reasons for the proliferation of chargers is that prior art chargers are product-specific, with added constraints on size, speed, power supply and compatibility with various battery chemistries. A dedicated charger for each of these batteries, or even for each type of these batteries, becomes economically and physically prohibitive. Likewise, adaptability to different AC and DC charging power sources is frequently lacking.
Implementation of many charging systems requires an electromechanical connection between the battery and charger that is designed for that single type of battery. However, it is apparent that a dedicated external charger for every new type and configuration of portable battery becomes less economically attractive with the acquisition by the consumer of more devices.
When the size and weight penalty imposed by the need for multiple spare batteries and chargers is combined with a disparate ratio of charge-time to run-time and the constant need for multiple nearby AC outlets, it can be seen that true portability will remain more an idealistic goal than a practical reality if all the power accessories that are needed to maintain portability weigh down the consumer.
Consequently, it would be desirable to address one or more of the deficiencies described above.
SUMMARY
In accordance with certain aspects of the present invention, a battery charger includes a housing defining a battery receptacle area configured to receive a battery therein, a piston, a moveable platform, wherein the piston and the platform are simultaneously urged in substantially orthogonal directions toward the battery receptacle area, and prongs configured to extend from the housing and electrically connect a power source to the battery when the battery is received in the battery receptacle area and engaged by the piston and moveable platform.
In accordance with yet other aspects of the present invention, a method for charging a battery includes connecting a pair of prongs of a battery charger to a power source and placing a battery into a battery receptacle area of the battery charger, wherein the battery is simultaneously maintained in a vertical charging position by a platform exerting a substantially uniform vertical pressure against a lower surface of the battery and a horizontal charging position by a piston exerting a substantially uniform horizontal pressure against a side surface of the battery.
In accordance with another aspect of the present invention, a method of manufacturing a battery charger assembly includes providing a housing configured to define a battery receptacle for receiving a battery therein, providing a piston internal to the housing that is urged toward the battery receptacle area by a spring, and providing a moveable platform internal to the housing that is urged toward the battery receptacle area by a spring, wherein a direction in which the piston is urged is substantially orthogonal to a direction in which the platform is urged.
It will become readily apparent to those skilled in the art from the following detailed description, wherein it is shown and described only exemplary configurations of a universal battery charger. As will be realized, the invention includes other and different aspects of an applicator and assembly and the various details presented throughout this disclosure are capable of modification in various other respects, all without departing from the spirit and scope of the invention. Accordingly, the drawings and the detailed description are to be regarded as illustrative in nature and not as restrictive.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a right exploded perspective view of the parts of a universal battery charger configured in accordance with one aspect of the disclosure;
FIG. 2 is a left exploded perspective view of the parts of a universal battery charger configured in accordance with one aspect of the disclosure;
FIG. 3 is a first cross-sectional view illustrating a first battery inserted into the universal battery charger for charging, in accordance with certain aspects of the present invention;
FIG. 4 is a second cross-sectional view illustrating a second battery inserted into the universal battery charger for charging, in accordance with certain aspects of the present invention;
FIG. 5 is a third cross-sectional view illustrating the second battery inserted into the universal battery charger for charging, in accordance with certain aspects of the present invention;
FIG. 6 is a fourth cross-sectional view illustrating the first battery inserted into the universal battery charger for charging, in accordance with certain aspects of the present invention;
FIG. 7 is a perspective view of the first battery being inserted into the universal battery charger, in accordance with certain aspects of the present invention;
FIG. 8 is a front elevation view of the universal battery charger before the first battery is inserted into the universal battery charger, in accordance with certain aspects of the present invention;
FIG. 9 is a front elevation view of the universal battery charger after the first battery has been inserted into the universal battery charger, in accordance with certain aspects of the present invention;
FIG. 10 is a front elevation view of the universal battery charger after the second battery has been inserted into the universal battery charger, in accordance with certain aspects of the present invention;
FIG. 11 is a front perspective view of the universal battery charger, in accordance with certain aspects of the present invention;
FIGS. 12 and 13 are cross-sectional views of the universal battery charger, in accordance with certain aspects of the present invention;
FIG. 14 is a right exploded perspective view of the parts of a second universal battery charger configured in accordance with one aspect of the disclosure; ( FIG. 1 )
FIG. 15 is a perspective view of exemplary batteries with which the second universal battery charger of FIG. 14 may be used;
FIG. 16 is a perspective cross-sectional view of the second universal battery charge into which a customized battery interface may be inserted in accordance with certain aspects of the present invention;
FIG. 17 is a perspective cross-sectional view of the second universal battery charger into which the customized battery adaptor has been inserted in accordance with certain aspects of the present invention;
FIG. 18 is a top plan cross-sectional view of the second universal battery charger into which the customized battery adaptor has been inserted in accordance with certain aspects of the present invention;
FIG. 19 is a perspective cross-sectional view of the second universal battery charger into which a third battery has been inserted in accordance with certain aspects of the present invention;
FIG. 20 is a top plan cross-sectional view of the second universal battery charger into which the third battery has been inserted in accordance with certain aspects of the present invention;
FIG. 21 is a top plan cross-sectional view of the second universal battery charger into which a fourth battery has been inserted in accordance with certain aspects of the present invention; and
FIG. 22 is a rear perspective view of a custom battery interface of the second universal battery charger configured in accordance with certain aspects of the present invention.
DETAILED DESCRIPTION
Various aspects of the novel systems, apparatus, and methods are described more fully hereinafter with reference to the accompanying drawings. The teachings disclosed herein may, however, be embodied in many different forms and should not be construed as limited to any specific structure or function presented throughout this disclosure. Rather, these aspects are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. Based on the teachings herein one skilled in the art should appreciate that that the scope of disclosure is intended to cover any aspect of the novel systems, apparatus and methods disclosed herein, whether implemented independently of or combined with any other aspect of the disclosure. For example, an apparatus may be implemented or a method may be practiced using any number of the aspects set forth herein. In addition, the scope of the disclosure is intended to cover such an apparatus or method which is practiced using other structure, functionality, or structure and functionality in addition to or other than the various aspects of the disclosure set forth herein.
Various aspects of a universal battery charger may be illustrated by describing components that are coupled, attached, and/or joined together. As used herein, the terms “coupled”, “attached”, and/or “joined” are used to indicate either a direct connection between two components or, where appropriate, an indirect connection to one another through intervening or intermediate components. In contrast, when a component is referred to as being “directly coupled”, “directly attached”, and/or “directly joined” to another component, there are no intervening elements present.
Relative terms such as “lower” or “bottom” and “upper” or “top” may be used herein to describe one element's relationship to another element illustrated in the drawings. It will be understood that relative terms are intended to encompass different orientations of a universal battery charger in addition to the orientation depicted in the drawings. By way of example, if a universal battery charger in the drawings is turned over, elements described as being on the “bottom” side of the other elements would then be oriented on the “top” side of the other elements. The term “bottom” can therefore encompass both an orientation of “bottom” and “top” depending on the particular orientation of the apparatus.
Various aspects of a universal battery charger may be illustrated with reference to one or more exemplary embodiments. As used herein, the term “exemplary” means “serving as an example, instance, or illustration,” and should not necessarily be construed as preferred or advantageous over other embodiments of a universal battery charger disclosed herein.
FIG. 1 is a right exploded perspective view of an exemplary universal battery charger 100 configured in accordance with one aspect of the disclosure, which is adapted to be able to operate with a variety of batteries of different sizes from a particular company, such as camera and/or camcorder batteries. Typically, batteries supplied by each company have the same voltage levels, and often only differ in physical aspects such as size. In many cases, the size is directly proportional to the amount of power storage of which the battery is capable because the size is based on the number of cells in each battery. A left exploded perspective view of the universal battery charger is illustrated in FIG. 2 .
The universal battery charger 100 may include an outer housing 101 (see also FIGS. 3 and 4 ) for protection of the electrical circuitry contained therein as well as for protection of the battery during charging. The outer housing 101 may be comprised of a cover 102 secured to a base portion 160 and may be made of any suitable non-conductive, impact resistant material, such as a hard plastic material, for example. The base portion 160 may be configured with an opening 162 so that, when the cover 102 is secured to the base portion 160 , the opening 162 provides access to an internal battery receptacle area 166 for receiving and securing a battery into the housing 101 .
The cover 102 may be configured with a window 104 through which a display circuit board 110 , used for displaying the charge/discharge status of the battery 190 , may be seen, as further described below. The display circuit board 110 may be used to display a charge/discharge completion time (e.g., estimated charge completion time), battery charge/discharge cycle time, current charging voltage, life of battery estimation, whether the charger is charging at a trickle charge rate, and other battery-related information. In one aspect of the disclosure, the display circuit board 110 may be implemented using one or more light emitting diodes (LEDs), such as an arrangement of LEDs 112 mounted on the top surface of the display circuit board 110 . The display circuit board 110 may also be implemented using liquid crystal displays (LCDs), analog displays (e.g., an analog meter), or other suitable means of displays.
The display circuit board 110 may be controlled by a main circuit board 114 capable of charging batteries of multiple voltages and having circuitry that automatically or manually adapts to the power profiles of different batteries, including voltage, total power capacity, battery chemistry type and recharging rate. In accordance with one aspect of the disclosure, the main circuit board 114 may include an automatic multi-voltage switching circuit for use with power outlets worldwide without additional adapters or attachments. In accordance with other aspects, the main circuit board 114 may be adapted to operate with the power supplied by a particular region, such as the 110-120V power used in the United States or the 220-240V power used in European countries. The base portion 160 may be configured with an opening 550 into which the main circuit board 114 and the display circuit board 110 are positioned.
In operation of the universal battery charger 100 , a battery, such as the battery 190 with contacts 192 depicted in FIGS. 1 and 2 , may be inserted through the opening 162 in the base portion 160 to be received into the battery receptacle area 166 . According to one aspect of the present invention, an access slot 106 may be provided on the cover 102 to provide additional clearance for a user's finger, for example, to slidably insert the battery 190 into a position of contact with a plurality of pins 800 . Thus, the contacts 192 may be electrically coupled to the main circuit board 114 using the appropriate pins from the plurality of pins 800 , as seen in the various elevational views illustrated by FIGS. 8 , 11 , 12 and 13 .
In one aspect of the disclosure, the plurality of pins 800 may be resiliently held into place by a frame 120 and the battery 190 may be held in a secure manner both (i) vertically and (ii) horizontally through the compression forces of (i) at least one bottom spring 150 pushing a platform 150 against the bottom of the battery 190 , and (ii) one or more side springs 152 pushing a piston 140 against the side of the battery 190 , respectively.
The frame 120 , in one aspect of the disclosure, may include one or more slots 124 that are matched to guides 142 on the piston 140 , the guides 142 being configured to slidably engage the one or more slots 124 . One or more slots may also be provided on a bottom surface of the top cover (not shown) that are configured to slidably engage guides 142 on the piston 140 . Thus, the guides 142 may engage the slots 124 in the frame 120 and/or the slots on the bottom surface of the cover 102 to encourage movement of the piston 140 in a defined manner horizontally without skewing or twisting, which prevents the piston 140 from becoming jammed. Similarly, the platform 130 may include two pair of guides 132 , 134 , that are matched to two respective pair of slots 126 , 122 on the frame 120 to encourage the platform 130 to move in a defined manner vertically without skewing or twisting, which can cause jams. In other aspects of the disclosure, any or all of the slots and guides may be eliminated or additional slots and guides may be added depending on the specific implementation. Generally, a larger platform 130 or piston 140 will require more guides and associated slots in the frame 120 .
The platform 130 may be configured with a spring seat for mounting the bottom spring 150 in a secured position. For example, as shown in FIGS. 3 and 4 , the spring seat 136 may comprise a cylindrical bore formed in a thicker portion of the platform 130 , the bore extending from an upper platform plate 138 and having a diameter that is slightly greater than or equal to an outer radial diameter of the bottom spring 150 . When assembled, an end portion of the bottom spring 150 may be inserted into the spring seat 136 so that the bottom spring 150 is compressed between a bottom wall 161 of the base portion 160 and the platform plate 138 of the platform 130 . In this manner, the platform 130 is continuously urged upward by the spring force toward the battery receptacle area 166 . The bottom wall 161 of the base portion 160 may be formed with additional spring securing features, such as a spring post 163 and a retaining ring 165 , for example, to further ensure a secure positioning of the bottom spring 150 . Thus, in combination with the guides 134 , the spring seat 136 and the additional spring securing features may ensure the proper positioning and vertical movement of the platform 130 . According to another aspect of the present invention, the platform 130 may be configured with a detent 139 that engages a lip 167 configured on the base portion 160 to provide an upper limit on the extent to which the platform 130 may move upward into the battery receptacle area 166 .
The piston 140 may be configured with spring seats 144 for mounting the side springs 152 in a secured position. For example, as shown in FIG. 5 , the spring seats 144 may comprise bores extending into a side surface of the piston 140 that have a diameter slightly greater than or equal to an outer radial diameter of the side springs 152 . When assembled, an end of the side springs 152 may be inserted into the spring seats 144 so that the side springs 152 are compressed between a side wall 167 of the base portion 160 and an inner wall 145 of the spring seat 144 . In this manner, the piston 140 may be continuously urged inward toward the battery receptacle area 166 .
The frame 120 , platform 130 , and piston 144 may be coupled together by way of the various guides and slots and mounted into the base portion 160 of the universal battery charger 100 with the bottom and side springs 150 and 152 respectively positioned as described above. The cover 102 may be secured to the base portion 160 in order to secure and maintain the internal components and circuitry of the universal battery charger 100 therein. As shown in FIGS. 7 and 8 , for example, the platform 130 and the piston 140 extend into the battery receptacle area 166 and are capable of receiving a battery of varying dimensions. The platform 130 and the piston 140 may include slanted or beveled leading surfaces, for example, to further enable the easy insertion and acceptance of the battery into the battery receptacle area 166 .
As shown in FIG. 3 , a first battery 302 with contacts 392 may be inserted through the opening 162 of the base portion 160 and received into the battery receptacle area 166 so that contacts on the battery engage the pins 800 . FIG. 12 is a cross-section view of the first battery 302 being inserted into the opening 162 . The first battery 302 may be effectively clamped vertically between a lower surface of the cover 102 and an upper surface of the platform 130 as a result of the force of the bottom spring 150 being distributed by the platform 130 to exert a substantially uniform upward pressure against a lower surface of the first battery 302 . Similarly, as shown in FIGS. 6 and 9 , the first battery 302 may be effectively clamped horizontally between the piston 140 and the frame 120 or a sidewall of the base portion 160 as a result of the force of the side springs 152 being distributed by the piston 140 to exert a substantially uniform inward pressure against a side surface of the first battery 302 . The dually applied and distributed spring forces may simultaneously maintain the first battery 302 in a secure vertical and horizontal charging position.
Referring to FIG. 4 , a second battery 402 that is of a smaller size than the first battery 302 may be inserted into the opening 162 of the bottom housing 160 . As described above, the second battery 402 may be maintained in an effective vertical charging position by being held secure against the bottom of the cover 102 due to the force of the bottom spring 150 on the platform 130 exerting a distributed upward pressure against a lower surface of the second battery 402 . Also referring to FIGS. 5 and 10 , it is illustrated that the second battery 402 may be maintained in an effective horizontal charging position by being held secure against the frame 120 or a side wall of the base portion 160 due to the force of the springs 152 on the piston 140 exerting a distributed inward pressure against a side surface of the second battery 402 . In the case of a smaller battery, the access slot 106 may provide access for a user to effect positioning of the battery in the battery receptacle area 166 . In another aspect of the present invention, the battery may be positioned in the battery receptacle area 166 simply by direct longitudinal pushing of a distal end of the battery through the opening 162 .
As seen in FIGS. 5 and 6 , the base portion 160 may include a plurality of screw holes 502 for securing the cover 102 using a plurality of screws. As further seen in FIG. 13 , an example of a screw hole 504 , into which a screw is inserted into a matching screw hole 502 in the base portion 160 may be secured, is shown in the top cover 102 . Although shown with screw holes for securing the cover 102 to the base portion 160 with screws, any suitable securing means may be used, including adhesives, welding, heat bonding, tab and slot configurations, and press fitting, for example.
The universal battery charger 100 may be configured with a fold-away wall plug 170 . As shown in FIGS. 1-4 , the wall plug 170 may be built into the base portion 160 with a pair of prongs 174 that is electrically connected to the main circuit board 114 . The fold-away wall plug 170 may include a rod 172 that is used to pivot the fold-away wall plug 170 from a first position, where the pair of prongs 174 is substantially flush with a lower surface 164 of the bottom housing 160 , to a second position, where the pair of prongs 174 may be deployed to extend substantially orthogonally from the lower surface 164 to be inserted into a power outlet. In one aspect, the prongs 174 of the fold-away wall plug 170 may be changed to other shapes for compatibility with the power outlets of any country.
FIG. 14 is a right exploded perspective view of a second exemplary universal battery charger 1400 configured in accordance with one aspect of the disclosure, which is adapted to be able to operate with a variety of batteries of different sizes for such devices as Digital Single-Lens Reflex (DSLR) cameras. Typically, batteries supplied by different companies have different voltage levels, and also differ in physical aspects such as in contact layout as well as size. In many cases, the size is directly proportional to the amount of power storage of which the battery is capable because the size is based on the number of cells in each battery. The second exemplary universal battery charger 1400 is able to operate with the various batteries supplied by different companies via a customized battery interface as further described herein.
The universal battery charger 1400 includes a cover 1402 secured to a base portion 1460 and may be made of any suitable non-conductive, impact resistant material, such as a hard plastic material, for example. The base portion 1460 may be configured with an opening 1462 so that, when the cover 1402 is secured to the base portion 1460 , the opening 1462 provides access to an internal battery receptacle area 1466 (see also FIG. 16 ) for receiving and securing a battery such as batteries 1490 a,b into the housing.
The cover 1402 may be configured with a window 1404 through which a display circuit board similar to the display circuit board 110 of the embodiment described in FIGS. 1-13 , may be used for displaying the charge/discharge status of the batteries 1490 a,b , as further described below. The display circuit board may be controlled by a main circuit board 114 , similar to the main circuit board 114 of the previously described embodiment, which is also capable of charging batteries of multiple voltages and having circuitry that automatically or manually adapts to the power profiles of different batteries, including voltage, total power capacity, battery chemistry type and recharging rate. The main circuit board is accessed through a plurality of contacts 1800 .
In operation of the universal battery charger 1400 , a battery, such as the batteries 1490 a,b with contacts 1492 a,b depicted in FIG. 15 , may be inserted through the opening 1462 in the base portion 1460 to be received into the battery receptacle area 1466 . According to one aspect of the present invention, an access slot 1406 may be provided on the cover 1402 to provide additional clearance for a user's finger, for example, to slidably insert batteries 1490 a,b into a position of contact with a plurality of contacts 2200 a,b on custom battery interfaces 1414 a,b . Thus, the contacts 1492 a,b may be electrically coupled to the main circuit board of the charger using the appropriate contacts from the plurality of contacts 2200 a,b , as seen in the various views illustrated by FIGS. 16-21 and as further described herein.
In one aspect of the disclosure, the plurality of contacts 1800 may be resiliently held into place by a frame 1420 and exposed via a plurality of openings 1802 . A custom battery interface such as the custom battery interfaces 1414 a,b may be used to provide customized interfaces between the plurality of contacts 1800 and the contacts for the batteries 1490 a,b . For example, the custom battery interface 1414 b may be used to electrically interface the contacts 1800 to the contacts 2200 b so that the battery 1490 b may be coupled to the main circuit board. The customized battery interfaces may be easily changed by a user inserting and removing the interfaces through an opening 1468 in the base portion 1460 and into an opening 1428 of the base 1420 . The custom battery interfaces may be held securely by their insertion into a slot 1408 with retaining rails 1410 in the cover 1402 that is matched to such features as slots 1412 a,b in the custom battery interfaces 1414 a,b . After insertion, the custom battery interfaces 1414 a,b are retained in an interface retaining portion 1668 . Thus, batteries of various electrical contact arrangements, including batteries with different number of contacts, may be charged using the same main circuit board.
FIG. 22 illustrates a plurality of contacts 2300 a for the custom battery interface 2214 a of the second universal battery charger 1400 configured in accordance with certain aspects of the present invention. As shown, the custom battery interface 2214 a also include a slot 2212 a to mate with retaining rails 1410 in the cover 1402 , as discussed with the slot 1412 a . As discussed above, the main circuit board is used to generate voltage and current to charge a variety of batteries that is connected to the second universal battery charger 1400 . In order to interface with all the different batteries, different custom battery interfaces may be used, as shown above. It should be noted that any number of contacts may be used for electrically interfacing the main circuit board to a battery. Thus, the number of contacts in the plurality of contacts on the custom battery interface that is used to interface the main circuit board with the battery may be customized.
As discussed further below, a battery such as the battery 1490 b may be held in a secure manner both (i) vertically and (ii) horizontally through the compression forces of (i) at least one bottom spring 1450 pushing a platform 1450 against the bottom of the battery 1490 b , and (ii) one or more side springs 1452 pushing a piston such as an arm 1440 against the side of the battery 1490 b , respectively. Thus, batteries of various sizes may be held securely within the universal battery charger 1400 .
The frame 1420 , in one aspect of the disclosure, may include one or more slots that are used to retain guides on the platform 1430 . For example, the platform 1430 may include two pair of guides 1432 , 1434 that are matched to two respective pair of slots 1426 , 1422 on the frame 1420 to encourage the platform 1430 to move in a defined manner vertically without skewing or twisting, which can cause jams. In other aspects of the disclosure, any or all of the slots and guides may be eliminated or additional slots and guides may be added depending on the specific implementation. Generally, a larger platform 1430 will require more guides and associated slots in the frame 1420 .
The platform 1430 may be configured with a spring seat for mounting the bottom spring 1450 in a secured position. Similar to the use of the spring seat 136 of the earlier described embodiment, as shown in FIGS. 3 and 4 , when assembled, an end portion of the bottom spring 1450 may be inserted into the so that the bottom spring 1450 is compressed between a bottom wall of the base portion 1460 and the platform 1430 . In this manner, the platform 1430 is continuously urged upward by the spring force toward the battery receptacle area 1466 . The bottom wall of the base portion 1460 may be formed with additional spring securing features, such as a spring post 163 and a retaining ring 165 of the previous embodiment, for example, to further ensure a secure positioning of the bottom spring 1450 . Thus, in combination with the guides 1434 , the spring seat and the additional spring securing features may ensure the proper positioning and vertical movement of the platform 1430 . According to another aspect of the present invention, the platform 1430 may be configured with a detent that engages a lip configured on the base portion 1460 to provide an upper limit on the extent to which the platform 1430 may move upward into the battery receptacle area 1466 .
The arm 1440 may be configured with spring retaining tabs 1444 for retaining the side springs 1452 in a secured position. For example, the arm 1440 may comprise openings 1446 extending into a surface of the tabs 1444 for a pin (not shown) to secure the side springs 1452 . When assembled, an end of the side springs 1452 may be inserted into the arm 1440 so that the side springs 1452 are compressed between a side wall 1467 of the base portion 1460 and an inner wall of the arm 1440 . In this manner, the arm 1440 may be continuously urged inward toward the battery receptacle area 1466 .
The frame 1420 , platform 1430 , and arm 1444 may be coupled together by way of the various guides and slots and mounted into the base portion 1460 of the universal battery charger 1400 with the bottom and side springs 1450 and 1452 respectively positioned as described above. The cover 1402 may be secured to the base portion 1460 in order to secure and maintain the internal components and circuitry of the universal battery charger 1400 therein. As shown in FIGS. 17 and 18 , for example, the platform 1430 and the arm 1440 extend into the battery receptacle area 1466 and are capable of receiving a battery of varying dimensions. The platform 1430 and the arm 1440 may include slanted or beveled leading surfaces, for example, to further enable the easy insertion and acceptance of the battery into the battery receptacle area 1466 .
As shown in FIG. 19 , the battery 1490 b with the contacts 1492 b may be inserted through the opening 1462 of the base portion 1460 and received into the battery receptacle area 1466 so that contacts 1492 b on the battery 1490 b engage the contacts 2200 b on the battery interface 1414 b , and through which, the contacts 1800 . The battery 1490 b may be effectively clamped vertically between a lower surface of the cover 1402 and an upper surface of the platform 1430 as a result of the force of the bottom spring 1450 being distributed by the platform 1430 to exert a substantially uniform upward pressure against a lower surface of the battery 1490 b . Similarly, as shown in FIGS. 19 and 20 , the battery 1490 b may be effectively clamped horizontally between the arm 1440 and the frame 1420 or a sidewall of the base portion 1460 as a result of the force of the side springs 1452 being distributed by the arm 1440 to exert a substantially uniform inward pressure against a side surface of the battery 1490 b . The dually applied and distributed spring forces may simultaneously maintain the battery 1490 b in a secure vertical and horizontal charging position.
Referring to FIG. 21 , the battery 1490 a that is of a smaller size than the battery 1490 b may be inserted into the opening 1462 of the bottom housing 1460 . As described above for the battery 1490 b , the battery 1490 a may be maintained in an effective vertical charging position by being held secure against the bottom of the cover 1402 due to the force of the bottom spring 1450 on the platform 1430 exerting a distributed upward pressure against a lower surface of the battery 1490 a , so that the battery 1490 a may be maintained in an effective horizontal charging position by being held secure against the frame 1420 or a side wall of the base portion 1460 due to the force of the springs 1452 on the arm 1440 exerting a distributed inward pressure against a side surface of the battery 1490 a . In the case of a smaller battery, the access slot 1406 may provide access for a user to effect positioning of the battery in the battery receptacle area 1466 . In another aspect of the present invention, the battery may be positioned in the battery receptacle area 1466 simply by direct longitudinal pushing of a distal end of the battery through the opening 1462 .
The universal battery charger 1400 may be configured with a fold-away wall plug similar to the fold-away wall plug 170 as shown in FIGS. 1-4 of the previously described embodiment, the wall plug 170 may be built into the base portion 160 with a pair of prongs that is electrically connected to the main circuit board. The fold-away wall plug may pivot from a first position, where the pair of prongs is substantially flush with a lower surface of the bottom housing 1460 , to a second position, where the pair of prongs may be deployed to extend substantially orthogonally from the lower surface of the outer housing 1460 to be inserted into a power outlet. In one aspect, the prongs of the fold-away wall plug may be changed to other shapes for compatibility with the power outlets of any country.
The previous description is provided to enable any person skilled in the art to understand fully the full scope of the disclosure. Modifications to the various configurations disclosed herein will be readily apparent to those skilled in the art. Unless specifically stated otherwise, the terms “some” or “at least one” refer to one or more elements. All structural and functional equivalents to the elements of the various aspects described throughout this disclosure that are known or later come to be known to those of ordinary skill in the art are expressly incorporated herein by reference and are intended to be encompassed by any claims that may be directed to the various aspects. Moreover, nothing disclosed herein is intended to be dedicated to the public regardless of whether such disclosure is explicitly recited by any claims.
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A battery charger includes a housing defining a battery receptacle area configured to receive a battery therein, a piston, a moveable platform, wherein the piston and the platform are simultaneously urged in substantially orthogonal directions toward the battery receptacle area, and prongs configured to extend from the housing and electrically connect a power source to the battery when the battery is received in the battery receptacle area and engaged by the piston and moveable platform. A method for charging a battery includes connecting a pair of prongs of a battery charger to a power source and placing a battery into a battery receptacle area of the battery charger, wherein the battery is simultaneously maintained in a vertical charging position and a horizontal charging position. A method of manufacturing a battery charger assembly includes providing a housing and providing a piston and a moveable platform internal to the housing.
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This is a continuation-in-part of application Ser. No. 469,885, filed May 14, 1974, now abandoned, which is a continuation of application Ser. No. 295,576, filed Oct. 6, 1972, now abandoned.
BACKGROUND OF THE INVENTION
The invention refers to a weaving machine of the so-called progressive shedding loom type, wherein a series of disadvantages of known such machines have been overcome by the provision of the following features:
A. Improved driving of the devices which insert and beat-up the weft threads between the warp threads, such devices hereinafter being referred to as "inserters".
B. The system of feeding the weft threads to the inserters, which in turn subsequently introduce the weft threads into the shed, is improved.
C. The heald actuating system which opens and closes the warp threads to allow passage of the inserters and which crosses the warp threads behind each inserter after the deposit thereby of a new weft thread, is improved.
However, before explaining in detail the characteristics of the invention which advantageously eliminate the disadvantages of known machines, and also before referring in detail to the different embodiments of the invention, in view of which even a dual weaving machine can be constructed which is capable of simultaneously producing two lengths of fabric with a minimum of additional elements, a brief explanation will be made of the characteristics as well as of the disadvantages of known machines of this type.
Presently known weaving machines of the progressive shed type are mainly constructed from a warp thread feeding roller and a roller which collects the fabric produced, such rollers being superposed and between which there is a shed tunnel wherein the warp threads are controlled by a plurality of healds which are positioned within planes which are perpendicular to the vertical planes occupied by the shafts of the rollers, and which are alternately linearly moved in directions which are also perpendicular to the planes occupied by the roller shafts.
The healds are mere elongated elements which have an opening through which the warp thread passes and which are connected in groups, each group being composed of at least two healds. The healds are superposed within each group, and comprised within the same perpendicular plane as those occupied by the shafts of the rollers.
The planes which define the position in space of each group of healds are therefore parallel to each other.
The warp threads, furthermore, after passing the corresponding healds, are driven very close to each other between two guide elements which force the warp threads to be joined from such moment onward until the fabric collecting roller is reached, whereat when operation starts the warp threads should be fixed.
The healds receive alternate opposed lineal movements within each group, so that the threads being controlled thereby are open or separated each time the healds which are driven in opposite directions away from each other, and so that the threads are subsequently crossed when the healds receive reversed movement. Before the healds are moved to opposite extreme positions, they are exactly superposed.
As can be appreciated from the fact that the warp threads are guided together after their passage through the healds, the separation and crossing of the threads, as produced by the healds, is effected from the point where the guide means force the threads to be held together.
Immediately on top of the guide means, which force the threads to be joined after being controlled by the healds, and moving within a path between such guide means and the healds, there are a plurality of inserters which are spaced from each other at short, regular intervals and which are synchronously moved. Each one of such inserters deposits a weft thread between the warp threads which, in view of the above mentioned arrangement, are separated in front of each inserter and cross behind the same, on top of the weft thread deposited thereby. Each inserter, at the same time as it deposits a weft thread, beats up the weft thread deposited by the preceding inserter, pressing the cross of warp threads thereon.
The shed tunnel is formed by the grouping of various warp threads controlled by the healds. Such shed is open when the warp threads are separated, thus permitting the passage of the weft inserter, and it is closed when the warp threads are crossed on top of the weft which has just been deposited.
Since there is, at each given moment considered, within the shed tunnel a plurality of weft inserters, of which that which is just entering the shed has all of the weft thread thereof, while that inserter which is leaving the shed has already exhausted the weft thread thereof, having deposited the same between the warp threads, and the remaining inserters have different amounts of their respective weft threads, it is clear that the groups of healds cannot act synchronously. That is, the healds cannot be displaced half towards one side and the other half towards the other side, since when the threads handled thereby are crossed, they would butt against the inserters which are interposed in their path. Consequently, the healds are progressively actuated, in a snake-shaped path, from the beginning of the shed tunnel, with the result that some groups are separated in front of the inserters while others are closed from behind, all of which takes place continuously and progressively.
In the above mentioned types of looms, the weft thread inserters are actuated by electrical or mechanical devices.
In the electrical type looms, driving is carried out by means of electromagnets functioning inside the shed, each one of which actuates a weft thread inserter element.
This system has two main inconveniences. The first relates to the weight of the electromagnets and their brackets, which results in a great inertia, reducing the speed of the machine and increasing the time necessary for braking. The other inconvenience is that, owing to the fact that the warp threads must be placed between the electro-magnet and the inserter device, they must bear the pressure between such two elements, which causes friction capable of damaging the warp thread.
In known mechanical systems, adjustment of beating up of the weft thread between inserters is effected by the individual advance of the teeth of the reed. These movements of the teeth of the reed are, in the majority of known systems, used to displace the inserters within the shed. One of the biggest problems of such systems, from the textile point of view, is that the individual movement of the teeth of the reed results in a change in density per warp of the fabric being produced, as a result of the play and wear on the teeth. Another important difficulty involves changing the density per warp of the fabric, since in order to achieve such change it is necessary to change all the elements forming the reed. Furthermore, from a mechanical point of view, serious drawbacks are caused by wear of the teeth of the reed through friction with the inserters, as well as the fact that the teeth of the reed must effect a long run or travel in order to achieve beating up of the weft thread. This is a limitation on the speed of the machine.
Furthermore, in known looms of the progressive shed type, there are various ways of feeding the weft to the inserters. However, all such known feeding systems have drawbacks which mainly reside in the fact that various inserters operate simultaneously within the shed. As a result, the inserters must be filled one after the other. Thus, the displacing movement of the weft thread is much higher when the bobbins of the inserters are to be filled than when the weft thread is to be inserted in the sheds.
A known weft feeding system uses a suction effect which draws the weft thread towards the interior of the tank with which each inserter is equipped. Thus, the thread is not wound on any bobbin whatsoever. This system has the inconvenience that the weft thread is not methodically placed within the inserter, and furthermore, when the thread is deposited in the sheds, it undergoes tension irregularities which produce defects in the fabric being produced. Another inconvenience is that derived from the speed to which the weft thread should be subjected during filling of the inserter. This makes measurement thereof difficult, and consequently makes difficult the achievement of an arrangement such that the threads stored in each of the inserters are the same and equivalent to the width of the fabric being manufactured. A further difficulty is due to the fact that since the inserters should operate one at a time at the feeding site, they have very little time in which to effect a thread loading operation. Thus, the feed mechanisms are very delicate, expensive and of short duration. Furthermore, in the inserter feed system under discussion, high quality threads should be used, since these threads are subjected to high tensions when pushed with a force which is sufficient in order to reach the high displacement speeds which are necessary.
SUMMARY OF THE INVENTION
In veiw of all these disadvantages with regard to the driving system of the weft inserters and to the feed system of the inserters, as well as to other not less important characteristics of known weaving machines of the type contemplated, among which the driving means of the healds, the manner in which such driving means are moved, and the manner in which such driving means are connected to the driving means of the inserters are important, the object of the present invention is to provide a series of modifications to the weaving machine, such modifications including the following features.
According to the invention, movement of the inserters in the interior of the shed is achieved by pressure exerted by projections provided in the teeth of the reed on pulling wheels provided in the inserter. The teeth of the reed are free and are so assembled that they can slide freely in an axial direction between stops. The teeth of the reed are subjected to reciprocating movements, and alternately travel short distances in opposite directions.
According to another feature of the invention, the reciprocating movement of the teeth of the reed is achieved by means of cams mounted on an endless chain which covers the width of the loom.
According to another feature of the invention, synchronization of the movement of the inserters with the warp threads is obtained due to the fact that the actuating cams of the healds are also mounted on the endless chain.
According to another feature of the invention, the driving of the teeth of the reed and of the healds is positive in both directions. This is obtained through the provision of the endless chain.
According to another feature of the invention, the guide elements and the support for the teeth of the reed and the healds, are substantially flat, fixed plates which are parallelly arranged and regularly spaced from each other.
According to another feature of the invention, the chains which draw carriers supporting the cams which actuate the healds and the teeth of the reed, can be mutually coupled to each other, so that they are moved together by common drive and driven pinions.
According to another feature of the invention, the bobbins of the inserters are filled by means of telescopic arms which turn radially about the same shafts to which the pinions which drive the chains drawing the actuating cams of the teeth of the reed and the healds are secured. Such radial telescopic arms move the inserters along tracks or rails which guide them from the time that an inserter leaves the shed until such inserter is again introduced into the shed.
According to another feature of the invention, the free end of each telescopic arm is provided with a freely rotating head having a crown which at one side thereof, adapts to a conical core of the bobbin of the inserter. The crown is provided with at least one tooth which meshes with one of several grooves provided in the bobbin, thereby forcing the bobbin to turn at opposite side thereof, the crown has a half ball-and-socket with a hole in the upper part thereof on which the crown can oscilate and held together by a flexible bellow which allows it to oscilate and avoids the loss of air pressure. A pinion forms a part of the head. Such pinion, when engaging with a semi-circular toothed track which is secured to the machine, forces the head assembly to turn.
According to another feature of the invention, the tooth track can be varied and adjusted, so that the bobbin of the inserter will make more or fewer turns during the time provided for refilling of the bobbin. Thus, the length of the weft thread wound on the bobbin may be adjusted, depending on the width of the fabric being produced.
According to another feature of the invention, each telescopic arm is provided with at least one weft thread feeding inlet, together with a corresponding weft thread guide.
According to another feature of the invention each telescopic arm is hollow throughout the length thereof, so that an air current can circulate in the outer portion thereof. Each arm, at the end thereof fixed to the machine assembly, is connected to a negative air pressure chamber, thus establishing a suction at the free end, in order to retain the free end of the weft thread during a time when weft threads are not being fed to the inserters.
According to another feature of the invention, the free end of each radial telescopic arm is provided with ends which can suitably be coupled to cavities with which the chassis of the weft inserters are provided in such a way that the inserters are forced to move when the weft thread is loaded, thus being obligated to carry out the work for which the weft thread feeding and measuring system in known weaving machines provided with multiple inserters has been designed.
BRIEF DESCRIPTION OF THE DRAWINGS
For a better understanding of the changes and modifications contemplated by the invention, the attached drawings, taken with the accompanying description, explain the characteristics of the invention with relation to a specific embodiment involving a dual weaving machine. However, it will be understood that when identical structural and functional principles are used, the scope of the present invention encompasses a simple weaving machine wherein only one length of fabric is produced instead of two, as is illustrated in the drawings, wherein:
FIG. 1 is an elevational view of a dual weaving machine of the continuous insertion progressive shed type which incorporates the characteristics of the invention;
FIG. 2 is a cross-sectional view of the machine, taken on lines II--II of FIG. 1;
FIG. 3 is an enlarged detail view of the portion of FIG. 2 which has been designated by the letter A;
FIG. 4 is a plan view of the separating plates which act as guide means for the various groups of healds and for the teeth of the reed which move the warp threads and the inserters of the weft threads; respectively;
FIG. 5 is a side elevational, schematic view of a portion of the group of plates illustrated in FIG. 4;
FIG. 6 is a perspective view of a heald;
FIGS. 7 and 8 are perspective views of the two types of teeth of the reed used in the loom and which are symmetric in configuration to each other;
FIG. 9 is an elevation showing the relative positions occupied by the two correlative teeth of the reed, represented in FIGS. 7 and 8 when they are superposed in an operative position;
FIG. 10 is a perspective view of one of the carriers supporting heald activating cams and teeth of the reed activating cams;
FIG. 11 is a side elevational view of one of the inserters used in the machine made according to the invention;
FIG. 12 is a front elevational view of the inserter of FIG. 11;
FIG. 13 is an upper plan view of the inserter of FIG. 11;
FIG. 14 is an enlarged sectional detail view of a portion of the winding bobbin of the inserter;
FIG. 15 is an elevational view of a portion of the chain which is used according to the invention to pull the carriers supporting the heald and the teeth of the reed activating cams;
FIG. 16 is a plan view illustrating the way in which the chains are coupled to each other;
FIG. 17 is a schematic cross-sectional view of the shed tunnel, taken along lines XVII--XVII of FIG. 2;
FIG. 18 is a perspective view of a coupling projection of the main elements of which the shed tunnel of the weaving machine is composed;
FIG. 19 is a cross-sectional view of the shed tunnel taken along lines XIX--XIX of FIG. 2;
FIG. 20 is a perspective view of a portion of the shed tunnel, the cover thereof having been omitted so that its construction and mode of operating can be better seen;
FIG. 21 is an upper plan view of a portion of the shed tunnel, the upper part of the casing of the tunnel having been omitted so that the relative arrangement which, at each given moment, is occupied by the cam rails, the inserters and the healds, can be clearly seen;
FIG. 22 is an enlarged upper plan view of the portion of the shed tunnel which is indicated with the letter B in FIG. 2;
FIG. 23 is a plan view, at the shed tunnel level, of the system for feeding the weft threads to the inserters;
FIG. 24 is a schematic, vertical partial section of the machine taken from one of the ends thereof, further illustrating the system for feeding the weft threads to the inserters;
FIG. 25 is an enlarged detail plan view of a portion of FIG. 23;
FIG. 26 is an enlarged perspective view of one of the arms which constitute the base of the system for feeding the weft threads to the inserters; and
FIG. 27 is a schematic perspective view illustrating the manner in which the inserters are inserted and the manner in which they function within the shed.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings, and with the above discussion in mind, the invention relates to a weaving machine of the type having continuous insertion through a progressive shed.
FIG. 1 illustrates a complete machine of the above type. The machine comprises a warp thread beam 1, a woven fabric beam 2, and a shed tunnel 3 in which the warp threads are controlled by a plurality of healds which are positioned within planes perpendicular to the warp, and which move linearly in opposite directions in planes perpendicular to the warp.
In the conventional manner, inserters are combined with the healds and travel along the interior of the shed, at regularly spaced intervals and with synchronous movement. Each of the inserters deposits a weft thread between the warp threads which open up in front of each inserter and cross at the back of such inserter, on top of the weft thread deposited thereby.
The changes contemplated by the invention permit, among other things, the construction of a dual weaving machine including a minimum of additional operative elements, and reside in three main features, i.e. the manner in which the inserters are actuated, the manner in which the healds are activated, and the manner in which the weft threads are fed to the inserters.
According to the invention, the shed tunnel 3, the external casing only of which has been represented in FIG. 1, has dual tunnels (see FIG. 2), each of which has within its interior two alignments of shield plates. These alignments of plates have both been labeled 4 in FIGS. 2, 3, 18 and 20, and the pluralities of plates forming the alignments 4 have been illustrated in detail in FIGS. 4, 5, 18, 19 and 20, wherein they have been labeled 5 and 6, respectively.
The plates 5 and 6 are all equal in configuration and are symmetrically arranged. The plates 5 of one alignment 4 are coplanar, in a transverse direction, with the plates 6 of the other alignment 4.
The plates, as shown in FIG. 5, are regularly spaced from each other, by means of blocking rods 7 and 8 which transverse the plates through holes 12 and 13 provided at the upper and lower plate ends, respectively. Separators 9, which maintain the plates regularly spaced, are positioned on the rods 7 and 8.
Plates 5 and 6 furthermore have extending therethrough a plurality of passing holes 14 which are traversed by bars 10. The plates also have, at the bottoms thereof, rectangular windows 15 which are traversed by a bar 11 having the same section and dimensions as windows 15.
The healds 16, one of which is shown in perpsective in FIG. 6, are made of the same material and have the same thickness as plates 5 and 6 and are mounted successively in groups between adjacent plates 5 and 6. The separating rods 10 maintain the levels or groups of healds separated from each other. The relative positions occupied by the healds 16, in relation to the plates 5 and 6, can be seen in FIGS. 19 and 20.
Each heald has an eye 17 through which a warp thread passes. Each heald 16 handles one or more warp threads of the fabric, and the movement of the warp threads transverse to the shed tunnel, due to transverse movement of the healds, causes crossing and uncrossing of the warp threads, or opening and closing of the shed, which with the insertion of the weft threads, produces weaving of the fabric.
The teeth of the reed are mounted on bars 11 between successive pairs of separating plates 5 and 6 adjacent the lower parts thereof. The purpose of the reed is to maintain the warp threads of the healds separated, to provide a guide for the inserters, and to activate the inserters so that they advance at the same rate as the healds.
The teeth of the reed used in the loom according to the invention are represented in detail in FIGS. 7 and 8, from which it can be seen that they are of two types, equal in configuration, but mirror images of each other.
The teeth 18 and 19 are alternately arranged, so that when superposed, they form a configuration as illustrated in FIG. 9.
In FIGS. 7, 8 and 9 it can be seen that each member 18 and 19 has two elongated orifices 20 which correspond, with regard to position, to orifices 15 of the plates 5 and 6, although orifices 20 are longer in the longitudinal dimension thereof then orifices 15 and the rectangular bars 11. Therefore, each member 18 and 19 can be displaced transverse of the shed tunnel, between two extreme positions.
The teeth of the reed have recesses 21 in the ends thereof, thus forming cam contacting ends 22, 23, 24 and 25, as will subsequently be discussed.
Each member 18 and 19 has, in the lower central portion thereof, a groove 26, and adjacent such groove, a downwardly extending projection 27.
As seen in FIG. 9, the grooves 26 and the projections 27 of the members 18 and 19 cooperate to form a channel 28 which acts as a support or rail for pressure wheels of the inserters. The channel 28 is partially defined by the projections 27 which, upon transverse movement of members 18 and 19, cause advancement of the inserters.
Driving of the healds is carried out by cam carriers, one of which is illustrated in FIG. 10, and several of which incorporated in the assembly in operative positions are illustrated in FIGS. 20 and 21. The carriers move parallel to the shed tunnel, along both sides of each tunnel thereof. Cams mounted on each carrier successively push the healds transversally of the tunnel. For each unit of length, e.g. one meter, of the shed tunnel there are provided a specific number, e.g. eight, pairs of cam carriers, forming two alignments, one on each side of each tunnel (see especially FIG. 21).
The carriers for each tunnel advance simultaneously and in parallel in the same direction, and the cams of the carriers on one side approach different levels of the healds then the cam of the respective carriers on the other side. Thus, each heald during operation is inscribed or moved continuously in a snake-like manner.
Each carrier incorporates, depending on the type of weaving involved, a specific number of cams. It should be emphasized that each cam of each carrier is formed by a band or endless belt 29 which turns between two pulleys 30 and 31. The relative spacing of the axes of the pair of pulleys 30 and 31 with respect to the longitudinal direction of the shed tunnel determines the path and amount of displacement of each heald (see again FIG. 21). When the displacement direction of the carriers is that indicated by arrow 38, the manner in which the belts 29 displace the healds located at different levels can be seen.
Grooves formed in the ends of each heald (see FIG. 6) allow the heald ends to be efficiently engaged both by cam belts 29 and 36 (see also FIG. 19).
In order to impart movement to the pulleys 30 and 31 of each cam carrier, the shaft 32 of one of the pulleys has an extension to which a small pinion 33 is secured.
Pinion 33 meshes with a rack 39 (see for example FIG. 20) one of which is fixed and arranged along each side of each tunnel of the shed tunnel. As a result, when the carrier advances by being moved by a chain 42, as will subsequently be discussed, rotation of pinion 32 causes pulley 30 and belt 29 to be rotated.
The carriers are furthermore guided throughout their travel and thus are provided with tracking elements such as wheels 34 and 35 which ride over cooperative tracks 40 and 41, as shown in FIG. 20, tracks 40 and 41 extending along each side of each tunnel.
The teeth of the reed are activated simultaneously with the healds by other cams, i.e. reed cams, which are mounted on the carriers and which are formed by two wheels 43 and 44 which are placed at different levels.
The carrier represented in FIG. 10 has two heald cams which correspond to two of the four heald levels and two reed cams. It can easily be understood however, that the number of cams of each carrier can be modified, depending on the number of levels of healds included in the shed tunnel. Each heald cam includes an endless belt to maintain the shed open for a sufficient time to enable the inserter to pass.
The inserters move simultaneously with the carriers. The inserters are shown in detail in FIGS. 11, 12, 13 and 14, and in an operative position within the shed in FIGS. 19, 20, 21 and 27.
The number of inserters corresponds to the number of pairs of carriers (8 per meter in a preferred embodiment).
The purpose of each inserter is to introduce a weft thread into the interior of the shed, and at the same time to perform beating up of the weft thread deposited by the proceeding inserter against crossed warp threads at a moment when the shed is open.
The inserter is advanced by being pushed by projections 27 during the transverse, cyclic and inverse displacement of the teeth of the reed caused by wheels 43 and 44 upon movement of the carriers.
The inserters, as can be appreciated from the above discussion, replace the shuttle and the batten or frame of a conventional loom, wherein the reed is employed to perform beating up.
The inserter (see FIGS. 11 to 14) includes a weft thread bobbin 45, two pressure wheels 46, two pulling wheels 47, and a frame 49 mounting such elements. The weft bobbin 45 has a plurality of raised flanges 48 (see especially FIG. 14) wherein the end of the weft thread to be wound is hooked, by means which will subsequently be explained. The periphery 50 of bobbin 45 is purposely designed to beat up the weft thread deposited by a preceeding inserter.
The pressure wheels 46 circulate through the channel 28 formed by the grooves 26 in the teeth of the reed (see FIGS. 7, 8 and 9).
The pulling wheels 47 are contacted by the projections 27 of the teeth of the reed (see FIGS. 7, 8 and 9), thus resulting in a pushing action which displaces the inserter along the shed tunnel, at the same rate as the carriers, as can particularly be seen in FIG. 21.
In other words, and with particular reference to FIGS. 7 through 9, 19 and 20, as the two carriers on opposite sides of each tunnel move therealong, the upper reed cam wheels 43 contact cam contacting edges 22 and 25 of members 18 and 19, respectively, thereby forcing members 18 and 19 away from each other. Thereafter, the lower reed cam wheels 43 contact the cam contacting edges 23 and 24 of members 18 and 19, respectively, thereby forcing members 18 and 19 inwardly toward each other. This results in projections 27 contacting the pulling wheels 47 of the respective inserter and moving the inserter along the tunnel along with the respective carriers.
In order to describe in detail the manner in which the cam carriers are moved, thus causing the transversal cyclic displacement of the healds and the advance of the inserters, reference will be made to FIGS. 2, 3, 15, 16, 20, 21 and 22 which illustrate the chains which move the carriers, the pinions activating the chains, and the means for allowing the chains to be separated within the tunnels and to be rejoined to each other so as to be moved together by the pinions.
At adjacent ends of each tunnel (two tunnels since the weaving machine described id dual) there is a pinion. One of the two pinions is visible in FIG. 2, although the position occupied by the other pinion will be understood as being under the frame carrying the thread bobbins shown at the lefthand side of the drawing. Around the two pinions are mounted two chains 42, which are particularly visible in FIGS. 3 and 22. The two chains each have a singular construction and are capable of being complemented, with the links of one chain meshing with the links of the other chain, so that the two chains may be moved as a single element by the pinions (see FIG. 16).
Wedges 51 are provided at each end of each tunnel to separate the two portions of the dual chain within the length of each tunnel, and determine the amount or distance of such separation. One of the wedges 51 can be seen in FIG. 3. The tapered end of the wedge also allows the two chains to be joined at the end of the tunnel, i.e. at the point at which the dual chain starts to be meshed with the pinion.
FIG. 3 clearly illustrates how the two portions of the dual chain are separated from each other, due to the intervention of the wedges 51, in the space between the two pinions. FIG. 22, on the contrary, illustrates how the chains are coupled to each other around the pinions.
The specific construction, generally in the shape of a V formed by end peaks separating a valley, of the links of each chain, as well as the way in which the two chains are coupled to each other, can be seen in FIG. 16. In this figure, as well as in FIG. 15, it can be seen that adjacent links are joined at end peaks by means of rollers 52, which when the two chains are joined contact the central zone or valley of the opposed links of the other chain, thus avoiding friction. Alternate links of each chain are provided with studs 53 to which the cam carriers are fixed. Thus, movement of the chains causes movement of the carriers.
The time during which each pair of carriers moves past the pinions which move the chain, is used by the respective inserter (which advances simultaneously with the carriers but is moved by independent means as explained below) to be rewound with weft thread.
The travel of the cam carrier, as well as that of the inserters, around the periphery of the pinions is facilitated by special guides which are provided as a prolongation of the tracks provided at both sides of the tunnels. These guides furthermore aid in feeding the weft thread to the inserters while they travel along the guides.
Between the entrance of the tunnel and the exit of the feeding devices of the inserters, there is provided a thread cutting element.
FIG. 17 shows the guides which help guide the cam carriers and the inserters around the periphery of the pinions which move the chains. There is shown a front view of an inserter 54 positioned between an upper guide 56 and a lower guide 57. The upper guide 56 also guides the cam carriers 55. Upper guide 56 has a gliding surface 58 of the guide. The upper guide 56 allows the two carriers of each carrier pair to be in contact, as they are forced together by the two chains being joined together. A groove 59, in which the pressure wheels of the inserters are housed, is formed in the lower surface of the upper guide 56. The bobbin 45 of the inserter rests on the lower guide 57.
It should be emphasized that the gliding surface glider 58, arranged at the upper part of guide 56, can receive directly thereon the pairs of reed cams or wheels of each pair of carriers, thus forming a track of antifrictional material, to facilitate sliding.
FIG. 18 illustrates a shed tunnel, a cam carrier 55 (together with the connecting element to the drawing chain, not represented), the rack 39 and the guides 40 and 41 of the cam carrier, inserters 54, various teeth of the reed 18 and 19, a group of healds 16 and a pair of alignments 4 of plates 5 and 6 which define the length of the shed tunnel. Portions of the semi-circular guides 56 and 57 are also represented, which guides are provided below the chain pulling pinions.
FIG. 19 shows the separating plates 5 and 6, the healds 16, the teeth of the reed 18 and 19, the warp threads, the cam carriers 55 with their heald and reed cams, driving pinions 33, the rack 39 and tracking means 34 and 35. Also, the casing which protects both sides of the shed tunnel and the carriers can be clearly seen. Below the teeth of the reed 18 and 19, the inserter 54 can be seen arranged between the teeth and the fabric 60.
FIG. 19 clearly shows how carriers 55, each one of which has two heald cams 29 situated at different levels, act on the alternate levels of healds 16, in such a way that cams 29 displace the healds 16 in opposite directions, opening the healds in order to allow passage of the inserter (i.e. open shed position which is that represented in the FIG. 19) and closing the healds behind the inserter and crossing the warp threads on top of the weft thread deposited by the inserter (i.e. at the functional moment following that illustrated).
This functioning of the cam carriers can be even better understood from FIG. 20 which corresponds to a portion of the shed tunnel seen in perspective. It will be seen that the healds situated at the same level, whether they are under the action of the cam of a given carrier or under the action of a respective cam of the carrier situated at the opposite side of the shed tunnel, are moved towards one side or the other of the tunnel.
FIGS. 19 and 20 likewise illustrate how the teeth of the reed, due to their peculiar construction and to the arrangement of the assembly as well as to the combined action of the cams 43 and 44 of each pair of carriers, are laterally alternately reciprocated, thereby imparting forward movement to the inserter 54, due to the pressure exerted by the projections 27 of the teeth of the reed on the pulling wheets 47 of the inserter.
From FIG. 21 it can be seen that the cam carriers operate in pairs, an inserter always being positioned between each pair. The shed is opened immediately before the inserter and closed immediately thereafter, as indicated by the snake-like or semi-sinusoidal lines formed by the eyes 17 of the healds 16.
As the chains 42 advance, belts 36 of carriers 35 pass along the shed tunnel and contact the ends of the healds 16, thus maintaining the same in the positions thereof established by the respective cam belts 29, until the inserters pass thereby.
Simultaneously, the reed cams (not visible in FIG. 21) move the teeth of the reed inwardly, so that the projections 27 push the pulling wheels 47 of the inserter 54, thus causing the inserter to advance. With this advance, a weft thread is placed between the warp threads, and beating up of the weft thread inserted by the preceding inserter is produced.
The specific manner in which the inserters function within the shed, each one depositing its weft thread between the warp threads, while also beating up the weft thread deposited by the preceding inserter, can clearly be seen from the schematic view represented in FIG. 27.
Feeding of the weft thread to the inserters is carried out by means of the assembly of elements shown in FIGS. 23 to 26.
FIG. 23 illustrates a shaft 61, which is the shaft of the chain pulling pinion shown on the right-hand side of FIG. 2.
Mounted around shaft 61 are a plurality of radial arms 62, each of which is provided with means to be coupled to an inserter. Each inserter 54 is contacted and carried by one of the arms 62 when it leaves one of the shed tunnels. Then the inserter 54 is displaced by arm 62, which also carries the end of a thread 63 which will be fed to bobbin 45 of the inserter.
Each arm 62 is comprised of two telescopically coupled portions 64 and 65, one 64 of which is fixed, while the other 65 is urged radially outwardly by a spring 66. Each arm, when not in contact with a respective inserter, is longer than the radius of the semi-circular portion of the path of the inserter from the time when it leaves the shed tunnel until it enters the opposite shed tunnel.
Each arm 62 has, at the forward end thereof, a fork 67 which bears against the frame of the respective inserter and thereby moves the inserter in the semi-circular path. Between the arms of the fork there is positioned a rotating head 68 and a pinion 69 integral therewith.
The pinion 69 of each arm 62 meshes with a substantially semi-circular rack 70 provided along the curvilinear path followed by the pinions. Thus, pinion 69 rotates, thereby causing the head 68 to rotate. When the fork 67 bears against the frame of the inserter 54, head 68 is coupled to the bobbin 45 of the inserter 54.
In each arm 62 there is installed a thread guide 71, by means of which a weft thread 63 is drawn from a storage bobbin 72 provided in an upper frame, one bobbin 72 being provided for each of the arms.
The weft thread 63, after having passed through the thread guide 71, is drawn into a hollow end of the rotating head 68, as shown particularly in FIG. 26. The hollow end of head 68 communicates through portion 65 of the arm, which is also hollow, with a source of reduced pressure (not shown).
As a result of the above arrangement, when the head 68 is coupled to the bobbin 45 of the inserter 54, a portion of the thread 63 is positioned in the angular path of the raised flanges 48 on the bobbin 45. Thus, when the bobbin 45 starts to rotate due to coupling engagement with rotating head 68, and as a result of the meshing of pinion 69 with the rack 70, the thread 63 is grasped by flange 48 and wound on the bobbin.
At the end of the travel of pinion 69 along the rack 70, the head 68 stops rotating and thread is no longer wound on the bobbin. A cutting element 73, shown in FIGS. 18 and 23, cuts the thread when the inserter is transferred from the corresponding arm 62 and is picked up by the teeth of the reed and starts to move along the new shed tunnel.
FIG. 24 illustrates the feeding of the inserters, wherein the pinion which moves the chains pulling the cam carriers and the cam carriers have not been illustrated in order to simplify the view. This figure shows the position occupied by the feeding bobbins 72, which are also partially represented in FIG. 2 and which can be seen at both sides of FIG. 1.
FIG. 25 illustrates in functional detail one of the arms 62. It can be seen clearly in FIG. 25 how each arm 62 is coupled to an inserter 54 and how the winding bobbin 45 is coupled to the rotating head 68.
FIG. 26 shows a detailed view of one of the arms, and particularly the construction of head 68, which is a flexible bellow capable of adapting its position on the bobbin of the inserter, when coupling takes place. Head 68 also has on the outer periphery thereof a tooth 74 which, in a preferred embodiment, is coupled to anyone of a series of grooves made in the periphery of the winding bobbin of the inserter to avoid relative slipping during the winding operations.
Various modifications may be made to the above described specific structural arrangements without departing from the scope of the invention.
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A continuous insertion weaving machine of the progressive shed type includes two coplanar endless chains which are supported and driven by two pinions. Coupling and uncoupling of the chains to the pinions is achieved by deflecting elements which cause a separation of the straight paths of the two chains. The chains move parallely along two shed tunnels which extend along the straight paths of both chains. The chains comprise means for moving driving elements of the shed tunnels, which driving elements, accompanied by the chains, act repeatedly in a cyclic manner within both shed tunnels.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This present application is a divisional application and claims full benefit of U.S. application Ser. No. 13/192,424 filed on Jul. 27, 2011 and claims the full benefit and priority of U.S. Provisional Application Ser. No. 61/368,231, entitled “Method and System for Treating Patients” filed on Jul. 27, 2010.
BACKGROUND
[0002] 1. Field of the Invention
[0003] The present invention relates to systems and methods for treating patients by administration of a predetermined sequence of physical manipulations to the patient's body. More particularly, the present invention provides long-term resolution of symptoms by correcting movement dysfunctions of certain joints in the patient's body, including manipulation of a predetermined sequence of joints in the patient's extremities. Disciplines that would be inclined to utilize embodiments of the present invention include chiropractic, naturopaths, sports medicine, physical therapy, professional and collegiate trainers, as well as applications to veterinary medicine.
[0004] 2. Description of the Related Art
[0005] Since the late 1800's, the chiropractic health care discipline has provided treatment options to patients to address a wide variety of disease processes and neuromusculoskeletal conditions. The treatment has often focused on correcting “subluxations” through a variety of manipulation techniques, some of which may be performed entirely by controlled administration of force by the chiropractic physician, and others through assistance of certain mechanical and/or electrical devices. As defined by the World Health Organization, a chiropractic subluxation constitutes “a lesion or dysfunction in a joint or motion segment in which alignment, movement integrity and/or physiological function are altered, although contact between joint surfaces remains intact. It is essentially a functional entity, which may influence biomechanical and neural integrity.”
[0006] Common chiropractic patient management involves spinal manipulation and other manual therapies to the joints and soft tissues. Spinal manipulation, which chiropractors may also call “spinal adjustment” or “chiropractic adjustment,” is the most common treatment used in chiropractic care to remove nerve interference, restore patient overall health, and also relieve pain. Complementary treatments may also include rehabilitative exercises, health promotion, electrical modalities, complementary procedures, and lifestyle counseling.
[0007] An array of diagnostic methods and treatment techniques were developed in the chiropractic profession to identify and correct chiropractic subluxations. Popular chiropractic treatment methods include: Diversified, Gonstead, SOT, Motion Palpation, Applied Kinesiology, Activator Method, Grostic, DNFT, Atlas Orthoginal, and Toftness. Some techniques start from the upper spine and work towards the lower spine, others from the lower spine to upper spine. Some focus on the upper and others focus on the lower spine. All chiropractic techniques involve random treatments of the spine.
[0008] Traditional chiropractic correction of the subluxation with random techniques usually involves a lengthy process of repetitive treatment which requires patients to receive regularly scheduled adjustments for months at a time. Patients are informed that since most conditions arise over long periods of deterioration, an extended treatment will program will be needed to regain the “momentum” required through repeated adjustments to alleviate the body's tendency to return to its subluxated state.
[0009] Patient compliance issues led to the formation of practice management companies designed to produce successful doctors who have learned specific methods to keep patients focused on their lengthy treatment programs. Testimonials of doctors who have doubled their monthly incomes with such patient management techniques can be found in most chiropractic newspapers and magazines. These programs emphasize that if the chiropractic physician can manage patients and keep them on their programs, the physician can be successful and wealthy.
[0010] Trust issues have surfaced as patient compliance became more the focus for some practitioners in the chiropractic profession, rather than patient welfare. Insurance companies have become less tolerant of treatment standards in the chiropractic discipline, and physical therapists are challenging the expertise of chiropractic physicians. Association with other health care professions such as allopathic medicine needs to be strengthened. Patients can become disenchanted with the costs associated with repetitive lifelong treatment, and with the extended treatment time needed to address health issues. The chiropractic profession is suffering from these and other major challenges. If the approach to chiropractic care were more streamlined and more efficient, both the patient and the chiropractic profession would benefit. For this to happen, a new model is needed.
[0011] Therefore, what is needed is a chiropractic treatment system that provides for expedited patient healing with a predicable number of treatments. What is also needed is a chiropractic treatment method that provides for reduction of sports injuries through coordinated adjustment of body structures. What is also needed is a method to enhance freedom of motion in motion-absorbing joints and components of the body to promote wellness and provide for long-term treatment and prevention of subluxations.
SUMMARY OF THE INVENTION
[0012] There is provided a system and method for treating a patient by administering a predetermined sequence of adjustments to a patient's body. Unlike the unstructured or random application of adjustments used in prior art chiropractic treatments, the treatment sequences and provided for herein unlock function of dysfunctional joint systems in a manner analogous to a combination lock mechanism. Disciplines that may utilize embodiments of the present invention include chiropractic, naturopaths, sports medicine, physical therapy, professional and collegiate trainers, as well as aspects of veterinary medicine. Through applications of the method of the present invention, patients may receive a predetermined number of treatment applications, and have long-lived or substantially permanent results from the treatment without the need for ongoing adjustments to spine or other body structures. In some instances, after receiving treatment, patients that continue to walk on hard, flat surfaces (which most patients will routinely encounter) may still benefit from periodic treatment of the foot/ankle areas.
[0013] Each day, many people walk an average 10,000 steps. Each step produces a ground reactive force of approximately 110% of body weight. This force is coupled through the foot and transmitted up the leg at approximately 200 miles per hour. The average amount of force a 200 pound individual would encounter in one day is estimated at 640 metric tons, or 700 U.S. tons.
[0014] The study of the human gait cycle shows that beginning with heel strike, feet adapt to the ground surface walked upon, and likewise, the feet absorb the shock of each step. This absorbing of shock slows down the ground reactive force so the surrounding tissues of the leg can further dampen it. The result is reduced stress on the musculoskeletal system.
[0015] The absorption of force is dependent on proper joint function throughout the foot and ankle. These joints must be able to move within their ranges to efficiently absorb shock. Unfortunately, the average foot and ankle joints do not move within their ranges, since they experience an abundance of joint dysfunction.
[0016] This joint dysfunction is caused, at least in part, by the nature of modern-day walking surfaces. Before paved walkways and solid flooring were commonplace, humans used to walk on irregular surfaces such as dirt, sand, moss, rocks, and tree roots. The normal deformation of the feet when traversing these uneven surfaces promoted more flexibility in the joints of the foot and ankle while walking. Additionally, natural surfaces were often more cushioned, which further reduced the stress coupled to the human body from the process of walking.
[0017] The surfaces we now walk on, concrete, asphalt, hardwood, tile and marble, are less forgiving and more rigid. These flat, hard surfaces do not promote joint flexibility, rather they promote joint dysfunction. Without proper joint function the foot and ankle are unable to efficiently absorb and dissipate ground reactive forces. This leads to pathological amounts of stress repeatedly travelling throughout the musculoskeletal system. Further, in an attempt to stabilize itself, the spine tightens muscles and compresses joints to adapt to this continuous force. The result is a degenerating spine that lacks function and mobility, creating an environment for injury.
[0018] It is known in the literature that joints in the sacroiliac region react to oncoming force by compression of the sacrum on the ileum. This takes place through a series of surrounding muscle contractions compressing the sacroiliac joint together, as the body “braces” for impact. Studies suggest that the body attempts to compress the joints together to enhance stability.
[0019] Underlying theories of the present invention are similarly founded on the following principles: modern-day humans are surrounded by an abundance of flat, hard, and mostly horizontal walking surfaces. Walking and running in this environment causes the joints in the feet and ankles to become dysfunctional. As a result, we can no longer absorb the shock from ground reactive forces efficiently. Every day, just from walking and related activities, approximately 700 tons of unimpeded force travel up legs, into the pelvis and spine. In an attempt to brace itself from repetitive heel strikes and the generated force, the human body compresses joints together throughout the musculoskeletal structure to provide stability. This compression of joints involves the feet, ankles, knees, hips, pelvis, spine, shoulders, elbows and wrists.
[0020] In the present model of chiropractic, in prior art approaches a practitioner will examine a new patient's spine and determine the presence of multiple joint dysfunctions, or subluxations. Random adjustments will be administered to the patient's spine based on a specific or combination of chiropractic techniques the particular doctor practices. The patient will leave the clinic and return to the surrounding “hardscape” which promotes further bracing and joint compression. It is with little surprise that the following day, the patient returns for treatment with the same joint dysfunction as before. The traditional reasoning of the chiropractic profession is repetitive, long term treatment is necessary to correct a condition which has been long standing.
[0021] In contrast, methods and systems of the present invention address the underlying issues that arise from the patient's traversal of surrounding “hardscape” surfaces. In one embodiment, joint dysfunctions within the gait cycle can be corrected to allow for more efficient transfer of forces, less bracing, and reduced joint compressions. For example, when normal motion is restored to the foot, the improved strike force handling of body structures allows the spine to flex and operate normally again, restoring normal nerve supply and joint function throughout the body. Methods of the present invention were developed to restore normal function by applying certain treatments in a specific order. The developed methods and systems of the present invention will allow the patient's body to respond favorably to a “pattern” of adjustments with an automatic correction of joint dysfunction. In a preferred embodiment, the patterns that are utilized by the practitioner treat the body systems in the order that follows the natural shockwave that propagates from the striding foot impacting the ground and travels up the leg through the pelvis and into the opposite body side in the thoracic, arm, and upper body regions. Treatment of the body systems related to the first stride impact is referred to herein as the “primary treatment cycle.” The second leg and upward body structures is treated in a similar manner in the order of shockwave propagation as the shockwave were to propagate from the second impacting foot into the body. Treatment of the body systems related to the second foot stride is referred to herein as the “secondary treatment cycle.” In a preferred embodiment, the patient's dominant leg (or dominant side) is determined from a pre-treatment evaluation, wherein the primary treatment cycle begins with the dominant foot/leg, and once the primary cycle is complete, the secondary treatment cycle begins with the non-dominant foot/leg and is applied upwards into the related body structures. In the preferred embodiments, patterns of adjustments commonly produce a permanent or very long-lasting correction of joint dysfunction in various areas of the patient's body.
[0022] In traditional chiropractic practice, physicians are taught various methods to adjust the upper thoracic region in their patients. Subluxations are commonly present in the spine at levels T1-T2, T2-T3, T3-T4. Using Gonstead and Diversified techniques, these joints can be mobilized with the practitioner's thumb pushing on the individual vertebrae. This is called a “thumb move.” This area can also be mobilized by pushing with the pisiform in the heel of the hand. This referred to as the “modified diversified pisiform.” These random approaches are very effective in restoring joint function to the upper thoracic region. However, the corrections are temporary and require repetitive treatments which offer no permanent benefit.
[0023] Embodiments of the present invention make persistent corrections to various body structures without direct physical manipulation of those body structures. For example, application treatment modalities of embodiments of the present invention allow the body structures to work together to achieve comprehensive readjustment, such as the self-adjustment of the thoracic spine without direct manipulation or treatment of the thoracic spine. A preferred embodiment of the present invention provides successful and persistent treatment results in 18 treatment steps consisting of a primary treatment cycle followed by a secondary treatment cycle; however, the practitioner may make adjustments to the treatment cycles to achieve the desired results in fewer or more treatment steps. On average, with the 18-step treatment approach, patients report substantial relief from symptoms, and such reports include favorable resolution of adverse symptoms related to: back and neck; hip and knee, foot, shoulder pain; tennis elbow; carpal tunnel; hamstring and groin injuries; headaches; migraine headaches; dizziness; disc problems; plantar fasciitis; Achilles tendonitis; and overall health. Further, treatment methods of the present invention assist patients with avoiding or delaying hip or knee replacement surgery when a diagnosis of joint degeneration has been made.
[0024] Application to Sports.
[0025] Treatment methods and systems of the present invention increase athletic ability by restoring normal joint mechanics, muscle and nerve function. Further embodiments of the present invention help treat and prevent common injuries that limit athletic performance, such as muscle strains of the groin and hamstring, as well as injuries to the plantar fascia and Achilles tendon. When a joint loses function, its corresponding muscle attachment (groin or hamstring, for example) becomes strained by the motion of surrounding joints. Once optimal function is restored to the affected joint through embodiments of the present invention, muscle performance exceeds the physical demands required in competitive sports activities.
[0026] One application of treatment methods of the present invention aids in reducing injury to both the hamstring and groin muscles during sporting activities by improving pubic symphysis mobility. In the human body, the respective ends of the hamstring and groin muscles are attached to the pelvis next to the pubic symphysis. The pubic symphysis is located in the front of the pelvis, behind the pubic area. The other respective ends of each muscle attach to the leg. When the pubic symphysis becomes locked or otherwise immobile, the corresponding muscles no longer track with the moving leg, which makes the muscles more susceptible to injury. Restoring normal motion to the pubic symphysis through methods of the present invention operate to decrease the occurrence of hamstring and groin injuries.
[0027] In a normally functioning pubic symphysis, the hamstrings and groin muscles will move together with the leg and the pelvis. If the pubic symphysis is locked or otherwise not functioning properly, the pubic bone is incorrectly anchored and causes improper motion of the leg, and problems arise with the attachment of the groin and hamstring muscles. In the case of a dysfunctional pubic symphysis joint, the hamstring and groin are only moving where they are attached to the leg, and in sports activities, where there is freedom of movement of the leg but improper coordinated movement of the pelvis, issues arise that may lead to injury such as hamstring and groin pulls and tears. While chiropractic practitioners have in the past performed adjustments to the pubic symphysis, mostly such adjustments resulted in the joint becoming re-locked in as soon as one day. However, it was found that a coordinated and structured set of adjustments, including the lower extremities, resulted in a longer lasting or permanent correction of pubic symphysis joint dysfunction. As provided herein, methods and systems of the present invention serve to prevent sporting injuries by restoring proper coordinated movement of the hip and leg through structured adjustments that provide long-term mobilization of the pubic symphysis.
[0028] In a preferred embodiment, a treatment method comprises administering to a patient a sequence of treatment steps in a primary treatment cycle, each of the treatment steps respectively comprising one or more treatment patterns, the treatment patterns respectively comprising one or more physical manipulations of body structures by a health care practitioner executed in a predetermined order; administering to a patient a sequence of treatment steps in a secondary treatment cycle, each of the treatment steps respectively comprising one or more treatment patterns, the treatment patterns respectively comprising one or more physical manipulations of body structures by a health care practitioner executed in a predetermined order; and wherein the sequence steps of the primary treatment cycle are applied starting from a bottom side of the dominant side of the body and moving toward the patient's upper body non-dominant side; and the sequence steps of the secondary treatment cycle are applied starting from a bottom side of the non-dominant side of the body and moving toward the patient's upper body dominant side. The dominant side of a patient's body may be determined by the practitioner before administering treatment, and may be performed by any desired method such as positioning the patient in a supine position with legs extended, alternatively moving the patient's knees towards the patient's chest, and monitoring the range of motion during the movement, and determining the dominant side of the patient corresponds to the side of the patient where the patient's leg encountered the most restrictive range of motion.
[0029] The sequence of treatment steps may be applied in any desired order. In a preferred embodiment, the sequence of treatment steps in the primary treatment cycle comprises sequential treatment of the patient's dominant-side foot, dominant-side knee, dominant-side hip, dominant-side pubic symphysis, dominant-side lower sacrum and upper ilium; non-dominant-side upper sacrum and upper ilium, non-dominant-side proximal clavicle, non-dominant-side shoulder, non-dominant-side elbow, and non-dominant-side wrist. In another embodiment, prior to the treatment of the patient's non-dominant-side proximal clavicle in the primary treatment cycle, the patient's dominant-side sacrotuberous ligament is treated with Logan-Basic Technique then the patient's non-dominant-side sacrotuberous ligament and/or long dorsal ligament is treated with with Logan-Basic Technique.
[0030] In a preferred embodiment, the sequence of treatment steps in the secondary treatment cycle comprises sequential treatment of the patient's non-dominant-side foot, non-dominant-side knee, non-dominant-side hip, non-dominant sidepubic symphysis, non-dominant-side lower sacrum and upper ilium, non-dominant-side upper sacrum and upper ilium, dominant-side proximal clavicle, dominant-side shoulder, dominant-side elbow, and non-dominant-side wrist. In an alternate embodiment, prior to the treatment of the patient's dominant-side proximal clavicle, patient's non-dominant-side sacrotuberous ligament is treated with Logan-Basic Technique, then the patient's dominant-side sacrotuberous ligament and/or long dorsal ligament are treated with Logan-Basic Technique.
[0031] Methods of the present invention may execute treatment steps on any desired schedule. For example, in a preferred embodiment, each of the treatment steps of the primary treatment cycle are administered to the patient no more often than one treatment step per day, and each of the treatment steps of the secondary treatment cycle are administered to the patient no more often than one treatment step per day.
[0032] The number of treatment steps per treatment cycle may be devised by the practitioner to satisfy any desired treatment goal; for example, in one embodiment nine treatment steps are administered to the patient in the primary treatment cycle and nine treatment steps are administered to the patient in the secondary treatment cycle, and a total treatment sequence may include any desired number of treatment steps such as 17, 18, or 20 treatment steps. Preferably, only one treatment steps is performed on the patient in any calendar day, but as desired to meet a treatment goal such as total treatment length or sufficiency of unlocking joints, a plurality of treatment steps may be performed on the same calendar day. Through embodiments of the present invention, the patient is treated without applying direct treatment manipulation to one of the cervical spine or the thoracic spine, yet these structures of the patient's body are unlocked through the body's own response to the applied treatment sequences.
[0033] Another embodiment includes a method for treating subluxations in a joint of an organism, the method comprising providing adjustments to structures in a dominant foot of the organism, followed by a non-dominant foot of the organism, whereby improved motility in the foot structures mitigate shock impulses that are coupled to the joint from the feet when the feet strike a hard surface. In yet another embodiment, a method for reducing injuries in a living organism comprises providing adjustments to structures related to a foot and leg of the organism thereby improving flexibility of a public symphysis joint in the organism.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] FIG. 1 illustrates a partial skeletal structure of a patient being treated with methods of the present invention, with the following treatment sequence locations identified: Sequence 1, Dominant-side Foot; Sequence 2, Dominant-side Knee, Sequence 3, Dominant-side Hip; and Sequence 4, Dominant-side Pubic Symphysis.
[0035] FIG. 2 illustrates a partial skeletal structure of a patient being treated with methods of the present invention, with the following treatment sequence locations identified: Sequence 5, Dominant-side Lower Sacrum and Upper Ilium; and Sequence 6, Non-Dominant-side Upper Sacrum and Upper Ilium.
[0036] FIG. 3 illustrates a partial skeletal structure of a patient being treated with methods of the present invention, with the following treatment sequence locations identified: Sequence 6 (continued) Non-Dominant-side Proximal Clavicle; Sequence 7, Non-Dominant-side Shoulder; Sequence 8, Non-Dominant-side Elbow; Sequence 9, Non-Dominant-side Wrist.
[0037] FIG. 4 illustrates a partial skeletal structure of a patient being treated with methods of the present invention, with the following treatment sequence locations identified: Sequence 10, Non-Dominant-side Foot; Sequence 11, Non-Dominant-side Knee, Sequence 12, Non-Dominant-side Hip; and Non-Sequence 13, Non-Dominant Side Pubic Symphysis.
[0038] FIG. 5 illustrates a partial skeletal structure of a patient being treated with methods of the present invention, with the following treatment sequence locations identified: Sequence 14, Non-Dominant-side Lower Sacrum and Upper Ilium; and Sequence 15, Non-Dominant-side Upper Sacrum and Upper Ilium.
[0039] FIG. 6 illustrates a partial skeletal structure of a patient being treated with methods of the present invention, with the following treatment sequence locations identified: Sequence 15 (continued) Dominant-side Proximal Clavicle; Sequence 16, Dominant-side Shoulder; Sequence 17, Dominant-side Elbow; Sequence 18, Non-Dominant-side Wrist.
[0040] FIG. 7 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 1.
[0041] FIG. 8 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 2.
[0042] FIG. 9 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 3.
[0043] FIG. 10 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 4.
[0044] FIG. 11 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 5.
[0045] FIG. 12 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 6.
[0046] FIG. 13 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 7.
[0047] FIG. 15 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 9.
[0048] FIG. 16 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 10.
[0049] FIG. 17 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 11.
[0050] FIG. 18 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 12.
[0051] FIG. 19 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 13.
[0052] FIG. 20 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 14.
[0053] FIG. 21 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 15.
[0054] FIG. 22 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 16.
[0055] FIG. 23 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 17.
[0056] FIG. 24 illustrates a table showing sequences in an aspect of a treatment process of the present invention, namely, Sequence Step 18.
[0057] FIG. 25 illustrates treatment sequence 1 of an alternative 20-step treatment process of the present invention.
[0058] FIG. 26 illustrates treatment sequence 2 of an alternative 20-step treatment process of the present invention.
[0059] FIG. 27 illustrates treatment sequence 3 of an alternative 20-step treatment process of the present invention.
[0060] FIG. 28 illustrates treatment sequence 4 of an alternative 20-step treatment process of the present invention.
[0061] FIG. 29 illustrates treatment sequence 5 of an alternative 20-step treatment process of the present invention.
[0062] FIG. 30 illustrates treatment sequence 6 of an alternative 20-step treatment process of the present invention.
[0063] FIG. 31 illustrates treatment sequence 7 of an alternative 20-step treatment process of the present invention.
[0064] FIG. 32 illustrates treatment sequence 8 of an alternative 20-step treatment process of the present invention.
[0065] FIG. 33 illustrates treatment sequence 9 of an alternative 20-step treatment process of the present invention.
[0066] FIG. 34 illustrates treatment sequence 10 of an alternative 20-step treatment process of the present invention.
[0067] FIG. 35 illustrates treatment sequence 11 of an alternative 20-step treatment process of the present invention.
[0068] FIG. 36 illustrates treatment sequence 12 of an alternative 20-step treatment process of the present invention.
[0069] FIG. 37 illustrates treatment sequence 13 of an alternative 20-step treatment process of the present invention.
[0070] FIG. 38 illustrates treatment sequence 14 of an alternative 20-step treatment process of the present invention.
[0071] FIG. 39 illustrates treatment sequence 15 of an alternative 20-step treatment process of the present invention.
[0072] FIG. 40 illustrates treatment sequence 16 of an alternative 20-step treatment process of the present invention.
[0073] FIG. 41 illustrates treatment sequence 17 of an alternative 20-step treatment process of the present invention.
[0074] FIG. 42 illustrates treatment sequence 18 of an alternative 20-step treatment process of the present invention.
[0075] FIG. 43 illustrates treatment sequence 19 of an alternative 20-step treatment process of the present invention.
[0076] FIG. 44 illustrates treatment sequence 20 of an alternative 20-step treatment process of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0077] Embodiments of the present invention involve application of physical adjustments to a patient's body using manual application of force, or through manipulation with assistance of various mechanical equipment. In the treatment tablesshown below, a directed application of force is applied in the manner and/or direction indicated for the listed body structures provided, and for example, P-A may indicate an application of force from the posterior to the anterior position of the named body structure. Some alternative embodiments of the present invention may utilize such instruments as an activator instrument, a toggle board, and a chiropractic table, all of which are described below.
[0078] A conventional activator instrument that may be used in accordance with the present invention is a prior-art type used in the chiropractic disciplines, and has features similar to a combination syringe and a pogo stick. The length of the activator used in embodiments of the present invention has a length of about 20 cm, although different sized activators may be used as the situation requires. The activator has a hard rubber foot with a diameter of about a centimeter along with an adjustable spring tensioner which presets the applied force. When pushed down, the activator delivers a small controlled mechanical “punch” to the specific area it is in contact with restoring motion to a restricted joint.
[0079] Another conventional instrument used in various embodiments of the present invention is what is known as a toggle board. The Thule toggle board is one particular type used in preferred embodiments herein. The Thule toggle board was originally designed for chiropractic treatment of the top vertebra in the cervical spine. It can also be used for the treatment of extremities for the correction of biomechanical joint dysfunctions. The toggle board comprises two sections, upper and lower. In one version used in aspects of the present invention, each section measures approximately
[0000] 8 inches in length, 5.5 inches in width, and 1 inch thick. The upper section is connected to the lower section at one end by a 5 inch by 0.75 inch steel bracket which attaches to the outside borders of the lower section of the toggle board. The upper section is a half inch cushion surface over a half inch solid wood foundation. This section is upholstered with a vinyl-type material. The underside of the upper section has a 2.5 inch by 2 inch hard plastic square which is secured by four perimeter bolts. The lower portion of the toggle board is solid wood, such as oak. Five inches from the end of this board there is a 3 inch aluminum lever on the lateral surface of this board which when lifted raises a hard plastic peg located on the top side of this solid wood board. This peg lifts approximately 0.5 inches which presses against the opposing hard plastic 2.5 inch by 2 inch located on the underside of the vinyl upholstered piece. The raising of this lever arm raises the upper upholstered piece slightly over 0.5 inches at the opened end. On the opposite lateral side of the board there is a 0.75 inch diameter circular flat knob which can be turned to adjust the amount of tension on the peg, which allows this board to adapt to heavier or lighter extremity weight. If for example we are adjusting a joint within the foot, the foot is placed on the vinyl padded upper section of the board. The practitioner then applies a downward force, causing the hard plastic peg to release causing the upper section to drop on to the lower section. The momentum of the upper section falling with the extremity weight striking the stationary lower section causes a slight jarring of the joint, restoring the desired motion to the restricted joint.
[0080] A chiropractic table is used in various embodiments of the present invention. In a preferred embodiment, the chiropractic table is a conventional table such as the Hill Air Drop HA90C. The specifications for the preferred chiropractic table are as follows: electrically controlled height 21.5 to 30.5 inches; tilting headpiece—30° negative and positive tilt; Air-Dual drop forward and straight-motion headpiece; Air-Thoracic breakaway; Air-Thoracic drop; Air-Lumbar drop; Air-Pelvic drop; Rocker foot pedal to raise or lower the table height; Air-powered foot control from foot end; Standard width—24 inches; Length—6 feet 3 inches; Foam top—2.5 inches; Arm rests, 13 inch face cut-out; and paper roll. The table is used with the patient either prone, supine or side lying, as specified herein. With various aspects of the present invention, adjustments are performed to areas of joint dysfunction in the extremities using the drop pieces mentioned above. In the preferred chiropractic table, these air drop pieces are supplied by a large air-storage tank and mini-compressor which are enclosed within the table's base skirting. A compressor runs periodically to replenish the air tank.
[0081] The preferred chiropractic table uses an Air-Breakaway controlled by a foot pedal. The pedal increases or decreases the air-spring pressure in the thoracic and lumbar sections providing a controlled recoil action. The table has electrically adjustable height. Height adjustment is actuated by a rocker foot pedal that is mounted to the base and can be accessed from either side of the table.
[0082] As noted with the toggle board, when the table piece drops there is a slight jarring of the joint, restoring the desired motion to the restricted joint. A directed manual “push” using mostly the patient's own body weight, is needed to activate the chiropractic table and toggle board drop piece mechanisms.
[0083] In alternative embodiments of the present invention, one diagnostic method used to determine the presence of joint dysfunction is called motion palpation. With motion palpation, the doctor sits behind the seated patient to examine this patient's spine. The doctor's left hand is commonly placed on the patient's left shoulder. The doctor's right hand is used by pressing with the flat of the first on the spinal segments, pushing forward slightly at each level. The doctor is checking for joint play (spring) between each vertebra. The normal actions of flexion, extension, left and right lateral flexion and rotation can be evaluated with this method. The joints of the pelvis, arms and legs also can be accurately motion palpated. Through motion palpation diagnosis,
[0000] it can be determined at what segments joint dysfunction is present and when and where corrective adjustments are needed. Once treatment is administered, the affected area is re-palpated to see if normal joint function has been restored.
[0084] Also, as mentioned previously, through motion palpation techniques the practitioner may also determine which leg is the body-dominant leg by having the patient lie supine on the patient's back, with both legs initially straight. The practitioner alternatively brings each leg, one at a time to the patient's chest, and through motion palpation determines which leg requires more force to bend to the chest and/or has less range of motion, and that leg for purposes of the treatment will be established as the dominant leg. Those of skill in the relevant arts also recognize that other techniques may be used to determine the dominant leg. For most of the population, the right leg has found to be the dominant leg.
[0085] Although preferred embodiments of the present invention do not require direct manipulation of the cervical or thoracic spine, in various embodiments of the present invention, manual treatment may be applied to the cervical spine using conventional chiropractic Gonstead and Diversified methods. Manual treatment of the sacral and iliac regions of the patient's body uses the Diversified “side posture” (side lying) adjustment.
[0086] Treatment by Patterns of Adjustments in Sequentially-Ordered Steps
[0087] Embodiments of the present invention employ adjustment patterns applied in a structured manner in sequential, time-ordered steps. Once properly applied, the sequential adjustment patterns provoke an automatic corrective response in the patient and in most cases, the patient does not require future repetitive treatments. As mentioned above, some patients, however, may benefit from periodic treatments to the foot/ankle area as walking on hard, flat surfaces may cause dysfunction to subsequently arise. Embodiments may include applications of any predetermined number of adjustment patterns administered over any predetermined fixed or variable time period.
[0088] Any number of sequence steps may be utilized to apply adjustment patterns. In the preferred embodiment, 18 treatment steps are utilized in the treatment sequence, which is administered as a time-regulated primary cycle (steps 1-9 in a preferred embodiment) followed by a secondary cycle (steps 10-18 in a preferred embodiment). In any one treatment sequence step, one or more treatment patterns may be applied to the patient as desired to obtain a desired treatment goal. In any treatment pattern, one or more adjustments are applied to the indicated structure of the patient's body, and in a preferred embodiment, the adjustments are applied in a predetermined order. In the preferred embodiment, each of the 18 treatment steps is respectively administered in order once per day in sequential days (not necessarily consecutive calendar days), wherein all of the adjustments in the adjustment pattern specified for that treatment step are administered in a predetermined order that day. In another embodiment, the 18-step treatment sequence may be shortened by combining one or more treatment patterns on any treatment day. The sequence steps may be spaced over any desired time period, such as daily, weekly or monthly according to patient preference and treatment results. In a preferred embodiment of the present invention called the GAITLINK method, one adjustment pattern comprising one or more sequential adjustments are applied per sequence step, with the sequence steps occurring once per day over a period of eighteen days (not necessarily consecutive days). Preferably, the patient rests at least overnight between applications of each treatment step. Referring to tables 1-18 below, in the preferred embodiment, the twenty-three adjustments shown in the adjustment pattern for Table (Sequence Step) 1 would be administered in order on day 1 of the treatment, then the ten adjustments of the adjustment pattern shown in Table (Sequence Step) 2 would be applied in the order shown on day 2, the three adjustments shown in the adjustment pattern for Table (Sequence Step) 3 would be administered in order on day 3 of the treatment, and so on until the 18-step sequence is completed. In the tables below, the primary treatment cycle comprises sequence steps 1-9 and the secondary treatment cycle comprises steps 10-18.
[0089] Alternatively, the eighteen-step treatment sequence could comprise the administration of multiple treatment patterns per treatment step, in any order to achieve a desired treatment goal. For example, the eighteen-step treatment sequence could be shortened by one step by combining any two treatment steps on a particular day. In one preferred alternate embodiment, both adjustment patterns of Sequence Step 9 (Table 9) and Sequence Step 10 (Table 10) are applied on the same treatment day, shortening the total treatment time by one day. In yet another embodiment shown in tables 1A-20A, the process could be lengthened by breaking up one or more treatment patterns onto different days, and in the embodiment shown, the proximal clavicle is now treated on a day separate from the sacrum/ilium to accomplish desired treatment goals such as locking or unlocking pelvic structures prior to treatment beginning for the upper body. Those of skill in the art also understand that sequence steps may be repeated as desired, and additional or different adjustment patterns may be utilized to obtain a desired treatment goal.
[0090] In the tables below, abbreviations used in the “Preferred Instrument” column are as follows: the activator instrument will be shown as (AT); the toggle board will be shown as (TT); the chiropractic table will be shown as (CT) and manual treatment will be shown as (MA). Patient Position abbreviations are as follows: Supine (SU); Prone (PR); Side lying (SL); Seated in chair (CH); and Standing (ST). The “#” column corresponds to the order of application of each adjustment to the patient.
Tables 1-18
Eighteen-Step Treatment
[0091]
[0000]
TABLE 1
Sequence Step 1
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Foot of
1
Ankle Mortise Long Axis
SU
MA
Dominant
Extension
Leg (for
2
First Ray Long Axis Extension
SU
MA
example,
3
Subtalar Joint Long Axis Extension
SU
MA
patient's
4
Subtalar Joint Medial to Lateral
SU
TT
right side)
Glide
5
Subtalar Joint Lateral to Medial
SL
TT
Glide
6
Subtalar Joint Medial to Lateral
SU
TT
Tilt
7
Subtalar Joint Lateral to Medial
SL
TT
Tilt
8
Talar Tilt Medial to Lateral
SU
TT
9
Talar Tilt Lateral to Medial
SL
TT
10
P-A Shear Calcaneus
PR
TT
11
Transtarsal Joint Force Application
SU
TT
12
Ankle Mortise A-P Shear with
SU
MA
Internal Rotation Tibia
13
Ankle Mortise P-A Shear with
SU
TT
External Rotation Tibia
14
A-P Calcaneus on Talus
SU
TT
15
Calcaneocuboid Dorsal to Plantar
SU
TT
Spin
16
Calcaneocuboid Plantar to Dorsal
SU
TT
Spin
17
Calcaneocuboid Lateral to Medial
SU
TT
Glide
18
TCN Joint Dorsal to Plantar Spin
SU
TT
19
First Cuneonavicular Joint
SU
TT
Dorsal/Plantar Spin
20
First Ray Complex Dorsal/Plantar
SU
TT
Spin
21
TCN Joint Plantar to Dorsal Spin
SU
TT
22
First Cumeonavicular
SU
TT
Joint Plantar/Dorsal Spin
23
First Ray Complex Plantar/Dorsal
SU
TT
Spin
[0000]
TABLE 2
Sequence Step. 2
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Knee of
1
A-P Tibia on Femur
SU
CT
Dominant
2
Flexion/Internal Rotation Tibia
SU
TT
Leg (for
on Femur
example,
3
Extension/External Rotation
SU
TT
patient's
Tibia on Femur
right side)
4
Internal to External Fibular
SU
TT
Rotation on Tibia (P-A)
5
External to Internal Fibular
SU
AT
Rotation on Tibia (A-P)
6
P-A Proximal Tibia on Distal
SU
TT
Femur
7
Lateral to Medial Femur on Tibia
SU
TT
8
Medial to Lateral Tibia on Femur
SU
TT
9
Medial to Lateral Femur on Tibia
SU
TT
10
Lateral to Medial Tibia on Femur
SU
TT
[0000]
TABLE 3
Sequence Step 3
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Hip
1
Circumduction Femur in
SU
CT
proximate
Acetabulum
Dominant
2
Superior to Inferior Distraction
SU
MA
Leg (for
Femur
example,
3
Gluteus Maximus/Piriformis 1B
SU
CT
patient's
Afferent Stretch
right side)
[0000]
TABLE 4
Sequence Step 4
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Pubic
1
Right Pubic Ramus Superior to
SU
CT
Symphysis
Inferior
proximate
2
Adduction with resistance at
SU
MA
Dominant
Symphysis
Leg (for
example,
patient's
riQht side)
[0000]
TABLE 5
Sequence Step 5
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Lower
1
P-A Sacrum on Ilium (involved
SL
CT
Sacrum
side down)
proximate
Dominant
Leg (for
example,
patient's
right side)
Upper Ilium
2
P-A 1-S Ilium on Sacrum
SL
CT
proximate
Dominant
Leg (for
example,
patient's
right side)
[0000]
TABLE 6
Sequence Step 6
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Upper
1
P-A Sacrum on Ilium (involved
SL
CT
Sacrum
side down)
proximate
Non-
dominant
Leg (for
example,
patient's
left side)
Upper Ilium
2
P-A S-1 Ilium on Sacrum
SL
CT
proximate
Non-
dominant
Leg (for
example,
patient's
left side)
Proximal
1
P-A M-L Proximal Clavicle
SU
CT
Clavicle on
force application
Non-
dominant
side (for
example,
patient's
left side)
[0000]
TABLE 7
Sequence Step 7
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Shoulder
1
Circumduction humerus in Glenoid
SU
CT
on Non-
fossa lateral/medial/A-P
dominant
2
Internal rotation humerus in
SU
CT
side (for
Gleniod fossa medial/lateral/A-P
example,
3
External rotation humerus in
SU
CT
patient's
Glenoid fossa medial/lateral/A-P
left side)
4
P-A S-1 distal clavicle on
CH
AT
Acromion process w/
internal rotation
5
Internal scapular glide on
CH
MA
abduction/ humerus/
Glenoid fossa
[0000]
TABLE 8
Sequence Step 8
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Elbow on
1
External to internal rotation of
ST
MA
Non-
proximal radius in ulnar notch
dominant
2
P-A proximal ulna on distal
ST
MA
side (for
humerus
example,
3
Medial to lateral - lateral to medial
ST
MA
patient's
glide of proximal ulna on
left side)
distal humerus
[0000]
TABLE 9
Sequence Step 9
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Wrist on
1
P-A Distal Radius on Proximal
ST
MA
Non-
Carpals
dominant
2
P-A Distal Ulna on Fibrocartiledge
ST
MA
side (for
3
P-A Distal Radioulnar Joint
ST
MA
example,
4
P-A A-P Glide Carpals
ST
MA
patient's
5
Superior to Inferior First
ST
MA
left side)
Metacarpal on Trapezium
[0000]
TABLE 10
Sequence Step 10
Pre-
ferred
Structure
Patient
Instru-
Treated
#
Adjustment Pattern Element
Position
ment
Foot of
1
Ankle Mortise Long Axis Extension
SU
MA
Non-
2
First Ray Long Axis Extension
SU
MA
dominant
3
Subtalar Joint Long Axis Extension
SU
MA
Leg (for
4
Subtalar Joint Medial to Lateral Glide
SU
TT
example,
5
Subtalar Joint Lateral to Medial Glide
SL
TT
patient's
6
Subtalar Joint Medial to Lateral Tilt
SU
TT
left side)
7
Subtalar Joint Lateral to Medial Tilt
SL
TT
8
Talar Tilt Medial to Lateral
SU
TT
9
Talar Tilt Lateral to Medial
SL
TT
10
P-A Shear Calcaneus
PR
TT
11
Transtarsal Joint Force Application
SU
TT
12
Ankle Mortise A-P Shear with
SU
MA
Internal Rotation Tibia
13
Ankle Mortise P-A Shear with
SU
TT
External Rotation Tibia
14
A-P Calcaneus on Talus
SU
TT
15
Calcaneocuboid Dorsal to Plantar
SU
TT
Spin
16
Calcaneocuboid Plantar to Dorsal
SU
TT
Spin
17
Calcaneocuboid Lateral to Medial
SU
TT
Glide
18
TCN Joint Dorsal to Plantar Spin
SU
TT
19
First Cuneonavicular Joint
SU
TT
Dorsal/Plantar Spin
20
First Ray Complex Dorsal/Plantar
SU
TT
Spin
21
TCN Joint Plantar to Dorsal Spin
SU
TT
22
First Cumeonavicular
SU
TT
Joint Plantar/Dorsal Spin
23
First Ray Complex Plantar/Dorsal
SU
TT
Spin
[0000]
TABLE 11
Sequence Step. 11
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Knee of
1
A-P Tibia on Femur
SU
CT
Non-
2
Flexion/Internal Rotation Tibia on
SU
TT
dominant
Femur
Leg (for
3
Extension/External Rotation Tibia
SU
TT
example,
on Femur
patient's
4
Internal to External Fibular
SU
TT
left side)
Rotation on Tibia (P-A)
5
External to Internal Fibular
SU
AT
Rotation on Tibia (A-P)
6
P-A Proximal Tibia on Distal
SU
TT
Femur
7
Lateral to Medial Femur on Tibia
SU
TT
8
Medial to Lateral Tibia on Femur
SU
TT
9
Medial to Lateral Femur on Tibia
SU
TT
10
Lateral to Medial Tibia on Femur
SU
TT
[0000]
TABLE 12
Sequence Step 12
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Hip
1
Circumduction Femur in
SU
CT
proximate
Acetabulum
Non-
2
Superior to Inferior Distraction
SU
MA
dominant
Femur
Leg (for
3
Gluteus Maximus/Piriformis 1B
SU
CT
example,
Afferent Stretch
patient's
left side)
[0000]
TABLE 13
Sequence Step 13
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Pubic
1
Right Pubic Ramus Superior to
SU
CT
Symphysis
Inferior
proximate
2
Adduction with resistance at
SU
MA
Non-
Symphysis
dominant
Leg (for
example,
patient's
left side)
[0000]
TABLE 14
Sequence Step 14
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Lower
1
P-A Sacrum on Ilium (involved
SL
CT
Sacrum
side down)
proximate
Non-
dominant
Leg (for
example,
patient's
left side)
Upper Ilium
2
P-A 1-S Ilium on Sacrum
SL
CT
proximate
Non-
dominant
Leg (for
example,
patient's
left side)
[0000]
TABLE 15
Sequence Step 15
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Upper
1
P-A Sacrum on Ilium (involved
SL
CT
Sacrum
side down)
proximate
Dominant
Leg (for
example,
patient's
right side)
Upper Ilium
2
P-A S-1 Ilium on Sacrum
SL
CT
proximate
Dominant
Leg (for
example,
patient's
riQht side)
Proximal
1
P-AM-L Proximal Clavicle
SU
CT
Clavicle on
force application
Dominant
side (for
example,
patient's
right side)
[0000]
TABLE 16
Sequence Step 16
Pre-
ferred
Structure
Patient
Instru-
Treated
#
Adjustment Pattern Element
Position
ment
Shoulder
1
Circumduction humerus in Glenoid
SU
CT
on
fossa lateral/medial/A-P
Dominant
2
Internal rotation humerus in
SU
CT
side (for
Gleniod fossa medial/lateral/A-P
example,
3
External rotation humerus in
SU
CT
patient's
Glenoid fossa medial/lateral/A-P
right side)
4
P-A S-1 distal clavicle on Acromion
CH
AT
process w/ internal rotation
5
Internal scapular glide on abduction/
CH
MA
humerus/Glenoid fossa
[0000]
TABLE 17
Sequence Step 17
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Elbow on
1
External to internal rotation of
ST
MA
Dominant
proximal radius in ulnar notch
side (for
2
P-A proximal ulna on distal
ST
MA
example,
humerus
patient's
3
Medial to lateral - lateral to medial
ST
MA
right side)
glide of proximal ulna on distalhumerus
[0000]
TABLE 18
Sequence Step 18
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Wrist on
1
P-A Distal Radius on Proximal
ST
MA
Dominant
Carpals
side (for
2
P-A Distal Ulna on Fibrocartiledge
ST
MA
example,
3
P-A Distal Radioulnar Joint
ST
MA
patient's
4
P-A A-P Glide Carpals
ST
MA
right side)
5
Superior to Inferior First
ST
MA
Metacarpal on Trapezium
Tables 1A-20A
Twenty-Step Treatment
[0092]
[0000]
TABLE 1A
Sequence Step 1
Pre-
ferred
Structure
Patient
Instru-
Treated
#
Adjustment Pattern Element
Position
ment
Foot of
1
Ankle Mortise Long Axis Extension
SU
MA
Dominant
2
First Ray Long Axis Extension
SU
MA
Leg (for
3
Subtalar Joint Long Axis Extension
SU
MA
example,
4
Subtalar Joint Medial to Lateral Glide
SU
TT
patient's
5
Subtalar Joint Lateral to Medial Glide
SL
TT
right side)
6
Subtalar Joint Medial to Lateral Tilt
SU
TT
7
Subtalar Joint Lateral to Medial Tilt
SL
TT
8
Talar Tilt Medial to Lateral
SU
TT
9
Talar Tilt Lateral to Medial
SL
TT
10
P-A Shear Calcaneus
PR
TT
11
Transtarsal Joint Force Application
SU
TT
12
Ankle Mortise A-P Shear with
SU
MA
Internal Rotation Tibia
13
Ankle Mortise P-A Shear with
SU
TT
External Rotation Tibia
14
A-P Calcaneus on Talus
SU
TT
15
Calcaneocuboid Dorsal to Plantar
SU
TT
Spin
16
Calcaneocuboid Plantar to Dorsal
SU
TT
Spin
17
Calcaneocuboid Lateral to Medial
SU
TT
Glide
18
TCN Joint Dorsal to Plantar Spin
SU
TT
19
First Cuneonavicular Joint
SU
TT
Dorsal/Plantar Spin
20
First Ray Complex Dorsal/Plantar
SU
TT
Spin
21
TCN Joint Plantar to Dorsal Spin
SU
TT
22
First Cumeonavicular
SU
TT
Joint Plantar/Dorsal Spin
23
First Ray Complex Plantar/Dorsal
SU
TT
Spin
[0000]
TABLE 2A
Sequence Step. 2
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Knee of
1
A-P Tibia on Femur
SU
CT
Dominant
2
Flexion/Internal Rotation Tibia on
SU
TT
Leg (for
Femur
examole
3
Extension/External Rotation Tibia
SU
TT
patient's
on Femur
right side)
4
Internal to External Fibular
SU
TT
Rotation on Tibia (P-A)
5
External to Internal Fibular
SU
AT
Rotation on Tibia (A-P)
6
P-A Proximal Tibia on Distal
SU
TT
Femur
7
Lateral to Medial Femur on Tibia
SU
TT
8
Medial to Lateral Tibia on Femur
SU
TT
9
Medial to Lateral Femur on Tibia
SU
TT
10
Lateral to Medial Tibia on Femur
SU
TT
[0000]
TABLE 3A
Sequence Step 3
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Hip
1
Circumduction Femur in
SU
CT
proximate
Acetabulum
Dominant
2
Superior to Inferior Distraction
SU
MA
Leg (for
Femur
example,
3
Gluteus Maximus/Piriformis 1B
SU
CT
patient's
Afferent Stretch
right side)
[0000]
TABLE 4A
Sequence Step 4
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Pubic
1
Right Pubic Ramus Superior to
SU
CT
Symphysis
Inferior
proximate
2
Adduction with resistance at
SU
MA
Dominant
Symphysis
Leg (for
example,
patient's
right side)
[0000]
TABLE 5A
Sequence Step 5
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Lower
1
P-A Sacrum on Ilium (involved
SL
CT
Sacrum
side down)
proximate
Dominant
Leg (for
example,
patient's
right side)
Upper Ilium
2
P-A 1-S Ilium on Sacrum
SL
CT
proximate
Dominant
Leg (for
example,
patient's
right side)
[0000]
TABLE 6A
Sequence Step 6
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Upper
1
P-A Sacrum on Ilium (involved
SL
CT
Sacrum
side down)
proximate
Non-
dominant
Leg (for
example,
patient's
left side)
Upper Ilium
2
P-A S-1 Ilium on Sacrum
SL
CT
proximate
Non-
dominant
Leg (for
example,
patient's
left side)
[0000]
TABLE 7A
Sequence Step 7
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Proximal
1
P-AM-L Proximal Clavicle
SU
CT
Clavicle on
force application
Non-
dominant
side (for
example,
patient's
left side)
[0000]
TABLE 8A
Sequence Step 8
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Shoulder
1
Circumduction humerus in Glenoid
SU
CT
on Non-
fossa lateral/medial/A-P
dominant
2
Internal rotation humerus in
SU
CT
side (for
Gleniod fossa medial/lateral/A-P
example,
3
External rotation humerus in
SU
CT
patient's
Glenoid fossa medial/lateral/A-P
left side)
4
P-A S-1 distal clavicle on
CH
AT
Acromion process w/
internal rotation
5
Internal scapular glide on
CH
MA
abduction/humerus/
Glenoid fossa
[0000]
TABLE 9A
Sequence Step 9
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Elbow on
1
External to internal rotation of
ST
MA
Non-
proximal radius in ulnar notch
dominant
2
P-A proximal ulna on distal
ST
MA
side (for
humerus
example,
3
Medial to lateral - lateral to medial
ST
MA
patient's
glide of proximal ulna on
left side)
distal humerus
[0000]
TABLE 1OA
Sequence Step 10
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Wrist on
1
P-A Distal Radius on Proximal
ST
MA
Non-
Carpals
dominant
2
P-A Distal Ulna on Fibrocartiledge
ST
MA
side (for
3
P-A Distal Radioulnar Joint
ST
MA
example,
4
P-A A-P Glide Carpals
ST
MA
patient's
5
Superior to Inferior First
ST
MA
left side)
Metacarpal on Trapezium
[0000]
TABLE 11A
Sequence Step 11
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Foot of
1
Ankle Mortise Long Axis
SU
MA
Non-
Extension
dominant
2
First Ray Long Axis Extension
SU
MA
Leg (for
3
Subtalar Joint Long Axis Extension
SU
MA
example,
4
Subtalar Joint Medial to Lateral
SU
TT
patient's
Glide
left side)
5
Subtalar Joint Lateral to Medial
SL
TT
Glide
6
Subtalar Joint Medial to Lateral
SU
TT
Tilt
7
Subtalar Joint Lateral to Medial
SL
TT
Tilt
8
Talar Tilt Medial to Lateral
SU
TT
9
Talar Tilt Lateral to Medial
SL
TT
10
P-A Shear Calcaneus
PR
TT
11
Transtarsal Joint Force Application
SU
TT
12
Ankle Mortise A-P Shear with
SU
MA
Internal Rotation Tibia
13
Ankle Mortise P-A Shear with
SU
TT
External Rotation Tibia
14
A-P Calcaneus on Talus
SU
TT
15
Calcaneocuboid Dorsal to Plantar
SU
TT
Spin
16
Calcaneocuboid Plantar to Dorsal
SU
TT
Spin
17
Calcaneocuboid Lateral to Medial
SU
TT
Glide
18
TCN Joint Dorsal to Plantar Spin
SU
TT
19
First Cuneonavicular Joint
SU
TT
Dorsal/Plantar Spin
20
First Ray Complex Dorsal/Plantar
SU
TT
Spin
21
TCN Joint Plantar to Dorsal Spin
SU
TT
22
First Cumeonavicular
SU
TT
Joint Plantar/Dorsal Spin
23
First Ray Complex Plantar/Dorsal
SU
TT
Spin
[0000]
TABLE 12A
Sequence Step. 12
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Knee of
1
A-P Tibia on Femur
SU
CT
Non-
2
Flexion/Internal Rotation Tibia on
SU
TT
dominant
Femur
Leg (for
3
Extension/External Rotation Tibia
SU
TT
example,
on Femur
patient's
4
Internal to External Fibular
SU
TT
left side)
Rotation on Tibia (P-A)
5
External to Internal Fibular
SU
AT
Rotation on Tibia (A-P)
6
P-A Proximal Tibia on Distal
SU
TT
Femur
7
Lateral to Medial Femur on Tibia
SU
TT
8
Medial to Lateral Tibia on Femur
SU
TT
9
Medial to Lateral Femur on Tibia
SU
TT
10
Lateral to Medial Tibia on Femur
SU
TT
[0000]
TABLE 13A
Sequence Step 13
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Hip
1
Circumduction Femur in
SU
CT
proximate
Acetabulum
Non-
2
Superior to Inferior Distraction
SU
MA
dominant
Femur
Leg (for
3
Gluteus Maximus/Piriformis 1B
SU
CT
example,
Afferent Stretch
patient's
left side)
[0000]
TABLE 14A
Sequence Step 14
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Pubic
1
Right Pubic Ramus Superior to
SU
CT
Symphysis
Inferior
proximate
2
Adduction with resistance at
SU
MA
Non-
Symphysis
dominant
Leg (for
example,
patient's
left side)
[0000]
TABLE 15A
Sequence Step 15
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Lower
1
P-A Sacrum on Ilium (involved
SL
CT
Sacrum
side down)
proximate
Non-
dominant
Leg (for
example,
patient's
left side)
Upper Ilium
2
P-A 1-S Ilium on Sacrum
SL
CT
proximate
Non-
dominant
Leg (for
example,
patient's
left side)
[0000]
TABLE 16A
Sequence Step 16
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Upper
1
P-A Sacrum on Ilium (involved
SL
CT
Sacrum
side down)
proximate
Dominant
Leg (for
example,
patient's
right side)
Upper Ilium
2
P-A S-1 Ilium on Sacrum
SL
CT
proximate
Dominant
Leg (for
example,
patient's
right side)
[0000]
TABLE 17A
Sequence Step 17
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Proximal
1
P-A M-L Proximal Clavicle
SU
CT
Clavicle on
force application
Dominant
side (for
example,
patient's
right side)
[0000]
TABLE 18A
Sequence Step 18
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Shoulder
1
Circumduction humerus in Glenoid
SU
CT
on
fossa lateral/medial/A-P
Dominant
2
Internal rotation humerus in
SU
CT
side (for
Gleniod fossa medial/lateral/A-P
example,
3
External rotation humerus in
SU
CT
patient's
Glenoid fossa medial/lateral/A-P
right side)
4
P-A S-1 distal clavicle on
CH
AT
Acromion process w/
internal rotation
5
Internal scapular glide on
CH
MA
abduction/humerus/
Glenoid fossa
[0000]
TABLE 19A
Sequence Step 19
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Elbow on
1
External to internal rotation of
ST
MA
Dominant
proximal radius in ulnar notch
side (for
2
P-A proximal ulna on distal
ST
MA
example,
humerus
patient's
3
Medial to lateral - lateral to medial
ST
MA
riQht side)
glide of proximal ulna on
distal humerus
[0000]
TABLE 20A
Sequence Step 20
Structure
Patient
Preferred
Treated
#
Adjustment Pattern Element
Position
Instrument
Wrist on
1
P-A Distal Radius on Proximal
ST
MA
Dominant
Carpals
side (for
2
P-A Distal Ulna on Fibrocartiledge
ST
MA
example,
3
P-A Distal Radioulnar Joint
ST
MA
patient's
4
P-A A-P Glide Carpals
ST
MA
riQht side)
5
Superior to Inferior First
ST
MA
Metacarpal on Trapezium
Logan Basic Technique-Style Modified Embodiment
[0093] An additional embodiment provides for treatment of the sacrotuberous ligament and/or long dorsal ligament as replacement for or as an adjunct to various hip and/or pelvic structure treatments mentioned previously. The sacrotuberous ligament is can be found at the lower and back part of the pelvis.
[0094] In general, the Logan Basic Technique is a prior art chiropractic technique wherein with the patient lies face down (prone), and the practitioner places a very light pressure on a pre-determined “leverage spot” on the patient's body; for instance, the sacral bone in the low back. In an embodiment of the present invention, the practitioner uses the Logan Basic Technique to apply a very light force to the sacrotuberous ligament and/or long dorsal ligament as and adjunct to or replacement of various pelvic treatments. In one exemplary modification of the preferred 18-Step treatment sequence shown in Tables 1-18, in sequence step 5, treatment of the dominant-side lower sacrum and upper ilium would be replaced by application of Logan-Basic Technique pressure by application by the practitioner's finger to the patient's dominant-side sacrotuberous ligament (proximal the patient's dominant side sacrum).
[0000] Then in sequence step 6, treatment of the non-dominant-side upper sacrum and upper ilium would be replaced by application of Logan-Basic Technique pressure by the practitioner's finger to the patient's non-dominant-side sacrotuberous ligament and/or long dorsal ligament (treatment to the proximal clavicle continues as shown in Table 6). Then similarly, in sequence step 14, treatment of the non-dominant-side lower sacrum and upper ilium would be replaced by application of Logan-Basic Technique pressure by application by the practitioner's finger to the patient's non-dominant-side sacrotuberous ligament (proximal the patient's non-dominant side sacrum). Then in sequence step 15, treatment of the dominant-side upper sacrum and upper ilium would be replaced by application of Logan-Basic Technique pressure by the practitioner's finger to the patient's dominant-side sacrotuberous ligament and/or long dorsal ligament (treatment to the proximal clavicle continues as shown in Table 15).
[0095] It is to be understood that the foregoing description is exemplary and explanatory only and is not restrictive of the invention, as disclosed or claimed. Changes and modifications may be made to the disclosed embodiments without departing from the scope of the present invention. These and other changes or modifications are intended to be included within the scope of the present invention, as expressed in the following claims, in the description herein, and in the referenced figures.
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There is provided a system and method for treating a patient by administering a predetermined sequence of adjustments to a patient's body. Unlike the unstructured or random application of adjustments used in prior art chiropractic treatments, the treatment sequences and provided for herein unlock function of dysfunctional joint systems in a manner analogous to a combination lock mechanism. Disciplines that may utilize embodiments of the present invention include chiropractic, naturopaths, sports medicine, physical therapy, professional and collegiate trainers, as well as aspects of veterinary medicine. Through applications of the method of the present invention, patients may receive a predetermined number of treatment applications, and have long-lived or substantially permanent results from the treatment without the need for ongoing adjustments to spine or other body structures.
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BACKGROUND OF THE INVENTION
[0001] This invention relates generally to an electronic blasting system and is particularly concerned with limiting the effects of undesirable leakage currents which may occur in the system.
[0002] As used herein “leakage current” includes current flow in a blasting system that does not directly contribute to the effective operation of electronic detonators in the system.
[0003] An electronic blasting system typically rakes use of a plurality of electronic detonators. Each detonator may Include one or more capacitors which are used to ensure autonomous operation of the detonator if connecting wires to the detonator are broken, for example due to the effect of a blast at an adjacent borehole which may manifest itself before the detonator is to initiate.
[0004] The energy density requirement imposed by current consumption of an electronic detonator, the energy required to initiate a fuse head and space constraints side a detonator tube normally suggest the use of tantalum capacitors over other capacitor technologies. A tantalum capacitor has a low internal leakage current and is suitable for use in a blasting system which may call for hundreds, or even thousands, of electronic detonators to be used in a single blast.
[0005] Although a tantalum capacitor performs well in this type of application it can suffer from a failure mode that could result in the capacitor short-circuiting. This type of event can be catastrophic in a blasting system in which electronic detonators are connected in parallel to one another and are powered through a shared wire bus connected to a control device which may be some distance from a blast bench.
[0006] A short circuit in a capacitor, which is inside a detonator, results in a high current consumption and severe voltage starvation on a wire bus to which the detonator is connected. This can reduce the voltage available for blasting which, in turn, can cause a misfire in the affected detonator and which can also cause other detonators in the blasting system to misfire. Alternatively a significant time delay may be incurred while the faulty detonator is being identified and remedial action is taken.
[0007] The aforementioned problem is exacerbated if this type of failure only occurs once a supply voltage is raised to a level which is sufficiently high to supply blasting energy. The voltage increase is typically done only once mining equipment and personnel hare been evacuated from a blasting area and production would thus be brought to a standstill during this time. A delay of this type can result in significant financial losses.
[0008] There are other failures which can be detrimental to a parallel blasting circuit. For example damage to the insulation of wires, that typically occurs when a detonator is loaded into a blast hole, can cause current leakage or a short-circuit. A similar adverse effect can be produced by the ingress of a fluid into a detonator due to poor sealing between a crimp plug and a detonator tube, and similar factors.
[0009] A further concern is that a current leakage problem may not be apparent immediately when a detonator is loaded into a blast hole but may only appear after some time, possibly as wire to the detonator stretches during hole slumping, or due to a slow ingress of fluid into the detonator over time.
[0010] A typical blasting system can tolerate leakage currents of the order of tens of milliamps before voltage starvation occurs at which stage detonators may misfire due to insufficient voltage levels.
[0011] One approach adopted to identify where a leakage current or short circuit problem occurs in a blast system is to query the detonators in the system, electronically, to establish whether sufficient voltage is available. This approach allows a problem blast hole to be identified. For example, a detonator in the blast hole can measure an applied voltage and then respond to an interrogating module indicating whether the voltage is adequate or too low. Alternatively, an indication of the position of a problem can be obtained if one or more detonators do not respond at all for example if insufficient voltage is available or if a fault is present.
[0012] The location of a single short circuit in a blast system can sometimes be identified by measuring the resistance between the bus wires. This approach works if the resistance per unit length of the bus wire is known and if there are no significant contributors current flow through the bus wire.
[0013] In some systems detonators are connected sequentially to a two-wire bus by means of electronic circuits each of which, typically, is housed in a connector located on surface adjacent a borehole. This sequential connection methodology can allow for accurate determination of the location of a leakage or short circuit problem as is contemplate in U.S. Pat. No. 8,646,387.
[0014] An alternative solution is presented in US patent application No. 2013/0036931. This application describes opening a switch in reply to a signal from a detonator in response to an event, thus potentially disconnecting a remaining chain of detonators from the wire bus. However, the disconnection of an entire chain of detonators is not helpful if the cause of the leakage problem lies in a single borehole.
[0015] U.S. Pat. No. 7,911,760 is similarly limited in that a remain chain of detonators is controlled via an actuator on a wire bus.
[0016] U.S. patent application Ser. No. 13/582,688 discloses the use of a resistor in a detonator connector. A current through the resistor is sensed by monitoring the voltage, over the resistor, which is used to switch the gate of a FET. The resistor is thus used as a sensing element and not for current limiting purposes.
[0017] Although it is possible to modify systems of the aforementioned kind to isolate problem holes, the electronics required are relatively complex and can be expensive.
[0018] The effect of leakage current in a blasting system can be limited by decreasing the resistance of the bus wire so that the voltage drop across the bus wire due to a leakage current is limited. This approach requires a thicker bus wire, or additional bus wire. Alternatively each end of the detonator bus wire connected to a control unit so that the bus wire can be driven from both ends. These methods can however produce additional delays, particularly if problems are experienced only when a blasting voltage is applied to the bus wire.
[0019] It is also possible to raise the blast voltage to overcome losses due to a problem near an end of the bus wire. This, however, can expose some detonators to a voltage which exceeds a rated operating voltage.
[0020] An object of the invention is to provide an inexpensive and easy to implement mechanism for limiting, at least to some extent, the impact of problems due to leakage currents.
SUMMARY OF THE INVENTION
[0021] The invention provides a blasting system which includes a blasting control machine, a detonator bus connected to the blasting control machine, a plurality of electronic detonators, a plurality of down-hole harnesses each detonator being connected to a respective down-hole harness, a plurality of connectors, each connector connecting a respective down-hole harness to the bus whereby the detonators are connected in parallel to the bus, and, in respect of each detonator, at least one current-limiting component which is connected in series with the respective down-hole harness and which limits current in the down-hole harness to a current level that can be accommodated by the blasting control machine in the presence of at least one fault, which causes current leakage, that is present either in the down-hole harness or internally in the detonator.
[0022] The predetermined current level may be the level of the current which would flow if the current-limiting component were absent.
[0023] The current the blasting machine is normally determined by considering the current consumption of a full load of detonators plus some margin to allow for leakage. For example, if a detonator consumes 20 μA when powered at a high voltage for blasting, and 300 detonators need to be accommodated on the harness, then a current of 6 mA is required, plus some margin to allow for leakage etc. In practice as the harness wire and detonators present a highly capacitive load to the blasting machine, additional current is required to “drive the harness” appropriately and to produce acceptable communication signals. In a typical blasting system the blasting current limit is in the range of 20 mA to about 100 mA, depending on the system and various other design considerations.
[0024] The fault may be at least one short circuit either on the down-hole harness or internally in the detonator.
[0025] The current-limiting component may be located within a housing of the respective connector or in an in-line module which is connected to the down-hole harness.
[0026] Preferably in use, the current-limiting component is located outside a blast hole in which the respective detonator is positioned. This helps to reduce the likelihood that the current-limiting component would be damaged while the blast hole is being loaded.
[0027] It is possible to connect a respective current-limiting component in series in each wire of the down-hole harness to restrict the nature of a problem which would occur if one wire were to be inadvertently coupled to earth. Such coupling could result in an undesirable current flow if another part of the blasting system were to be earthed in some way.
[0028] In one form of the invention the current-limiting component comprises a resistor. It is possible to make use of a current-limiting diode or a JFET equivalent but, in general, these devices are more expensive than a resistor.
[0029] In an alternative approach the current-limiting component includes a current-limiting circuit that, in response to the current in the respective down-hole harness, disconnects the down-hole harness from the bus if the current exceeds a predetermined level.
[0030] It is within the scope of the invention to take current measurements over a period of time before a decision to disconnect is made. This makes the circuit insensitive to typical high start-up currents which may occur when a capacitor inside a detonator is discharged and the down-hole harness to the detonator is powered.
[0031] The current-limiting circuit may be non-latching so that, when the current is reduced to an acceptable level, the connection to the down-hole harness is restored.
[0032] Preferably, though the current-limiting circuit is latching so that the down-hole harness remains disconnected from the bus until power is removed for a reasonable period. This approach minimises the effect of a problem blast hole on the remainder of the blast system although it is then not possible to fire the affected detonator.
[0033] It is generally not viable to make use of a conventional fuse or resettable fuse to limit the current in a manner similar to what has been described, for the current concerned are typically too for commercially available fuses. Additionally, a non-resettable characteristic can be unsuitable if a user wishes to resolve a problem under certain conditions, for example if a particular detonator is critical to a blasting plan. In these circumstances, in order to minimize the effect of a leakage circuit, it may be desirable to connect the detonator to a first bus that is driven independently of a second bus and its associated detonators.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] The invention is further described by way of examples with reference to the accompanying drawings in which:
[0035] FIG. 1 schematically illustrates a blasting system according to one form of the invention,
[0036] FIG. 2 is a view on an enlarged scale of a connector which is suitable for use in the system shown in FIG. 1 ,
[0037] FIG. 3 shows another form of the invention, and
[0038] FIG. 4 shows details of a circuit for use in the arrangement of FIG. 3 .
DESCRIPTION OF PREFERRED EMBODIMENTS
[0039] FIG. 1 of the accompanying drawings illustrates a blasting system 10 which includes a blasting control machine 12 , an elongate wire bus 14 which typically is located on surface and which is connected to the machine 12 , a plurality of boreholes or blast holes 16 , a plurality of detonator down-hole harnesses 18 , a plurality of electronic detonators 20 and a plurality of connectors 22 . The connectors 22 are shown in FIG. 1 in dotted outline, for ease of reference and, similarly, in FIGS. 2 and 3 .
[0040] Each connector 22 is used to make a respective connection between the bus 14 and an associated down-hole harness 18 which, in turn, is connected to a respective detonator 20 . In this way the detonators are connected in parallel to each other via the bus 14 .
[0041] Each detonator 20 includes electronic elements and, typically, a custom designed control circuit (ASIC) (not shown), all mounted inside a detonator can, as is known n the art.
[0042] Explosive material, not shown, placed in each borehole is exposed to the respective detonator.
[0043] In a conventional approach resistors inside the detonator can to the value of about 1 kohm are connected in series with the ASIC. These resistors serve to protect the ASIC against a high applied voltage and also determine the level of talkback current modulation. For example, when powered from an 8 v supply rail the detonator will generate current modulation pulses of 4 mA. However, if the voltage is raised to a blasting voltage level of approximately 25 v, a capacitor short circuit would result in approximately 12.5 mA of current consumption which could be detrimental to blasting depending on the length of the bus line 14 and of the respective down-hole harness 18 , the values of the respective associated resistances, and the effect thereof in relation to the maximum allowed leakage current.
[0044] Numerical values in this specification are exemplary only, and are non-limiting.
[0045] A more damaging situation occurs when a short circuit on a down-hole harness 18 results in the resistors being bypassed. The current consumption is then limited to the lesser of the current output limit of the blasting control machine 12 , which is used to control the blasting process, and the current consumption which is attributable to the blasting voltage applied to the bus 14 up to the location of the short circuit. For example if the resistance presented to the blasting control machine 12 is 100 ohm and the blasting voltage is 25 v, the current load is approximately 250 mA. This means that detonators which are wired after the short circuit, i.e. which are downstream of the fault, would receive no appreciable voltage and would not fire.
[0046] Assume that two resistors 24 each of 2.4 kohm are connected in series with the aforementioned 1 kohm resistors and are located in the housing of the connector 22 which connects the down-hole harness 18 to the surface bus 14 —see FIG. 1 .
[0047] In normal communications, with an 8 v supply rail, the talkback current is reduced (for the given figures) to 8/(1000+1000+2400+2400)=1.17 mA. This low current reduces the signal to noise ratio of received detonator communication signals but it is still within the capabilities of a receiver in the blasting control machine 12 to detect and demodulate. The voltage loss which is induced during normal operation is also acceptable as a typical operating current of the order of 10 μA per detonator results in a negligible voltage drop across the series-connected 2.4 kohm resistors.
[0048] At a blasting voltage of 25 v, a short circuit in the down-hole harness 18 , again assuming a resistance of 100 ohm, produces a current of 25/(100+2400+2400)=5.10 mA, a current value which is within the current leakage capabilities of the system.
[0049] FIG. 2 illustrates a housing 30 of a connector 22 which includes contacts 32 and contacts 36 for connecting wires 14 A and 14 B of the surface bus 14 , to wires 18 A and 18 B of the respective downhole harness 18 . The housing 30 contains two resistors 40 and 42 respectively, preferably of equal value, which are connected in series with the wires 18 A and 186 respectively. The resistance of each resistor (for the given set of values) is of the order of 2.4 kohms. The resistors 40 and 42 of FIG. 2 are the same as the resistors 24 referred to in connection with FIG. 1 .
[0050] The contacts 32 and 36 are shown in a notional sense only. Typically use is made of a custom-designed insulation displacement connector (IDC). Each line of the bus wire is directly connected to a respective connector and, at the same time, provision is made for a wire of the downhole harness to be connected to the same connector via a series resistor.
[0051] The resistors 40 and 42 limit the magnitude of leakage current to earth which could occur in each wire 18 A and 18 B. In other respects the operation of the blasting system would be in accordance with conventional techniques. Preferably, the current-limiting resistors 40 , 42 are on surface i.e. inside the connector housing 30 so that the resistors are not exposed to damage which could arise during loading of the respective borehole 16 .
[0052] Values of the resistors are given for explanatory purposes only. In practice the chosen resistor values are specific to a particular blasting system. The resistive values can be adjusted to take account of various factors and to suit a blasting system which has different operating characteristics bearing in mind however that the object is to limit the current in the downhole harness from exceeding a predetermined current value.
[0053] In the blasting systems described with reference to FIGS. 1 and 2 the resistors 24 , 40 and 42 are used, directly, to limit the magnitude of the current flowing to the respective detonator. This effective and low cost technique, to counter the effect of a leakage current, is distinguishable from the approach referred to in connection with U.S. Ser. No. 13/582688 which describes the use of a resistor, in a connector, as a current sensing element and not to restrict the magnitude of the current.
[0054] FIGS. 1 and 2 illustrate two resistors in use in each connector housing with one resistor being associated with each respective downhole wire. This is not necessarily the case. A single resistor could be used, preferably positioned on or in the connector housing. A single resistor only protects a single wire against a short to earth. In practice the most likely unwanted occurrence is that wires in the blast hole are connected to each other (i.e. the wires are shorted). A single resistor in one wire would then address this event.
[0055] FIG. 3 illustrates a blasting system 10 A in which components which are the same as those referred to in connection with FIGS. 1 and 2 have like reference numerals.
[0056] Connectors 22 A in the blasting system 10 A are different from the connectors 22 shown in FIG. 2 in that they do not include internal current-limiting resistors. Instead a respective current-limiting circuit 50 is connected in series to each down-hole harness in principle the circuit 50 provides a function which is similar to that offered by the current-limiting resistors. The circuit 50 measures the current 52 in the down-hole harness 18 over a period of time. If the current 52 rises above a predetermined value the circuit 50 , which contains a semi-conductor-based switch such as an FET, open circuits and isolates the associated detonator 20 from the surface bus 14 . The circuit 50 then latches and the detonator 20 remains disconnected from the bus and no power is applied to the detonator, for a reasonable period.
[0057] FIG. 4 illustrates aspects of a possible implementation of the circuit 50 . The wires 18 A and 18 B are connected to a diode bridge 56 which, together with a capacitor 58 provides power for the circuit via various connections (not shown).
[0058] A resistor 60 and a capacitor 62 , in parallel, produce a voltage which is dependent on the magnitude of the down-hole harness current and which is applied to a differential comparator 64 .
[0059] The combination of the resistor 60 and the capacitor 62 also allows short bursts of high current to be ignored, a feature which is useful to avoid triggering upon reception of current modulated communication signals from the detonator or upon initial start-up when the detonator capacitor is discharged and a higher current is drawn until the detonator capacitor is fully charged.
[0060] The differential comparator 64 compares the voltage from the combination of the resistor 60 and capacitor 62 , irrespective of the polarity thereof, to a chosen reference voltage 66 which is applied to a reference pin on the comparator and which is representative of the desired trigger current for the circuit. The reference voltage is produced by appropriate circuitry, not shown.
[0061] When the reference voltage is exceeded the comparator 64 switches and an output signal is applied to a latching circuit 70 which in turn controls the connection and disconnection of the associated detonator 20 to the surface harness via a voltage controlled switch 74 .
[0062] Initially, upon power-up, the latching circuit 70 is set so that the switch 74 is closed and the detonator 20 is connected to the surface harness. When the specified current limit is exceeded and detected by the comparator 64 , for a period of time the duration of which is determined by the resistor 60 and capacitor 62 , the latching circuit 70 is reset by the output of the comparator 64 and the detonator 20 is disconnected from the surface harness by the switch 74 which is opened.
[0063] In order to reset the circuit 50 power is removed so that the capacitors 58 and 62 can discharge. Upon power-up as described, the switch 74 is closed and the detonator 20 is then reconnected to the surface bus.
[0064] The circuit of FIG. 4 only senses the current in one wire to the detonator. This technique can however be extended so that the current in the second wire is also sensed.
[0065] The current-limiting circuit 50 does consume current and it requires several components for its effective implementation. The use of resistors to limit current, as has been described with reference to FIGS. 1 and 2 , is thus of lower cost and easier to implement although such use does not offer the latching characteristic which is available with the circuit 50 .
[0066] In FIG. 3 the circuit 50 is shown displaced from the connector 22 A but this is exemplary only for the circuit is preferably located inside the connector housing 30 or is otherwise directly physically associated with the connector 22 A.
[0067] The invention allows detonators, which are subject to leakage current-induced voltage losses, to be identified, for example, by means of querying the detonators as is known in the art. The effect is such that the detonator concerned would probably not fire successfully. However blasting can proceed as the voltage which is supplied to other detonators would not be adversely affected.
[0068] A benefit of the invention lies in the fact that it is low in cost and simple to implement. The invention allows a blast to continue even if leakage problems are detected at a high voltage which would ordinarily have prevented blasting completely or would have resulted in misfires in detonators apart from those detonators which are directly affected by the current leakage problems.
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A detonator system wherein a detonator is connected via a down-hole harness to a bus extending from a blast controller and wherein a component is connected in series with the down-hole harness to limit leakage current in the harness to a level which can be accommodated by the blast controller.
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BACKGROUND OF THE INVENTION
The present invention relates to an apparatus for monitoring irregularities and/or changes in the structure of a textile yarn coming from an open-end spinning turbine, the monitoring apparatus being of the type which includes a measuring value sensor to sense irregularities and an evaluation circuit which, upon the occurrence of irregularities, generates a signal to actuate an indicator and/or to switch off the spinning turbine.
Such an apparatus is disclosed in German Offenlegungsschrift [laid-open application] No. 2,509,259. In that apparatus, a sensor is provided in the yarn removal path to generate an analog signal which is representative of the thickness of the yarn. A pulse is generated each time this analog signal exceeds or drops below threshold values, i.e., when the thickness of the yarn is above or below a selected range, and the resulting pulses are counted in a counter, the occurrence of at least a given number of pulses within a given period of time causing a display or switch-off signal to be emitted.
Monitoring of the yarn being produced in an open-end spinning machine is recommended because irregularities, particularly thickness variations in the yarn may occur irregularly in cycles or even at regular intervals and thus would lead to undesirable moire effects in fabrics produced from that yarn.
Such thicker or thinner portions are produced mainly as a result of deposits of dirt particles in the rotor of the spinning turbine, and additionally by other causes.
The yarn may also exhibit changes in its structure.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to simplify the detection of such thickness variations and/or changes in structure, at least in the type of open-end spinning turbine which has its own individual drive member.
This and other objects are achieved, according to the present invention by associating with the drive member of such a spinning turbine a sensor which responds to changes in the drive member current consumption. Various motors can be used as the drive member. When a brushless d.c. motor is used, the motor current changes are particularly distinct.
The present invention is based on the realization that certain changes in the yarn being produced in the spinning turbine will vary the mechanical load, or torque, on the motor during yarn removal and thus the current consumption of the motor. This can occur, for example, as a result of the creation of a thicker section in the yarn due to a locally limited dirt deposit in the spinning rotor fiber collection trough, or upon the occurrence of a change in yarn structure due to extensive deposits in the fiber collection trough, or as a result of wear in the fiber collection trough. The variations in current consumption are due to the changed, particularly enlarged, yarn mass per unit length, producing a change in friction, and the changed, particularly greater, air resistance exhibited by the yarn.
It is known that in the operation of an open-end spinning turbine, the binding point rotates somewhat faster than the spinning rotor itself. The binding point is that point along the fiber collection trough circumference where the fibers are bound into the yarn and the yarn ceases to contact the collection trough. The difference in rates of rotation is, for example, between 10 and 50 Hz. With a yarn removal speed of, for example, 200 m/min and a rotor circumference of about 15 cm, the binding point will rotate about 20 Hz faster than the rotor itself. A periodic thicker or thinner section in the yarn will thus produce a periodic increase or decrease, respectively, in current consumption having a frequency of about 20 Hz.
The current being supplied to the motor can be sensed by a circuit including, for example, a lowpass filter which permits signals at this frequency to pass while filtering out the much higher drive current commutation frequency. The evaluation circuit in this case will be designed to produce a warning or switching signal upon the occurrence of a given number of changes which lie above and/or below a threshold.
The evaluation circuit can also be designed to respond to a single deviation, and possibly a deviation having a certain duration, or a given magnitude in one or either direction from the desired current consumption.
Both types of change, i.e. a single and possibly long duration deviation, and a periodically varying fluctuation, can be evaluated and used simultaneously. In addition, the monitoring apparatus according to the invention can be combined with an additional monitoring apparatus whose sensor responds to radial deflections of the rotor or of its bearing, in the case of a turbine whose rotor bearing is elastically mounted and is thus subject to such radial deflections. In this case the only changes which can be sensed, however, are those produced by locally defined imbalances, e.g., deposits. The radial deflection sensor could be a displacement measuring device operating in an inductive, capacitive or other known manner, or a sensor which could be of the inductive type, responsive to the velocity of the radial deflection movement. The periodic change here occurs at the rotor rotation frequency. Here again a switching or warning signal is produced when one or a given number of changes occur during a given period of time.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is partly a cross-sectional side view of an open-end spinning turbine equipped with an individual brushless d.c. motor, and partly a schematic block circuit diagram of an associated evaluation circuit for monitoring drive current changes according to the invention.
FIG. 2 is a block circuit diagram of another embodiment of an evaluation circuit according to the invention.
FIG. 3 is partly a cross-section detail view and partly a block circuit diagram of a sensor and an evaluation circuit for sensing imbalance signals, which circuit can be used in addition to the evaluation circuits of FIGS. 1 and 2.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows an open-end spinning turbine equipped with its own drive system, which is exemplary of the type of spinning turbine in which the present invention can be used.
The turbine includes a rotor 1 provided with a cup-shaped or bell-shaped part 9 which has a bore 3 at the center of its base 2. In the bore 3 a pin 5 is positioned, and the free end 6 of the pin projects into a bearing bush 7. Free end 6 and bush 7 together constitute a journal bearing, the bush being the stationary part of the bearing and end 6 being the rotary part thereof. The center of gravity of the rotor is located at least approximately on its axis of symmetry 8, and between the axial ends of the bearing bush 7. A part 10 of a stator 11 projects into the cup-shaped rotor part 9, and has a bore 12 to accommodate the bearing bush 7. The bearing bush 7 is elastically supported in the bore 12 by means of parts of elastic material which are constructed as O-rings 13. These O-rings lie in annular grooves 15 in the interior surface of the bore 12, as well as in annular grooves 17 in the outer surface of the bearing bush 7.
An electric motor is provided for driving the rotor 1. To this end substantially radially magnetized permanent magnets 20 are positioned on the inner surface of the cup-shaped part 9 of rotor 1. The permanent magnets 20 have an alternating polarity in the peripheral direction and are fastened to the rotor as individual magnets.
Windings 19 are provided on the outer face of the stator part 10 and are associated with the permanent magnets. A current is caused to flow through the windings so that the rotor is driven, for example, like a brushless direct current motor. The windings 19 are constructed without iron so as to prevent additional forces or moments from being generated which an act on the bearing and which would otherwise be present in an electric motor constructed in this way.
The front end of the rotor (to the left in FIG. 1) is constructed to have a funnel-like form 14. When using this device in spinning frames, or turbines, operating according to the open-end method, the material to be spun is introduced into the funnel-like front end of the rotor and drawn off in a known manner. If, for example, as a result of manufacturing tolerances or of the material located in the funnel 14, the center of gravity of the rotor is not located exactly on the axis of symmetry 8, the rotor can still rotate about its largest central principal axis of inertia adjacent axis 8 because of the floating bearing which is provided as above described, thereby preventing creation of additional bearing forces.
The importance of the construction of the drive motor as an iron-free electric motor is then enhanced in that it also ensures that no additional radial forces or moments are exerted on the bearing even by the drive itself, that is to say, even if the rotor does not rotate exactly about the axis 8. In order to reduce drive losses due to the air resistance, which occur particularly at high speed, the rotor is surrounded on its outside by a stationary housing 18.
Assuming that the windings 19 have the form of a three-phase winding, the three phases are connected in succession to d.c. power source 21 by means of a commutating switch 22. For reasons of simplicity only the conductor pair for one winding phase is shown connected to the switch. The commutation operation of switch 22 is well known in the art and will not be explained in detail here.
A resistor 23 is connected into the current input lead from source 21 and a voltage proportional to the supply current is derived therefrom. If the reaction torque on the motor changes due to the occurrence of a thicker or thinner yarn section the drive current amplitude changes correspondingly. The voltage across resistor 23 is supplied to a series-connected filter 24 dimensioned so that, for example, only signal frequency components< 100 Hz reach its output. Thus it is essentially a voltage which corresponds to the fundamental frequency of the current peaks produced by such thicker yarn sections or current dips produced by thinner yarn sections which passes through filter 24 to a threshold value switch 25 and if this voltage is of the appropriate amplitude, a pulse will reach a counter 26 connected to the output of switch 25.
Counter 26 counts, or adds, the pulses supplied thereto during each time period, the duration of which is set by a time member 27, and when a given counter state is exceeded during one of these time periods, the counter emits an output signal, for example, to switch on the warning lamp 28 or to actuate the switch 29 which switches off the drive to the turbine.
If, in addition, a longer duration increase and/or decrease in current magnitude are to be sensed, the voltage observed across resistor 23 is fed, in the circuit shown in FIG. 2, to a comparator 30 which compares this voltage with a desired voltage and, beginning with a given deviation from the desired voltage, emits an output signal which actuates the warning and/or switching device 28, 29, for example, only if the deviation continues for more than a given time, the duration of which is determined by a time member 31. The comparator 30 may include a memory member which derives the comparison value, i.e., the desired voltage from the previously determined actual signal, e.g., during the preceding 1 second, so that here, too, a change produces an output signal.
In addition to monitoring the current in the manner shown in FIGS. 1 and/or 2, the radial deflections of the bearing 7 or of the rotor 1, 5 of the turbine of FIG. 1 as the result of imbalances produced by thicker yarn sections can be detected, as shown in FIG. 3, by means of a sensor 32 which operates, for example, according to the piezoelectric principle and is associated with one of the elastic O-rings 13 of the elastically mounted bearing. Sensor 32 produces pulses in response to fluctuations in pressure, which pulses are fed via threshold value switches 33 to a counter 34 which upon counting a given number of pulses within a given period of time emits an output signal to members 28 and 29, shown in FIGS. 1 and 2.
The current consumption of a turbine drive motor is dependent on several things. Changes in that current for which a warning or switch-off signal should be produced may be, for example, more than 5%. The duration of time member 31 of FIG. 2 may be 1 or several seconds. The number of changes allowed in the circuit of FIG. 1 may be less than 50. Similarly the changes allowed in FIG. 3 may also be less than 50.
It will be understood that the above description of the present invention is susceptible to various modifications, changes and adaptations, and the same are intended to be comprehended within the meaning and range of equivalents of the appended claims.
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In order to monitor irregularities and changes in structure of yarn being produced in an open-end spinning turbine provided with its own individual drive motor, there is provided a circuit which senses and evaluates changes in the current consumption by the motor.
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This invention relates to papermaker's belts and has to do with a biplanar fabric for clothing the forming area of the papermaking machine, although fabrics in accordance with the invention also may be used for other paper machine applications.
BACKGROUND OF THE INVENTION
Fundamentally, the forming area of the papermaking machine has been clothed by fabrics woven from synthetic materials, i.e., man-made fibers. The general structure of these fabrics has taken two basic forms -- the first comprising a monoplane fabric and the second a double layer or duplex fabric. In a monoplane fabric the woven members travel through the fabric passing from one surface to the other surface in each repeat of the pattern across the width and length of the fabric. The successive warp or filling members will lie side-by-side as near to the center plane of the fabric as the balance in the weave pattern will permit, with the warp and filling yarns interlaced. Thus, the weave pattern, float length and stiffness/diameter of the yarn are the controlling factors which establish the parameters of the fabrics which can be formed. In order to achieve greater strength, stiffness and service life, a double layer or duplex fabric has been used.
A duplex fabric is one in which greater stiffness and strength is obtained by using stacked filling yarns, i.e., sets of filling yarns which are stacked one above the other in two planes. In a duplex fabric, the filling yarns do not interlace from surface to surface; rather, the warp yarns form a double house for the filling yarns in such a way that the sets of filling yarns remain directly over and under each other, the warp yarns crisscrossing between the filling yarns on each side of the fabric, the warp yarns thereby locking the filling yarns in their over and under configuration.
A typical duplex fabric, identified as "prior art", is illustrated in FIG. 1. As seen therein, warp yarns 1, 2, 3 and 4 (which in use lie in the cross-machine direction when the fabric is endless and in the machine direction when the fabric is woven flat) pass between the sets of filling yarns, the yarns 6 and 7 in each set being stacked one above the other in spaced apart planes. The weave illustrated produces an identical pattern on each surface of the fabric. A duplex pattern of this character has been found to have certain disadvantages, particularly when used as a forming fabric. One of the disadvantages results from the cross-machine knuckles which are formed at the points 8 where the warp yarns pass around the filling yarns 7 on the bottom surface or machine side of the fabric. These knuckles are particularly subject to wear and offer minimal protection to the load bearing machine direction yarns 7. In addition, the knuckles coincide with and accentuate the straight and rigid machine direction yarns 7 and create tracking and roll oscillation problems.
Another problem inherent in duplex weave patterns currently in use is the presence of open areas or pockets, indicated at 9 in FIG. 1, which in numerous instances create fabrics having an excessively open construction which causes dimensional instability. In addition, where such open areas exist, reactive forces are captured within the cross-machine yarns 1, 2, 3 and 4 as they cross and interlace between the sets of machine direction yarns 6 and 7. These reactive forces create rigidity relative to any two sets of machine direction pairs, and this restrictive condition in a fabric which inherently has little cross-machine stability prevents the flow and redistribution of the stress producing forces, thereby contributing to the formation of undersirable pockets, roping and wrinkles.
The present invention seeks to overcome the foregoing disadvantages by providing biplanar fabrics which close the objectionable open areas and at the same time provide greater fabric life, particularly on the machine wear surface, as well as better tracking and smoother running with less fatigue related problems.
SUMMARY OF THE INVENTION
In accordance with the invention the sets of machine direction or filling yarns, while formed in two planes, are not stacked directly over and under each other, but rather the two yarns in each set are offset laterally relative to each other so that the sets of filling yarns are diagonally disposed and lie in what may be characterized as interdigitating relation. This configuration effectively closes the open areas or pockets which are characteristic of conventional duplex fabrics.
Another feature of the invention lies in the increased exposure of the warp or cross-machine direction yarns on one side of the fabric. Increased exposure of the warp yarns on the machine side of the fabric acts to reduce wear of the machine direction filling yarns, which are the load bearing members when the fabric is in use. For example, the warp yarns may be given two and two floats on the machine surface of the fabric to provide greater fabric life as well as better tracking and smoother running. Other weave patterns also may be used, the essential consideration being the increased exposure of the cross-machine direction yarns on the machine side of the fabric.
For certain papermaking applications, the fabric can be inverted so that the paper is formed on the surface of the fabric having the greater exposure of cross-machine direction warp yarns. In this instance the surface characterics of the paper forming surface are improved and machine drag is reduced on the machine surface of the fabric.
Accordingly, a principal object of the invention is the provision of biplanar fabrics having improved machine direction strength as well as improved cross-machine stability.
Another object of the invention is the provision of fabrics having sets or pairs of filling yarns formed in biplanar relation, by which is meant that the upper and lower filling yarns do not necessarily lie in spaced apart planes as in a conventional duplex fabric, but rather the planes defined by their facing surfaces may coincide or overlap. This biplanar relationship is the result of the diagonal disposition of the sets of filling yarns relative to each other and the manner in which the warp yarns pass between them, the warp yarns in one direction passing diagonally from one surface of the fabric to the other between adjacent pairs of the laterally offset filling yarns, and diagonally between the upper and lower filling yarns in another set in the opposite direction, thereby effectively closing the open areas or pockets which are formed when the filling yarns are stacked one above the other and the warp yarns are passed diagonally between the two yarns in each vertically aligned pair.
A further object of the invention is the provision of biplanar fabrics which are particularly suited for clothing the forming area of a papermaking machine, the fabrics providing enhanced stability and longer useful life.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic vertical sectional view illustrating a conventional prior art duplex fabric.
FIG. 2 is a diagrammatic vertical sectional view illustrating a fabric in accordance with the present invention.
FIG. 3 is a diagrammatic vertical sectional view illustrating a modification having a different weaving pattern.
FIG. 4 is also a diagrammatic vertical sectional view illustrating another modification of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 2 of the drawings, the fabric illustrated comprises warp yarns 1A, 2A, 3A and 4A, together with sets of filling yarns 6A and 7A which, in accordance with the invention, are diagonally disposed relative to each other. In effect, the filling yarns 7A, which in this instance are on the machine side of the fabric, lie in interdigitating relation relative to the filling yarns 6A. The upper and lower filling yarns may lie in spaced apart planes although preferably the facing surfaces of the upper and lower filling yarns in each set will overlap, as illustrated by the planes x and y in FIG. 2. The warp yarns 1A-4A also extend diagonally between the upper and lower surfaces of the fabric. Thus, the yarn 1A passes over the yarn 6A of the first or leftmost set of filling yarns and then diagonally downwardly between the first and second sets of filling yarns, the yarn 1A then extending along the bottom surface of the fabric until it passes under the yarn 7A of the third set of filling yarns, whereupon it extends diagonally upwardly between the yarns 6A and 7A of the fourth set of filling yarns, the pattern being repeated as the yarn 1A passes over the yarn 6A of the fifth or rightmost set of filling yarns illustrated.
In like manner, the warp yarn 2A passes over the yarn 6A of the second set of filling yarns and extends diagonally downwardly between the second and third sets of filling yarns, the yarn 2A then extending along the bottom surface of the fabric until it passes under the yarn 7A of the fourth set of filling yarns, whereupon it passes diagonally upwardly between the yarns 6A and 7A of the fifth set of filling yarns so that the pattern is repeated as the warp yarn 2A passes over the filling yarn 6A in the sixth set of filling yarns (not shown). As will be evident from FIG. 2, the warp yarns 3A and 4A will successively follow a like pattern, which pattern may be characterized by the warp yarn passing over the upper filling yarn in a first diagonally disposed set of filling yarns and then diagonally downwardly between the first and a second set of diagonally disposed filling yarns and then under the lower filling yarn in the second set as well as under the lower filling yarn in the next adjacent or third set of diagonally disposed filling yarns, whereupon the warp yarn extends diagonally upwardly between the upper and lower filling yarns of a fourth set of the diagonally disposed filling yarns. Each of the warp yarns has two floats, indicated at 10, and the resultant fabric has the surface characteristics of a twill weave.
As will be readily understood by the worker in the art, the pattern lends itself to a number of variations, one of which is illustrated in FIG. 3. As seen therein, the basic pattern is the same, namely, over one upper filling yarn in a first diagonal set, diagonally downwardly between the first and second sets of filling yarns, beneath two lower filling yarns in the second and third sets, and then diagonally upwardly between the upper and lower filling yarns of the fourth set. Thus warp yarns 1B and 2B are the same as in FIG. 2, but in this instance the positions of warp yarns 3B and 4B are reversed, with warp yarn 3B passing over the upper filling yarn in the fourth set, whereas warp yarn 4B passes over the upper filling yarn in the third set. Such rearrangement results in a variation in both the top and bottom surfaces of the fabric forming a four harness satin or crow's foot pattern on the top surface.
It will be understood that additional pattern variations may be achieved by altering the sequence of the warp yarns, as for example, 1, 3, 2, 4, as will be understood by the worker in the art. In addition, the number of warp yarns may be increased to provide additional variations in either or both surfaces of the fabric being formed, the essential considerations being the diagonal disposition of the sets of filling yarns and the greater exposure of the warp yarns on one surface of the fabric.
While a preference is expressed for a pattern wherein the warp yarns pass under two adjacent lower filling yarns, the number of filling yarns beneath which each warp yarn passes may be increased. For example, each of the warp yarns may pass beneath three or four, or even more, adjacent lower filling yarns before returning diagonally upwardly to the upper surface of the fabric. If the fabric is to be used in inverted condition, it will be understood that the two, three or more float configuration will be on the upper or papermaking side of the fabric. Thus, as illustrated in FIG. 4, a fabric is provided comprising warp yarns 1C, 2C, 3C, 4C and 5C, together with diagonally disposed sets of upper and lower filling yarns 6C and 7C, thereby providing an inverted fabric in which the warp yarns have a three float pattern, indicated at 11.
The nature of the materials from which both the warp and filling yarns are formed does not constitute a limitation on the invention. Normally the yarns will be synthetic and may comprise either monofilament or multifilament yarns, or combinations thereof.
It is to be understood that modifications may be made in the invention without departing from its spirit and purpose, and consequently it is not intended that the invention be limited other than in the manner set forth in the claims which follow. It is also to be understood that the terms "upper" and "lower" as they appear in the claims are used in a relative sense to set forth the relationship between the warp and filling yarns, the fabrics being reversible depending upon the characteristics desired for their respective paper and machine surfaces.
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A papermaker's belt particularly suited for use as a forming fabric, the fabric being of biplanar construction with sets of upper and lower filling yarns interconnected by warp yarns extending between the upper and lower surfaces of the fabric, the fabric being characterized by diagonally disposed sets of upper and lower filling yarns with the warp yarns extending diagonally between adjacent sets of the filling yarns in one direction and diagonally between the upper and lower yarns of another set of filling yarns in the opposite direction.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority under 35 U.S.C. § 119 on U.S. provisional application Ser. No. 60/183,948, filed on Feb. 22, 2000.
BACKGROUND OF INVENTION
[0002] 1. Field of the Invention
[0003] The invention relates to a device for quickly and easily estimating the required floor covering for a particular sized room and, more particularly, to an estimating device that determines the extra length of floor covering required to cover the fill area for a specified room and a specified floor covering width.
[0004] 2. Description of the Related Art
[0005] All commercial and residential construction typically includes one or more rooms whose floor is covered by a floor covering that is manufactured in rolls of predetermined width. Typical floor covering materials include carpet, linoleum, etc. Carpeting, for example, is commonly manufactured in widths of 12 feet, 13 feet 6 inches, and 15 feet.
[0006] Throughout the construction process, there is a repeated need to estimate the amount of floor covering needed to cover a particular room. The contractor, wholesaler, and floor covering salespeople can all have a need to estimate the quantity of floor covering needed to cover a particular room.
[0007] The floor covering estimating process is susceptible to many sources of errors or inefficiencies. One source of error occurs because most rooms, even rectangular rooms have at least one room dimension that does not coincide with the manufactured width for a particular floor covering, resulting in the major portion of the room being covered by a single piece of the floor covering having a length equal to the room dimension and a width equal to the manufactured width (the full width area or full run portion) and the remainder of the room (the fill area generally having a width less than the floor covering manufactured width) being filled by sections of the floor covering cut to a width less than the floor covering manufactured width. Depending on the shape of the room, it can have multiple fill areas.
[0008] The length of floor covering needed to cover the full width area is simple to calculate. The fill area is more difficult to calculate because the floor covering manufactured width typically does not coincide with the fill area width and it is desirable to minimize the total area of floor covering purchased to cover the full width area and the fill area, requiring the estimator to determine which fractions of the manufactured width will most efficiently cover the fill area while minimizing the additional length of the floor covering that must be purchased. The calculation of the extra length needed to cover the fill area is exacerbated in that the fill area for most rooms will vary depending on which dimension or direction the full width run is oriented. For example, in a rectangular room, the room has a major dimension and a minor dimension. Depending on the length of the major and minor room dimension and the floor covering manufactured width, making the full width run parallel to one of the major and minor dimensions will result in a lower total area of floor covering than if the full width run is parallel to the other dimension. To determine which dimension the full width run should align with to minimize the total floor covering area required, the estimator must make multiple estimations of the total area of floor covering required by orienting the full width floor covering run along both of the dimensions and then calculating the corresponding fill to determine the floor covering orientation that results in the minimum area of floor covering. The need to calculate multiple estimates on a single room increases the likelihood that an error might be made by the estimator.
[0009] The potential source for error in estimating the appropriate amount of floor covering is further exacerbated in that many types of floor covering are sold in square yards and most building plans are sized in square feet. Although the mathematical conversion from square yards to square feet or visa versa is well known and relatively common, in practice, the actual calculation is the source of many errors. The errors in the area calculation is compounded by not all blueprints being drawn to the same scale, which can lead to an incorrect calculation for the total area of the room.
[0010] There is a need in the floor covering industry to have a simple and easy to use device for quickly calculating the minimum amount of floor covering required for a particular room while accounting for the particular scale of a drawing, the particular width of the floor covering, and the particular dimension in which the floor covering is sold.
SUMMARY OF INVENTION
[0011] The invention relates to a device for estimating the length of the floor covering needed from a roll of floor covering having a predetermined width to cover a room, including any fill area based on a scale diagram of the room showing walls bounding the room. The device comprises a generally planar body having an upper surface and opposing lower surface for contacting the diagram. A first positioning guide is provided on the body for aligning the body on the diagram about a first direction. A second positioning guide is provided on the body for aligning the body on the diagram about a second direction. Floor covering width and length indicia are provided on the body along the first and second axes, respectively. Fill width indicia is provided on the body and corresponds to the first direction. A data matrix comprising multiple cells is defined by the intersection of the fill width indicia and the floor covering length indicia. At least some of the cells contain a fill length data indicia who's value is the length of the floor covering needed for a fill area corresponding to the intersecting fill width indicium and floor covering length indicium itself.
[0012] Preferably, at least one of the first and second positioning guides is an edge surface of the body. Alternatively or in combination, at least one of the first and second positioning guides is a line provided on the body. Yet another alternative or combination includes at least one of the first and second positioning guides being a slot formed in the body. While the range of values for the indicia can be any desired, is preferred that the width indicia at least include a value corresponding to the width of the floor covering whose length is being estimated.
[0013] The device can further comprises a second data matrix having multiple cells. Each of the cells corresponds to a floor covering length indicia and contains an area data value representing the area covered by a piece of floor covering of the predetermined width and the corresponding floor covering length indicia. The floor covering predetermined width is preferably selected from one of 12 feet, 13 feet 6 inches, and 15 feet. The floor covering width and length indicia are also of a predetermined scale. Is preferred that this predetermined scale be equal to the scale of the diagram. Suitable scales include one-eighth inch equals one foot, one-quarter inch equals one foot, and three-sixteenths inch equals one foot.
[0014] In one aspect, the floor covering width indicia can define the fill width indicia, negating the need to have separate indicia for both values. The floor covering width and length indicia can also form the corresponding first and second positioning guides.
[0015] The body can comprise first and second spaced sides and first and second spaced ends connecting the spaced sides to form a generally rectangular body. The body preferably has a width equal to the length of the sides and the body width is scaled relative to the predetermined width of the floor covering. The scale of the body width is equal to the scale of the diagram for which the floor covering is being estimated. Suitable scales include the one-eighth inch equals one foot, one-fourth inch equals one foot, and three-sixteenths inch equals one foot. Preferably, the floor covering predetermined width is one of 12 feet, 13 feet 6 inches, and 15 feet.
[0016] When the body takes a generally rectangular shape, it is preferred that the first end forms the first positioning guide and the first side formed the second positioning guide. In this configuration, it is also preferred that the floor covering width indicia is adjacent to and extends along the first end and the floor covering length indicia is adjacent to an extends along the first side. The fill width indicia can be defined by the floor covering width indicia or can parallel the floor covering width indicia as desired.
BRIEF DESCRIPTION OF DRAWINGS
[0017] In the drawings:
[0018] [0018]FIG. 1 illustrates a first embodiment of the floor covering estimating device according to the invention for a floor covering having a manufactured width of 15 feet;
[0019] [0019]FIG. 2 illustrates the use of the first embodiment floor covering estimating device to determine the floor covering needed along a for the full-width area for a sample room along a first room dimension;
[0020] [0020]FIG. 3 illustrates the use of the first embodiment floor covering estimating device to determine the extra length of the floor covering needed to complete the fill area for the example of FIG. 3;
[0021] [0021]FIG. 4 illustrates the use of the first embodiment floor covering estimating device to determine the length of the floor covering the particular room for the full-width run along a second dimension;
[0022] [0022]FIG. 5 illustrates a second embodiment of the floor covering estimating device according to the invention for a floor covering having a manufactured width of 12 feet;
[0023] [0023]FIG. 6 illustrates a third embodiment of the floor-covering device according to the invention for a floor covering having a manufactured width of 13 feet 6 inches; and
[0024] [0024]FIG. 7 illustrates a fourth embodiment of the floor-covering device according to the invention.
DETAILED DESCRIPTION
[0025] [0025]FIG. 1 illustrates a floor covering estimating device in the form of a template 10 having opposing ends 11 of a predetermined width W T and opposing sides 13 of a predetermined length L T . A width indicia 12 is disposed along the upper and lower edges of the width W T . Similarly, a length indicia 14 is disposed along the edges of the length L T . The width indicia and length indicia 12 and 14 are preferably selected to conform to a predetermined scale, such as a ¼ inch equals one foot scale as illustrated in FIG. 1. Preferably the width and length indicia 12 , 14 are divided into full and half marks, representing one foot and half foot increments. The width and length indicia are placed on both sides of the template 10 for convenience. Together, one pair of the width and length indicia form the indices of a matrix or grid representing the physical dimension of the template 10 .
[0026] It should be noted, that for purposes of the invention, the width and length indicia 12 , 14 can be selected for any desired scale. Preferably the scales are those most commonly used in the construction industry, such as ⅛ inch equals one foot, ¼ inch equals one foot, and {fraction (3/16)} inch equals one foot. It should also be noted that the width W T of the template 10 is preferably selected to correspond with a commonly sold floor covering width, such as 12 feet, 13 feet 6 inches, and 15 feet.
[0027] A column of first area indicia 16 is disposed on the template and positioned between the width and length indicia 12 , 14 . The area indicia 16 includes individual area values that are physically located on the template 10 so that they align with each of the full and half length indicia 14 . The value of the area indicia 16 corresponds to the floor covering full width, 15 feet in the case of template 10 , multiplied by the length indicia 14 .
[0028] The area indicia 16 as illustrated in FIG. 1 preferably displays the area in units of square feet. A second column of area indicia 18 extends along an opposite side of the template 10 and is similar to the first area indicia 16 , except that the second area indicia displays values of area in units of square yards.
[0029] It should be noted that while the template 10 preferably uses dimensions of square feet and square yards for the area indicia 16 , 18 , it is within the scope of the invention for any desired dimension to be used. Also, although two area indicia 16 , 18 are disclosed in the template 10 , any number of area indicia can be used and would depend on the particular needs of the user.
[0030] A fill width indicia 20 is arranged in columnar form and disposed between the area indicia 16 and 18 . The intersection of the fill width indicia 20 and the length indicia 14 forms a data matrix comprising a plurality of cells arranged in multiple rows and columns, with each of the cells containing fill widths 22 . The fill widths 22 of a particular cell correspond to the length of floor covering needed to fill an area having a width equal to the corresponding fill width indicia 20 and length indicia 14 .
[0031] For the template 10 , the predetermined fill widths 22 correspond to floor covering fill widths of 2 feet 6 inches, 3 feet, 5 feet, and 7 feet 6 inches. These predetermined fill widths are selected based on the most commonly occurring fill widths for a 15 foot width. The fill widths can include more, less, or different fill width data. The fill width data will also vary for carpets of different widths. For example, the common fill widths for a 12 foot wide floor covering are 2, 3, 4, and 6 feet. The common fill widths for a 13 foot 6 inch wide floor covering are 2 feet 3 inches, 3 feet 3 inches, 4 feet 6 inches, and 6 feet 9 inches.
[0032] The columnar indicia disposed underneath each of the predetermined fill width indicia 22 are physically positioned on the template 10 so that they align with one of the length indicia 14 . The value of the columnar indicia disposed below the predetermined fill width indicia 22 represents the additional length that must be added to the full width floor covering length to permit a complete covering of a fill area corresponding to the predetermined fill width indicia 22 while minimizing the total area of the floor covering required to cover a room.
[0033] An explanation of the use of the template 10 will aid in the understanding of the importance of the spatial relationship and numerical value of the width indicia 12 , length indicia 14 , area indicia 16 , area indicia 18 , fill width indicia 20 , and predetermined fill width indicia 22 . FIG. 2 illustrates the template 10 in the context of an architectural drawing 24 having a room 26 with a room width W R of 17.5 feet and a room length L R of 14 feet. The room width W R and length L R can be thought of as the major and minor dimensions for the room 26 and also serve as the reference directions for positioning the template. To begin the floor covering estimating process, the template 10 , which is of the same scale as the architectural drawing 24 , is placed on the architectural drawing 24 so that one of the corners, preferably the upper right, of the template 10 coincides with a corner of the room 26 and the length L T of the template 10 coincides with the length L R of the room 26 . In other words, the side of the template 10 is aligned with the diagram in a direction according to the room length and the end of the template 10 is aligned with the width of the room in a second direction. Essentially, the template ends 11 and sides 13 form positioning guides for positioning the template relative to the drawings such that the template end 11 is aligned relative to the room length and the template side 13 is positioned relative to the room width. In this manner, the full width run is parallel to the minor dimension of the room 26 .
[0034] The user draws a line 28 along the side of the template 10 , which divides the room 26 into a full width area 30 and a fill area 32 . The length of the room is then noted along the length L T of the template 10 by referencing the length indicia 14 , which is 14 feet in the case of the room 26 . The area value corresponding to the 14 foot length value is selected from the area indicia 16 or 18 . For purposes of this example, the area indicia 16 is selected, which shows the area covered by the template in the room 26 for the full width run is 210 square feet. The full width area represents the area of the room 26 that a full width of the floor covering will cover in a length of 14 feet.
[0035] Once the full width area is determined, the amount of floor covering for the fill area 32 must be calculated. Referring to FIG. 3, the template 10 is moved so that the left hand length side of the template 10 is aligned with the room edge in the fill area and overlies the line 28 . The template 10 is preferably transparent or translucent to permit the lines of the drawing 24 to be viewed through the template 10 . The width indicia 12 is examined to determine the width of the fill area 32 , which is 2 feet 6 inches in the example. The user then consults the fill width information 20 and selects the predetermined fill width indicia 22 corresponding to the measured fill width of 2 feet 6 inches. In the predetermined fill width indicia 22 corresponding to a 2 feet 6 inch fill width, the user selects the value in the fill width data column that corresponds to the room length L R of 14 feet, which equals 2 feet 6 inches. The 2 feet 6 inch value is the minimal additional length of floor covering that is required to cover the 2 foot 6 inch by 14 foot fill area 32 while minimizing the total area of the floor covering for a floor covering having a predetermined width of 15 feet. The total area of additional floor covering needed for the fill area is calculated by multiplying the additional length required for the 2 foot 6 inch fill area (2 feet 6 inches) by the width of the floor covering 15 feet, resulting in a floor covering fill area amount of 37.5 square feet.
[0036] The total square footage of floor covering needed to cover the room 26 is the sum of the area of the full width run (210 square feet) and the floor covering fill area total area (37.5 square feet) for a total area of 247.5 square feet. Thus, 247.5 square feet of floor covering is required to cover the floor of the room 26 if the full run is along the major dimension L R . The total area can easily be estimated using the template 10 by adding together the length of the full width run (14 feet) and the fill length (2 feet 6 inches) to obtain a total length (16 feet 6 inches), finding the total length on the template and examining the corresponding area. In a similar manner, the total area can be converted to square yards from square feet.
[0037] To cover the floor of any room with the minimal amount of carpet and, thus, at the lowest expense, it is necessary to estimate the amount of floor covering with the full width run along the major dimension W R . The direction of the full width floor covering run can result in different fill widths, which in most cases yields different total areas of floor covering required to cover the same room. Referring to FIG. 4, the floor covering is estimated by using the major dimension W R as the full width dimension. The steps of estimating the total floor covering along the major dimension W R are identical to the minor dimension L R except for the orientation of the template 10 with the major dimension W R . Therefore, the steps will not be described in detail and only the results will be discussed.
[0038] Since the floor covering width is wider than the room width W R , there will be no fill area. The full width area 30 ″ of the room 26 is 262.5 square feet as seen in FIG. 4 since the full width run is 17 feet 6 inches. Orienting the floor covering in this manner eliminates seams in the carpet, but wastes a 1 foot by 17 foot 6 inch strip.
[0039] The total length of carpet needed to cover the room 26 is the full run along the room length L R of 16 feet 6 inches for a total area of 242.5 square feet. This is compared to the total length of the floor covering when the full width is aligned with the dimension W R , which is 17 feet 6 inches for a total area of 262.5 square feet. As can be seen by these two estimations, less floor covering is needed to cover the room 26 if the full width run aligns with the minor dimension L R .
[0040] It should be noted that the amount of material saved by having the full width run along the major or minor dimension will vary depending on the particular room size, the floor covering width, shape, and the fill area width. In some cases, there will be no savings as both approaches will result in the same total length of floor covering. However, the estimates must be made for both dimensions to ascertain the savings, if any. Also, for the example of FIG. 4, the estimator could opt for a different floor covering width.
[0041] The values for the predetermined fill width indicia 22 are calculated by determining the fill segment size that will minimize the total area of floor covering required to fill the fill area for a floor covering of a given width. This calculation is not as simple as buying the smallest area of carpet need to physically cover the fill area because many floor coverings are manufactured with a repeating pattern and carpet floor coverings are manufactured with a grain. The pattern and grain must be kept in mind when determining the fill width.
[0042] For example, in the floor covering estimation along the dimension L shown in R FIGS. 2 and 3, the fill area is 2 feet 6 inches by 14 feet. Given that the floor covering width is 15 feet, one could purchase an additional 2 feet 6 inches of floor covering in the 15 foot width and use one 2 feet 6 inches by 15 feet piece to fill the fill area 32 . However, that would require orientating the fill width portion of floor at ninety degrees relative to the full run. It is likely the rotation of the floor covering will result in a misalignment of any pattern on the floor covering. If the floor covering is carpet, then the grain of the fill area carpet will not align with the grain of the full run carpet, resulting in an aesthetically unappealing installation. The fill widths of the template 10 according to the invention help the estimator determine the minimum amount of floor covering needed for a proper installation.
[0043] It is of tremendous value to the floor covering estimator to have the optimum length corresponding to a particular fill width disposed on the template 10 in a physical location so that the additional fill length corresponds to the length of the fill area. The spatial association of the optimum length for a given fill width with the fill area length permits the floor estimator to quickly and easily estimate the most cost effective amount of floor covering needed to cover the floor for a particular room. This is a great advantage of the floor-covering estimating device according to the invention. In the past, the estimator would have had to calculate the optimum additional length, resulting in a loss of time and increasing the risk of error.
[0044] The floor covering estimating device according to the invention further simplifies the estimating process by providing a template 10 that has width and length indicia 12 , 14 that correspond to the particular scale of the drawing 24 illustrating the room 26 whose floor covering is to be estimated. The placing and alignment of the template 10 on the drawing permits the user to almost instantaneously calculate the full width run length of the floor covering along with determining the corresponding area by reading the length and area indicia directly off the template. The template 10 further simplifies the determination of the fill area, which is accomplished by simply drawing a line along the right hand edge of the template 10 . The fill area is then quickly and simply determined by noting the width of the fill area upon moving the template and finding the corresponding additional floor covering length that corresponds to the room length.
[0045] The usefulness of the invention becomes greater as the room shape becomes more complex. The examples in this application are limited to simple rectangular rooms with no closets, bump outs, insets, etc. As the shape of the room becomes more complex so does the difficulty of estimating the minimum amount of carpet. If a room becomes very complex, it is common for many estimators to request a much larger area of floor covering than necessary to simplify the estimation process. For example, if the room of FIGS. 2 and 3 had an inset, such as a built-in bench or cabinet, extending into the room, an estimator may be tempted to estimate the amount of floor covering required as the 15 foot width in a length equal to the width W R , resulting in the waste of the floor covering that would have to be cut away for the inset. The template 10 of the invention provides for a simple and accurate estimation of complex room shapes, eliminating the need for over estimating.
[0046] [0046]FIGS. 5 and 6 illustrate second and third embodiments of 10 ″ and 10 of the template 10 . The second and third embodiments 10 ″, 10 are substantially identical to the first embodiment 10 and will not be described in detail other than noting the important distinctions. The second embodiment 10 ″ is floor covering having a manufactured width of 12 feet. The area indicia 16 ″ is limited to a single column unlike the two columns of area indicia 16 , 18 of the first embodiment. However, the single column of area indicia 16 ″ of the second embodiment contained both area values in square feet and square yards separated by a slash. The fill width indicia 20 ″ has predetermined fill width indicia 22 arranged in fill width of 2 feet, 3 feet, 5 feet, and 6 feet 9 inches, which are the most common fill widths for a 12 foot wide floor covering.
[0047] The third embodiment template 10 has width indicia 12 and length indicia 14 located about the width and length of the template 10 . The area indicia is arranged in two columns 16 , 18 , corresponding to area values and square foot units and square yard units, respectively. The fill width indicia 20 includes predetermined fill width indicia 22 in values of 2 feet, 3 feet, 5 feet, and 6 feet 9 inches, which are the most common fill widths for a 13 foot wide floor covering.
[0048] It is worth noting that the fill width indicia on the template 10 is for clarity sake limited to the most commonly occurring fill widths for a particular floor covering width. However, it is within the scope of the invention for the fill width data to be provided for the entire floor covering width. In such a configuration, the width indicia 12 would serve the dual role of the width indicia 12 and the headings for the fill width indicia 22 . The intersection of the width indicia 12 and the length indicia 14 would then define the data matrix containing the fill width data. Not all of the cells of the data matrix need to have fill width data. FIG. 7 illustrates a portion of the template 10 where the width indicia 12 also functions as the fill width indicia 22 and not all of the cells of the resulting data matrix contain fill width information.
[0049] If the data matrix takes up a sufficient amount of space on the template 10 so that there is not enough space to clearly display the area indicia 16 , 18 , the physical size of the template 10 can be increased so that one or both of the area indicia 16 , 18 can be moved outside of the area bounded by the width and length indicia 12 , 14 , such as is disclosed in FIG. 7.
[0050] In this configuration, if the area indicia 16 is moved to the left of the length indicia (as viewed in FIG. 1), it is convenient to use another structure other than the template sides 13 to function as a positioning guide for the template. Other suitable structures would include a line as 40 as shown in FIG. 7, which is preferably used when the template is made of a non-opaque material, or a slot (not shown), which is preferably used when the template is made of an opaque material.
[0051] Also in this configuration, if the area indicia 18 is moved to the right of the length indicia (as viewed in FIG. 1), it is convenient to use another structure other than the template sides 13 to function as a line-drawing guide. A suitable structure would include a slot 42 formed in the template 10 . The slot 42 should be wide enough to permit the insertion of a tip from a writing utensil. Such a slot could also be used for the positioning guide when the template is made from an opaque material.
[0052] While the invention has been specifically described in connection with certain specific embodiments thereof, it is to be understood that this is by way of illustration and not of limitation, and the scope of the appended claims should be construed as broadly as the prior art will permit.
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A device for estimating the length of the floor covering needed from a roll of floor covering having a predetermined width to cover a room, including any fill area based on a scale diagram of the room showing walls bounding the room. The device comprises a generally planar body having an upper surface and opposing lower surface for contacting the diagram. A first positioning guide is provided on the body for aligning the body on the diagram about a first direction. A second positioning guide is provided on the body for aligning the body on the diagram about a second direction. Floor covering width and length indicia are provided on the body along the first and second axes, respectively. A fill width indicia is provided on the body and corresponds to the first direction. A data matrix comprising multiple cells is defined by the intersection of the fill width indicia and the floor covering length indicia. At least some of the cells contain a fill length data indicium having a value that represents the length of the floor covering needed for a fill area corresponding to the intersecting fill width indicium and floor covering length indicium itself.
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This is a continuation of co-pending application Ser. No. 026,687 filed on Mar. 17, 1987, now abandoned.
TECHNICAL FIELD
The present invention describes a process for the manufacture of sintered mixed oxides, mainly for use as nuclear fuel, which are completely soluble in nitric acid alone. They are obtained starting with solutions of nitrates of the constituent elements.
The process is preferably applied to mixtures involving two or more elements which can take part in the composition of a nuclear fuel, for example U, Pu, Th, and other fissile or fertile elements, but also their combination with rare earth metals such as cerium or gadolinium. In this latter case, the process relates to the manufacture of control rods based on mixed sintered oxides, for example uranium/gadolinium.
The process can also be applied to uranium alone.
The material of the constituent elements of the mixtures can be of different origins: it may or may not have undergone irradiation, and may have any isotopic composition. In particular, uranium can be natural or enriched uranium, non-irradiated or derived from plants for reprocessing irradiated fuel after cooling and separation of the Pu and the fission products.
PRIOR ART
The processess for manufacture of fuels in the form of oxides are well known, both those for making fuels containing uranium alone and those for mixed fuels containing mixtures in variable proportions of two or more elements such as U, Pu, Th, etc.
Mixed fuels, for example U+Pu, can be made either from a mixture of powders (UO 2 and PuO 2 ) or from solutions of nitrates of each of the components.
They generally take the form of pellets, the term which will be used hereinafter and which will also denote any other geometrical form capable of being used for the production of fuel elements.
1. Starting with a mixture of powders, the main operations are as follows:
crushing the powders,
mixing the powders,
shaping and pressing the pellets,
high-temperature sintering,
grinding the pellets to bring them to size and examination of the texture.
The manufacturing scrap is recycled, according to the type of defect, to the sintering, to the crushing or further upstream for storage or possible redissolution.
2. Starting with solutions of nitrates, the main operations are:
mixing the solutions of the components of the fuel,
concentration of the solution obtained,
production of a mixed oxide in an appropriate physical form, uranium at this stage being at valency VI and Pu at valency IV,
where appropriate, calcining to obtain U 3 O 8 ,
reduction to obtain uranium IV,
stabilization of the uranium IV,
and then, as above:
shaping and pressing the pellets,
sintering,
grinding.
In this case also the oxides or pellets which do not conform to the specification, are recycled, after possible crushing, to calcining, to reduction, to the sintering or further upstream, in order to obtain a starting nitrate solution, after a dissolving operation followed, where appropriate, by a purification operation.
For the operation of production of a mixed oxide, several processes are known:
the uranium and plutonium are coprecipitated using ammonia, the precipitates is separated from the mother liquor containing dissolved ammonium nitrate, and this coprecipitate is dried and then calcined to obtain a mixed oxide in the form of grains, the particle size of which can be more or less readily adjusted using suitable precipitation devices known in other contexts;
the uranium and plutonium are coprecipitated using ammonia by a sol-gel process so as to obtain, after decantation, drying and calcining, microspheres of mixed oxides (see, for example, U.S. Pat. No. 4,397,778, French Pat. No. 2,501,061 or French Pat. No. 2,386,104).
In both of these possible techniques, there is generation of a radioactive effluent mainly containing ammonium nitrate and contaminated with heavy metals and radioactivity; it has to be processed before disposal or upgrading.
denitration is performed in the presence of an aid, enabling an intermediate oxide to be obtained having a large specific surface area, which is then suitable for the pressing and sintering of the fuel pellets. Such a process is described in French Pat. No. 2,498,364, in which the value of denitration is, in fact, noted although the latter is performed with the addition of ammonium nitrate. Denitration performed without an aid, as described in French Pat. No. 2,496,324, leads to an oxide which has to be crushed in order that it may be sintered.
When the grinding is complete, the shaped fuel material is obtained ready for use for producing finally the fuel assemblies introduced into nuclear boilers of the PWR, BWR, fast neutron or other type. After irradiation, cooling and dismantling of the assemblies, the irradiated fuel material is extracted from the assemblies and dissolved so as to be able to separate chemically the unburned uranium, the plutonium and the fission products. This dissolving process is difficult, because PuO 2 is only slightly soluble in pure nitric acid; this dissolution is achieved only in the heated state in the presence of hydrofluoric acid, and this causes problems in relation to the corrosion resistance of the reactors and other equipment. For PuO 2 to be soluble in pure nitric acid, UO 2 and PuO 2 have to be in solid solution, it being possible for this solid solution to be obtained during sintering provided that there is a very homogeneous distribution of PuO 2 in UO 2 and very intimate contact between these two species before sintering. This can be achieved if the starting powders are very finely divided (15 to 20 μm) or if the procedure employs coprecipitation or denitration.
TECHNICAL PROBLEM
The main difficulties to be solved, or the advances which the experts are currently seeking to achieve, relate to the simplification of these processes, which employ products which are highly radioactive or dangerous such as plutonium. In this field, the simplifications result in considerable gains as regards the safety of the personnel or the environment, and in installation and operating costs.
A first series of problems arises from the handling of the powders.
At present, available Pu is mainly in the form of PuO 2 powder and, in order that it may be used in mixed fuels, this requires expensive fine crushing in order to be able to obtain very good homogeneity of distribution of the Pu in the powder mixture. For example, in a pellet, not more than 5% of the PuO 2 present must be in particles of diameter greater than 200 μm.
Crushing of this kind, and similarly the mixing of the powders, cause cost and health problems on account of the formation of aerosols which are difficult to neutralize. These problems arise whenever certain operations are performed on the oxides or powders, such as:
crushing of the cooled irradiated fuel, prior to dissolving it in nitric acid in the presence of hydrofluoric acid for reprocessing of the fuel, the problems being heightened in this case by the presence of fission products;
crushing during recycling of the fuel pellets which do not conform to the specifications, either to produce a powder, shaped again by pressing and sintered, or to make the product soluble;
in the process starting with nitrate solutions, crushing designed to achieve very good flowability of the oxide powder obtained after the coprecipitation and calcining.
A second problem arises from the fact PuO 2 is only soluble in nitric acid in the presence of hydrofluoric acid.
In particular, with the mixed fuels obtained from powders, this dissolution can, as has just been seen, be achieved only after crushing of the pellets. This greatly complicates the operations of reprocessing the fuel, or recycling the waste, and there is consequently an advantage to be gained from producing pastilles which are directly soluble in nitric acid alone. The use of hydrofluoric acid is expensive, requires appropriate additional equipment and causes a number of operating problems; for example, in French Pat. No. 2,480,019, a process is described for removing the fluoride ions thereby introduced.
The dissolution of the mixed fuels must, moreover, be complete.
a third problem arises, in the process starting with nitrate solutions, from the presence of a liquid effluent generated by the coprecipitating alone or via a sol-gel process. The processing and the disposal of this radioactive effluent must be regarded as forming an integral part of the process. In effect, in the nuclear sector, any cycle for treatment of effluent must be closed and not give rise to any waste.
These problems have to be solved while retaining the intrinsic qualities of the intermediate products obtained during the production of the fuel. In particular, the powders must:
flow freely, including under the action of gravity alone, during transfers from one vessel to another or during the shaping of the fuel. This flowability is due to the crushing in the processes starting with powders. In the processes starting with nitrate solutions, it is obtained directly if a sol-gel process is used for the production of the intermediate oxide. In contrast, if simple coprecipitation is used, a simple breaking up of clumps or gentle crushing may be necessary;
retain properties, such that the shaping of the fuel and the sintering can be carried out under the conditions which are known at present.
Likewise, the finished fuel must obviously comply with the very strict specifications in force.
To solve the problem of completely dissolving (less than 0.5% of insoluble material) the sintered mixed oxide fuel material without employing expensive prior fine crushing or addition of hydrofluoric acid, different processes have been proposed which vary in the ease with which they may be carried out:
for example, a process described in French Pat. No. 2,419,924, starting with a nitrate mixture, consists in oxidizing the Pu in this solution to state VI, in precipitating a mixed carbonate in the presence of a solution of (NH 4 ) 2 CO 3 , NH 3 and CO 2 , in filtering, thereby creating an effluent which requires processing, and in calcining and reducing the whole precipitate before the traditional shaping and sintering operations. This process is a variant of coprecipitation;
French Pat. No. 2,403,628 describes a process for handling powders with successive crushing, granulation and compacting stages before sintering, which has the disadvantages which are specifically due to the crushing stages;
French patent application No. 2,513,000 describes a process for pre-processing before dissolution for reprocessing the irradiated fuel, consisting in adding alkali metal salts or alkaline earth metal salts, and in heating to convert the oxides to uranates or plutonates and simultaneously to accomplish a pulverization of the fuel. Despite this, this process does not permit the complete dissolution of the Pu;
processes in a molten medium have also been described, using, for example, nitrate baths (BE 818,189).
SUBJECT OF THE INVENTION
The subject to the invention is a process for manufacturing mixed nuclear fuel based on sintered oxides, which enables fuel pellets to be obtained which are soluble, as they are, in nitric acid, thereby avoiding the use of hydrofluoric acid.
The subject of this process is also to eliminate wholly or partially the crushing operations which, in the prior art, can be necessary for complete dissolution of the pellets once they have been irradiated and cooled, or of the pellets scrapped during manufacture, or for making the powder mixtures homogeneous. It thus enables all risks of dangerous aerosol formation to be eliminated.
Its subject is also to eliminate the production of any effluent in the process, thereby making the process clean.
Another subject of the process is to obtain intermediate oxides which flow well.
Another subject is to obtain sintered shaped items or pellets which comply fully with the specification customarily required for the manufacture of nuclear fuels.
DESCRIPTION OF THE INVENTION
The process according to the invention, for the manufacture of mixed nuclear fuels based on a sintered mixture of uranium and at least one oxide of the elements of the group comprising Pu and Th, other fissile or fertile elements, rare earths including gadolinium, etc., but preferably of U and Pu, starting with solutions of nitrates of these elements, comprises:
(a) mixing the nitrate solutions in the desired proportions;
(b) concentrating this mixture solution by any means, under vacuum or otherwise, so as to remove the free water and, for example, to obtain uranyl nitrate in the hexahydrate form and plutonium nitrate, in which the plutonium can be in state IV and/or VI, in pentahydrate or hexahydrate forms, respectively;
(c) heat treatment to obtain an intermediate mixed oxide containing U in state VI and Pu in state VI and/or VI;
(d) where appropriate, calcining in the atmosphere at a temperature of at least 600° C., in cases where the mixed oxide obtained in (c) would be too reactive to be reduced directly, bringing, in particular, the uranium oxide to the state U 3 O 8 , and/or in cases where such a temperature would be necessary to convert a nitrate of an element in the mixture completely to oxide;
(e) reducing this oxide to bring the uranium and the plutonium to state IV;
(f) where appropriate, an operation for stabilization of the mixed oxide obtained;
(g) shaping and pressing the mixed oxide obtained, stabilized where appropriate, so as to obtain a so-called green item in any shape suited to the type of fuel element to be manufactured but preferably in the form of pellets;
(h) sintering in a reducing and/or gently oxidizing atmosphere at temperatures ranging from 700° C. to 1700° C., depending on the atmosphere chosen; and
(i) grinding the items obtained, enabling the items to be brought to size and the possible defects of texture (cracks, etc.) to be revealed.
It is characterized in that, for the purpose of producing an intermediate oxide during stage (c) without the production of effluent and without the consequent need to operate a process for processing and disposal of this effluent, of producing a powder of intermediate mixed oxides in stages (c), (d), (e) and (f) of high flowability, of producing compact items which can be sintered under the known conditions of the prior art, of producing sintered compact items which are soluble, as they are, in nitric acid alone, that is to say without the need to perform crushing or any other prior treatment of the said irradiated items or the manufacturing scrap and using for this dissolution only nitric acid alone, without adding hydrofluoric acid, denitration is performed by heating to obtain directly, without the addition of an aid, an oxide, mixed or otherwise, having high reactivity and characterized by a large specific surface area, either directly from the concentrated solution obtained in (b) or after crystallization, by cooling this solution, in the form of solid particles.
Several variants of thermal denitration, all designed to obtain an intermediate oxide having high reactivity during stage (c), possessing the advantages and characteristics noted above, are possible:
a first variant, starting with the concentrated solution obtained in (b), consists in crystallizing it in a first stage, either in the form of solid particles by flaking or by any other cooling process, or in the form of spherical solid particles obtained, for example, by spraying the concentrated solution into a cooled inert fluid or by granulation on a support composed of the oxide itself or by any other means, and in treating these particles, in a second stage, by a thermal denitration process which gives directly, without the addition of an aid, an oxide of high reactivity having a large specific surface area, as described in French Pat. No. 2,536,737 which forms an integral part of the present description. This thermal denitration is mainly performed under a partial pressure of water vapour of less than 8.7 kPa (65 mm of Hg) so that, during the heating, to a temperature of at least 260° C., the latter always remains below the melting point of the said particles; it leads finally to an intermediate mixed oxide having a large specific surface area which proves capable of being sintered after the stages of calcining where appropriate, and of reduction, according to the known processes;
another variant, starting with the concentrated solution obtained in (b), is characterized in that the solution is treated directly by a two-stage thermal denitration process, giving directly, without the addition of an aid, oxides having a large specific surface area as described in French Pat. No. 2,526,006 which forms an integral part of the present description, wherein, mainly, the first stage is performed up to a temperature generally of between 160° C. and 260° C. to give a dehydrated solid and the second stage up to a temperature equal at most to 600° C.; the mixed oxide having a large specific surface area obtained is capable of being sintered after additional calcining where appropriate and reduction, according to the known processes. In some cases, in particular when the denitration of an element in the mixture is difficult, it is necessary, as noted above, to perform an additional calcining at a temperature above 600° C. in order to obtain an oxide which can be sintered. Such is the case, for example, for gadolinium, where it is necessary to heat to approximately 800° C.;. Another variant possessing, in addition to the advantages and characteristics noted above, that of eliminating the possible calcining envisaged in (d), which would have been intended exclusively to decrease the reactivity of the oxides, also starts with the concentrated solution obtained in (b), and is characterized in that the solution is treated by a thermal denitration process giving directly, without the addition of an aid, mixed oxides of predetermined reactivity, the latter being adjusted by the specific surface area as described in French patent application No. 2,555,566 corresponding to U.S. Pat. No. 4,687,601 which forms an integral part of the present description, the process being performed mainly in two stages, the first in order to dehydrate the solution (b) incompletely, the second in order to decompose the product derived from the first under controlled pressure of water vapour which, depending on its value, determines the reactivity obtained;
other variants possessing, in addition to the advantages noted above, that of eliminating wholly or partially the phases of removal of the nitrogen in the different processes of thermal denitration are characterized in that:
in cases where the denitration is performed according to the process described in French Pat. No. 2,536,737, performed starting with solid nitrates, the process is stopped as soon as an infusible product has been obtained and the reduction envisaged in stage (e) is performed directly on the dehydrated infusible solid product obtained at the end of the first stage;
in cases where the denitration is performed according to the process described in French patent application No. 2,555,566, performed starting with nitrates in solution, the reduction envisaged in stage (e) of the partially dehydrated solid obtained at the end of the first stage is performed directly.
The mixed oxide powders obtained in (c) are perfectly freely flowing. However, in some cases, if the flowability was insufficient, it would be necessary to provide for a non-contaminant breaking up of clumps, which would enable the result to be achieved without having the disadvantages of fine crushing.
The pure solutions of uranium nitrate or plutonium nitrate, or of the nitrate of any other element used for making the mixture (a) can be obtained by various means. In particular, the solution of uranile nitrate can contain uranium originating from only one or from several of the following sources:
natural uranium,
non-irradiated enriched uranium,
non-irradiated depleted uranium,
irradiated enriched uranium (from reprocessing),
irradiated depleted uranium (from reprocessing).
In cases where enriched uranium is used, it can be derived from traditional enrichment plants where it is customarily obtained in the form of pure UF 6 , and it then undergoes a series of known chemical conversions designed to bring to the form of solutions, for example, successively, hydrolysis, reduction, calcining and dissolution. In cases of laser enrichment, the enriched uranium is obtained in the form of impure metal which is then dissolved in nitric acid, in the presence or absence of an oxidizing agent such as air, oxygen, hydrogen peroxide, etc., which is purified by known means such as backwash-extraction with tributyl phosphate solvent, to obtain a uranile nitrate solution capable of being used directly for the production of the mixtures of stage (a). Before dissolution, the metal can also be oxidized by any suitable means, such as air or oxygen, so as to reduce the consumption of nitric acid or the emission of nitrous vapours during the dissolution.
The denitration operation is performed with emission of water vapour and nitrous vapours NO x . According to an improvement of the present process, these nitrous vapours can be trapped, oxidized with air, oxygen, hydrogen peroxide or any other oxidizing agent, and then condensed so as to recover the nitric acid, which can be recycled directly or after concentration and without further treatment, for example for the dissolution operations.
The process according to the invention is preferably applied to U+Pu mixtures, it being possible for the ratio by weight Pu/(U+Pu) to reach 0.4, but also to combinations with rare earth metals, in particular cerium and gadolinium. It is also applied to the production of fuels containing uranium alone.
The Applicants have found that, surprisingly, the operations of reduction, of shaping by pressing and of sintering performed using these intermediate mixed oxides, obtained directly by one of the so-called high reactivity denitration processes, can be performed under working conditions identical to those used with intermediate mixed oxides derived from processes of the coprecipitation or powder mixture type, although the oxides from high reactivity denitration possess different physical properties. It has also found that the amount of binder added for the sintering could be considerably reduced.
The process according to the invention thus leads to sintered oxide fuel items, usually pellets, which are directly soluble in nitric acid alone, without prior crushing and without the addition of hydrofluoric acid, regardless of whether or not these pellets have undergone irradiation. The recycling of manufacturing scrap, and likewise the dissolution of cooled spent fuels for the purpose of reprocessing, are thus carried out under much simpler and safer conditions, since very fine crushing is no longer necessary.
The prorduct also satisfies very amply the requirements in respect of the rate of dissolution stated by the specialists; it is of the same order of magnitude as that obtained with uranium alone. The same applies to the dissolution yield, which is very high since it exceeds 99.9%. These exceptional results are due to the fact that the solid UO 2 +PuO 2 solution obtained through the effect of the sintering temperature is very good, as a result of the extremely intimate mixing of the different constituent elements, which is not destroyed by the denitration.
In coprecipitation, the constituents do not all precipitate under identical conditions, and this partially destroys this homogeneity obtained during liquid phase mixing and on denitration.
Thus, the homogeneity of the sintered mixed oxide is virtually perfect, since not only does it comply with the specification (no particle of PuO 2 exceeds a diameter of 400 μm measured by α- autoradiography and the mean diameter is less than 100 μm), but also no plutonium-bearing particle is detected either by α-autoradiography, X-rays or microprobe analyser.
Similarly, all the other properties demanded for the fuel are much more amply satisfied, in particular, higher densities, dimensional stability, perfect homogeneity, improved texture (absence of cracks, etc.), porosity and particle size.
EXAMPLES
Example 1
In this example, the Pu(NO 3 ) 4 solution was first prepared by concentrating by distillation 1000 cm 3 of a solution of 1.25 normal with respect to nitric acid and containing 21.95 g of Pu, to bring it to a volume of 330 cm 3 .
726.8 g of uranile nitrate hexahydrate were then added to obtain a nitrate mixture in solution in which the ratio (Pu/U+Pu)=0.06.
The mixed solution obtained was concentrated at up to approximately 140° C.
This solution was then crystallized by flaking, cooling it to minus 95° C. 744 g of solid product were obtained.
This product was then dehydrated and denitrated according to the process described in Patent FR No. 2,535,737, heating under a total reduced pressure of less than 0.13 kPa (1 mm of mercury) and maintaining the temperature of the product during the temperature rise always below its melting point:
rate of temperature rise obtained: 250° C./h.
maximum temperature reached: 400° C.
The specific surface area of the intermediate oxide obtained is 40 m 2 /g.
The calcining of this product was carried out for 1 h at 600° C. and followed by the breaking up of clumps by hand, the product then passing a 125 μm sieve.
The reduction was carried out at 600° C. for 1 h with hydrogen diluted to 5% in argon.
The stabilization was carried out at 40° C. with an argon/air mixture:
______________________________________10 min with an argon/air ratio = 5:120 min with an argon/air ratio = 2:140 min with an argon/air ratio = 1:1______________________________________
and was followed by cooling under vacuum.
The pelletizing was carried out with a floating-die hydraulic press by direct pressure after adding 0.7% of Zn stearate.
3 tests were carried out: at 3.5 t/cm 2 , 4.5 t/cm 2 and 5.5 t/cm 2 .
The sintering was carried out in a reducing atmosphere (Ar/H 2 mixture containing 5% of hydrogen) according to the following heating scheme:
150° C./h up to 900° C.
300° C./h up to 1640° C., followed by a 6 h plateau period.
By way of experiment, a second 6 h plateau period at 1740° C. was applied.
The following results were obtained:
______________________________________ DensitiesPelletizing (as % of the theoretical density)pressure Plateau at Plateau atTest t/cm.sup.2 Green Sintered 1640° C. 1740° C.______________________________________1 3.5 45.5 94.4 94.7 94.62 4.5 49.0 95.0 94.8 94.63 5.5 51.7 93.2 93.3 93.3______________________________________
It is seen that the densities are acquired as soon as the product is sintered, and that maintenance at a temperature plateau is unnecessary. The densities comply with the specifications.
The yields of dissolution in 14N nitric acid at 100° C. for 6 h are excellent:
99.94% for the sintered product of test (3)
99.99% for the product resintered at 1740° C. of test (2)
99.96% for the sintered product of test (1).
Autoradiography, while detecting a slight heterogeneity of the distribution of Pu, nevertheless shows that the product satisfies the specifications, and the heterogeneity has no influence on the rate or yield of dissolution.
Example 2
The starting substances and the process followed in this example were the same as in Example 1. It differs therefrom mainly in that the breaking up of clumps is omitted and, in addition, some parameters were slightly modified.
In the denitration, the rate of temperature rise obtained was 250° C./h and the temperature reached was 380° C. The reduced pressure was identical.
The calcining was performed at 525° C. for 1 h. The breaking up of clumps was omitted.
The reduction and the stabilization were identical.
At this stage, the whole product was passed through a 1.6 mm sieve.
The pressing was performed with 0.4% of Zn stearate with a pressure of 5 t/cm 2 .
The sintering was followed by a 6 h plateau period at 1640° C.
The green density obtained was 44.9% of the theoretical density.
The sintered density obtained was 93.9% of the theoretical density.
The omission of the breaking up of clumps had only a slight effect.
Example 3
In this example, the starting solutions were the same as in Example 1. The calcining was omitted.
The concentration was stopped at 120° C.
The crystallization by flaking was performed at 40° C.
The denitration was performed under vacuum according to the working conditions of Example 1, and stopped at 420° C.
This product was subjected directly to reduction under an atmosphere of a mixture of argon containing 5% of hydrogen, at a temperature of 700° C.
The stabilization was carried out at 40° C. as in Example 1. At this stage, the product was passed through a 1 mm sieve.
The pelletizing was carried out under a pressure of 5.8 t/cm 2 .
The sintering was continued until a 6 h plateau period was obtained at 1600° C. under an Ar, 5% H 2 atmosphere.
The green density obtained was 50.5% of the theoretical density.
The sintered density obtained was 96.3% of the theoretical density.
The dissolution yield in hot (100°) nitric acid for 6 h was still very high: 99.94%.
Example 4
In this example, the starting solution was obtained according to a process identical to that of Example 1, but with a Pu/(U+Pu) ratio equal to 0.25 and the omission of the breaking up of clumps.
The concentration was stopped at 140° C.
The crystallization by flaking was performed at 80° C.
The denitration was performed as in Example 3, stopping at 420° C. to obtain a solid intermediate product which was directly subjected to reduction in an Ar, 5% H 2 atmosphere at 700° C.
The stabilization was carried out as in Example 1 at 40° C.
At this stage, the product was passed through a 1.5 mm sieve.
The pelletizing was identical to that of Example 3 (5.8 t/cm 2 ).
The sintering was also identical to that of Example 3.
The green density was obtained was 50.8% of the theoretical density.
The sintered density obtained was 93.6% of the theoretical density.
The dissolution yield in hot (100° C.) 14N nitric acid for 6 h was still very high: 99.93%.
Example 5
In this example, a process identical to that of Test 1 was used, but starting with a solution containing only uranium.
The starting solution was obtained by distilling 840 cm 3 of 1.25N nitric acid solution (quantity of acid which corresponds to the Pu solution of Example 1) to bring it to a volume of 330 cm 3 . 610.5 g of uranile nitrate hexahydrate were then added to it.
The concentration was stopped at 128° C.
The crystallization by flaking was performed at 105° C., obtaining 665 g of product.
The latter was then subject to dehydration/denitration according to the same protocol as in Example 1, in particular:
no melting of the product
reduced pressure of 0.13 kPa (1 mm of mercury)
rate of temperature rise: 250° C./h
maximum temperature reached: 400° C.
The specific surface area obtained is 32 m 2 /g.
The calcining, reduction and stabilization were performed under the same conditions as in Example 1.
The pelletizing was also performed under the same conditions, the pressures used being 3.5 t/cm 2 and 4.5 t/cm 2 .
The sintering was also carried out under the same conditions with, in particular, 6 h plateau periods at 1640° C. and 1740° C.
The results obtained are as follows:
______________________________________ DensityPelletizing (as % of the theoretical density)pressure Plateau at Plateau atTest t/cm.sup.2 Green Sintered 1640° C. 1740° C.______________________________________4 3.5 49.4 93.9 95.2 95.85 4.5 52.1 95.3 95.2 95.8______________________________________
The densities comply with the specifications and are of the same order of magnitude as in the case of the U/Pu mixtures.
Example 6
This example may serve as a reference example, since it consisted in producing a fuel containing uranium alone according to a customary process of the prior art.
The starting substance was UF 6 , which was first hydrolysed; the product obtained was then reduced with hydrogen to give a UO 2 powder which was then stabilized and then treated according to the process of Example 1 (or 5).
The pelletizing was performed at 2.5 t/cm 2 , 3.5 t/cm 2 and 5.0 t/cm 2 .
The sintering was performed under an Ar, 5% H 2 atmosphere with a 6 h plataeu period at 1640° C.
The results obtained are as follows:
______________________________________Pelletizingpressure Density (as % of the theoretical density)Test t/cm.sup.2 Green Plateau at 1640° C.______________________________________6 2.5 42.2 94.77 3.5 48.5 95.38 5 54.4 95.7______________________________________
The results of Examples 5 and 6 relating to uranium alone, one of them treated according to the process of the invention and the other according to an accepted process of the prior art, are in complete agreement.
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A process is disclosed for producing sintered mixed metal oxide nuclear f pellets containing UO 2 and the oxide of at least one other fissionable or rare earth element M, the pellets being directly soluble in nitric acid without nitric acid additive or prior treatment of the pellets. The process comprises the steps of mixing together nitrate solutions of the elements, concentrating the mixture of solutions, thermally denitrating the concentrated nitrate mixture without additives, to obtain an intermediate mixed oxide powder, calcining the intermediate mixed oxide powder, reducing the calcined mixture, stabilizing the uranium oxide UO 2 in the reduced oxide mixture, shaping and pressing the resulting stabilized, reduced oxide mixture to obtain pellets of green material, sintering the pellets of green material and grinding the sintered pellets. The intermediate steps of this process produce mixed oxide powders of high flowability and good sinterability without the necessity of crushing which tends to produce troublesome effluent or dangerous aerosols of solids.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Pat. App. No. 61/58,5038 filed Jan. 10, 2012, the entirety of which is hereby incorporated by reference.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] This invention was not federally sponsored.
BACKGROUND OF THE INVENTION
Field of the invention
[0003] This invention relates to the general field of washing machines, and more specifically toward a system for dispensing substances into a washing machine. A plurality of preferably different sized or shaped cartridges are located within removable drawers. Each cartridge contains a particular substance, such as laundry detergent, bleach, or fabric softener, that is released into the washing machine. The system also includes a means to identify the substance contained within the cartridge as well as when and how much of the substance should be released into the washing machine. At the appropriate time, the system dispenses an appropriate amount of substance into the washing machine. A pump pulls the substance out of the container and into the washing basin of a washing machine. Alternatively, a valve is opened and the substance pours into the washing basin due to gravitational forces.
[0004] Washing machines enable users to wash their clothes in a shorter period of time and with greater ease than otherwise possible when doing it by hand. Whether it is a top loading or side loading washing machine, the clothes are soaked in water and agitated to get the clothes clean. Often, one or more substances such as laundry detergent, fabric softener, or bleach are added to the water to aid the cleaning process. However, how much of each substance and when it is added depends upon various factors, including the type of substance and the wash cycle set on the washing machine. Many users will place laundry detergent directly into the washing machine as it fills with water, then place fabric softener into a special container that releases the fabric softener at the appropriate time, and may also place bleach into yet another container that releases the bleach at its appropriate time.
[0005] Handling laundry detergent, fabric softener, bleach, or other common substances used to clean clothes can be unpleasant and even harmful. For example, bleach, which may include chlorine, is a respiratory irritant that attacks mucous membranes and can burn the skin. When adding these substances to the washing machine, either into the washing basin or into a separate receptacle, the amount of each substance must be measured. Pouring from a container into a measuring device, and then into the appropriate location in the washing machine often results in inadvertent spills as well as requiring that the measuring device be cleaned.
[0006] Thus there has existed a long-felt need for a system that dispenses an appropriate amount of a particular substance at the appropriate time into a washing machine without requiring a user to potentially come into contact with that substance. Furthermore, there is a need for a system that automatically dispenses a plurality of substances into a washing machine at the appropriate time during a wash cycle.
SUMMARY OF THE INVENTION
[0007] The current invention provides just such a solution by having a system for dispensing substances into a washing machine. A plurality of preferably different sized or shaped cartridges are located within removable drawers. Each cartridge contains a particular substance, such as laundry detergent, bleach, or fabric softener, that is released into the washing machine. The system also includes a means to identify the substance contained within the cartridge as well as when and how much of the substance should be released into the washing machine. At the appropriate time, the system dispenses an appropriate amount of substance into the washing machine. A pump pulls the substance out of the container and into the washing basin of a washing machine. Alternatively, a valve is opened and the substance pours into the washing basin due to gravitational forces.
[0008] It is a principal object of the invention to provide a system that enables users to safely, cleanly, and efficiently add substances to a washing machine.
[0009] It is another object of the invention to provide a system for dispensing one or more substances into a washing machine at the appropriate time.
[0010] It is a further object of this invention to provide a system for dispensing the correct amount of a particular substance into a washing machine.
[0011] It is an additional object of the invention to provide a system for reducing human error in dispensing substances into a washing machine.
[0012] It is yet another object of the invention to provide a dispensing system that is self-contained so as to eliminate pouring a substance form a separate container into a washing machine.
[0013] It is a further object of the invention to provide a system that regulates the amount of a substance dispensed into a washing machine to increase efficiencies and eliminate waste.
[0014] In a particular embodiment, the current invention is a system for dispensing a substance into a washing machine comprising a plurality of cartridges, a plurality of level indicators, a plurality of barcode readers, a plurality of dispensing tubes, and a cover, where each cartridge comprises handle, a barcode, a vent, and a delivery tube adapter, where each of the plurality of dispensing tubes mates with a delivery tube of a cartridge, where a substance contained within each cartridge may flow through the delivery tube, where fluid that flows through the delivery tube is inserted into a washing machine, where each level indicator mates with the vent of a cartridge and determines the amount of substance contained within the cartridge, where each barcode reader reads data from a barcode of a cartridge and destroys the barcode of the cartridge, whereby the system for dispensing a substance dispenses a substance from each cartridge at a time and volume determined by the data read from the barcode of each cartridge.
[0015] In another embodiment, the current invention is a method of dispensing a substance into a washing machine comprising the steps of: accepting a cartridge, where the cartridge comprises a vent and a barcode; scanning the barcode of the cartridge; destroying the barcode of the cartridge such that it cannot be read again; inserting a level indicator through the vent and into the cartridge; and dispensing a substance contained within the cartridge into a washing machine; whereby data collected from scanning the barcode is used to determine the volume and timing of dispensing the substance contained within the cartridge into the washing machine.
[0016] In an additional embodiment, the current invention is a system for dispensing a substance comprising: a barcode reader, a level indicator, and a cartridge, where the cartridge comprises a vent and a barcode, where the barcode reader reads the barcode of the cartridge, where the barcode reader destroys the barcode of the cartridge after the barcode reader has read the barcode, where the level indicator is inserted through the vent and determines the level of a substance remaining within the cartridge.
[0017] There has thus been outlined, rather broadly, the more important features of the invention in order that the detailed description thereof may be better understood, and in order that the present contribution to the art may be better appreciated. There are additional features of the invention that will be described hereinafter and which will form the subject matter of the claims appended hereto. The features listed herein and other features, aspects and advantages of the present invention will become better understood with reference to the following description and appended claims.
BRIEF DESCRIPTION OF THE FIGURES
[0018] The accompanying drawings, which are incorporated in and form a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the principles of this invention.
[0019] FIG. 1 is perspective view of a washing machine with a dispensing system according to selected embodiments of the current disclosure.
[0020] FIG. 2 is a partial view of the dispensing system and its integration into a drawer of a washing machine according to selected embodiments of the current disclosure.
[0021] FIG. 3 is a perspective view of cartridges according to selected embodiments of the current disclosure.
[0022] FIG. 4 is a perspective view of a washing machine with a dispensing system and integrated stain remover sprayer according to selected embodiments of the current disclosure.
[0023] FIG. 5 is a perspective view of a cartridge according to selected embodiments of the current disclosure.
DETAILED DESCRIPTION OF THE INVENTION
[0024] Many aspects of the invention can be better understood with the references made to the drawings below. The components in the drawings are not necessarily drawn to scale. Instead, emphasis is placed upon clearly illustrating the components of the present invention. Moreover, like reference numerals designate corresponding parts through the several views in the drawings.
[0025] FIG. 1 is perspective view of a washing machine with a dispensing system according to selected embodiments of the current disclosure. The dispensing system 10 according to the current invention resides on the top of a washing machine 90 . The dispensing system 10 has a cover 11 that is connected to the back of the dispensing system 10 by a hinge. The dispensing system 10 accepts cartridges, such as a detergent cartridge 20 , fabric softener cartridge 21 , and a bleach cartridge 22 . A level indicator 31 is used to determine the amount of fluid left within each cartridge. Barcode scanners 33 scan the barcode of each cartridge and then puncture (thereby destroying) each barcode after it is scanned. Described in more detail below, the barcode enables the dispensing system to determine what substance is in the cartridge as well as how much of and when to dispense the substance contained therein.
[0026] FIG. 2 is a partial view of the dispensing system and its integration into a drawer of a washing machine according to selected embodiments of the current disclosure. After a cartridge is inserted into the dispensing system, barcode readers 33 scan the barcode of each cartridge. After scanning the barcode, the barcode readers 33 move downward toward the cartridge and pierce each barcode thereby destroying it. By destroying the barcode, the dispensing system prevents repeated use (such as refilling) of the cartridges since the barcode reader 33 will not read a destroyed barcode. Level indicators 31 are also lowered though a vent in each cartridge. In a particular embodiment, each cartridge has a cap that covers the vent, which is removed before it is inserted into the dispensing system. At the appropriate time, fluid from each cartridge is dispensed through delivery tubes 35 to dispensing tubes 37 , which deposit the fluid in an appropriate area of a cleaning substance drawer 91 of a washing machine. The cleaning substance drawer 91 may include a detergent area 91 , a fabric softener area 93 , and a bleach area 94 . The dispensing tubes 37 deposit the appropriate fluid into the appropriate area.
[0027] FIG. 3 is a perspective view of cartridges according to selected embodiments of the current disclosure. Three cartridges are shown: a detergent cartridge 20 , fabric softener cartridge 21 , and a bleach cartridge 22 . The detergent cartridge 20 contains laundry detergent and is the largest of the three cartridges shown. The fabric softener cartridge 21 contains fabric softener and is the second largest cartridge shown. The bleach cartridge 22 is the smallest cartridge shown and contains bleach. Each cartridge includes a vent 27 that is covered with a cap (not shown) when stored or otherwise not in use and not inserted within the dispensing system. A barcode 25 is also placed on each cartridge, which is used to identify the particular substance contained within the cartridge and the particular use instructions associated therewith.
[0028] FIG. 4 is a perspective view of a washing machine with a dispensing system and integrated stain remover sprayer according to selected embodiments of the current disclosure. The dispensing system 10 , in addition to a detergent cartridge, fabric softener cartridge, and bleach cartridge, may include a stain remover cartridge 23 . A tube extends therefrom and thrown an opening in the dispensing system and is connected to a sprayer 39 . The sprayer 39 includes a trigger, which can be pulled to dispense a stain remover substance contained within the stain remover cartridge 23 . Thus, a user may quickly and efficiently treat a stained item of clothing by using the sprayer 39 integrated with the dispensing system 10 .
[0029] FIG. 5 is a perspective view of a cartridge according to selected embodiments of the current disclosure. The detergent cartridge 20 includes a handle 26 that is used to grasp the detergent cartridge. A vent 27 is an opening that is used to allow air to enter the detergent cartridge 20 as the substance contained therein is withdrawn. A level indicator (not shown in this figure) may also extend through the vent opening 27 to measure the amount of substance remaining in the detergent cartridge 20 . A barcode 25 identifies that particular substance within the detergent cartridge 20 . The substance within the detergent cartridge 20 is withdrawn through a delivery tube 35 . The delivery tube mates with the detergent cartridge 20 via a dispensing tube adapter 36 . As the detergent cartridge 20 is inserted into the dispensing system, the delivery tube 35 mates the delivery tube adapter 36 , which is integrated into the detergent cartridge.
[0030] The level indicators are inserted through the vent and are used to determine the amount of substance remaining in the particular cartridge. A float moves up and down depending on the level of the substance (fluid) in the cartridge. In other words, as the substance is removed from the cartridge, the float travels downward. Sensors determine the location of the float, and through this the relative amount of substance left in the cartridge.
[0031] In a particular embodiment, the dispensing system includes fluid pumps. The fluid pumps are in fluid connection with the cartridges via delivery tubes. Each fluid pump 50 is in electrical connection to a circuit board, such as a motherboard of the dispensing system or washing machine. Solenoid valves may also be utilitized to block and unblock the flow of the fluid from the cartridge and to the washing machine cleaning substance drawer. In this manner, the fluid pump and/or solenoid valves are turned on and off as directed by the internal circuitry of the system and/or washing machine.
[0032] In another embodiment, the barcode includes data such as the type of substance within the cartridge, volume of the cartridge, manufacturing date, serial number, or codes or encrypted data that verifies the source and authenticity of the laundry detergent cartridge. By checking the data on the barcode of the cartridge, the system ensures that only compatible cartridges manufactured for the system will dispense the substance contained therein. Furthermore, the appropriate volume and timing of the substance to be dispensed is automatically read in by the system and implemented accordingly, thereby reducing user error.
[0033] In an alternative embodiment, the barcode includes only encrypted identifying data that is used to query a remote network connected server. By way of example, the barcode reader reads in the data from the barcode. It then uses this data to make a request to a remote server over the internet. The request is made as an http request made over a wifi-network that is connected to the internet. The data from the barcode, either encrypted or decrypted, is transmitted to the remote server, which then responds with various data related to the cartridge. The response data may include confirmation as to whether or not the cartridge is authentic, whether or not the cartridge has been used previously, the substance located within the cartridge, the amount of substance that should be dispensed per load of laundry, at what point in the cycle the substance should be dispensed, and how much substance is located within the cartridge.
[0034] The laundry detergent cartridge includes a vent, handle, and a barcode. The length of the laundry detergent cartridge of a particular embodiment is 14.5 inches, where the handle is 2.5 inches and the remaining portion is 12 inches, and the width of the laundry detergent cartridge is 5.875 inches.
[0035] In an alternative embodiment, the laundry detergent cartridge has a generally trapezoidal shape, where the width of the top part is 5.875 inches and the width of the bottom part is 5.0625 inches. The height of the laundry detergent cartridge is 5.5 inches. The trapezoidal shape helps ensure that the laundry detergent cartridge has the proper orientation when it is placed into the dispensing system. Notches in the laundry detergent cartridge may be used to align the laundry detergent cartridge in the appropriate position and location in the dispensing system.
[0036] A vent cap allows for air to vent into a cartridge as the substance contained within is removed from the cartridge. The vent cap may be a screw-type cap, wherein the vent cap is placed over a vent and screwed into position. When screwed shut, the vent cap closes the vent. When vent cap is unscrewed, the vent is opened and air is allowed to pass therethrough. Without venting the cartridge, fluid would not easily flow out of the cartridge and through the delivery tube.
[0037] The fabric softener cartridge is smaller than the laundry detergent cartridge. Often, more laundry detergent is used than fabric softener per load of laundry. Therefore, the fabric softener cartridge needs to hold less fabric softener than the laundry detergent cartridge needs to hold laundry detergent. In this particular embodiment, the main part of the fabric softener cartridge is 7.125 inches long and 3.5 inches wide. The fabric softener cartridge also includes a handle for grasping and maneuvering the fabric softener cartridge and a vent cap for allowing air to vent into the fabric softener cartridge as fabric softener is removed from the fabric softener cartridge.
[0038] In an alternative embodiment, the fabric softener cartridge has a generally trapezoidal shape, where the width of the top part is 3.5 inches. The height of the fabric softener cartridge is 5.25 inches. The trapezoidal shape helps ensure that the fabric softener cartridge has the proper orientation when it is placed into the dispensing system. Notches in the fabric softener cartridge align the fabric softener cartridge in the appropriate position and location in the dispensing system.
[0039] In a particular embodiment, the laundry detergent cartridge holds 170 oz. of laundry detergent and the bleach cartridge holds 5 oz. of bleach.
[0040] In practice, a user opens the lid to the dispensing system, removes the vent cap that covers the vent of a cartridge, and then inserts the cartridge into the dispensing system. The user then closes the lid and the dispensing system reads in the barcode located on the cartridge, verifies its authenticity, and then punctures the barcode making it unreadable in the future. If necessary and enabled, the dispensing system queries a remote server for additional information on the cartridge, such as type of substance, size of the container, and dispensing instructions. At the same time or subsequent to reading the barcode, level indicators are inserted through the vent to read in the level of substance remaining within the cartridge.
[0041] The user will then place dirty laundry into the washing machine, and start a washing cycle. The dispensing system dispenses an appropriate amount of the substance contained within the cartridge into the washing machine at the appropriate time. For example, a first substance may be deposited into the cleaning substance drawer of the washing machine when the cleaning cycle begins, while a second substance is deposited fifteen minutes after the cycle beings, and then a third substance is deposited 5 minutes before the cleaning cycle ends.
[0042] Multiple loads of laundry may be run for each cartridge. When the level indicators determine that there is little substance left within a particular cartridge, such as substance for five or fewer loads, a user is notified. Notifications include without limitation a blinking light, illuminated light, a beep, a buzz, a text message, an email, or red/yellow/green lights and/or bars.
[0043] After a cartridge is empty, the user opens the lid of the dispensing system. As the lid is opened, the level indicators are removed from each cartridge and the user may grasp the handle of the empty cartridge and remove it from the dispensing system. If each cartridge is designed to deliver substance for the same number of loads of laundry, and not necessarily the same amount of substance, then all of the cartridges should need to be replaced at roughly the same time.
[0044] The system described herein has been shown with three different sized cartridges. One skilled in the art will appreciate that fewer or more than three d cartridges of the same or different substances may be implemented. For example, a four-cartridge system may be used where four different substances are desired to automatically dispense into the washing machine. Furthermore, multiple cartridges of the same type and/or size and shape (such as multiple laundry detergent cartridges) may be implemented into the system. Additionally, gravity or pressure pumps may be used to move the fluid substance contained within the cartridge.
[0045] It should be understood that while the preferred embodiments of the invention are described in some detail herein, the present disclosure is made by way of example only and that variations and changes thereto are possible without departing from the subject matter coming within the scope of the following claims, and a reasonable equivalency thereof, which claims I regard as my invention.
[0046] All of the material in this patent document is subject to copyright protection under the copyright laws of the United States and other countries. The copyright owner has no objection to the facsimile reproduction by anyone of the patent document or the patent disclosure, as it appears in official governmental records but, otherwise, all other copyright rights whatsoever are reserved.
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A system for dispensing substances into a washing machine is disclosed. A plurality of preferably different sized or shaped cartridges are located within removable drawers. Each cartridge contains a particular substance, such as laundry detergent, bleach, or fabric softener, that is released into the washing machine. The system also includes a means to identify the substance contained within the cartridge as well as when and how much of the substance should be released into the washing machine. At the appropriate time, the system dispenses an appropriate amount of substance into the washing machine. A pump pulls the substance out of the container and into the washing basin of a washing machine. Alternatively, a valve is opened and the substance pours into the washing basin due to gravitational forces.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority to U.S. patent application Ser. No. 14/252,727, filed Apr. 14, 2014, which is a Continuation Application of U.S. application Ser. No. 13/651,349, filed Oct. 12, 2012, now U.S. Pat. No. 8,700,145, issued Apr. 15, 2014, which claims priority to the benefit of U.S. Provisional Patent Application No. 61/699,470, filed Sep. 11, 2012, U.S. Provisional Patent Application No. 61/614,369, filed Mar. 22, 2012, U.S. Provisional Patent Application No. 61/598,185, filed Feb. 13, 2012, U.S. Provisional Patent Application No. 61/558,287, filed Nov. 10, 2011, and U.S. Provisional Patent Application No. 61/627,532, filed Oct. 13, 2011. This application is also a Continuation-In-Part of U.S. patent application Ser. No. 13/095,570, filed Apr. 27, 2011, which claims the benefit of U.S. Provisional Patent Application No. 61/328,621, filed Apr. 27, 2010 and which is a Continuation-In-Part of U.S. patent application Ser. No. 12/485,040, filed Jun. 15, 2009, which claims the benefit of: U.S. Provisional Patent Application No. 61/077,648, filed Jul. 2, 2008; U.S. Provisional Patent Application No. 61/078,954, filed Jul. 8, 2008; U.S. Provisional Patent Application No. 61/086,116, filed Aug. 4, 2008; and U.S. Provisional Patent Application No. 61/149,387, filed Feb. 3, 2009. All of these applications are incorporated herein by reference as if reproduced in their entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable.
REFERENCE TO A MICROFICHE APPENDIX
Not applicable.
BACKGROUND
Stroke is a leading cause of adult disability in the United States, with upper motor deficits being the primary result of the disability. These motor disabilities greatly affect quality of life for the patient and their loved ones. In addition, the loss of motor function exacts a financial toll on the healthcare system of nearly $70 billion yearly. Patients with hemiplegia or hemiparesis generally regain walking without the use of an assistive device while only half to one-third of patients regain some degree of use of their upper extremity, even after intensive rehabilitation therapy. The severe functional impairment affects occupational performance, and as a result, few stroke victims are able to return to work. Upper limb motor disabilities from stroke have an unfavorable effect on the activities of daily living critically affecting the quality of life for the stroke victim as well as family members and caregivers.
Physical rehabilitation can result in significant improvements in motor outcomes after stroke. Improvements in recovery of upper extremity function have also been reported for electromyographic feedback, motor imagery, robotics, and repetitive task practice, though large scale clinical trials have yet to be implemented. Unfortunately for most patients, the gains are not enough to have a large impact on daily living. Further, current rehabilitative therapies, such as constraint-induced movement therapy, are restricted to individuals with mild to moderate deficits. Few options are available for those stroke survivors with moderate to severe deficits. Therefore, there is still a tremendous need for methods that improve recovery of function even further.
To enhance recovery further, adjuvant therapies have been tried. For example, amphetamines can be effective at enhancing recovery of motor abilities beyond that seen with physical rehabilitation alone; however, even the positive results for motor outcomes are only incremental, and amphetamine use has many well-known side effects. Several small, randomized controlled trials have shown that epidural stimulation significantly improves motor recovery in animal models and in human stroke survivors. Unfortunately, the method requires brain surgery associated with the potential for significant complications and is not likely to reach widespread clinical use in stroke patients. Also, a recent randomized clinical trial failed to demonstrate improved efficacy compared with intensive physical rehabilitation.
Less invasive methods for cortical stimulation have also been combined with physical rehabilitation. Again, however, while real gains in function are observed, the gains are modest, for the most part. Thus, a great need still exists for a method to improve motor function further.
Current rehabilitation techniques do not sufficiently restore lost function in many individuals. Statistically significant improvements to motor deficits can be induced even several months after stroke. However, these improvements do not consistently improve quality of life for the vast majority of patients and their caretakers, thus greater improvements in motor skills are needed following rehabilitation.
Motor therapies typically involve practicing either fine motor or gross motor skills. Repetition is generally the mechanism of the therapies. In some variations, such as constraint therapy and mirror therapy, other mechanisms are engaged.
Some examples of typical motor therapies may be actions such as: squeezing a dynamometer, turning on/off a light switch, using a lock and key, opening and closing a door by twisting or depressing different doorknobs, flipping cards, coins and other objects over, placing light and heavy objects at different heights, moving pegs to hole and remove pegs from hole, lifting a shopping basket/briefcase, drawing geometric shapes, dressing, typing, reaching and grasping light and heavy objects, grasping and lifting different (size, shape, and texture) objects, doing a precision grasp, writing, drawing connect the dots, opening and closing a jar or medication bottle, lifting an empty and full cup/glass, using feeding utensils, cutting food, stirring liquids, scooping, pouring a glass of water with the paretic hand; or using the paretic hand to stabilize the glass and pouring with the good hand, picking an object and bring to target, using a spray can, cutting with scissors, or brushing teeth/hair.
U.S. Pat. No. 6,990,377 (Gliner, et al.) describes a therapy to treat visual impairments. The therapy includes presenting various types of visual stimuli in conjunction with stimulation of the visual cortex. The therapy described in Gliner does not control the timing relationship of the stimuli and the stimulation.
U.S. Patent Application Publication 2007/1079534 (Firlik, et al.) describes a therapy having patient interactive cortical stimulation and/or drug therapy. The therapy has patients performing tasks, detecting patient characteristics and modifying the stimulation depending on the detected patient characteristics. The therapy described in Firlik does not control the timing relationship between the tasks and the cortical stimulation.
It is common in the prior art to suggest that stimulation of the cortex, the deep brain, the cranial nerves and the peripheral nerves are somehow equivalent or interchangeable to produce therapeutic effects. Despite these blanket statements, stimulation at different parts of the nervous system is not equivalent. It is generally understood that the vagus nerve is a nerve that performs unique functions through the release of a wide array of neuromodulators throughout the brain. To generate certain kinds of plasticity, the timing of the stimulation of the vagus nerve is critical in producing specific therapeutic effects.
U.S. Pat. No. 6,104,956 (Naritoku, et al.) is representative of work done using vagus nerve stimulation (VNS) to treat a variety of disorders, including epilepsy, traumatic brain injury, and memory impairment. The VNS is delivered without reference to any other therapy. To improve memory consolidation, VNS is delivered several minutes after a learning experience. Memory consolidation is unrelated to the present therapy for treating motor deficits.
SUMMARY
For purposes of summarizing the disclosure, certain aspects, advantages, and novel features of the disclosure have been described herein. It is to be understood that not necessarily all such advantages may be achieved in accordance with any particular embodiment of the disclosure. Thus, the disclosure may be embodied or carried out in a manner that achieves or optimizes one advantage or group of advantages as taught herein without necessarily achieving other advantages as may be taught or suggested herein.
In an embodiment, the disclosure includes a method of treating motor deficits in a stroke patient, comprising assessing a patient's motor deficits, determining therapeutic goals for the patient, based on the patient's motor deficits, selecting therapeutic tasks based on the therapeutic goals, performing each of the selected therapeutic tasks repetitively, stimulating the vagus nerve of the patient during the performance of the selected therapeutic tasks, and improving the patient's motor deficits.
In a second embodiment, the disclosure includes a method of treating motor deficits in a stroke patient, comprising assessing a patient's motor deficits, determining therapeutic goals for the patient, based on the patient's motor deficits, selecting therapeutic tasks based on the therapeutic goals, performing each of the selected therapeutic tasks repetitively, observing the performance of the therapeutic tasks, initiating the stimulation of the vagus nerve manually at approximately a predetermined moment during the performance of the therapeutic tasks, stimulating the vagus nerve of the patient during the performance of the selected therapeutic tasks, and improving the patient's motor deficits.
In a third embodiment, the disclosure includes a method of treating motor deficits in a stroke patient, comprising assessing a patient's motor deficits, determining therapeutic goals for the patient, based on the patient's motor deficits, selecting therapeutic tasks based on the therapeutic goals, performing each of the selected therapeutic tasks repetitively, detecting the performance of the therapeutic task, automatically initiating vagus nerve stimulation at a predetermined moment during the detected performance of the therapeutic task, stimulating the vagus nerve of the patient during the performance of the selected therapeutic tasks, and improving the patient's motor deficits.
In a fourth embodiment, the disclosure includes a system for providing therapy for a motor deficit, comprising, an implantable stimulation system including an implantable pulse generator (IPG), lead and electrodes to stimulate a patient's vagus nerve, a clinical controller with stroke therapy software, an external communication device to communicate between the clinical controller and the implantable stimulation system, and a manual input device, coupled to the clinical controller, wherein the manual input device is engaged during performance of a therapeutic task causing the clinical controller to send a signal using the external communication device to the implantable stimulation system, so that a patient's vagus nerve is stimulated during the performance of the therapeutic task.
In a fifth embodiment, the disclosure includes a system for providing automated therapy for a motor deficit, comprising, an implantable stimulation system including an IPG, lead and electrodes to stimulate a patient's vagus nerve, a clinical controller with stroke therapy software, an external communication device to communicate between the clinical controller and the implantable stimulation system, and a motion detection system, coupled to the clinical controller, wherein the motion detection system detects performance of a therapeutic task and at a predetermined time during the therapeutic task causing the clinical controller to send a signal using the external communication device to the implantable stimulation system, so that a patient's vagus nerve is stimulated during the performance of the therapeutic task.
These and other features may be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of this disclosure, reference is now made to the following brief description, taken in connection with the accompanying drawings and detailed description, wherein like reference numerals represent like parts.
FIG. 1 is a flowchart depicting a task selection and therapy parameter selection process for a paired-VNS motor therapy, in accordance with an embodiment;
FIG. 2 is a flowchart depicting a setup and administration process for a paired-VNS motor therapy, in accordance with an embodiment;
FIG. 3 is a flowchart depicting another setup and administration process for an automated paired-VNS motor therapy protocol, in accordance with an embodiment;
FIG. 4 is a graph depicting the timing of a therapeutic motion and examples of possible stimulation timing variations for paired VNS;
FIG. 5 depicts an implantable vagus nerve stimulation system, in situ, in accordance with an embodiment;
FIG. 6 is a functional block diagram depicting a paired-VNS motor therapy system including a manual VNS switch, in accordance with an embodiment;
FIG. 7 is a functional block diagram depicting an automated paired-VNS motor therapy system, in accordance with an embodiment;
FIG. 8 is a screenshot of an initial interface screen, in accordance with an embodiment;
FIG. 9 is a screenshot of a therapy information screen, in accordance with an embodiment;
FIG. 10 is a screenshot of a stimulation parameter input screen, in accordance with an embodiment;
FIG. 11 is a screenshot of a therapy input screen, in accordance with an embodiment;
FIG. 12 is a screenshot of an IPG parameter input screen, in accordance with an embodiment;
FIG. 13 is a screenshot of a therapy delivery screen, in accordance with an embodiment;
FIG. 14 is a schematic diagram of an automated pairing system, in accordance with an embodiment; and
FIG. 15 is a screenshot of an automated therapy screen, in accordance with an embodiment.
DETAILED DESCRIPTION
It should be understood at the outset that although an illustrative implementation of one or more embodiments are provided below, the disclosed systems and/or methods may be implemented using any number of techniques, whether currently known or in existence. The disclosure should in no way be limited to the illustrative implementations, drawings, and techniques illustrated below, including the exemplary designs and implementations illustrated and described herein, but may be modified within the scope of the appended claims along with their full scope of equivalents. The present application describes several embodiments, and none of the statements below should be taken as limiting the claims generally.
Where block diagrams have been used to illustrate the embodiments, it should be recognized that the physical location where described functions are performed are not necessarily represented by the blocks. Part of a function may be performed in one location while another part of the same function is performed at a distinct location. Multiple functions may be performed at the same location. In a functional block diagram, a single line may represent a connection, in general, or a communicable connection, particularly in the presence of a double line, which may represent a power connection. In either case, a connection may be tangible, as in a wire, or radiated, as in near-field communication. An arrow may typically represent the direction of communication or power although should not be taken as limiting the direction of connected flow.
Therapy
VNS is paired with a motor therapy by providing the stimulation at some time during the motor therapy, for example, the beginning of the motion. Because the cortical plasticity is generated by the stimulation for a short time period, as short as a few seconds, the VNS should be provided so that most of the VNS is during the motions that constitute the therapy.
With reference to FIG. 1 , a flowchart 100 depicts a task selection and therapy parameter selection process for a paired-VNS motor therapy 100 , in accordance with an embodiment. The process 100 begins with a patient evaluation at 102 . The patient evaluation may include a standard medical evaluation, medical history, and assessment of the patient's motor deficit. Persons of ordinary skill in the art are aware of other information that can be included in a patient evaluation. The patient's motor deficit or handicap may be assessed using standard motor deficit assessment criteria, such as Fugl-Meyer, Barthel Index, Box and Block Test, Canadian Occupation Performance Measure (COPM), Functional Independence Measure (FIM), Motor Assessment Scale (MAS), Action Research Arm Test (ARAT), Modified Rankin Scale, Nine hole peg test, NIH Stroke scale, Stroke Impact Scale (SIS) or any other appropriate assessment measures.
The process 100 may continue with setting the therapeutic goals at 104 . Therapeutic goals may include such things as tying shoes, unlocking doors, eating, or performing other basic life tasks. Persons of ordinary skill in the art are aware of other types of goals.
Taking into consideration the therapeutic goals, a set of tasks are selected at 106 that either address specific muscle groups necessary to achieve the therapeutic goals, mimic the basic life tasks, or mimic some portion of those tasks. For example, if the goal is to be able to unlock a door, then the task of inserting a key and turning the key in a lock may be selected as a task. On the other hand, if the patient is suffering from more serious disabilities in this regard, then the task of reaching and grasping an object may be selected, as a first step toward the task of unlocking a door.
Tasks may include: Reach and grasp; Lift objects from table; Circumduction and bimanual tasks (mainly involving wrist and distal joints); Stacking objects; Slide credit card in slot; Turning on and off light switch; Squeezing objects; Writing; Typing; Stirring liquid in a bowl (bimanual); Dial a cell phone (bimanual); Fold towels or clothes (bimanual); Wear a belt; Tying shoelaces; Eating; Brushing teeth; Combing hair.
Each of the tasks is defined with a spectrum of levels. The task of moving a weight, for example, may include smaller weights and larger weights. Given a patient's abilities and the therapeutic goals, the initial task level is selected at 108 . The patient may begin performing the task at the selected level. As the therapy proceeds, the level of the task may be changed to reflect changes in the patient's ability to perform the task. If a patient becomes adept at performing a task at the selected level, the level may be increased. If the patient struggles to perform the task at a given level, the level may be decreased.
Each task may be repeated many times. In a typical therapy, a task may be repeated from about 30 to about 50 times in a session. The number of repetitions for each task is selected at 110 . The stimulation parameters for the vagus nerve stimulation, such as the amplitude, pulse width, the duration of the pulse train, frequency, and train period are selected at 112 .
With reference to FIG. 2 , a setup and therapy delivery process 200 is shown. The physical items necessary for a selected task may be setup in the appropriate therapy space at 202 . The task and task parameters, such as what counts as success, are explained to the patient at 204 . The task delivery software is used to control the delivery of stimulations and to record data at 206 . When the patient is instructed that the therapy has begun, the patient performs the first selected task at 208 , in accordance with the instructions given. At approximately a determined point in the performance of the task, the manual input device is used to cause the vagus nerve of the patient to be stimulated at 210 . Typically, the vagus nerve is stimulated with a 500 millisecond pulse train at approximately 0.8 milliamperes. The 500 millisecond duration has been selected as sufficient to generate directed plasticity. Experiments have shown that a 500 millisecond stimulation generates directed plasticity that lasts less than 8 seconds. While longer pulse trains may be effective, the shorter duration is typically preferred because the shorter stimulation leads to less side effects. Following stimulation at 212 , there is a period of non-stimulation, which may be at least as long as the preceding period of stimulation. The period of non-stimulation may be a safety measure and may be part of the therapeutic process. When the task has been completed, the task level may be evaluated at 214 , to determine if the task level is too simple or too advanced for the patient. The task level may be changed at this point, as appropriate. The patient then performs the task again at 208 until the task has been repeated a predetermined number of times.
With reference to FIG. 3 , a setup and automated therapy process 300 is shown. The physical items necessary for a selected task may be setup in the appropriate therapy space at 302 . The setup may include initiating software to administer the automation. The task and the task parameters, such as what counts as success, are explained to the patient at 304 . The task delivery software is used to control the delivery of stimulations and to record data at 306 . When the patient is instructed that the therapy has begun, the patient performs the first selected task at 308 , in accordance with the instructions given. A clinical control device detects task performance at 310 . Cameras or other sensors may be used for to detect the patient's movements. At a determined point in the performance of the task, the control device causes the vagus nerve of the patient to be stimulated at 312 . Following stimulation, there is a period of non-stimulation at 314 , which may be at least as long as the preceding period of stimulation. The period of non-stimulation may be a safety measure and may be part of the therapeutic process. When the task has been completed, the task level may be evaluated at 316 , to determine if the task level is too simple or too advanced for the patient. The task level may be changed at this point, as appropriate. The patient then performs the task again at 308 until the task has been repeated a predetermined number of times.
With reference to FIG. 4 , a graph depicts the timing of the therapeutic task and examples of vagus nerve stimulation timing. Before a motion begins, the patient forms a mental intention and soon after, the motion begins. The task may typically include a series of motions. For example, a task may include, reaching, grasping, moving, releasing, and returning. Between each of these motions is a transition point or step that may be used to time the stimulation. Finally, the motion ends.
The vagus nerve stimulation may be effectively delivered at various times during the therapeutic task. For example, line a shows a vagus nerve stimulation given after the intention to move is formed and before the motion begins. Line b shows a vagus nerve stimulation delivered after the motion begins. Line c shows a vagus nerve stimulation delivered after a first transition point or step in the therapeutic task. Line d shows a vagus nerve stimulation delivered after a second transition point or step in the therapeutic task. Line e shows a longer vagus nerve stimulation delivered between the time the motion starts and shortly after the motion ends. The extended stimulation duration shown at line e may be a single long pulse train or a series of half-second pulse trains. Line f shows three vagus nerve stimulations delivered during the therapeutic task, after the motion begins, after the first step and after the second step. Any of these VNS delivery methods may be used singularly or in combination.
Other systems may be used to monitor movements, so that appropriate VNS timing can be determined. For a wrist flexion, we might use a camera to model the movement as a wire frame (e.g., bones with joints) and compare the movement to past attempts and to optimal (e.g., normal) movement in order to find the best movements that the patient can generate. Movements, such as walking, grasping or tying, may be quantified as location, direction, speed, and angle of each joint as a function of time. For speech production, vocalizations might be compared to previous sounds and normal speech sounds produced by others. Vocal movements might be quantified based on the intensity, duration, pitch, formant structure (vowels), formant transitions (consonants), voice-onset time, and other standard methods of quantifying speech sounds.
Selecting the appropriate paired VNS period depends on the nature of the motion and the equipment used to provide the pairing timing.
VNS could also be delivered during the planning stages before movement begins. This usually takes only a few hundred milliseconds but can be extended by giving a sensory cue that instructs the subject what motion needs to be done followed by a trigger cue some seconds later telling them when to begin the movement. This strategy makes it possible to specifically pair VNS with motor planning, which is an important part of motor control.
VNS may be paired with the best movements in order to shape future movements to be smooth and efficient (e.g., avoid spasticity, tremors, co-contraction of opposing muscles, or the use of muscles that would not normally be used to accomplish the task). VNS could also be delivered after the movement is completed and determined to be effective (e.g., the best movement of the attempts occurring in the last about 30 seconds).
Thus, VNS could be delivered before, during, or after movement. A measurement may show that the movement will be, is, or was effective (e.g., acceptable or better than average). Pairing may mean temporally associated with, not necessarily simultaneous. For the rat study discussed below, all VNS was delivered after the end of the target movement. However, in many cases, the rats continue with the movement after the target movement is achieved such that VNS is sometime delivered while the rat is moving.
VNS may be paired with supervised, massed practice movement therapy three times per week. The duration of the therapy may be six weeks. The duration of each therapy session may be approximately one hour. The therapist may determine each session's therapy tasks to progress toward the Canadian Occupational Performance Measure (COPM) goals established at the intake evaluation. Goals may focus on upper limb rehabilitation—most tasks may typically require four movement components: reaching, grasping, manipulating, and releasing an object. During each session the ‘primary therapy principles’ may be used to guide the development of the tasks to be performed each day. Prior to each therapy visit, the therapist team may meet and develop the task plan, ensure available materials and determine the plan to increase and decrease difficulty to and determine a realistic number of repetitions to be set as a goal.
The therapy implements several principles. The first principle is task specificity. Improvement of a motor skill requires practice of the movement; thus, each task may include components of reach, grasp, manipulate, and release specifically related to the target task.
Another therapy principle is that of repetition. Large numbers of repetitions of each task is required to master a motor skill, so the goal for therapy is to perform from about 30 to about 50 repetitions of a given task in a one-hour session (about 120-about 200 total repetitions per session). The focus of each therapy session may involve from about 3 to about 5 tasks in order to achieve the high numbers of repetitions.
Another therapy principle is active engagement. Optimal learning occurs with high levels of motivation and engagement. Thus, participants may help to set goals, therapists may make it clear how the target task relates to each goal, task practice may be varied to minimize boredom, and the task may be constantly adapted to require active engagement and effort to complete.
Another therapy principle is massed practice. Within a session, massed practice promotes better learning than distributed practice. Thus, the therapeutic environment needs to allow continuous repetition. For example, therapist may line up 10 objects in a row to allow for continued repetition. Rest breaks are given only if requested by the patient or required by the VNS.
Another therapy principle is variable practice. Variable practice can be important for learning transfer. The movement components may stay the same, and the context of the components may change between trials or sessions.
The therapy session should consist of from about 3 to about 5 tasks to allow variability and patient engagement. A reach & grasp task may be included in each session. The majority of patients need work in this area, so including it as a required task allows for consistency between patients and useful in judging rehabilitation with assessments.
The therapy session may, at least initially, take place under the supervision of one or more therapists. The patient may perform the action without assistance from the therapist. The therapist may manually deliver the VNS trigger during the “key” part of the movement that is being trained (typically when the subject touches or is about to touch the object during the reach). Alternatively, automatic delivery could be used. Tasks may be appropriately graded to require processing and effort by the patient but some degree of success. As a general guideline, if the patient is unable to complete the task successfully after approximately five attempts, it should be downgraded in difficulty. This guideline may be superseded by the therapist's clinical judgment regarding the patient's motivation, ability, and fatigue. If the patient is able to complete the task with little difficulty approximately (e.g., from about 10 to about 20 times) it should be upgraded in difficulty. If they can complete it, but it is slower than normal, then it is still a challenging task, and variety may need to be introduced to alleviate boredom.
The upgrading and downgrading of tasks is dependent on the patient's goals as well as the effort required. The level of strength and endurance required for the goal is also an important consideration. For some patients, even higher repetitions may be required to achieve the endurance needs. The goal for repetitions of each task may be set ahead of time by the therapist and communicated to the patient.
Grading of tasks can involve several different components: Physical position of the patient. The patient may be standing to introduce variety, add endurance, and add balance components to the task performance. Alternatively, the patient may be sitting.
The position of the task materials may be changed. The height of the task materials may be changed. The depth of the task materials, placing the materials further away from patient, may be changed. The degree from midline of objects (left, midline, or right) may be varied. The weight of task materials may be changed. The size of the objects may be changed.
Adaptive equipment/materials may be used. A DYCEM mat may be used to prevent an item from sliding. The therapist may hold item to stabilize it. Materials may be used to increase the grip of a small object to match ability (e.g., use foam to build up a pen to make it easier to grasp).
The speed of task movement may be changed. A certain number of repetitions per minute may be implemented to focus on the speed of movement. The patient may be encouraged to slow down task performance
The stability of the object may be changed. The object to grasp may be stable. The object to grasp may be moving (e.g., a ball is rolling on a table). The object may be placed on slippery surface or a sticky surface.
The same task can be practiced with different forms of material to achieve variety but still maintain high levels of repetition of the overall task. For example, to work on grasp and release of small objects, a plethora of everyday objects could be used, such as coins, paperclips, credit cards, cell phones, etc.
Task performance may be monitored by the therapist, and each VNS stimulation may be recorded by the software and presented to the therapist as a visual counter on the screen.
If in the therapist's assessment there are other rehabilitation issues that may require intervention, such as restricted range of motion, this can be addressed outside of the about one hour motor practice or addressed prior to the start of the VNS therapy. If there are significant non-motor impairments, such may disqualify the participant.
Patients may not be given a home exercise program of specific items to practice. However, they may be told to participate in their normal every day activities and be encouraged to “practice using your impaired upper extremity as much as possible”.
EXAMPLES OF GOAL AND TASK GRADING
Example 1
Grasp and Release. The patient's goal is to be able to unload dishwasher. The target task involves the ability to grasp, manipulate, and release a variety of objects along with a variety of strength and range of motion requirements and some degree of endurance (e.g., being able to stand for the entire duration).
Materials: spoon, fork, knife, large serving spoon, large and medium mixing bowl, coffee mug, drinking glass, small plate, large dinner plate, a DYCEM mat, foam.
Method: First, Patient sits at table with objects at midline Second, for each task repetition, the patient reaches out to grasp object and place on shelf about six feet above the table. Third, 10 objects are lined up to allow continuous repetition of the movement and achieve high numbers.
Grading: The task can be upgraded in difficulty by: challenging patient that a certain number of repetitions be completed in one minute; using a variety of sizes instead of the same size/shape in a row; requiring the patient stand to perform; requiring the patient bend down to retrieve the object; requiring the patient reach higher to place the object; requiring the patient sort and place each object in the correct position in a drawer; mixing bilateral lifting with single hand tasks; silverware is placed in a basket to be removed from; weight baring is required in one limb to stabilize during a task (e.g., the patient leans on his less affected arm and practices wiping the table with the impaired arm); and/or including bilateral tasks that aren't symmetrical (e.g., the patient uses a spray bottle with the impaired hand and cleans with the less affected arm).
The tasks can be downgraded in difficulty by: wrapping the object in foam to make it easier to grasp; placing objects on a DYCEM mat to minimize slipping; requiring object be moved from impaired hemifield to less impaired hemifield; and/or performing bilateral tasks.
Introducing variety and still achieving high numbers of repetitions. First, the goal for this task is 200+ repetitions. Since the goal is a complex task that involves several components this may be the only task performed is this session. Second, for the first part of the session, the task may be designed to primarily challenge the grasp. The individual may grasp objects in a variety of challenging ways with less challenge focused on the reach or manipulate aspect of the entire task, for 100 repetitions (e.g., 10 objects×10 repetitions) This may take about 25 minutes. There is a line of objects set up, thus there may be very little rest between repetitions. The second part may have greater emphasis on the reach part of the task, but the task is still repeating the components. The individual may now pick up a relatively easy object, that is further away from him, requiring a reach to different aspects of the field in front of him. Each of these trials may take longer. He may perform 35 trials of this from a variety of reach locations, which may require approximately 15 minutes. For variety, the object could be close and the he would be required to reach at the limits of his ability for the release of the object. Finally, the third part may focus on manipulation and precision. For these trials, the initial grasp and reach is not as difficult, but the manipulation/release may be repeated, e.g. about 75 times in about 20 minutes. This may require precise placement of an object (e.g., the participant has to stack a set of spoons on top of each other or place cups in a precise stack. The day's session was focused on the goal with all repetitions were focused specifically toward the same task, but different aspects of the goal were emphasized to eliminate boredom and fatigue.
Example 2
Handwriting. The patient's goal involves being able to write checks and thank you notes.
Materials: pen, paper, pencil, dry erase board, cylindrical foam, sand tray, shaving cream, and tray.
Method: First, the patient sits at a table with a tray with a mound of shaving cream. Second, the patient practices spreading the cream evenly throughout the tray. Third, the patient practices free writing with a finger or with a stylus. Fourth, the patient practices loop drawing or free writing with writing utensil of choice. Fifth, the patient practices filling out forms or line writing within constrained box.
Grading: The tasks can be upgraded in difficulty by: increasing the number of words written (e.g., phone number, address, sentences); decreasing task difficulty by using built up writing utensils to aid in grip; and/or decreasing task difficulty by using dry erase board, shaving cream, writing large letters or loops.
Example 3
Bilateral activity. The patient's goal involves folding laundry.
Materials: 10 wash cloths, 10 hand towels, 10 bath towels, 10 t-shirts, 10 pairs of socks.
Method: First, the patient may sit or stand at the table. Second, the patient may fold towels at midline. Third, all towels may be folded in half and then in half again using bilateral upper extremities. Fourth, folded towels may be placed in laundry basket.
Grading: Tasks may be decreased or increased in difficulty by changing the size and weight of objects. Tasks may be decreased or increased in difficulty by changing the number of folds required in the object. Task can be increased or decreased in difficulty by changing the location of where the object is to be grasped or placed. The therapist may unfold the towels to allow rapid repeat of task.
Example 4
Fine motor tasks. The patient's goal involves fishing.
Materials: 10 fishing lures, various sized bobbers, fishing weights, fishing line, a tackle box, and a fishing reel.
Method: First, The tackle box is placed at the patient's midline. Second, fishing weights bombers and lures are placed on the affected side. Third, the patient is instructed to pick up items and place them in the top box. Fourth, the patient is instructed to pick up items one at a time. Fifth, the patient practice is tying a fishing line. Sixth, the patient practices stabilizing the fishing rod with one hand and reeling with the other hand.
Grading: Increase or decrease task difficulty by increasing or decreasing the size of the items in the tackle box. Increase or decrease the difficulty by increasing or decreasing the weight of items at the end of the fishing line.
Example 5
A discrete, specific task. The patient's goal involves opening doors.
Materials: A set of experimental doors knobs with various types of locks, keys, and actual doors.
Method: First, the key is built up with foam or putty to allow easier grasp of the key. Second, the knobs/locks are placed at an easily accessible height to allow the patient to sit and perform the task. Third, actual doors are used and the patient has to fully open the door and walk through.
Grading: A variety of knob types are used requiring different aspects of grasp. The knobs/locks are placed at progressively more difficult positions. The actual doors are light or heavy.
Systems and Devices
With reference to FIG. 5 , an implantable vagus nerve stimulation system 500 is shown in situ. The implantable vagus nerve stimulation system 500 includes an IPG 506 , electrodes 502 , and a lead 504 connecting the IPG 506 to the electrodes 502 . The IPG 506 may be implanted in the chest of a patient 512 . The lead 504 travels below the skin to the neck of the patient 512 . The electrodes 502 may be of the cuff-electrode type and may be attached to the left vagus nerve 508 in the neck of the patient 512 . The IPG 506 sends electrical stimulation pulses through the lead 504 to the electrodes 502 , causing stimulation of the vagus nerve 508 . The IPG 506 , lead 504 , and electrodes 502 function similarly to the implantable vagus nerve stimulation systems commonly used in the treatment of epilepsy and as described in the parent patent application to this application.
Vagus nerve stimulation may be delivered with electrodes placed in direct contact (or proximate to) the left cervical vagus nerve, in the patient's neck. Other forms of stimulation may be used, including transcutaneous electrical or magnetic stimulation, physical stimulation, or any other form of stimulation. An example of a transcutaneous electrical stimulation system that could be adapted for use in the described therapy may be found in U.S. Pat. No. 7,797,042. Stimulation of the vagus nerve may be done at other sites along the vagus nerve and branches of the vagus nerve.
With reference to FIG. 6 , a stroke therapy system 600 is shown. The implanted stimulation system 500 communicates wirelessly with an external communication device 602 . The external communication device is coupled to a clinical controller 604 . The clinical controller 604 may be a computer, such as a laptop computer, running specialized paired VNS stroke therapy software. A manual input device 606 may be coupled to the clinical controller 604 . The manual input device 606 may be a hand switch, a foot switch, a mouse button, or a keyboard key. When the manual input device 606 is switched or pressed, the clinical controller 604 sends a signal to the external communication device 602 . The external communication device 602 sends a signal to the implanted stimulation system 500 . The implanted stimulation system 500 receives the signal at the IPG 506 and generates stimulation of the vagus nerve at the electrodes 502 .
With reference to FIG. 7 , a stroke therapy system 700 is shown. The implanted stimulation system 500 communicates wirelessly with an external communication device 602 . The external communication device is coupled to the clinical controller 604 , which may be coupled to manual input device 606 . A camera 608 and sensor 610 may also be coupled to the clinical controller 604 . The camera 608 and/or sensor 610 detect motion or attributes of the motion. The data detected by the camera 608 and/or sensor 610 are processed by the clinical controller 604 . When the data indicates a threshold has been reached during the performance of the therapeutic task, the clinical controller 604 may send a signal to the external communication device 602 , and the external communication device 602 may send a signal to the implanted stimulation system 500 . The implanted stimulation system 500 receives the signal at the IPG and generates stimulation of the vagus nerve at the electrodes. The manual input device 606 may be used to control the delay between stimulations.
The system may also implement magnet mode, where a hand-held magnet may be swiped over the IPG in order to cause a stimulation. The specialized stroke software may include a magnet mode setting, to provide for use of this mode. When in magnet mode, swiping the hand-held magnet will deliver a pre-programmed stimulation (i.e. at whatever settings were programmed). The reason for this feature is the physician and patient do not need to be in proximity of the computer/external controller, an arrangement that may work better for some kinds of tasks. When not in magnet mode the magnet causes stimulation to stop, as a safety feature.
The clinical controller 604 may run specialized stroke therapy software. The specialized stroke therapy software manages patient data, controls the stimulations, sets the stimulation parameters, and records data from the therapy. FIGS. 8-13 show screenshots from an embodiment of the stroke therapy software. With reference to FIG. 8 , a screen shot shows an initial page of the specialized stroke therapy software. The initial page allows the user to navigate to input screens for programming the implant, set the therapy parameters, and access patient data. With reference to FIG. 9 , a screen shot depicts the input screen for programming the implantable system. With reference to FIG. 10 , a screen shot depicts an input screen for further programming the implantable system. With reference to FIG. 11 , a screen shot depicts an input screen for advanced settings. With reference to FIG. 12 , a screen shot depicts an input screen for implantable parameters. With reference to FIG. 13 , a screen shot depicts a therapy delivery screen. On the therapy delivery screen, a therapeutic task may be selected.
With reference to FIG. 14 , an automated stimulation pairing system 800 is shown. One or more objects 802 such as a cylinder, a key, a block, or any other object suitable for manipulation-type tasks is placed in a workspace. Portions of the patient's body, such as a hand or fingers, may also serve as objects. The object 802 is marked with a colored marker 804 such as a piece of colored tape, a spot of paint, a colored sticker or any appropriate manner of marking an object with color. For some tasks, such as rotation, the colored marker 804 needs a long edge and a short edge, as shown. Any object 802 can be marked with a sticker or tracking sphere and tracked for the therapy. A camera 608 or a plurality of cameras 608 are placed around the workspace so that the object 802 and the marker 804 is within view of the camera 608 . Cameras 608 may also be used to monitor the patient rather than an object or marker. In accordance with an embodiment, a camera may be placed above the workspace. The cameras 608 are connected to the clinical controller 604 . Specialized software running on the clinical controller 604 uses data from the cameras 608 to determine the relative position, velocity, rotation or any other metric related to the performance of the given task. The clinical controller 604 uses the determined metric to decide when stimulation is appropriate and sends a stimulation signal to the external communication device 602 . A manual interrupt 606 may be implemented so that a therapist can interrupt and control the rate of stimulation. The automated system 800 may be completely automated, in a closed loop setup so that the next stimulation is automatic. The automated system 800 may be arranged in an open loop fashion, so that the therapist must intercede before the next stimulation.
The specialized software monitors x,y,z translations of objects with an attached target. The specialized software includes parameters for a variety of tasks that may be performed using this type of closed loop automated system. Using a single camera and colored markers, a wide variety of tasks can be automated. Motion, speed, height, initiation of translation, acceleration, angular rotation, angular velocity, angular acceleration, force, velocity, acceleration, angular acceleration, path length, time to target, distance traveled to target, range of motion, height of object and combinations of these and other metrics can be used to trigger stimulation. Some example tasks include: slide a cup, lift a cup, spin a cup, Lift a cup and move it to some other location, move an object by rotating your wrist, turn a key, flip a coin, pick up a spoon. Tasks may be combinations of movements or tasks, such as lifting a cup and bring it to the mouth, lifting a penny and putting it on a shelf, lifting a key, putting it in a lock and turning the key, or sliding a cup to some point, picking it up, and spinning it 30 degrees. The tasks may be designed to isolate movements of specific muscle groups. Adaptive tracking of a base metric, based on past performance within a session or between sessions, can be used to generate improvement.
The automated paired stimulation system may be arranged so that when the object 802 is moved into or out of a pre-defined boundary that surrounds the object, vagus nerve stimulation is triggered.
A marker 804 can be placed on the patient's hand or arm rather than on an object.
When the object 802 when lifted or lowered in the z-axes i.e. towards the camera 608 , the change in the area of the marker 804 may be detected and used to trigger stimulation.
The object 802 may be moved to specified places on the surface. For example, the task may require the patient to move the task object 802 to a square on the surface. When the object is successfully moved to the square, the VNS stimulation is triggered.
Stimulation is triggered during the movements. The specialized software may stimulate on the best trials, such as shortest path length, fastest movement, optimal acceleration, minimal jitter, maximum height and other metrics, to provide pairing with improved performance.
The manual interrupt 606 may be adapted to require the therapist after a stimulation from the automatic software to press the manual interrupt 606 to indicate a new stimulation can be permitted. This allows the physician or patient to reset the object 802 or for the physician to demonstrate the movement without accidentally causing a stimulation.
In accordance with another embodiment, EMG (muscle electrical activity) may be measured and used to trigger paired vagus nerve stimulation. It is also possible to quantify or image specific movements of the patient such as a patient's walking gait, eye position or tongue position and pair them with VNS. Muscle activity in muscle groups that are only partly under voluntary control (e.g. bladder and sphincter) may be used to trigger paired vagus nerve stimulation.
The automated system may support such tasks as: Reach and grasp; Reach and grasp (small/large objects) (gross and fine movements, dexterity); Point and/or press objects with finger (accuracy); Insert small objects into wells of different sizes (accuracy); Flip cards or sheets of paper (Circumduction and dexterity); Lift objects from table; Circumduction and bimanual tasks (mainly involving wrist and distal joints); Lock and key (Circumduction); Turning a doorknob (Circumduction); Open and close a pill bottle (bimanual; flexion extension wrist); Pour water from a pitcher to glass (bimanual).
Motion can be detected using a camera or other detection devices. The system may operate by detecting change in color of the object by a camera, breaking an IR beam PIR motion sensor, engaging a force transducer, turning a knob or dial potentiometer, pressing a button, flipping a switch, activating a motion sensor, activating a piezoelectric sensor, ultrasonic sensors for detecting distance, or any other appropriate measure of motion.
The automated system may be designed to do is to determine a “good” trial and only stimulate on a good trial. A good trial may be determined by comparing the history of past movements, running an appropriate algorithm on a clinically relevant parameter(s) and using this determination to trigger stimulation. Good could be defined ahead of time by speed, acceleration, strength, range of motion, like degree of wrist turn, or any other appropriate defining quality.
Similar automated systems are described in U.S. Pat. Nos. 6,155,971 and 7,024,398.
With reference to FIG. 15 , a screenshot of a specialized automated pairing software is depicted. Patient data and motion parameters may be entered or selected. A camera view detects the motion of an object and provides vagus nerve stimulation, in accordance with the selected parameters.
Support
Although sensory and motor systems support different functions, both systems can exhibit topographic reorganization of the cortex following training or injury. Tone training (conditioning or artificial stimulation) can increase the representation of the tone in the auditory cortex. Operant training on a tactile discrimination task increased somatosensory cortical representation of the digit used in training. Similar changes can occur in the motor cortex following training with precise digit movements. Motivation and frequency of training influence the degree of cortical map plasticity. Deprivation caused by peripheral injury changes the organization of sensory and motor cortices. For example, digit amputation or nerve transection causes receptive fields in the inactivated somatosensory cortex to shift to neighboring digits. Likewise, transecting the facial nerve reduces the number of motor cortex neurons that elicit vibrissae movements while increasing the number eliciting forelimb movements. Targeted lesions to the sensory or motor cortex can cause the surrounding healthy cortical areas to take on some of the damaged area's lost functionality. Drugs that block reorganization of cortical representations in the sensory cortex can also block reorganization in the motor cortex. Collectively, these results suggest that the mechanisms regulating cortical plasticity are common to both sensory and motor cortices.
The vagus nerve may send afferents to a number of nuclei known to release neuromodulators associated with cortical plasticity, including the locus coreleus, raphe nuclei, and the basal forebrain. The vagus nerve has several efferents to major organs in the body, including the heart; however, a large portion of the vagus nerve consists of afferent connections to several targets in the midbrain. Low-current stimulation of the left vagus nerve is a commonly used treatment for drug-resistant epilepsy that is associated with minimal risks. Complications associated with stimulation to the heart are avoided due to the limited contributions of the left vagus nerve to cardiac activity and the minimal levels of current. Unilateral stimulation of the vagus nerve can result in bilateral activation of the nucleus of the solitary tract and its projections to the locus coeruleus and raphe nucleus. Activation of the locus coeruleus can lead to activation of the nucleus basalis through α1 adrenoreceptors. Although the exact mechanisms of action are not entirely yet understood, VNS has demonstrated several beneficial effects for major depression, mood enhancement, improved memory, decision making, and improved cognitive abilities in Alzheimer's patients, and it reduces edema following brain trauma. Due to the known release of multiple neuromodulators, VNS has recently become an object of study in regulating cortical plasticity.
Pairing VNS with motor therapies can be accomplished using several types of pairing systems. A timing control device can initiate or provide the therapy and the VNS at appropriate times. A timing control device can monitor the therapy and provide VNS at appropriate times during the therapy. A timing control device can receive manual inputs from a patient or clinician during the therapy and generate VNS at appropriate times.
Several experiments have been performed that demonstrate the effectiveness of pairing motor therapy with VNS. The methods and results of those experiments are described below.
The wheel spin task required the rat to spin a textured wheel towards themselves. Rats used movements of the wrist and digits to complete this task. Stimulation and reward occurred after the rat spun the wheel about 145° within about one second period. The lever press task required the rat to depress a spring-loaded lever twice within about 0.5 seconds. The range of motion required to complete this task pivoted primarily around the shoulder joint. Stimulation and reward occurred after the second lever press.
Although sensory and motor systems support different functions, both systems exhibit dependent cortical plasticity under similar conditions. If mechanisms regulating cortical plasticity are common to sensory and motor cortices, then methods generating plasticity in sensory cortex should be effective in motor cortex. Repeatedly pairing a tone with a brief period of VNS increases the proportion of primary auditory cortex responding to the paired tone. It was predicted that repeatedly pairing VNS with a specific movement would result in an increased representation of that movement in primary motor cortex. As such, VNS was paired with movements of the distal or proximate forelimb in two groups of rats. After about five days of VNS movement pairing, intracranial microstimulation was used to quantify the organization of primary motor cortex. Larger cortical areas were associated with movements paired with VNS. Rats receiving identical motor training without VNS pairing did not exhibit motor cortex map plasticity. These results suggest that pairing VNS with specific events may act as a general method for increasing cortical representations of those events. VNS-movement pairing could provide a new approach for treating disorders associated with abnormal movement representations.
Repeatedly pairing VNS with a tone may cause a greater representation of that tone in primary auditory cortex. This map expansion is specific to tones presented within a few hundred milliseconds of VNS. No previous study has reported the effects of pairing VNS with a specific movement on cortical plasticity. If the mechanisms regulating map plasticity in the auditory cortex are the same in the motor cortex, then VNS-paired with a movement should generate map plasticity specific to the paired movement. In one embodiment, VNS was paired with a specific movement to test if this method could be used to direct specific and long-lasting plasticity in the motor cortex.
In one embodiment, thirty-three rats were randomly assigned to receive a vagus nerve cuff electrode or a non-functional, sham vagus nerve cuff electrode. After recovery from the surgery implanting the nerve cuff, thirty-one rats were trained to perform one of two operant motor tasks using either their proximal or distal forelimb. After the rats learned to reliably generate the required movement, VNS was paired with the movement several hundred times each day for about five days. For twenty-five of these rats, intracranial microstimulation (ICMS) was used to quantify the reorganization in the primary motor cortex about 24 hours after the last training session. Instead of ICMS, six of the non-stimulated rats received ischemic motor cortex damage and were retested to confirm that accurate performance of the task requires motor cortex. Motor cortex ICMS was performed on two rats that had functional VNS electrodes and received the same amount of VNS but received no motor training Δn additional group of eight experimentally naïve rats that had not received motor training or VNS also underwent motor cortex ICMS.
A comparison of the motor maps from the rats with sham cuffs to the rats with functional cuffs allows a determination as to whether pairing VNS with the movements enhances cortical plasticity. Comparison of the motor maps from rats that were performing a task during VNS with rats that were not performing a task during VNS allows a determination as to whether the motor task was required to generate motor cortex plasticity.
Forty-one adult, female Sprague-Dawley rats were used in this experiment. The rats were housed in a 12:12 hour reversed light cycle environment to increase their daytime activity levels. During training, the rats' weights were maintained at or above 85% of their normal body weight by restricting food access to that which they could obtain during training sessions and supplementing with rat chow afterward when necessary.
Rats were implanted with a custom-built cuff electrode prior to training. Stimulating cuff electrodes were constructed as previously described. In one embodiment, two TEFLON-coated multi-stranded platinum iridium wires were coupled to a section of Micro-Renethane tubing. The wires were spaced about two mm apart along the length of the tubing. A region of the wires lining the inside circumference of the tube about eight mm long was stripped of the insulation. A cut was made lengthwise along the tubing to allow the cuff to be wrapped around the nerve and then closed with silk threads. This configuration resulted in the exposed wires being wrapped around the vagus nerve at points separated by about two mm, while the leads exiting the cuff remained insulated. These insulated wires were tunneled subcutaneously to the top of the skull and attached to an external connector. A second group of randomly chosen rats received similar cuffs, but with silk threads in place of the platinum iridium wires.
In one embodiment, all the steps of the surgeries were the same regardless of the type of cuff implanted. Rats were anesthetized using ketamine hydrochloride and xylazine with supplemental doses provided as needed. After rats were no longer responsive to toe pinch, incision sites atop the head and along the left side of the neck were shaved and cleaned with betadine and about 70% isopropyl alcohol. The application of opthomalic ointment to the eyes prevented corneal drying during the procedure and a heating pad maintained the rats' body temperature at about 37° Celsius (C.). Doses of cefotaxime sodium and a dextrose/Ringer's solution were given to the rats before and during the surgery to prevent infection and provide nourishment throughout the surgery and recovery. Bupivicaine injected into the scalp and neck further ensured that the rats felt no discomfort during surgical procedures. An initial incision and blunt dissection of the scalp exposed the lambda landmark on the skull. Four to five bone screws were manually drilled into the skull at points close to the lambdoid suture and over the cerebellum. After an acrylic mount holding a two-channel connector was attached to the anchor screws, an incision and blunt dissection of the muscles in the neck exposed the left cervical branch of the vagus nerve. As in humans, only the left vagus nerve was stimulated because the right vagus nerve contains efferents that stimulate the sinoatrial node and can cause cardiac complication.
In one embodiment, eighteen rats received the platinum iridium bipolar cuff-electrodes while another thirteen received the sham cuffs in which silk thread replaced the platinum iridium wires. Leads (or silk threads) were tunneled subcutaneously and attached to the two-channel connector atop the skull. All incisions were sutured and the exposed two-channel connector encapsulated in acrylic. A topical antibiotic cream was applied to both incision sites. After surgery, the rats with silken threads looked identical to the rats with wired cuffs after the surgeries. Rats were provided with amoxicillin (about 5 mg) and carprofen (about one mg) in tablet form for three days following the surgeries and were given one week of recovery before training began. During the week of recovery, rats were habituated to having the stimulator cable coupled to the two-channel connector on their heads. This method of cuff electrode construction, implantation, and stimulation delivery has repeatedly been shown to consistently result in VNS that persists over the full-term of the experiment.
In one experiment, rats were trained on either the wheel spin task (n=10 rats) or the lever press task (n=21 rats). Training occurred in two daily sessions for five days each week. Both tasks involved quick movement of the forelimb in order to receive a sugar pellet reward. Rats initiated each trial, but a delay of at least two seconds was required between trials to allow the rats to eat the sugar pellet. The wheel spin task required the use of muscles located primarily in the distal forelimb, especially the wrist, while the lever press task required the use of the shoulder and the proximal forelimb.
The initial shaping procedures were similar for both motor tasks. In one embodiment, rats were placed in a cage and allowed to freely explore the area. A tether was coupled to the rats' heads to familiarize the animals with the feeling of the connection. Each time the rats approached the response device (e.g., the lever or wheel), they received a 45 mg sugar pellet dispensed into a pellet dish located within the cage. Restrictions were gradually placed on rewarding the rats' proximity to the response device until the rats had to be next to, and then touching, and finally using the device to receive the reward. An experimenter conducted shaping procedures manually. Rats typically took four 30-minute sessions to become familiarized to the response device. After shaping, all training sessions were automated using custom-written programs.
In one embodiment, rats that trained on the wheel spin task were required to spin a textured wheel below the floor of the training cage to receive a sugar pellet reward. Trials were initiated by the rats, but rewards were spaced at least two seconds apart by the computer program. In one embodiment, rats were initially rewarded for spinning the wheel about 3° within a one-second period when each new stage began. After about 35 successful spins of the wheel, the degree of rotation required for a reward increased to about 30°, then about 75°, and finally about 145°. After about 35 rewards at the highest rotational requirement, the rats advanced to the next stage of training (e.g., more restricted access to the wheel) where they repeated all of the levels of increasing rotation again as previously described. Rats demonstrated a paw preference early in training and continued to use that paw for the remainder of the sessions.
In one embodiment, rats depressed a lever initially located inside the training cage to receive a sugar pellet reward. The training cage was a wire cage with dimensions of approximately 20 centimeter (cm)×20 cm×20 cm with a Plexiglas wall opposite the door. In one embodiment, all training sessions other than the shaping sessions were about fifteen minutes long and occurred about twice daily. Trials were initiated by the rats, but rewards were only given to trials occurring at least five seconds apart. After receiving about 60 pellets in about two shaping sessions by pressing the lever, the rats learned to press the lever twice in an about three-second period for the same reward. The interval between lever presses that elicited a reward was reduced from about three seconds to about two seconds, then about one second, and finally about 500 milliseconds (ms), with about 15 successful trials as the criterion for advancing. After successfully pressing the lever twice within about 500 ms about forty-five times, the lever was gradually withdrawn out of the cage. The lever was initially located about four cm inside the cage, then moved to about two cm inside the cage, and then to about 0.5 cm, about 1.5 cm, and about 2.0 cm outside of the cage. The criterion for retracting the lever was about 15 successful double-lever presses for each position, except for about 0.5 cm outside the cage, which required 30 successful trials. In one embodiment, rats reached through a window in the Plexiglas wall that was about one cm×about seven cm to reach the lever outside the cage. The edge of the window was located about two cm from the cage wall, while the lever was offset so that the middle of the lever lined up with the edge of the window furthest from the wall. This arrangement restricted the rats so that they could only comfortably press the lever with their right paw. This aspect of the task design was important for confirming the importance of the motor cortex for the lever press task with motor cortex lesions.
To confirm that accurate performance on the lever press task requires motor cortex, six rats implanted with the nerve cuffs and trained on the lever-press task without stimulation received motor cortex lesions and were retested for about two days following about one week of recovery. Based on procedures by Fang et al., (2010), the vasoconstrictor endothelin-1 was used to selectively lesion the caudal forelimb area of the motor cortex. Basic surgical procedures for cleaning, anesthesia, and post-surgical care were the same as the cuff implantation surgery. After cleaning the top of the head, an incision was made longitudinally and a craniotomy was performed over the primary motor cortex caudal forelimb area contralateral to the trained forelimb (about 2.75 mm to about −0.75 mm anteroposterior and about 2.25 mm to about 3.75 mm mediolateral, relative to bregma). Endothelin-1 (about 0.33 microliters (μL) of about 0.3 micrograms (μg) mixed in about 0.1 μL saline) was injected at a depth of about 1.8 mm using a tapered Hamilton syringe along a grid within the craniotomy at about 2.5 mm, about 1.5 mm, about 0.5 mm, and about −0.5 mm anteroposteriorally, and about 2.5 mm and about 3.5 mm mediolaterally relative to bregma for a total of eight sites according to one embodiment. KwikCast silicone gel was used to replace the removed skullcap and the skin was sutured. The lever press task was the only task tested with motor cortex lesions due to the ease with which the forelimb used in the task could be restricted. The lever press task could not be completed with the left forelimb because of the cage design. Lesions were made in the left motor cortex forcing the rat to try to use its impaired right forelimb to complete the task. Impairments to the distal forelimb accompany impairments to the proximal following motor system lesions. Additionally, the lesion size covers the entire caudal forelimb area; therefore, it is expected that impairments to the lever press task would also indicate impairments to the wheel spin task.
During the final stage of the motor tasks, reaching through a window about 1.2 cm wide and spinning the wheel about 145° within about one second period or pressing the lever located about two cm outside the cage twice within about 500 ms triggered a food reward and VNS. Stimulations were delivered approximately 75 ms after the wheel reached 145° or the lever triggered the second press. Rats typically continued to spin the wheel or press the lever beyond the required criterion, such that the movements were still occurring during VNS. In one embodiment, VNS was always delivered as a train of about 15 pulses at about 30 hertz (Hz). Each about 0.8 milliamps (mA) biphasic pulse was about 100 microseconds (μs) in duration. The train of pulses was about 500 ms in duration. Previous studies have demonstrated that the amplitude of electroencephalographic measures may be reduced and neuronal desynchrony may increase during VNS using the described electrode implantation, which may indicate a successful stimulation of the vagus nerve. VNS-movement pairing during the final stage of training continued for one week (in one embodiment, 10×about 30 minute sessions for the wheel-spin task and 10×about 15 minute sessions for the lever-press task), delivering around 1,200 total stimulations. Previous research has shown that this form of VNS does not alter heart rate, blood oxygenation level, or ongoing behavior, suggesting that the stimulation is neither aversive nor rewarding to the animals.
In one embodiment, connections and stimulations from the external stimulator to the rats were identical between rats implanted with functional or sham VNS electrode cuffs. The sham cuffs with silk threads in place of platinum iridium leads did not carry an electrical charge when stimulated. This difference in the cuffs allows experimenters to remain blind during training to stimulated and sham rats.
The day after the last training session of VNS movement pairing, the organization of primary motor cortex contralateral to the trained paw was defined using standard ICMS mapping procedures. In one embodiment, an additional eight rats that did not train or receive VNS also underwent ICMS procedures to the left cortex to compare the effects of training on motor cortex organization. After placing the rat in a stereotaxic frame with a digital readout, a craniotomy was performed to expose the motor cortex. In one embodiment, parylene-coated tungsten electrodes were inserted to a depth of about 1,800 micrometers. Stimulation occurred following a grid with about 500 μm spacing. Sequential electrode placements were made at least one mm apart where possible. ICMS was delivered once per second. In one embodiment, each stimulation consisted of an about 40 ms pulse train of about ten 200 μs monophasic cathodal pulses delivered at about 286 Hz. Stimulation intensity was gradually increased (from about 20 to about 200 microamperes (μA)) until a movement was observed. If no movement was observed at the maximal stimulation, then the site was deemed nonresponsive. The borders of primary motor cortex were defined based on unresponsive sites and stopped at the posterior-lateral vibrissae area, which is known to overlap the somatosensory cortex.
In one embodiment, motor mapping procedures were conducted with two experimenters, both blind to the experimental condition of the rat. The first experimenter placed the electrode and recorded the data for each site. Because the motor cortex is organized with similar movements often occurring in the general vicinity of each other, the second experimenter was kept blind to the electrode placement to avoid potential biasing. The second experimenter delivered stimulations while observing which parts of the body moved in response. Movements were classified based on the part of the body that moved using the threshold stimulation current. Larger movements were obtained using higher current stimulations and were used when necessary to disambiguate movements too small to confidently classify at threshold levels. The first stimulation site was placed in an area often resulting in movement of the lower forelimb. Subsequent stimulation sites were randomly chosen and did not extend beyond established border (e.g., unresponsive) sites. Movements of the vibrissae, face, eye, and neck were classified as “head”. Movements of the shoulder, elbow, and upper forelimb, e.g., proximal forelimb, were classified as “upper forelimb”. Movements of the wrist and digits were called “distal forelimb”. “Hindlimb” included any movement in the hindlimb of the rat. Cortical area was calculated by multiplying the number of sites eliciting a response by about 0.25 mm 2 . Four sites equal about one mm 2 .
To confirm that VNS alone does not produce motor cortex map reorganization, two rats that were never trained to perform a motor task were placed into a training cage and received randomly delivered VNS (e.g., not paired to a specific movement). Except for the movement pairing, VNS in this group was identical to the groups above. In one embodiment, each animal was passively stimulated for two 30-minute sessions per day with an about two-hour break between sessions, and repeated for about five days. Within each session, stimulation occurred for a time from about 8 to about 16 seconds, giving an average stimulation time of about 11.25 seconds. At the end of each session, about 160 stimulations were given, which amounted to about 1,600 stimulations. Animals were ICMS mapped about 24 hours following the final passive VNS session.
Rats were shaped to the wheel spin task in about 4±0.3 sessions and the lever press task in about 4±0.3 sessions. Rats reached the last stage of the wheel spin task in about 27±5 sessions and the lever press task in about 8±1 session. The percent of successfully completed trials on the wheel spin task on the first day of VNS paired training was about 77±4%. The same measure for the lever press task on the first day of VNS paired training was about 78±4%. Microelectrode mapping techniques were used to determine the organization of the motor cortex after five days of VNS paired training on the last stage. Maps of the motor cortex were derived from about 3,595 electrode penetrations (average about 103 sites per animal).
In all rats tested, the anterior portion of the motor map generated movements of the rat's head, including the jaw, vibrissa, and neck. The middle region of the map generated movements of the forelimb and the posterior region generated movements of the hindlimb. As in earlier reports, it was possible to divide the forelimb area into a small rostral region that is mostly surrounded by head responses and a larger caudal forelimb area that borders the hindlimb area.
In one embodiment, the organization of primary motor cortex was not significantly altered by training without VNS. The average area representing the distal forelimb, proximal forelimb, head, and hindlimb were not significantly different across the naïve, wheel spin, or lever press trained rats that had sham VNS cuffs electrodes and received no VNS. As a result, these three control groups are averaged for group analyses and referred to as the non-VNS group.
In one embodiment, rats that received VNS paired with the wheel spin task exhibited a significant reorganization of the motor cortex. In the non-VNS rats, the head and distal forelimb occupy approximately the same amount of cortical area Hindlimb and proximal forelimb comprises a smaller region of the motor map. Wheel spin/VNS pairing resulted in an about 15% larger distal forelimb area (about 1.0 mm 2 ), an about 25% smaller head area (about −1.75 mm 2 ), and no proximal forelimb area in this particular animal compared to the naive. These changes in cortical area for the Wheel spin/VNS paired group were pronounced when compared to the non-VNS group. On average, pairing VNS with the wheel spin task resulted in an about 32% increase in the cortical area representing the distal forelimb compared to the non-VNS group. This increase was accompanied by an about 38% smaller head area and an about 63% smaller proximal forelimb area, but no change in the area devoted to hindlimb. These results suggest that repeatedly pairing VNS with a particular movement can generate a specific increase in the motor cortex representation of that movement.
To confirm that the observed cortical plasticity was specific to the movement paired with VNS, the reorganization of motor cortex was documented in rats that received VNS paired with a lever press task. Since this task primarily involves movement of the proximal forelimb, an increased proximal forelimb representation after lever press/VNS pairing was expected. The lever press/VNS rat had about 1600% (about four mm 2 ) more area devoted to the proximal forelimb area compared to the naïve rat. Pairing VNS with the lever press movement reduced the head area by about 39% (about −2.75 mm 2 ) and distal forelimb area by about 59% (about −4 mm 2 ) in this rat compared to the naïve rat. Like the wheel spin/VNS trained rat, the lever press/VNS rat had the same sized hindlimb representation as the naïve rat. These examples suggest that the motor cortex plasticity observed following VNS-movement pairing may be specific to the paired movement and not a general effect of VNS.
On average, rats that received VNS during the lever task exhibited about 159% increase in the proximal forelimb area compared to the non-VNS group. The lever press/VNS group had an about 23% smaller distal forelimb area and an about 29% smaller head area than the non-VNS group. The most profound differences were observed between the wheel spin/VNS rats and the lever press/VNS rats. Although both groups received identical VNS, wheel spin trained rats had an about 72% larger distal forelimb area than the lever press rats and the lever press rats had an about 598% larger proximal forelimb area compared to the wheel spin trained rats. These results may demonstrate that VNS-movement pairing can generate large-scale reorganization of motor cortex and confirm that the reorganization is specific to the movement repeatedly paired with VNS.
In one embodiment, VNS was delivered at random times in two rats before documenting the organization of motor cortex using ICMS techniques. Motor cortex in these rats was similar to naïve rats and there was no evidence of the reorganizations that were observed after either the lever press or the wheel spin movements were paired with VNS. This observation combined with task specificity of the motor cortex plasticity observed in the trained rats that received VNS suggests that VNS-movement pairing may be sufficient to generate motor cortex reorganization.
In one embodiment, there was no difference in the average stimulation thresholds for the groups receiving movement paired VNS and the non-VNS group. The differences in average stimulation thresholds between past studies and the current study may be due to our using a somewhat deeper level of anesthesia. The rats trained with VNS paired on the wheel spin task had an average distal forelimb stimulation threshold not too different from the wheel spin trained group with sham VNS cuff electrodes. The VNS paired with lever press group's proximal upper forelimb stimulation thresholds was not considerably different from the lever press group trained with sham VNS cuff electrodes. Similar stimulation thresholds between paired-VNS and non-VNS trained rats demonstrate that the observed movement representation reorganizations are not due to altered levels of excitability in the cortex. This result is consistent with several papers that have found cortical representation changes in the motor cortex from training occurs without ICMS threshold changes. Morphological changes, such as synaptogenesis, have been observed with past motor cortical reorganization accompanying training and may account for a mechanism of change in movement paired VNS.
The performance on the lever press task before and after ischemic motor cortex damage in six rats was compared. In one embodiment, performance was markedly impaired in every rat. Average performance fell from 93±1% successful double-tap attempts for the last two days before surgery to 75±5% for the two days of testing conducted after a week of recovery. This result tends to confirm that this task like other skilled motor tasks may depend on motor cortex for accurate performance.
The task performance in each group was compared to confirm that movement paired VNS does not make the task more difficult. In one embodiment, no behavioral differences were observed between VNS and sham groups on the wheel spin task in the total number of successful trial, the velocity at which the wheel was spun, or the percentage of successfully completed trials per session. VNS rats showed no impairment on the lever press task and, in fact, exhibited shorter lever press intervals and triple pressed the lever more often than the sham rats. Although VNS enhanced some aspects of the lever press task, the percent of successful trials and the total number of successful trials were not different between the VNS and sham rats. These results may indicate that VNS is unlikely to have enhanced map reorganization by making the task more difficult.
It was predicted that repeatedly pairing brief stimulation of the vagus nerve with a specific movement would result in a larger representation of that movement in the motor cortex. As such, about 0.5 sec of VNS was delivered each time rats used their distal forelimb to rotate a wheel. After several hundred pairings, the cortical representation of the distal forelimb was markedly larger in these rats compared to naïve rats and rats that performed the same movements without VNS. A second group of rats was trained on a motor task using a different part of their body to confirm that map reorganization was specific to the movement paired with VNS. Pairing VNS with a lever press task that required the use of the proximal forelimb resulted in a markedly larger proximal. Impaired performance in a group of rats following ischemic lesions to the caudal forelimb area tends to confirm the involvement of the motor cortex in this task. The observations that map expansion was specific to the movement paired with VNS and that neither of the tasks without VNS nor VNS without the task training generated map reorganization indicates that movement paired VNS is sufficient to direct map plasticity.
Pairing VNS with a motor event generated cortical plasticity comparable to that observed using a similar paradigm in the auditory system. Presenting a tone with a brief period of VNS causes a significant expansion of the paired tone's representation in the auditory cortex. Presenting tones or VNS alone did not alter the auditory cortex's tonotopic organization. These two studies suggest that the plasticity enhancing mechanisms of event-paired VNS may be shared with the auditory and motor cortex.
A number of studies have reported that training on skilled motor tasks increases cortical representations for the movements involved. The results disclosed herein do not contradict these findings, as one of the landmark studies demonstrating training induced cortical plasticity using a skilled reaching task also demonstrated a lack of reorganization for a lever press task. The lack of observed cortical change following training on the lever press and wheel spin tasks may be due to a number of reasons. The cortical reorganization observed in a skilled reaching task has been attributed to the accuracy of the movements necessary to complete the task which may be absent in our lever press and wheel spin tasks. There is also a possibility that the sampling distance of about 500 μm is too coarse to see cortical changes associated with tasks in the current study, although this spacing has previously demonstrated training induced plasticity in the aforementioned skilled reaching task. Another possibility is the cortical changes observed following motor and auditory learning have been shown to be transient while the acquired skill remains stable over time. The lever press and wheel spin trained rats were mapped approximately 10 and 20 days after their initial training session, respectively, possibly occurring after cortical changes associated with training would have been observed. If this possibility occurred, then the VNS-paired training may have prolonged or reestablished the observed changes in the motor cortex organization.
The exact mechanisms by which VNS directs plasticity in motor or sensory cortex are unknown. VNS causes the release of several molecules known to enhance cortical plasticity, including acetylcholine, norepinephrine, serotonin, and brain derived neurotrophic factor. Perfusing norepinephrine into an adult cat's visual cortex produces kitten-like plasticity in a test of ocular dominance shifts following monocular deprivation. Serotonin specific neurotoxins and receptor blockers prevent normal ocular dominance shifts in kittens in monocular deprivation, implicating the importance of serotonin for normal plasticity. Another important study showed that enhancing serotonin release with fluoxetine can stimulate plasticity in adult cats. Blocking the release of acetylcholine prevents cortical plasticity and interferes with skill learning and recovery from brain damage. The use of the muscarinic antagonist scopolamine blocks the effect of VNS on spontaneous firing rate in the auditory cortex, further supporting the influence of VNS on the cholinergic system. Adding brain derived neurotrophic factor induces plastic changes in ocular dominance shifts in adult rats following monocular deprivation. Combining more than one of these elements can lead to greater plasticity than the influence of the elements singularly. The ability of VNS paired with wheel-spin or lever-press training to produce cortical plasticity supports the importance of the VNS triggered release of these molecules in enhancing cortical plasticity. VNS is likely to generate cortical map plasticity specific to the associated event through the synergistic action of multiple plasticity enhancing molecules.
The simultaneous presentation of VNS with a specific sensory or motor event can be sufficient to increase cortical representation of that movement. As discussed above, a sugar pellet was used to reward the animal's behavior immediately after the completion of a trial. As a result, VNS was delivered during the behavioral task that finished just a few seconds prior to the animal eating the pellets. It would not have been surprising to see an increased representation of the head and jaw in this study.
In a previous study, our lab demonstrated that changes in auditory cortex were temporally specific to tones paired with VNS. Two randomly interleaved tones were presented every about 15 to about 45 seconds for several thousand trials to a rat with only one of the tones paired with VNS. The number of sites responding to the VNS paired tone increased significantly, while the number of sites for the tone presented within tens of seconds of the VNS did not. These observations are consistent with past studies demonstrating that pairing nucleus basalis stimulations with tones only alters the tone's representations when stimulations occurred within seconds of the tone presentation.
The results disclosed herein demonstrate that the head representations did not increase because of VNS just prior to chewing. This result indicates that the plasticity enhancing actions of VNS are temporally precise, lasting less than about one or about two seconds. These results demonstrate that brief pulses of VNS can be used to direct highly specific plasticity. Additionally, VNS without paired behavioral training did not result in map reorganization, further supporting our conclusion that the cortical changes triggered by VNS are enhanced by task specific pairing. Methods for enhancing plasticity that rely on slow-acting mechanisms may not be as effective in generating the same accuracy of plasticity as VNS-pairing. Pharmaceuticals often elevate or diminish certain neurotransmitters for several hours. Several movements or sensory events may occur repeatedly during this time, potentially creating unwanted plasticity. The temporal precision of the VNS-pairing method for enhancing cortical plasticity should offer advantages in efficiency and efficacy as compared to methods with less precise actions.
In one embodiment, motor map expansions did not accompany enhanced task performance in rats trained on the VNS paired wheel spin or lever press tasks. This is not necessarily at odds with the prediction that event paired VNS increase functional recovery through increasing functional plasticity following cortical damage. Map reorganization has been shown to be important for enhancing behavioral outcomes during the learning process (Reed et al., 2011). Rats demonstrating increased tonotopic representations for low frequencies following paired nucleus basalis stimulation demonstrated faster learning of a tone discrimination task compared to controls. However, rats that had already learned the tone discrimination did not behaviorally benefit from the induced plasticity. From these results, the authors concluded that “cortical map expansion plays a major role in perceptual learning but is not required to maintain perceptual improvements”. In the present disclosure, the rats had already learned the tasks when they began receiving VNS, otherwise they may have demonstrated an accelerated learning rate compared to the sham groups. The enhanced propensity for cortical reorganization accompanying event-paired VNS may increase rehabilitative learning.
Stroke and traumatic brain injury often damage movement-controlling areas of the motor cortex resulting in hemiparesis or hemiplegia. Following cortical injury, lost motor representations can partially regenerate in neighboring areas within motor cortex. The size of the regenerated representations is highly correlated with the functional recovery of lost movements, but this recovered area and ability is a fraction of those seen pre-injury. Physical training in healthy animals can greatly increase cortical representation of the muscles used, during learning of the task, but rehabilitative physical training in rats after a motor cortical injury is less effective at generating this increased representation. Movement paired VNS in intact rats generates a comparable amount of cortical plasticity in approximately the same amount of time as physical training. Movement paired VNS is also able to enhance plasticity where plasticity is not observed with training alone. Since increased cortical plasticity is related to increased functional recovery following cortical injury, it is possible that movement paired VNS could enhance the recovery of specific motor functions following cortical injury, compared to rehabilitative training alone.
Non-invasive brain stimulation techniques, such as repeated transcranial magnetic stimulation and transcranial direct current stimulation, show promise as methods for inducing better functional recovery with rehabilitative training following stroke than training alone. These techniques apply a localized current to the scalp to manipulate electrical fields in the cortex without the need for surgery or pharmaceuticals. These methods are thought to work primarily through influencing levels of cortical excitability, but also cause increased levels of neurotrophic factors, serotonin, and dopamine. Combining paired-VNS methods with non-invasive brain stimulation may lead to even greater recovery than either method used alone through activating different plasticity enhancing mechanisms.
Periodic VNS is Food and Drug Administration (FDA) approved as a safe and effective treatment of certain types of refractory epilepsy as well as treatment-resistant depression. Protocols for treating epilepsy comprise about 30 seconds of VNS every about five minutes, 24 hours per day. Periodic VNS using a stimulation protocol similar to that used in treating epilepsy has improved functional recovery in rats with fluid percussion injury to the cortex. This protocol requires about 145 times the daily current injection compared to what was used in the method disclosed herein. The above-disclosed results tend to demonstrate that motor and auditory events can be precisely timed with VNS to markedly alter motor and auditory system organization, respectively. It seems likely that therapies using paired VNS might be a more effective therapy for increasing functional recovery following cortical damage.
Selectively pairing VNS has already shown promise in normalizing abnormal cortical organizations in the treatment of tinnitus in rats. The overrepresentation of a tone was reduced by pairing VNS with tones spanning the rats hearing range except for the tones near the tinnitus frequency. This eliminated the behavioral correlate of tinnitus in rats for several months past the cessation of the treatment. A similar strategy of pairing VNS with movements may improve the treatment of disorders related to abnormal representations in the motor system, such as dystonias. Although the causes are not fully understood, patients with dystonia demonstrate disturbed cortical inhibition that is improved with the application of transcranial magnetic stimulation. Current evidence supports that reducing the overrepresented motor area during these treatments is associated with a reduction in dystonic symptoms. As disclosed herein, the larger representations observed from the VNS paired movements were accompanied by smaller nearby cortical representations, such as movements of the head. Selectively increasing the size of surrounding muscle representations might decrease the overrepresentation of the dystonic muscles. Movement paired VNS of non-dystonic, surrounding movements may decrease the overrepresentation of the dystonic muscles. The strategic pairing of non-dystonic movements with VNS provides a novel potential therapy to treat focal dystonia.
Clinical and pre-clinical data has been collected to support the effectiveness of the tinnitus therapy and parameters.
Selection of the vagus nerve for stimulation is not arbitrary. The vagus nerve produces specific effects when stimulated at a specific time relative to a physical task. The peripheral nervous system, central nervous system including the brain and spinal cord are typically used by others as therapeutic stimulation locations. The choice of stimulation location largely determines the behavioral and neurophysiologic outcome. Even though similar neural populations are activated by input from two different locations, the manner in which they are activated, for example, the pattern of activity generated within the neuron population may depend on the time course of activation, release of one or more neuromodulators, attention state, etc. The neurophysiological consequences therefore are bound to be different. Given the large (and unknown) number of variables that can influence the activation of a given neural population, the mechanisms are likely to be complex and unpredictable. There is no calculus to determine which locations may produce which effects. Finding a location that produces a given effect can only be done experimentally. It is not valid to suggest that stimulation at one location makes it obvious to stimulate at a different location, even if the goal is to stimulate the same population of neurons.
The same can be said for stimulation parameters. At a given stimulation location, stimulation according to one set of parameters may not necessarily produce the same (or similar) effects as a stimulation according to another set of parameters. The frequency of stimulation, the current amplitude of stimulation, the duration of each stimulation, the waveform of stimulation, as well as other stimulation parameters can change the results of stimulation.
Our experiments have shown that the effect generated by VNS pairing is very short, less than 15 seconds. A first tone at a first frequency when paired with VNS generated an increase in the number of neurons that respond to the paired frequency. A second unpaired tone at a second frequency, played 15 seconds after the paired VNS did not show a corresponding increase in the number of neurons that respond to the second frequency. Nothing in the prior art indicates this kind of precise timing requirement.
Similarly, we have performed experiments in which multiple tones at a given frequency were paired with VNS and given 30 seconds apart. This was done in the tinnitus study (Engineer et al., 2011) in which VNS was paired with each of the randomly interleaved tones every 30 seconds (e.g., 1.3 kilohertz (kHz)+VNS, then wait for 30 seconds, then give 6.3 kHz+VNS, and then wait for 30 seconds and so on). The tones were selected such that they surrounded the tinnitus frequency and the tinnitus frequency itself was excluded. The idea was to shrink the representation of the tinnitus frequency thereby restoring the map and synchronous activity back to normal. When the same tones were presented eight seconds apart, the effect was less than if the tones were presented 30 seconds apart, which was surprising.
To cite another example, we have performed a series of experiments where a tone is repeatedly paired with a foot-shock to establish a conditioned fear response. Subsequently, when the tone was presented without a foot-shock, the rat would freeze, anticipating a foot shock. If the tone, without the foot-shock, is then presented repeatedly, the fear caused by the tone would eventually be extinguished, undoing the conditioning. By pairing the tone (without the foot-shock) with VNS, the fear is extinguished much more quickly. However, presenting the tone by itself and then giving VNS minutes later, the fear is extinguished at the normal rate.
Further experiments have demonstrated the effect of the described therapy. VNS paired with a movement improves motor performance in a rat model of ischemic stroke. VNS paired with movement improves a motor deficit several weeks after an ischemic lesion. VNS delivered two hours after rehabilitation did not show any significant difference from rehabilitation alone.
These results demonstrate that the precise timing between VNS and the event as well as the interval separating the VNS-event pairings appear to be important for inducing highly specific plasticity.
Neurostimulation does not behave in a predictable fashion. Different stimulation locations produce different results, even when both locations are cranial nerves. For example, synchronization in the cerebral cortex is a manifestation of epilepsy. Stimulating the vagus nerve causes desynchronization of the cortex neurons, which has been proposed as a potential mechanism for how vagus stimulation prevents an epileptic seizure. Stimulation of the trigeminal nerve, another cranial nerve, causes desynchronization as well. To determine whether the plasticity induced by VNS is specific to the vagus nerve, we paired stimulation of the trigeminal nerve with a 19 kHz tone. However, when we paired trigeminal stimulation with a tone, in the same way we paired VNS with a tone, we did not observe any plasticity that was specific to the paired tone. Pairing the trigeminal stimulation with a tone at a given frequency did not change the response to that frequency even though it caused desynchronization like in the previous study. Each stimulation location is unique across the full range of effects. It appears that VNS may be uniquely suited to direct cortical plasticity and suggests that the vagus nerve is likely a key conduit by which the autonomic nervous system informs the central nervous system of important stimuli.
Both VNS pairing and nucleus basalis stimulation (NBS) pairing have been shown to change the number of neurons responding to a paired frequency. To be effective, the current amplitude parameter of the stimulation for VNS pairing is more than twice the current amplitude used for NBS pairing. There is an important difference between the neuromodulators released by NBS from those released by VNS, so significant differences between the results of NBS and VNS are expected.
Another experiment demonstrated that pairing a single tone at a specified frequency with VNS increased the number of neurons responding not only to that frequency but to close frequencies, e.g., increased the bandwidth compared to control rats. For NBS pairing, the bandwidth was not significantly different from control rats. Unlike VNS pairing, NBS pairing is highly invasive and may be unsuitable to provide a practical therapeutic benefit. Similar results in one circumstance cannot be extended to predict similar results in another, even slightly different, circumstance. Different stimulation parameters have to be used for effective VNS pairing and NBS pairing.
Because of the specific neurotransmitter mechanisms that generate the specific plasticity required for the described therapies, some drugs may reduce the effectiveness. Muscarinic antagonists, norepinephrine blockers that are centrally acting, norepinephrine uptake inhibitors, nicotinic antagonists, Selective serotonin reuptake inhibitors, drugs that block serotonin and drugs that block dopamine may all reduce the effectiveness of the paired VNS therapies.
None of the description in the present application should be read as implying that any particular element, step, or function is an essential element that must be included in the claim scope: the scope of patented subject matter is defined only by the allowed claims. Moreover, none of these claims is intended to invoke paragraph six of 35 U.S.C. section 112 unless the exact words “means for” are followed by a participle. The claims as filed are intended to be as comprehensive as possible, and no subject matter is intentionally relinquished, dedicated, or abandoned.
At least one embodiment is disclosed and variations, combinations, and/or modifications of the embodiment(s) and/or features of the embodiment(s) made by a person having ordinary skill in the art are within the scope of the disclosure. Alternative embodiments that result from combining, integrating, and/or omitting features of the embodiment(s) are also within the scope of the disclosure. Where numerical ranges or limitations are expressly stated, such express ranges or limitations should be understood to include iterative ranges or limitations of like magnitude falling within the expressly stated ranges or limitations (e.g., from about 1 to about 10 includes, 2, 5, 4, etc.; greater than 0.10 includes 0.11, 0.12, 0.15, etc.). For example, whenever a numerical range with a lower limit, R l , and an upper limit, R u , is disclosed, any number falling within the range is specifically disclosed. In particular, the following numbers within the range are specifically disclosed: R=R l +k*(R u −R l ), wherein k is a variable ranging from 1 percent to 100 percent with a 1 percent increment, i.e., k is 1 percent, 2 percent, 5 percent, 4 percent, 5 percent, . . . , 50 percent, 51 percent, 52 percent, . . . , 75 percent, 76 percent, 77 percent, 78 percent, 77 percent, or 100 percent. Moreover, any numerical range defined by two R numbers as defined in the above is also specifically disclosed. Use of the term “about” means±10% of the subsequent number, unless otherwise stated herein. Use of the term “optionally” with respect to any element of a claim means that the element is required, or alternatively, the element is not required, both alternatives being within the scope of the claim. Use of broader terms such as comprises, includes, and having should be understood to provide support for narrower terms such as consisting of, consisting essentially of, and comprised substantially of. Accordingly, the scope of protection is not limited by the description set out above but is defined by the claims that follow, that scope including all equivalents of the subject matter of the claims. Each and every claim is incorporated as further disclosure into the specification and the claims are embodiment(s) of the present disclosure. The discussion of a reference in the disclosure is not an admission that it is prior art, especially any reference that has a publication date after the priority date of this application. The disclosure of all patents, patent applications, and publications cited in the disclosure are hereby incorporated by reference, to the extent that they provide exemplary, procedural, or other details supplementary to the disclosure.
While several embodiments have been provided in the present disclosure, it should be understood that the disclosed systems and methods might be embodied in many other specific forms without departing from the spirit or scope of the present disclosure. The present examples are to be considered as illustrative and not restrictive, and the intention is not to be limited to the details given herein. For example, the various elements or components may be combined or integrated in another system or certain features may be omitted, or not implemented.
In addition, techniques, systems, subsystems, and methods described and illustrated in the various embodiments as discrete or separate may be combined or integrated with other systems, modules, techniques, or methods without departing from the scope of the present disclosure. Other items shown or discussed as coupled or directly coupled or communicating with each other may be indirectly coupled or communicating through some interface, device, or intermediate component whether electrically, mechanically, or otherwise. Other examples of changes, substitutions, and alterations are ascertainable by one skilled in the art and could be made without departing from the spirit and scope disclosed herein.
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A method of treating motor deficits in a stroke patient, comprising assessing a patient's motor deficits, determining therapeutic goals for the patient, based on the patient's motor deficits, selecting therapeutic tasks based on the therapeutic goals, performing each of the selected therapeutic tasks repetitively, observing the performance of the therapeutic tasks, initiating the stimulation of the vagus nerve manually at approximately a predetermined moment during the performance of the therapeutic tasks, stimulating the vagus nerve of the patient during the performance of the selected therapeutic tasks, and improving the patient's motor deficits.
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FIELD OF THE INVENTION
[0001] This invention relates to methods, reagents and kits for enriching nucleic acid sequences. More particularly, the present invention relates to methods, reagents and kits for sample preparation including sample modification, sample enrichment and amplification.
BACKGROUND
[0002] Haplotype information can be vital in the analysis of disease by determining whether two or more sequence variants are located on the same nucleic acid fragment. This is of special interest in tumour research and diagnosis where it is important to know if two or more inactivating mutations occur on the same or different chromosomes. Similarly better information about which genotypes are located on the same nucleic acid segment can greatly increase the information derived from genotyping data and in the statistical analysis of genetic linkage or linkage disequilibrium of inherited traits and markers such as single nucleotide polymorphisms, SNPs (e.g. [1-3]).
[0003] To date there has been no method developed that satisfactorily solves the problem of how to obtain haplotype information in vitro, that is to determine which gene variants are located, over some distance, on the same nucleic acid molecule.
[0004] Current analysis of heritable diseases is hampered by the fact that given the genotypes of the parents, it is still often impossible to confirm if a particular allele is obtained from the mother or from the father. In theory, with the ability to distinguish between haplotypes, more meioses would be informative and thereby facilitate genetic linkage analysis. Another area where haplotyping has proven to be of interest is in the study of genetic effects on a subject's response to different drugs. Recent publications have shown that haplotype information is important to be able to relate genetic factors to a patient's response to various drugs, [4].
[0005] Currently, there are only a few methods available for obtaining haplotype information. When lineage data and nucleic acid samples are available linkage analysis is applicable. It is also possible to use statistical methods to calculate possible allele-combinations from allele frequencies to gain information on a haplotype. However, this technique can only be used with a small number of alleles at the same time and on population-size data, and the analysis only provides statistical evidence for the presence of a given haplotype. Haplotype information can also be gained from hemizygous X- and Y-chromosomes, where haplotypes are immediately apparent from the genotype.
[0006] The possibility to study cells with only one autosome chromosome is utilised in some in vivo techniques. One approach is the creation of rodent-human hybrid cells, for example using the so called “Conversion technology” [2].Some of the rodent-human hybrid cells will contain one of the two possible copies from a human chromosome. A second approach is to use hydatidiform moles, i.e. tissues that due to a fertilisation defect only contain genetic material from the sperm (complete hydatidiform mole) thereby containing only one copy of each chromosome.
[0007] There are also some in vitro molecular techniques that can be used to determine haplotypes. One technique is the sub-cloning of all nucleic acid sequences of interest, isolating individual clones and subsequently genotyping them. Allele-specific analysis through Fibre Fluorescent In Situ Hybridisation is another possible approach, however it has not yet been convincingly shown to be useful for SNP based haplotyping. A third approach is double PCR Allele Specific Amplification (double-PASA [5], a double allele-specific Polymerase Chain Reaction (PCR) which gives linkage information of two adjacent polymorphic sites. Pyrosequencing [6] and mass spectrometry may be used to analyse haplotypes over short distances, i.e. <100 nt.
SUMMARY OF THE INVENTION
[0008] Methods, reagents and kits to analyse haplotypes, genotypes and enrichment of selected sequences are described herein. These methods and reagents are, in addition to aspects mentioned in the background chapter, also of interest for population genetics, identification of lineage in plant and animal breeding and in analysis of microorganisms.
[0009] In one aspect of the invention, a general technique is provided to obtain haplotypes through enrichment for one nucleic acid segment to include a specific variant at a given position. Thereby any variant position in a sample could be used for selection, followed by analysing genetic variants elsewhere in the same nucleic acid fragment.
[0010] In another aspect of the invention the same principle can be used for genotyping or to generate probes that reveal the genotype at particular loci.
[0011] Accordingly, the present invention provides a method for sample preparation that optionally includes the steps of: (a) cleavage of a nucleic acid so that a fragment containing the sequence to be investigated is created with or without addition of oligonucleotide probes (b) selective modification of one variant of the nucleic acid sequences (c) enrichment of the selected variant, and (d) analysis of the nucleic acid.
[0012] The present invention also provides one or several probes for use in the described methods. A first set of probes/probe preferably directs site specific cleavage at predetermined sites of the sample upon hybridisation. Preferably, A second set of probes/probe is used to specifically modify the sample based upon the presence or absence of a given sequence variant. A third set of probes is used for amplification of the sample and a fourth set of probes is used for scoring the genotypes.
[0013] The present invention describes several ways to enrich a nucleic acid sequence or sequences from a multitude of sequences on the basis of the sequence or on the basis of a particular sequence variation at a given position.
DETAILED DESCRIPTION OF THE INVENTION
[0014] The terms “nucleic acid”, “nucleic acid sequence”, “nucleic acid fragment”, “nucleic acid segment”, “nucleic acid probe”, “oligonucleotide”, “target nucleic acid sequence” or “target sequence” describe interchangeably and without preference, a plurality of nucleotides, covalently linked as such to form linear molecules of DNA or RNA.
[0015] The term “variant” describes interchangeably and without preference a nucleic acid encoding a variant, which may for example be selected from the group including any one or more of the following; a single nucleotide sequence variant, deletion sequence variant, insertion sequence variant, sequence length variants, and sequence variation among paralogous or orthologous nucleic acid sequence, or among edited sequences or splice variants
[0016] Examples of different approaches are as follows.
[0017] The first approach, described in part in FIG. 1 , is based on cleavage of DNA at any predetermined site through the use of so called nucleic acid adapters, hereafter called adapters, that are targets or part of targets for restriction enzymes preferably type II or type IIs restriction enzymes [7,8]. Adapters and sample are mixed, denatured and subsequently allowed to cool. The adapters hybridise to their complementary regions in the sample nucleic acid. One of the adapters is positioned so that the resulting cleaved sample DNA contains a variant position at the 5′ position (A). Added restriction enzymes cleave the sample and, through addition of a ligation template that anneals to both the 5′ and 3′ end of the cleaved sample DNA, circular molecules are obtained by ligation of the ends that are brought next to each other (B). This circularisation is driven by the higher relative concentration of two ends belonging to the same molecule compared to those of two different copies of the same or similar molecules. If the added template is complementary to the sample DNA-ends, juxtaposing these, then ligation of the two ends can occur. If a mismatch between the sample DNA and the ligation template exists at the variant position used for selection, or if there are no free ends at the site intended for ligation, then ligation will not occur. Circularised molecules can then be enriched for through the use of exonucleases that degrade uncircularised DNA, and/or amplification of the circularised DNA, for example with rolling circle amplification (RCA) can be performed ([9,10]).
[0018] Alternatively, the adapter could be positioned upstream of the variant position used for selection. Optionally this adapter could be completely omitted. After cleavage, as described earlier, one or a plurality of oligonucleotides is added, (template), which hybridises to both the 3′ end and to an upstream sequence around the variant position, as shown in FIG. 2A . This provides a specificity step. The structure is then cleaved by chemical, enzyme or other means to generate a structure, as shown in FIG. 2B . Where an enzyme is used, any enzyme capable of cleaving such a structure may be used [11]. The enzyme is preferably selected from, FEN nuclease, Mja nuclease, native or recombinant polymerase from Thermus aquatiqus, Thermus thermophilus , or Thermus flavus , or any enzyme selected according to the teachings of Lyamichev et al [11] or U.S. Pat. No. 5,846,717, which are incorporated herein by reference. The variant position used for selection can either be removed by cleavage, or the cleavage can be performed so that the variant position is the 5′-most nucleotide of the sequence. Hence the major selective step is in the subsequent ligation reaction. The use of nucleic acid ligation for allele distinction is well described in the literature, for example [12,13]. To ensure that the cleaved substrate is eligible for ligation the 3′ sample nucleotide must be complementary to the added template. This can be achieved directly from cleavage of the sample, in which case it is possible to ligate the DNA directly.
[0019] Another approach, which confers increased specificity, is to construct the added template so that it contains one extra nucleotide, giving a gap between the hybridised 3′ and 5′ sequences, similar to that observed for the SNP. By adding only the complementary nucleotide to the cleavage reaction a substrate for cleavage will only be generated from nucleic acid sequences that contain the complementary nucleic acid sequence.
[0020] Yet another approach is to construct the added template so that there will be a gap. This gap may be filled in by the addition of a complementary oligonucleotide, as shown in FIG. 2C . Optionally, this gap filling oligonucleotide can be labelled with an affinity tag, for example a specific sequence or specific molecule for subsequent affinity purification. The gap filling oligonucleotide can also be of a specific sequence to be used for circular DNA amplification as described in co-pending application PCT/SE02/01378.
[0021] Cleavage of the sample DNA can also be achieved with restriction enzymes through the addition of oligonucleotides that hybridise to the selected sequence. The 5′ cleavage site may or may not be influenced by the variable sequence. Circularisation and selection is then conducted via any of the above-mentioned approaches.
[0022] Instead of circularising the DNA, the nucleic acid fragment ends can be protected via addition of protecting adapters to one or both ends based on selective addition at a variant position at at least one of the ends, as shown in FIG. 3 . Generation of the 3′ or 5′ sample ends could be achieved either through cleavage at the variable position or upstream at a generic site, as previously described. In the latter case cleavage will be performed via structure-specific cleavage as previously described. This protected linear substrate can now be enriched for, through degradation of unprotected sample using exonucleases. Selective amplification of the protected allele can be performed based on the presence of the added sequence/sequences.
[0023] It is not necessary to generate restriction sites in the sample or to denature double stranded DNA. Any number of restriction enzymes having recognition sequences located on either side but not within the sequence of interest, can be used.
[0024] Double stranded DNA can be digested at a multitude of sites with one or several different restriction enzymes. Digestion at one or several of the sites may or may not be affected by a sequence variant. If one specific sequence variant affects digestion by a restriction enzyme at a given site, only one of the alleles will become circularised upon ligation with a ligation template in the form a ligation casette. A ligation cassette consists of a pair of prehybridized complementary oligonucleotides with single stranded sequences protruding at one or both ends to form a correct ligation site for the choosen sequences to be ligated. Only the circularised allele becomes a template for circular amplification by e.g. rolling circle amplification. If the sample is kept double stranded throughout the process the RCA amplified allele will be the only single stranded DNA in the sample. This single stranded DNA can then be genotpyed by a single strand specific genotyping method such as, including by way of example only, padlock probes, oligonucleotide ligation assay or invader assay. The principle of specifically generate only a subset of a sample single stranded can be utlized with any method capable of performing such an action and is not to be limited to the one mentioned. Subsequent analysis with single strand specific methods reveals the genotype of only the selected, and thus single stranded sequence.
[0025] In one version an exonuclease is added to make one or both ends of a restriction enzyme digested double stranded sample partially single stranded before circularization. A choosen specific sequence is circularized, templated by an added oligonucleotide or pairs of oligonucleotides either directly or via a structure-specific enzyme cut, as described above, followed by specific ligation. The strands are then gap-filled, followed by DNA ligation. Only the correct allele can be made into a complete circle possible to amplify with RCA.
[0026] A further variant to generate single stranded DNA from a restriction enzyme digested of a double stranded sample is to specifically degrade only one of the strands with exonucleases. This can be achieved, by way of example only, through making a proper choice of restriction enzymes that will produce a sticky end that is not a substrate for the chosen exonuclease or exonucleases; or via DNA ligation adding a protecting sequence to one or both of the ends; or via DNA ligation add a chemically modified and protected sequence to one or both of the ends. The single stranded DNA can then be circularized, either directly via specific ligation or via a structure-specific enzyme cut followed by specific ligation as previously described.
[0027] It is also possible to circularise double stranded DNA with or without the addition of a ligation cassette, as described earlier, to make one of the strands so it can prime an RCA with the intact circularised strand as template. After a predefined time the polymerase is inactivated and an oligonucleotide complementary to a specific part of the amplification product is added so that it creates a restriction enzyme site in one of the alleles. After restriction enzyme digestion the digested allele is recircularised, according to the description in co-pending application PCT/SE02/01378, making it resistant to exonuclease degradation. After exonuclease treatment, serving to degrade all linear nucleic acids and thereby avoiding branched amplification of the non-circularized allele, a second generation RCA is conducted, primed with a second oligonucleotide, effectively amplifying only the circularised allele.
[0028] The enriched sample can be subjected to genotyping through any method and compared to results from genotyping of the total sample. Examples of methods which may be used are oligonucleotide ligation assays [12], padlock probes [13], primer extension assays [14], pyrosequencing [15], invader technology[16], mass-spectroscopy [17] or homogenous PCR methods e.g. Taqman [18] or molecular beacons [19]. However, other methods may be employed with equal utility. By using the enriched sample instead of a whole sample as the test sample it is also feasible to use any suitable method-, to find new/unknown mutations or polymorphisms. Thereby all possible mutations in the enriched segment may be detected, also unknown ones, for example by Sanger sequencing or by hybridising the enriched sample to an array in order to resequence the sample and in this respect also find new or unknown mutations. The methods could be, but are not limited to the use of, mismatch recognising enzymes for example T4 endo VII [20], DHPLC resequencing, Sanger or array, or pyrosequencing [15]. However, other methods may be employed with equal utility. The resulting genotypes will reveal the specific haplotype of the sample.
[0029] Accordingly, the present invention provides one or several sets of probes. A first set of probes/probe direct site specific cleavage at predetermined sites of the sample upon hybridisation. A second set of probes/probe is used to specifically modify the sample based upon a sequence variant. A third set of probes is used for amplification of the sample and a fourth set of probes is used for scoring the genotypes.
[0030] Instead of investigating the genotypes all along the selected nucleic acid one can use the same principle for genotyping the variant position used for selection. Upon cleavage of sample DNA an oligonucleotide can be added that anneals to the 3′ end of a generated fragment and to a stretch upstream, around the variant position to be scored, so that a probe with a hybridising region at its 5′ end is formed, (as shown in FIG. 4A ), or a probe with a non-hybridising region at its 5′ end is formed, (as shown in FIG. 4B ). If necessary this structure can then be cleaved as previously described. The use of ligase will complete the nucleic acid circle. The circle can then be enriched for, using exonuclease treatment and nucleic acid amplification, preferably rolling circle amplification. Preferentially the oligonucleotide added contains a sequence between the 3′ and the 5′ hybridising end that consist of a selected sequence used for later hybridisation that can be rendered double stranded through the addition of a second oligonucleotide, shown in FIG. 4A as object 1 . The added oligonucleotide could contain a recognition sequence for a type IIs restriction enzyme and preferably a sequence as dissimilar as possible compared to other oligonucleotides used for other loci, as described in co-pending application PCT/SE02/01378, the contents of which are incorporated herein by reference. Detection of the circularised nucleic acid or amplification products templated by the circularised nucleic acid is used to score the genotype of the selected position.
[0031] Due to the intramolecular nature of the ligation reaction it is feasible to perform many reactions at the same time (from one to several tens of thousands). At any practical concentration the fragments will circularise intramolecularly in preference to intermolecular reactions.
[0032] Accordingly, the present invention further provides one or a set of probes. A first set of probes/probe directs site-specific cleavage at predetermined sites of the sample upon hybridisation. A second set of probes/probe is used to specifically modify the sample based upon a sequence variant. A third set of probes is used for amplification of the enriched sample.
[0033] The variant position could be, but is not limited to a sequence variant polymorphism which may be selected from the group including any one or more; deletion variant, insertion variant, sequence length variant, single nucleotide polymorphism, substitution variant, paralogous or orthologous nucleic acid sequences, edited sequences or splice variants.
[0034] The present invention is also to be used as a mean to isolate and enrich for a specific sequence or sequences among a multitude of sequences, with the intention of further manipulation of the enriched sequence/sequences. The methods could be any, sole or a combination of but not limited to, amplification, quantification, sequencing, variant scoring, using the enriched sequence/sequences as probes or to compare different enriched samples on the basis of for example amount of sample.
[0035] Accordingly, the present invention further provides one or a set of probes. A first set of probes/probe directs site specific cleavage at predetermined sites of the sample upon hybridisation. A second set of probes/probe is used to specifically modify the sample based upon a nucleotide sequence. A third set of probes is used for amplification of the enriched sample.
[0036] In all of the above-mentioned methods where DNA samples are mentioned they could be exchanged with RNA or cDNA samples.
[0037] An added oligonucleotide probe can also be treated by the same principles and to be used for subsequent genotyping, as shown in FIG. 5 , if the added oligonucleotide anneals forming a non-hybridising region at the 5′ end. Cleavage of this structure will generate a molecule that can be circularised with a ligase. Ligation will depend on whether the 5′ nucleotide is matched or not with the sample. This circularised probe can then be detected either directly or via the presence of amplification products (based on the presence of the circle or amplification products of the circle). The presence of such a product describes the nature of the variant position. The added oligonucleotide could preferentially contain a molecule or sequence in the 5′ part that is used as an affinity tag for removal of unmodified circles before amplification of the circularised probes.
[0038] Accordingly, the present invention provides one or a set of probes. A first set of probes to be specifically modified based on the nature of a nucleotide in the target nucleic acid. A second set of probes could be used for purification of the sample. A third set of probes is used for amplification of the modified probes.
[0039] Embodiments of the invention will now be described in greater detail, by way of example only not in any way to limit the invention, with reference to the accompanying drawings, of which;
[0040] FIG. 1 is a schematic representation of cleavage and circularisation of sample nucleic acid through the use of adapters;
[0041] FIG. 2 is a schematic representation of structure specific cleavage for circularisation of sample nucleic acids;
[0042] FIG. 3 is a schematic representation of addition of protecting ends to a linear nucleic acid sample;
[0043] FIG. 4 is a schematic representation of the use of gap-oligonucleotides for circularisation of sample nucleic acids;
[0044] FIG. 5 is a schematic representation of scoring SNPs through circularisation of nucleic acid probes;
[0045] FIG. 6 shows (A) the result from a real-time PCR experiment and (B) the gel of the same amplification reactions from an experiment of cleaving, ligating and rolling circle amplification of BAC DNA;
[0046] FIG. 7 is a schematic representation (A) of the experimental set-up for detection of circularisation of nucleic acids via inverse PCR and (B) a photo of an agarose gel showing the result of such an experiment where BAC DNA cut with FokI adapters, circularised with ligase, circular molecules enriched for via exonucleases and finally used for template in an inverse PCR reaction;
[0047] FIG. 8 is showing an image of a poly acrylamide gel of radioactive labelled nucleic acids showing cleavage and ligation of structure specific cleaved nucleic acids with native DNA Taq polymerase and Tth ligase; and
[0048] FIG. 9 is showing a photo of an ethidium bromide stained gel of amplification products obtained from an experiment with cleaved BAC DNA that had been circularised via cleavage by a structure specific enzyme and the two ends joined by a ligase.
EXAMPLES
Example 1
[0049] Circularisation of DNA after cleavage with restriction enzymes followed by enrichment through exonuclease treatment and rolling circle amplification. (See FIG. 4 )
[0050] A BAC clone (RP11-381L18, BacPac resources, Children's hospital, Oakland) with a genomic fragment containing the gene ATP7B was used. DNA was isolated by the rapid alkaline lysis miniprep method and the DNA concentration was determined measuring UV A 260 .
[0051] HpaII 5 U (New England Biolabs) was used to cleave a double stranded (ds) template in buffer (10 mM Tris-HCl pH 7.5, 10 mM MgCl 2 , 1 mM DTT) for 2 hours at 37° C. before heat-inactivation of the enzyme. Two pmol of the ds template was cleaved with HpaII. After the cleavage, the reaction was diluted to different concentrations (10 4 -10 8 molecules/μl).
[0052] The template was ligated into a circle using 0.5 units of T4 DNA ligase, 1×T4 DNA ligase bf (66 mM Tris-HCl pH 7.6, 6.6 mM MgCl 2 , 10 mM DTT, 66 μM ATP) and 10 nM ligation template, 5′Biotin-tt ttt ttt ttt ttt gtc tgg aaa gca aac cgg tgc cca ccc atg a 3′ SEQ ID NO1, in each reaction. After denaturation and subsequent addition of ligase to half of the reactions (see below), the samples were incubated at 37° C. for 30 min and then the ligase was heat-inactivated at 65° C. for 20 minutes
[0053] After ligation, the samples were treated with exonucleases. Exonuclease V (5 units) was used for 30 min 37° C. before heat-inactivation. The result was detected by performing a PCR with the following primers, 5 acg ccc acg gct gtc at 3′ SEQ ID NO2 and 5′ tgg acg tct gga aag caa a 3′ SEQ ID NO3, (1 μM) located on both sides of the ligation junction. In 50 mM Tris HCl pH 8,3, 50 mM KCl, 200 μM dNTP, 0.125 u Taq GOLD polymerase (Perkin Elmer), 0.08×SYBR Green (Molecular Probes) as reporter molecule, and 1xROX (Molecular Probes) as standard, temperature cycles as follows 95° C. 10 min activation of Taq polymerase followed by 40 cycles of 95° C. 20 sec, 52° C. 1 min, 72° C. 20 sec. The experiments yield a cycle threshold value, Ct which is inversely proportional to the amount of starting material in the sample.
[0054] After the PCR amplification the reactions products were electrophoresed in a 3% agarose gel to ensure that a product of the correct length had been produced.
[0055] The results are shown in FIG. 4 , where A) Graph showing the fluorescence readings from a real-time PCR experiment read in an ABI 7700. The figures to the left corresponds to the numberings in B. Reactions were as follows; #2,3—No template control, #4 sample+ligase, #5 Sample−ligase, #6 sample+ligase+RCA, #7 Sample—ligase+RCA
[0056] B) A 3% agarose gel of the PCR reactions shown in A. Lane 1 in B is loaded with a 100 bp-ladder (lowest band around 50 bp). Lane 2-7 corresponds to the same reactions. The arrow denotes the size for a correct length product.
Example 2
[0057] Enrichment of circular DNA over non-circular DNA through the use of different exonucleases.
[0058] BAC DNA as described in example 1 were cleaved and ligated as described in EXAMPLE 1. Half of the sample was ligated with T4 DNA ligase and half of the sample was not. The two reactions were further divided into five different reactions of each (+/−ligase) treated as follows.
1 5 u ExoV and 1 mM ATP, 2. 5 u ExoI, 50 u ExoIII and 25 u T7gene6 3. 5 u ExoI 50 u ExoIII and 2,45 u Lambda exo 4. 50 u ExoIII, 0,5 u ExoVII and 2,45 u Lambda Exo 5. 5 u ExoI, 0,5 u ExoVII in 1×Tris buffer
[0064] All reactions were incubated at 37° C. for 30 minutes before heat inactivation of the nucleases at 80° C. for 20 minutes. The results were determined as described in example 1. After the PCR amplification, the reaction products were electrophoresed in a 3% agarose gel, and the nucleic acid visualised to ensure that a product of the correct length had been produced (not shown). The results are shown in table 1.
TABLE 1 Shows the result from an exonuclease treatment of cleave DNA that had been or had not been circularised with ligase. Exo treatment: +ligase: Ct value −ligase: Ct value ExoV(5 U) + ATP(1 mM) 24.49 35.82 ExoI (5 U) + ExoIII (50 U) + 21.33 33.52 T7Gen6 (25 U) ExoI (5 U) + ExoIII (50 U) + 21.52 35.07 λExo (2.45 U) ExoIII (50 U) + ExoVII 22.85 35.70 (0.5 U) + λExo (2.45 U) ExoI (5 U) + ExoVII 28.05 34.70 (0.5 U) + 1× Tris bf
Example 3
[0065] Circularisation of DNA after denaturation of dsDNA, hybridisation of FokI adapters, cleavage of the DNA at predetermined sites, specific circularisation of the cleaved fragment based on an SNP at the 5′prime end and enrichment of the circularised DNA. (See FIG. 7 )
[0066] BAC DNA was purified as described in example 1.
[0067] BAC DNA was diluted in a series and denatured by heat. After denaturation the samples were directly put on ice.
[0068] Different amounts (10 1 -10 10 molecules) of BAC DNA were cleaved with 2 units FokI and 2 fmol FokI adapters (FokI adapter 5′UTR 5′ cgc atc cca cgt ggg atg cga aag caa aca ggg gt 3′ SEQ ID NO 4, FokI adapter C2930T C-allele 5′ gcc atc cgt gca cgg atg gct gca cag cac cgt gat 3′ SEQ ID NO5, FokI adapter C2930T T-allele 5′ gcc atc cgt gca cgg atg gct gca cag cac cat gat 3′ SEQ ID NO6) in 10 mM Tris-HCl pH 7.5, 10 mM MgCl 2 , 1 mM DTT, 50 mM NaCl, 1 xBSA1 for 2 hours 37° C. before heat-inactivation of the enzyme.
[0069] The ends of the generated fragment nucleic acid were ligated into a circle using 8 fmol of the correct/incorrect ligation template (20+20 WDgDNA 5′UTR-Ex13 C-allele, 5′ ctc ggc tct aaa gca aac agg tga tgg acg tct gga aag ctt t 3′ SEQ ID NO7, 20+20 WDgDNA 5′UTR-Ex13 T-allele 5′ ctc ggc tct aaa gca aac aga tga tgg acg tct gga aag ctt t 3′ SEQ ID NO8). One unit T4 DNA ligase and 1×T4 DNA ligase buffer was used, and the reactions were incubated for approximately 30 minutes at 37° C. before heat-inactivation of the DNA ligase. The circles were exonuclease treated with 5 units ExoV and 1 mM ATP and the samples were incubated in 37° C. for 30 min before heat-inactivation at 80° C. for 20 minutes.
[0070] PCR amplification was performed with primers (Frw WDgDNA 5′UTR-Ex13 5′ cag agg tga tca tcc ggt ttg 3′ SEQ ID NO9, Rew WDgDNA 5′UTR-Ex13 5′ gga gag gag gcg cag agt gt 3′ SEQ ID NO10), 0.5 μM of each, located on both sides of the ligation junction. With a total volume of 50 μl, 200 μM dNTP, 1 unit Taq GOLD polymerase, 1×PCR buffer (10 mM Tris-HCl pH 8.3, 50 mM KCl, 1.5 mM MgCl 2 , 0.001% (w/v) gelatine). 40 amplification cycles were run after activation of the polymerase: 95° C. 15 sec, 58° C. 1 min and 72° C. 20 sec. The amplified nucleic acids were detected by electrophoresis in a 3% agarose gel and visualisation by staining with ethidium bromide.
[0071] The results are shown in FIG. 6B . The following samples were loaded into the different lanes; 1—Marker, 2 No template control, 3-8 samples from a 10-fold dilution series (10 10 -10 1 ) of BAC DNA with correct ligation template and ligase, 9 sample with correct ligation template but minus ligase, 10-12 samples from a 10-fold dilution series (10e10 to 10e9) with a ligation template corresponding to the wrong allele, T instead of C). The arrow denotes the size of a correct length product.
Example 4
[0072] Selective ligation of oligonucleotides cleaved with a structure specific enzyme. (See FIG. 8 )
[0073] The reactions were performed in 1×Tth buffer (1 mM NAD, 10 mM DTT and 0,1% Triton X-100). 20 μl reactions containing 0.5 pmol of the upstream, downstream and target oligonucleotides respectively (primer22+1 5′ gta ttt gct ggg cac tca ctg ca 3′ SEQ ID NO11, ArmC 5′ tcc aga cgt cca tca cgg tgc tgt gca ttg cct g 3′ SEQ ID NO12 or ArmT 5′ tcc aga cgt cca tca tgg tgc tgt gca ttg cct g 3′ SEQ ID NO13, Template2930 5′cag gca atg cac agc acc gtg cag tga gtg ccc agc aaa tac3′ SEQ ID NO14), 1 unit of Tth ligase and native Taq polymerase. The reactions were prepared on ice and initiated by transfer to a Thermal Cycle where the following program was run: 95° C. 20 sec, 72° C. 30 min for 2 cycles. The upstream or downstream oligonucleotide was radio labelled and the samples were analysed on a 10% denaturing polyacrylamide gel. Ten pmol target DNA was end-labelled with 1.65 pmol γ- 32 P dATP (NEN). 4.9 U T4 PNK enzyme and 1×T4 PNK buffer (0.05 M Tris-HCl pH 7.6, 10 mM MgCl 2 , 10 mM 2-mercaptoethanol) was added to each labelling reaction and the tubes were incubated for 45 min in 37° C. EDTA (1 mM) was added and the samples were boiled for 5 min in a water bath. The unincorporated nucleotides were removed from the labelling reaction with a MicroSpin™ G-50 column (Amersham Pharmacia Biotech).
[0074] The experiments with the radio labelled oligonucleotides were detected on a 10% polyacrylamide gel containing 7 M UREA. The gel was run with 0.5×Tris Borat EDTA buffer at 30 W for approximately 30 min and was dried in a gel dryer for 2 hours 80° C. The dried gel was exposed to a phosphorimager screen overnight.
[0075] The results are shown in FIG. 8 . Oligonucleotides yielding structure A was used in experiments 1-6 and oligonucleotides yielding structure B was used in experiments 7-12. (i) denotes the size of un-reacted oligonucleotide in experiments 1-6, (ii) the size for ligated product in reactions 1-6, (iii) uncleaved oligonucleotide used in reactions 7-12 and (iv) cleaved oligonucleotide in reactions 7-12. 32P denotes a radioactive label on respective oligonucleotide.
[0076] Lanes 1-6 shows the results from experiments with oligonucleotide 1 labelled with 32 P. Lane 1, T-allel (wrong)—Taq polymerase, lane 2 C-allel (correct)—Taq polymerase, lane 3 T-allele—Tth ligase, lane 4 C-allel—Tth ligase, lane 5 T-allel, lane 6 C-allele.
[0077] Lanes 7-12 show the results from experiments with oligonucleotide 2 radio labelled with P 32 Lanes 7, 9, 11 is with the T-allele (incorrect) and lane 8,10,12 is with the C-allele (correct). Lanes 7-8 minus Taq polymerase, lanes 9-10 minus Tth ligase.
[0078] Lane 13 shows size markers.
Example 5
[0079] Circularisation of BAC DNA after cleavage with restriction enzymes, intramolecular hybridisation and cleavage with a structure specific enzyme followed by ligation, as shown in FIG. 9 .
[0080] BAC DNA was purified as described in example 1.
[0081] Denatured, ss BAC DNA (1×10 10 molecules) was cleaved with 10 units DraIII in buffer (10 mM NaCl, 5 mM Tris-HCl, 1 mM MgCl 2 , 0.1 mM DTT pH 7.9) was used. DraIII was allowed to cleave the DNA for 1 hour 37° C. before heat-inactivation.
[0082] This experiment was also done with genomic DNA. 10 10 molecules were cleaved by 1 pmol of each adapter (cleave DraIII up2930 5′ act gga cac aac gtg acg aac ttg ggt 3′ SEQ ID NO15 and cleave DraII down2930 5′ cag ggc tca cac gca gtg agt gcc c 3′ SEQ ID NO16) designed to hybridise to sequences in exon 13. The subsequent concerted structure-specific cleavage and ligation reaction contained the same reagents as above and 2 pmol of ligation any of two different templates (20+20 DraIII-C 5 ′ taa acg acc cgt gag tga cgc aca ggt cac ggg ggg ac 3′ SEQ ID NO17 or 20+20 DraIII-G 5′ taa acg acc cgt gag tga cgg aca ggt cac ggg ggg ac 3′ SEQ ID NO18). The samples were divided into two parts and on one half was subjected to a RCA. A real-time PCR was performed on the samples with primers located on both sides of the ligation junction. In a total volume of 50 μl the following reagents were included: 2.5 μl sample, 1×PCR bf, 100 μM dNTP, 1 unit Taq GOLD polymerase, 0.5 μM of each primer, 1×ROX and 0.08×SYBR. After activating the polymerase 95° C. for 10 min, 40 cycles of the following program was run in a Thermal Cycler: 95° C. 20 sec, 58° C. 1 min and 72° C. 30 sec.
[0083] DraIII and specific adapters designed to hybridise to sequences in exon 13 of ATP7B cleaved BAC DNA at predetermined sites. The target DNA was denatured to become single-stranded and the adapters were designed to create recognition and cleavage sites for DraIII. DraIII cleavage created a substrate that was used in the structure-specific cleavage, which generated the 5′ located SNP.
[0084] The results are shown in FIG. 8 . Shown is the samples run on a 3% agarose gel. Lane 1 is a size marker, lane 2 and 3 PCR no template controls, lane 4 sample, lane 5 without Taq polymerase, lane 6 without Tth ligase and lane 7 without BAC DNA.
REFERENCES
[0085]
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5. Liu Q, Thorland E C, Heit J A, Sommer S S: Overlapping PCR for bidirectional PCR amplification of specific alleles: a rapid one-tube method for simultaneously differentiating homozygotes and heterozygotes. Genome Res 1997, 7:389-398.
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16. Lyamichev V, Mast A L, Hall J G, Prudent J R, Kaiser M W, Takova T, Kwiatkowski R W, Sander T J, de Arruda M, Arco DA, et al.: Polymorphism identification and quantitative detection of genomic DNA by invasive cleavage of oligonucleotide probes. Nat Biotechnol 1999, 17:292-296.
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This invention relates to methods, reagents and kits for enriching nucleic acid sequences. More particularly, the present invention relates to methods, reagents and kits for sample preparation including sample modification, sample enrichment and amplification
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. application Ser. No. 10/938,990, filed on Sep. 9, 2004, and titled “I NTELLIGENT M EMORY D EVICE WITH ASCII R EGISTERS ”, which application claims priority to prior U.S. Provisional Patent Application Ser. No. 60/540,671, filed Jan. 29, 2004 and titled “I NTELLIGENT M EMORY D EVICE A RCHITECTURE ,” which application is hereby incorporated by reference into the instant application.
[0002] This application is related to U.S. patent application Ser. No. 10/831,649, filed Apr. 23, 2004 and titled “I NTELLIGENT M EMORY D EVICE ”, docket number 372614-04301, now U.S. Pat. No. 7,594,232, which application is hereby incorporated by reference into the instant application.
FIELD OF THE INVENTION
[0003] The present invention relates generally to computer design and computer architecture and more specifically to a new class of multi-tasking, multi-processor systems.
DESCRIPTION OF THE RELATED ART
[0004] The three major problems facing computer designers today involve (i) memory latency; (ii) multi-processor co-ordination; and (iii) compiler complexity. Intelligence, in the classical computer architecture, is located in a Central Processor Unit (CPU) or CPU array, while working storage is located in non-intelligent memory devices. Over time a vicious cycle has evolved in which operating system designers have expected faster processors and larger working memories and have designed operating systems (OSs) and associated compilers to take advantage of these improved processors and memories.
[0005] However, a dichotomy exists between random logic gates of a CPU and arrays of logic storage gates in a memory, because each physically evolved in specialized manner, due to different manufacturing optimizations. The interface between logic and memory limits current processor architecture. Attempts to minimize this problem have driven both CPU and memory design for a decade or more. Approaches to this include: (i) cache memories and pipelining; (ii) faster interfaces, such as those used in RDRAM or SRAM; (iii) on-chip memory integration; (iv) use of multi-threaded processors; (v) use of co-processors; and (vi) language improvements.
[0006] Each of these approaches is discussed below. Memory latency arguments focus on single processors, but apply to multi-processors, since memory latency is typically independent of the number of processors accessing memory.
Pipelining
[0007] Because memory technology and processor/logic manufacturing technology evolved separately, large capacity memories cannot be integrated with high speed processors on one die, so the two have classically been packaged separately and wired together. The distances and capacitances associated with this wiring involve access delays many times those involved in on-chip access. An early approach to this problem involved “pipelining,” in which several registers were inserted in the path and attempts were made to keep filling the pipeline while the processor drained the pipeline. A problem with this approach is branching wherein the pipeline must be flushed and refilled at the branch target location.
Cache Memories
[0008] Pipelines evolved into on-chip cache memories to provide much faster access. By operating from cache memory, the processor can operate at full speed, until a branch occurs to a location not in cache. Probably the most prevalent strategy today is multi-level cache, with the fastest caches being the smallest and closest to the processor. For example, the Intel Itanium's level-three (L3) cache memory is too small to store lots of large pointers so it uses up to 32 Mbytes of level-two (L2) cache. Very large operating systems (OSs) try to run code from the same base address, causing aliasing problems in caches and flushes. In general, processor performance is limited by memory latency. It has been pointed out that, in the future, at 5 to 10 GHz CPU operating frequencies, a DRAM access is several thousand clock cycles. What is a processor to do during these cycles?
[0009] Of course, the obvious answer is make memory devices faster. Yet as long as the CPU and memory technologies differ, the devices will be on separate die. At high speeds, parallel busses cannot remain synchronized, so super high frequencies are used in a single serial channel. For example, the Rambus XDR™ interface is projected to hit the 6 Gigabit rate by 2006. Nevertheless, memory latencies will never be zero and the problem will not be completely solved via faster memory.
On-Chip Memory Integration
[0010] With the inability to solve the “off-chip latency problem” one might expect that “on-chip” memory provides a solution. However, due to the separate evolutionary paths taken by CPU and memory manufacturing technologies, this is unlikely to occur soon. The “off-chip” approach provides the ability to use as little or as much memory as is appropriate, unlike the “on-chip” solution where memory size is fixed. Although, in theory, many different sizes could be manufactured, the multi-million dollar, exponentially increasing costs of masks argues against this, even if the technology were feasible. System-on-Chip (SOC) devices do use on-chip, generally distributed, memory, however these devices are typically designed for cameras, cell phones, or other applications in which a fixed size of memory is feasible. SOC-relevant measures of optimality tend to be power consumption, not high speed, so this does not solve the general purpose CPU problem, which is based on the fact that CPU address space can always exceed on-chip memory capacity.
Multi-Threaded Processors
[0011] Another architectural approach to latency is multi-threading, in which programs are treated as ‘threads’ or loci of execution that are essentially independent of each other. When one program stalls due to memory latency, the CPU switches to execute a different thread while the first thread's cache is being refilled in an attempt to mask the effects of memory latency. Not every one agrees with this approach. Intel added multi-threading to the 386 architecture, but 386-compatible manufacturers, such as VIA and Transmeta, argue: “Multi-threading is an admission you can't keep the pipeline full” and Advanced Micro Devices, another 386 manufacturer says: “ . . . putting multiple cores on a die will become a more important trend than multi-threading individual processors.”
[0012] Some CPU manufacturers have introduced hardware multi-threading. For example, MIPs offers two approaches: In the first, a hardware thread manager controls which thread is running on the CPU, while the second approach uses application-level thread support, in which the operating system must keep track of the threads. The latter is compatible with thread-friendly languages such as Java, while the first may be more appropriate to programs that do not understand the thread concept. Automatically switching between threads can clobber shared resources, such as Floating-Point Computation Units, whose state typically must be saved and restored when task-switches occur. This assumes that computational resources are required only for the single thread, since true multi-tasking use of multi-register FPUs typically require complete register bank save/restore upon each task switch, and thus would appear to defeat hardware multi-threading. MIPS implies this is true by arguing that DSP hardware coprocessors are used, not because CPU instructions cannot perform the computations, but because single thread CPUs, even with real time OS, cannot guarantee hard real-time deadlines. Multi-threading allows one thread to receive a minimum percentage of CPU cycles, such that the critical task essentially runs its own virtual CPU.
[0013] Another manufacturer, Ubicom, uses a proprietary 32-bit general-purpose processor with hardware support for up to eight threads, multiple register sets, a hardware Scheduler unit and hardware allocation table to drive the Scheduler unit. By switching between register sets, the device achieves zero cycle context switching. Instead of saving and restoring register contents for each thread, each thread simply works with its own dedicated register set. Ubicom does not include FPUs, so the associated context switch problems are avoided.
Use of Coprocessors
[0014] Yet another approach to memory latency is via the use of co-processors. These have classically been I/O-oriented such as UARTs and USB controllers, Ethernet controllers, digital signal processors, disk controllers and the like.
[0015] Several recent approaches to off-CPU processing do not relate to I/O. The NanoAmp JAVA Accelerator, a coprocessor that executes JAVA byte codes, sits between the processor and memory and allows an immediate pass-through mode to allow CPU access to memory. When the accelerator is operating, it feeds the host CPU instructions to keep it occupied in a polling loop, monitoring the status of the coprocessor. This closely coupled mechanism is appropriate to a CPU executing a Java program, and very little else, since a polling processor is doing no useful work.
[0016] In contrast, the Cybernetic Micro Systems P-51 device provides a memory interface to an 8051 CPU that is seen as memory by the host CPU, while running general purpose programs in support of the host (See U.S. Pat. No. 6,021,453, titled “Microprocessor Unit For Use In An Indefinitely Extensible Chain Of Processors With Self-Propagation Of Code And Data From The Host End, Self-Determination Of Chain Length And ID, (And With Multiple Orthogonal Channels And Coordination Ports”, and U.S. Pat. No. 6,219,736, titled “Universal Serial Bus (USB) RAM Architecture For Use With Microcomputers Via An Interface Optimized For Integrated Services Digital Network (ISDN)”). The advantage is that memory now becomes useful for processing data, not just storing data. The coupling between host CPU and coprocessor can be coupling via an interrupt signal line or memory mailboxes and is not limited to Java or any other type of program or program language. Programs must be specifically written to take advantage of such a coprocessor.
[0017] In a similar vein, Micron Technology has described the “Yukon,” an array of memory Processing Elements to off-load the CPU. The pilot chip has arithmetic logic units with registers to improve a software pipeline to move data between the ALUs and on-chip DRAM. The Micron “Yukon” and Cybernetics “P-51” devices are the prior art believed closest to the invention described herein.
Other Solutions
[0018] Two other approaches to the problem have been suggested by Stanford University and UC Berkeley. Although Berkeley calls their approach “intelligent RAM,” this is a misnomer. They essentially integrate the CPU and RAM memory on the same die, as discussed above. “The devices are called IRAMs because most of the transistors on the merged chip will be devoted to memory.” So they think of the processor as being added to memory as opposed to the memory being added to the processor. This is semantical wordplay and has no relation to the “intelligent memory architecture,” iMEM, described herein. Similarly, the Stanford approach includes a standard (MIPs) CPU on a chip with multiple floating point units and supporting register files. This also falls under the “SOC on-chip integration” concept, and is unrelated to the iMEM architecture of the current invention.
Languages
[0019] The above discussion focuses on the memory latency problem. iMEM is designed to ameliorate this problem, and problems associated with computer languages, such as: Assembly, Fortran, BASIC, Pascal, APL, C, C++, Forth, Java and associated compilers.
[0020] When computers were invented, memory elements (flip/flops) typically cost $100 per vacuum tube-based bit. Economics dictated binary encoding, as instructions were encoded and interpreted as efficiently as possible. For perspective we should note:
[0021] In 1971, the first computer-on-a-chip had about 1,500 gates; In late '80s, the average ASIC size was about 10K gates; In mid '00s, the average ASIC size was about 10M gates; and
[0022] In mid '00s, the current CPU size will be about 100M gates.
[0023] Today, with millions of logic gates and memory bits available on a chip for about $10, one must ask why binary encoding is still in use. Probably the main reason is the large number of software tools available for converting ASCII-coded programs into binary executables. As long as processors require binary executables, this is the way things will be done. In light of this history, one might ask “why ASCII?”; the more appropriate question is “why not ASCII?” The world-wide communication system, the Internet, is ASCII based; the universal data scheme, XML, is also ASCII; and all user programmable computers are typically programmed in ASCII (or the UNICODE superset) and then converted to binary instructions and/or data. Why do we need this conversion process? Coding should, by default, be ASCII, unless there is a good reason for binary encoding. Therefore, the preferred implementation of iMEM hardware is ASCII encoded, although iMEM architecture is completely compatible with a binary implementation. The primary tool for ASCII encoded hardware is an ASCII text editor.
[0024] Computer operating systems arose from the same historical economics that necessitated computer languages and compilers. Early OSs managed binary communications and mass storage and scheduled programs for execution. Later OSs supported multi-tasking, when more than one program needed to run “simultaneously.” The same arguments that apply to ASCII vs. binary encoding apply to multi-tasking, and again to multi-processing. When tens of millions of gates are available for design, there is no reason to design processors in the same way that they were designed when only thousands of gates were available. As is described below, iMEM architecture is intended to address the memory latency, multi-processor coordination, and compiler complexity problems.
BRIEF SUMMARY OF THE INVENTION
[0025] A computing system in accordance with the present invention includes one or more Processing Elements, a memory with two interfaces, and a multi-task controller. The multi-task controller includes a Scheduler unit, a Dataflow unit, an Executive unit, and a Resource Manager unit.
[0026] The memory has a first interface for connecting to a host processor and a second interface and the memory being divided into a plurality of logical partitions, where each partition having a range of memory addresses and at least one partition has information describing a particular task. The information includes contents of task state register and one or more task data registers, and each task data register has an ASCII name. Each of the units of the multi-task controller (MTC) is separately coupled to each of the other units and the Dataflow unit is configured to transfer data between the second interface of the memory and one of either the Scheduler unit, the executive unit, or Resource Manager unit. The dataflow unit is also configured to manage a mapping between registers with ASCII names and the memory addresses of a particular task. The Scheduler unit is coupled to the second interface of the memory and to the Processing Elements, the Dataflow unit is coupled to the second interface of the memory, and the Resource Manager unit is coupled to the one or more Processing Elements. The Resource Manager unit is configured to find an available Processing Element for carrying out a function of a task and to assign a Processing Element to a current task by providing a linkage between said available Processing Element and the task. The Scheduler unit is configured to select a task as the current task, to obtain the state of the current task, and select an assigned Processing Element to carry out a function of the current task. The Executive unit is configured to decode ASCII-encoded instructions relating to a task and request the Resource Manager unit to set up a processing element to carry out a function of a task. The number of Processing Elements and number of tasks are independent of each other.
[0027] A method in accordance with the present invention is a method of processing one or more tasks using one or more processing elements coupled to a multi-task controller, where the multi-task controller is coupled to a memory at a first interface and a host processor is coupled to the memory at a second interface. The method includes selecting, from the memory via the first interface, a next task for execution, where the task has a stored state and a sequence of ASCII-encoded task instructions and obtaining the stored state for the selected task. For a task in a ‘Ready_to_execute’ state, the method includes accessing the next task instruction in the sequence. If the task instruction is ‘request_resource’ instruction, the method includes generating appropriate signals, setting the task state to ‘Wait_for_resource’, and proceeding to the step of selecting a next task. If the task instruction is a ‘perform_processing’ instruction, the method includes loading the relevant task data into the processing element, activating the processing element, linking the processing element to the task, setting the task state to ‘Wait_for_response’, and proceeding to the step of selecting a next task. If the task instruction is a ‘transfer_result’ instruction, the method includes unloading the result from the processing element, copying to the relevant task data register, and setting the task state to ‘Ready_to_execute’. If the task instruction is a ‘signal_host’ instruction, the method includes generating the appropriate signal to the host, setting the task state to ‘Suspend’, and proceeding to the step of selecting a next task. If the ASCII-encoded task instruction specifies a non-processing operation to be performed, the method includes performing the specified non-processing function, and setting the task state to ‘Ready_to_execute’. For a task in the ‘Wait_for_resource’ state, the method includes waiting until a processing element is available to perform a function of the selected task and setting the task state to ‘Ready_to_execute.’ For a task in the ‘Wait_for_response’ state, the method includes determining whether or not a response is available from the linked processing element, and setting the task state to ‘Ready_to_execute,’ and if a response is not available, setting the task state to ‘Wait_for_response.’ For a task in a ‘Suspend’ state, the method includes waiting for the host processor to set the task state to ‘Ready_to_execute’, after the host processor appropriately accesses the memory via the second interface.
[0028] Computer systems typically contain a processor subsystem, one or more memory spaces, and an I/O subsystem. Multi-processor systems simply multiply the above by an integer, with some means of coupling the processors. Since the 1970 Illiac-IV innumerable such systems have been proposed and many systems have been built, yet few are well known for solving any significant problems. There are at least two reasons for the general lack of success of such specialized multi-processor systems.
[0029] First, interconnection schemes are typically complex, involving multiple pathways and/or complex switching systems, with complex physical interconnect and associated algorithms.
[0030] Second, programming such systems is extremely difficult. Few tools exist for unique multi-processor architecture, and the tools created for classical architectures were designed for single-processor implementations, thus software hurdles are significant.
[0031] A third involves the economics of scale. If only a few, or a few hundred, such processors are to be built, they inevitably cost far more than processors manufactured by the millions. This applies to software issues also. Software written for multi-processor implementations costs at least as much as commercial software developed for mass-market processors, but is not amortized over millions of processors, as is commercial software.
[0032] Intelligent Memory is subject to none of the above problems. First, intelligent memory connection to the processor is (in the simplest case) identical to non-intelligent memory, and is thus compatible with all of today's processors.
[0033] Second, access to intelligent memory is identical to access to normal, non-intelligent, memory and therefore uses identical processor instructions and software.
[0034] Third, intelligent memory is subject to the same economies of scale as normal memory, which offers some of the greatest economic scale benefits existing today.
[0035] Fourth, the economics of scale that apply to memories are so great that memories tend to become low profit commodities. Intelligent memory, because of the added value, the intelligence, should command a premium, and therefore be commercially successful.
[0036] Fifth, in the default state, the intelligence should be disabled, and the memory should therefore be (conceptually) identical to normal memory. This has the extreme advantage of being compatible with all currently existing software, while offering extraordinary capability to new or extended software.
[0037] The chief advantage of the iMEM architecture is the distribution of intelligence across most of the silicon in a computer system as opposed to the typical and historical case in which all intelligence resides in the CPU and none in the memory. Note that both classical CPU/memory systems and CPU/iMEM systems may possess intelligent I/O such as storage or communication controllers, but these are incidental to and independent of the intelligence we are discussing.
[0038] For compute-intensive CPU operations, all data must flow from memory into the CPU, where the computations are performed, and the results must then flow back into memory. This causes the CPU/memory interface to be the system bottleneck, as has been the case for a decade or so. A large portion of current computer design consists of attacking this bottleneck problem.
[0039] In compute-intensive iMEM-based systems, the data generally do not flow across the CPU/iMEM interface, except initially, and all iMEMs can be simultaneously processing data, with occasional or appropriate results being offered to the CPU. A given memory bandwidth supports far more data processing in an iMEM system than is the case for classical memory. The actual improvement is generally linear with respect to the number of iMEM devices.
[0040] A further advantage is that iMEM hides its intelligence until it is specifically requested by the CPU. Therefore startup procedures, BIOS operations, and OS operations need not be aware that iMEM exists, providing compatibility with any and all CPU systems extant.
[0041] Typical fields of application for iMEM consist of particle-in-cell problems such as weather models, or N-body tracking problems such as protein folding or UAV airspace deconfliction, etc. These are the type of problems that are currently addressed by super computers or by mesh configurations of ordinary PCs. Super computers are very expensive, and often of fixed capacity, and may be relatively deficient in software support/tools. In fact, many recent supercomputers are comprised of arrays of commercial processors, and can be augmented by iMEM with no basic architectural changes.
[0042] iMEM, unlike super computers, provides a low cost solution, which is extendable in almost unlimited fashion, with cost of system enhancement linearly proportional to the number of iMEM devices. In addition, iMEM is closely coupled to the CPU via the standard PCI (or other) memory bus, providing orders of magnitude more speed than a mesh computer network, which is coupled via serial communications channels operating typically over miles of wiring and requiring hundreds or thousands of PCs. The use of hundreds or thousands of iMEM devices is both lower cost and higher computation speed. Additionally, the power of existing mesh computer networks can be augmented by adding iMEM to each CPU in the mesh.
[0043] iMEM requires little special software since CPU operations simply initialize the data registers and read results when appropriate. If the ASCII iMEM option is implemented programming can be performed with typical text editors with no compilation required.
BRIEF DESCRIPTION OF THE DRAWINGS
[0044] These and other features, aspects and advantages of the present invention will become better understood with regard to the following description, appended claims, and accompanying drawings where:
[0045] FIG. 1A shows a CPU and classical memory;
[0046] FIG. 1B shows CPU and iMEM architecture of the present invention;
[0047] FIG. 2A shows a CPU classical memory address space;
[0048] FIG. 2B shows a CPU-iMEM address space;
[0049] FIG. 3A shows the iMEM architectural structure and subsystems;
[0050] FIG. 3B shows the inputs and outputs of the Scheduler unit;
[0051] FIG. 3C shows the inputs and outputs of the Dataflow unit;
[0052] FIG. 3D shows the inputs and outputs of the Executive unit;
[0053] FIG. 3E shows the inputs and outputs of the Resource Manager unit;
[0054] FIG. 4 shows the iMEM task/page organization;
[0055] FIG. 5 shows a suspended task being accessed by the host CPU. If not suspended, the task executes and waits for resources and responses;
[0056] FIG. 6 shows ASCII iMEM Task Coding Structure;
[0057] FIG. 7 . shows each task status register containing eight default index registers. The index registers are represented in ASCII code by ‘h’ . . . ‘o’;
[0058] FIG. 8 illustrates the iMEM distributed ASCII interpretation architecture preferred for indexed addressing operations and additional hardware support for such index-related page addressing. Data flow paths between task memory and Processing Elements are not shown;
[0059] FIG. 9 shows the iMEM configuration parameters on system page;
[0060] FIG. 10 shows an alternative iMEM data path between memory and Processing Element that preserves iMEM task scheduling and execution architecture, while supporting appropriate data size;
[0061] FIG. 11 shows the iMEM ASCII code hierarchy. Native ASII code in task code space is interpreted by iMEM hardware. Hi-level ASCII code in task data space can be interpreted either by the native task code software or by appropriate Processing Element hardware;
[0062] FIG. 12 shows the ASCII name structure supporting single-character ASCII register names;
[0063] FIG. 13 shows iMEM ASCII code translation algorithm;
[0064] FIG. 14A shows load from data version of the iMEM Index Register architecture;
[0065] FIG. 14B shows load from address version of the IMEM Index Register architecture;
[0066] FIG. 15 shows the iMEM Task Index Register that provides compatibility with Intel 386 Global Descriptor Table architecture;
[0067] FIG. 16 shows a standalone iMEM device can support a communications channel and a program input subsystem in place of a host CPU;
[0068] FIG. 17A shows a standard CPU-hosted ‘vertical’ array of iMEMs;
[0069] FIG. 17B shows a P-51-like ‘horizontal’ array of iMEM devices which are PE-linked;
[0070] FIG. 18 shows an iMEM branching array topology with PE-linked iMEM tree;
[0071] FIG. 19 shows the preferred implementation of iMEM reconfigurable architecture which restricts reconfiguration to one or more Processing Elements;
[0072] FIG. 20 shows the preferred iMEM clock domain distribution/topology;
[0073] FIG. 21 shows a preferred iMEM ‘wakeup’ mechanism;
[0074] FIG. 22 shows the Processing Element signals and structure;
[0075] FIGS. 23A , B, C schematically shows the operation of a preferred embodiment; and
[0076] FIG. 24 shows a flow chart of the basic state transitions.
DETAILED DESCRIPTION OF THE INVENTION
The IMEM Structure
[0077] Common to all of the above attempts to solve the memory latency problem, except Cybernetic's and Micron's, is maintenance of the CPU-memory dichotomy, i.e., all of the intelligence is positioned in the processor, none in the memory. The invention described herein alters this architecture as shown in FIG. 1B . The processor characteristics include (i) autonomous processing; (ii) local memory space(s) access; and (iii) I/O channels. The memory characteristics include (i) an address bus; (ii) a data bus; and (iii) a control bus (Read, Write, Enable, Ready, etc.). The intelligent memory characteristics include: (i) an address bus; (ii) a data bus; (iii) a control bus; (iv) processing disabled by default; (v) processing enabled via the memory interface; and (vi) optional I/O channels.
[0078] The iMEM device looks like classical memory to the CPU 50 and responds as such to the CPU address 120 , control 124 , and data busses 122 . Within the iMEM, however, exists considerable intelligence 700 , with access to all data stored in memory 100 . iMEM intelligence can access memory data, assumed placed in memory by the CPU, and either interpret or operate 600 on said data. The interpreted data guides the iMEM intelligence, which typically accesses data from memory, operates on the data, and deposits the results of the operation in the memory, at the same or another location. Optionally, iMEM can signal the CPU via a READY or INTERRUPT signal. If this option is implemented, it represents another departure from classical memory, which, with no intelligence, can never signal the use of any operation other than access. Memory address space, as it appears to the CPU is shown in FIG. 2A . Memory address space as it is implemented using iMEM is shown in FIG. 2B . The host CPU treats iMEM address ranges as pages 101 , 102 , 103 , etc. that possess structure and that are linked to processors 201 , 202 , 203 . However, CPU only accesses memory; there is no CPU direct access to the processor array. iMEM devices are compatible with classical memory and CPUs normally access both memory and iMEM during operation. The location of iMEM depends on system memory address decoding. CPUs generally use a PCI bridge to interface to iMEM, although the preferred iMEM implementation can also possess P-51-like pin-strapped address ranges for multi-iMEM addressing requiring no external decoding logic. The structure of iMEM is shown in FIG. 3A and the individual units are shown in FIGS. 3B-3E .
[0079] While memory interfaces to intelligent I/O have been implemented in many ways, such I/O is typically limited to relatively few channels, ISDN lines, motors, storage disks, etc. iMEM, on the other hand, is limited not by the number of extended I/O devices but by the size of the CPU address space. For 32 and 64 bit CPUs this can be quite large. Herein lies much of the power and utility of the iMEM. Often orders of magnitude more gates are implemented in memory storage than in a CPU, say 10 gigabits of memory to 10 M gates of CPU. With classical memory, those 10 gigabits have no intelligence and do no processing. Only the 10 to 100 million logic gates of the CPU process data. With iMEM, all 10 to 100 gigabits of data can be actively processing in parallel with CPU processing, potentially offering orders of magnitude increase in processing power. Current 90 nm processes allow manufacturing of 175 million gates/die and 65 nm processes are being developed.
[0080] iMEM distributed intelligence differs from multi-processor architecture, which typically replicates homogenous CPUs over an array structure. Such CPUs are then programmed in similar fashion, using say, C or JAVA languages, which are not particularly amenable to partitioning over multi-processors.
[0081] A primary goal behind the development of iMEM was to be hardware and software compatible with all processors on the market, utilizing currently available tools, not requiring new tools, and operating with current operating systems. While, in principle, iMEM processing could be implemented via a CPU embedded in the iMEM device, (such as in the Cybernetics P-51 device) the preferred implementation employs a collection of Finite State Machine (FSM)-based modules as shown in FIG. 3A .
[0082] iMEM architecture improves systems that tend to perform array operations, or operations on many sets of data that represent essentially identical elements, say atoms in a protein, or phrases in a dictionary. In such cases computation performed in memory augment the power of the CPU, possibly by orders of magnitude. In the preferred implementation iMEM intelligence can be “hidden,” that is, the iMEM processing can be suspended, and iMEM reduced to classical memory functionality.
IMEM Task Structure
[0083] Because many iMEM-based applications involve “many element” problems, where each element is typically represented by a data structure that is the same for all elements, and is operated on by a set of operations that are also applied to all other elements, the preferred iMEM implementation divides memory into multiple partitions, each partition containing, at minimum, the element data structure. In most cases, the partition also contains the element operations. If both element data and operations are contained in the partition, then the partition effectively becomes a task. If each element possesses essentially equivalent data structure and operations, then the memory partitions are equal sized, and are referred to as “pages.” In FIG. 4 , a page contains a task 175 , consisting of task code 165 , task data 160 , and task status 155 .
[0084] In the preferred implementation, shown in FIG. 3A , the first page, page 0 110 , is reserved for the system, while pages 1 . . . N are dedicated to tasks 1 . . . N (represented by the curly braces 175 ). Also, the preferred iMEM implementation allows variable page size, where the “current” size is conveyed to the iMEM by the CPU via a “page-size” register 105 on page 0 . In addition, the Tasks data/code boundary may also be variable, and also conveyed by CPU to iMEM via a “task-boundary” register 107 on page 0 .
[0085] Because the preferred iMEM implementation supports multiple tasks 175 distributed over an equal number of memory pages, the iMEM controller is denoted MTC for Multi-Task Controller 700 . In operation, the MTC selects the “current task” 150 , accesses the task state 155 , and determines the appropriate action. The preferred iMEM implementation supports at least the following states:
[0086] Executing//if different from Ready_to_Execute
[0087] Suspended
[0088] Ready_to_execute
[0089] Wait_for_resource
[0090] Wait_for_Response
[0091] Interrupting//if different from Suspended
[0092] When iMEM MTC detects a Suspended task, it performs no processing, but selects the “next” task, where any appropriate “next task selection” algorithm may be used.
[0093] Interrupting tasks are those that have signaled via an interrupt Request signal or via the task status for polled systems, that CPU attention is required. The CPU, upon detecting the Interrupting state, can examine further status info to determine the cause of the interrupt. The iMEM MTC treats tasks in the Interrupting state as if Suspended, and selects the next task. The CPU, upon servicing the interrupt, can change the task state to either Suspended or Ready to Execute, as appropriate.
[0094] Suspended tasks can only be brought out of suspension via the operation of the host CPU. That is, once a task enters the suspended state in the iMEM, it remains suspended unless and until the host CPU changes its state by writing to (or possibly reading from) the relevant state-register in the specific iMEM task. The host CPU accesses memory across the interface 125 , consisting of address bus 120 , data bus 122 , and control bus 124 .
[0095] If the MTC detects that a task is Ready_to_execute, then the MTC enables the iMEM Execution subsystem and this subsystem causes the relevant task pointer to be fetched (from the task state 155 or working copy thereof 330 ) and used to access via interconnect 420 the next task instruction from task code space 165 .
[0096] A Ready_to_execute task, depending upon the instruction executed, can remain ready, or can be suspended, or can enter a wait state, either waiting for a resource to be ready or for a result/answer/response to be available. The resource that iMEM tasks typically wait for is a Processing Element, 600 , and the answer that an iMEM task awaits, is typically the result of the operation performed by the Processing Element. This result is typically the result of a data processing operation, computation, or search, but may be a time delay trigger or other non-data event.
[0097] As shown in FIG. 3A , the MTC 700 contains a Scheduler unit 200 that analyzes the task state. In the preferred implementation, the Scheduler unit selects the “next” task page (via page address bus 220 ) and causes the task state to be accessed. If the Scheduler unit determines the task is ready, it causes the task code to be fetched and enables the Execution subsystem 400 .
[0098] Although the Scheduler unit supplies the “page” address 220 , neither the Scheduler unit nor the Execution units applies (non-page) addresses to RAM. For this purpose a “data-flow” subsystem 300 is implemented. The Dataflow unit responds to control signals 225 from the Scheduler unit, signals 425 from the Executive unit, or signals 525 from the Resource Manager unit 500 , and provides handshake and/or static signals to these units, using the same control busses. The Scheduler unit receives task-state information via bus 325 from the Dataflow unit and can update task-state info to the Dataflow unit over the same bus.
[0099] The Dataflow unit 300 manages the (non-page portion of the) address 320 to RAM, the READ and WRITE and ENABLE signals 324 to RAM and the data bus 322 to/from RAM. Data from the RAM is distributed to other MTC subsystems by the Dataflow unit, as appropriate.
[0100] Although the iMEM device may contain one data Processing Element, PE 600 , the preferred implementation contains multiple such elements, represented by braces 675 . In this case the Resource Manager unit 500 manages the control of and interface to the Processing Element 600 selected by the Scheduler unit PE select bus 210 .
[0101] In the preferred implementation the multi-tasking, multi-processing element controller 700 , consisting of Scheduler unit 200 , Executive unit 400 , Resource Manager unit 500 , and Dataflow unit 300 , provides a linkage between the current task 150 and any associated Processing Element (PE) 600 .
[0102] The Executive unit 400 uses control bus 410 to receive signals from the Scheduler unit 200 , and to advise the Scheduler unit that the task cannot execute further. A second control bus 415 is used to request either a Processing Element 600 or a response from a PE, as well as to convey the results of these requests. Although these requests originate in the Executive unit and are sent to the Scheduler unit, the Scheduler unit passes the requests to the Resource Manager unit 500 via control busses 240 and 250 , which inquire as to whether a resource or a result is available and carry the response from the Resource Manager unit. The Scheduler unit uses the PE select bus 210 to enable a given processor. Although the connectivity is not shown in FIG. 3 , the Resource Manager unit also monitors the Task select address 220 and the PE select bus from the Scheduler unit, as is described in iMEM operations.
[0103] The Resource Manager unit 500 also receives commands from the Executive unit over control bus 440 , governing data transfers between task data registers and the selected Processing Element and signals the Executive unit using bus 450 when such transfers are complete. In addition, the Resource Manager unit manages all PE control and data busses as well as the PE status bus 625 , which signals the ready status of the Processing Element 600 . In the preferred implementation, the PE control strobes are carried on PE control bus 550 , a separate bus 560 carries function commands and data to the PE, and another separate bus 660 carries data and status information from the PE to the manager.
[0104] The data that flows from task data registers 160 to the Processing Element 600 flows through the Dataflow unit over bus 322 and hence over bus 522 to the Resource Manager unit and then bus 560 to the PE for processing. Results from the PE flow over bus 660 to the Resource Manager unit, then bus 522 to the Dataflow unit, and finally over bus 322 to the target task data register (not necessarily the same register from which the info came.) The data flows between Dataflow unit 300 and Resource Manager unit 500 are coordinated via control bus 525 .
[0105] Note that the Processing Element may also have an I/O bus 680 connected to a Memory or 110 interface 690 , for whatever purposes are appropriate. For example, search processes may load a specific phrase or other data element into the PE, as described above, and the PE may then use interface 690 to a data base repository to perform the search or sort.
Description of IMEM Operation
[0106] Such an implementation operate as follows, in one embodiment. The preferred iMEM implementation utilizes an external clock and reset line. Upon power-up the device is reset and appears to the CPU as a classical memory. In this mode the CPU can decide upon page size and page boundary (between task data and task code) and number of tasks, then write this information into the appropriate register/locations ( 103 , 105 , 107 ) on the system page, page 0 110 , and then proceed to initialize the iMEM task pages by writing data to task data registers 160 , code to task code space 165 , and task state to task state registers 155 , on a page by page basis 150 / 175 . When memory has been thus prepared, the CPU can perform the ‘wakeup’ procedure, described later, to bring the iMEM into operation.
[0107] At this point the Scheduler unit 200 begins operating by zeroing the task select bus 220 and then asserting ‘get task’ 1002 of FIG. 23 , which is a signal sent to the Dataflow unit over the task control bus 225 . Upon receiving the ‘get task’ command, the Dataflow unit 300 begins fetching the task state from task 0 , which is not a true task but is the system control/configuration page 110 . This info is then used by the Scheduler unit to set the number of tasks present (unless pin strapped number of tasks is used) and, optionally, set the page size and boundary between task data and task code (boundary=start of task code.) The Scheduler unit then applies the number of tasks to the task select bus 220 of FIG. 3A , thereby selecting the page address of the ‘last’ task. (The task select bus is decremented down to zero, and when zero is reached, the task selection recycles to the ‘last’ task, unless another task scheduling algorithm is used.) With the task selection on bus 220 of FIG. 3A , the Scheduler unit again re-asserts ‘get_task’ signal 1002 of FIG. 23 over bus 225 . The signal ‘get_task’ is cleared by handshake on bus 225 when task state is read by the Dataflow unit.
[0108] Upon detecting the ‘get_task’ signal from the Scheduler unit, the Dataflow unit applies the address of the first status byte to bus 320 , and appropriate memory control signals (RD and CE) to bus 324 and reads the first byte of state information from the task state registers 155 via data bus 322 . Sequential accesses read the remaining task state bytes 155 and stores these bytes in the working task state registers 330 . The task state 1004 is conveyed to the Scheduler unit 200 via task info bus 325 and the Scheduler unit 200 interprets this information.
[0109] The Scheduler unit finds the task in one of the five valid states:
[0110] Interrupting
[0111] Suspended
[0112] Ready_to_execute
[0113] Wait_for_resource
[0114] Wait_for_response
[0000] If the task state is Suspended, the Scheduler unit sequences to the next task, typically by decrementing the task select address 218 on 220 and issuing ‘get_task’ again to the Dataflow unit.
[0115] If the task state is Ready_to_execute, the Scheduler unit receives the ‘task_PE’ info over the task info bus 325 , which indicates the Processing Element 600 in the PE array 675 that is currently linked to the task 150 , if any. If this PE is zero, no PE is selected, otherwise, if the PE_ID 216 is non-zero, the appropriate selection address is applied to the PE select bus 210 . At the same time the ‘execute’ signal 1006 is asserted to the Executive unit 400 via the task control bus 410 .
[0116] The Executive unit begins in the ‘idle’ state and, in response to the ‘execute’ signal 2 1006 , issues a ‘fetch_Code’ command 1008 to the Dataflow unit 300 over task control bus 425 . The Dataflow unit 300 accesses the current task pointer from the working task state registers 330 and proceeds, via 320 , 322 , 324 , to fetch the task code 1010 from task code space 165 . This code is presented to the Executive unit 400 via bus 420 and the ‘got_Code’ signal 1012 is asserted by the Dataflow unit over bus 425 . The Executive unit 400 then decodes the task code 1010 and takes the appropriate action. Because a major use of iMEM is to process task register data 160 using an appropriate Processing Element 600 (from PE array 675 ), a typical task begins by requesting a resource, indicated in the preferred implementation by ASCII task code ‘$’ 1014 .
[0117] When the Executive unit detects the ‘request_resource’ instruction (‘$’), it asserts both the ‘request_PE’ signal 1016 to the Scheduler unit 200 via task control bus 410 , and the ‘update_task’ signal 1018 to the Scheduler unit 200 via the resource request bus 415 and sets its own state to ‘idle’ 1020 , awaiting the next execution event.
[0118] The Scheduler unit, upon detection of the ‘request PE’ signal 1016 from 410 issues a request, PE_avail? 1022 to the Resource Manager unit 500 via the ‘PE_avail?’ bus 250 and, upon detection of ‘update_task’ signal, performs the following:
[0119] The Scheduler unit de-asserts the ‘execute’ signal 1024 to the Executive unit 400 , and signals the next state=Wait_for_resource 1026 to the Dataflow unit 300 via task info bus 325 , while also asserting ‘set_task_state’ 1028 in the task control bus 225 , causing the Dataflow unit to change the task state from Ready_to_execute to Wait_for_resource in the working state register file 330 .
[0120] The Scheduler unit also passes the ‘update_task’ signal 1030 from the Executive unit to the Dataflow unit 300 , via control bus 225 , causing the Dataflow unit 300 to write the task state from working registers 330 to task state registers 155 in task 150 in memory 100 , via Data flow busses 320 , 322 , 324 .
[0121] The Scheduler unit then waits for ‘task_updated’ signal 1032 (on bus 225 ) from the Dataflow unit. When ‘task_updated’ 1032 is seen, the next task is selected via task select bus 220 , and the ‘get_task’ signal 1034 again asserted on bus 225 to the Dataflow unit.
[0122] For ease of exposition, assume that the next task, fetched from the collection of tasks 175 , is found to be in the Wait_for_resource state 1036 . In this case the Scheduler unit does not assert ‘execute’ to the Executive unit but asserts the ‘Is_PE_avail?’ signal 1038 to the Resource Manager unit 500 , via the PE_avail? bus 250 , then wait for an acknowledgement from the Manager.
[0123] When the Resource Manager unit, which has been idle, detects the ‘Is_PE_avail?’ signal on bus 250 , it tests the PE Ready signals on bus 625 , and, if a PE is available, records this fact in Links 510 and responds with a positive assertion Ack 1042 on bus 250 , otherwise, a negative assertion results on 250 , and the Resource Manager unit returns to idle state.
[0124] If the Resource Manager unit found an available PE, then the identity of the PE, PE_id 1040 is returned to the Scheduler unit via 250 and the Resource Manager unit ‘locks’ the PE (using Links 510 ) to prevent any other task from acquiring this resource. The Resource Manager unit then returns to idle state and clears the ‘availability’ signals on bus 250 .
[0125] When the Scheduler unit observes the acknowledgement Ack 1042 on bus 250 , it determines whether the PE is available or not. If not, then the Scheduler unit uses bus 220 to select the next task from task set 175 and proceeds. If an available PE was found, the Scheduler unit sets the task state to Ready_to_execute 1044 (‘update_task’ 1046 ), asserts the ‘execute’ signal 1048 on task control bus 410 , and also passes the PE identifier (PE_id), via task info bus 325 to the Dataflow unit, where it is written into working state registers 330 , before the task state is updated in 155 .
[0126] Because it was assumed that the task opcode ‘$’ was encountered by the Executive unit, it is further assumed that, once the Wait_for_resource state returns to Ready_to_execute, the Executive unit finds an instruction that makes use of the requested resource. A realistic example would be the ASCII code sequence ‘+AB=C’, which indicates that the addition operation ‘+’ should be performed (in the PE) upon the contents of task registers ‘A’ and ‘B’ and the result, when available, transferred to register ‘C’. We now describe the operations performed for this sequence of ASCII codes. Upon decoding the ‘+’ opcode 1050 , the Executive unit saves the operator and begins the following.
[0127] In the preferred implementation, the current task number, which appears on 220 , is seen by the Resource Manager unit (not shown in FIG. 3 [but potentially transferred over ‘PE_avail’ bus]) and is used to ‘tag’ the PE with the task number. This is accomplished when the Executive unit issues a ‘save_tag’ signal 1052 over transfer control bus 440 to Resource Manager unit 500 .
[0128] The Resource Manager unit then writes the ‘save_tag’ function via 560 to the PE using the PE control bus signal 550 , followed by the ‘task_select’ value 220 , which is written into the PE tag register 645 , of the PE selected by bus 210 , where bus 210 was setup by the Scheduler unit when the resource was found to be available (and also written to the working task state 330 ), so that the task has a record of which PE has been assigned and locked to it. As a result of the above operations, the task state contains the PE identifier, and the PE contains the task identifier, or tag. This linkage can be used for pre-emptive scheduling, error detection or any other purpose as appropriate. Note that the linkage is also contained in the Resource Manager unit 500 in links 510 , where the lock is maintained.
[0129] Upon completion of the save_tag operation (or concurrently) the Executive unit 400 fetches the register name ‘A’ from task code space 165 , by issuing a ‘fetch_REG’ signal 1054 to the Dataflow unit 300 via bus 425 , then issues a ‘load_PE’ command 1056 to the Resource Manager unit 500 via the data transfer control bus 440 . The Resource Manager unit 500 uses the Dataflow unit control bus 525 to request data 1058 for the PE, and, with handshaking on bus 525 , expects data fetched from task data register ‘A’ in 160 by the Dataflow unit 300 to appear on data path 522 for writing to the PE via data bus 560 under control of signals on bus 550 . The Resource Manager unit continues this operation until all data from Register ‘A’ has been loaded into the PE, either based on fixed data size or a data terminator.
[0130] Upon completion of the data transfer 1060 , signaled to the Executive unit 400 over the transfer complete bus 450 , the Executive unit 400 typically sends a ‘Push’ command 1062 over bus 440 , which is sent to the PE via bus 560 and bus 550 to cause the PE to push the data just loaded onto the stack to make room for new data. When this transfer is complete as indicated by a signal on bus 450 , the Executive unit 400 then begins the fetch of the next register name ‘B’ by means of fetch_reg 1064 from task code area 165 and the same load sequence, load_PE 1066 , request_data 1068 , transfer_complete 1070 , as that for loading ‘A’ to the PE is repeated.
[0131] When both ‘A’ and ‘B’ have been loaded, the Executive unit retrieves the ‘+’ operator, stored at the beginning of the sequence, and sends via 440 the ‘+’ function using send_op 1072 to the PE via the Resource Manager unit 560 and 550 . When the transfer is complete 450 , the Executive unit asserts the ‘request_Answer’ signal 1074 to the Scheduler unit, via 415 , and the ‘update_task’ signal 1076 via 415 , and returns to the idle state.
[0132] The Scheduler unit, seeing the ‘request_Answer’ signal 1074 de-asserts ‘execute’ using the ‘!Execute’ signal 1078 and sets the task state to Wait_for_Response 1080 via 325 where it is written to 330 , and passes the ‘update_task’ signal 1084 to Dataflow via 225 , thus causing the task state 155 to be saved for task 150 . The Scheduler unit then causes the next task to be selected using the get_task signal 1086 . The response is the task_state (‘wait_for_response’) 1088 from the dataflow unit 300 .
[0133] When the above task, or another task waiting for an answer, is next detected, the Scheduler unit asserts the ‘is_Answer_avail?’ signal 1090 over bus 240 to the Resource Manager unit 500 , which, having recorded the linkage 510 between the requesting task (currently task selected 220 ) and the assigned PE, tests the relevant PE Ready signal 625 from the PE array 675 , and responds ‘yes’ or ‘no’ via bus 240 based on whether the PE is ready with an answer or not.
[0134] If the answer is not ready, the Scheduler unit advances to the next task. If the answer is ready as indicated by ‘ans_avail’ 1092 , the Scheduler unit asserts the ‘execute’ signal 1094 to the Executive unit 400 and changes the task state in 330 to Ready_to_execute 1114 via task info bus 325 . After the Execute Unit is finished, the task state is updated by ‘update_task’ 1116 and the ‘!Execute signal’ 1118 is issued to the Executive unit 400 .
[0135] The Executive unit 400 , fetching the next task code as usual, detects the ‘=’ code 1098 , and asserts (in the preferred implementation) a ‘read_tag’ signal 1100 on bus 440 to the Resource Manager unit 500 , which proceeds, via 560 , 660 , 550 to read the tag 645 using ‘read_tag’ 1100 , from PE 600 , serving at a minimum as a check on linkage, then Executive unit 400 asserts ‘read_status’ 1102 via bus 440 , causing the Resource Manager unit 500 to read the PE status information 648 (again via 560 , 660 and 550 ). This status information can contain PE ready status, error status, equality or comparison status, or other, as appropriate to the particular PEs (although heterogeneous PEs should strive for identical status format, if feasible.)
[0136] Assuming that no error occurred and that the desired result was not simply the status of the operation (‘>’, ‘=’, ‘<’) but the resultant data, the Executive unit 400 again issues the ‘fetch_reg’ command 1102 to the Dataflow unit 300 to obtain the target register (‘C’) from task code, then issues the ‘save_PE’ command 1106 via bus 440 to the Resource Manager unit 500 .
[0137] Upon detection of the ‘save_PE’ signal 1106 (inverse of ‘load_PE’), the Resource Manager unit 500 reads the answer (assumed at the top of stack in the PE) from the PE and places the data (or the first byte thereof) on data path 522 , while issuing a ‘take_data_from_PE’ signal 1108 to the Dataflow unit 300 via data flow control bus 525 . The Dataflow unit 300 , using register name ‘C’, computes the address of the target data register and writes the data into task data space, handshaking with the Resource Manager unit 500 . This operation continues until all of the answer data has been transferred from the PE result stack 620 to the target register 160 , then the Resource Manager unit 500 signals ‘transfer_complete’ signal 1110 via bus 450 to the Executive unit 400 , which asserts the ‘release_PE’ signal 1112 via bus 440 to the Resource Manager unit 500 , and the ‘update_task’ signal 410 to the Scheduler unit.
[0138] When the Resource Manager unit detects the ‘release_PE’ signal 1112 , it ‘unlocks’ the PE 1115 , that is, removes the association of the current PE with the current task (in Links 510 ), thus effectively returning the PE to the pool of ‘available’ PEs.
[0139] Thus, we have executed the ASCII task code ‘$+AB=C’ in the iMEM architecture.
[0140] Although iMEM supports far more functionality than described above, the operations described are typical of interactions between Scheduler, Executive, Dataflow, and Resource Manager units and corresponding access to memory and Processing Elements. Other operations, such as ‘copy data from task code space to task data register’ or ‘signal CPU via IRQ 126 and Suspend task’ can be seen to be compatible with the above described operation, and implementable by one skilled in the art. To copy data from task code space to task data space involves the Executive and the Dataflow units, independently of the Resource Manager unit. In the same manner, a task code execution may involve only the Executive unit and Resource Manager unit (after the task code fetch completed) such as ‘initialize a PE’ or ‘request PE internal function’, etc. Finally, a suspended task is ignored by the Scheduler unit, thereby allowing the CPU to access the task's data and/or code space. After the desired access has been completed, the CPU can modify the task state 155 , typically setting the task state from Suspended to Ready_to_execute, at which point the Scheduler unit would once again begin scheduling the task. Note that, even if the task state modification collided with the task state access by the Scheduler unit, such that the CPU made the task Ready_to_execute immediately after the Suspended state was read, the Scheduler unit does not update the task state, thereby preserving the ready state until the next ‘pass’, as is normal for Ready tasks waiting to execute. FIG. 23 schematically shows the above operation with unnecessary redundancy removed.
[0141] FIG. 24 shows a flow chart of the basic state transitions of iMEM. In steps 1122 and 1124 , the iMEM waits for a Processing Element (PE) to become available. If a PE is available, the state of iMEM goes to ready, in step 1126 . In this state, if iMEM needs to communicate with the host CPU in step 1128 , it does so and suspends itself in step 1130 , waiting for a response, as determined in step 1132 . Otherwise, iMEM requests a processing element, in step 1134 , and checks for its availability, in step 1136 . If a PE is available, a link is sent to the PE in step 1138 , and iMEM waits for a response from the PE, in steps 1140 and 1142 . When a response is received, iMEM returns to the ready state.
Brief Summary OF IMEM Operation
[0142] The Scheduler unit selects a task/page and signals the Dataflow unit to get the task. If the task is READY, then Scheduler unit signals Execution to execute the task code.
[0143] The Executive unit encounters a wait-for-resource instruction (via Data-flow) and signals a resource request to the Resource Manager unit, through the Scheduler unit.
[0144] If no resource is available, Scheduler unit sets the task state to Wait_for_resource.
[0145] Otherwise, the Resource Manager unit (eventually) finds an available PE and signals such.
[0146] The Executive unit issues a “LINK & LOCK” command to Resource Manager unit or Dataflow units, (or both).
[0147] The Resource Manager unit “tags” or links the PE to the task by writing the current task page to the PE (which stores the tag/link) and sets a “lock” bit or flag, maintained by the Resource Manager unit to prevent said PE appearing available to another task.
[0148] The Dataflow unit, under control of Resource Manager unit, transfers task data to PE (or from task code to data register under control of Executive unit).
[0149] The Scheduler unit, in coordination with other units, commands Dataflow unit to set task state to Wait-for-Answer and update task in RAM.
[0150] The Scheduler unit then advances, via appropriate algorithms, to the next task. Eventually, the “next task” is a task waiting for an answer.
[0151] The Scheduler unit asks the Resource Manager unit if answer-is-available. If not, the task continues to wait.
[0152] If so, the Resource Manager unit manages the transfer of data from the Processing Element, PE, to the task data space in RAM, then signals the Executive unit that the data transfer is complete.
[0153] The Executive unit tells the Resource Manager unit to release the resource (the PE) and the Scheduler unit to update the task state (to READY). The PE returns to the “available” pool and task processing continues as appropriate.
[0154] The number of task instructions executed before the task is returned to READY state is implementation dependent and should best match the implementation to the problem. In most cases it is assumed that, at some point, a task may reach a state where it is appropriate to provide some result to the host CPU. The preferred implementation signals the CPU, typically through an interrupt line, and enters the SUSPENDed state 802 , awaiting CPU response, although in some cases it may be appropriate for task execution to continue. In general, CPU/iMEM interaction is coordinated as follows (see FIG. 5 ):
[0155] SUSPENDed task awaits CPU
[0156] CPU (reads or writes) (task data and/or code) 804
[0157] CPU alters task state to READY
[0158] READY task resumes operation/execution 806
[0159] Eventually task signals CPU and suspends itself
IMEM Architecture is Both Task Code and Task Data Independent
[0160] iMEM architecture can be tailored to a specific application class. The iMEM architecture described above is independent of task code and data implementations. The specific instruction coding (interpreted by the Executive unit) and the specific data types and sizes do not affect the general iMEM operation described above (except to simplify implementation.) For this reason task code and data implementations may be problem specific. Although some problems may be optimally solved via such specificity in (task instruction and data) encoding, we specify a preferred iMEM encoding scheme that should be employed unless other considerations suggest otherwise.
[0161] The iMEM operations described above are extremely general, that is, tasks execute and change state according to the events occurring during execution, and data is transferred from task memory to Processing Elements and operations performed, then the results are transferred into task memory space. Thus, a generic encoding of task operations is both possible and desirable.
Description of IMEM ASCII Task Code
[0162] The preferred task encoding is ASCII, that is, task instructions are represented by ASCII codes, including ASCII arithmetic codes, +, −, /, as well as punctuation and other ASCII symbols. The preferred data structure is Register-based, and uses ASCII Register names, ‘A’..‘Z’.
[0163] Though this naming convention implies that we have a maximum of 26 data registers (per task), it is consistent with the goals of the iMEM architecture. The ability to refer to task data registers by an ASCII name is so powerful that limiting the register set to 26 data registers per task is acceptable. A typical iMEM application is a many-body problem, typically one body per task. Such bodies can usually be characterized by fewer than 26 parameters so that this limitation should not be unduly constraining. If it is, we can double register space by making the register name case sensitive. Even with 26 registers (per task), the iMEM has a larger register set than most classical and many current CPUs. This task structure is shown in FIG. 6 , which depicts a field for the task state 808 , a task pointer 810 , a task processor 812 , and a task operation 814 . Preferred implementations use byte wide (8-bit) task code memory, which is compatible with and accessible by most CPUs. The width of the data registers is completely unspecified, but is typically a multiple of 8 bits.
[0164] Note that the ASCII-named registers may contain the data to be operated on, or may contain pointers to the data to be operated on, or both.
[0165] Consider a typical ASCII encoded task instruction:
[0000] ‘$+ AB=C ’ (or ‘$ A+B=C ’)
[0000] The above instruction is decoded by the iMEM Executive unit as follows:
[0000] ‘$’ => wait for resource ‘+’ => add the two following registers ‘A’ => send 1st Register to PE ‘B’ => send 2nd Register to PE = => wait for answer, transfer results ‘C’ => Register for result storage ‘ ’ => ignore spaces, used for readability
Other task code instruction(s):
[0000]
:B-123.456
//copy‘-123.456’ into Register B
$(A>B) ? g : h
// compare Register A to Register B, do g if >, else do h
%
// suspend self, wait host intervention (assert IRQ)
0
// End of task code, repeat from start of task code
[0000]
* + − / > < & | . ~ —
ASCII Data Processing Operators
! {grave over ( )} : $ = ? # % @ ; \ ″ {circumflex over ( )} ,
ASCII System Operators
[ ] ( ) { }
ASCII Partition Operators
0 1 2 3 4 5 6 7 8 9
ASCII Numeric data
A B C . . . X Y Z
ASCII Register names
a b c d e f g
ASCII Function names
h i j k I m n o
ASCII Index Register names
p q r s t u v w x y z
ASCII Reserved symbols
0x01 . . . 0x1A
ASCII Ctrl Operators
IMEM ASCII Data Processing
[0166] The ASCII task encoding scheme described above is data independent, if one assumes that the host loads the data registers initially, and then unloads them directly, and if the Dataflow unit, Resource Manager unit, and PE elements are implemented appropriately.
[0167] Thus, iMEM works, as described, with ASCII task code and binary data, but also works with ASCII data, given the same qualifications. For some tasks, such as search and sort, ASCII data is most appropriate. In other cases, such as numeric processing it is harder to determine the appropriate data format/encoding. For example, stock market prices are typically entered as ASCII numbers and displayed as ASCII numbers. Even if the binary computation is faster than ASCII computation, the overall computation speed may be slower when ASCII-to-binary-to-ASCII translation overhead is considered. There are also silicon or equivalent costs involved. For typical floating point units of the type found in Intel Pentium CPUs, the data is 80 bits wide, and paths in the FPU are 80-bits wide. For ASCII floating point units the internal paths are only four bits wide, allowing more effective use of silicon. Thus, for example, Intel CPUs typically contain one to four FPUs, while initial FPGA-based iMEM devices contain up to twenty-five ASCII FPUs.
[0168] Although our preferred implementation uses ASCII data and data processing, there is nothing about the iMEM architecture requiring such, or precluding Unicode implementation.
IMEM ASCII Architecture
[0169] As described above, iMEM architecture supports both binary data and code. The preferred implementation assigns upper case ASCII alphabetic characters as register names, and assigns ASCII operators (+, −, *, /, _, >, <, ?, !, @, #, $, etc.:, as opcodes. Because there are innumerable problems to solve, and only a finite number of ASCII operators, iMEM specifies a preferred operator assignment, but specific problems may be better served with an alternate assignment, therefore there is no strict insistence on a particular operator interpretation in the iMEM architecture. For example, the “+” sign should typically cause addition to be performed in arithmetic systems, but could mean concatenations in sorting applications.
[0000]
+AB = C
+AB = C
+BA = C
A = 123
A = “cat”
A = “cat”
B = 456
B = “dog”
B = “dog”
C = 579
C = “catdog”
C = “dogcat”
[0170] Note that the arithmetic+operation is commutative, while the alphabetic operation is not. Note also that the implementation of the Executive unit is the same for both arithmetic and alphabetic operations but the Processing Element performs the operations differently, as would be expected for a computation Processing Element versus a sorting element. The preferred iMEM implementation of ASCII operations preserves to the maximum extent, the behavior of the Execution, Scheduler unit, Dataflow, and Resource Manager units and expects the Processing Element(s) to interpret the operations appropriately. With this understanding of iMEM ASCII operators, we define a default set of operations.
[0171] The default set of ASCII operators is further partitioned into two sets of operators. Operators in the first set are interpreted by the Executive unit, while operators in the second set are interpreted by the Processing Element. For example, the description of iMEM operation described in detail the interpretation of the following instruction,
[0000] $+ AB=C.
[0172] In the example, the “$” is interpreted by the Executive unit as a request for resource operation. Then, the “+” was recognized as requiring at least two register operands, but was sent to the Processing Element for actual interpretation and execution. The “=” operator was interpreted by the Executive unit as a transfer operator, and the result of the “+” operator was transferred from the Processing Element to the target register, C.
[0173] In the simplest iMEM architecture the following operators are sent to a Processing Element for interpretation:
[0000]
<OPR>
<Default interpretation>
+
Add, concatenation
−
Sub, difference
*
Mul, product
/
Div, partition
>
GT, greater than
<
LT, less than
.
Decimal Point
&
And, subset
\
Or, subset
~
Not, outset
{ }
Reserved
—
Reserved
[0174] The following operators are interpreted by the Executive unit:
[0000] <OPR> <Default interpretation> $ Request Resource # Hexadecimal :k #75 % Request Host and Suspend = Transfer result to register ? Test for Branch @ Call register or branch indirect : Location operator ′ Pass through operator (to PE) ″ String delimiter (overrides space, etc.) ( ) Scope operators [ ] Index operators \ Reserved ; Delimit instructions, switch task (this task = READY ! Interrupt host or send I/O output , Separator {circumflex over ( )} Ctrl, {circumflex over ( )}A send task code = 01 to Executive unit
Finally, the preferred iMEM implementation also interprets multi-character operations.
IMEM Index Registers
[0175] In the preferred implementation, the ASCII-named data registers hold data sent to or received from the Processing Elements. In addition to these primary data registers, we implement binary index registers and assign lower case ASCII names to them. The default set of byte-wide binary index registers 816 labeled ‘h’ . . . ‘o’ are included in the task status registers as shown in FIG. 7 . Multi-byte-wide index registers are consistent with this scheme.
[0176] Index Registers can be initialized, incremented, decremented, and tested, and can be used to index data registers by task and to index into code space for branching. Examples of index register usage are shown:
[0000]
:n #04
// load index register n with hexadecimal value 04
n+
// increment index register n
n−
// decrement index register n
k: $+AB = C
// k is label, index register k loaded with task ptr.-> “$”
@k
// k is branch target, copy index register k into task ptr.
IMEM Register Index Addressing
[0177] The addition of index registers supports ‘branch to label’ operation as described above, and also opens the possibility of data register indexing. In the preferred implementation, the following syntax represents such indexing:
[0178] A[n]//n is task/page index for data register A
[0179] The interpretation of A[n] is that ‘n’ declares the task from which register ‘A’ is accessed.
[0000] $+AB = C // wait resource, add A and B, wait response, transfer to C $+A . . . F = G // wait resource, sum A through F, wait result, transfer to G $+A[i]B[j] = C[k] // wait resource, add A from task i to B from task j, wait result, transfer to C of task k.
In each of the above expressions, the system operator “$” causes the system to wait for an available Processing Element, then to fetch the data operands from the relevant named data registers, send these operands to the Processing Element, and tell the Processing Element to perform the data operation “+”. It is significant that no assumptions have been made about the nature of the data operands, or the nature of the “+” operation. The system is assumed to be able to fetch data from named data registers, and copy results to a named register, and the Processing Element is assumed to be able to perform the “+” operation. It does not matter whether an arithmetic operation is performed on binary data, or on ASCII decimal data or whether concatenation is performed on ASCII data strings, the iMEM systems behave in essentially the same manner.
[0180] Because all tasks share the same register structure, addressable by alphabetic characters ‘A’ through ‘Z’, the same letter can refer to the same register on all pages, and the index register allows the actual task/page from which the register is to be accessed to be specified. In order to accomplish this type of indexing, there needs to be a mechanism that can alter the ‘page’ address 820 during the access, then restore the current task page address for continued task code execution. Such a mechanism is shown in FIG. 8 . In this implementation, the indexed page address 346 is sent from the Dataflow unit 300 and multiplexed by multiplexer 800 , under Dataflow unit control signal 345 , with the system page address provided by the Scheduler unit 200 .
[0181] An alternative use of indexed addressing could be used to select a particular Processing Element as follows:
[0000] $[ n]+AB=C wait for resource n , add A and B , wait response, transfer to C
[0000] In this case, the $ resource request is immediately followed by an index operation specifying the address of the Processing Element desired. (Alternatively, control characters can address PEs.) This assumes heterogeneous elements and is generally unnecessary for homogeneous Processing Elements. Because the preferred implementation uses homogeneous elements, we assume such in the following. Excluding the case of indexed Processing Element addressing, the register indexed addressing can be interpreted in the Dataflow unit, per se. The advantage of such interpretation is that there is no necessary flow between task code memory, the Dataflow unit, the Execution system, and back to the Dataflow unit, all of which takes time, measured in clock cycles.
[0182] Performing register indexing in the Dataflow unit allows much faster operation than would the same interpretation in the Execution system, and leads us to consider what other operations can or should be performed in the Dataflow unit. One such operation is the hexadecimal numeric operator, which follows an index register specifier and precedes numeric value to be stored in said index register. As described above, :n#03 is interpreted to mean that index register n is to be loaded with hexadecimal value 03, which produces the value 00000011 and stores it in index register n. The interpretation of each of the ASCII characters in this sequence can be performed by the Dataflow unit, again avoiding the necessary handshaking between the Dataflow and Execution subsystems, and thereby speeding up the process considerably. Note that, except for the simple hex-to-binary conversion, the necessary operations are all addressing and data access operations, and therefore properly belong in the Dataflow unit. With this in mind, we also examine the operations associated with using index registers to hold label addresses, and with subsequent use of such to facilitate branching in task code. For task code spaces of 256 bytes or less, the label address itself can be stored in the index register, while for larger task code spaces, relative addressing is preferred, unless the default memory width is greater than 8 bits, in which case absolute addressing may be preferred. In any case, these addressing operations are fetched from memory by the Dataflow unit, the relevant index register and task code addresses computed, and either the relevant task code address is stored in the specified index register, for labels, or the contents of the specified index register (the branch target in @n) is accessed, and copied into the working task pointer register, for branching operations. These addressing manipulations, accesses, and modifications are all naturally performed in the Dataflow unit, with no necessary help or intervention from the Execution system.
Distributed ASCII Operator Interpretation
[0183] The consequence of the above description is as follows. We earlier specified a two set ASCII code interpretation mechanism, in which some ASCII codes were interpreted by the Execution subsystem, and some were sent to the Processing Element subsystem to be interpreted. If we add the index register based operations described above, we see that a better implementation is the novel three partition distributed ASCII code interpretation just seen. In this scheme, we include the Ctrl operator, ̂, which operates on capital ASCII alphabetic characters, ANDing the letter with 10111111 to clear the 6th bit, producing a result from 0x01 to 0x1A, denoted by Ctrl-A through Ctrl-Z, which operators are to be interpreted by the Execution subsystem in the preferred implementation. However, we see that the compaction of the two ASCII characters can be performed in the Dataflow unit, which now recognizes the ̂ character, fetches the next alphabetic character, clears bit 6 , and sends the resultant Ctrl character to the Execution system to be interpreted.
[0184] The three operator sets for distributed ASCII code processing are summarized. In the preferred iMEM architecture the following operators are sent to a Processing Element for interpretation:
[0000] <Operator> <Default interpretation> + Add, concatenation − Sub, difference * Mul, product / Div, partition > GT, greater than < LT, less than Decimal point & And, subset | Or, superset ~ Not, outset { } Reserved — Reserved (underscore)
The following operators are interpreted by the Executive unit:
[0000] <Operator> <Default interpretation> $ Request resource % Request host and suspend = Transfer result to register ? Test for branch : Location operator followed by data register specifier {grave over ( )} Pass through operator (to PE). “ String delimiter (overrides space, etc.) ( ) Scope operators \ Reserved ; Delimit instructions, switch task (this task = READY) ! Interrupt host or send I/O output , Separator
The following operators are interpreted by the Dataflow unit:
[0000] <Operator> <Default interpretation> ‘h’ . . . ‘o’ Index register specifiers [ ] Index operators # Hexadecimal :k #75 or :A#75FE32 etc {circumflex over ( )} Ctrl, {circumflex over ( )}A sends task code = 01 to Executive unit ({circumflex over ( )}B = 02, etc) @ branch indirect through index register : Location operator followed by index register specifier
The processing of all ASCII operators, both system and data operations should be executed in the same way over all preferred implementations. The scheme is illustrated in FIG. 8 , in which ASCII operators are shown in the subsystem in which they are interpreted. iMEM architecture is compatible with any number of ASCII mappings. For instance, in the above example the characters ‘<’, ‘>’ are interpreted by the computational Processing Element as less than and greater than. Another implementation could treat ‘<’ and ‘>’ as XML delimiters to be interpreted by either the Execution subsystem or the Processing Element, etc.
[0185] Note also that the ‘Pass-through’ operator can be either “command by command” or toggle, that is, the pass-through operator can cause one command to be sent to the current PE, or can cause all following commands to be sent to the PE until the next pass-through operator toggles the pass-through mode, returning control to normal execution/interpretation mechanisms. In this way, the iMEM architecture can effectively support multiple “languages,” wherein each separate language is addressed to an appropriate Processing Element.
ASCII IMEM Data Independence
[0186] As discussed above, the use of ASCII task codes and ASCII Register names, does not require the use of ASCII data, but is compatible with almost any data type, from ASCII numeric to binary numeric to image maps (.BMP, etc.), voice waveforms, etc., assuming that the data registers have appropriate capacity. In preferred implementations, task data registers are 16 bytes long, but they could easily be one, two, four, or eight bytes long, or much longer. Register size can be implementation specific, or can be specified as part of the task state info for each task.
[0187] In addition to register size, the task page size and the boundary between task data and task code (=start of task code) can be variable, and included in the task state info for each task. Although the preferred implementation uses fixed size pages, allowing the Scheduler unit to ‘randomly access’ tasks, variable page sizes could be supported by the Scheduler unit following links from the current task to the ‘next’ task, using the page info in the task state to compute the end of the current task and the start of the next. If ‘random-like access’ is required, the Scheduler unit can build a task address table as each new task is encountered, thus allowing access to any (already encountered) task regardless of varying task sizes.
[0188] In addition to task state, task data, and task code segments on each page, iMEM can support other segments such as symbol table, stack storage, or object template segments, etc. The preferred mechanism for supporting additional segments is by extension to the list of pointers and counters as shown in FIG. 9 . FIG. 9 shows the page 0 /system page. If segments are sequential, then successive sizes are sufficient to define numerous segments per task. With fixed page size, these configuration parameters I, J, K, L, M, and N are located on the system page 900 , where I is the word size in bytes, J is the number of words per increment, K is the number of tasks in the iMEM, L is the number of increments per page, M is the number of increments per data register, and N is the number of increments offset to the task code. Note that for one gigabyte of RAM and a page size of 4K bytes, the Scheduler unit can support approximately 250,000 tasks. Conversely, for pages of 256K bytes, the Scheduler unit could support 4K tasks. It can be seen that the fixed page size, system-page-based configuration parameter table is indefinitely flexible.
IMEM Data Path Width and Unicode Implementations
[0189] Because the iMEM configuration is defined via specific parameters on the system page, these parameters can by redefined and iMEM reconfigured by host CPU software. A major architectural question having to do with such dynamic reconfiguration concerns the basic data path width. If the path width varies, there must be corresponding variation in the memory, the Dataflow unit, the Resource Manager unit, and the Processing Elements, whereas if the data path is constrained to a fixed word size, with only the number of words variable, then changes in iMEM are confined to the Processing Elements, with few, if any, changes required in memory, data-flow, or Resource Manager unit circuitry. Note that a byte wide path quite naturally supports any ASCII data types, while also supporting 8-, 16-, 32-, 64-, or N-byte binary data types. Although the sequential handling of byte-wide data consumes greater time than wider paths, the silicon (or other substrate) requirements are less, so it may be feasible to trade-off data flow speed for compensating gains in the number of tasks and/or Processing Elements. The preferred iMEM implementation therefore uses byte wide data paths, but any width data path is compatible with iMEM, as long as all data handling circuits are implemented appropriately. Note also that a 16-bit memory and data path width supports Unicode data and instructions in the same natural manner that the 8-bit architecture supports ASCII coding. Thus, a preferred 16-bit architecture is Unicode-based with all ASCII operations preserved from the preferred 8-bit implementation. The same data independence applies to Unicode implementations as to ASCII implementations.
Alternative Dataflow Organization
[0190] The iMEM architecture described above uses the Dataflow unit to handle addresses to memory, memory control signals and memory data access, and presents the data to the Resource Manager unit, with handshaking.
[0191] An alternative memory access mechanism involves the Resource Manager unit signaling the Dataflow unit to supply the relevant address to memory while the Resource Manager unit takes control of the memory control signals 560 , 562 , 564 and data bus 522 , as shown in FIG. 10 . In the preferred implementation the Dataflow unit 300 maintains byte-wide access 350 to memory 100 (to preserve ASCII task codes), while data transfers between memory and Processing Element(s) can be any appropriate width. The data bus can enter the Resource Manager unit module or can connect directly to the processor bus, with processor bus control signals managed by the Resource Manager unit. In this manner iMEM becomes largely data path width independent, in that task scheduling and task code execution do not depend directly on data path width.
ASCII Code Hierarchy
[0192] In addition to the distribution of native ASCII operator interpretation over three subsystems described above, iMEM devices can support at least two levels of ASCII code interpretation, native code at the task code level, via iMEM architecture implementation, and higher level code at the task data level, whereby the interpretation of ASCII commands stored in task data registers is performed by either the ASCII task code per se, the Processing Element hardware, or both. In this sense, ASCII commands read from task data space correspond to a ‘high level interpreted language’, while ASCII task code read from task code space corresponds to ‘native code’, which corresponds to binary executables in classical CPU architecture. For clarity, we stress that the iMEM ASCII native task code differs from classical CPUs in that the interpretation of the ASCII opcodes is performed directly by logic, with no binary executables involved, unlike classical CPUs in which ASCII commands are assembled or compiled into binary executables and linked and loaded into CPU code space.
[0193] In FIG. 11 , the high level code, shown in register A, is price (“IBM”) and the low level task code 165 is $[i] ‘A=X. iMEM begins executing the task code by fetching the resource request, $, and noting that the next character is the bracket, [, indicating an index is required. iMEM then fetches the index, i, and uses the result to request the specific resource 600 , P[i]. The task then waits until PE[i] is available. When PE[i] is available, the task resumes, and the next task code, ‘, is fetched. This, in the preferred implementation, is the pass-through operator, which should be followed by either a data register name or a quote string. The effect of ‘A is to pass the contents of the data register A to PE[i], where it is interpreted. In this case, PE[i] searches for the price of IBM stock. Because iMEM assumes that data register pass-through commands produce results, the task then enters the Wait_for_response state. (Note: pass-through quote strings do not wait for result.) When PE[i] finds the stock price, it signals such, and the task then copies the price into register X, as indicated by the task code. In this fashion iMEM native ASCII task code is interpreted by Execution hardware, while higher level application code is interpreted by Processing Element(s).
ASCII IMEM Compiler-Less Architecture
[0194] ASCII iMEM devices do not require compilers or assemblers, since ASCII task code is executed directly by the iMEM hardware, with no intermediate forms required. Because Assemblers, and Compilers are CPU and Operating System specific, this is a major advantage of iMEM. Because literally all modern computer systems provide some type of ASCII editor, iMEM is thus compatible with all CPUs and OSs, not simply those for which iMEM compilers have been written.
[0195] Although single character names are convenient from an execution perspective, the use of longer alphabetic or alphanumeric names can be supported in a simple fashion by using the register ‘image’ on the system page 900 , page 0 , to hold multi-character names, thus system page register ‘A’ holds the (terminated) string name for task register ‘A’, and so forth. This scheme works for array operations in which all tasks operate on data in the same way, and all task data registers have the same meaning across tasks. For example if register ‘Q’ holds the electric charge for every task, then system register ‘Q’ can hold the ASCII string ‘charge’ identifying the type of data in all Q-registers. Based on this scheme, shown in FIG. 12 , iMEM hardware can translate string names to register names and register names to string names, for “friendlier” programming. The actual iMEM task code that executes should always use the single character register names. In the default iMEM implementation, the CPU is assumed to setup both data registers and task codes, however standalone iMEM implementations, which allow program input from I/O channels, could use task register name strings, while converting actual task code to single character names. Thus, for example, for task code containing 26 or fewer independent variables, iMEM could build and scan the system page ‘symbol tables’ to translate arbitrary variable names to single character ASCII register names, allowing iMEM execution.
IMEM ASCII Translation
[0196] The iMEM Dataflow unit is used to fetch the task code from code space, upon receipt of the ‘get_Code’ signal from the Executive unit. Because the Dataflow unit also reads the task status 155 into the working task state registers 330 , Dataflow can also look at the task state value, and, if the state is Ready_to_execute, can access the task pointer and ‘prefetch’ the task code. This capability offers a significant ASCII translation capability to iMEM architecture. An example is described below and illustrated in FIG. 13 .
[0197] The System page, page 0 , can be used to hold ASCII multi-character names for iMEM task data registers as described above. Following the registers on the system page, is system space available for task code support. In particular, multi-character ASCII commands can be stored in this space, followed by a specific byte of code to be described. These commands can be used to translate ASCII commands in task code space as follows.
[0198] When the Dataflow unit loads a Ready_to_execute 910 task state, it fetches the task pointer and prefetches, in step 912 , the task code byte and the ‘next byte’. If the task code byte is a valid iMEM code, typically an operator or punctuation character, as determined in step 914 , the fetch terminates and, in step 932 , it is sent to the execution unit. However, if the task code is an alphabetic character (reserved for Register names or labels) and the ‘next byte’ is also alphabetic, as determined in step 914 , then the Dataflow unit assumes that the task code space holds (at least one) multi-character ASCII command that requires translation. The Dataflow unit then continues to prefetch, in step 916 , alphabetic bytes until either a space byte, 0x20, or a byte with bit 7 set is encountered, as determined in step 920 .
[0199] If the byte following the command has bit 7 set, as determined in step 920 , then the Dataflow unit determines that this is actual task code to be presented to the Executive unit, when the ‘get_Code’ signal, in step 918 , is asserted.
[0200] If the byte following the command is a space character, as determined in step 920 , then Dataflow assumes that the System Page contains a table of ASCII commands followed by single bytes with bit 7 set, and proceeds to search, in step 922 , the System page for the matching command. (Note that Dataflow must zero the Page address from the Scheduler unit while accessing System page.) The Dataflow unit searches the System page task code space for a character that matches the first byte of the command and continues scanning as long as the bytes match. If the first mismatch occurs, as determined in step 924 , when the space character is encountered in the task code, then the corresponding byte in System space is assumed to be the single byte code with bit 7 set, and, after confirming, in step 926 , that bit 7 is properly set, the Dataflow unit accesses the code, and writes it into the current task code page, overwriting, in step 928 , the space character. In this way, a single search is required to translate the multi-byte ASCII command in the current task code space into a single byte used by the Executive unit. Thus, the next time the Dataflow prefetch mechanism encounters the multi-character ASCII code, it reaches, not the space, but the single byte with bit 7 set, as determined in step 920 , and therefore does not initiate the search of the System page. In the ideal case, the prefetch occurs, in step 912 , while the rest of the system is otherwise occupied, and requires little, if any, additional time for handling the multi-byte commands. Note that this mechanism allows the host CPU to build the translation tables in the System page in support of ASCII command task coding. Alternatively, in the standalone version, these tables are implemented in non-volatile memory. In anticipation of re-configurable technologies, the system can use bit 6 of the special code to distinguish between interpretation by the Executive unit and Processing Element as follows.
[0201] If bit 6 of the special code is zero, the Executive unit can interpret the code. If bit 6 is set to one, then the Executive unit can send the task code to the Processing Element through the Resource Manager unit, for interpretation and execution. In this way the iMEM architecture and scheduling and execution mechanisms can be preserved, while the Processing Elements can be reconfigured and programmed from task code using meaningful ASCII commands set up by the CPU in the System page translation table.
[0202] It is obvious that one skilled in the art could extend these mechanisms in various ways in support of the hardware ASCII code translation process, eliminating the need for the compiler technologies normally associated with such execution.
The IMEM CPU Task Index Register
[0203] The Task Index Register 180 , on the CPU side of the memory 100 , corresponds to the Page address register on the MTC side of the memory, in that it selects the page to be accessed by the lower address bits. As shown in FIGS. 14A and 14B , the Task Index register can be loaded from the address bus 120 , or the data bus 124 , as appropriate, via CPU control of the Index latch signal 182 . After the Task Index register 180 has been loaded, all CPU addresses appearing on the address bus access the Task Index-selected page of memory. In a segmented architecture, such as the Intel 386 and compatible CPUs, it is then feasible to create a segment corresponding to task status, another segment corresponding to task data, and another corresponding to task code space, such that these three segments always access the desired segments of the current task, where the current task, from the CPU perspective, is selected by the Index register, as shown in FIG. 15 .
[0204] In systems that poll for iMEM interrupts by reading the task status register and examining the task state instead of using a hard interrupt, the Index register may be implemented using a pre-settable counter, such that the counter can be loaded from a data or address bus as described above, or can be loaded with pin-strapped information. The counter 940 of FIG. 15 can then be incremented (or decremented) via a signal produced by the output of a comparator 942 that compares the low address generated for a CPU read instruction with the on-page address of the status register, thus facilitating a polling scan of each task's status by the CPU without the necessity of having the CPU modify the contents of the index register between tasks. If the counter 940 is an up/down counter, then the normal behavior consists of a read of a task state that is not interrupting, followed by the auto increment (say) to the next task page, where the read is repeated. If the state is found to be interrupting, then the Index register now has selected the next page, not the interrupting page, therefore the CPU can immediately decrement the counter to return to the interrupting page. Since it is assumed that most tasks are not interrupting at a given time, then this is the most efficient way to scan.
IMEM Standalone Architecture
[0205] The CPU-based iMEM depends upon a host CPU to initialize memory and awaken the iMEM device. A standalone (hostless) iMEM optionally self-awakens and self initializes. Self-awakening requires little explanation. All devices that begin functioning after a power-on-reset effectively self-awaken. Self-initialization is also quite common and is ultimately based on non-volatile storage of initial code and data, including status data. Such non-volatile info is either directly accessed upon startup, or is copied into working RAM for operation.
[0206] Standalone iMEM devices either perform fixed functions, requiring no external program input, or require a program input channel 950 , as shown in FIG. 16 . The program input channel and subsystem 950 must minimally provide the following functionality:
[0207] Establish communication channel(s) and support communication protocol(s);
[0208] Provide RAM address selection (and address auto-increment) function(s); and
[0209] Provide RAM data write operation to download code and data to iMEM.
[0210] Alternatively, a more intelligent program input subsystem recognizes the iMEM task structure, and supports ‘per task’ programming vs. simply writing to specified RAM locations.
[0211] The distribution of ‘program input’ intelligence between iMEM and the program input subsystem is arbitrary. The program input subsystem can autonomously setup communications, download task state, code, and data, and then awaken iMEM, just as a host CPU would behave, or the iMEM can self-awaken, self initialize, optionally attempt to open a communication channel (or wait for one to be opened), and then wait for program input from the channel. These and other standalone iMEM support mechanisms are obvious to one skilled in the art.
[0212] An abundance of communication interfaces, including USB, ISDN, Ethernet, Wireless, and even UART and PS/2 Keyboard interfaces are feasible in support of iMEM standalone operation. With these power-up changes, iMEM can function in a standalone manner, with no CPU, or loosely coupled to a CPU via said communications channel.
IMEM Arrays
[0213] iMEM architecture is designed to add true intelligence to memory, in order to support CPU-based systems in ways not before possible. Specifically, one host CPU can support multiple iMEM devices, up to the limit of the CPU address space, using the CPU address bus.
[0214] Although iMEM distributed intelligence differs from multi-processor architecture, iMEM standalone arrays can be implemented, with either heterogeneous Processing Elements or homogeneous Processing Elements. iMEM devices can be linked in arrays similar to other Klingman inventions, such as P-51 Chains, (U.S. Pat. No. 6,021,453) and N-cell arrays (see U.S. patent application titled “A Basic Cell For N-Dimensional Self-Healing Arrays”, Attorney Docket No. 372614-03701, filed Mar. 20, 2000) due to the fact that iMEM Processing Elements optionally support a second interface 690 in FIG. 3A , either directly or through a shared switching module, allowing iMEMs, either hosted or standalone, to be cascaded or chained in the P-51 manner (see U.S. Pat. No. 6,021,453, titled “Microprocessor Unit For Use In An Indefinitely Extensible Chain Of Processors With Self-Propagation Of Code And Data From The Host End, Self-Determination Of Chain Length And ID, (And With Multiple Orthogonal Channels And Coordination Ports”) In addition, the use of ASCII data reduces the data port widths in a manner desirable for use in ‘N-cell’ architectures. (see U.S. patent application titled “A Basic Cell For N-Dimensional Self-Healing Arrays”, Attorney Docket No. 372614-03701, filed Mar. 20, 2000) These ‘vertical’ and ‘horizontal’ array options are shown in FIGS. 17A and 17B , respectively.
[0215] Because iMEMs support an arbitrary number of Processing Elements, and each PE can optionally support another memory interface, then each PE can support a ‘downstream’ iMEM device, which can, in turn, support a multiplicity of PE-hosted iMEMs, and on, ad infinitum. An iMEM tree can be constructed limited only by practical concerns such as cost or power ‘consumption, but architecturally unlimited. In this manner, iMEM branching arrays can be constructed with either homogeneous or heterogeneous Processing Elements, and with or without each PE supporting a downstream iMEM device. That is, any one of a given iMEM's Processing Elements can host another iMEM or not, on a PE-specific basis. This net-like architecture, shown in FIG. 18 , becomes even more powerful when re-configurable PEs are considered.
[0216] Re-Configurable IMEM Architecture
[0217] The data format and data handling portions of iMEM can vary significantly from implementation to implementation. These can be ‘hard’ variations, in which a fixed data type is specified at powerup, along with appropriate data Processing Elements, or ‘soft’ variations such that configurable logic technology allows ‘on-line’ modification to data structures, data types, data-flow, and data-processing logic. Because, in theory, infinitely variable logic systems essentially unconstrain implementation architecture, to be useful, in a design sense, one must constrain architectures that are intended to interface naturally to today's CPUs, but that should also be capable of evolving to take advantage of expected technological advances, particularly in the area of dynamic reconfigurability.
[0218] In expectation that real-time re-configurable logic circuitry is essentially unlimited in its application, such that portions of the logic can be statically fixed, while other portions can be dynamically reconfigured, either on a cycle by cycle basis, for synchronous circuitry, or module by module, for asynchronous systems. Those portions held fixed are used to implement iMEM control architecture, while the changing circuitry implement the data processing, and data-flow, portions of iMEM, as shown in FIG. 19 . The preferred implementation of iMEM reconfigurable architecture preserves the interpretation and execution of iMEM ASCII System operators by the Execution subsystem, while reconfiguring one or more Processing Elements to re-interpret the iMEM ASCII Data operators (+ − * / ˜ & | . _). Reconfigurable implementations support both homogeneous and heterogeneous Processing Element arrays. The shaded portion of FIG. 19 represents reconfigurable subsystem(s).
IMEM Clock Domains
[0219] The least frequently invoked signals tend to be the signals between the Scheduler unit and the Executive unit, which typically occur at the beginning and end of a task invocation.
[0220] In contrast, the data transfer operations and their management, occur frequently, almost constantly, therefore the events should be triggered/clocked as frequently as possible.
[0221] “As frequently as possible” means that the maximum changes occur per cycle, and this maximum is two, since we can effect transitions on both positive and negative edges of the clock.
[0222] Therefore, part of the iMEM architecture concerns the distribution of clock domains over the system. In terms of current technology, this implies, optimally, a single ‘external’ clock with synchronous connectivity, as is well understood by those skilled in the art. In terms of future technology, asynchronous modules, almost ‘islands’ in logic space, may exist with no global clock, and iMEM clocking should be compatible with such.
[0223] In all clocking schemes, iMEM uses ‘parallel’ clocking for transitions between less frequently invoked systems/modules, and uses ‘anti-parallel’ between frequently invoked and interacting modules, as shown in FIG. 20 . The direction of the arrow in each module indicates the clock edge upon which transitions occur. Tasks represent a dual-port wrapper around RAM and hence show different clock edges. In particular, in one embodiment, the PEs are clocked on the rising edge, the resource manager unit on the falling edge, the scheduler unit and executive unit on the rising edge, the dataflow unit on the falling edge, the iMEM side of the memory on the rising edge and the host side of the memory on the falling edge.
IHIDDEN:
[0224] Although not necessary to the iMEM architecture, it is very desirable that the iMEM intelligence be hidden unless explicitly desired. Thus, the preferred implementation of the iMEM appears as a classical memory upon power-up, and requires activation by the host CPU before assuming any intelligent behavior.
[0225] Such activation could, of course, derive from external pins that the CPU manipulates through CPU I/O port(s) in the manner that PCI memory interface devices are made visible. (PCI configuration space).
[0226] The use of I/O ports is generally undesirable, and, in the case of a large number of iMEM devices in a system, even more so. For this reason the preferred “wakeup” method for iMEMs is classical memory compatible. That is, the algorithm applied to an iMEM awakens its intelligence, while the same algorithm applied to a classical memory has no unusual effect.
The “Wakeup” Algorithm
[0227] The preferred “wakeup” algorithm 952 for iMEM devices consists of a series of specific memory accesses to a specified memory address. For example and according to FIG. 21 , assume that address 16 in the iMEM address space is first read in step 954 , then a known sequence of bytes is written to the same address, say “(C)2000εKlingman,” as indicated by steps 956 to 960 . If this procedure is followed exactly, the iMEM awakens, and expects all relevant configuration information to exist in memory. Thus, before the wakeup algorithm is executed, the host CPU is expected to write relevant iMEM information into the memory.
[0228] After awakening, the iMEM performs any necessary testing on memory configuration data, and possibly other self-tests, and writes a summary byte, in step 960 , to the special address 16 . Thus, the CPU, after performing the above algorithms, can delay for a short specified time duration and then read address 16 , in step 962 , in iMEM space. If the value is ASCII ‘n’, the last value written by the CPU, then the memory is a classical memory, and does not exhibit intelligence. If the CPU reads a byte other than ‘n’ from address 16 , then the CPU can conclude that an iMEM occupies this address space, and, further, can determine the status of the iMEM after it has completed memory checks and self tests. This final CPU read of address 16 fully awakens the iMEM device, which begins task processing according to the information previously written to the iMEM by the CPU, as shown in FIG. 21 .
[0229] Although this sequence of iMEM access by the CPU is extremely specific and nonrandom, nevertheless, it is (somewhat) conceivable that the CPU could read address 16 in iMEM space, then, quite by accident, write the special 16 bytes to this address, and finally even read address 16 , thus inadvertently awakening the iMEM. To almost completely eliminate this possibility, the preferred iMEM implementation further checks to see that no address other than 16 is seen from the first read to the last read, including the 16 writes.
Processing Element Interface
[0230] As discussed earlier, the width of the datapath from memory to Processing Element is unspecified, but the preferred implementation uses an 8-bit data path. The following specification describes a preferred ASCII Floating-Point Computation Unit Processing Element interface. The interface consists of an eight-bit bi-directional data bus and the following control signals:
[0000] unit_ready 970 output unit_select 972 input func_write 974 input data_read 976 input data_write 978 input
And the following internal structures:
[0231] Tag_register 980
[0232] Function register 982
[0233] Status register 984
[0234] Accuracy register 986
[0235] Data register stack 988
[0236] In the preferred iMEM implementation, the Scheduler unit subsystem controls an array of unit select control signals, one per Processing Element. The Resource Manager unit controls the func_write 974 , data_read 976 , and data_write 978 signals, these three signals being shared by all Processing Elements, but only the selected Processing Element (the one receiving unit_select 972 ) responding to said signals. In similar fashion, the 8-bit bidirectional data bus 975 is shared by all Processing Elements, with every Processing Element except the selected one driving the data bus into the high impedance state. Each Processing Element controls a unit_ready signal 970 , with all such signals monitored by the Resource Manager unit.
[0237] During operation, if the Resource Manager unit determines that a given Processing Element is ready, and the specific Processing Element has received unit_select 972 , the Resource Manager unit drives a function code onto the data bus 975 , and asserts the func_write 974 strobe. The function code is written into the Processing Element where it is interpreted and used to specify the nature of the current transaction. The Resource Manager unit then removes the function code from the data bus 975 . If a data read operation is being performed, the Resource Manager unit places the data bus 975 in the high impedance state, and asserts the data_read control signal 976 , causing the Processing Element to drive the appropriate data onto the data bus 975 . If a data write operation is being performed, the Resource Manager unit asserts the data_write control signal 978 , and causes the data source to place data on the data bus 975 to be written to the selected Processing Element, where it is handled according to the function specified in the preceding step. The relevant signal timing and register structure is shown in FIG. 22 .
[0238] Although the present invention has been described in considerable detail with reference to certain preferred versions thereof, other versions are possible. Therefore, the spirit and scope of the appended claims should not be limited to the description of the preferred versions contained herein.
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An ASCII-based processing system is disclosed. A memory is divided into a plurality of logical partitions. Each partition has a range of memory addresses and includes information associated with a particular task. Task information includes contents of task state register and one or more task data registers, with each task data register having an ASCII name. Each task data register is successively labeled with a unique alphabetic character label starting with the character ‘A.’ A dataflow unit within the processing system is configured to manage a mapping between registers with ASCII names and the memory addresses of a particular task. Task instructions can include ASCII characters that indicate a request for resources and indicate the ASCII-character designated names of task data registers on which the task instruction operates. A processing element receiving the task instruction performs the operation indicated by the ASCII operator code on the indicated task data registers.
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BACKGROUND
The present invention relates to latching mechanisms for container closures. In particular the invention is concerned with a mechanism for latching in the closed position the door or drawer of a fire-resistant container for the protection of magnetic data media or other like temperature-sensitive articles (for convenience herein such containers will hereafter be referred to as "data cabinets"), although mechanisms according to the invention may be of more general utility in relation to the latching of container closures where similar design considerations apply.
It is evident that the door, drawer or other closure of a data cabinet must fit tightly to the body of the cabinet when closed in order to minimise the risk of hot gases leaking into the cabinet around the door under fire conditions. Furthermore it must be recognised that when exposed to a fire there is a considerable risk that thermal distortion of the cabinet--or impacts due to falling debris or the collapse of the floor upon which the cabinet is standing--may tend to open up gaps around the closure, particularly in the larger sizes of cabinet. For this reason it is desirable to provide a plurality of latching points for the closure. It is also an aim of the invention to provide a mechanism which, for user-convenience, permits slam-closing of the closure.
The invention accordingly resides in a latching mechanism for the closure of a container comprising a plurality of spaced-apart latching elements biased to extend into latching positions in which they are adapted to retain the closure in its closed position; means for withdrawing the latching elements from their latching positions in response to operation of a handle or other like user-operable member; retaining means for automatically retaining the latching elements in their withdrawn positions consequent upon the aforesaid withdrawal; and release means for automatically releasing said retaining means, thereby to allow the latching elements to move to their latching positions, consequent upon movement of the closure to its closed position.
The invention will now be more particularly described, by way of example, with reference to the accompanying drawings, in which:
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic vertical section through a data cabinet equipped with a latching mechanism according to the invention, with a portion of the cabinet shown in side elevation;
FIG. 2 is a schematic horizontal section through the cabinet of FIG. 1;
FIG. 3 is a view in the direction of the arrow "A" in FIG. 1 of a locking/triggering unit incorporated in the door of the cabinet, with the operating handle and cover plates removed; and
FIGS. 4a and 4b respective views in the direction of the arrow "B" in FIG. 2 of the mechanism at the central latching point for the cabinet door in its latched and released conditions.
DESCRIPTION OF THE INVENTION
Referring to FIGS. 1 and 2, the illustrated data cabinet has a body 1 comprising inner and outer steel skins between which is a filling 2 consisting of selected heat-insulating and heat-absorbing materials arranged to achieve the desired degree of temperature stability within the cabinet under fire conditions. The door 3 of the cabinet is hinged to the body at 4 and likewise comprises steel skins with a filling 5 of selected materials similar to the body filling 2. As is usual, the door and body have stepped profiles where they meet and the door is equipped in this region with a continuous seal 6 to minimise the in-leak of hot gases around the door under fire conditions.
When closed, the door is clenched tightly against the body to compress the seal 6, and is retained against opening by latches provided at three separate positions. At the top and bottom edges of the door bolts 7 and 8 are biased by springs 7a and 8a to extend into detentions 9 and 10 provided in the body. At a more central position on the opening side edge of the door there is a compartment 11 (FIG. 2) which houses a sliding latch plate 12 (to be more fully described below with reference to FIG. 4), this plate latching into a fixed bar 13 which extends forwardly from the side edge of the cabinet body. It is this central latch which in normal usage provides the clenching action for the door, i.e. the force holding the seal 6 in compression; the top and bottom bolts 7 and 8 in this condition have a slight clearance in their detentions, the purpose of the latter bolts being essentially to resist distortion movement of the the top and bottom of the door away from the body under fire conditions. The three latching elements 7, 8 and 12 are arranged to be released simultaneously to permit the door to open, by the mechanism now to be described.
A cranked operating handle 14 is pivoted on a horizontal axis 15 in a recess at the front face of the door. By pulling this handle forwards it is caused to pivot so as to depress its rearwardly-directed operating arm 16 (FIG. 1), the latter cooperating with a mechanism indicated generally at 17 in FIGS. 1 and 2 located in a compartment 17A behind the handle. This mechanism is more fully illustrated in FIG. 3 and includes a vertically-slidable plate 18 which is depressed when the arm 16 of the handle 14 pushes down on a roller 19 carried at the top end of the plate. Anchored to the top of this plate at 20 and 21 are two cables 22 and 23 which run through the door to the top and bottom bolts 7 and 8 respectively, so that as the plate 18 is depressed the bolts 7 and 8 are withdrawn from their detentions 9 and 10 against their spring biases by the plate 18 pulling the respective cables 22 and 23. A further cable 24 is anchored to the bottom of the plate 18 at 25 and runs over a pulley 26 mounted on a fixed spindle 27. From the pulley 26 this cable runs down through the door to the latch plate 12 shown in FIG. 4a. The latter plate is biased by springs 28 so that its nose portion 29 engages in a recess 30 in the fixed bar 13 carried by the cabinet body. It will be appreciated, however, that as the anchorage 25 is lowered with the plate 18 the cable 24 is pulled around the pulley 26 to raise up the latch plate 12 and release it from the bar 13.
Depressing the plate 18 by pulling the handle 14, therefore, serves to release each of the latching elements 7, 8 and 12 via the respective cables 22, 23 and 24 and opening of the door will automatically follow under the action of the compressive load in the seal 6 and the pulling force on the handle. As the door opens, however, a further function occurs as explained below.
With reference to FIG. 3, an L-shaped retaining member 31 is independently pivoted on the spindle 27 behind the pulley 26. This retainer is biased in the counter-clockwise sense (as viewed in FIG. 3) by a spring 32 attached to a fixed post 33 but, while the plate 18 is in its upper (latching) position the retainer is prevented from pivoting by an abutment block 34 carried by the plate 18 and engaging the face 35 of the short arm of the retainer. When, however, the plate 18 moves down under the action of the handle 14 the retainer is released by the block 34 to move counter-clockwise into a position in which its surface 36 now overlies the block 34 to prevent return, upward movement of the plate 18. A cable 37 is also anchored at 38 to the end of the long arm of the retainer and runs down to a second sliding plate 39 behind the latching plate 12 at the central latching point (FIG. 4). In the latched condition of the door the plate 39 is held down by a flange 40 at its lower end engaging under the end of the bar 13, but as the door opens this plate is released by the bar and rises up to the FIG. 4b position under the action of the cable 37 as the retainer 31 is permitted to pivot counter-clockwise as described above. In the position assumed by the retainer 31 after door opening--i.e. holding down the plate 18--it will be appreciated that all three latching elements 7, 8 and 12 are held by their respective cables 22, 23 and 24 to lie in their retracted positions and thus pose no impediment to the subsequent slam-closing of the door.
As the door is slammed shut from the above-described condition, its side edge approaches the fixed bar 13 in the sense of arrow "C" in FIG. 4b and the flange 40 on the sliding plate 39 engages the inclined surface 41 of the bar 13 during the last part of the closing movement, so as to cam that plate downwards and, through the cable 37, sharply pull off the retainer 31 from the abutment block 34. The plate 18 is thus now freed to spring up and allow the mechanism 17 to return to the condition shown in FIG. 3, as the now-released latching elements 7, 8 and 12 shoot simultaneously under their spring biases into their detentions 9, 10 and 30 to retain the door in its closed condition. Operation of the handle 14 to close and latch the door is not therefore required.
In order that the door becomes properly clenched when slam-closed it is of course essential for the central latching plate nose 29 to engage in the recess 30 of bar 13. It is therefore important that the release of the retainer 31--and the consequent release of the latch plate 12--is in proper synchronism with the passage of the nose 29 over the recess 30. A situation which could occur if the timing is not correct is that the latch plate 12 is held up over the bar 13 while the top and bottom bolts 7 and 8 (which have a larger clearance in their detentions) are shot; the door would therefore appear to be properly closed but its clenching would not in fact be complete. In order that this timing can be properly set the anchorage 38 for the cable 37 to the retainer 31 accordingly includes a screw adjuster as seen in FIG. 3.
For locking the door when closed, any suitable key- or other code-operated mechanism can be provided for disabling the operation of the mechanism 17. In FIG. 3 this is exemplified by a pair of locks 42 whose bolts 43 when thrown block the downward movement of respective plates 44 attached to the plate 18.
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A data cabinet door has a plurality of latch bolts connected by cables to a central actuating plate. When the plate is depressed by a handle to release the bolts it is itself retained in the released position by a lever acting under the bias of a spring, to keep the bolts withdrawn. This lever is connected by a cable to a release plate associated with one of the latches so that when the door is slam-closed the release plate engages an abutment on the cabinet body and pulls the lever to release the plate, which latter springs up once more and permits all the latches to engage.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 07/892,076, filed Jun. 2, 1992, now abandoned, which in turn is a continuation-in-part of U.S. patent application Ser. No. 07/633,810, filed on Dec. 26, 1990, and issuing as U.S. Pat. No. 5,147,197, on Sep. 15, 1992.
FIELD OF THE INVENTION
This invention relates generally to melt spinning filaments or fibers using a spinneret. More particularly, this invention relates to an apparatus for changing the number and size of filaments being spun from a single spinneret.
BACKGROUND OF THE INVENTION
Spinneret assemblies for spinning synthetic filaments or fibers typically include an inlet block having an inlet port through which the material to be spun is introduced into the spinneret assembly and a chamber containing filtering material, a distribution plate, a distribution cavity, a metering plate and a spinneret plate. The metering plate includes a number of apertures having a compound shape, consisting of a capillary and a counterbore. The spinneret plate normally includes a corresponding number of bores having a compound shape consisting of a counterbore and a capillary or spinning orifice.
U.S. Pat. No. 3,095,607 to Cobb describes a typical spinneret assembly. Other spinneret assemblies are described in U.S. Pat. No. 3,028,627 to McCormick; U.S. Pat. No. 2,883,261 to McGeorge; U.S. Pat. No. 3,225,383 to Cobb; U.S. Pat. No. 3,289,249 to Nakayama et al.; U.S. Pat. No. 3,601,846 to Hudnall; U.S. Pat. No. 3,659,988 to Walczak; and U.S. Pat. No. 4,738,607 to Nakajima et al.
It is sometimes desirable to change the number of filaments or deniers of the filaments being spun from a single spinneret. Reasons for altering the filament count may include product variations, keeping the total tow denier constant while changing the individual filament denier, changing quenching characteristics and maintaining spinning speed at higher denier per filament where extruder capacity is limited. Also, mixed denier filaments produce unique product characteristics.
The traditional method for changing filament count is to individually plug spinneret capillaries using a soft metal bar of approximately the same diameter as the counterbore. This method is time consuming, risks damage to the spinneret, and does not insure a leak-free seal.
The traditional method of generating mixed deniers is to make expensive, precision metering plates for each mixture.
Another known method for spinning a number of different filament counts from a single spinneret plate is described in U.S. Pat. No. 3,336,633 to Curran. Curran employs metering plates having a number of apertures lower than the number of orifices in the spinneret plate. Since the compound shape of the apertures in the metering plate are normally precision drilled to provide a desired pressure drop, the metering plates are relatively expensive to produce and maintaining a stockpile of metering plates to provide a variety of fiber counts may be cost-prohibitive.
U.S. Pat. No. 2,980,492 to Jamieson et al. describes an apparatus for making mixed denier filaments. The apparatus requires two separate cavities within a single spin pack. Each cavity corresponds to its own portion of the spin pack. This complicated arrangement allows polymer to be fed at two different feed rates, thereby making different denier filaments.
SUMMARY OF THE INVENTION
It is an object of the invention to provide a simple and inexpensive apparatus for changing the filament count and denier mixture from a spinneret plate.
It is also an object of the invention to provide an apparatus which provides a good seal of one or more capillaries of a spinneret plate without endangering the very expensive spinneret capillaries.
It is a further object of this invention to economically change the deniers of individual filaments in a single yarn spun from the spinneret while avoiding the high cost and expense of purchasing new precision metering plates.
These objectives and other advantages are achieved by providing a sealing plate upstream of the spinneret.
One aspect of the present invention involves a spinneret assembly including a spinneret plate with an upstream side and having a number of bores, each bore with one or more tapered sections; and a sealing plate adjacent to the upstream side of the spinneret plate and forming an interface therewith. The sealing plate has cylindrical flow channels formed therein. At least some of said flow channels have a first diameter and at least some of said flow channels have a second diameter which is smaller than the first diameter. Each of said flow channels corresponds in position to a bore in the spinneret plate.
In another aspect of the invention, a spinneret assembly includes a spinneret plate with an upstream side having a number of bores, each bore with one or more tapered sections; and a sealing plate positioned upstream from the spinneret plate. The sealing plate has cylindrical flow channels which are fewer in number than the bores. Each of the flow channels corresponds in position to a bore in the spinneret plate.
Yet another aspect of the present invention involves a spinneret assembly for extruding polymeric material under pressure, including a spinneret plate having a number of bores and an upstream side; and upstream thereof, and next adjacent thereto, a sealing plate made of a material and having flow channels therein and which sealingly deflects under spinning pressure. The deflection does not exceed the ultimate plastic limit of the sealing plate material. Each of the flow channels corresponds in position to a bore in said spinneret plate.
The present invention will now be described more fully with reference to the accompanying drawings, in which illustrative embodiments of the invention are shown. This invention can, however, be embodied in many different forms and the invention should not be construed as being limited to the specific embodiments set forth herein. Rather, Applicants provide these embodiments so that this disclosure will be thorough and complete and will fully convey the intent of the invention to those skilled in the art.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded perspective view of the spinneret assembly in accordance with the invention.
FIG. 2 is a partial axial longitudinal section of an alternative embodiment of a spinneret assembly in accordance with the invention.
FIG. 3 is a partial axial longitudinal section of another alternative embodiment of the present invention.
FIG. 4 is a partial cross-section of a modification of the embodiment of FIG. 3.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 1, a spinneret assembly includes an inlet block 3 and a spinneret plate 4. The spinneret plate 4 includes a number of bores 5. The bores 5 may be of compound shape, having a relatively large counterbore 6 at the upstream side and a relatively small spinning orifice 7 through which the material being spun exits the spinneret plate 4.
Between the inlet block 3 and the spinneret plate 4 is sealing plate 10. Sealing plate 10 includes one or more flow channels 11, each of which is positioned to correspond with one of the bores 5 in the spinneret plate 4. The sealing plate 10 contains at least one less flow channel 11 than the number of bores 5 in the spinneret plate 4. Thus, the sealing plate 10, will block at least one bore 5 of the spinneret plate 4, preventing the passage of the material being spun, thereby changing the filament count from the spinneret. As seen in FIG. 1, there is no flow channel corresponding to bore 5a in spinneret plate 4, thereby changing the filament count from 5 to 4 from the illustrated spinneret. Surprisingly, as illustrated in the Examples below, the denier and number of filaments may be adjusted with the present invention.
Sealing plate 10 can be manufactured from any suitable material, such as, for example, mild steel, stainless steel, brass or aluminum. However, the material characteristics will dictate the appropriate thickness of the sealing plate. The thickness of the sealing plate must be such that the plate deflects to form a seal around the edge of the counterbore of the spinneret capillary. However, the sealing plate must not be so thin that the pressure above the seal generates a force great enough to exceed the ultimate plastic limit of the material in the shearing zone generated at the edge of the counterbore. This could result in bursting of the sealing plate and loss of the seal. In the case where the sealing plate is also used to adjust the diameter of the filaments, the thickness and properties of the sealing plate must be further limited to prevent failure at the sealing plate aperture (metering hole) due to generation and propagation of a crack. This can be further reduced by the method of aperture manufacture. For example, cleanly drilled, punched, etched or machined round holes are less likely to initiate cracks than non-round or jagged holes.
Sealing plate 10 and flow channels can be formed by any suitable manufacturing technique such as, for example, die cutting, drilling, punching, stamping, etching, machining, or molding. Any suitable means may be employed to align the various components of the spinneret assembly in precise register with each other and to maintain the assembled spinneret assembly in a tight fitting relationship. For example, apertures (not shown) may be formed in each component which, in the assembled spinneret assembly, provide thruways accommodating terminally threaded aligning bolts or rods (not shown) which receive locking nuts (not shown).
The overall dimensions of the spinneret plate 4 and the sealing plate 10 may vary considerably. In general, the spinneret plate and the sealing plate will have the same or substantially the same planar dimensions. While in some instances spinneret plates may be as large as a few feet in length, typically, the planar dimensions range from about 1.0 to about 12 inches in length and about 1.0 to about 8.0 inches in width. The thickness of the spinneret and sealing plate may be the same or different. Preferably, however, the sealing plate 10 will be substantially thinner than the spinneret plate 4. Typically, the thickness of spinneret plate 4 is between about 0.25 and about 1.5 inches, while the thickness of sealing plate 10 is preferably between about 0.003 and about 0.1 inches.
The location or pattern of the bores 5 in spinneret plate 4 and the corresponding flow channels 11 in sealing plate 10 may also vary considerably. Additionally, the diameter of the bores 5 and the flow channels may vary, ranging, for example, between about 0.1 to about 0.3 inches in diameter. Preferably, the diameter of the flow channel 11 corresponds to the diameter of the counterbore 6 at the upstream side of spinneret plate 4.
Referring now to FIG. 2, in another embodiment of the invention, the spinneret assembly includes an inlet block 23, a metering plate 28, and a spinneret plate 24. Sealing plate 30 is located between the metering plate 28 and the spinneret plate 24.
The metering plate 28 has a number of apertures 29 bored therein. The number and location of the apertures 29 in the metering plate 28 correspond to the number and location of bores 25 in the spinneret plate 24. The sealing plate 30 includes a number of flow channels 31 formed therein.
The flow channels 31 are positioned to correspond with the apertures 29 in the metering plate 28 and the bores 25 in the spinneret plate 24. The sealing plate 30 contains at least one less flow channel 31 than the number of apertures 29 and bores 26. Thus, the sealing plate 30 will prevent the passage of the material being spun from aperture 29a to bore 25a, thereby reducing the filament count from the spinneret.
The sealing plate may also contain apertures of different sizes as shown in FIG. 3. FIG. 3 shows in cross-sectional elevation another embodiment of the spin pack of the present invention. As shown, spinneret assembly 50 includes inlet block 52, plate 54, sealing plate 56 and spinneret plate 58.
Plate 54 has a number of apertures 60 bored therein. The number and location of apertures 60 correspond to the number and location of bores 62 in spinneret plate 58.
Sealing plate 56 includes a number of flow channels therein. Two sizes of flow channels are shown. Larger channels 64 facilitate larger denier filaments when molten polymer passes therethrough to spinneret plate 58 and bores 62. Small channel 66 likewise facilitates small denier filaments. The larger channels may be as large as the opening diameter of the spinneret plate.
FIG. 4 is a partial cross-section of a modification of FIG. 3 wherein one spinneret bore 62a is sealed by sealing plate 56a.
As shown, when apertures are of different sizes, they may or may not be fewer in number than bores 62. This causes differing flows to proceed to the spinneret capillaries. The total flow through any component flow channel is determined by the total pressure drop. Orifices in a spinneret or a metering plate usually are identical so that uniform filament cross-section and denier per filament (DPF) can be achieved. With the sealing plate of the present invention having varying hole sizes in the plate, a unique yarn with different filament deniers and geometries can be made using the normal spinneret or spinneret-metering plate combination.
While not wishing to be bound by theory, the following may explain the operation of the present invention. At the top of the sealing plate (or metering plate if one is used), polymer pressure is generally equalized from channel to channel due to the rather free lateral flow of polymer. This results in approximately the same pressure drop for different polymer paths from the sealing plate (or metering plate) top to the spinneret bottom face as governed by the following equation: ##EQU1## where ΔP i and ΔP j denote polymer pressure drops for two arbitrary polymer paths, and the subscript k denotes the Kth segment in an individual polymer path. Polymer pressure drop of a segment can be obtained from: ##EQU2## where L k , A k , D hk are the segment length, area and hydraulic diameter respectively. λ k is the segment (orifice) shape factor. The polymer rheological parameters, m k and n k , are based on the assumption that the polymer obeys the power law as defined by π=mγ n , where π is the shear stress and γ is the average wall shear rate. Q i is the volumetric rate of polymer flow in that channel. Since a filament denier is proportional to the polymer flow rate of the channel it comes from, the denier ratio of two filaments is equal to the ratio of corresponding polymer flow rates. If the power law parameters of a polymer (m and n) are known, the denier ratio of any two filaments can be calculated according to Equations 1 and 2 by using actual dimensions of the orifices (holes).
If polymer shear rates in different channels and segments are within a power of ten, the DPF ratio (R dpf ) of an arbitrary filament to the smallest filament in the yarn can be estimated by the following simplified equation: ##EQU3## where DPF n and DPF o are the deniers of an arbitrary and the smallest filament in the yarn and D r is the diameter ratio of the arbitrary hole to the smallest hole. L sk , S sk and A sk are the length ratio, perimeter ratio and area ratio of a segment to the smallest hole in the sealing plate. Dr is the sealing plate diameter ratio. An average value for n for the shear rate range should be determined.
It should be understood that the sealing plate may be positioned adjacent to the upstream face of the metering plate, or at any other position in the spinneret assembly provided that the sealing plate prevents the passage of the material to be spun into one or more particular spinneret bores, thereby changing the filament count.
EXAMPLE 1
A series of continuous filament yarns is made using nylon 6 polymer of 2.7 relative viscosity. The molten polymer is extruded through a spinneret with 102 trilobal-shaped orifices, each comprising three intersecting slots of 0.125 mm wide and 0.914 mm long. Main operating conditions are: polymer temperature 270° C., polymer throughput 246 g/min/spinneret, quench air flow rate 93.9 ft/min (28.6 m/min) and winding speed 650 m/min. Three spinneret packs are made using the configuration demonstrated in FIG. 2 with 75, 60 and 49 open channels, respectively, in the sealing plates. The sealing plates are 0.003" (0.076 mm) thick with 0.047" (1.19 mm) diameter holes. A control spin pack is also made using the same configuration but without a sealing plate. Although polymer throughput was the same, yarns produced by these four spin packs are different in number of filaments, DPF and modification ratio (MR) as listed in TABLE 1.
TABLE 1______________________________________ Control Sample Identification A B C D______________________________________Yarn denier 3685 3647 3656 3654Number of filaments 102 75 60 49Denier per filament 36.1 48.6 60.9 74.6Modification ratio 2.64 2.80 3.20 2.92______________________________________
EXAMPLE 2
A series of continuous filament yarns is made using nylon 6 polymer of 2.7 relative viscosity. The molten polymer is extruded through a spinneret with 68 trilobal-shaped orifices which are identical to the orifices described in EXAMPLE 1. Main operating conditions are: polymer temperature 270° C., polymer throughput 177 g/min/spinneret and winding speed 600 m/min. Three spinneret packs are made using the configuration demonstrated in FIG. 2 with 58, 52 and 46 open channels in the sealing plates. The sealing plates are 0.003" (0.076 mm) thick with 0.047" (1.19 mm) diameter holes. Another spin pack is also made using the same configuration but having 85 orifices in the spinneret and without a sealing plate. Quenching air flow rate was adjusted for each spin pack to get the same 3.0 modification ratio for all four yarns. Yarns produced by these four spin packs differ in number of filaments and DPF as listed in TABLE 2.
TABLE 2______________________________________ Control E F G H______________________________________Yarn denier 1108 1133 1111 1119Number of filaments 85 58 52 46Denier per filament 13.0 19.5 21.4 24.3______________________________________
EXAMPLE 3
A continuous filament yarn is made using nylon 6 polymer of 2.7 relative viscosity. The molten polymer is extruded through a spinneret with 102 trilobal-shaped orifices which are identical to the orifices described in EXAMPLE 1. The spinneret pack is made using the configuration demonstrated in FIG. 3. The sealing plate is 0.400 mm thick. Holes in the sealing plate are in two different sizes as shown in FIG. 3 and with diameters of 3.175 mm and 0.350 mm respectively. Main operating conditions are: polymer temperature 270° C., polymer throughput 287 g/min/spinneret, quench air flow rate 97.5 ft/min (29.7 m/min) and winding speed 630 m/min. The whole yarn is 4154 denier. The resultant filament DPFs and MRs are listed in TABLE 3.
TABLE 3______________________________________ No. of Holes Hole DiameterFilament Size or Filaments (mm) DPF MR______________________________________Large 17 3.175 100.2 3.01Small 85 0.350 28.8 2.64______________________________________
EXAMPLE 4
Two continuous filament yarns are made using nylon 6 polymer of 2.7 relative viscosity. The molten polymer is extruded through a spinneret with 68 trilobal-shaped orifices which are identical to the orifices described in EXAMPLE 1. Two spinneret packs are made using the configuration demonstrated in FIG. 3. The sealing plates are 0.015" (0.381 mm) thick. Holes in each sealing plate are in two different sizes. Main operating conditions are: polymer temperature 270° C., polymer throughput 177 g/min/spinneret, quench air flow rate 93.9 ft/min (28.6 m/min) and winding speed 600 m/min. Each yarn produced contains filaments with two different sizes. The hole sizes and filament properties are listed in TABLE 4.
TABLE 4______________________________________Sample Filament No. of Holes Hole DiameterNo. Size or Filaments (mm) DPF MR______________________________________Il Large 14 1.588 53.8 3.37Is Small 54 0.794 37.9 3.27Jl Large 14 3.175 57.4 3.27Js Small 54 0.794 36.9 3.09______________________________________
EXAMPLE 5
A series of continuous filament yams is made using nylon 6 polymer of 2.7 relative viscosity. The molten polymer is extruded through a spinneret with 68 trilobal-shaped orifices which are identical to the orifices described in EXAMPLE 1. Three spinneret packs are made using the configuration demonstrated in FIG. 3. The sealing plates are 0.020" (0.508 mm) thick. Holes in each sealing plate are in two different sizes. Main operating conditions are polymer temperature 270° C., polymer throughput 177 g/min/spinneret, quench air flow rate 93.9 ft/min (28.6 m/min) and winding speed 600 m/min. Each yarn produced contains filaments with two different sizes. The hole sizes and filament properties are listed in TABLE 5.
TABLE 5______________________________________Sample Filament No. of Holes Hole DiameterNo. Size or Filaments (mm) DPF MR______________________________________Kl Large 24 1.588 50.1 3.09Ks Small 44 0.794 34.9 2.95Ll Large 24 2.381 54.5 3.05Ls Small 44 0.794 33.6 2.99Ml Large 24 3.175 55.4 3.05Ms Small 44 0.794 32.5 2.96______________________________________
As will be appreciated by those skilled in the art, the cost of manufacturing a number of sealing plates for use in accordance with the present invention is significantly less than the cost of producing a corresponding number of metering plates or spinneret plates to effect various changes in filament count or denier mixtures. This is due primarily to the ease and simplicity of forming the flow channels in the sealing plate of the invention compared to the difficulties encountered in forming the compound shape of the precision drilled apertures in metering plates and spinneret plates.
The foregoing description is to be considered illustrative rather than restrictive of the invention, and those modifications which come within the meaning and range of equivalence of the claims are to be included therein.
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A sealing plate upstream of a spinneret has cylindrical flow channels, at least some of which have a first diameter. Each of the flow channels corresponds in position to a bore in the spinneret plate. The number and denier of extruded filaments can be altered by simply changing the plate. The plate provides a seal by deflecting under the extrusion pressure.
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RELATED APPLICATIONS
[0001] This application is a continuation claiming priority benefit of U.S. Ser. No. 13/541,536 filed Aug. 8, 2015 and U.S. Ser. No. 61/504,873, filed Jul. 6, 2011 incorporated herein by reference.
BACKGROUND OF THE DISCLOSURE
Field of the Disclosure
[0002] This disclosure relates to the field of fabric (i.e. clothes) washing apparatus which are portable, and operable without a running source of water, and without a power source. The washing apparatus operates with a volume of liquid cleaner (water) and manual manipulation of a handle.
SUMMARY OF THE DISCLOSURE
[0003] Disclosed herein is a portable washing apparatus for the washing of fabrics. The washing apparatus in one example comprising: a base member configured to fit within a watertight container; a frame extending vertically from and removably attached to the base member; a cross support extending horizontally across the frame and removably attached thereto; and an agitator having a lower end attached to the base member so as to freely rotate thereupon. The agitator having an upper end attached to the cross support so as to freely rotate there under. The washing apparatus may also include a driving portion having a user-engagement handle, a shaft, and an agitator engagement portion. The driving portion may utilize a system of detents and grooves whereupon oscillating vertical movement of the driving portion by the user is translated to rotary movement of the agitator.
[0004] In one form, the portable washing apparatus as disclosed is arranged wherein the base member comprises a plurality of identical base portions which are removably connected to each other to form the base member.
[0005] The portable washing apparatus may also be arranged wherein the frame comprises a plurality of vertical supports. Each vertical support having a lower end removably attached to the base and an upper end removably attached to an upper ring.
[0006] The frame of the portable washing apparatus may comprise: a cross support having a surface defining a non-cylindrical hole therein; wherein the driving portion comprises a non-cylindrical shaft; and wherein the non-cylindrical hole engages the non-cylindrical shaft an prohibits rotation of the driving portion relative to the frame.
[0007] The driving portion of the portable washing apparatus as may also comprise at least one detent extending radially therefrom. Wherein the agitator comprises a surface defining a bore; and wherein the bore comprises surfaces defining at least one spiral indent which receive the detents extending radially from the driving portion such that linear oscillation of the driving portion results in rotational movement of the agitator.
[0008] The portable washing apparatus also may include at least one spiral indent which is arranged such that linear oscillation of the driving portion results in rotational oscillation of the agitator.
[0009] The portable washing apparatus in one form is configured to fit entirely or substantially within a portable fluid container (rigid or collapsible) during operation.
[0010] The portable washing apparatus may be formed wherein the base member comprises a plurality of raised portions extending longitudinally therefrom so as to maintain a significant portion of the base member above the lower inner surface of a portable fluid container during operation to function as a dirt trap.
[0011] The portable washing apparatus as disclosed may include a plurality of extensions protruding from a longitudinal central member.
[0012] The portable washing apparatus may also be arranged wherein the frame comprises a plurality of clamp arms which engage the upper surface of a rigid portable fluid container so as to maintain position of the frame relative to the rigid portable fluid container.
[0013] The portable washing apparatus as disclosed may utilize a cover substantially enclosing the apparatus with or without a separate cross member.
[0014] The portable washing apparatus as disclosed may utilize a collapsible bag, a rigid bucket, or other fluid container or reservoir. The collapsible bag may be positioned radially within a plurality of vertical supports, or may be positioned external of the vertical supports.
[0015] A portable washing apparatus for the washing of fabrics is disclosed. The washing apparatus comprising: a bottom plate configured to fit external of a watertight container; a base member configured to fit within the watertight container; a frame extending vertically from and removably attached to the bottom plate. A cross support may be included, extending horizontally across the frame and removably attached thereto. An agitator having a lower end attached to the base member so as to freely rotate thereupon is positioned within the watertight container. The agitator having an upper end attached to the cross support so as to freely rotate there under. A driving portion having a user-engagement handle, a shaft, and an agitator engagement portion is also included. The driving portion and agitator having a system of detents and grooves whereupon oscillating vertical movement of the driving portion by the user is translated to rotary movement of the agitator.
[0016] In one form, the cross member comprises a cover substantially enclosing the apparatus.
[0017] In one configuration, the bottom plate comprises a plurality of identical plate components; and the cover comprises a plurality of the identical plate components.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] FIG. 1 is an isometric view of the disclosed apparatus in one configuration.
[0019] FIG. 2 is an isometric view of the apparatus of FIG. 1 within a container.
[0020] FIG. 3 is a plan view of the apparatus of FIG. 1 in a disassembled configuration.
[0021] FIG. 4 is an end view of the configuration of FIG. 3 .
[0022] FIG. 5 is a side view of an agitator component of the apparatus of FIG. 1 .
[0023] FIG. 6 is an end view of the component of FIG. 5 .
[0024] FIG. 7 is a side cutaway view of the component of FIG. 6 taken along line 7 - 7 .
[0025] FIG. 8 is a side view of an operating handle component of the apparatus of FIG. 1 .
[0026] FIG. 9 is an isometric view of the top side of a split base component of the apparatus of FIG. 1 .
[0027] FIG. 10 is an isometric view of the bottom side of the component of FIG. 9 .
[0028] FIG. 11 is a top (plan) view of a cross member component of the disclosed apparatus.
[0029] FIG. 12 is a side hidden line view of the cross member component shown in FIG. 11 .
[0030] FIG. 13 is a bottom hidden line view of the cross member component shown in FIG. 11 .
[0031] FIG. 14 is an isometric view of the disclosed apparatus with a top cover and additional bottom plate.
[0032] FIG. 15 is a front view of the apparatus as shown in FIG. 14 .
[0033] FIG. 16 is a first vertical view of a plate component of the disclosed apparatus.
[0034] FIG. 17 is a side view of the plate component shown in FIG. 16 .
[0035] FIG. 18 is a second vertical view of the plate component shown in FIG. 16 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0036] Before beginning a detailed description, an axes system 10 is shown in FIG. 1 comprising a vertical axis 12 , and a radial axis 14 which is centered upon the center of the long axis of the agitator component 22 and is directed radially outward. This axes system is intended to aid in description of the disclosed apparatus and is not intended to be limiting.
[0037] Looking again to FIG. 1 , one configuration of a portable washing apparatus 20 is shown. The portable washing apparatus 20 generally comprises three independent but interoperating portions: a driving portion 24 , a frame portion 26 , and an agitator portion 28 . Each of these portions are assembled together for a washing device which does not require running water to operate, and also does not require a power source such as wind, hydro, electric, or other outside power sources. While the apparatus may be mechanized, it operates well with a user (human) simply filling the machine with a cleaning fluid and then manipulating the handle.
[0038] Looking to FIG. 2 , the apparatus is configured wherein a fluid holding container 102 is also provided. The container 102 in this configuration surrounds the frame portion 26 , and agitator portion 28 . In another configuration, the container 102 may be provided between the frame portion 28 and agitator portion 28 . This fluid container 102 may be a rigid element such as a bucket, barrel, or similar apparatus, or may be a flexible container such as for example a bag. Collapsible buckets may be especially useful as they are easily collapsed and thus take up less space for shipping or storage.
[0039] Returning to FIG. 1 , the frame portion generally comprises a base 30 which in one form comprises a first portion 32 and second portion 34 with a seam 36 therebetween. The configuration of these portions can be more easily seen in FIGS. 9 and 10 where it can be seen that to reduce manufacturing and replacement costs, the first portion 32 and second portion 34 may be formed as identical components. By using the illustrated semicircular portions, interconnected by way of a plurality of surfaces defining holes 38 and interoperating detents 40 a single molded component can form both of these first and second portions 32 / 34 . In addition, the bottom side 42 may comprise a plurality of raised portions 44 providing a fluid gap between the base 30 and the lower inner surface of the container 30 to increase the cleaning action of the apparatus. Additionally, a plurality of channels 46 may be formed in the upper surface 48 of the base 30 to further increase cleaning action, as well as provide additional rigidity and support to the overall apparatus. In one form, the raised portions 44 fit within channels 46 to improve stackability of the apparatus. In the drawings, the mating surface 50 between individual components is planar, although other shapes could alternatively be utilized.
[0040] A plurality of vertical supports 52 may be provided as shown in FIGS. 1 , 3 , and 4 which provide vertical separation between the base 30 and an upper ring 54 . One of the vertical supports is not shown in FIG. 1 , so that the surfaces defining holes 58 and 60 can more clearly be seen. The upper ring 54 may also be comprised of separate and interconnecting components. In the drawings, the components are semicircular, but other shapes may also be used. In one configuration, the lower end 56 of the vertical supports 52 fits into one of several surfaces defining holes 58 in the base 30 . These surfaces defining holes 58 may also be seen in FIGS. 9 and 10 . In FIG. 1 , one of the vertical supports 52 is removed to show the holes 58 in the base 30 , as well as one of several holes 60 in the upper ring 54 .
[0041] In one configuration, the upper end 62 of the vertical supports 52 comprises a pin 64 to interconnect the individual components of the upper ring 54 , and maintain relative position between the upper ring 54 and the vertical supports 52 .
[0042] In one configuration, a cross support 66 is utilized as shown in FIGS. 1 and 2 comprising a surface defining a central void 68 for receiving of the driving portion 24 . In FIGS. 11-13 it can be seen how in this embodiment, the void 68 is non-circular so as to prohibit rotation of the driving portion 24 relative to the cross support 66 .
[0043] In one configuration, the cross support 66 comprises recesses 70 for maintaining proper position upon the upper ring 54 , as well as surfaces 72 for maintaining the apparatus 20 in relative position to the container 30 . In one form as shown in FIG. 2 , the cross support 66 comprises clamp arms 74 which further hold the container 30 in position relative to the cross support 66 . In this embodiment, both the cross support 66 and clamp arms 74 are also held in position by the pins 64 on to which they are pressed.
[0044] In one form, a collapsible bag 108 may be utilized which fits over the apparatus and comprises grommets 110 , holes, strings, etc. which fit over the pins 64 . The upper ring 54 is then installed over the grommets, and this assembly holds the bag in place. In another form, the bag may fit within the vertical supports 52 in the same manner.
[0045] Looking to FIG. 5 , a detail view of the agitator 22 in one configuration is shown. While this configuration comprises a plurality of four extensions 76 (three of which can be seen in this figure) and each extension 76 comprises hills 78 and valleys 80 . Each of the extensions 76 being attached to or formed as extensions of a central member 104 . The particular arrangement of these surfaces is not critical as many different configurations could be utilized for aesthetic or functional purposes. An end view of the four arm embodiment, is shown in FIG. 4 . As shown in FIG. 5 , a recess 82 is provided in the upper end of the agitator 22 which fits upon a matching surface 98 of the cross support 66 as can be seen in FIGS. 12 and 13 . Additionally, on the other vertical end, a bearing 84 is provided which fits within and revolves upon a surface 86 defining a bore or bearing surface as shown in FIGS. 9 and 10 . This bearing 84 as shown in FIG. 7 may also provide a cap to prohibit pumping action of cleaning water through the center 86 of the agitator 22 during operation. These surfaces 82 / 84 at the upper and lower vertical ends of the agitator 22 maintain the agitator 22 in relative position to the other components or portions of the apparatus 20 as it is being rotated (actuated).
[0046] Looking to FIG. 7 , a cross sectional view of this configuration of the agitator 22 is shown wherein the inner surface 86 of the agitator 22 is configured to receive detents extending from the driving portion 24 . In particular, looking to FIG. 8 it can be seen how the driving portion 24 comprises a shaft 88 which may be non-cylindrical, and a handle 90 which is configured to be grasped by the user while being moved (actuated) in an oscillating vertical motion as shown by the arrow 92 . Non-cylindrical being defined herein as a longitudinal extrusion of a geometric shape, wherein the geometric shape is not a circle. At the lower end of the driving portion 24 , a plurality of detents 94 may be provided which are configured to engage a plurality of helical “rifling” channels 96 formed within the inner surface 86 of the agitator 22 as seen in FIG. 7 . In this embodiment, the cross support 66 as already described does not permit relative rotation of the driving portion 24 , and also does not permit vertical movement of the agitator 22 . Thus, as the handle 90 is oscillated vertically, the detents 94 rotate the agitator 22 back and forth in direction of travel 100 shown in FIG. 1 as can be understood by one of ordinary skill in the art.
[0047] In an alternate configuration, the components are reversed such that the shaft 88 comprises the helical rifling portion, and the engaging surface of the agitator 22 is linear. Other mechanisms such as a system of gears may be utilized instead of the helical rifling portion.
[0048] In yet another alternate configuration, the detents may be formed in a spiral shape and engage grooves in the opposing component.
[0049] Looking to FIGS. 3 and 4 , it can be seen how the entire apparatus can be disassembled into its component parts easily, and in some configurations without tools. This makes the apparatus particularly useful where shipping and/or storage is difficult, while backpacking, and in other environments where more industrialized ways of cleaning clothing are commonplace.
[0050] FIGS. 14-15 show a configuration wherein a bottom plate and top cover 114 are provided. The bottom plate 112 is placed under the base member 30 and the top cover 114 may operate with a cross member similar to that shown in FIGS. 11-13 or may serve the same function. As shown, a bag 108 is provided and places radially inward of the supports 52 and external of the base member 30 and agitator 22 . Again, the bag 108 may have grommets 110 or similar fasteners to attach to the upper end of the frame, such as at the upper end of the supports 52 .
[0051] FIGS. 16-18 show one example of the disclosed cover 114 and bottom plate 112 which again may be formed of a single cast. For example a plurality of the plate components 126 may be provided wherein a single cast component forms both sides of each of the cover 114 and bottom plate 112 . In this example, the surface 98 ′ functions in the same way as the surface 98 previously disclosed. A plurality of holes 118 ′ are provided for attachment to either the upper or lower end of the supports 52 . A groove 120 is provided to assist in alignment of the supports 52 during assembly. Groove 120 also serves as a lip to fit over the outer edge of solid containers and to minimize splashing of water outside of the container while operating the handle. The groove may also be shaped to snap lock onto the side of a solid container such as a lid for a standard 5 gallon bucket. Each plate component 126 in this example also comprises a recess 122 and a projection 124 which engage opposing surfaces of an adjacent component 126 to form the bottom plate 112 or top cover 114 .
[0052] One added benefit of this example is the ease in which a component may e replaced. As several identical supports 52 , several identical plates 126 , and several identical base portions 32 are used in each assembly, there are fewer unique parts. A single replacement plate 126 may be used to replace one of the four plates used in this example if broken or damaged.
[0053] One form of assembling this example is to assemble the bottom plate 112 by connecting two plate components 126 with the grove side up, then attaching a number of the supports 52 to the bottom plate. The bag 108 may then be positioned within the supports 52 and attached at the top thereof. The base member 30 may then be assembled and placed into the bag 108 . The agitator 22 and driver 24 may then be attached to the base member 30 . The bag 108 may then be filled with cleaning fluid and fabric (i.e. clothes). The cover 114 may then be assembled about the shaft 88 and attached to the upper end of the supports 52 . As previously mentioned, the handle 90 may then be manipulated to rotate the agitator 22 and clean the fabric.
[0054] In one form, each of the components could be made of plastics or plastic equivalents to reduce in cost, or alternatively could be made of metals or natural materials where such materials are more plentiful and replacement parts are easier to manufacture when made of these materials. Generally, ease of manufacture by casting has been taken into account, and the majority of the parts can easily and cheaply be cast either in plastics, metals, or other such materials.
[0055] While the present invention is illustrated by description of several embodiments and while the illustrative embodiments are described in detail, it is not the intention of the applicants to restrict or in any way limit the scope of the appended claims to such detail. Additional advantages and modifications within the scope of the appended claims will readily appear to those sufficed in the art. The invention in its broader aspects is therefore not limited to the specific details, representative apparatus and methods, and illustrative examples shown and described. Accordingly, departures may be made from such details without departing from the spirit or scope of applicants' general concept.
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This disclosure relates to the field of washing apparatus which are portable, and operable without a running source of water, and without a power source. The washing apparatus operates with a volume of liquid cleaner (water) and manual manipulation of a handle. The apparatus may also be dis-assembled by a user without tools for shipping or storage in a much smaller space.
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FIELD OF INVENTION
[0001] The present invention relates to a control lever having one end adapted for attachment to a resting device such as a chair and another end having a tactile contour for identifying the control lever. The invention also relates to a chair having a plurality of levers where each of said levers have a different tactile contour for distinguishing the levers. A guide is associated with said plurality of levers having different tactile shapes. The invention also relates to a method of correlating a plurality of lever control arms with respective corresponding plurality of movements of a chair, using a guide.
BACKGROUND TO THE INVENTION
[0002] Resting devices such as a chair or bed may be adjusted to fit the comfort of an individual user.
[0003] Contemporary chairs particularly utilised in an office are becoming more sophisticated with respect to the different adjustments that can be made to these types of chairs. Typically such chairs provide that both the back and the seat of the office chair can be separately adjusted to a number of different settings by utilising a plurality of chair lever control arms. Generally speaking, all chair lever control arms or controls are generally located below the chair seat. This is generally the case for adjustable beds of the type having control arms located below the bed.
[0004] A particular draw back of such prior art chairs resides in the likelihood that understanding of the use of the controls is often difficult. Much of the difficulty results from the positioning of the lever control arms below the chair seat where they are not readily visibly assessable.
[0005] Accordingly, it is not unusual that the operation of most chair controls is understood after a trial and error test done by a person using the chair. Such person will generally try each control to determine its function and may reach a full understanding of the chair controls only after extended chair usage. This can be frustrating as the chair control arms can move a chair part, which has already been set to an appropriate optimal position, and require resetting. In some case, such person may not be able to properly reset the chair for optimal usage.
[0006] In other cases movement of the lever control arms or devices without an understanding of its function can lead to adjustment of the chair parts which is inappropriate. For example, some chairs are equipped with a tension device that is rotatable and adjusts the tension on the “free float” tilting motion of the chair. This “free float’ motion may be locked (i.e. prohibits the swing) or unlocked by a chair lever arm. If the tension is adjusted for a heavy person and a light person sits on the chair it is possible that the light person may be catapulted forward by the spring activated movement when the lever arm is unlocked.
[0007] Accordingly, various prior art devices have heretofore been constructed in order to address the difficulties referred to above.
[0008] For example, reissue U.S. Pat. Re 36,928 relates to an operational guide mounted to an adjustable chair where the guide includes a card having a pictorial guide for operating the adjustable chair located on the top side of the card.
[0009] Moreover, some prior art chairs included lever control arms having an end with a serrated edge along one side thereof.
[0010] In other cases, Braille has been disposed on a top surface of a lever control arm in order to permit a blind person to locate the particular lever control arm and convey information regarding same.
[0011] However, it is difficult for the general public to decipher the meaning of a serrated edge or Braille disposed on a lever control arm. Furthermore it is generally difficult to visually represent a serrated edge or Braille on a screen or guide which is easy to see or understand.
[0012] Moreover the prior art devices have not addressed the issue of assisting a user to understand the operation of a lever control arm, apart from providing an instructional manual in a booklet of written form. In some prior art devices summaries of instructions are provided on a card as shown in Re 36,928 or card pivoting outwardly from an arm of a chair.
[0013] According, it is an object of this invention to provide an improved lever control arm for a chair, which is more easily and readily understood by the general public.
[0014] It is a further object of this invention to provide an improved chair having control levers for adjusting a chair having an improved method of conveying information concerning its functionality.
[0015] It is an aspect of this invention to provide a control lever having one end adapted for attachment to a resting device for controlled adjustment thereof and another end having a tactile contour for identifying the control lever.
[0016] It is another aspect of this invention to provide a plurality of levers each having one end adapted for attachment below a chair seat or controlling separate movements of a chair, each said lever having another end having tactile shapes different from one another so as to distinguish said levers.
[0017] It is another aspect of this invention to provide a chair having a selectively moveable back and seat and a plurality of control arms attached below said seat for activating selected movements of said back and seat wherein said one of said control arms includes an end having a tactile shape different from an end of another one of said control arms.
[0018] It is another aspect of this invention to provide a chair having a selectively moveable back and seat including a first lever control arm having one end attached below the seat and another end presenting a tactile shape, said first lever arm activating a selected movement of said back or seat; a second lever control arm having one end attached below said seat and another end presenting a tactile shape, said second lever control arm activating another selected movement of said back or seat different from said first lever control arm; said tactile shape of said second lever arm different from said tactile shape of said first lever arm; and a guide presented by the arm of the chair for displaying the different tactile shapes and the associated movements of said first and second lever control arms.
[0019] It is another aspect of this invention to provide a guide for a chair having a plurality of lever control arms with ends having different tactile shapes, for activating a selective orientation of a back or seat of a chair comprising: a screen having visual representations corresponding to each said different tactile shapes; information associated with said visual representations and corresponding to selective orientations activated by said plurality of lever control arms respectively.
[0020] It is another aspect of this invention to provide a method of correlating a plurality of separate movements of a chair with a plurality of lever control arms activating said movements respectively comprising the steps of: providing a plurality of lever control arms with ends having different tactile contour shapes; displaying a guide having said shapes with information associated with said movements of said plurality of lever control arms respectively.
[0021] These and other objects and features of the invention shall now be described in relation to the following drawings.
BRIEF DESCRIPTION OF DRAWINGS
[0022] FIG. 1 is the rear perspective view of an office type chair having moveable chair parts and controls for those moveable chair parts. The chair shown in FIG. 1 is of a conventional design and is labelled as prior art.
[0023] FIG. 2 is a perspective view of a chair and a display or control guide according to one preferred embodiment of the present invention.
[0024] FIG. 3 is an enlarged perspective view of the armrest from the chair of FIG. 2 according to a further preferred embodiment of the present invention.
[0025] FIG. 4 is an enlarged perspective view of the control lever arms removed from the chair FIG. 2 .
DETAILED DESCRIPTION OF THE INVENTION
[0026] In the description that follows, like parts are marked throughout the specification and drawings with the same respective reference numerals. The drawings are not necessarily to scale and in some instances proportions may have been exaggerated in order to more clearly depict certain features of the invention.
DESCRIPTION OF THE PRIOR ART
[0027] FIG. 1 shows a typical example of a prior art office type chair 1 . The chair includes a chair back 3 , a chair seat 5 , and a support frame 8 which includes a vertical column 7 and a frame 9 which supports the chair 1 .
[0028] The back 3 and seat 5 of the chair 1 are adjustable to different positions. For example, the chair back 3 may be vertically adjusted at an angle relative to the seat 5 . Moreover the seat 5 may be adjusted relative the horizontal. Furthermore, the height of the seat 5 may also be adjusted from ground level, in a manner well known to persons skilled in the art. Furthermore, other parts of the chair may also be adjustable.
[0029] The different adjustments or movements of each of the above chair parts is activated by a number of control levers or chair lever control arms 11 . Generally speaking prior art lever control arms 13 , 15 , and 17 are identically shaped. Generally speaking the prior art devices comprise lever arms 13 , 15 , and 17 having a substantially flat circular paddle at one end of the lever arm as shown. Furthermore they generally lie in substantially planar side-by-side relationship in close proximity to one another.
[0030] Accordingly, a user will generally have difficulty distinguishing one control arm 13 from the others 15 and 17 . Generally speaking the user will need to operate the control to determine which chair part is controlled by the respective control lever 13 , 15 , and 17 . If the correct chair control lever 11 is not chosen, difficulties may arise as described above.
[0031] FIG. 2 shows a chair 41 according to one preferred embodiment of the present invention. The chair 41 includes a back 43 and a seat 45 with a lower frame 46 . The lower frame 46 includes height adjustment means 47 and a frame 48 to which the seat 45 is attached and supported.
[0032] The height adjustment means 47 can comprise of a number of devices including telescoping cylinders which comprise a gas cylinder for adjusting the height of the seat 45 relative to the floor in a manner well known to those persons skilled in the art.
[0033] A plurality of control levers or lever control arms 49 are disposed below the seat 45 . In particular, the plurality of lever control arms 49 extend from the frame part 48 . Three lever control arms 52 , 54 and 56 are shown although any number of lever control arms may be utilised. Each of the lever control arms 52 , 54 and 56 present one end 59 , 61 and 63 respectively which are adapted for attachment to the chair. In particular, the one end 59 , 61 and 63 of the lever control arms 52 , 54 and 56 respectively extend from the frame part 48 and are fastened to the appropriate adjustment mechanisms not shown but well known to those persons skilled in the art. For example, the one end 59 , 61 and 63 of the lever control arms 49 may be snapped on or virtually engaged by the appropriate adjustment mechanisms.
[0034] The other end 53 , 55 , 57 of the lever control arm 52 , 54 and 56 respectively have a shape or tactile contour for identifying the control levers 49 . In particular, each of the other ends 53 , 55 , 57 of the control levers 49 have a tactile contour which is different from one another so as to easily and readily distinguish the lever. The geometric shapes shown in the drawings, namely the circle, square and triangle are easily and readily distinguishable from one another by tactile contact with a users fingers (since the levers are located below the seat and out of view) in a way which has not been done before, either by serrated edge, Braille, or otherwise.
[0035] Each of the tactile contours 53 , 55 and 57 are substantially flat or planar and define a substantially two-dimensional tactile shape for identifying the control levers 49 . In particular, the tactile shapes 53 , 55 and 57 are planer having a peripheral edge 65 , 67 and 69 defining the shapes. The peripheral edges 65 , 67 and 69 may be flat, smooth or curved.
[0036] The tactile contours or shapes 53 , 55 and 57 as shown in the figures are disposed substantially horizontally relative to the chair 41 and seat 45 although they can also be disposed substantially vertically or other orientation relative to the chair 41 .
[0037] The shapes of the other end 53 , 55 and 57 of the control levers 49 are in one embodiment selected from the group of circular, rectangular, triangular, square, oval or half-circular shapes. However other geometrical shapes, letters or symbols can be selected such as an arrow which may be oriented upwardly or downwardly to convey a selected message. Generally, this group defines planer shapes. The invention should not be limited to the shapes belonging to this group, as the group has been included as an example only. Any tactile contour shape can be selected so long as it is easily and readily distinguished by a person's tactile feel by the fingers or the like. It is possible that 3-dimensional shapes such as spheres, pyramids or cubes could be utilised, although it has been found that planer 2-dimensional shapes as described are easily distinguishable by touch or feel.
[0038] Furthermore these shapes are in one embodiment disposed in two dimensional space, with a depth (i.e. third dimension) defining a peripheral edge 39 , 41 , and 43 of tactile contour 53 , 55 , and 57 of lever arms 52 , 54 , and 56 respectively.
[0039] In one embodiment the tactile contours are defined and perceived by a user operably contacting the peripheral edge 39 , 41 , and 43 which define the shapes 53 , 55 , and 57 .
[0040] Alternatively the planar surfaces S, T, C of tactile contours 53 , 55 , and 57 may be contoured. For example S may have a smooth surface, while T may be stippled and C being concave, provided such surface is capable of tactile perception and can be visually perceived and in one embodiment represented by indicia such as a visual symbol or in writing.
[0041] Accordingly, the user of a chair is able to reach down and grasp any of the lever control arms 49 and recognise the distinctive shapes or contours that has been grasped as either circular, triangular, square, half-circular, rectangular, oval or the like. As such, the person may then activate the appropriate control lever to adjust or move the respective response in adjusting or moving the seat 45 or back 43 of the chair.
[0042] Such user may then easily remember the particular function of the lever control arms 49 after a few uses as the tactile contours have different shapes. The geometric shapes shown in the figures i.e. circle, triangle, and square are easily remembered.
[0043] Furthermore the side to side spacing can be selected to permit unobstructed manipulation without interference from the other control arms by a users fingers.
[0044] A person can in accordance with another embodiment of this invention, utilise a display or control guide With the invention described above to determine what the particular control lever will do from the shape of the tactile contour.
[0045] More specifically, FIG. 2 shows a control guide or display 65 may comprise a computer monitor, which is associated with the plurality of levers 49 . The computer monitor 65 may be disposed in the vicinity of the chair 41 so that a person sitting in the chair 41 can easily view the monitor screen, which will show or visually display representations of all of the shapes embraced by the tactile shapes 53 , 55 and 57 .
[0046] In the embodiment shown the computer screen 66 will visually illustrate a circular, triangular and square representation. In one embodiment, the circular shape will appear at the top of the screen, while the triangular shape will appear at the middle of the screen, and the square shape appear at the bottom of the screen. Each of the shapes will have associated therewith on the screen information pertinent to the control having the particular shape.
[0047] For example, the circular shape 57 is shown on the computer monitor 65 with indicia or information 85 beside it that the circular shape lever control arm 49 will tilt the chair back 43 vertically relative to the seat 45 . The triangular tactile shape 55 will also appear on the computer monitor 65 with indicia or information 83 beside it that the triangular lever will move the seat 45 at an angle to the horizon. The square tactile shape 53 will appear on the computer monitor 65 with indicia or information 77 beside it that activating the lever 49 will move the seat 45 vertically, upwardly or downwardly relative to a surface.
[0048] Accordingly, a person using the chair 41 could then refer to the visual shapes described above on the monitor screen and reach down and feel for the particular control arm 49 that they need to make a particular chair adjustment.
[0049] In another embodiment, the control guide information 77 , 83 , and 85 may be on a website, which could be accessed by the user. Alternatively, the control guide 65 may comprise of written information obtained in a booklet 67 , which can be stored in association with the chair as shown. Such booklet 67 may have pictures of the various different shapes and information concerning the operation and adjustment of each of the controls according to the shape of the handles.
[0050] In another embodiment, the control guide 65 may be an audible rather than a visual guide. The user of the chair 41 can access this information by pressing a switch 33 , which may be disposed on the arm 71 and an audible recording which has been stored on, in or in association with the chair 41 , will then be activated and heard through an audio output such as a speaker 70 provided in the back of the chair or other location. Appropriate wires (not shown) and power supplies (not shown) can be provided to activate the audio information. Alternatively, the switch 33 may activate the speaker 70 by wireless means.
[0051] FIG. 3 shows still another embodiment of the invention in which the control guide or display 65 is carried or provided in the armrest 71 of the chair. The display is electronic in one embodiment. The display or control guide 65 is presented on the upper surface of the armrest 71 and in one embodiment will be visible at all times. The control guide 65 can comprise of a liquid crystal display screen or other electronic screen, which can display the shapes of the tactile contours and include information concerning the various functions of the levers 49 . The display 65 can also comprise of buttons 57 , 55 and 53 which correspond to the shape of the tactile contours which in one embodiment can be pressed so as to provide information 79 , 83 , and 87 respectively. Information 79 , 83 and 87 corresponding to the levers 49 having the contour shapes 57 , 55 and 53 are displayed in association therewith as shown in FIG. 3 .
[0052] Alternatively, the visual representation 57 , 55 and 53 can comprise of a visual electronic image, which is active by the touch of a finger that changes the electronic characteristics such as inductance or the like to turn on the written information 79 , 83 and 87 respectively.
[0053] Alternatively the shapes of the buttons 57 , 55 , 53 may be embossed printed or recessed into the material of the arm rest during the fabricating or moulding step which buttons could include the words “RAISE”, “LOWER” and “TILT” for example embossed, printed or recessed inside or close to the buttons to act as a guide to the user of the chair. This would act as a guide to the user feeling the lever arms and looking at the shapes on the armrest to prompt the user as to the function of the appropriate lever arm.
[0054] Furthermore by utilising the easily recognisable tactile shapes as described in association with shapes that are easily visually represented on a guide such as a computer screen or electronic display on a chair arm (where resolution may be limited) the user can select the appropriate lever arm for the desired movement of the chair. These advantages are not readily available on those prior art chairs utilising a serrated edge on a lever arm (i.e. pixel size of the screen may not permit visual representation of a serrated edge, particularly to someone with poor eyesight) or Braille on the surface of a lever arm.
[0055] In one embodiment shown in FIGS. 2 and 3 the order or sequence is the same on the display 65 as on the levers 57 55 and 53 to assist in remembering and operation. In other words the visual appearance or order of the buttons 57 , 55 and 53 on the display 65 is the same as the order of the tactile contours 57 , 55 and 53 . However the invention is not to be limited to this particular order as benefits can be experienced with the sequence of the lever arms being different from the buttons.
[0056] Although not shown it is possible that a hinged cover can be attached to the upper surface of the armrest 71 so as to cover the display or the control guide 65 . The information 77 , 83 and 85 is more visually accessible to the user of the chair 41 than the controls, which are located below the chair seat. The user of the chair 41 is able to simply reach down to feel the tactile shape of the ends of the lever control arms 49 which are readily recognisable to the touch of the user and then the user can refer to the control guide 65 to determine which lever control activates which part of the chair.
[0057] Although the invention has been described herein with lever control arms 49 , which are substantially of the same length, such lever control arms 49 may have different lengths.
[0058] The information to be displayed can be selected to include basic instructions concerning the operation of the lever control arms 49 or the literal information can scroll across the screen to provide full operational information concerning the chair as well as the lever control arms 49 .
[0059] Although only three lever control arms 49 have been described a plurality of lever control arms can be utilised. Alternatively, at least two lever control arms can be utilised in accordance with the invention described herein. As described above, each of the levers 52 , 54 and 56 are associated with a control guide or display 65 , which display includes a visual representation corresponding to the shape and information corresponding to the separate movements of the chair. Furthermore it is also possible that one or more control arms 49 be disposed on both side of the seat 45 .
[0060] The display 65 has indicia 77 , 83 and 85 for correlating the different tactile shapes of the control means and their associated movements.
[0061] The invention described herein shows a chair 41 having a selectively moveable back 43 and seat 45 including:
(a) a first lever control arm 52 having one end 59 attach below the seat 45 and another end 53 presenting a tactile shape, said first lever arm 52 activating a selective movement of the back 43 or seat 45 ; (b) a second lever control arm 54 having one end 61 attach below the seat 45 and another end 55 presenting a tactile shape, said second lever arm 54 activating another selective movement of the back 43 or seat 45 different from the first lever control arm 52 ; (c) the tactile shape 55 of the second lever arm 54 is different from the tactile shape 53 of the first lever arm 52 ; (d) a display 65 presented by the arm of the chair 41 for displaying the different tactile shapes and indicia from the associated movements of the first and second lever control arms.
[0066] The invention described above also illustrates a display 65 for a chair 41 having a plurality of lever control arms 52 , 54 and 56 for activating a selected orientation of the back 43 or a seat 45 of the chair 41 comprising:
(a) a screen 66 having visual representations corresponding to each of the different tactile shapes; and (b) information 79 , 83 and 87 associated with the visual representations and corresponding to the selected orientations activated by the plurality of lever control arms respectively.
[0069] Finally the invention described herein illustrates a method of correlating the plurality of movements of a chair with a plurality of lever chair control arms 49 respectively comprising the steps of:
(a) providing a plurality of lever control arms having ends with different tactile contour shapes; (b) displaying a guide having the shapes with information associated with said movements of said plurality of level control arms respectively.
[0072] Although the preferred embodiment as well as the operation in use have been specifically described in relation to the drawings, it should be understood variations of the preferred embodiment can be achieved by a person skilled in the trade without departing from the spirit of the invention as claimed herein.
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A control lever having one end adapted for attachment to a resting device for controlling movement thereof, and another end having a tactile contour for identifying said control lever.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method of removing a metal impurity contained in a hydrofluoric-acid-containing chemical solution used in the steps in manufacturing a semiconductor device.
2. Description of Related Arts
With an increase in integration density of a VLSI, demand for cleaning a silicon wafer surface becomes severer. As contaminants on the silicon wafer surface, fine particles, a metal, an organic material, an oxide film, and the like are known.
An oxide film is removed by etching using a hydrofluoric-acid-containing solution. However, although the oxide film can be removed by this process, when a metal impurity (copper, gold, or the like) is contained in the hydrofluoric-acid-containing chemical solution, this metal impurity is attached to a wafer to adversely affect the electrical characteristics of the wafer. For this reason, the hydrofluoric-acid-containing solution in which a metal impurity is accumulated by dipping wafers in the hydrofluoric-acid-containing solution must be regenerated and used by purifying the hydrofluoric-acid-containing solution, or the hydrofluoric-acid-containing solution must be replaced with a new one.
As a conventional method of removing a metal impurity, a distillation method, an ion-exchange resin method, and a silicon granule adsorption method (Japanese Patent Laid-Open Nos. 3-102827 and 4-286328) are used.
The distillation method is not suitably applied to purification of a solution mixture such as a hydrofluoricacid-containing chemical solution because the composition ratio of the solution changes after distillation. An ion-exchange resin method can be suitably applied to only a diluted hydrofluoric acid solution, and cannot be suitably applied to a chemical solution which contains high-concentration hydrofluoric acid or ammonium fluoride.
A method of removing a metal impurity contained in a hydrofluoric-acid-containing chemical solution performed by a silicon granule adsorption method is as follows. That is, the hydrofluoric-acid-containing chemical solution is brought into contact with silicon granules, the metal impurity in the hydrofluoric-acid-containing chemical solution is removed by adsorbing the metal impurity on the silicon granules.
In removing the metal impurity contained in the hydrofluoric-acid-containing chemical solution using the above conventional silicon granule adsorption method, when this method is used for a long time, the metal impurity adsorbed on silicon granule surfaces is oxidized by oxygen dissolved in the hydrofluoric-acid-containing chemical solution, and the metal impurity is disadvantageously dissolved in the hydrofluoric-acid-containing chemical solution again.
SUMMARY OF THE INVENTION
The present invention has been made to solve the above problems in the prior art, and has as its object to provide a method of stably removing a metal impurity contained in a hydrofluoric-acid-containing chemical solution for a long time to an extent corresponding to a purity which makes it possible to perform the steps in manufacturing a semiconductor device.
In order to achieve the above object, according to the first aspect of the present invention, there is provided a method of removing a metal impurity, comprising the steps of removing oxygen dissolved in a hydrofluoric-acid-containing chemical solution, and, in order to remove a metal impurity contained in the hydrofluoric-acid-containing chemical solution free from the dissolved oxygen, bringing the hydrofluoric-acid-containing chemical solution into contact with silicon granules to adsorb the metal impurity on the silicon granules.
According to the second aspect of the present invention, there is provided a method of removing a metal impurity, comprising the steps of removing oxygen dissolved in a hydrofluoric-acid-containing chemical solution, and, in order to remove a metal impurity contained in the hydrofluoric-acid-containing chemical solution free from the dissolved oxygen, circulating the hydrofluoric-acid-containing chemical solution in a column filled with silicon granules to adsorb the metal impurity on the silicon granules.
According to the third aspect of the present invention, there is provided a method of removing a metal impurity wherein the silicon granules according to the first and second aspects are metal-precipitated silicon granules each having a silicon Granule surface on which a metal is precipitated.
According to the present invention, since the dissolved oxygen contained in a hydrofluoric-acid-containing chemical solution is removed, the metal impurity adsorbed on the silicon granule surfaces can be prevented from being dissolved in the hydrofluoric-acid-containing chemical solution again.
When metal-precipitated silicon granules each having the silicon granule surface on which the metal is precipitated are used as silicon granules to improve metal impurity adsorption performance, the adsorbed metal impurity is prevented by the same effect as described above from being dissolved in the hydrofluoric-acid-containing chemical solution again.
Therefore, the metal impurity in the hydrofluoric-acid-containing chemical solution can be stably removed (concentration level of 0.01 ppb or less) for a long time.
The above and many other advantages, features and additional objects of the present invention will become manifest to those versed in the art upon making reference to the following detailed description and accompanying drawings in which preferred structural embodiments incorporating the principles of the present invention are shown by way of illustrative example.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view showing an apparatus for explaining Example 1 of the present invention and a comparative example thereof;
FIG. 2 is a graph showing a change in copper concentration in a hydrofluoric acid solution as a function of time in Example 1;
FIG. 3 is a sectional view showing an apparatus for explaining Example 2 of the present invention;
FIG. 4 is a graph showing a change in copper concentration in a solution from a column as a function of a column circulation time in Example 2;
FIG. 5 is a sectional view showing an apparatus for explaining Example 3 of the present invention; and
FIG. 6 is a graph showing a change in copper concentration in a solution from a column as a function of a column circulation time in Example 3.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention will be described below on the basis of several preferred embodiments. According to the embodiments, a diluted hydrofluoric acid solution is used as a hydrofluoric-acid-containing chemical solution, copper is used as a metal impurity, and gold-precipitated silicon granules each having a silicon granule surface on which gold is precipitated are used as silicon granules.
FIG. 1 is a sectional view showing an apparatus for explaining Example 1 of the present invention and a comparative example thereof.
A copper-containing (1 ppm) 5% diluted hydrofluoric acid solution 4 (100 ml) was poured into each of reaction vessels 2 and 3 placed on a magnetic stirrer 1, and the reaction vessel 3 was defined as a reaction vessel used for explaining Example 1 of the present invention.
In the copper-containing (1 ppm) 5% diluted hydrofluoric acid solution in the reaction vessel 3, nitrogen bubbling was performed by a nitrogen bomb 5 to remove dissolved oxygen from the solution. In the copper-containing (1 ppm) 5% diluted hydrofluoric acid solution in the reaction vessel 2, nitrogen bubbling was not performed to compare this comparative example with Example 1. Gold-precipitated silicon granules 6 (10 g) were added in each of the solutions in the reaction vessels 2 and 3, and these solutions were stirred by stirrers 7.
FIG. 2 shows changes in copper concentration in the hydrofluoric acid solutions with respect to a stirring time. As is apparent from FIG. 2, it was found that, when oxygen dissolved in the hydrofluoric acid solution was removed, copper could be stably adsorbed and removed for a long time until the copper concentration became 0.01 ppb or less. On the other hand, it was found that, when nitrogen bubbling was not performed, copper temporarily adsorbed on the gold-precipitated silicon granules 6 was dissolved in the hydrofluoric acid solution again so as to increase the copper concentration.
FIG. 3 is a sectional view showing an apparatus used in Example 2 of the present invention. This apparatus is constituted by a solution tank in which a copper-containing (1 ppm) 5% diluted hydrofluoric acid solution 8 is poured, a pump 9, a nitrogen bomb 10, and a column 12 filled with gold-precipitated silicon granules 11 (20 g). Nitrogen bubbling was performed in the copper-containing (1 ppm) 5% diluted hydrofluoric acid solution 8 by the nitrogen bomb 10 to remove the dissolved oxygen from the solution, and the solution was caused to pass through the column 12 at a flow rate of 12 ml/min so as to adsorb and remove copper from the solution by the gold-precipitated silicon granules 11.
FIG. 4 shows a change in copper concentration in a solution 13 from the column 12 as a function of a column circulation time. In comparison, FIG. 4 also shows a result obtained when nitrogen bubbling is not performed. It was found that, when the nitrogen bubbling was not performed, the copper concentration in the solution from the column increased to elute copper adsorbed on the gold-precipitated silicon granules 11. On the other hand, and it was found that, when the nitrogen bubbling was performed, no copper was detected in the solution from the column, and copper could be stably adsorbed and removed for a long time until the copper concentration became a concentration of 0.01 pph or less.
As Example 3, a case wherein a metal impurity removing apparatus is incorporated in an oxide film etching apparatus will be described below with reference to FIG. 5.
The oxide film etching apparatus incorporating with the metal impurity removing apparatus is constituted by a chemical tank 14 in which a 5% diluted hydrofluoric acid solution 20 is stored, a pump 15, a nitrogen bubbling apparatus 16, a column 18 filled with gold-precipitated silicon granules 17, and a filter 19 for removing fine particles from the hydrofluoric acid solution and silicon granules produced by the silicon-granule-filled column 18.
The nitrogen bubbling apparatus 16 is constituted by a nitrogen bomb 26, a bubbling tank 27, and a pump 28. Oxygen dissolved in the hydrofluoric acid solution 20 is removed from the hydrofluoric acid solution 20 by performing nitrogen bubbling.
The chemical tank 14 has a copper concentration monitor 21 and a pump 22 and receives a copper-containing (1,000 ppm) 5% diluted hydrofluoric acid solution 23 and a 5% diluted hydrofluoric acid solution 24 through the pump 22. While a copper concentration in the chemical tank 14 is monitored, the copper-containing (1,000 ppm) 5% diluted hydrofluoric acid solution 23 or the 5% diluted hydrofluoric acid solution 24 is added to the 5% diluted hydrofluoric acid solution 20 in the chemical tank 14. In this case, copper contamination having an arbitrary concentration can be experimentally simulated, and the copper concentration in the chemical tank 14 can be kept constant. Therefore, the performance of a metal impurity removing apparatus 25 according to the present invention can be evaluated and confirmed.
According to the above method, the 5% diluted hydrofluoric acid solution 20 having a copper concentration adjusted to 1 ppm was supplied from the chemical tank 14 at a flow rate of 21 ml/min, and circulated through the bubbling tank 27, a column 18 filled with the gold-precipitated silicon granules 17 (400 g), the filter 19, and the chemical tank 14 in this order. A small amount of solution flowing from the column was extracted from a valve 29, and the copper concentration of this solution was quantitatively analyzed. FIG. 6 shows a change in copper concentration in the solution from the column as a function of a circulation time. In comparison, FIG. 6 also shows a result obtained when nitrogen bubbling is not performed. It was found that, when the nitrogen bubbling was not performed, the copper concentration in the solution from the column increased, and copper was eluted from the column.
It was found that, when nitrogen bubbling was performed, no copper was detected, and copper could be stably adsorbed and removed until the copper concentration became a concentration of 0.01 ppb or less.
As a method of removing dissolved oxygen, in addition to the nitrogen bubbling, a method such as a vacuum deaeration method, a film deaeration method, or a reduction method using a catalytic resin is known. The same effect as the effect of suppressing elution of a metal impurity adsorbed on silicon granules when nitrogen bubbling is performed can be expected.
In addition, when the metal impurity removing apparatus used in the present invention is used to be connected to a chemical circulation line for washing a silicon wafer or etching an oxide film, a hydrofluoric-acid-containing chemical solution can be circulated and regenerated, and the service life-of the chemical solution can be considerably prolonged.
Note that in Examples 2 and 3, although gold is used as a metal precipitated on silicon granule surfaces such that a metal impurity in a hydrofluoric-acid-containing chemical solution is highly efficiently adsorbed and removed, a metal which is rarely oxidized may be used in place of gold.
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A method of removing a metal impurity, including the steps of: removing oxygen dissolved in a hydrofluoric-acid-containing chemical solution; and in order to remove a metal impurity contained in the hydrofluoric-acid-containing chemical solution free from the dissolved oxygen, bringing or circulating the hydrofluoric-acid-containing chemical solution into contact with or in a column filled with silicon granules to adsorb the metal impurity on the silicon granules.
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FIELD OF THE INVENTION
The present invention relates to apparatus for protecting CMOS transistors from electro static discharge, and in particular the use of external well resistors to provide such protection.
BACKGROUND OF THE INVENTION
In conventional CMOS processes, built-in resistors from the active areas of a transistor protect the pull-up and pull-down devices by absorbing a portion of voltage drops, and also serve to limit the total amount of current that is allowed to flow through the devices during electrostatic discharge (ESD) events. However, in processes where the resistance of the active areas is small, or is reduced to improve the frequency response of CMOS circuitry, the active area resistance no longer functions to provide such a current limiting effect. A need exists to provide for limiting the current through active devices during ESD events without adversely affecting the speed at which such devices operate.
SUMMARY OF THE INVENTION
The present invention provides a method and apparatus for limiting the amount of current flowing through active devices during an ESD event. Well resistors are coupled in series with the pull-up and pull-down transistor pair and the power supply and ground respectively to limit such current. A first well resistor is connected between Vet power supply line and the pull up transistor to limit current flow to the output when the ESD event strikes the Vcc supply line. A second well resistor is connected between a Vss ground line and the pull down transistor to limit current flow to the output when the ESD event strikes the Vss ground line. The well resistors do not substantially adversely affect the switching speeds of the transistors because they are formed external to the transistors.
In one preferred embodiment, the externally formed well resistors are coupled in series with the pull-up and pull-down devices of a CMOS output driver. The first resistor increases the overall resistance and thereby reduces current flow between the Vcc power supply to the output. The second resistor increases the overall resistance and thereby reduces potential current flow between the Vss ground to the output. Both resistors also provide a large voltage drop during high currents, limiting voltage applied across the transistors. Thus the impact of ESD events occurring on either Vss or Vcc to the devices is limited.
In further embodiments, only one of the pull-up and pull-down devices is protected by an externally formed well resistor depending on which of the Vss or Vcc busses are most likely to be associated with an ESD event. When space on a semiconductor die is limited, protecting only the active areas most likely to be affected by an ESD event provides a designer the ability to provide increased reliability while maintaining high circuit densities.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a circuit diagram indicating the electrical connections of the N-well resistors of the present invention.
FIG. 2 is a simplified cross section view of a substrate having a portion of the circuit of FIG. 1 formed therein.
FIG. 3 is a simplified cross section view of a substrate showing an alternative arrangement of the N-well resistors of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In the following detailed description of the preferred embodiment, reference is made to the accompanying drawings which form a part hereof, and in which is shown by way of illustration specific preferred embodiments in which the invention may be practiced. These embodiments are described in sufficient detail to enable those skilled in the art to practice the invention, and it is to be understood that other embodiments may be utilized and that structural, logical present inventions. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the present invention is defined only by the appended claims.
Numbering in the Figures is usually done with the hundreds and thousands digits corresponding to the figure number, with the exception that the same components may appear in multiple figures. Signals and connections may be referred to by the same number or label, and the actual meaning should be clear from the context of use.
In FIG. 1, an output driver shown generally at 110 provides an output, DQ shown at 111, for circuitry contained on a standard semiconductor die. A pull-up (PU) CMOS enhancement mode insulated gate field effect n channel transistor is shown at 112 with it's complimentary pull-down (PD) n channel transistor indicated at 114. The source of transistor 112 is coupled to the drain of transistor 114. The drain of pull-up transistor 112 is coupled through a first N-well resistor R1 indicated at 116 to power supply voltage Vcc. The source of pull-down transistor 114 is coupled through a second N-well resistor R2 indicated at 118 to ground voltage Vss. Thus, each transistor is coupled in series with a N-well resistor to respective busses on which an ESD event is most likely to occur. The N-well resistors serve to limit the current through the channels of the transistors during such an event to reduce the chances of any damage occurring to the transistors. Also, higher currents will result in higher voltages across the N-well resistors, serving to limit the amount of voltage applied to the transistors during an ESD event.
The gate of transistor 112 is coupled to a signal originating from a bit or word line of a dynamic random access memory (DRAM) 113 which is formed on the same substrate as the transistor pair. The complement of the DRAM signal is provided to the gate of transistor 114. The source of the pull up transistor 112 and drain of the pull down transistor 114 are coupled to provide a fast switching high impedance output DQ. The pair serve as a CMOS output driver for providing signals which are coupled to a separate device, such as a bus driver for providing signals which are coupled to a separate device, such as a bus in a personal computer, or a connector in a circuit card. It should be noted that in many field effect transistors, the source and drain are essentially interchangeable, and interconnections specified herein should not be interpreted as solely limited to those described. In addition, in many cases, the doping of semiconductor structures may be reversed on a wholesale basis to obtain similar functions.
A cross section of one of the transistor and resistor pair is shown in FIG. 2. A P type substrate 220 is used to form transistor 114. Active areas 222 and 224 are formed with N+ doping to form the source and drain respectively. This type of field effect transistor is called an N-channel device. Metal contacts 228, and 230 are formed through an insulating layer 232 to provide electrical contact for the source and drain respectively. A metal contact, not visible in this cross section, is formed over a gate dielectric 234 to provide electrical contact for the gate. In addition, in one preferred embodiment, silicide, preferably formed of a metal strapped polysilicon material, with tungsten (TuSi2), titanium (TiSi2) or other suitable metal, is applied to the surface of the active N+ areas 222 and 224 as shown at 235 to decrease their resistance, thereby increasing the switching speed of transistor 114. The sheet resistance of the silicide is preferably around 6 ohms per square but may vary with different materials and concentrations. In many prior transistors, the active area resistance served to limit the current through the transistor during an ESD event. Since the resistance of the active areas is now decreased, they no longer serve well for that function.
The N-well resistor, shown at 118 and formed external to the transistor 114 now serves the function of limiting current through the transistor during an ESD event. In one embodiment, the active area drain 230 is coupled by a conductive metal, polysilicon or other suitable conductive layer 236 to the N-well resistor 118, via an N+ region, which is then connected by a further N+ region to a conductive layer 238 to Vss. In another embodiment, the source, 230 is coupled by conductive layer 236 to the N-well resistor 118, which is then connected by conductive layer 238 to the output DQ. Thus, the N-well resistors may be placed on either side of the transistors 112 and 114, so long as they provide a series connection with the transistor to limit current during an ESD event.
Because the N-well resistor is formed external to the transistor 114, it has no direct affect on the switching speed of the transistor itself. It is also, not a critical device that must have closely controlled characteristics. Thus, it may be formed on the edges of the die containing circuitry for which the output driver 110 provides output DQ which is available for connection to other die or devices. Since the edges of a die or chip are subject to the most stress and potential defects due to cutting of the die and misalignment of processes, circuitry is not normally placed in such areas. Thus, the real estate used to form the N-wells is not normally used for circuitry, so the number of usable circuits obtainable on the die is not reduced.
In a further embodiment, only one of pull up transistor 112 and pull down transistor 114 is protected by an externally formed well resistor depending on which of the Vss or Vcc busses are most likely to be associated with an ESD event. When space on a semiconductor die is limited, protecting only the active areas most likely to be affected by an ESD event provides a designer the ability to provide increased reliability while maintaining high circuit densities.
In FIG. 3, an alternative position for an N-well resistor 318 is shown. The N-well resistor 318 is now formed partially overlapping an active area source or drain 314, allowing the active area to provide the dual function of both serving as a source or drain for a transistor, and to serve as a first contact area for N-well resistor 318. A second contact area 316 formed at a far end of the N-well area 318 is coupled to a metalized area, which as in the embodiment of Figure two is coupled to either a supply voltage, or the output. This alternative embodiment saves space on the die, allowing room for further circuitry.
It is to be understood that the above description is intended to be illustrative, and not restrictive. Many other embodiments will be apparent to those of skill in the art upon reviewing the above description. The scope of the invention should, therefore, be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled.
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A circuit for providing electrostatic discharge (ESD) protection is disclosed. The circuit comprises a pair of CMOS field effect pull up and pull down transistors with reduced resistance source and drain, having a well resistor formed external to them between supply and ground busses respectively. During an ESD event, the well resistors serve to both limit the current flow through the transistors, and reduce the voltage drop across them.
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CROSS-REFERENCE TO SOURCE CODE APPENDIX
Appendix A, which is part of the present disclosure, contains VERILOG source code for implementing one embodiment of this invention as described more completely below.
A portion of the present disclosure contains material that is subject to copyright protection. The copyright owner has no objection to the facsimile reproduction by anyone of the patent document or the patent disclosure, as it appears in the Patent and Trademark Office patent files or records, but otherwise reserves all copyright rights whatsoever.
BACKGROUND
A video stream is a sequence of video frames where each frame is a still image. A video player, such as a DVD player, displays one frame after another at approximately 30 frames per second to generate a video. In MPEG-2 format, frames are digitized so that each pixel is represented by a brightness component of luma (“Y”) and two color components of chroma blue (“Cb”) and chroma red (“Cr”). The color of a pixel is black when its luma value is at a minimum regardless of its chroma blue and chroma red values. Conversely, the color of the pixel is white when its luma value is at a maximum regardless of its chroma blue and chroma red values. Luma, chroma blue, and chroma red have a nominal range of 0 to 255.
A DVD player can read a DVD bitstream from a DVD disk and display on a monitor a main video (that occupies a majority of the area of the monitor) superimposed by a subpicture (hereinafter “SPU”). The subpicture normally occupies a small area of the monitor (e.g., occupies 10% of the total area). A DVD bitstream contains, among other data three elementary streams: a main video elementary stream, an audio elementary stream, and a SPU elementary stream. Subpictures are “[g]raphic bitmap overlays used in DVD-Video to create subtitles, captions, karaoke lyrics, menu hightlighting effects, and so on.” See the book entitled “DVD Demystified” by Jim Taylor, p. 424, McGraw-Hill, 1999. Chapter 4 and the glossary of DVD Demystified are hereby incorporated by reference. In one example, the main video is a movie and the SPU is the subtitle for the movie.
In addition to the main video superimposed with the SPU, the DVD player can display (see FIG. 1) an on-screen display (“OSD”) of the DVD controls, such as a volume bar, superimposed over the main video. In some DVD players, fade in and fade out are used to replace a background color with the main video (or vice versa). During such replacement, the OSD does not fade in and fade out with the main video so that consumers continue to view the OSD during the transition from the background color to the main video. However, fading (in or out) of the main video affects the colors of the pixels in the portion of the OSD that is superimposed on the main video, so that the pixels in OSD change colors during the fading.
SUMMARY
In one embodiment, a fade circuit (also called “fader”) supports transition between display of a video (that has a first portion to be changed and a second portion left unchanged) and display of a background color (such as blue) by adjusting two or more components (e.g., the luma component (Y) and one or both of chroma components (Cb and Cr)) of one or more to-be-displayed pixels (e.g., all pixels in the second portion that is to be left unchanged or alternatively all pixels of the video). The adjustment includes, for example, one or more arithmetic operations, so that the one or more pixels maintain color at two or more moments during the transition (preferably at all times in the transition). By adjusting the luma and chroma components together, one or more colors of the second portion remain constant during the transition between display of the video and the background color. Maintaining colors of the second portion allows a user to clearly see the information displayed by the second portion during the transition.
In one specific implementation, the luma component is adjusted by subtracting (or adding) a fade factor (that changes over time) to form a gradually changing luma component. In this implementation, the chroma components are simultaneously adjusted by another arithmetic operation. In one example, the chroma components are scaled by (1) subtracting a predetermined value from each chroma component to form a resultant, (2) multiplying the resultant with a scale factor (that changes over time) to form a product, and (3) adding the predetermined value to the product to form a faded chroma component. Preferably, but not necessary, the same predetermined value and the same scale factor are used for the two chroma components.
In one embodiment, a mix circuit combines the faded components of a first video (hereinafter referred to as “first pixel components”) with components of a second video (hereinafter referred to as “second pixel components”), for example using an arithmetic operation. The combined (mixed) components (hereinafter called “mixed pixel components”) are displayed on a monitor wherein the second video is superimposed over the first video. To mix a first pixel component with a second pixel component, one example of a mix circuit adds (1) the product of the first pixel component and a mix weight (mw) with (2) the product of the second pixel component and another mix weight (1−mw). The same results can be accomplished by adding (1) the second pixel component to (2) the product of a mix weight (mw) and the difference between the first pixel component and the second pixel component.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a DVD image of the prior art having a main video image, and superimposed thereon each of a subpicture image and an on-screen display image.
FIG. 2A illustrates a multimedia system including a video playback device 102 that displays a superimposed image having fixed colors during fade in and fade out in one embodiment as described herein.
FIG. 2B illustrates, in a block diagram, an embodiment of a fade circuit 514 (also called “fader”) of video playback device 102 of FIG. 2 A.
FIG. 3 illustrates, in a block diagram, various components inside video playback device 102 of FIG. 2 A.
FIG. 4 illustrates, in a block diagram, a multimedia decoder 228 of FIG. 3 .
FIG. 5A illustrates, in a block diagram, a display controller 410 of multimedia decoder 228 of FIG. 4 in one implementation.
FIG. 5B illustrates various signals held in a host register 512 illustrated in FIG. 5 A.
FIG. 6 illustrates, in a flow chart, a method used by display controller 410 of FIG. 5A to fade a video in this implementation.
FIG. 7 illustrates, in a block diagram, an embodiment of a subpicture mix 510 (also called “SPU mix”) of display controller 410 of FIG. 5 A.
FIG. 8 illustrates, in a block diagram, an embodiment of fader 514 of FIG. 5 A.
FIG. 9 illustrates, in a block diagram, an embodiment of an on-screen display mix 516 (also called “OSD mix”) of FIG. 5 A.
FIG. 10 illustrates, in a block diagram, another embodiment of the OSD mix 520 of FIG. 5 A.
DETAILED DESCRIPTION
In one embodiment, a fader 514 (FIG. 2B) transitions between the display of a background color and the display of a main video image (in a process called “fading”) while maintaining the colors of an on-screen display (“OSD”) image superimposed thereon. In this embodiment, fader 514 adjusts the luma component as well as one or both chroma components of the main video image so that colors of the OSD image remain at least substantially unchanged (e.g., not noticed by a human). By adjusting the luma and chroma components, the colors of the OSD image are kept unchanged during fading of the main video image. Maintaining colors of the OSD image unchanged allows viewers to clearly see the information displayed by the OSD image during and subsequent to fading.
In one implementation, fader 514 includes an arithmetic unit 849 that adjusts the luma component to form a faded luma component. Fader 514 further includes another arithmetic unit 848 that adjusts at least one of the chroma components to form one or more faded chroma components. Fader 514 outputs the faded luma and chroma components to an OSD mix 516 . OSD mix 516 mixes the faded luma and chroma components with the to-be-displayed OSD luma and chroma components.
In one embodiment, each of fader 514 and OSD mix 516 are included in a video playback device 102 (FIG. 2A) that displays on a monitor 106 the video contents of a multimedia disk in a disk drive 104 . Video playback device 102 is controlled in the normal manner, for example, through a remote control 110 . Video playback device 102 can also play the audio contents of the multimedia disk through speakers 108 A- 108 F. Video playback device 102 is, for example, a DVD player model DVP S 330 available from Sony Corporation of Tokyo, Japan.
Video playback device 102 includes a read head 220 (FIG. 3) that scans a multimedia disk 216 spun by a spindle motor 214 to produce a stream of bits (hereinafter “raw bitstream”). The raw bitstream is filtered by a digital signal processor (“DSP”) 210 to produce a filtered bitstream. DSP 210 also controls spindle motor 214 and read head 220 through a power amp 212 . The filtered bitstream is buffered by a channel control 222 and demodulated by a demodulator 224 to form a demodulated bitstream. The demodulated bitstream is decoded and error corrected by an error correction decoder (“ECC”) 226 to produce a Digital Versatile Disk (“DVD”) bitstream. The DVD bitstream is decoded by a multimedia decoder 228 to produce digital audio and video signals. Digital to analog converters (“DAC”) 236 and 238 respectively convert the digital audio and video signals to analog signals for display on monitor 106 . DAC 238 is, for example, a NTSC/PAL rasterizer for televisions. A host processor 230 controls the operations of DSP 210 , ECC 226 , and multimedia decoder 228 .
In one embodiment, multimedia decoder 228 (FIG. 3) decodes the DVD bitstream to produce at least two elementary bitstreams. The elementary bitstreams includes a main video elementary bitstream and a subpicture (“SPU”) elementary bitstream. Multimedia decoder 228 can construct a main video image from the main video elementary bitstream and a SPU image from the SPU elementary bitstream. Multimedia decoder 228 can also superimpose the SPU image over the main video image by combining (mixing) the pixels of the main video image (hereinafter called “main video pixels”) with the pixels of the SPU image (hereinafter called “SPU pixels”). The main video image superimposed with the SPU image is hereinafter called “SPU mix image” and the pixels formed from mixing the main video pixels with the SPU pixels are hereinafter called “SPU mix pixels.”
In this embodiment, multimedia decoder 228 can further superimpose an OSD image over the main video image (or the SPU mix image) by combining (mixing) the main video pixels (or the SPU mix pixels) with the pixels of the OSD image (hereinafter called “OSD pixels”). The main video image (or the SPU mix image) superimposed with the OSD image is hereinafter called “OSD mix image” and the pixels formed from mixing the main video pixels (or the SPU mix pixels) with the OSD pixels are hereinafter called “OSD mix pixels.”
In one embodiment, multimedia decoder 228 includes a microcontroller 402 (FIG. 4) that communicates commands to and from processor 230 through host register 512 (FIG. 4 and FIG. 5B) in a host interface 404 . Host interface 404 also communicates data, e.g., a DVD bitstream, to a variable length decoder (“VLD”) 406 . VLD 406 includes a pre-parser 418 that parses the DVD bitstream into elementary bitstreams. The elementary bitstream includes, for example, an audio elementary bitstream, a main video elementary bitstream, and a SPU elementary bitstream. A memory interface 408 communicates the elementary bitstreams to their respective buffers in a memory 204 (FIG. 3 and FIG. 4 ).
VLD 406 also includes a post-parser 420 that decodes and passes the audio elementary bitstream, the main video elementary bitstream, and the SPU elementary bitstreams from their respective buffers in memory 204 to their respective devices: an audio decoder 416 , a main video decoder 414 , and a SPU decoder 412 .
Audio decoder 416 decodes, for example, DVD compliant audio elementary bitstreams (e.g., MPEG-2 audio elementary bitstream) to audio packets. Audio decoder 416 saves the decoded audio packets in an area (called “audio packet store”) in memory 204 .
Video decoder 414 decodes, for example, DVD compliant video elementary bitstreams (e.g., MPEG-2 video elementary bitstream) to main video images. Video decoder 414 saves the main video images in three areas (called “video frame stores”) in memory 204 . The three video frame stores save, for example, an intra-frame, a forward predicted frame, and a bi-directional predicted frame.
SPU decoder 412 decodes, for example, DVD compliant SPU elementary bitstream to SPU images. SPU decoder saves the SPU images in an area (called “SPU image store”) in memory 204 .
An OSD/display controller 410 retrieves the main video images from the main video frame stores in memory 204 and superimposes either a SPU image or an OSD image, or both, over the main video image (FIG. 1 ). Display controller 410 outputs the final image in 4:2:2 component format.
In one embodiment, OSD/display controller 410 (FIG. 5A) includes a memory address generator 502 . Memory address generator 502 , under the control of a timing generator 515 , addresses the video frame stores in memory 204 through memory interface 408 to read main video pixel data into a vertical filter 504 . In one implementation, memory address generator 502 and timing generator 515 are the respective conventional address generator and timing generator described in “L64021 DVD Audio/Video Decoder Technical Manual,” which is incorporated by reference in its entirety.
Vertical filter 504 filters the main video pixel data to vertically scale the main video images and to produce main video images of 4:2:2 component format. A freeze filter 506 filters the main video pixel data to improve the image quality of the main video images in case a main video image is paused. A horizontal filter 508 filters the main video pixel data to horizontally scale the main video images. Horizontal filter 508 passes the main video pixel data to a SPU mix 510 . In one implementation, vertical filter 504 , freeze filter 506 , and horizontal filter 508 are conventional filters described in “L 64021 DVD Audio/Video Decoder Technical Manual,” which is incorporated by reference above.
In one embodiment, display controller 410 starts in action 602 (FIG. 6 ). Action 602 is followed by action 604 . In action 604 , display controller 410 determines if host processor 230 desires to superimpose a SPU image over a main video image to form a SPU mix image. Host processor 230 stores an active signal SPU_enable in a storage element 512 A of host register 512 (FIG. 5B) if host processor 230 wishes to superimpose a SPU image over a main video image. If storage element 512 A stores an active signal SPU_enable, action 604 is followed by action 606 . Otherwise, action 604 is followed by action 608 .
In action 606 , display controller 410 mixes the main video pixel data with the SPU pixel data according to a SPU mix weight (e.g., “mw spu ”) to form a SPU mix pixel data. In one embodiment, display controller 410 includes a SPU decoder 412 (FIG. 4 and FIG. 5A) that addresses the SPU image store in memory 204 to read SPU pixel data into a SPU mix 510 . SPU decoder 412 also synchronizes the SPU pixel data to the main video pixel data that are provided to SPU mix 510 . In one implementation, SPU decoder 412 is a conventional SPU decoder described in “L64021 DVD Audio/Video Decoder Technical Manual,” which is incorporated by reference above.
In one variation, SPU mix 510 mixes the main video pixel data and the SPU pixel data according to the SPU mix weight from SPU decoder 412 as follows.
Y SPU mix =Y video *mw SPU +Y SPU *(1 −mw SPU ) (1)
Cb SPU mix =Cb video *mw SPU +Cb SPU *(1 −mw SPU ) (2)
Cr SPU mix =Cr video *mw SPU +Cr SPU *(1 −mw SPU ) (3)
Subscript “SPU mix” indicates the pixel components of the SPU mix image, subscript “video” indicates the pixel components of the main video image, and subscript “SPU” indicates the pixel components of the SPU image.
Alternatively, the above equations can be rewritten to reduce the number of multiplication operations as follows:
Y SPU mix =Y SPU +( Y video −Y SPU )* mw SPU (4)
Cb SPU mix =Cb SPU +( Cb video −Cb SPU )* mw SPU (5)
Cr SPU mix =Cr SPU +( Cr video −Cr SPU )* mw SPU (6)
When displayed, SPU mix pixel data generates a main video with SPU overlay. Action 606 is followed by action 608 . In one embodiment, actions 604 and 606 are optional.
In action 608 , display controller 410 fades the main video image (or the SPU mix image if an SPU image was superimposed over a main video image in action 606 ) by adjusting the chroma components (Cb and Cr) in addition to the luma (Y) components of the pixels. Note that fade in and fade out of just the main video image (or the SPU mix image) can be accomplished by adjusting only the luma values of the main video pixels (or SPU mix pixels). Chroma blue and chroma red components remaining constant during such fading have little impact on the colors of the pixels when the luma components are changed to approach the maximum value (e.g., 255) or the minimum value (e.g., 0).
However, when the main video image is combined with an OSD image (described in detail later), the luma components of the OSD pixels allow the chroma blue and chroma red components of the main video pixels (or SPU mix pixels) to be seen despite the adjustment to the luma components of main video pixels (or SPU mix pixels). This results in an OSD that changes colors during fade in and fade out of the main video image (or SPU mix image) due to chroma blue and chroma red contributions from the main video pixels (or SPU mix pixels).
In one embodiment, display controller 410 includes a fader 514 that adjusts the luma components, the chroma blue components, and chroma red components of the main video pixels (or SPU mix pixels) during fade in and fade out so that the OSD does not change color. In one variation, fader 514 fades the main video image by adjusting the luma component and the two chroma components of the main video pixels as follows.
Faded Y video =Y video −fade factor (7)
Faded Cb video =( Cb video −128)*scale factor+128 (8)
Faded Cr vidoe =( Cr video −128)*scale factor+128 (9)
In another variation, fader 514 fades the SPU mix image by adjusting the luma component and the chroma components of the SPU mix pixels using the same arithmetic operations (7)-(9) as follows.
Faded Y SPU mix =Y SPU mix −fade factor (10)
Faded Cb SPU mix =( Cb SPU mix −128)*scale factor+128 (11)
Faded Cr SPU mix =( Cr SPU mix −128)*scale factor+128 (12)
Host processor 230 controls fade in and fade out by storing values for the fade factor and the scale factor in respective storage elements 512 C and 512 D of host register 512 (FIG. 5 B). Host processor 230 stores a value of 0 for the fade factor and value of 1 for the scale factor if no fading of the SPU mix is desired (no fading of the main video image or the SPU mix image). In any event, the faded luma, chroma blue, and chroma red cannot become less than the minimum value of 0 or greater than the maximum value of 255 (clipped at 0 or 255). The scale factor is also restricted between −1 and 1 to provide a smooth transition between video display and the background color. Host processor 230 sets the fade factor and the scale factor by storing their respective values in respective storage elements 512 C and 512 D of host register 512 . Fader 514 outputs the faded pixel data to an OSD mix 516 (FIG. 5 A). Action 608 is followed by action 610 .
In action 610 , display controller 410 determines if host processor 230 desires to superimpose an OSD image over the main video image (or the SPU mix image if an SPU image was superimposed over a main video image in action 606 ) to form an OSD mix image. Host processor 230 stores an active signal OSD_enable in a storage element 512 B of host register 512 (FIG. 5B) if host processor 230 wishes to superimpose an OSD image over a main video image (or the SPU mix image). If storage element 512 B stores an active signal SPU_enable, action 610 is followed by action 612 . Otherwise, action 610 is followed by action 614 .
In action 612 , display controller 410 mixes the main video pixel data (or the SPU mix pixel data) with the OSD pixel data according to an OSD mix weight (e.g., “mw OSD ”) to form an OSD mix pixel data. When displayed, OSD mix pixel data generates a main video image (or a SPU mix image) with OSD overlay. In one embodiment, display controller 410 includes an OSD decoder 518 that, under command of timing generator 515 , addresses an OSD image store in memory 204 to read OSD pixel data into an OSD mix 516 . OSD decoder 518 synchronizes the OSD pixel data to the main video pixel data (or the SPU mix pixel data) provided to OSD mix 516 from fader 514 . OSD pixel data is written into the OSD image store in memory 204 by host processor 230 . In one implementation, OSD decoder 518 is a conventional OSD decoder described in “L64021 DVD Audio/Video Decoder Technical Manual,” which is incorporated by reference above.
In one variation, OSD mix 516 combines the main video pixel data with the OSD pixel data according to the OSD mix weight from OSD decoder 518 to form the OSD mix pixel as follows.
Y OSD mix =Faded Y video *mw OSD +Y OSD *(1 −mw OSD ) (13)
Cb OSD mix =Faded Cb video *mw OSD +Cb OSD *(1 −mw OSD ) (14)
Cr OSD mix =Faded Cr video *mw OSD +Cr OSD *(1 −mw OSD ) (15)
Subscript “OSD mix” indicates the pixel components of the OSD mix image.
Alternatively, the above equations can be rewritten to reduce the number of multiplication operations as follows:
Y OSD mix =Y OSD +(Faded Y video −Y OSD )* mw OSD (16)
Cb OSD mix =Cb OSD +(Faced Cb video −Cb OSD )* mw OSD (17)
Cr OSD mix =Cr OSD +(Faded Cr video −Cr OSD )* mw OSD (18)
In another variation, OSD mix 516 combines the SPU mix pixel data with the OSD pixel data according to the mix weight (hereinafter called “mw OSD ”) from OSD decoder 518 to form the OSD mix pixel as follows.
Y OSD mix =Faded Y SPU mix *mw OSD +Y OSD *(1 −mw OSD ) (19)
Cb OSD mix =Faded Cb SPU mix *mw OSD +Cb OSD *(1 −mw OSD ) (20)
Cr OSD mix =Faded Cr SPU mix *mw OSD +Cr OSD *(1 −mw OSD ) (21)
Alternatively, the above equations can be rewritten to reduce the number of multiplication operations as follows:
Y OSD mix =Y OSD +(Faded Y SPU mix −Y OSD )* mw OSD ( 22 )
Cb OSD mix =Cb OSD +(Faced Cb SPU mix −Cb OSD )* mw OSD (23)
Cr OSD mix =Cr OSD +(Faded Cr SPU mix −Cr OSD )* mw OSD (24)
Action 612 is followed by action 614 . In action 614 , display controller 410 provides processed pixel data (main video pixel data, SPU mix pixel data, or OSD mix pixel data) to DAC 238 for display on monitor 106 . Action 614 is followed by action 604 .
In one implementation, the main video pixel data, the SPU pixel data, and the OSD pixel data are in 4:2:2 component format. Horizontal filter 508 (FIG. 5A) outputs, for example, 8 bits of main video pixel data to SPU mix 510 at each clock pulse. Every 8 bits of main video pixel data represents one of three pixel components (e.g., luma, chroma blue, or chroma red) of the main video image. Accordingly, a pixel component of the main video image is provided to SPU mix 510 at each clock pulse.
Similarly, SPU decoder 412 (FIG. 5A) provides, for example, 8 bits of SPU video pixel data to SPU mix 510 at each clock pulse. Every 8 bits of SPU video pixel data also represents one of three pixel components of the SPU image. SPU decoder 412 synchronizes the pixel components of the SPU image with the pixel components of the main video.
In this implementation, host processor 230 stores signal SPU_enable, signal OSD 13 enable, signal fade factor, and signal scale factor in respective storage elements 512 A- 512 D. Host processor 230 controls multimedia decoder 228 by writing (in response to user instruction) different values into the just-described storage elements 512 A- 512 D of host register 512 . In one example, if a user instructs video playback device 102 to display main video with SPU overlay (e.g., through remote control 110 ), host processor 230 responds to the user's instruction by storing an active signal SPU_enable in storage element 512 A.
In another example, if a user instructs video playback device 102 to stop the main video (or SPU mix) through remote control 110 , host processor 230 writes values for fade factor in storage element 512 C (e.g., increasing over 2 seconds from 0 to a maximum of 255 to fade out) and scale factor in storage element 512 D (decreasing over 2 seconds from 1 to a minimum of 0 to fade out) for one or more frames of the main video (or SPU mix) to transition the main video (or SPU mix) to the background color. In this example, if a user instructs video playback device to play the main video (or SPU mix) through remote control 110 , host processor 230 writes values for fade factor signal 512 C (decreasing over time to a minimum of 0 to fade in) and scale factor signal 512 D (increasing over time to a maximum of 1 to fade in) for each frame of the main video (or SPU mix) to transition the background color to the main video image (or SPU mix).
SPU mix 510 (FIG. 7) includes a subtractor 702 that has ports 701 and 703 respectively coupled to buses 718 and 720 . Bus 718 carries a pixel component of the main video image from horizontal filter 508 and bus 720 carries a pixel component of the SPU image from SPU decoder 412 . Subtractor 702 subtracts the SPU pixel component signal from the main video pixel component signal and provides a difference signal on a bus 704 .
A multiplier 706 has ports 705 and 707 respectively coupled to buses 704 and 722 . Bus 722 carries a SPU mix weight (e.g., “mw SPU ”) from SPU decoder 412 . Multiplier 706 multiplies the signal received on port 705 with the signal of the SPU mix weight and provides a product signal on a bus 708 . An adder 710 has a port 709 coupled to bus 720 and a port 711 coupled to bus 708 . Adder 710 adds the signal received on port 709 to the signal received on port 711 and provides a result signal on a bus 712 .
A multiplexer 714 has ports 713 and 715 respectively coupled to buses 718 and 712 . Multiplexer 714 also has a control terminal 717 coupled to line 718 that carries a control signal (e.g., “signal SPU_enable”) from SPU_enable bit 512 A in host register 512 . If signal SPU_enable is active, multiplexer 714 propagates the signals received on terminal 715 (a pixel component of a SPU mix image) to a bus 716 . Otherwise, multiplexer 714 propagates the signals received on terminal 713 (a pixel component of the main video image).
Fade circuit 514 (FIG. 8) includes a demultiplexer 802 that has a port 801 coupled to bus 716 from SPU mix 510 . Demultiplexer 802 has a control terminal 803 coupled to a line 846 carrying a control signal (also called “component_type”) from timing generator 515 . Demultiplexer 802 propagates signals received on port 801 (1) to a bus 804 when signal component_type is, for example, active and alternatively (2) to a bus 828 when signal component_type is, for example, inactive. Therefore, timing generator 515 drives active or inactive signal component_type so that demultiplexer 802 passes only the chroma components (Cb and Cr) onto bus 804 and only the luma components (Y) onto bus 828 .
Chroma components are processed by a subtractor 806 , a multiplier 812 , an adder 818 , and a clipper 824 (e.g., collectively forming arithmetic unit 848 ). Subtractor 806 has ports 803 and 805 respectively coupled to buses 804 and 808 , Bus 808 carries a predetermined signal that is hardwired in fade circuit 514 . For example, the predetermined signal may have m bits of active signals and n bits of inactive signal. In one variation, the predetermined signal has a value of 128 (1 bit of active signal and 7 bits of inactive signal). Subtractor 806 subtracts the predetermined signal from the chroma blue or chroma red signal received on port 803 and outputs a result signal on a bus 810 .
Multiplier 812 has ports 807 and 809 respectively coupled to buses 810 and 814 . Bus 814 carries a scale factor signal written by host processor 230 in host register 512 . Multiplier 812 multiplies the signal received on port 807 with the scale factor signal received on port 809 and outputs a product signal on a bus 816 .
Adder 818 has a port 811 coupled to bus 816 and a port 813 coupled to bus 808 that carries the predetermined signal having a value of, for example, 128 . Adder 818 adds the predetermined signal to the signal received on port 811 and outputs a result signal on a bus 822 .
Clipper 824 has a port 815 coupled to bus 822 . If the signal received on port 815 is greater than 255 or less than 0, clipper 824 propagates a respective signal 255 or 0 to a bus 826 . Otherwise, clipper 824 propagates the signal received on port 815 on bus 826 .
Luma components are processed by a subtractor 830 and a clipper 836 (e.g., collectively forming arithmetic unit 849 ). Subtractor 830 has ports 817 and 819 respectively coupled to buses 828 and 832 . Bus 832 carries a fade factor signal set by host processor 230 in host register 512 . Subtractor 830 subtracts the fade factor signal from the luma signal received on port 817 and outputs a result signal on a bus 834 .
Clipper 836 has a port 821 coupled to receive a signal from bus 834 , and functions in the same manner as that described above in reference to clipper 824 , to generate a signal on bus 838 .
A multiplexer 840 has ports 823 and 825 respectively coupled to buses 826 and 838 . Multiplexer 840 also has a control terminal 827 coupled to a line 842 carrying signal component_type. Multiplexer 840 propagates to a bus 844 (1) signals received on port 823 if signal component_type is, for example, active and (2) signals received on port 825 if signal component_type is, for example, inactive.
OSD mix 516 (FIG. 9) includes a subtractor 902 that has ports 901 and 903 respectively coupled to buses 844 and 920 . Bus 844 carries a pixel component from fader 514 and bus 920 carries a pixel component of an OSD image from OSD decoder 518 . Subtractor 902 subtracts the signal of the OSD pixel component from signal of the pixel component received on port 901 and provides a difference signal on a bus 904 .
A multiplier 906 has ports 905 and 907 respectively coupled to buses 904 and 922 . Bus 922 carries the OSD mix weight (e.g., “mw OSD ”) from OSD decoder 518 . Multiplier 906 multiplies the signal received on port 905 with the signal of the OSD mix weight and provides a product signal on a bus 908 . An adder 910 has ports 909 and 911 respectively coupled to buses 920 and 908 . Adder 910 adds the signal received on port 909 to the signal received on port 911 and provides a result signal on a bus 912 .
A multiplexer 914 has ports 913 and 915 respectively coupled to buses 844 and 912 . Multiplexer 914 also has a control terminal 917 coupled to a line 918 that carries a control signal (e.g., “signal OSD_enable”) from OSD_enable bit 512 B in host register 512 . If OSD_enable bit 512 B is active, multiplexer 914 propagates the signals received on terminal 915 (a pixel component of an OSD mix image) to a bus 916 . Otherwise, multiplexer 914 propagates the signals received on terminal 913 (a pixel component of the video image received from fade circuit 514 ) to bus 916 . Bus 916 is coupled to DAC 238 (FIG. 3 ). DAC 238 converts the pixel components into analog signals for display on monitor 106 (FIG. 2 A).
In one variation, an OSD mix 520 (FIG. 10) includes a multiplier 1002 , a multiplier 1004 , and an adder 1010 . Multiplier 1002 has ports 1001 and 1009 respectively coupled to buses 844 and 922 . Multiplier 1002 multiplies the signal received on port 1001 with the signal of the OSD mix weight received on port 922 and provides a product signal on a bus 1006 .
Multiplier 1004 has ports 1003 and 1011 respectively coupled to buses 920 and 1014 . Bus 1014 carries a signal of one less the OSD mix weight (e.g., 1−mw OSD ). Bus 1014 is, for example, from OSD decoder 518 . Multiplier 1004 multiplies the signal received on port 1003 received on port 1011 and provides a product signal on a bus 1008 .
Adder 1010 has ports 1005 and 1007 respectively coupled to buses 1006 and 1008 . Adder 1010 adds the signals received on port 1005 and port 1007 and provides a result signal on a bus 1012 . In this variation, port 915 of multiplexer 914 is coupled to bus 1012 .
Numerous modifications and adaptations of the embodiments described herein will be apparent to the skilled artisan in view of the disclosure. As one example, the SPU mix 510 can be similarly configured as OSD Mix 520 of FIG. 10, where subtractor 702 , multiplier 706 , and adder 710 are replaced by two multipliers and an adder. Also, instead of using the linear arithmetic operations to implement fade in and fade out, a nonlinear operation can be used. Instead of using a single arithmetic unit 848 (FIG. 2 B and FIG. 8) for both chroma values, two arithmetic units can be used, one for each chroma value. Also instead of adjusting the pixel components of luma, chroma blue, and chroma red, fader 514 can be used to adjust pixel components in other color space such as RGB and YUV. Numerous such changes and modifications are encompassed by the attached claims.
APPENDIX A
-- q has layer 2 (spu) mixed IN
PROCESS (reset, clk)
variable tmp : integer;
variable tmp_luma : integer;
variable tmp_chroma : integer;
variable tmp_chroma_fade_out : integer;
variable tmp_chroma_scaled : integer;
variable chroma_scaled_vec : std_logic_vector(21 downto
0);
variable tmp_fade_out : integer;
BEGIN
IF (reset = ‘1’) THEN
q <= ( others => ‘0’ );
ELSEIF (clk′EVENT AND clk = ‘1’) THEN
IF ((spu_enable = ‘0’) OR (video_only = ‘1’))
THEN
tmp := 32 * b_int;
ELSE
tmp := 32 * a_int + z_int;
END IF;
tmp_luna : =
conv_integer(signed(fade_out_1));
tmp_chroma: = conv_integer(signed(fade_out_c));
IF (fade_out_en = ‘1’ AND pel_is_main = ‘1’)
THEN
IF (pel_state_2d(0) = ‘0’) THEN --
chroma
-- b_int = tmp*2, tmp=*2, tmp_b_int*32,
thus tmp_chroma * 64
tmp_chroma_scaled := (tmp -
128*64) * tmp_chroma;
chroma_scaled_vec :=
conv_std_logic_vector(tmp_chroma_scaled,22);
tmp_chroma_fade_out :=
conv_integer(signed(chroma_scaled_vec(21
downto 8)));
tmp_fade_out :=
tmp_chroma_fade_out + 128*64;
ELSE
tmp_fade_out := tmp − tmp_luna *
64;
IF (tmp_fade_out < 0) THEN
tmp_fade_out := 0;
ELSIF (tmp_fade_out > 64*255)
THEN tmp_fade_out := 64*255;
END IF;
END IF;
ELSE
temp _fadeout := tmp;
END IF:
q <= conv_std_logic_vector (tmp_fade_out,
14);
END IF;
END PROCESS;
|
A fade circuit adjusts the luma as well as one or more chroma components of a main video so that the fade ins and fade outs of the main video do not change the color of an on-screen display image, such as the volume bar. In one embodiment, luma component (Y) is adjusted by subtracting a fade factor from the luma component to form a faded luma component. At the same time, one or more chroma components (Cb and Cr) are scaled by (1) subtracting a predetermined value from the chroma component to form a resultant, (2) multiplying the resultant with a scale factor to form a product, and (3) adding the predetermined value to the product to form a faded chroma component.
| 6
|
[0001] This is a national phase filing of the Application No. PCT/DE96/01369, which was filed with the Patent Corporation Treaty on Jul. 19, 1996, and is entitled to priority of the German Patent Application P 195 26 386.3, filed Jul. 19, 1995.
FIELD OF THE INVENTION
[0002] This invention relates to a DNA coding for a peptide of a papilloma virus major capsid protein. Moreover, this invention deals with a papilloma virus genome containing such a DNA. In addition, this invention concerns proteins coded by the papilloma virus genome and virus-like particles as well as antibodies directed against them and their use for diagnosis, treatment and vaccination.
BACKGROUND OF THE INVENTION
[0003] It is known that papilloma viruses infect the epithelium of human beings and animals. Human papilloma viruses (hereinafter referred to as HP viruses) are found in benign epithelial neoplasms, e.g warts, condylomas in the genital zone, and malignant epithelial neoplasms, e.g carcinomas of the skin and the uterus. Zur Hausen, 1989, Cancer Research 49:4677-4681. HP viruses are also considered for the growth of malignant tumors in the respiratory tract. Zur Hausen, 1976, Cancer Research 36:530. Besides, HP viruses are considered at least jointly responsible for the growth of squamous carcinomas of the lung. Syrjänen, 1980, Lung 158:131-142.
[0004] Papilloma viruses have an icosahedral capsid without envelope in which a circular, double-stranded DNA molecule of about 7900 bp is present. The capsid comprises a major capsid protein (L 1 ) and a minor capsid protein (L 2 ). Both proteins, coexpressed or L 1 expressed alone, result in vitro in the formation of virus-like particles Kirnbauer et al., 1993, Journal of Virology 67:6929-6936.
[0005] Papilloma viruses cannot be proliferated in monolayer cell culture. Therefore, their characterization is extremely difficult, the detection of papilloma viruses already creating considerable problems. This applies especially to papilloma viruses in carcinomas of the skin. A reliable detection thereof and thus well-calculated steps taken thereagainst are not possible by now.
[0006] Thus, it is the object of the present invention to provide a product by which papilloma viruses can be detected, particularly in carcinomas of the skin. Furthermore, a product should be provided to be able to take therapeutic steps against these papilloma viruses.
SUMMARY OF THE INVENTION
[0007] This invention relates to a DNA coding for a peptide of a papilloma virus major capsid protein. Moreover, this invention deals with a papilloma virus genome containing such a DNA. Furthermore, this invention concerns proteins coded by the papilloma virus genome and virus-like particles as well as antibodies directed thereagainst and the use thereof for diagnosis, treatment and vaccination.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] [0008]FIG. 1 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS19-6 with DSM (Deutsche Sammlung von Mikroorganismen und Zellkulturen [German-type collection of micro-organisms and cell cultures]) under DSM 10104 on Jul. 11, 1995.
[0009] [0009]FIG. 2 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS200-1 with DSM under DSM 10096 on Jul. 11, 1995.
[0010] [0010]FIG. 3 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS201-1 with DSM under DSM 10097 on Jul. 11, 1995.
[0011] [0011]FIG. 4 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS202-8 with DSM under DSM 10098 on Jul. 11, 1995.
[0012] [0012]FIG. 5 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS203-2 with DSM under DSM 10099 on Jul. 11, 1995.
[0013] [0013]FIG. 6 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS204-4 with DSM under DSM 10100 on Jul. 11, 1995.
[0014] [0014]FIG. 7 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS205-1 with DSM under DSM 10101 on Jul. 11, 1995.
[0015] [0015]FIG. 8 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS206-2 with DSM under DSM 10109 on Jul. 13, 1995.
[0016] [0016]FIG. 9 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS207-22 with DSM under DSM 10102 on Jul. 11, 1995.
[0017] [0017]FIG. 10 shows the base sequence and the amino acid sequence, derived therefrom, of a DNA coding for a peptide of L 1 of a papilloma virus. This DNA was deposited as plasmid VS208-1 with DSM under DSM 10103 on Jul. 11, 1995.
DETAILED DESCRIPTION OF THE INVENTION
[0018] It is the object of the present invention to provide a product by which papilloma viruses can be detected, particularly in carcinomas of the skin. Furthermore, a product is provided which enables to take therapeutic steps against these papilloma viruses.
[0019] Accordingly, the subject matter of the invention relates to a DNA coding for a peptide of a papilloma virus major capsid protein (L 1 ), the peptide comprising the amino acid sequence of FIG. 1, FIG. 2, FIG. 3, FIG. 4, FIG. 5, FIG. 6, FIG. 7, FIG. 8, FIG. 9 or FIG. 10 or an amino acid sequence differing therefrom by one or more amino acids.
[0020] A further subject matter of the invention relates to a DNA coding for a peptide of a papilloma virus major capsid protein, the DNA comprising the base sequence of FIG. 1, FIG. 2, FIG. 3, FIG. 4, FIG. 5, FIG. 6, FIG. 7, FIG. 8, FIG. 9 or FIG. 10 or a base sequence differing therefrom by one or more base pairs.
[0021] The above DNA has the following sequence homology with respect to known papilloma viruses:
DNA of FIG. 1: 69.1% with respect to HP virus 65 DNA of FIG. 2: 80.7% with respect to HP virus 24 DNA of FIG. 3: 69.4% with respect to HP virus 48 DNA of FIG. 4: 66.3% with respect to HP virus 48 DNA of FIG. 5: 66.9% with respect to HP virus 65 DNA of FIG. 6: 66.4% with respect to HP virus 65 DNA of FIG. 7: 69.1% with respect to HP virus 4 DNA of FIG. 8: 68.7% with respect to HP virus 48 DNA of FIG. 9: 76.6% with respect to HP virus 48 DNA of FIG. 10: 81.8% with respect to HP virus 68
[0022] According to the invention, the above DNA can be present in a vector and expression vector, respectively. A person skilled in the art is familiar with examples thereof. In the case of an expression vector for E. coli, these are e.g pGEMEX, pUC derivatives, pGEM-T and pGEX-2T. For the expression in yeast e.g. pY100 and Ycpadl have to be mentioned, while for the expression in animal cells e.g. pKCR, pEF-BOS, cDM8 and pCEV4 have to be indicated.
[0023] The person skilled in the art knows suitable cells to express the above DNA present in an expression vector. Examples of such cells comprise the E. coli strains HB101, DH1, x1776, JM101, JM 109, and XL1-Blue, the yeast strain Saccharomyces cerevisiae and the animal cells L, NH-3T3, FM3A, CHO, COS, Vero, and HeLa.
[0024] The person skilled in the art knows in which way the above DNA has to be inserted in an expression vector. He is also familiar with the fact that the above DNA can be inserted in connection with a DNA coding for another protein and peptide, respectively, so that the above DNA can be expressed in the form of a fusion protein.
[0025] A further subject matter of the invention relates to a papilloma virus genome which comprises the above DNA. The expression “papilloma virus genome” also comprises an incomplete genome, i.e. fragments of a papilloma virus genome, which comprise the above DNA. This may be e.g a DNA coding for L 1 or a portion thereof.
[0026] A common process can be used for the provision of the above papilloma virus genome, which comprises the following processing steps:
[0027] (a) isolation of the total DNA from a biopsy of epithelial neoplasm,
[0028] (b) hybridization of the total DNA of (a) with the above DNA so as to detect a papilloma virus genome included in the total DNA of (a), and
[0029] (c) cloning of the total DNA of (a) containing the papilloma virus genome, in a vector and optionally subcloning the resulting clone, all processing steps originating from common DNA recombination technique.
[0030] As far as the isolation, hybridization and cloning of cell DNA is concerned, reference is made by way of supplement to Sambrook et al., Molecular Cloning A Laboratory Manual, second edition, Cold Spring Harbor Laboratory (1989).
[0031] The expression “epithelial neoplasm” comprises any neoplasms of epithelium in man and animal. Examples of such neoplasms are warts, condylomas in the genital zone and carcinomas of the skin. The latter are used preferably to isolate the above papilloma virus genome.
[0032] The expression “vector” comprises any vectors suitable for cloning chromosomal DNA and extrachromosomal DNA, respectively. Examples of such vectors are cosmids such as pWE15 and Super Cos1, and phages such as λ-phages, e.g. λZAP expression vector, λZAPII vector and λgt10 vector. In the present case, λ-phages are used preferably. The above vectors are known and obtainable from the company of Stratagene.
[0033] Papilloma virus genomes according to the invention may be present in integrated form in chromosomal DNA or in extrachromosomal fashion. The person skilled in the art is familiar with processes serving the clarification thereof. He also knows processes serving for finding out the optimum restriction enzymes for cloning the papilloma virus genomes. He will orient himself by genomes of known papilloma viruses. In particular, the person skilled in the art will pay corresponding attention to the above-mentioned HP viruses.
[0034] The provision of a papilloma virus genome referred to as VS19-6 is described by way of example. For this purpose, the total DNA is isolated from a biopsy of a squamous cell carcinoma, cleaved by BamHI and separated eletrophoretically in an agarose gel. The agarose gel is then subjected to a blotting method so as to transfer the DNA to a nitrocellulose membrane. It is inserted in a hybridization method in which the DNA of FIG. 1 is used as labeled sample, optionally in combination with a DNA of HP virus 65. Hybridization with the papilloma virus DNA present in the total DNA is obtained.
[0035] Moreover, the above total DNA cleaved by BamHI is cloned in a λ-phage. The corresponding clones, i.e. the clones containing the papilloma virus DNA are identified by hybridization with the DNA of FIG. 1, optionally in combination with a DNA of the HP virus 65. The insert of these clones is then subjected to a further cloning in a plasmid vector so as to obtain a clone which contains the papilloma virus genome VS19-6-G. The genome is confirmed by sequencing.
[0036] Further papilloma virus genomes are provided analogously. They are designated in accordance with the DNAs used for their provision, namely by: VS200-1-G, VS201-1-G, VS202-8-G, VS203-2-G, VS204-4-G, VS205-1-G, VS206-2-G, VS207-22-G and VS208-1-G, respectively.
[0037] A further subject matter of the invention relates to a protein which is coded by the above papilloma virus genome. Such a protein is e.g. a major capsid protein (L 1 ) or a minor capsid protein (L 2 ). An above protein is prepared as usual. The preparation of L 1 and L 2 , respectively, of the papilloma virus genome VS19-6-G is described by way of example. For this purpose, the HP virus 65 related to the DNA of FIG. 1 is used. The full sequence and the position of individual DNA regions coding for proteins are known in connection therewith. These DNAs are identified on the papilloma virus genome VS19-6-G by parallel restriction cleavages of both genomes and subsequent hybridization with various fragments concerning the DNA encoding L 1 and L 2 , respectively. They are confirmed by sequencing. The DNA coding for L 1 is referred to as VS19-6-G-L 1 DNA and the DNA coding for L 2 is referred to as VS19-6-G-L 2 DNA.
[0038] Furthermore, the DNA coding for L 1 and L 2 , respectively, is inserted in an expression vector. Examples thereof are mentioned above for E. coli, yeast and animal cells. In this connection, reference is made to the vector pGEX-2T as regards the expression in E. coli by way of supplement. Kimbauer et al., supra. Having inserted the VS19-6-G-L 1 DNA and VS19-6-G-L 2 DNA, one obtains pGEX-2T-VS19-6-G-L 1 and pGEX-2T-VS19-6-G-L 2 , respectively. After transforming E. coli, these expression vectors express a glutathione S transferase L 1 fusion protein and glutathione S transferase L 2 fusion protein, respectively. The proteins are purified as usual.
[0039] The bacculovirus system and vaccinia virus system, respectively, is mentioned for a further expression of the above DNA encoding L 1 and L 2 , respectively. Expression vectors usable for this purpose are e.g. pEV mod. and pSynwtVI for the bacculovirus system. Kirnbauer et al., supra. Especially vectors with the vaccinia virus “early” (p7.5 k) promoter and “late” (Psynth, p11K) promoter, respectively, have to be mentioned for the vaccinia virus system. Hagensee et al., 1993, Journal of Virology 67:315-322. The bacculovirus system is preferred in the present case. Having inserted the above DNA encoding L 1 and L 2 , respectively, in pEV mod., one obtains pEVmod.-VS19-6-G-L 1 and pEVmod.-VS19-6-G-L 2 , respectively.
[0040] The former expression vector as such or both expression vectors jointly lead to the formation of virus-like particles after infection of SF-9 insect cells. In the former case, such a particle comprises an L 1 protein, while in the latter case, it contains an L2 protein in addition to an L 1 protein.
[0041] A virus-like particle of the latter case is also obtained by inserting the above VS 19-6-G-L 1 and VSI9-6-G-L2 DNAs jointly in the expression vector pSynwtVI and using the resulting pSynwtVI-VS19-6-G-L1/L2 for the infection of SF-9 insect cells. The above virus-like particles are purified as usual. They also represent a subject matter of the invention.
[0042] A further subject matter of the invention relates to an antibody directed against an above protein and virus-like particle, respectively. The preparation thereof is made as usual. It is described by way of example for the preparation of an antibody which is directed against a virus-like particle comprising L 1 of VS19-6-G. For this purpose, the virus-like particle is injected subcutaneously into BALB/c mice. This injection is repeated at intervals of 3 weeks each. About 2 weeks after the last injection, the serum containing the antibody is isolated and tested as usual.
[0043] In a preferred embodiment, the antibody is a monoclonal antibody. For its preparation, spleen cells are removed from the mice after the above fourth injection and fused with myeloma cells as usual. The further cloning also takes place according to known methods.
[0044] By means of the present invention, it is possible to detect papilloma viruses, particularly in carcinomas of the skin. For this purpose, the DNA according to the invention can be used as such or when comprised by a further DNA. The latter may also be a papilloma virus genome or a portion thereof.
[0045] The present invention also enables the provision of formerly unknown papilloma viruses. They are found especially in carcinomas of the skin. In addition, the invention supplies proteins and virus-like particles which originate from these papilloma viruses. Moreover, antibodies are provided which are directed against these proteins and particles, respectively.
[0046] The present invention also enables to take diagnostic and therapeutic steps in the case of papilloma virus diseases. Moreover, it supplies the possibility of building up a vaccine against papilloma virus infections. Thus, the present invention represents a break-through in the field of papilloma virus research.
[0047] The below examples explain the invention in more detail. The following preparations and examples are given to enable those skilled in the art to more clearly understand and to practice the present invention. The present invention, however, is not limited in scope by the exemplified embodiments, which are intended as illustrations of single aspects of the invention only, and methods which are functionally equivalent are within the scope of the invention. Indeed, various modifications of the invention in addition to those described herein will become apparent to those skilled in the art from the foregoing description and accompanying drawings. Such modifications are intended to fall within the scope of the appended claims.
EXAMPLES
A. Example 1
Identification of the Papilloma Virus Genome VS19-6-G
[0048] The total DNA is isolated from a biopsy of a squamous cell carcinoma of an immuno-suppressed person. 10 μg of this DNA are cleaved by the restriction enzyme BamHI and separated electrophoretically in a 0.5% agarose gel. At the same time, 10 μg of the above DNA, which was not cleaved, is also separated. The agarose gel is subjected to a blotting method so as to transfer the DNA from the agarose gel to a nitrocellulose membrane. It is employed in a hybridization method in which the above DNA of FIG. 1 is used in combination with the HP virus-65 DNA as 32 P-labeled sample. Hybridization with the blotted DNA is obtained.
[0049] The person skilled in the field of DNA recombination technique is familiar with the above methods. Reference is made to Sambrook et al., supra, by way of supplement.
Example 2
Cloning of the Papilloma Virus Genome VS19-6-G.
[0050] The biopsy DNA obtained from Example 1 is cleaved by the restriction enzyme BamHI. The resulting fragments are used in a ligase reaction in which the dephosphorylated vector λZAP express cleaved by BamHI is also present. The resulting recombinant DNA molecules are packed in bacteriophages, and they are used for infecting bacteria. For these processing steps, the ZAP express vector kit offered by the company of Stratagene is used. The resulting phage plaques are then subjected to a hybridization process which uses the 32 P-labeled DNA of FIG. 1 employed in Example 1 in combination with 32 P-labeled HP virus-65 DNA. Hybridization with corresponding phage plaques is obtained. The BamHI fragments of VS19-6-G are isolated therefrom and used in a further ligase reaction together with a BamHI-cleaved, dephosphorylated plasmid vector, pBluescript. The resulting recombinant DNA molecules are used for transforming bacteria, E. coli XL 1-Blue. By restriction cleavages and hybridization with the above DNA samples, respectively, a bacterial clone containing the papilloma virus genome VS19-6-G is identified. The plasmid of this bacterial clone is referred to as pBlue-VS19-6-G.
[0051] All references cited within the body of the instant specification are hereby incorporated by reference in their entirety.
1
30
1
419
DNA
Papilloma virus
CDS
(1)...(417)
1
gga tcc atg cag gat ggt gac atg tgt gat ata gga ttc gga gct tgc 48
Gly Ser Met Gln Asp Gly Asp Met Cys Asp Ile Gly Phe Gly Ala Cys
1 5 10 15
aat ttc agg gca ttt cag caa gat agg tca ggt gtt cct tta gat ata 96
Asn Phe Arg Ala Phe Gln Gln Asp Arg Ser Gly Val Pro Leu Asp Ile
20 25 30
gta gat agt act tgc aag tat cca gac ttt ttg aaa atg aca aaa gac 144
Val Asp Ser Thr Cys Lys Tyr Pro Asp Phe Leu Lys Met Thr Lys Asp
35 40 45
aag tat ggt gat gaa tgc ttc ttt ttt ggt cgt cga gag cag ttg tat 192
Lys Tyr Gly Asp Glu Cys Phe Phe Phe Gly Arg Arg Glu Gln Leu Tyr
50 55 60
gca agg cat tat ttt acc aga gca ggc aca ata ggt gat tct att cca 240
Ala Arg His Tyr Phe Thr Arg Ala Gly Thr Ile Gly Asp Ser Ile Pro
65 70 75 80
acg cca tat cag gaa tct gaa ttt tac aga tct cca cag gat agc cag 288
Thr Pro Tyr Gln Glu Ser Glu Phe Tyr Arg Ser Pro Gln Asp Ser Gln
85 90 95
gct cag aat aat gtg gat tct cac att tat gta gcc act cct agt ggt 336
Ala Gln Asn Asn Val Asp Ser His Ile Tyr Val Ala Thr Pro Ser Gly
100 105 110
tct tta act agc agt gat gct cag ctg ttt aac aga cct tat tgg ctc 384
Ser Leu Thr Ser Ser Asp Ala Gln Leu Phe Asn Arg Pro Tyr Trp Leu
115 120 125
caa aat gct caa ggt acc aat aac gga atg gat cc 419
Gln Asn Ala Gln Gly Thr Asn Asn Gly Met Asp
130 135
2
139
PRT
Papilloma virus
2
Gly Ser Met Gln Asp Gly Asp Met Cys Asp Ile Gly Phe Gly Ala Cys
1 5 10 15
Asn Phe Arg Ala Phe Gln Gln Asp Arg Ser Gly Val Pro Leu Asp Ile
20 25 30
Val Asp Ser Thr Cys Lys Tyr Pro Asp Phe Leu Lys Met Thr Lys Asp
35 40 45
Lys Tyr Gly Asp Glu Cys Phe Phe Phe Gly Arg Arg Glu Gln Leu Tyr
50 55 60
Ala Arg His Tyr Phe Thr Arg Ala Gly Thr Ile Gly Asp Ser Ile Pro
65 70 75 80
Thr Pro Tyr Gln Glu Ser Glu Phe Tyr Arg Ser Pro Gln Asp Ser Gln
85 90 95
Ala Gln Asn Asn Val Asp Ser His Ile Tyr Val Ala Thr Pro Ser Gly
100 105 110
Ser Leu Thr Ser Ser Asp Ala Gln Leu Phe Asn Arg Pro Tyr Trp Leu
115 120 125
Gln Asn Ala Gln Gly Thr Asn Asn Gly Met Asp
130 135
3
419
DNA
Papilloma virus
3
ggatccattc cgttattggt accttgagca ttttggagcc aataaggtct gttaaacagc 60
tgagcatcac tgctagttaa agaaccacta ggagtggcta cataaatgtg agaatccaca 120
ttattctgag cctggctatc ctgtggagat ctgtaaaatt cagattcctg atatggcgtt 180
ggaatagaat cacctattgt gcctgctctg gtaaaataat gccttgcata caactgctct 240
cgacgaccaa aaaagaagca ttcatcacca tacttgtctt ttgtcatttt caaaaagtct 300
ggatacttgc aagtactatc tactatatct aaaggaacac ctgacctatc ttgctgaaat 360
gccctgaaat tgcaagctcc gaatcctata tcacacatgt caccatcctg catggatcc 419
4
434
DNA
Papilloma virus
CDS
(1)...(432)
4
gga tcc atg gag gac ggt gag atg gca gac ata gga tat ggt aat ctt 48
Gly Ser Met Glu Asp Gly Glu Met Ala Asp Ile Gly Tyr Gly Asn Leu
1 5 10 15
aat ttt aaa gct tta cag gaa aat agg cct gat gtt agt ctt gat att 96
Asn Phe Lys Ala Leu Gln Glu Asn Arg Pro Asp Val Ser Leu Asp Ile
20 25 30
gtc aat gaa acc tgc aaa tat cca gat ttt ttg aag atg caa aat gat 144
Val Asn Glu Thr Cys Lys Tyr Pro Asp Phe Leu Lys Met Gln Asn Asp
35 40 45
gtt tat gga gac tcc tgt ttc ttt ttt gct cgt aga gag caa tgt tat 192
Val Tyr Gly Asp Ser Cys Phe Phe Phe Ala Arg Arg Glu Gln Cys Tyr
50 55 60
gcc aga cac ttt ttt gta aga ggt ggc aac gta ggg gat gac att cct 240
Ala Arg His Phe Phe Val Arg Gly Gly Asn Val Gly Asp Asp Ile Pro
65 70 75 80
ggt gaa caa ata gac gca ggc aca tat aaa aat gat ttt tac att cca 288
Gly Glu Gln Ile Asp Ala Gly Thr Tyr Lys Asn Asp Phe Tyr Ile Pro
85 90 95
gga gca tca ggt cag aca caa aat aaa ata ggt aac tcc atg tat ttc 336
Gly Ala Ser Gly Gln Thr Gln Asn Lys Ile Gly Asn Ser Met Tyr Phe
100 105 110
cca aca gtt agt ggc tca tta gtg tct agt gat gct cag ctg ttt aat 384
Pro Thr Val Ser Gly Ser Leu Val Ser Ser Asp Ala Gln Leu Phe Asn
115 120 125
agg ccc tac tgg ctc caa cgc gca cag ggc cac aac aac ggc gtg gat 432
Arg Pro Tyr Trp Leu Gln Arg Ala Gln Gly His Asn Asn Gly Val Asp
130 135 140
cc 434
5
144
PRT
Papilloma virus
5
Gly Ser Met Glu Asp Gly Glu Met Ala Asp Ile Gly Tyr Gly Asn Leu
1 5 10 15
Asn Phe Lys Ala Leu Gln Glu Asn Arg Pro Asp Val Ser Leu Asp Ile
20 25 30
Val Asn Glu Thr Cys Lys Tyr Pro Asp Phe Leu Lys Met Gln Asn Asp
35 40 45
Val Tyr Gly Asp Ser Cys Phe Phe Phe Ala Arg Arg Glu Gln Cys Tyr
50 55 60
Ala Arg His Phe Phe Val Arg Gly Gly Asn Val Gly Asp Asp Ile Pro
65 70 75 80
Gly Glu Gln Ile Asp Ala Gly Thr Tyr Lys Asn Asp Phe Tyr Ile Pro
85 90 95
Gly Ala Ser Gly Gln Thr Gln Asn Lys Ile Gly Asn Ser Met Tyr Phe
100 105 110
Pro Thr Val Ser Gly Ser Leu Val Ser Ser Asp Ala Gln Leu Phe Asn
115 120 125
Arg Pro Tyr Trp Leu Gln Arg Ala Gln Gly His Asn Asn Gly Val Asp
130 135 140
6
434
DNA
Papilloma virus
6
ggatccacgc cgttgttgtg gccctgtgcg cgttggagcc agtagggcct attaaacagc 60
tgagcatcac tagacactaa tgagccacta actgttggga aatacatgga gttacctatt 120
ttattttgtg tctgacctga tgctcctgga atgtaaaaat catttttata tgtgcctgcg 180
tctatttgtt caccaggaat gtcatcccct acgttgccac ctcttacaaa aaagtgtctg 240
gcataacatt gctctctacg agcaaaaaag aaacaggagt ctccataaac atcattttgc 300
atcttcaaaa aatctggata tttgcaggtt tcattgacaa tatcaagact aacatcaggc 360
ctattttcct gtaaagcttt aaaattaaga ttaccatatc ctatgtctgc catctcaccg 420
tcctccatgg atcc 434
7
410
DNA
Papilloma virus
CDS
(1)...(408)
7
gga tcc cta gag gat ggt gat atg ggt gat ata gga ttt ggg cat gct 48
Gly Ser Leu Glu Asp Gly Asp Met Gly Asp Ile Gly Phe Gly His Ala
1 5 10 15
aat ttt agc cgt tta caa gaa gat aaa gca ggt gtg cca tta gaa tta 96
Asn Phe Ser Arg Leu Gln Glu Asp Lys Ala Gly Val Pro Leu Glu Leu
20 25 30
gtg gac act ttt agt ata tgg cct gac ttt tta cgc atg acc agt gat 144
Val Asp Thr Phe Ser Ile Trp Pro Asp Phe Leu Arg Met Thr Ser Asp
35 40 45
ata tat gga gat gct gtg ttt ttt tgg gga aag cga gaa cat atg ttt 192
Ile Tyr Gly Asp Ala Val Phe Phe Trp Gly Lys Arg Glu His Met Phe
50 55 60
gcc aga cat tta tgg gca aga gct gga act atg ggc gac gct att cca 240
Ala Arg His Leu Trp Ala Arg Ala Gly Thr Met Gly Asp Ala Ile Pro
65 70 75 80
gat aat aat gca gag ttt ttt ctg cat ccc aat ggt gca cct caa aat 288
Asp Asn Asn Ala Glu Phe Phe Leu His Pro Asn Gly Ala Pro Gln Asn
85 90 95
aag tta gcc tca ttt gct tat ttt cca aca cct agt ggt tct ctt aat 336
Lys Leu Ala Ser Phe Ala Tyr Phe Pro Thr Pro Ser Gly Ser Leu Asn
100 105 110
acc agt gat aat caa ttg ttt aat aag ccg tat tgg ttg cga aaa gct 384
Thr Ser Asp Asn Gln Leu Phe Asn Lys Pro Tyr Trp Leu Arg Lys Ala
115 120 125
cag ggc acc aac aat ggg atg gat cc 410
Gln Gly Thr Asn Asn Gly Met Asp
130 135
8
136
PRT
Papilloma virus
8
Gly Ser Leu Glu Asp Gly Asp Met Gly Asp Ile Gly Phe Gly His Ala
1 5 10 15
Asn Phe Ser Arg Leu Gln Glu Asp Lys Ala Gly Val Pro Leu Glu Leu
20 25 30
Val Asp Thr Phe Ser Ile Trp Pro Asp Phe Leu Arg Met Thr Ser Asp
35 40 45
Ile Tyr Gly Asp Ala Val Phe Phe Trp Gly Lys Arg Glu His Met Phe
50 55 60
Ala Arg His Leu Trp Ala Arg Ala Gly Thr Met Gly Asp Ala Ile Pro
65 70 75 80
Asp Asn Asn Ala Glu Phe Phe Leu His Pro Asn Gly Ala Pro Gln Asn
85 90 95
Lys Leu Ala Ser Phe Ala Tyr Phe Pro Thr Pro Ser Gly Ser Leu Asn
100 105 110
Thr Ser Asp Asn Gln Leu Phe Asn Lys Pro Tyr Trp Leu Arg Lys Ala
115 120 125
Gln Gly Thr Asn Asn Gly Met Asp
130 135
9
410
DNA
Papilloma virus
9
ggatccatcc cattgttggt gccctgagct tttcgcaacc aatacggctt attaaacaat 60
tgattatcac tggtattaag agaaccacta ggtgttggaa aataagcaaa tgaggctaac 120
ttattttgag gtgcaccatt gggatgcaga aaaaactctg cattattatc tggaatagcg 180
tcgcccatag ttccagctct tgcccataaa tgtctggcaa acatatgttc tcgctttccc 240
caaaaaaaca cagcatctcc atatatatca ctggtcatgc gtaaaaagtc aggccatata 300
ctaaaagtgt ccactaattc taatggcaca cctgctttat cttcttgtaa acggctaaaa 360
ttagcatgcc caaatcctat atcacccata tcaccatcct ctagggatcc 410
10
437
DNA
Papilloma virus
CDS
(1)...(435)
10
gga tcc att gag gat gcg gat atg agt gat ata gga ttt gga gct gtg 48
Gly Ser Ile Glu Asp Ala Asp Met Ser Asp Ile Gly Phe Gly Ala Val
1 5 10 15
aat ttt agc act ttc tct gaa agc cgg gct gat gca cct tta gaa tta 96
Asn Phe Ser Thr Phe Ser Glu Ser Arg Ala Asp Ala Pro Leu Glu Leu
20 25 30
atc aat tct att agt aaa tgg cct gat ttt att caa atg tct aag gat 144
Ile Asn Ser Ile Ser Lys Trp Pro Asp Phe Ile Gln Met Ser Lys Asp
35 40 45
att tat ggc gat aga atg ttt ttc ttt gga aaa cgt gag cag atg tat 192
Ile Tyr Gly Asp Arg Met Phe Phe Phe Gly Lys Arg Glu Gln Met Tyr
50 55 60
gca aga cac aca ttt tgt aaa gat ggt gct gtg gga gat gct att cca 240
Ala Arg His Thr Phe Cys Lys Asp Gly Ala Val Gly Asp Ala Ile Pro
65 70 75 80
gaa aat tta aat aat gat gag gat gtt cat cat agg ttt tta tta aat 288
Glu Asn Leu Asn Asn Asp Glu Asp Val His His Arg Phe Leu Leu Asn
85 90 95
cct aag cct gac gca cca cca tat tca aac tta gga aac agt act tac 336
Pro Lys Pro Asp Ala Pro Pro Tyr Ser Asn Leu Gly Asn Ser Thr Tyr
100 105 110
ttt cct atg cca agt ggt tca tta gtt agt agt gaa act caa tta ttt 384
Phe Pro Met Pro Ser Gly Ser Leu Val Ser Ser Glu Thr Gln Leu Phe
115 120 125
aac aga cca ttt tgg cta cat cga gca cag ggc acc aat aac ggc atg 432
Asn Arg Pro Phe Trp Leu His Arg Ala Gln Gly Thr Asn Asn Gly Met
130 135 140
gat cc 437
Asp
145
11
145
PRT
Papilloma virus
11
Gly Ser Ile Glu Asp Ala Asp Met Ser Asp Ile Gly Phe Gly Ala Val
1 5 10 15
Asn Phe Ser Thr Phe Ser Glu Ser Arg Ala Asp Ala Pro Leu Glu Leu
20 25 30
Ile Asn Ser Ile Ser Lys Trp Pro Asp Phe Ile Gln Met Ser Lys Asp
35 40 45
Ile Tyr Gly Asp Arg Met Phe Phe Phe Gly Lys Arg Glu Gln Met Tyr
50 55 60
Ala Arg His Thr Phe Cys Lys Asp Gly Ala Val Gly Asp Ala Ile Pro
65 70 75 80
Glu Asn Leu Asn Asn Asp Glu Asp Val His His Arg Phe Leu Leu Asn
85 90 95
Pro Lys Pro Asp Ala Pro Pro Tyr Ser Asn Leu Gly Asn Ser Thr Tyr
100 105 110
Phe Pro Met Pro Ser Gly Ser Leu Val Ser Ser Glu Thr Gln Leu Phe
115 120 125
Asn Arg Pro Phe Trp Leu His Arg Ala Gln Gly Thr Asn Asn Gly Met
130 135 140
Asp
145
12
437
DNA
Papilloma virus
12
ggatccatgc cgttattggt gccctgtgct cgatgtagcc aaaatggtct gttaaataat 60
tgagtttcac tactaactaa tgaaccactt ggcataggaa agtaagtact gtttcctaag 120
tttgaatatg gtggtgcgtc aggcttagga tttaataaaa acctatgatg aacatcctca 180
tcattattta aattttctgg aatagcatct cccacagcac catctttaca aaatgtgtgt 240
cttgcataca tctgctcacg ttttccaaag aaaaacattc tatcgccata aatatcctta 300
gacatttgaa taaaatcagg ccatttacta atagaattga ttaattctaa aggtgcatca 360
gcccggcttt cagagaaagt gctaaaattc acagctccaa atcctatatc actcatatcc 420
gcatcctcaa tggatcc 437
13
416
DNA
Papilloma virus
CDS
(1)...(414)
13
gga tcc atg gag gat ggt gaa atg ggc gac ata ggc ttt gga gcc ttt 48
Gly Ser Met Glu Asp Gly Glu Met Gly Asp Ile Gly Phe Gly Ala Phe
1 5 10 15
aat ttt aaa gcc cta cag aaa gat cgt gct ggt gtt agt tta gat tta 96
Asn Phe Lys Ala Leu Gln Lys Asp Arg Ala Gly Val Ser Leu Asp Leu
20 25 30
gtt gat aca ttc agt ata tgg cca gac ttt tta aaa atg act aat gat 144
Val Asp Thr Phe Ser Ile Trp Pro Asp Phe Leu Lys Met Thr Asn Asp
35 40 45
ata tat ggt gac agt atc ttt ttt tat ggt aaa aga gaa cag cta ttt 192
Ile Tyr Gly Asp Ser Ile Phe Phe Tyr Gly Lys Arg Glu Gln Leu Phe
50 55 60
agt aga cac ttg tgg gcc cgc gca gga acg gct gga gat gcc att cca 240
Ser Arg His Leu Trp Ala Arg Ala Gly Thr Ala Gly Asp Ala Ile Pro
65 70 75 80
tct cct gat aac aaa aat cta ata ttt cag ggt gat gat gca gtg cca 288
Ser Pro Asp Asn Lys Asn Leu Ile Phe Gln Gly Asp Asp Ala Val Pro
85 90 95
caa aag act gct ggg tct ttt act tat ttt agt gcc cct agt ggg tca 336
Gln Lys Thr Ala Gly Ser Phe Thr Tyr Phe Ser Ala Pro Ser Gly Ser
100 105 110
tta aca act agt gat tct cag tta ttt aat agg cca tat tgg tta aga 384
Leu Thr Thr Ser Asp Ser Gln Leu Phe Asn Arg Pro Tyr Trp Leu Arg
115 120 125
aga gct caa ggt acc aac aac ggt gtg gat cc 416
Arg Ala Gln Gly Thr Asn Asn Gly Val Asp
130 135
14
138
PRT
Papilloma virus
14
Gly Ser Met Glu Asp Gly Glu Met Gly Asp Ile Gly Phe Gly Ala Phe
1 5 10 15
Asn Phe Lys Ala Leu Gln Lys Asp Arg Ala Gly Val Ser Leu Asp Leu
20 25 30
Val Asp Thr Phe Ser Ile Trp Pro Asp Phe Leu Lys Met Thr Asn Asp
35 40 45
Ile Tyr Gly Asp Ser Ile Phe Phe Tyr Gly Lys Arg Glu Gln Leu Phe
50 55 60
Ser Arg His Leu Trp Ala Arg Ala Gly Thr Ala Gly Asp Ala Ile Pro
65 70 75 80
Ser Pro Asp Asn Lys Asn Leu Ile Phe Gln Gly Asp Asp Ala Val Pro
85 90 95
Gln Lys Thr Ala Gly Ser Phe Thr Tyr Phe Ser Ala Pro Ser Gly Ser
100 105 110
Leu Thr Thr Ser Asp Ser Gln Leu Phe Asn Arg Pro Tyr Trp Leu Arg
115 120 125
Arg Ala Gln Gly Thr Asn Asn Gly Val Asp
130 135
15
416
DNA
Papilloma virus
15
ggatccacac cgttgttggt accttgagct cttcttaacc aatatggcct attaaataac 60
tgagaatcac tagttgttaa tgacccacta ggggcactaa aataagtaaa agacccagca 120
gtcttttgtg gcactgcatc atcaccctga aatattagat ttttgttatc aggagatgga 180
atggcatctc cagccgttcc tgcgcgggcc cacaagtgtc tactaaatag ctgttctctt 240
ttaccataaa aaaagatact gtcaccatat atatcattag tcatttttaa aaagtctggc 300
catatactga atgtatcaac taaatctaaa ctaacaccag cacgatcttt ctgtagggct 360
ttaaaattaa aggctccaaa gcctatgtcg cccatttcac catcctccat ggatcc 416
16
413
DNA
Papilloma virus
CDS
(1)...(411)
16
gga tcc atg gag gac ggt gag atg agt gat aca ggt ttt ggt gct atg 48
Gly Ser Met Glu Asp Gly Glu Met Ser Asp Thr Gly Phe Gly Ala Met
1 5 10 15
aat ttt gat aat cta tgc gag gac aga gct tca ttt cct tta gac att 96
Asn Phe Asp Asn Leu Cys Glu Asp Arg Ala Ser Phe Pro Leu Asp Ile
20 25 30
ata aat gag acc tcc aag tgg cct gat ttt cta aaa atg aat aaa gat 144
Ile Asn Glu Thr Ser Lys Trp Pro Asp Phe Leu Lys Met Asn Lys Asp
35 40 45
cct tat gga gat cat ata ttt ttc ttt ggt tta cga gag cag tta tat 192
Pro Tyr Gly Asp His Ile Phe Phe Phe Gly Leu Arg Glu Gln Leu Tyr
50 55 60
tcc aga cat cat ggt gct cgg gga gga aaa atg gga gat act att cca 240
Ser Arg His His Gly Ala Arg Gly Gly Lys Met Gly Asp Thr Ile Pro
65 70 75 80
gaa aat aca gca ggc gaa tat tat tat cct cct act gat ggt gct cag 288
Glu Asn Thr Ala Gly Glu Tyr Tyr Tyr Pro Pro Thr Asp Gly Ala Gln
85 90 95
caa aat ata ggt tca cat att tat ttc aat act gtt agt gga tct tta 336
Gln Asn Ile Gly Ser His Ile Tyr Phe Asn Thr Val Ser Gly Ser Leu
100 105 110
aca tct tca gaa act cag ata ttt aat agg cca tat ttt tta caa cgt 384
Thr Ser Ser Glu Thr Gln Ile Phe Asn Arg Pro Tyr Phe Leu Gln Arg
115 120 125
gca cag ggc aca aac aac gga gtg gat cc 413
Ala Gln Gly Thr Asn Asn Gly Val Asp
130 135
17
137
PRT
Papilloma virus
17
Gly Ser Met Glu Asp Gly Glu Met Ser Asp Thr Gly Phe Gly Ala Met
1 5 10 15
Asn Phe Asp Asn Leu Cys Glu Asp Arg Ala Ser Phe Pro Leu Asp Ile
20 25 30
Ile Asn Glu Thr Ser Lys Trp Pro Asp Phe Leu Lys Met Asn Lys Asp
35 40 45
Pro Tyr Gly Asp His Ile Phe Phe Phe Gly Leu Arg Glu Gln Leu Tyr
50 55 60
Ser Arg His His Gly Ala Arg Gly Gly Lys Met Gly Asp Thr Ile Pro
65 70 75 80
Glu Asn Thr Ala Gly Glu Tyr Tyr Tyr Pro Pro Thr Asp Gly Ala Gln
85 90 95
Gln Asn Ile Gly Ser His Ile Tyr Phe Asn Thr Val Ser Gly Ser Leu
100 105 110
Thr Ser Ser Glu Thr Gln Ile Phe Asn Arg Pro Tyr Phe Leu Gln Arg
115 120 125
Ala Gln Gly Thr Asn Asn Gly Val Asp
130 135
18
413
DNA
Papilloma virus
18
ggatccactc cgttgtttgt gccctgtgca cgttgtaaaa aatatggcct attaaatatc 60
tgagtttctg aagatgttaa agatccacta acagtattga aataaatatg tgaacctata 120
ttttgctgag caccatcagt aggaggataa taatattcgc ctgctgtatt ttctggaata 180
gtatctccca tttttcctcc ccgagcacca tgatgtctgg aatataactg ctctcgtaaa 240
ccaaagaaaa atatatgatc tccataagga tctttattca tttttagaaa atcaggccac 300
ttggaggtct catttataat gtctaaagga aatgaagctc tgtcctcgca tagattatca 360
aaattcatag caccaaaacc tgtatcactc atctcaccgt cctccatgga tcc 413
19
428
DNA
Papilloma virus
CDS
(1)...(426)
19
gga tcc att caa gat ggg gat atg tgc gat att ggc ttt gga gca gcc 48
Gly Ser Ile Gln Asp Gly Asp Met Cys Asp Ile Gly Phe Gly Ala Ala
1 5 10 15
aat ttt aaa gca tta cag caa gat aaa tca ggt gtt cct tta gat att 96
Asn Phe Lys Ala Leu Gln Gln Asp Lys Ser Gly Val Pro Leu Asp Ile
20 25 30
gtt gac agt ata tgt aaa tgg cca gat att att aaa atg gag caa gaa 144
Val Asp Ser Ile Cys Lys Trp Pro Asp Ile Ile Lys Met Glu Gln Glu
35 40 45
ata tat gga gac aga tta ttt ttc ttt act aaa cgt gag caa gct tat 192
Ile Tyr Gly Asp Arg Leu Phe Phe Phe Thr Lys Arg Glu Gln Ala Tyr
50 55 60
gcc agg cat tat ttc gct cgt gca gga att aat ggt gat tct tta cca 240
Ala Arg His Tyr Phe Ala Arg Ala Gly Ile Asn Gly Asp Ser Leu Pro
65 70 75 80
gat gca atg aaa cca gga gaa tat tat ctc tct cct aag ttg gga gat 288
Asp Ala Met Lys Pro Gly Glu Tyr Tyr Leu Ser Pro Lys Leu Gly Asp
85 90 95
gag caa gta ccc cag aaa gac tta gga tcg cat att tat ttt cct aca 336
Glu Gln Val Pro Gln Lys Asp Leu Gly Ser His Ile Tyr Phe Pro Thr
100 105 110
gtt agt ggt tct ttg gtt tct agt gaa aat cag tta ttt aac aga cca 384
Val Ser Gly Ser Leu Val Ser Ser Glu Asn Gln Leu Phe Asn Arg Pro
115 120 125
tat tgg ttg cag aaa tct cag ggc aca aac aac ggc gtg gat 426
Tyr Trp Leu Gln Lys Ser Gln Gly Thr Asn Asn Gly Val Asp
130 135 140
cc 428
20
142
PRT
Papilloma virus
20
Gly Ser Ile Gln Asp Gly Asp Met Cys Asp Ile Gly Phe Gly Ala Ala
1 5 10 15
Asn Phe Lys Ala Leu Gln Gln Asp Lys Ser Gly Val Pro Leu Asp Ile
20 25 30
Val Asp Ser Ile Cys Lys Trp Pro Asp Ile Ile Lys Met Glu Gln Glu
35 40 45
Ile Tyr Gly Asp Arg Leu Phe Phe Phe Thr Lys Arg Glu Gln Ala Tyr
50 55 60
Ala Arg His Tyr Phe Ala Arg Ala Gly Ile Asn Gly Asp Ser Leu Pro
65 70 75 80
Asp Ala Met Lys Pro Gly Glu Tyr Tyr Leu Ser Pro Lys Leu Gly Asp
85 90 95
Glu Gln Val Pro Gln Lys Asp Leu Gly Ser His Ile Tyr Phe Pro Thr
100 105 110
Val Ser Gly Ser Leu Val Ser Ser Glu Asn Gln Leu Phe Asn Arg Pro
115 120 125
Tyr Trp Leu Gln Lys Ser Gln Gly Thr Asn Asn Gly Val Asp
130 135 140
21
428
DNA
Papilloma virus
21
ggatccacgc cgttgtttgt gccctgagat ttctgcaacc aatatggtct gttaaataac 60
tgattttcac tagaaaccaa agaaccacta actgtaggaa aataaatatg cgatcctaag 120
tctttctggg gtacttgctc atctcccaac ttaggagaga gataatattc tcctggtttc 180
attgcatctg gtaaagaatc accattaatt cctgcacgag cgaaataatg cctggcataa 240
gcttgctcac gtttagtaaa gaaaaataat ctgtctccat atatttcttg ctccatttta 300
ataatatctg gccatttaca tatactgtca acaatatcta aaggaacacc tgatttatct 360
tgctgtaatg ctttaaaatt ggctgctcca aagccaatat cgcacatatc cccatcttga 420
atggatcc 428
22
416
DNA
Papilloma virus
CDS
(1)...(414)
22
gga tcc ctg gaa gat ggt gaa atg gga gat att ggg ttt ggt gca gca 48
Gly Ser Leu Glu Asp Gly Glu Met Gly Asp Ile Gly Phe Gly Ala Ala
1 5 10 15
aat ttt aaa acg tta caa aag gac aga gcc gga gtc agc tta gat tta 96
Asn Phe Lys Thr Leu Gln Lys Asp Arg Ala Gly Val Ser Leu Asp Leu
20 25 30
gta gac act ttt agc att tgg cct gac ttt tta aaa atg act aat gat 144
Val Asp Thr Phe Ser Ile Trp Pro Asp Phe Leu Lys Met Thr Asn Asp
35 40 45
att tac gga gat agt atg ttt ttc ttt gga aaa cgt gag cag ctc ttt 192
Ile Tyr Gly Asp Ser Met Phe Phe Phe Gly Lys Arg Glu Gln Leu Phe
50 55 60
ggc aga cat ctt tgg aca aga gca ggt act ccc ggc gat gca att cct 240
Gly Arg His Leu Trp Thr Arg Ala Gly Thr Pro Gly Asp Ala Ile Pro
65 70 75 80
act cca gaa aat ata aac tta ata ttt cca gct gat gat ggc act agt 288
Thr Pro Glu Asn Ile Asn Leu Ile Phe Pro Ala Asp Asp Gly Thr Ser
85 90 95
caa aag gat gca ggg tct ttc act tac ttt act tca gct agt gga tct 336
Gln Lys Asp Ala Gly Ser Phe Thr Tyr Phe Thr Ser Ala Ser Gly Ser
100 105 110
ctt aat act agc gat tca caa tta ttt aat aga cct tac tgg ctt cga 384
Leu Asn Thr Ser Asp Ser Gln Leu Phe Asn Arg Pro Tyr Trp Leu Arg
115 120 125
cgt gca caa ggc aca aac aat ggc gtg gat cc 416
Arg Ala Gln Gly Thr Asn Asn Gly Val Asp
130 135
23
138
PRT
Papilloma virus
23
Gly Ser Leu Glu Asp Gly Glu Met Gly Asp Ile Gly Phe Gly Ala Ala
1 5 10 15
Asn Phe Lys Thr Leu Gln Lys Asp Arg Ala Gly Val Ser Leu Asp Leu
20 25 30
Val Asp Thr Phe Ser Ile Trp Pro Asp Phe Leu Lys Met Thr Asn Asp
35 40 45
Ile Tyr Gly Asp Ser Met Phe Phe Phe Gly Lys Arg Glu Gln Leu Phe
50 55 60
Gly Arg His Leu Trp Thr Arg Ala Gly Thr Pro Gly Asp Ala Ile Pro
65 70 75 80
Thr Pro Glu Asn Ile Asn Leu Ile Phe Pro Ala Asp Asp Gly Thr Ser
85 90 95
Gln Lys Asp Ala Gly Ser Phe Thr Tyr Phe Thr Ser Ala Ser Gly Ser
100 105 110
Leu Asn Thr Ser Asp Ser Gln Leu Phe Asn Arg Pro Tyr Trp Leu Arg
115 120 125
Arg Ala Gln Gly Thr Asn Asn Gly Val Asp
130 135
24
416
DNA
Papilloma virus
24
ggatccacgc cattgtttgt gccttgtgca cgtcgaagcc agtaaggtct attaaataat 60
tgtgaatcgc tagtattaag agatccacta gctgaagtaa agtaagtgaa agaccctgca 120
tccttttgac tagtgccatc atcagctgga aatattaagt ttatattttc tggagtagga 180
attgcatcgc cgggagtacc tgctcttgtc caaagatgtc tgccaaagag ctgctcacgt 240
tttccaaaga aaaacatact atctccgtaa atatcattag tcatttttaa aaagtcaggc 300
caaatgctaa aagtgtctac taaatctaag ctgactccgg ctctgtcctt ttgtaacgtt 360
ttaaaatttg ctgcaccaaa cccaatatct cccatttcac catcttccag ggatcc 416
25
425
DNA
Papilloma virus
CDS
(1)...(423)
25
gga tcc cta gag gat ggg gag atg ggt gat ata gga ttt ggt gct gct 48
Gly Ser Leu Glu Asp Gly Glu Met Gly Asp Ile Gly Phe Gly Ala Ala
1 5 10 15
aat ttt gct aag ctt atg caa gat aga gct ggt gta cct ctg gaa tta 96
Asn Phe Ala Lys Leu Met Gln Asp Arg Ala Gly Val Pro Leu Glu Leu
20 25 30
ata gat agt att agt ata tgg cca gat ttt cta aaa atg aca aag gat 144
Ile Asp Ser Ile Ser Ile Trp Pro Asp Phe Leu Lys Met Thr Lys Asp
35 40 45
att tat gga aat gaa gta ttt ttc ttt gga aaa cgc gag caa tgt tat 192
Ile Tyr Gly Asn Glu Val Phe Phe Phe Gly Lys Arg Glu Gln Cys Tyr
50 55 60
gct cgc cat tta ttt gcc aga gct ggt act atg gga gaa cca gta cct 240
Ala Arg His Leu Phe Ala Arg Ala Gly Thr Met Gly Glu Pro Val Pro
65 70 75 80
aat gag act aat gga gta aat ttt ata aat gca aaa cca gga gat cca 288
Asn Glu Thr Asn Gly Val Asn Phe Ile Asn Ala Lys Pro Gly Asp Pro
85 90 95
aat ccc agg agc gct cat atg ggt tct tca gta tac ttt gca aca cct 336
Asn Pro Arg Ser Ala His Met Gly Ser Ser Val Tyr Phe Ala Thr Pro
100 105 110
agt ggc tcc ctt aat acc agt gat tca caa ata ttt aac aga cct tat 384
Ser Gly Ser Leu Asn Thr Ser Asp Ser Gln Ile Phe Asn Arg Pro Tyr
115 120 125
tgg tta cga cgg gct caa gga acg aac aac ggc atg gat cc 425
Trp Leu Arg Arg Ala Gln Gly Thr Asn Asn Gly Met Asp
130 135 140
26
141
PRT
Papilloma virus
26
Gly Ser Leu Glu Asp Gly Glu Met Gly Asp Ile Gly Phe Gly Ala Ala
1 5 10 15
Asn Phe Ala Lys Leu Met Gln Asp Arg Ala Gly Val Pro Leu Glu Leu
20 25 30
Ile Asp Ser Ile Ser Ile Trp Pro Asp Phe Leu Lys Met Thr Lys Asp
35 40 45
Ile Tyr Gly Asn Glu Val Phe Phe Phe Gly Lys Arg Glu Gln Cys Tyr
50 55 60
Ala Arg His Leu Phe Ala Arg Ala Gly Thr Met Gly Glu Pro Val Pro
65 70 75 80
Asn Glu Thr Asn Gly Val Asn Phe Ile Asn Ala Lys Pro Gly Asp Pro
85 90 95
Asn Pro Arg Ser Ala His Met Gly Ser Ser Val Tyr Phe Ala Thr Pro
100 105 110
Ser Gly Ser Leu Asn Thr Ser Asp Ser Gln Ile Phe Asn Arg Pro Tyr
115 120 125
Trp Leu Arg Arg Ala Gln Gly Thr Asn Asn Gly Met Asp
130 135 140
27
425
DNA
Papilloma virus
27
ggatccatgc cgttgttcgt tccttgagcc cgtcgtaacc aataaggtct gttaaatatt 60
tgtgaatcac tggtattaag ggagccacta ggtgttgcaa agtatactga agaacccata 120
tgagcgctcc tgggatttgg atctcctggt tttgcattta taaaatttac tccattagtc 180
tcattaggta ctggttctcc catagtacca gctctggcaa ataaatggcg agcataacat 240
tgctcgcgtt ttccaaagaa aaatacttca tttccataaa tatcctttgt catttttaga 300
aaatctggcc atatactaat actatctatt aattccagag gtacaccagc tctatcttgc 360
ataagcttag caaaattagc agcaccaaat cctatatcac ccatctcccc atcctctagg 420
gatcc 425
28
398
DNA
Papilloma virus
CDS
(1)...(396)
28
gga tcc ctt gag gat ggg gaa atg ata gat aca ggc tat ggt gcc atg 48
Gly Ser Leu Glu Asp Gly Glu Met Ile Asp Thr Gly Tyr Gly Ala Met
1 5 10 15
gac ttt cgt aca ttg cag gaa acc aaa agt gag gta cca cta gat att 96
Asp Phe Arg Thr Leu Gln Glu Thr Lys Ser Glu Val Pro Leu Asp Ile
20 25 30
tgc caa tcc gtg tgt aaa tat cct gat tat ttg cag atg tct gct gat 144
Cys Gln Ser Val Cys Lys Tyr Pro Asp Tyr Leu Gln Met Ser Ala Asp
35 40 45
gta tat ggg gac agt atg ttt ttt tgt ttg cgc aag gaa cag ttg ttt 192
Val Tyr Gly Asp Ser Met Phe Phe Cys Leu Arg Lys Glu Gln Leu Phe
50 55 60
gcc agg cac ttt tgg aat aga ggt ggc atg gtg ggc gac aca ata cct 240
Ala Arg His Phe Trp Asn Arg Gly Gly Met Val Gly Asp Thr Ile Pro
65 70 75 80
tca gag tta tat att aaa ggc acg gat ata cgt gag cgt cct ggt act 288
Ser Glu Leu Tyr Ile Lys Gly Thr Asp Ile Arg Glu Arg Pro Gly Thr
85 90 95
cat gta tat tcc cct tcc cca agt ggc tct atg gtc tct tct gat tcc 336
His Val Tyr Ser Pro Ser Pro Ser Gly Ser Met Val Ser Ser Asp Ser
100 105 110
cag ttg ttt aat aag ccc tat tgg ttg cat aag gcc caa ggc cac aat 384
Gln Leu Phe Asn Lys Pro Tyr Trp Leu His Lys Ala Gln Gly His Asn
115 120 125
aac ggg atg gat cc 398
Asn Gly Met Asp
130
29
132
PRT
Papilloma virus
29
Gly Ser Leu Glu Asp Gly Glu Met Ile Asp Thr Gly Tyr Gly Ala Met
1 5 10 15
Asp Phe Arg Thr Leu Gln Glu Thr Lys Ser Glu Val Pro Leu Asp Ile
20 25 30
Cys Gln Ser Val Cys Lys Tyr Pro Asp Tyr Leu Gln Met Ser Ala Asp
35 40 45
Val Tyr Gly Asp Ser Met Phe Phe Cys Leu Arg Lys Glu Gln Leu Phe
50 55 60
Ala Arg His Phe Trp Asn Arg Gly Gly Met Val Gly Asp Thr Ile Pro
65 70 75 80
Ser Glu Leu Tyr Ile Lys Gly Thr Asp Ile Arg Glu Arg Pro Gly Thr
85 90 95
His Val Tyr Ser Pro Ser Pro Ser Gly Ser Met Val Ser Ser Asp Ser
100 105 110
Gln Leu Phe Asn Lys Pro Tyr Trp Leu His Lys Ala Gln Gly His Asn
115 120 125
Asn Gly Met Asp
130
30
398
DNA
Papilloma virus
30
ggatccatcc cgttattgtg gccttgggcc ttatgcaacc aatagggctt attaaacaac 60
tgggaatcag aagagaccat agagccactt ggggaagggg aatatacatg agtaccagga 120
cgctcacgta tatccgtgcc tttaatatat aactctgaag gtattgtgtc gcccaccatg 180
ccacctctat tccaaaagtg cctggcaaac aactgttcct tgcgcaaaca aaaaaacata 240
ctgtccccat atacatcagc agacatctgc aaataatcag gatatttaca cacggattgg 300
caaatatcta gtggtacctc acttttggtt tcctgcaatg tacgaaagtc catggcacca 360
tagcctgtat ctatcatttc cccatcctca agggatcc 398
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This invention relates to a DNA coding for a peptide of a papilloma virus major capsid protein. Moreover, this invention deals with a papilloma virus genome containing such a DNA. Furthermore, this invention concerns proteins coded by the papilloma virus genome and virus-like particles as well as antibodies directed thereagainst and the use thereof for diagnosis, treatment and vaccination.
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FIELD OF THE INVENTION
The invention relates to a lubrication system for a gearbox and a wind turbine.
BACKGROUND OF THE INVENTION
The invention concerns a system for supplying lubrication oil to the planet bearings in a gearbox, particularly a wind turbine gearbox.
There is a category of epicyclic gearboxes where the bearing is supported flexibly relative to the planet carrier, for in general improving load sharing between the planet gears, and load distribution across the width of the individual planet gear.
Examples are described in e.g. patent documents nos. WO 03/014566 (Hansen), U.S. Pat. No. 6,994,651 (Timken) and DE 10 2004 023151 (Jahnel-Kestermann).
Positive feed of oil to the planet bearings is in general a known technology for planetary gearboxes, and has for years been standard in e.g. automotive applications. Particularly for wind turbine gearboxes, a couple of specific solutions have been published e.g. in patent documents nos. WO 03/078870 (Hansen) or EP 1 431 575 (Winergy).
Particularly for such flexibly supported planet bearings, the known lubrication solutions have a shortcoming to bring the oil forward to the bearing. On the one hand, the oil system needs to be flexible enough to follow the motion of the planet shaft, and on the other hand the oil system must under no circumstances prevent the free translational motion of the planet shaft in the bearing.
It is an object of the present invention to provide a lubrication system without the abovementioned problem.
THE INVENTION
The invention relates to a lubrication system for a gearbox with stationary and rotating gearbox parts particularly in a wind turbine, the system comprising
lubrication distribution means in the stationary and rotating gearbox parts such as lubrication bores and openings, and
one or more rotary transmissions establishing a transmission channel between lubrication distribution means in the stationary and rotating gearbox parts
where the one or more rotary transmissions include at least two connecting means.
Hereby is established a lubrication system which allows more flexibility and displacement in a gearbox without interrupting the lubrication flow. Further, a flexible connection from rotary transmission to the individual lubrication points on the rotating gearbox parts is established, allowing translation of the lube point relative to the rotation structure in all directions.
In an aspect of the present invention, the at least two connecting means comprises two annulus and flexible U-profiles and the rotary transmission comprises two sets of lip means. Hereby is established a rotary transmission which tolerates axial offsets between the mounting surfaces, e.g. by the inner lip changing its position versus the outer lip.
In an aspect of the invention, the at least two connecting means comprise sets of lip means. This is advantageous in that lip means is a simple, efficient and inexpensive way of sealing a joint between rotating connecting means and a stationary connecting means.
In an aspect of the present invention, one of the at least two connecting means stretches into the other in order to establish a flexible transmission e.g. the initial sets of lip means in the lubricant flow direction being the inner lip means which are forced against the latter and outer set of lips.
Making the lip means overlap by stretching into each other is advantageous, in that pressure from the flowing lubricant will force the lip means together in the overlap zone, thereby further sealing the rotary transmission.
In an aspect of the present invention, one or both lip means comprises a tapering shape toward the contact area of the lip means. Hereby it is possible to establish a response of the rotary transmission in a given situation e.g. designing a self-protecting against excessive lubrication pressure in the rotary transmission by bending the outer lips outward at or above a defined value.
In an aspect of the present invention, at least one of the lip means are made from an elastic material such as plastic or rubber e.g. PTFE coated, a soft material such as brass or bronze, a compound such as rubber lips on a sheet metal carrier e.g. vulcanised. By the choice in materials, the lip means are advantageously less prone to wear. The carrier material may hold certain spring properties e.g. with the same effect as the tapered shape.
In an aspect of the present invention, the lubrication system includes a lubrication flow path comprising a bore in an annulus gear, a bore in the housing and/or a bore in a component attached to the housing as a stationary gearbox part and a bore in a planet carrier as a rotating gearbox part, a rotary transmission, a flexible external connection or an internal channel to distribution bores in or in proximity of a planet shaft. Hereby, the rotary transmission is located closest to the bearing which connects the rotating and the stationary system, meaning that the relative displacement between the parts is less than elsewhere, which makes the transmission easier, more reliable, and less prone to wear.
It should be noted that in this context, the term shaft is to be considered equivalent with any kind of axle, pin or other devices suited for serving as a more or less fixed mounting for a rotating part.
In an aspect of the present invention, the lubrication system includes at least two lubrication flow paths comprising at least one bore in an annulus gear, at least one bore in the housing and/or at least one bore in a component attached to the housing as a stationary gearbox part and at least one bore in a planet carrier as a rotating gearbox part, at least two rotary transmissions, at least one flexible external connection or at least one internal channel to distribution bores in or in proximity of a planet shaft.
Independent and redundant distribution systems for lubrication may hereby be established. Further, the lubrication system may have two channels for heavy load situations or emergency situations such as a blockage in one channel.
In an aspect of the present invention, a rotation connection comprising a pipe and a bushing between a flexible external connection and a planet shaft is established, hence allowing the planet shaft rotational freedom without influencing the lubrication path.
In an aspect of the present invention, the flexible external connection is a hose allowing for translational movements in the gearbox.
A hose is a simple and inexpensive way of establishing a flexible fluid connection between parts moving slightly in relation to each other in a wind turbine gearbox.
In an aspect of the present invention, the one or more rotary transmissions is positioned in an axial direction, in a radial direction or in both an axial direction and in a radial direction.
Placing the rotary transmissions in an axial direction, a radial direction or both is advantageous in that hereby the parts can be made less complex and in that this enables a more simple assembly procedure, thereby reducing the cost.
In an aspect of the present invention, the one or more rotary transmissions are positioned in an area between stationary and rotating gearbox parts in order to establish a transmission channel between lubrication distribution means in the stationary and rotating gearbox parts by the at least two connecting means extending out from the stationary and rotating gearbox parts.
Placing the rotary transmission in the area between a stationary and a rotating gearbox part is advantageous because it is thereby avoided to integrate the transmission in one or both of the parts and thereby costs are reduced.
The invention also relates to a wind turbine comprising a drive train including a gearbox, and a lubrication system as described above for the gearbox.
Wind turbine gearboxes are different from most other types of gearboxes by the fact that they have to be able to cope with much more flexure and deflection of both the nacelle structure in which the gearbox is mounted and in the gearbox strengthening structure itself. This is due to the massive size of modern wind turbines combined with the demand of low weight, low cost and high output. It is therefore particularly advantageous to use a lubrication system according to the present invention for transferring lubricant between mutually rotating parts of a wind turbine gearbox.
In an aspect of the present invention, the gearbox is an epicyclic gearbox such as a planetary, star or solar gearbox or any kind of compound gearbox and/or gearboxes with one or more bearing rows.
Epicyclic gearboxes are relatively low weight, low cost and small in relation to the load they are able to transfer but due to the generic design of the epicyclic gearboxes this gearbox type is more prone to flexure and deflections and it is therefore advantageous to use a lubrication system according to the present in a epicyclic gearbox.
FIGURES
The invention will be described in the following with reference to the figures in which
FIG. 1 illustrates a large modern wind turbine,
FIG. 2 illustrates a first embodiment of a gearbox and lubrication system according to the invention,
FIG. 3 illustrates a further embodiment of a gearbox and lubrication system according to the invention,
FIGS. 4 a to 4 d illustrate embodiments of a rotary transmission in the lubrication system according to the invention,
FIG. 5 illustrates an embodiment of the lubrication system according to the invention with a lubrication bore in the planet carrier,
FIG. 6 illustrates an embodiment of the lubrication system according to the invention with two rotary transmissions,
FIG. 7 illustrates an embodiment of a vertical or radial rotary transmission in the lubrication system according to the invention, and
FIG. 8 illustrates an example of a rotation connection between a flexible external connection and a planet shaft.
DETAILED DESCRIPTION
FIG. 1 illustrates a modern wind turbine 1 mounted on a foundation 8 . The wind turbine comprises a tower 2 , including a number of tower sections such as tower rings, and a wind turbine nacelle 3 positioned on top of the tower 2 . The wind turbine rotor 6 , comprising three wind turbine blades 5 , is connected to the hub 4 through pitch mechanisms 7 . Each pitch mechanism 7 includes a blade bearing which allows the blade 5 to pitch in relation to the wind. The hub 4 is connected to the nacelle 3 through a shaft which extends out of the nacelle front. The shaft is connected through a gearbox mechanism to an electric generator wherein the connection may comprise one or more shaft bearings such as rotor and generator bearings.
FIGS. 2 and 3 illustrate a first and further embodiment of gearbox 9 and a lubrication system according to the invention. The gearbox 9 is preferably a planetary gearbox in a wind turbine 1 .
The lubrication oil is supplied to the planet bearing 20 through the planet shaft 22 .
This requires (a) to transfer oil from a stationary frame 23 to the rotating system 11 , and (b) to conduct oil further on to the flexibly supported planet shafts 22 .
(a) For transferring oil from the stationary to the rotating system, a bore 14 is arranged in an axial direction through the annulus gear 10 . This bore is supplied with oil from the stationary housing 23 . A rotating transmission 15 feeds the oil from this bore 14 through the stationary annulus gear 10 towards the rotating planet carrier 11 . This position comes closest to the bearing 28 which connect the rotating and the stationary system, meaning that the relative displacement between the parts is less than elsewhere, which makes the transmission easier, more reliable, and less prone to wear.
It shall be emphasised that the transfer of lubrication oil may also be from a part of the housing 23 or any component mounted in a stationary manner to the housing 23 to the rotating system i.e. without using a path through the annulus gear 10 .
(b) Once transferred in the rotating system, the oil can either be conducted through channels (an embodiment illustrated in FIG. 5 ) in the rotating planet carrier 11 to the planet shafts 22 , or by a flexible external connection 17 from the planet carrier 11 to the planet shaft 22 . This flexible connection 17 may for example be a simple hose 17 , which would be able to follow the planet shaft 22 without constraining displacements.
Wobbling is a local axial and/or radial uneven movement in the gearbox system and the flexibility of the lubrication system according to the invention is especially relevant in relation to:
1. Rotation of one gearbox part e.g. the planet carrier 11
2. Translation e.g. the flexible planet shaft 22
3. Rotation of the planet shaft 22 vs. the planet carrier 11
4. Axial movement
5. Radial movement
FIGS. 4 a and 4 b illustrate a preferred embodiment of a rotary transmission 15 in the lubrication system according to the invention.
The rotary transmission 15 may be arranged by two flexible U-profiles 24 a , 24 b engaging with each other and especially over an overlap distance L. The oil pressure injected through the bore 14 will cause the lips of the inner profile 24 a to inflate, until they contact the outer profile 24 b . At the same time, the flexibility of the outer profile 24 b will allow the two lips to follow each other in case of radial offsets between their mounting surfaces. The system can also tolerate axial offsets between the mounting surfaces, just by the inner lip 24 a changing its position versus the outer lip 24 b (i.e. a change in the distance L).
Wear in the contact between the lips 24 a and 24 b can be controlled by proper choice of materials (or surface treatment e.g. by coating with PTFE or alike), and is further reduced by the fact that this contact is always submerged in oil.
Depending on the surface area of the outer lip 24 b which is exposed to the oil pressure, and the elasticity of this lip, the system may be designed to be self-protecting against excessive pressure. Too high pressure may cause the outer lip 24 b to bend outwards, until some oil can escape, and the pressure is released until equilibrium is achieved. This functionality may be used to control the flow to the bearing 20 as a function of oil viscosity, which again is a function of oil temperature.
There is no preference whether the inner lip 24 a is mounted on the stationary or the rotary part, the system can work both ways.
FIG. 4 b illustrates inner and outer lip means 24 a , 24 b of the rotary transmission 15 in an enlarged view. The outer lips are shown with a tapering shape toward the contact area of the lips and the inner lips with a uniform shape, but any type of relevant shape may be used for the lips.
FIG. 4 c illustrates an embodiment of the inner and outer lips 24 a , 24 b of the rotary transmission 15 in a further enlarged view and with a different profiling of the lips by introducing a number of outward elevations in the inner lips 24 a and/or a number of inward elevations in the outer lips 24 b.
FIG. 4 d illustrates a further embodiment of inner lips 24 a with a compound solution. As illustrated, a sheet metal carrier in the lips is applied with a rubber coating e.g. in a vulcanising process in order to establish a flexible lip means. It shall be emphasised that the solution may be used in the inner as well as the outer lips 24 a , 24 b.
FIG. 5 illustrates an embodiment of the lubrication system according to the invention wherein the bore 16 in the planet carrier is continued to a position in proximity of the planet bearing 20 . A hose 17 connects the bore 16 with a bore 18 in a bearing support or raceway 29 . The hose 17 may be replaced by different bores in the planets 21 or moved to the other side of the planets 21 by bores through the planets 21 .
FIG. 6 illustrates an embodiment of the lubrication system according to the invention with two rotary transmissions 15 a , 15 b . Each of the two rotary transmissions 15 a , 15 b is connected to separate bores 14 a , 16 a ; 14 b , 16 b in the stationary annulus gear 10 and/or planet carrier 11 , respectively. The two bores 16 a , 16 b in the planet carrier 11 are connected to a common hose 17 .
A lubrication system including two rotary transmissions 15 a , 15 b (or more) may be used as independent and redundant distribution systems for lubrication e.g. if a lubrication component fails in one system the other system may continue the lubrication.
Further, the lubrication system may have two channels including two rotary transmissions 15 a , 15 b (or more) but no further redundancy e.g. one channel for normal lubrication situations and one more for heavy load situations or emergency situations such as a blockage in the normal situation channel.
The figure illustrates the lubrication system as positioned inside a main bearing 28 in relation to the centre line CL of the gearbox 9 . However, it shall be emphasised that the lubrication system may also be positioned on the outside of the main bearing 28 .
FIG. 7 illustrates an embodiment of a vertically or radially aligned rotary transmission 15 in the lubrication system with the lip means 24 a , 24 b facing up and down, respectively in order to establish an overlap distance L.
FIG. 8 illustrates an example of a rotation connection 27 between a flexible external connection 17 and a planet shaft 22 .
For a gearbox design where the planet shaft 22 has the freedom to constantly or occasionally rotate relative to the planet carrier 11 , for example in compound epicyclic arrangements, a rotation connection 27 from the flexible hose 17 to the planet shaft 22 may be required.
One simple execution of this transmission could be a bushing 26 from a soft material with low friction (such as PTFE or bronze) fitted into the planet shaft 22 . The hose 17 could then be connected to one end of a pipe 25 which is non-rotatably but else free linked to the planet carrier 11 , whilst the other end of the pipe 25 protrudes into the planet shaft 22 through the bushing 26 . It is not required that the seat between bushing 26 and pipe 25 is oil tight. The gap must only be tight enough to create a flow resistance that is larger than the passage through the planet bearing 20 .
The illustrated outer bearing 20 should be understood as a symbolic indication of the planets 21 further rotation inside the gearbox.
The solution is particularly relevant for bearings 20 with more bearing rows, where the oil is distributed through channels in the inner ring, or between the bearings.
The invention described has been exemplified above with reference to specific examples of epicyclic gearboxes 9 e.g. planetary gearboxes with a stationary annulus gear 10 . However, it should be understood that the invention is not limited to the particular examples but may be designed and altered in a multitude of varieties within the scope of the invention as specified in the claims e.g. epicyclic gearboxes 9 with stationary sun 12 or planet gear 21 (solar or star gearboxes).
Further, the epicyclic gear 9 may comprise more than one stage wherein different connection parts between the stages may comprise bores 14 , 16 , 18 or flexible connections 17 such as hoses in order to establish the necessary distribution channels in the lubrication system.
Reference list
In the drawings the following reference numbers refer to:
1.
Wind turbine
2.
Wind turbine tower
3.
Wind turbine nacelle
4.
Wind turbine hub
5.
Wind turbine blade
6.
Wind turbine rotor with at least one blade
7.
Blade pitch mechanism
8.
Wind turbine foundation
9.
Gearbox such as planetary gearbox
10.
Annulus gear or ring gear
11.
Planet carrier
12.
Sun gear
13.
Output shaft or high speed shaft
14.
Bore in the annulus gear
15.
Rotary transmission
16.
Bore in the planet carrier
17.
Flexible external connection e.g. a hose
18.
Bore in the planet shaft
19.
Opening in the planet carrier for e.g. a hose
20.
Planet bearings
21.
Planet gear
22.
Planet shaft
23.
Stationary housing of the gearbox
24a, 24b.
Sets of lips in the rotary transmission
25.
Pipe
26.
Bushing
27.
Rotation connection between flexible
external connection and planet shaft
28.
Bearing e.g. a main bearing
29.
Bearing support or raceway
L.
Overlap distance
CL.
Centre line of gearbox
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The invention relates to a lubrication system for a gearbox with stationary and rotating gearbox parts particularly in a wind turbine. The system includes lubrication distribution means in the stationary and rotating gearbox parts such as lubrication bores and openings. One or more rotary transmissions establish a transmission channel between lubrication distribution means in said stationary and rotating gearbox parts where said one or more rotary transmission include at least two connecting means. The invention also relates to a wind turbine with a drive train including a gearbox, and a lubrication system.
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PRIORITY
[0001] This application claims the benefit of U.S. Provisional Application No. 60/372,816 filed on Apr. 17, 2002.
FIELD OF THE INVENTION
[0002] The present invention relates generally to generating displays. More particularly, the present invention relates to generating displays for vending machines.
BACKGROUND OF THE INVENTION
[0003] Creating displays is a time intensive endeavor, which requires a large amount of programming. In creating displays, such as displays for vending machines, a display layout can be created to show what each screen should look like, how the screens should function and how the screens should link to one another. For example, when creating a display for a ticket vending machine, it may become necessary to determine what types of screens are needed for the purchase and distribution of a fare ticket. Within each screen different actions must be taken. For example, if a user wanted to purchase a metro ticket for a subway a first screen may include an area to select what type of ticket must be purchased. There may be three options, a monthly pass, a weekly pass, or a daily pass and a button associated with each of these options. Once one of these buttons is depressed, another screen may be displayed, such as payment type. For example, if a user chose to purchase a monthly pass and depressed the button associated with the monthly pass, a new screen would be displayed. This new display would request that the user choose a payment type. For example, the payment type may be credit card, debit card or cash. A button could be associate with each of these payment types. If the user chose credit card by depressing the button next to the credit card payment display, the display may prompt the user to insert a credit card into the appropriate slot. Once the credit card was inserted into the appropriate slot, another display may be shown, showing that transaction was complete and requesting the user to obtain the monthly pass from a storage bin below in the ticket vending machine.
[0004] From the above example, it is evident that there are many different displays and combinations of displays based on user inputs. In order to create these screens it would require someone to go through each of these situations to determine which display should be chosen or activated after each action item. Once a designer has determined all of the different displays and actions that they would want this ticket vending machine to accomplish, this would have to be communicated to a computer programmer. The computer programmer would then analyze these displays and action items to create a program to accomplish the goals of the display designer. As in any designing system involving more than one person, this may require many revisions and communications between the designer and the programmer in order to get the display to look exactly as the designer had anticipated and wished. Accordingly, a display creating interface for a vending machine is needed that will allow the display designer to create displays and action items without the use of a computer programmer.
[0005] In addition, it would be desirable to have an interface that would allow the user to see what the display would look like as the designer is creating the display.
[0006] It would further be desirable to have a system in which program codes such as C++ code are generated from this template and could become compiled and downloaded onto a vending machine.
SUMMARY OF THE INVENTION
[0007] It is therefore a feature and advantage of the present invention to provide a display creating interface that will allow a designer to create display and action items without the use of a computer programmer. It is another feature and advantage of the present invention to provide a display creating interface which will create programming code from the templates which can be turned into an executable and downloaded onto the vending machine without the use of a computer programmer.
[0008] The above and other features and advantages are achieved through the use of a novel display creating interface for a vending machine as herein disclosed. In accordance with one embodiment of the invention, a display creating interface for a vending machine includes a template generator that defines a template of a display having active areas and description areas associated with active areas. An active area generator is provided in communication with the template generator to define actions to be associated with the active areas. A program generator is provided in communication with the template generator and the active area generator to generate programming code defining the template.
[0009] In accordance with another embodiment of the invention, a method for creating a display for a vending machine includes the steps of creating a display for a vending using a template having active areas and description areas associated with the active areas. Functions are created which are associated with the active areas. Programming code is then generated from the template.
[0010] In accordance with another embodiment of the present invention, a system for creating a display for a vending machine includes a means for creating a display for a vending machine using a template having active areas and description areas associated with the active areas. A means is provided for creating functions to be associated with the active areas. Another means is provided for generating programming code from the template.
[0011] There has thus been outlined, rather broadly, the more important features of the invention in order that the detailed description thereof that follows may be better understood, and in order that the contribution to the art may be better appreciated. There are, of course, additional features of the invention that will be described below and which will form the subject matter of the claims appended hereto.
[0012] In this respect, before explaining at least one embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments and of being practiced and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein, as well as the abstract, are for the purpose of description and should not be regarded as limiting.
[0013] As such, those skilled in the art will appreciate that the conception upon which this disclosure is based may readily be utilized as a basis for the designing of other structures, methods and systems for carrying out the several purposes of the present invention. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] [0014]FIG. 1 is an illustration of a template used to make a display of the present invention.
[0015] [0015]FIG. 2 is a block diagram showing how to create a display of the present invention.
[0016] [0016]FIG. 3 is a flow diagram showing the method steps used in making a display of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0017] The present invention provides a way of creating displays using templates for vending machines. The present invention allows users to configure displays for vending machines, such as ticket vending machines, through the use of a wizard called a screen painting wizard. A user interface is provided so that transaction logic can be defined as a group of activities performed on a ticket vending machine by a user in order to buy goods being vended, supply information or monetary goods to the vending machine for the purpose of buying goods being vended, and collecting information of interest from the user in exchange for goods being vended.
[0018] An example of transaction logic is to buy a stored value from the vending machine after money is inserted into the vending machine. In order to accomplish this, the user will have to go through a series of screens or displays to indicate what type of transaction the user in interested. Money or some kind of credit can be inserted into the machine to purchase a service. Once the money or credit has been inserted into the machine, or otherwise credited, the vending machine can dispense a card or fare card in the case of a ticket vending machine for mass transportation. It is noted that the vending of these services is not only limited to ticket vending machines for mass transit, but could be used in other areas such as vending machines for tickets for movies, and products such as snacks or other services or products.
[0019] A single transaction for these products or services will have numerous screens associated with these transactions. Each screen will show and collect information from the user by using buttons that are depressed, or insertion of money or some type of credit system to the vending machine. The wizard will allow the programmer to design the look and feel of the entire screen or display. Through the use of the wizard, an interface will allow the user to design various messages on the screen, program various buttons on the screen, and design banners and pictures to appear on the screen.
[0020] In some instances, the user interface is split up into 15 cells arranged in a 3 by 5 matrix. There are five buttons on each side of this matrix. Each button aligns with a row. A sticker is a user interface component that contains text banners and pictures. Stickers can be pasted onto a cell or can span multiple cells. Pressing a button next to the sticker will activate the sticker and launch into some type of function or transaction. FIG. 1 is an illustration of the 3×5 matrix having 15 cells, 110 , and buttons 120 . As is illustrated in FIG. 1, not only can buttons 120 be aligned with the rows, but buttons 120 could also be aligned with the columns. There are multiple configuration for aligning or arranging the buttons and cells. FIG. 1 is only an illustration of one possible embodiment of the invention.
[0021] [0021]FIG. 2 is a block diagram showing how a display may be made using a template. In order to design a display using the templates, several design objectives must be laid out. First, the user must decide what the transaction objectives are, what actions will be necessary to achieve these objectives and in what order each action should occur. Along these lines, it must be determined what types of information are needed from the user, whether money should be collected from the user, whether some type of fare card should be collected from the user, what needs to be vended etc. The second design objective is to determine what type of information needs to be remembered during a transaction and posted to a database. The database will keep information such as user and in the case of mass transportation, destinations, times, etc. Another design objective is to determine individual screens that must be shown for each transaction. Once the screens are decided, buttons must be created to execute functions or transactions on each screen. Another objective is to design how to vend or distribute receipts, fare cards, etc., to the user for each transaction.
[0022] Once these design objectives are laid out, the designer can use the wizard to create displays to achieve the design objectives. As shown in box 210 in FIG. 2, variables and data types are created to store information that need to be remembered during a transaction and later posted to a database. As shown in box 220 of FIG. 2, a template of instances for each transaction objective must be created. This may involve breaking down the objectives into further steps. For example, one objective may be to collect money from the user. This step may be broken into two sub steps. First, the mode of payment would have to be decided (i.e., credit/debit/cash/metro card) and the means for actually getting the payment, i.e. create a different template instance based on what is selected as the mode of payment.
[0023] In box 230 of FIG. 2, screens are created. Stickers and banners must be designed for each of the screens where a sticker is placed right next to a button will activate the button. Pressing that button on this screen will then launch into another screen. This can be specified in the sticker. As shown in box 230 , groups are created of the template instances to complete a transaction. The wizard will have language constructs, which will allow the user to create groups. Some constructs allow looping inside a set of templates for a preset number of times. This allows for cases like allowing a user to purchase more than one fare card at a time, or other types of looping functions or transactions.
[0024] A designer can also attach the creative transaction to some sticker and place it on the main screen, so that the end user can start off with this transaction by pressing the button next to the screen. This is useful when there are multiple types of services or products, which are associated with a single vending machine. This will give the user the ability to choose which transaction the user wishes to engage in without going through too many multiple screens.
[0025] The generation of the display through the template using the screen painting wizard is done through box 240 where INI files are generated or any other type of programming code files can be generated. Once the display and screen have been created through the template painting wizard, the wizard can be directed to create a programming code, such as C++ files. In box 250 the INI code is translated into C++ code. In box 260 , the C++ code is compiled into executable code to create an executable file, which can be downloaded and run on a vending machine, such as a ticket vending machine. Once the executable file is created, the executable file can be downloaded into a ticket vending machine user interface (box 270 ). In one embodiment of the invention, these executable files can be moved to a LINUX box where a compile will create all binaries needed for the final TVM. These can then be downloaded into the actual TVM.
[0026] [0026]FIG. 3 shows the method steps that can be used in creating a display using a template through the display wizard interface. In step 310 , the general design of the template for each display is created. In step 320 , stickers and button for the template are created where certain buttons may be associated with other stickers. When the buttons are depressed, certain transactions can be associated with the buttons and can jump to other displays or other transactions or functions.
[0027] In step 330 , other messages or banners can also be created which are not associated with the buttons, such as advertisements or general information. Once all of the displays, stickers and buttons have been created to the designer's preferences, programming code is created in step 340 .
[0028] In step 340 the wizard interface can create C++ files. These files can be moved to a LINUX box where a compile will create all binaries needed for the final TVM. In step 350 the programming code is compiled into an executable code. In step 360 , the executable code is downloaded onto a vending machine.
[0029] The many features and advantages of the invention are apparent from the detailed specification, and thus, it is intended by the appended claims to cover all such features and advantages of the invention which fall within the true spirit and scope of the invention. Further, since numerous modifications and variations will readily to those skilled in the art, it is not desired to limit the invention to the exact construction and operation and illustrated, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention.
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A display creating interface for a vending machine that includes a template generator that defines a template of a display having active areas and description areas associated with the active areas. An active area action generator is provided in communication with the template generator to define actions to be associated with the active areas. A program generator is provided in communication with the template generator and active area generator to generate programming code defining the template.
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FIELD OF THE INVENTION
The invention relates to a method for the preparation of a polymeric shaped article containing an electrically conductive polymer, wherein a base shaped article containing a matrix polymer is contacted with an anode in the presence of an electrolyte-containing medium containing monomer units, which on polymerisation form an electrically conductive polymer, and wherein a voltage is applied between the anode and a second electrode which is in contact with the electrolyte-containing medium.
BACKGROUND OF THE INVENTION
A similar method is described by O. Niwa et al. in Makromol. Chem., Rapid Commun. 6, No. 6, 1985, pp. 375-379. According to the method described therein, an insulating polymeric base film has been applied to an anode, which is placed in an electrolyte solution also containing pyrrole. As a result of an applied voltage, the pyrrole monomers diffuse from the electrolyte solution to the base film, where they polymerise to form polypyrrole. In this way, a film with electrically conductive properties is obtained. The pyrrole monomers polymerise both on and within the base film.
The method described by O. Niwa et al. is suitable for the preparation of a polymeric shaped article with electrically conducting properties. The method of Niwa has the disadvantage of being uneconomically low in productivity. Firstly, only a relatively small piece of base film, essentially having the same size as the anode, can be applied at a time. Further, the application of the base film onto the anode is time-consuming since a very intimate contact over the whole of the surface is required. Then the process of making the film conductive is dominated by the intrinsically slow diffusion of the pyrrole through the film and finally the conductive film has to be peeled off from the anode on the risk of damaging the film, that tends to stick to the anode.
A further disadvantage is that the base shaped article applied by Niwa swells in the electrolyte solution, so causing the mechanical properties of the base shaped article to deteriorate and making the film stick to the anode. Another added disadvantage of the base shaped article applied by Niwa is that a high voltage needs to be applied in order to realise a short polymerisation time or a high rate of production.
SUMMARY AND OBJECTS OF THE PRESENT INVENTION
The present invention aims to provide a method that does not have the disadvantages set out above. The method according to the invention is characterised in that the applied base shaped article possesses electrically conducting properties and that the contact between the shaped article and the anode is established by moving the article along the anode, at least part of the article being in contact with the anode.
The method according to the invention allows a highly conductive film to be obtained at a high production rate in a continuous process. Contacting times of only minutes have appeared to be sufficient for obtaining a highly conductive article. No sticking of the film to the electrode occurs, thus waste being avoided.
A further advantage of the shaped article failing to adhere to the electrode is that the method generates very little waste. Furthermore, it has appeared that the method according to the invention allows a shaped article to be produced with a very short polymerisation time, wherein the electrically conductive polymer is homogeneously distributed. The applied base shaped article does not swell during wetting, so that the mechanical properties of the base shaped article do not deteriorate. As a result, if the method is applied, for instance, continuously, a higher production rate can be applied.
From according to EPO 234,467 it is known to apply electrochemically an electrically conductive polymer to a base film already possessing conductive properties, but just as in the Niwa reference a batch process is used. The problem to be solved in the EPO 234,467 lies in the thickness of the base film. Any increase in productivity is not achieved and contacting times of hours are still required.
The shaped article so obtained is highly suited for EMI shielding. Examples of objects that need EMI shielding are computers and telephones.
BRIEF DESCRIPTION OF THE FIGURE
FIG. 1 schematically represents a device for practicing the method according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The polymeric base shaped article applied in the method according to the invention possesses electrically conducting properties. The electrically conducting properties are obtained, for instance, by incorporating an electrically conductive polymer in the polymeric base shaped article. The polymeric base shaped article contains a matrix polymer also. Depending on the requirements for the polymeric base shaped article in terms of, for instance, the mechanical properties, any polymer may in principle be selected. Thermoplastic polymers are eminently suitable as matrix polymer because of their processability. Suitable thermoplastic polymers are, for instance, polyvinyl chloride or copolymers of vinyl chloride and other vinyl monomers, polyvinylidene fluoride or copolymers of vinylidene fluoride and other vinyl monomers, polystyrene or copolymers of styrene and other monomers for instance maleic anydride and maleimide, polyacrylates or copolymers of an acrylate with other monomers, polyvinyl carbazole, polyolefins such as polyethylene, ultra-high weight polyethylene (UHMWPWE) and and polypropylene, polyvinyl acetate, polyvinyl alcohol, polyesters for instance polyethylene terephthalate and polybutylene terephthalate, polycarbonates, polyetherimides, polyimides, polyamides, polyamide imides, polyethylene oxide, polybutadiene rubbers, polytetrafluoroethylene and the like. If desired, a mixture of several polymers may be used as thermoplastic polymer. Ultra-high molecular weight polyethylene is preferably used as matrix polymer because of its good mechanical properties.
The applied polymeric base shaped article possesses electrically conducting properties. The specific conductivity of the applied polymeric base shaped article is preferably greater than 0.001 S/cm. More preferably, the specific conductivity is greater than 0.1 S/cm. For the purposes of the present invention a shaped article is understood to be, for instance, a film, a fibre, a board or other object. The thickness of the applied polymeric base shaped article usually lies between 5 μm and 1 mm but preferably between 10 μm and 300 μm. The applied polymeric base shaped article is preferably porous, at least a proportion of the pores preferably being accessible from the outside surface of the shaped article. The volume porosity of the applied base shaped article is usually greater than 30%, more preferably greater than 50% and even more preferably greater than 65%. Porous films containing a thermoplastic matrix polymer are described in EP-A-105629, EP-A-309136, EP-A-288021 and WO-A-86/02282. Films containing a polyolefin as matrix polymer are described in, for instance, EP-A-193318. Films containing an ultra-high molecular weight polyethylene as matrix polymer are described in, for instance, EP-A-378279 and EP-A-163424.
These films as such do not possess electrically conductive properties. They can be made electrically conductive for instance by impregnating them with a solution of a monomer, polymerisable to a conductive polymer and contacting the impregnated film with a catalyst to form a conductive polymer inside the film. Also the mirror process is feasible, wherein the film is impregnated with a solution of a catalyst and subsequently exposed to for instance a vapour of a monomer, polymerisable to a conductive polymer. A preferred method is to impregnate the film with a solution containing of a precursor monomer and a catalyst together and activating the precursor monomer to have a conductive polymer formed in situ. A precursor monomer is to be understood to be a monomer blocked with a substituting group on a position taking part in the polymerisation, the substituting group being easily removable to obtain the corresponding reactable monomer.
The electrically conductive polymer in the polymeric base shaped article is made up of monomer units chosen from, for instance, the group formed by pyrrole, thiophene, indole, carbazole, furan, aniline, isothianaphthene, acetylene and derivatives of these monomers. Given the level and stability of the electrically conducting properties, an electrically conductive polymer is to be preferred that is made up of pyrrole units, thiophene units and/or aniline units. If desired, the electrically conductive polymer is made up of a mixture of several of the above-mentioned monomer units.
The electrolyte-containing medium usually contains a solvent. The solvent is often selected from the group formed by water, aromatic compounds for instance benzene, toluene and xylene, alcohols for instance methanol and ethanol, hydrocarbons for instance pentane and hexane, ethers for instance dioxane, diethyl ether, ethyl-methyl ether and tetrahydrofuran, ketones for instance acetone, diethyl ketone and methyl-ethyl ketone, halogenated compounds for instance CHCl 3 , CH 2 Cl 2 , CH 3 Cl and carbon tetrachloride, esters such as ethyl formiate and ethyl acetate, and compounds for instance acetonitrile, nitromethane, dimethyl sulfoxide, dimethyl formamide, triethyl phosphate, dimethyl acetamide and pyridine. A mixture of several solvents may be used also. Preferably, an aprotic, non-nucleophilic solvent is applied.
Common and known ionic or ionizable compounds may be used as electrolyte. Suitable electrolytes contain, for instance, anions of strong, oxidizing acids, or aromatics with acid groups which, if desired, may be substituted with alkyl groups and/or nitro groups. Highly suitable electrolytes contain as cations an alkali metal cation such as Li + , Na + or K + , an NO + or NO 2 + cation or an --onium cation of, for instance, nitrogen such as R 4 N + or of phosphorus, such as R 4 P + . The R groups in the --onium cations are selected independently of each other from the group formed by hydrogen, alkyl groups with 1-6 carbon atoms, cycloaliphatic groups with 6-14 carbon atoms and aromatic groups with 6-14 carbon atoms. Examples of such --onium cations are tetramethyl ammonium cations, tetraethyl ammonium cations, tri-n-butyl ammonium cations, tetra-n-butyl ammonium cations, triphenyl phosphonium cations and tri-n-butyl phosphonium cations. Highly suitable electrolytes contain as anion for instance BF 4 --, AsF 4 --, AsF 6 --, SbF 6 --, SbCl 6 --, PF 6 --, ClO 4 --, HSO 4 -- or SO 4 2 -- groups. In addition, anions of aromatic compounds with acid groups are especially suitable to be used. Examples of such anions are the C 6 H 5 COO-- group and anions of sulphonic acid groups, which, if desired, are substituted with alkyl groups such as the benzene sulphonate anion and the tosylate anion. As well as anions of aromatic compounds with acid groups, anions of aromatic compounds with nitro groups are especially suitable to be used. Examples of such electrolytes are salts of nitrophenol, of aromatic carboxylic acids substituted with nitro-groups, and of aromatic sulphonic acids substituted with nitro-groups. The electrolyte concentration in the medium usually lies between 0.001 and 1 mole per liter but preferably between 0.01 and 0.1 mole per liter.
The electrolyte-containing medium also contains monomer units. These monomer units are chosen from, for instance, the group formed by pyrrole, thiophene, indole, carbazole, furan, aniline, isothianaphthene, acetylene and derivatives of these monomers. The electrolyte-containing medium may optionally contain a mixture of several of the above-mentioned monomer units. Examples of derivatives of these monomers are N-methyl pyrrole, N-ethyl pyrrole, N-propyl pyrrole, N-n-butyl pyrrole, N-phenyl pyrrole, N-tolyl pyrrole, N-naphthyl pyrrole, 3-methyl pyrrole, 3,4-dimethyl pyrrole, 3-ethyl pyrrole, 3-n-propyl pyrrole, 3-n-butyl pyrrole, 3-phenyl pyrrole, 3-tolyl pyrrole, 3-naphthyl pyrrole, 3-methoxypyrrole, 3,4-dimethoxypyrrole, 3-ethoxypyrrole, 3-n-propoxypyrrole, 3-phenoxypyrrole, 3-methyl-N-methyl pyrrole, 3-methoxy-N-methyl pyrrole, 3-chloropyrrole, 3-bromopyrrole, 3-methyl thiopyrrole, 3-methylthio-N-methyl pyrrole, 2,2'-bithiophene, 3-methyl-2,2'-bithiophene, 3,3'dimethyl-2,2'-bithiophene, 3,4-dimethyl-2,2'-bithiophene, 3,4-dimethyl-3',4'-dimethyl-2,2'-bithiophene, 3-methoxy-2,2'-bithiophene, 3,3'-dimethoxy-2,2'-bithiophene, 2,2'5,2"-terthiophene, 3-3,3-dimethyl-2,2',5'2"-terthiophene, 2-cyclohexyl aniline, aniline, 4-propanoyl aniline, 2-(methyl-amino)aniline, 2-(dimethyl amine)aniline, o-toluidine, 4-carboxyaniline, N-methyl aniline, m-hexyl aniline, 2-methyl-4-methoxy carbonyl aniline, N-propyl aniline, N-hexyl aniline, m-toluidine, o-ethyl aniline, m-ethyl aniline, o-ethoxy aniline, m-butyl aniline, 5-chloro-2-ethoxy aniline, m-octyl aniline, 4-bromoaniline, 2-bromoaniline, 3-bromoaniline, 3-acetamidoaniline, 4-acetamidoaniline, 5-chloro-2-methoxyaniline, 2-acetyl aniline, 2,5-dimethyl aniline, 2,3-dimethyl aniline, 4-benzyl aniline, 4-amino aniline, 2-methyl thiomethyl aniline, 4-(2,4-dimethyl phenyl)aniline, 2-ethyl thioaniline, n-methyl-2,4-dimethyl aniline, n-propyl-m-toluidine, n-methyl-o-cyanoaniline, 2,5-dibutyl aniline, 2,5-dimethoxyaniline, o-cyanoaniline, tetrahydronaphthyl amine, 3-(n-butyl sulphonic acid)aniline, 2-thiomethyl aniline, 2,5-dichloroaniline, 2,4-dimethoxyaniline, 3-propoxymethylaniline, 4-mercaptoaniline, 4-methyl thioaniline, 3-phenoxy aniline, 4-phenoxy aniline, n-hexyl-m-toluidine, 4-phenyl thioaniline, n-octyl-m-toluidine and 4-trimethylsilyl aniline. The concentration of the monomer units in the electrolyte-containing medium usually lies between 0.01 and 1 mole per liter but preferably between 0.1 and 0.3 mole per liter. The temperature of the electrolyte-containing medium usually lies between 0° and 100° C. but preferably between 10° and 40° C.
The electrodes employed in the method according to the invention are selected from the commonly used electrodes. Such electrodes contain, for instance, platinum, gold, silver, palladium, titanium, chromium-nickel or stainless steel. Indium-tin oxide-coated electrodes may be employed also. Preferably, use is made of platinum electrodes.
Electrochemical set-ups in which the method according to the invention may be applied are described in, for instance, EPO 142,089 and EPO 99,055. In the method according to the invention, one of the electrodes referred to above functions as an anode. The polymeric base shaped article possessing electrically conducting properties is brought into contact with the anode. To this end, the base shaped article may be sliding along the anode or fixed to the anode. Preferably, a method is used whereby a very long base shaped article is continuously slided along the anode. The continuous method makes it possible to produce a shaped article whose electrically conducting properties are homogeneously distributed over the shaped article. It is especially advantageous to pass the base shaped article along the anode so that there is hardly any electrolyte-containing medium between the anode and the shaped article. The contact time, during which the base shaped article is contacted with the electrolyte-containing medium, usually lies between 0.1 and 20 minutes. The contact time preferably lies between 0.1 and 5 minutes. If desired, the method according to the invention is repeated several times. In a special embodiment a base shaped article is slided along a first, cylindrical electrode, in which process one side is contacted with the electrolyte-containing medium, and subsequently along a second, cylindrical electrode, in which process the other side is contacted with the electrolyte-containing medium. In the method according to the invention, the current density between the anode and the other electrode, the cathode, is usually 5-20 mA/cm 2 .
The shaped article produced by the method according to the invention usually contains 5-95 percent by weight electrically conductive polymer, calculated relative to the total weight of matrix polymer and electrically conductive polymer. Preferably, this is 25-85 percent by weight. The specific conductivity of the produced shaped article usually is greater than 10 S/cm, preferably greater than 50 S/cm. The electrically conducting properties of the shaped article produced by the method according to the invention are measured. To this end, the specific conductivity, for instance, is measured by the so-called four-point method. This method is briefly described in EPO 314,311. A more detailed description is to be found in H. H. Wider, Laboratory Notes on Electrical and Galvanomagnetic Measurements, Elsevier, New York, 1979. The specific conductivity is measured by this method:
σ=(L/A)*(1/R),
where
σ=specific conductivity [S/cm]
L=distance between the two inner electrodes [cm]
R=resistance [ohm]
A=cross-sectional cross-sectional area
The base shaped article applied in the method according to the invention may optionally contain up to 60 percent by volume fillers and/or antioxidants. Examples of fillers that may be added are talc, fibres, pigments, kaolin, wollastonite and glass.
If desired, low-molecular components and impurities, if any, may be removed from the shaped article obtained by the method according to the invention by extraction and/or evaporation. These methods are commonly known.
The invention is elucidated by the following examples without being limited thereto.
EXAMPLES AND COMPARATIVE EXPERIMENTS
EXAMPLE I
A porous UHMW-PE film (length 40 meters; width 8.5 cm; thickness 35 μm; volume porosity 83%) was impregnated with a solution of 4 grams pyrrole-2-carboxylic acid and 11.2 grams FeCl 3 in a mixture of 36 ml tetrahydrofuran and 60 ml methanol. The impregnated film was rolled onto a reel and heated to a temperature of 100° C. for 15 minutes. After extraction, a base film was obtained with a specific conductivity of 0.2 S/cm.
FIG. 1 is a schematic representation of a device by means of which the method according to the invention may be applied. The base film obtained was placed in the device according to FIG. 1. To this end, the base film was placed on a take-off reel 1, passed along a guide pulley 2 and between an anode 3 and a cathode 4 and a guide pulley 5 and attached to a take-up reel 6. A cathode reservoir 7 was filled with 180 ml of a solution of 4.8 grams p-toluene sulphonic acid, 3.3 ml pyrrole and 2.5 ml water in 250 ml acetonitrile. The length of the applied anode (3) was 10 cm. The rate of travel of the base film was 5.4 cm/minute, resulting in a contact time, during which the base film was wetted with the electrolyte solution, of approximately 110 seconds.
Electrolysis was effected at a current density between the anode and the cathode of 14.1 mA/cm 2 . A good, homogeneous polypyrrole coating was deposited on the base film. The specific conductivity of the resultant, smooth film was 30 S/cm.
EXAMPLE II
A conductive base film produced analogously to Example I was continuously passed along the anode at a speed of 1.8 cm/minute, the conditions being equal to those in Example I. The specific conductivity of the film so produced was 70 S/cm.
COMPARATIVE EXPERIMENT A
Example II was repeated except that a non-conductive UHMW-PE base film (length 40 meters; width 8.5 cm; thickness 35 μm; porosity 83%) was passed along the anode. The film so produced was not electrically conductive.
COMPARATIVE EXPERIMENT B
Comparative experiment A was repeated except that the rate of travel of the base film was 0.18 cm/minute. During the experiment, travel of the base film along the anode was severely hampered by the film tending to adhere to the anode and by polyrrole depositing on the anode. The specific conductivity of the film so produced was 20 S/cm.
The examples demonstrate that in the method according to the invention the shaped article does not adhere to the electrode so that the method may be practised continuously. Failure of the shaped article to adhere to the electrode causes the method according to the invention to generate only very little waste. The method according to the invention produces, in a very short polymerisation time, a shaped article the electrically conductive polymer in which is homogeneously distributed. The applied base shaped article does not swell during wetting so that the mechanical properties of the base shaped article do not deteriorate. This allows a higher rate of production to be applied in, for instance, a continuous method.
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Method for the preparation of a polymeric shaped article containing an electrically conductive polymer wherein a base shaped article possessing electrically conductive properties is moved along an anode, at least part of the article being in contact with the anode, in the presence of an electrolyte-containing medium containing monomer units, which on polymerization form an electrically conductive polymer and wherein a voltage is applied between the anode and a second electrode which is in contact with the electrolyte-containing medium. It has appeared that, in the method according to the invention, the shaped article does not adhere to the electrode so that the method may be practiced continuously. A further advantage of the shaped article failing to adhere to the electrode is that the method according to the invention generates very little waste. Furthermore, it has appeared that the method according to the invention allows a shaped article to be produced with a very short polymerization time, the electrically conductive polymer in which being homogeneously distributed. The applied base shaped article does not swell during wetting, so that the mechanical properties of the base shaped article do not deteriorate. As a result, if the method is applied, for instance, continuously, a higher rate of production can be applied.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the priority of U.S. Provisional Patent Application Ser. No. 62/130,078, filed on Mar. 9, 2015 (pending), the disclosure of which is incorporated by reference herein.
FIELD OF THE INVENTION
[0002] This invention is specifically intended for civilians, off duty police, plain clothes police, detectives, and anyone else who wants to carry a concealed subcompact, compact, or, full size hand gun without a holster while enhancing features such as concealability, security, and comfort under the least amount of clothes.
BACKGROUND
[0003] For many years and to this present day there have been many ways and different systems for concealing a handgun for personal protection. Options currently include: holsters outside the waistband under an over coat, under the arm shoulder holsters, inside the waist band holsters, and the list goes on. With many of these systems the object is to not have your gun “print,” or to show through your clothes so no one knows you are carrying a gun. At the present time the number one choice to carry a concealed handgun is in a holster inside the waist band, referred to herein as “IWB”. With IWB holsters comes bulk, discomfort, and the possibility of purchasing additional pants with a larger waist size to accommodate the holster, not to mention adding even more thickness to your gun, which in turn will make it “print” more. As a result, many people will carry a smaller gun. The vast majority of these IWB holsters do not have any means of securing the gun. Others will have some sort of lock or strap, or other device for further securing the weapon. An IWB is not intended for a fast withdrawal from the holster when the gun is needed in a life and death situation. Most of today's IWB holsters have a tension grip on the hand gun to keep it from falling out of the holster, but no means of preventing an unauthorized use of your hand gun. IWB holsters are limited to either one angle for holstering the weapon, or they are very limited as to the adjustability for individual needs, and each IWB holster is specific to a particular hand gun, i.e., they are not universal.
SUMMARY
[0004] Generally, the invention provides a device for carrying a handgun in a concealed manner. The device includes a stabilizer key capable of being secured to and/or otherwise carried on the handgun as an integrated or separate unit, and a clip capable of being secured to apparel of a user. The clip includes a receiver for releasably engaging the stabilizer key, and allowing the stabilizer key to slide into and out of the receiver of the clip for insertion and withdrawal of the handgun. The device can include other features and options, such as summarized below.
[0005] A lock is provided and is movable between locked and unlocked positions for locking the stabilizer key in the receiver in the locked position and allowing withdrawal of the stabilizer key from the receiver in the unlocked position. A magnet is secured to the clip for providing further securement of the handgun to the clip when the stabilizer key is engaged with the receiver. The stabilizer key further comprises a raised rail element and the receiver further comprises an elongate slot. It will be appreciated that the receiver and stabilizer key may take many other forms instead. The elongate slot or other receiver is contained in an adjustable element that allows an orientation of the elongate slot or receiver to be angularly adjusted to adjust the angular orientation of the handgun when the raised rail element is contained in the elongate slot. The stabilizer key and therefore the handgun are capable of being locked in the adjusted angular orientation. The clip further comprises a U-shaped element capable of being clipped over a waistband and/or belt of a user. The U-shaped element further includes a curved slot. A fastening element couples the receiver to the curved slot allowing the angular orientation of the elongate slot to be adjusted relative to the U-shaped element for adjusting an angular orientation of the handgun as mentioned above.
[0006] The invention further provides a method for carrying a handgun in a concealed manner. The method includes securing a clip to apparel of a user, the clip including a receiver for releasably engaging a stabilizer key on a handgun. The stabilizer key is slid into the receiver of the clip to releasably secure the handgun on the apparel of the user. The method can include further features and/or steps as options such as summarized below.
[0007] The method further comprises locking the stabilizer key in the receiver with a locking element, and moving the locking element to an unlocked position to allow withdrawal of the stabilizer key from the receiver. The handgun is secured to the clip with a magnet when the stabilizer key is engaged with the receiver. The stabilizer key further comprises a raised rail element and the receiver further comprises an elongate slot, and the method further comprises inserting the raised rail element into the elongate slot. An angular orientation of the elongate slot is changed or adjusted to change the angular orientation of the handgun when the raised rail element is contained in the elongate slot. The receiver is locked in the adjusted angular orientation. The clip further comprises a U-shaped element and the method further comprises clipping the U-shaped element over a waistband and/or belt of a user. The U-shaped element further includes a curved slot, and a fastening element couples the receiver to the curved slot. The method further comprises adjusting an angular orientation of the elongate slot relative to the U-shaped element for adjusting an angular orientation of the handgun.
[0008] Various additional advantages and features will become more readily apparent to those of ordinary skill in the art upon review of the following detailed description of the illustrative embodiments taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1A is an exploded perspective view showing all components/hardware, along with receiver/rail relationship to each other in accordance with one embodiment of the device.
[0010] FIG. 1B is a perspective view illustrating connection of the raised rail into the receiver.
[0011] FIG. 2A is a perspective view illustrating connection of an alternative embodiment of a raised rail into the receiver.
[0012] FIG. 2 depicts all components/hardware in exploded view, along with the receiver and the alternative embodiment of the raised rail.
[0013] FIGS. 3A and 3B are perspective views showing an embodiment of a receiver, magnet, clip, and lock portion of the device from an inside, or rear view.
[0014] FIGS. 4A and 4B are perspective views showing an embodiment of a receiver, magnet, and clip portion of the device from an inside, or rear view and without a lock portion installed.
[0015] FIGS. 5A and 5B are perspective views showing an embodiment including the receiver, magnet, clip, and a lock portion from an outside, or front view.
[0016] FIGS. 6A and 6B are perspective views showing the receiver, magnet, and clip portion of the device from an outside, or front view without a lock portion installed.
[0017] FIGS. 7A and 7B are perspective views showing the receiver, clip, and lock portion of the device from an inside, or rear view without any magnet.
[0018] FIGS. 8A and 8B are perspective views showing the receiver and clip portion of the device from an inside, or rear view without any lock or magnet.
[0019] FIGS. 9A and 9B are perspective views showing the receiver, clip and lock portion from an outside, or front view.
[0020] FIGS. 10A and 10B are perspective views showing the receiver and clip portions of the device from an outside, or front view without the lock portion.
[0021] FIG. 11 is a perspective view showing the stabilizer key portion of the device separate, and attached to a firearm in the form of a handgun.
[0022] FIG. 12 is a perspective view of an alternative raised rail portion of a device both separated from, and attached to a firearm in the form of a handgun.
[0023] FIG. 13 shows the device in working form attached to apparel in the form of the waistband of a pair of pants and a belt, with the firearm at an extreme angle.
[0024] FIG. 14 is a perspective view of a handgun with an alternative embodiment of a raised rail.
[0025] FIG. 14A is a perspective view illustrating insertion of a raised rail or key element into a receiver of the device.
[0026] FIG. 15 is an exploded perspective view of an alternative embodiment of a clip having a receiver, and being angularly adjustable to adjust the angle of a firearm as desired by a user.
[0027] FIG. 16 is an assembled perspective view of the clip and receiver of FIG. 15 .
[0028] FIG. 17 is a cross-sectional view taken generally along line 17 - 17 of FIG. 16 but also showing the raised rail.
[0029] FIG. 18A is an elevational view of the clip and receiver of FIG. 16 .
[0030] FIG. 18B is an elevational view similar to FIG. 18A , but with a slotted portion of the receiver removed for clarity and showing angular adjustment with respect to the clip portion of the device.
DETAILED DESCRIPTION
[0031] FIGS. 1A and 1B illustrate a first embodiment of the device 1 . In FIG. 1A , the device 1 is comprised of a stabilizer key 40 in the form of an elongate rail. In this embodiment, the elongate rail 40 comprises an assembly of two outer pieces 40 a, 40 c and an inner piece 40 b secured together by, for example, threaded fasteners 90 . The rail 40 is secured to the side of the firearm 2 , such as a handgun, by any convenience or desired manner, e.g., adhesive. Alternatively, the stabilizer key 40 may be integrally formed with the firearm 2 . The stabilizer key 40 may take other forms, such as raised elements of other shapes. The device 1 is further comprised of a receiver 10 , a U-shaped clip 20 , and a lock 30 . The lock 30 aligns with the elongate slot portion 10 a in the receiver 10 and is secured by threaded fasteners 80 and nuts 70 to a curved slot 20 a in the U-shaped clip 20 . This will be described further below.
[0032] FIG. 1B illustrates how the stabilizer key 40 or elongate rail in this embodiment slides into the elongate slot 10 a of the receiver 10 . As shown in FIG. 13 , the U-shaped clip 20 fits over the waistband and/or belt 22 of a user and the handgun 2 may then be secured to the outer side of the U-shaped clip 20 by sliding the elongate rail 40 into the elongate slot 10 a of the receiver 10 . The lock 30 is used to optionally further secure the end of the rail 40 and thereby prevent inadvertent withdrawal or removal of the handgun 2 . In this regard, a tab 30 a of the lock engages the end of the rail 40 . To remove the handgun 2 , the user lifts up slightly on the outer end portion 30 b or bent portion of the lock 30 to release the rail 40 and allow the rail 40 to be slid out of the elongate slot 10 a. For this purpose, the lock 30 is resilient and springs back to its original locked position.
[0033] FIGS. 2 and 2A illustrate another embodiment in which an elongate rail 50 is a single integral element again adhered to the outside of the handgun 2 by any desired manner, such as using any suitable adhesive. It may instead comprise an element integral with the firearm 2 . This embodiment further includes a magnet 60 that is retained between the receiver 10 and the lock 30 and held in place by the lock 30 as best shown in FIGS. 3A and 3B . The rail 50 may be formed from magnetic material, such as carbon steel, and the magnet 60 is a strong permanent magnet (e.g., neodymium) such that the magnetic force will hold the rail 50 within the elongate slot 10 a without the need for a mechanical lock system.
[0034] FIGS. 4A and 4B are similar to FIGS. 3A and 3B , but illustrate the device 1 without the lock 30 . In this case, the magnet 60 may be secured in any desired manner.
[0035] FIGS. 5A and 5B are rear views illustrating the assembly of the lock 30 , the magnet 60 , and the receiver 10 , together with the U-shaped clip 20 .
[0036] FIGS. 6A and 6B are similar views to FIGS. 5A and 5B , but illustrate the assembly without the lock 30 and, for example, the magnet 60 secured to the receiver 10 in any other desired manner.
[0037] FIGS. 7A and 7B illustrate the assembly as shown in FIGS. 5A and 5B without the magnet 60 , but including the lock 30 secured with fasteners 80 .
[0038] FIGS. 8A and 8B are similar to FIGS. 7A and 7B , but illustrate the device 1 without the lock 30 and without the magnet 60 . It will be appreciated that in various designs or embodiments, the elongate slot 10 a itself may hold the elongate raised rail 40 , 50 or other key in place in any suitable manner, such as by way of a friction fit.
[0039] FIGS. 9A and 9B are similar to FIGS. 8A and 8B , but illustrate a rear view of the device 1 , including the lock 30 secured by fasteners 70 , 80 to the curved slot 20 a.
[0040] FIGS. 10A and 10B are respective rear views of the device 1 , without any lock 30 secured in place and without any magnet 60 , but with only the receiver 10 secured to the U-shaped clip 20 by way of threaded fasteners 70 , 80 received in the curved slot 20 a. It will be appreciated that when these fasteners 70 , 80 are tightened, the receiver 10 will be locked at a desired angular orientation, such as the orientation shown. The range of adjustment angles may vary, such as from about 20° to horizontal to about 90° to horizontal. This sets the angular orientation of the handgun 2 as desired by the user, depending on their preferences for that angle, as well as preferences for the location at which the U-shaped clip 20 will be secured to the apparel of the user.
[0041] FIGS. 11 and 12 are respective views illustrating the two embodiments of the elongate rail 50 , 40 secured to the side of the handgun 2 . As mentioned previously, FIG. 13 illustrates the handgun 2 secured to the device 1 from a perspective inside the waistband 20 of a pair of pants.
[0042] FIGS. 14 and 14A illustrate another possible embodiment for an elongate, raised rail 100 secured to the side of a handgun 2 and insertion of the rail 100 within a receiver 110 comprising an elongate hole 110 a.
[0043] FIGS. 15 through 18 illustrate another embodiment of the invention comprising a receiver 10 that engages a rail 40 ( FIG. 17 ). The receiver 10 again is a plate assembled to align a slot 10 a with a curved slot 20 a in a U-shaped clip 20 ′, and the device 1 ′ further includes an elongate plate 120 aligned with the slot 10 a for essentially allowing the rail 40 to be slid between the receiver plate 10 and the elongate plate 120 with a snug fit as the rail 40 slides into the elongate slot 10 a, as best shown in FIGS. 16 and 17 . The receiver plate 10 is fastened to the elongate plate 120 and the clip 20 ′ by a pair of threaded fasteners 130 , nuts 140 and washers 150 such that the receiver plate 10 and the attached elongate plate 120 may be oriented as desired along with curved slot 20 a as shown in FIGS. 18A and 18B . The various components of the device 1 ′ may be formed from any material or combinations of materials, such as metal(s) and/or nonmetals (e.g., polymers). As previously mentioned, the angular orientation will determine the angular orientation of the handgun 2 ( FIG. 1 ) that is engaged with the receiver plate 10 and elongate plate 120 as the rail 40 slides into the slot 10 a. The orientation of the receiver plate 10 and elongate plate 120 is locked by tightening the fasteners 130 at the desired location along the curved slot 20 a.
[0044] Devices made with accordance with the various aspects described herein may be secured to any type of apparel worn by a user, such as pants and/or belts of any suitable design. The device is also ambidextrous and may even be positioned at any point along the user's waist, including the left, the right, or the front or rear. By utilizing the angular orientation that is most extreme, e.g., approximately 20° from horizontal, the user can make the firearm appear smaller, and produce a better angle from which to draw the firearm. Of course, the same benefits are realized for smaller firearms as well. With a lock, as disclosed herein for example, or using other manners of firmly securing the stabilizer key, the firearm will be secure within the device but still easily drawn. The device may be used inside or outside the waistband, and alternatively may be clipped onto any vertical belt as in backpacks or other shoulder-type straps. The device allows the user to withdraw their firearm in one swift move, reaching for the firearm and withdrawing in the same desired direction. Many other systems require the user to unlock in one direction and then proceed to withdraw the firearm in another direction. As mentioned above, the various components of the device may be formed of any desired materials or combinations of materials. Some examples include polypropylene, Kydex® (acrylic PVC), PVC, acrylic or other polymers, and various types of metals, such as steel, stainless steel, titanium, cold rolled steel, hot rolled steel, etc. One manner of wearing the device will position the receiver inside the waistband of the user's pants with a portion of the clip extending over the upper edge of the user's pants and engaging with the user's belt. Another manner will position the receiver outside the user's pants. In essence, the clip will contain the upper edge of the pants and belt.
[0045] While the present invention has been illustrated by the description of specific embodiments thereof, and while the embodiments have been described in considerable detail, it is not intended to restrict or in any way limit the scope of the appended claims to such detail. The various features discussed herein may be used alone or in any combination. Additional advantages and modifications will readily appear to those skilled in the art. The invention in its broader aspects is therefore not limited to the specific details, representative apparatus and methods and illustrative examples shown and described. Accordingly, departures may be made from such details without departing from the scope or spirit of the general inventive concept.
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A device for carrying a handgun in a concealed manner includes a stabilizer key capable of being secured to and/or carried on the handgun. A clip is capable of being secured to apparel of a user. The clip includes a receiver for releasably engaging the stabilizer key, and allowing the stabilizer key to slide into and out of the receiver of the clip for insertion and withdrawal of the handgun.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to video data compression.
2. Description of the Prior Art
Some video data compression systems, such as systems defined by the MPEG II standard 1 , use a number of different coding techniques to encode successive pictures of a video signal.
Typically, the video signal is divided into successive groups of pictures (GOPs). Within each GOP at least one picture is encoded as an "I-picture", or intra-picture, using only information present in that picture itself. This means that I-pictures can later be decoded without requiring information from other pictures, and so provide random entry points into the video sequence. However, the converse of this is that the encoding of I-pictures cannot make use of the similarity between successive pictures, and so the degree of data compression obtained with I-pictures is only moderate.
Further pictures within each GOP may be encoded as "P-pictures" or predicted pictures. P-pictures are encoded with respect to the nearest previous I-picture or P-picture, so that only the differences between a P-picture and a motion-compensated previous P- or I-picture needs to be transmitted.
Finally, some of the pictures within a GOP may be encoded as "B-pictures" or bidirectional pictures. These are encoded with respect to two other pictures, namely the nearest previous I- or P-picture and the nearest following I- or P-picture. B-pictures are not used as references for encoding other pictures, so a still higher degree of compression can be used for B-pictures because any coding errors caused by the high compression will not be propagated to other pictures.
Although the MPEG specification allows for flexibility in the allocation and dependencies of I, P and B pictures, these allocations are generally fixed for a particular system.
It has also been proposed that the MPEG specification could be modified so that B-pictures could be derived from only a single other (preceding or following) I-picture or P-picture. Furthermore, it has been proposed that the number (one or two) and relative position (preceding or following position) of pictures used in the derivation of a B-picture could be made variable from picture to picture, or even from macroblock to macroblock within a B-picture. In particular, it has been proposed that the choice could be made by comparing the coding errors which would result from deriving a B-picture from the three possible picture sources described above (i.e. a preceding picture only, a following picture only, or a preceding and a following picture).
It is a constant aim in the field of video compression and an object of this invention to improve the degree of data compression which can be obtained.
SUMMARY OF THE INVENTION
This invention provides video data compression apparatus in which input data representing at least portions of a picture can be encoded by generating motion data representing image motion between that picture and at least two different sets of one or more reference pictures, the apparatus comprising:
means for comparing test data indicative of the quantity of motion data required for encoding with respect to the sets of reference pictures; and
means responsive to the comparing means for selecting the set of reference pictures for which the test data indicates the lowest quantity of motion data, for use in encoding the input data.
The invention recognises that the coding error rate is not the only factor relevant to the choice of how to encode a picture (e.g. in dependence on one or more other pictures). It is also important to consider the quantity of data required to encode the resulting picture, and in particular the motion vectors required for each coding scheme. This will have the effect of weighting the selection towards schemes using fewer (or more compactly encoded) motion vectors.
Therefore, in the present invention the decision on how to derive the picture in question (or a portion of it) is based at least in part on the quantity of data required to encode the motion vectors for each possible choice of reference pictures. In this way, the most favourable set of motion vectors, being the set requiring the least data to encode, can be selected. This can help to reduce the overall data rate required to encode the video signal, and so improve the degree of data compression achieved by the video compression system.
Generally for pictures derived from two surrounding reference pictures, two sets of motion vectors will be required: one to point to a preceding reference picture and one to point to a following reference picture. In other words, the quantity of data required for encoding the motion vectors will be roughly double that required to encode motion vectors pointing to a single reference picture. However, the converse of this is that if the picture can be derived by averaging two references, the picture quality will tend to be better (i.e. there will tend to be fewer encoding errors when two references are used), and particularly so in cover/uncover situations such as camera pans. Accordingly, in order to take this into account, it is preferred that the test data is also indicative of respective encoding errors obtained by encoding the input data with respect to the sets of reference pictures. In this case, it is preferred that the motion data comprises one or more motion vectors.
Preferably the motion data represents one or more motion vectors; and the test data is also indicative of the quantity of data required to encode the input data using the one or more motion vectors.
Preferably the apparatus comprises means for encoding the motion vectors so that the quantity of data required to encode a motion vector increases with increasing motion vector size. Using this technique, in one preferred embodiment, the test data for a set of reference pictures is dependent upon the size of the motion vectors corresponding to that set.
The sets of reference pictures could be selected from many different permutations of preceding or following pictures, or both. For example, the sets of reference pictures could comprise two or more sets selected from the group consisting of:
(i) only a temporally preceding picture;
(ii) only a temporally following picture; and
(iii) a temporally preceding picture and a temporally following picture.
The invention is applicable whether the pictures are fields or frames.
Preferably the input data comprises data representing a rectangular block of a picture.
This invention also provides a video data compression method in which input data representing at least portions of a picture can be encoded by generating motion data representing image motion between that picture and at least two different sets of one or more reference pictures, the method comprising the steps of:
comparing test data indicative of the quantity of motion data required for encoding with respect to the sets of reference pictures; and
in response to the comparing step, selecting the set of reference pictures for which the test data indicates the lowest quantity of motion data, for use in encoding the input data.
The invention is applicable to, for example, B-pictures of an MPEG-related system, but it should be noted that the invention could equally be applied to other video compression schemes.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and advantages of the invention will be apparent from the following detailed description of illustrative embodiments which is to be read in connection with the accompanying drawings, in which:
FIG. 1 is a schematic block diagram of a video compression apparatus;
FIG. 2 schematically illustrates a sequence of video fields of a video signal;
FIG. 3 schematically illustrates a decompressor;
FIG. 4 is a schematic block diagram of a second video compression apparatus; and
FIG. 5 schematically illustrates a picture selector.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 1, a video signal compression apparatus comprises a frame reorderer 10, a motion estimator 20), a trial quantiser 30, a GOP delay 40, a subtracter 50, a data compressor 60 and a data decompressor 70. The apparatus receives uncompressed video data at an input terminal 80 and generates compressed video data at an output terminal 90.
Many features of the apparatus of FIG. 1 operate in a very similar manner to corresponding features of an MPEG encoder described in the specification cited above and any other documents. Such features will not be described in detail here.
Briefly, therefore, the frame reorderer 10 acts on a group of pictures (GOP) to reorder the pictures so that each picture within the GOP is compressed after those pictures on which it depends. For example, if a B-picture depends on a following P- or I-picture (in the display order of the pictures), it is reordered to be compressed after that P- or I-picture.
For some of the pictures (B-pictures), a selection is made on a macroblock-by-macroblock basis as to how the data of the B-picture should be encoded. Broadly, the choice is between encoding with respect to only a preceding I- or P-picture, only a following I- or P-picture, or both of a preceding and a following I- or P-picture. (This selection is made within the data decompressor 70, to be described in more detail below).
The trial quantiser performs a trial compression on at least part of the video data of each GOP, to assess a suitable quantisation factor for use in the final compression of the video data. The GOP delay 40 is used to allow the trial quantisation to occur before the final compression process is applied to pictures of a GOP.
The pictures of a GOP are finally compressed by the compressor 60. For an I-picture, the encoding is formed using only intra-picture techniques, so the I-picture is supplied directly from the GOP delay 40 to the compressor 60 (i.e. a zero input is supplied to the subtracting terminal 55 of the subtracter 50). The I-picture is compressed by the compressor 60 using a quantisation factor derived with reference to the trial quantiser 30, and is supplied as a compressed I-picture at the output terminal 90.
P- and B- pictures are encoded with respect to pictures which have already been encoded by the final compressor 60. In fact, for these pictures, it is the difference between a picture and predicted versions of the one or more pictures on which it depends which are encoded. To achieve this, the picture for encoding is supplied to the subtracter 50 from the GOP delay 40, and predicted versions (i.e. encoded and subsequently decoded by the decompressor 70) of the picture or pictures on which it depends are supplied to the subtracting input 55 of the subtracter 50. The output of the subtracter 50 is therefore a difference signal, which is then compressed by the compressor 60.
As part of the operation of the compressor 60, motion vectors representing image motion between a current macroblock and blocks of other pictures from which the current macroblock is derived are encoded as variable length codes such as Huffman codes. The VLC coding process follows the usual pattern in which smaller, more commonly occurring motion vectors arc encoded to form shorter VLC codes, and larger, less commonly occurring motion vectors arc encoded to form longer VLC codes.
FIG. 2 is a schematic diagram illustrating a sequence of fields f1. . . f6 of a video signal. Time is represented along a horizontal axis from left to right.
In FIG. 2 it is assumed that a field f3 is a B-picture to be derived from preceding and/or following fields or frames. Several derivations are possible. For example, f3 could be derived from:
f1 (preceding field of the same polarity)
f2 (preceding field of the opposite polarity)
(f1+f2) (preceding frame)
f5 (following field of the same polarity)
f6 (following field of the opposite polarity)
(f5+f6) (following frame)
f1 and f5 (preceding and following fields of the same polarity)
and other permutations. Also, derivations from fields or frames which are not temporally adjacent to the current field could be considered.
Accordingly, it is possible for a dynamic choice to be made between all or a subset of these possibilities. In FIG. 3, for clarity of the diagram, only three choices are considered: these are two types of uni-directional prediction from a single field of the same polarity, and bi-directional prediction from surrounding fields of the same polarity. In FIG. 5, frame-based derivation is also tested.
In FIGS. 3 and 5 the selection is made on a macroblock-by-macroblock basis (where a macroblock is typically a block of 16×16 (luminance) pixels). By choosing a coding scheme for each macroblock individually, the most appropriate scheme for different parts of the picture can be selected. Also, the hardware requirements are reduced, since it is not necessary to examine all of the picture at a time to select a coding scheme. However, in other embodiments, the coding scheme could be selected on the basis of an examination of the coding performance of the whole picture, or the scheme for an entire picture could be selected by testing the coding performance of only a subset of the picture (e.g. one macroblock).
FIG. 3 is a schematic diagram of a part of the data decompressor 70. (In actual fact, some features of FIG. 3, in particular the motion estimators 100, 110 and the field stores 150, 170 to be described below arc not found in the decompressor 70, but are included in FIG. 3 all the same to assist in explanation of the picture selection techniques).
Each B-picture to be compressed is treated as a series of separate macroblocks (MB). A macroblock is supplied in parallel to a forward motion estimator 100, a backward motion estimator 110 and adders 120, 130 and 140.
The forward motion estimator 100 compares the current macroblock with blocks at the same and surrounding positions in a temporarily following (source) I- or P-picture 150, to generate one or more motion vectors representing the motion of the contents of that macroblock between the current and following image.
A forward predictor 160 then uses that motion vector and data representing the forward field 150 to predict the contents of the current macroblock from the forward field. The output of the prediction is supplied to the adder 120.
Similarly, the backward motion estimator 110 uses data representing the preceding I- or P-picture 170 to generate one or more motion vectors. A backward predictor 180 then uses the backward field data 170 to create a predicted version of the current macroblock which is supplied to the adder 140.
The forward-predicted and backward-predicted macroblocks are also supplied to an adder 190 in which the average of the forward and backward predictions is calculated (one-half of the sum of the forward and backward predictions). The output of the adder 190 is supplied to the adder 130.
One of the two inputs to each of the adders 120, 130 and 140 is a subtracting input, so that the output of these three adders represents the differences between the original current macroblock and the predicted macroblock generated by forward prediction (output of the adder 120), backward prediction (output of the adder 140) and by-directional prediction (output of the adder 130).
The output of each adder is supplied to a respective bits estimator 200, 210, 220 which estimates the number of bits which will be required to code the difference data for that macroblock. These operate by detecting the mean of the sum of squares of the difference between the actual and predicted macroblocks.
In parallel with this process, two VLC length look-up tables 230, 240 receive the one or more motion vectors generated by the forward and backward motion estimators 100, 110, and use the values of those vectors to look-up the length of a variable length code which will subsequently be used to encode the vectors In other words, the VLC length look-up tables do not generate the actual VLC codes to represent the vectors (this is a relatively processor-intensive task), but they simply provide the number of bits which will be required for the VLC codes.
The outputs of the bits estimators and the VLC length look-up tables are then combined by adders 250, 260, 270 and 280, according to the following table:
______________________________________VLC length and bits estimate for output of adder 250forward uni-directional predictionVLC length and bits estimate for output of adder 280backward unidirectional predictionVLC lengths and bits estimate for output of adder 270bi-directional prediction______________________________________
In other words, the respective outputs of the adders 250, 270 and 280 provide indications of the number of bits which will actually be required to encode the current macroblock and associated motion vector(s) by the three possible methods under consideration (forward prediction, bi-directional prediction and backward prediction respectively). These bit counts can then be compared by comparators 290 to generate an output signal 300 specifying that one of the coding techniques which will result in the lowest bit count. The output 300 controls the operation of the apparatus of FIG. 1 to select appropriate reference pictures for use in the coding of B-pictures.
FIG. 4 is a schematic diagram of another embodiment of a video compression apparatus.
The apparatus of FIG. 4 is very similar to that of FIG. 1, and indeed many of the component parts bear the same reference numerals. However, a difference is that the decision on which reference fields to use for encoding B-pictures is made by a picture selector 20 forming part of the motion estimator. This provides a control signal to control the operation of the compressor 60, the decompressor 70 and the subtracter 50.
FIG. 5 is a schematic diagram of the picture selector 75 of FIG. 4.
In FIG. 5, a current macroblock is supplied in parallel to a forward motion estimator 310, which performs forward motion estimation with respect to forward fields 320; a backward motion estimator 350 which performs motion estimation with respect to backward fields 340, and a bi-directional motion estimator 330, which uses the "best vectors" identified in forward and backward motion estimation to perform motion estimation with respect to the forward fields 320 and the backward fields 340.
Each motion estimator produces not only motion vectors but also a mean absolute error (MAE) signal, which is (in this embodiment) the mean of absolute luminance differences between pixels at corresponding positions in the current macroblock and the block of the forward (or backward or both) image used for motion estimation. The MAE is, in effect, a by-product of the motion estimation process as described in the above reference.
In fact, each of the motion estimators produces vectors and an MAE value for field- and frame- (pairs of fields) -based motion estimation. In each case, the vectors and MAE values are passed to a respective adder 360.
The output of each adder 360 is a sum of the vector components and the MAE value for the two inputs supplied to the adder. Therefore, in this embodiment, the exact number of bits which will be required to encode the macroblock or to encode the vectors is not assessed (although this could be done using a VLC length look-up table and/or a bits estimator similar to those in FIG. 3). Instead, it is recognised that the MAE value tends to be correlated with the number of bits which will be required to encode the difference data for that macroblock, and the size of the motion vectors (or the vector magnitude) tends to be correlated with the number of bits required to encode the vector. Therefore, the respective sums of these values can be compared by a comparator 370 to generate an output signal 380 indicative of the encoding technique having the lowest sum of vector components and MAE. In this case, the output signal 380 forms the control output of the picture selector 25 of FIG. 4.
In each of the above embodiments, it will be appreciated that the choice of fields or frames to use in the coding of B-pictures can be communicated to the receiver of the compressed video data using known features of the normal MPEG data stream.
Although illustrative embodiments of the invention have been described in detail herein with reference to the accompanying drawings, it is to be understood that the invention is not limited to those precise embodiments, and that various changes and modifications can be effected therein by one skilled in the art without departing from the scope and spirit of the invention as defined by the appended claims.
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A video data compression system in which input data representing at least portions of a picture can be encoded by generating motion data representing image motion between the picture and at least two different sets of one or more reference pictures. The system is operable to compare test data indicative of the sum of the quantity of motion data and quantity of error data required for encoding with respect to the sets of reference pictures, select the set of reference pictures for which the test data indicates the lowest sum, and use the selected set of reference pictures to encode the input data.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to rack and pinion gear devices. More specifically, the present invention relates to an apparatus for properly indexing the pinion to the rack during assembly.
2. Disclosure Information
Rack and pinion devices are commonly used to transform rotations of a pinion into translations of a rack. Electrical switches and mechanical selectors frequently employ a rack and pinion device. Commonly, operators use switch devices to select a single function from several optional functions. An example of such an application is a climate control system operated through a rotary switch as found in motor vehicles. The operator selects an operating mode, such as "vent" from several options, such as floor, defrost, air conditioning, etc., by rotating the dial to the desired function. Another common motor vehicle application is the ignition key switch.
A problem in assembling switches employing rack and pinion devices is properly aligning the pinion to the rack. Alignment is difficult because the rack and pinion are meshed in a "blind spot," meaning that it is difficult to visually inspect the meshing. If the rack and pinion are not meshed properly during assembly, when the operator makes a selection, the desired function may not be activated. For example, when the ignition key is rotated to the "LOCK" position, the switch may actually engage the "ACCESSORY" position. When the apparatus is assembled in this condition, the switch is "misstaged." Preventing misstaging requires meticulous alignment during assembly, a time and labor intensive procedure. Ultimately, misstaging can result in a dissatisfied customer and increased warranty costs associated with removal and realignment of the switch.
Various devices have been proposed for indexing a rack and pinion. For example, U.S. Pat. No. 2,410,643 discloses a rack and pinion mechanism that provides self alignment for longitudinally engaging mechanisms. Longitudinal engagement occurs when the relative motion between the rack and pinion is on the longitudinal axis of the rack. This is not helpful, however, when the rack and pinion are engaged laterally, particularly in a blind spot. Lateral engagement occurs when the relative motion between the rack and pinion occurs generally perpendicularly to the longitudinal axis of the rack.
It would be desirable to provide an apparatus that would ensure accurate staging of a rack and pinion mechanism in which the pinion laterally engages the rack in a blind spot. It would be further desirable to provide a device that prevents a switch assembly from being assembled in a misstaged condition.
SUMMARY OF THE INVENTION
The present invention provides a solution to misstaging a rack and pinion mechanism. In accordance with the present invention, there is disclosed a switch apparatus comprising an elongate rack having a plurality of rack teeth disposed thereon, the rack is axially reciprocal. Additionally, the switch apparatus has a pinion adapted to matingly engage the rack. The switch apparatus further comprises a mechanism for aligning the pinion relative to the rack along an axis generally Parallel to the axis of the rack teeth. The switch apparatus also comprises a mechanism for preventing misstaging of the pinion relative to the rack.
One advantage the present invention provides is consistent engagement of a rack and pinion switch apparatus assembled under blind assembly conditions. Other advantages of the present invention will become apparent to those skilled in the art from the drawings, detailed description and claims which follow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the interior of an automobile.
FIG. 2 is an exploded perspective view of a steering column mounted ignition switching assembly.
FIG. 3 is a perspective view of an installation tool assembly prepared for installation of the present invention.
FIG. 4 is a perspective view of a rack gear according to the present invention.
FIG. 5 is a top view of the installation tool fully inserted in the cylindrical bore in accordance of the present invention.
FIG. 6 is a cross-sectional view taken along line 6--6 of FIG. 5.
FIG. 7 is a cross-sectional view taken along line 7--7 of FIG. 6.
FIG. 8 is a top plan view of the installation tool and switch apparatus components in the rotated position in accordance with the principles of the present invention.
FIG. 9 is a cross-sectional view taken along line 9--9 of FIG. 8.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, FIGS. 1 and 2 show a motor vehicle 10 having an ignition key cylinder 12 mounted to a steering column 14. Steering column 14 includes a steering column housing 16 having an integrally formed cylindrical bore 18 and a guide bore 19 for housing the ignition key cylinder 12. A switch apparatus 20, according to the present invention, operatively interconnects the ignition key cylinder 12 to an ignition switch block 22. It should be readily apparent to one skilled in the art that this invention applies equally to a broad range of devices employing rack and pinion mechanisms such as automotive climate control switches and automotive rack and pinion steering systems.
The switch apparatus 20 includes a retainer 24, a generally planar disk 26 having an axial protuberance 28, a pinion 30 having a plurality of pinion teeth 32 circumferentially disposed thereabout which meshingly engage a rack 34 through a plurality of rack teeth 36. During assembly, the protuberance 28 engages a notch 38 disposed on the rack 34 at a predetermined location.
In one embodiment, as shown in FIGS. 2, 3 and 6, the protuberance 28 comprises an axial arcuate extension integrally cast with disk 26. The protuberance 28 fits onto the outer circumference 42 of the pinion 30, and circumferentially occupies the space of approximately two Pinion teeth 32. Additionally, the protuberance 28 has an axial length of approximately one half the axial length of the pinion 30. Although the disk 26 of the described embodiment is made utilizing sintered metal technology, the invention is not so limited. Alternative materials including, but not limited to, die cast metals, stamped steels and plastics would function equally well.
The pinion 30 includes a set of short pinion teeth 44 having an axial length of approximately one-half the axial length of the pinion 30. The short teeth 44 surround approximately 270 degrees of the pinion 30. A set of long pinion teeth 46 make up the remaining teeth of the pinion 30. The free space 45 provided by the set of short pinion teeth 44 accommodates the protuberance 28 during assembly and subsequent rotation of the pinion 30. The set of short pinion teeth 44 extend around the Pinion 30 for at least as many degrees as the switch 12 rotates in operation. The switch in the described embodiment rotates less than 270 degrees about the rotational axis of the switch.
In one embodiment, the distal end of rack 34 is connected to an ignition switch block 22 for activating the vehicle 10. Rack 34 includes the notch 38 comprising a single short rack tooth 40, as shown in FIGS. 4 and 6. The location of the notch 38 on rack 34 establishes the Positioning of properly staged rack 34. The notch 38 has a depth of approximately one half the length of a rack tooth 36. According to the present invention, the width of the notch 38 must closely match the mating width of the protuberance 28 to prevent misstaging. The specific notch of the described embodiment is only one example. For instance, the notch could be two teeth wide, or be a separate receiving hole located completely apart from the rack teeth. For instance, a hole disposed on the side of the rack 34 below the teeth 36. As with the pinion 30, the functionality of the present invention is not dependent on the process of manufacture or the material chosen for the rack 34. For example a sturdy plastic will work as well as a die cast or stamped rack.
An assembly tool 48, shown in FIG. 3, simultaneously aligns and installs the retainer 24, disk 26 and pinion 30 in cylindrical bore 18 of the steering column housing 16. With the rack 34 positioned in the guide bore 19, the tool 48 aligns and inserts the components in the bore 18. The tool 48 and cylindrical bore 18 are matingly keyed for positive alignment. Similarly, the retainer 24, disk 26, and pinion 30 are individually keyed to the tool 48 providing proper orientation within the cylindrical bore 18.
As the assembly tool 48 positions the pinion 30 in engagement with rack 34, the protuberance 28 simultaneously engages the notch 38. FIGS. 5-7 show the protuberance 28 and pinion 30 fully engaged with the rack 34. In this position, an operator rotates the tool 48, which in turn rotates the disk 26 and pinion 30 causing the retainer 24 to seat in the installed position , illustrated in FIGS. 8 and 9. This rotation causes the disk 26 to engage with the retention tabs 52 of the cylindrical bore 18 in the steering column housing 16. Simultaneously, the protuberance 28 rotates away from the rack 34 into a final installed position within the free space 45 on the pinion 30 that allows reciprocation of the rack 34.
However, when the assembly tool 48 is inserted in the cylindrical bore 18, if the rack 34 is not Properly staged, the protuberance 28 will not engage the notch 38. This will prevent complete insertion of the assembly tool in the bore 18. The retention tabs 52 will operatively interfere with the disk 26 to prevent tool 48 from rotating. Therefore, unless the protuberance 28 properly engages notch 38 in rack 34, the installation fails and misstaging is prevented.
It should be apparent that the described embodiment is not the only way of achieving the advantages of the present invention. As an example, an assembly tool having a permanently attached protuberance for engaging a receiving hole on the rack would also provide the same function. Assembly of the rack and pinion would only result when the protuberance properly engaged the hole in the rack. Various other modifications are also apparent without departing from the spirit and scope of the present invention. It is the following claims, including all equivalents, which define the scope of the present invention.
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A rack and pinion mechanism in a switch apparatus which ensures proper staging of the pinion to the rack during assembly is disclosed. A protuberance engages a receiver disposed on the rack and operates to prevent final assembly of the pinion to the rack unless both are properly staged. This minimizes the occurrence of misstaged switches assembled in blind installation conditions.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a reissue of U.S. Pat. No. 7,645,380, which is a continuation of U.S. patent application Ser. No. 10/997,452, filed Nov. 24, 2004, now U.S. Pat. No. 7,537,706, which is a continuation of U.S. patent application Ser. No. 09/943,111, filed Aug. 30, 2001, now U.S. Pat. No. 6,872,318, which is a continuation of U.S. patent application Ser. No. 09/606,952, filed Jun. 29, 2000, now U.S. Pat. No. 6,284,143, which is a continuation of U.S. patent application Ser. No. 09/220,401, filed Dec. 24, 1998, now U.S. Pat. No. 6,083,407, which is a continuation of U.S. patent application Ser. No. 08/756,273, filed Nov. 25, 1996, now U.S. Pat. No. 5,855,775, which is a-continuation-in-part of U.S. patent application Ser. No. 08/638,017, filed Apr. 25, 1996, now abandoned, which is a continuation-in-part of U.S. patent application Ser. No. 29/038,499, filed May 5, 1995, now abandoned. Each of these applications is incorporated by reference in its entirety.
BACKGROUND
1. Field of Invention (Technical Field)
The present disclosure relates to apparatuses for remediation of dissolved chlorinated hydrocarbons in aquifer regions by injecting micro-fine bubbles effective for active in situ groundwater remediation for removal of dissolved chlorinated hydrocarbon solvents and dissolved hydrocarbon petroleum products. Remediation of saturated soils may also be obtained by employment of the present apparatuses.
2. Background Prior Art
There is a well recognized need to cleanup subsurface leachate plumes in aquifer regions and contaminated sites including, in particular, dry-cleaning establishments and U.S. Military Air bases. Applicant is aware of prior art devices that have used injection of air to facilitate biodegradation of plumes.
However, an apparatus using micro-fine bubbles including a multi-gas oxidizing agent for the controlled remediation of a site containing poorly biodegradable organics, particularly dissolved chlorinated solvents, has not been shown.
In fact the Federal Agency (EPA, KERR Environmental Laboratory, ADA, Oklahoma) responsible for review of clean-up procedures at Marine Corp Air Base at Yuma, Ariz. has determined that there is no prior reference which discloses the use of the present apparatuses and has ordered independent pilot tests to provide test results confirming the results previously obtained by the present apparatuses.
U.S. Pat. No. 5,221,159, to Billings, shows injection of air into aquifer regions to encourage biodegradation of leachate plumes which contain biodegradable organics together with simultaneous soil vacuum extraction.
U.S. Pat. No. 5,269,943, METHOD FOR TREATMENT OF SOILS CONTAMINATED WITH ORGANIC POLLUTANTS, to Wickramanayake, shows a method for treating soil contaminated by organic compounds where an ozone containing gas is treated with acid to increase the stability of the ozone in the soil environment and the treated ozone is applied to the contaminated soil to decompose the organic compounds.
U.S. Pat. No. 5,525,008, REMEDIATION APPARATUS AND METHOD FOR ORGANIC CONTAMINATION IN SOIL AND GROUNDWATER, to Wilson, provides a method and apparatus for in-situ treatment of soil and groundwater contaminated with organic pollutants. It involves concentration of a reactive solution required to effect treatment of the contaminated area and injecting the reactive solution into one or more injectors that are inserted into the ground. The apparatus is scaled and positioned so as to assure flow and to allow reactive solution to flow through the contaminated area thereby reacting chemically. Preferably, the reactive solution is an aqueous solution of hydrogen peroxide and metallic salts.
U.S. Pat. No. 5,178,755, UV-ENHANCED OZONE WASTEWATER TREATMENT SYSTEM, to Lacrosse, mixes wastewater with ozonated liquid within a multi-stage clarifier system and suspended solids are removed.
Notwithstanding the teachings of the prior art, there has not been shown an apparatus for remediating a site contaminated with poorly biodegradable organics, particularly dissolved chlorinated solvents, with micro-fine bubbles including an encapsulated multi-gas oxidizing agent in a controlled manner. In situ remediation is accomplished using the present instrumentalities by employing microporous diffusers which inject multi-gas bubbles containing an ozone oxidizing agent into aquifer regions to strip and rapidly decompose poorly biodegradable organics or to accelerate biodegradation of leachate plumes which contain biodegradable organics thereby overcoming at least some disadvantages of the prior art.
SUMMARY
The present disclosure relates to sparging apparatuses for injection of oxidizing gas, in the form of small bubbles, into aquifer regions to encourage in situ remediation of subsurface leachate plumes.
In particular, sparging apparatuses are disclosed for employing microporous diffusers to inject micro-fine bubbles containing encapsulated gas bubbles into aquifer regions to encourage biodegradation of leachate plumes which contain biodegradable organics, or Criegee decomposition of leachate plumes containing dissolved chlorinated hydrocarbons. The sparging apparatuses, employing microporous diffusers for injecting an encapsulated multi-gas oxidizing agent, are particularly useful in promoting extremely efficient removal of poorly biodegradable organics, such as dissolved chlorinated solvents, without the use of vacuum extraction of undesirable by-products of remediation. Furthermore, remediation occurs by employing encapsulated multi-gas oxidizing agent for destroying organic and hydrocarbon material in place with out release of contaminating vapors.
Unlike the prior art, the contaminated groundwater is injected with an air/ozone mixture wherein micro-fine air bubbles strip the solvents from the groundwater and the encapsulated ozone acts as an oxidizing agent in a gas/gas reaction to break down the contaminates into carbon dioxide, very dilute HCl and water. This system is known as the C-Sparger® system.
The present system, hereinafter C-Sparger® system, is directed to low-cost removal of dissolved chlorinated hydrocarbon solvents such as perc from contaminated soil and groundwater aquifers. The C-Sparger® system employs microporous diffusers, hereinafter Spargepoints®, for producing micro-fine bubbles containing an oxidizing agent that decomposes chlorinated hydrocarbons into harmless byproducts. The C-Sparger® system also incorporates: means for pumping a multi-gas oxidizing mixture through the Spargepoint® into groundwater in a soil formation, a bubble production chamber to generate bubbles of differing size, a timer to delay pumping until large bubbles have segregated from small bubbles by rise time, and a pump which forces the fine bubbles and liquid out into the soil formation. The pumping means intermittently agitates the water in the well in which the C-Sparger® is installed in order to effectively disturb the normal inverted cone-shaped path of the bubbles injected by the Spargepoint®. Water agitation results in random bubble dispersion to ensure improved contact between the oxidizing agent (contained in each bubble) and the pollutant. The pulsing action promotes movement of the bubbles through the porous formation. It is the in situ stripping action and maintenance of low solvent gas concentration in the bubbles which increases the efficacy and speed of remediation of a site.
The apparatus of the present disclosure is particularly useful in efficiently removing poorly biodegradable organics, particularly dissolved chlorinated solvents, without the use of vacuum extraction, wherein remediation occurs by destroying organic and hydrocarbon material in place without the release of contaminating vapors.
The multi-gas system comprises an oxidizing gas encapsulated in micro-bubbles, generated from microporous diffusers, that are matched to soil porosity. A unique bubble size range is matched to underground formation porosity and achieves dual properties of fluid like transmission and rapid extraction of selected volatile gases. Bubble size is selected so as to maintain vertical mobility. In order to accomplish a proper matching, a prior site evaluation test procedure is devised to assess the effectiveness of fluid transmission at the remediation site.
Small bubbles with a high surface to gas volume ratio are advantageous in promoting rapid extraction of volatile organic compounds, such as PCE, TCE, or DCE. Pulsed injection of small bubbles and consequent rise time is matched to the short half-life of an oxidative gas, such as ozone, to allow rapid bubble dispersion into predominantly water-saturated geological formations, and extraction and rapid decomposition of the volatile organic material. The unique apparatus of the present disclosure provides for extraction efficiency with resulting economy of operation by maximizing contaminant contact with oxidant by selective rapid extraction providing for optimum fluidity of bubbles through media which can be monitored.
The use of microporous diffuser points provides a more even distribution of air into a saturated formation than the use of pressurized wells. A sparge system installed to remediate contaminated groundwater is made more cost-effective by sparging different parts of the plume area at sequenced times. Through the proper placement of sparge locations and sequence control, any possible off-site migration of floating product is eliminated. With closely spaced Spargepoints®, water mounding is advantageous because it prevents any off-site escape of contaminant. Water mounding is used to direct floating product toward extraction sites.
The microporous diffusers and multi-gas system, referred to as Spargepoints® and C-Sparger® Systems, are designed to remove dissolved organics and solvents (chlorinated hydrocarbons) such as PCE, TCE, and DCE from contaminated groundwater. The micro-fine bubbles, produced by the Spargepoints®, contain oxygen and ozone which oxidize the chlorinated hydrocarbons to harmless gases and weak acids. High initial concentrations of these dissolved organics have been, under some specific-circumstances, reduced to levels of 1 ppb or less in periods of a few weeks. None of the models to date are designed for explosive environments.
The present systems employ a plurality of configurations consisting of Series 3500 and Series 3600 C-Sparger® models. The 3600 Series is larger and has more capacity. Specifically, the 3600 Series has a better compressor rated for continuous use, a larger ozone generator, a second Spargepoint® below the first Spargepoint® in each well, and larger diameter gas tubing. Both model series have control units that can support: one (Models 3501 & 3601), two (Models 3502 & 3602) and three separate wells (Models 3503 & 3603). The one, two, and three well models differ in the number of relays, internal piping, external ports and programming of the timer/controller.
Normal operation for C-Sparger® systems includes carrying out, in series for each well, the following functions on a timed basis: pumping air and ozone through Spargepoint® diffusers into the soil formation, pumping aerated/ozonated water into the soils and recovering treated water above. Treatment is followed by a programmable period of no external treatment and multiple wells are sequenced in turn. Agitation with pumped water disturbs the usually inverted cone-shaped path of bubbles through the soils and disperses them much more widely. This increases contact and greatly improves efficiency and speed of remediation. Vapor capture is not normally necessary.
Series 3500 and 3600 systems include a control module, one to three well assemblies depending on specific model selected, a 1.0 ft. long submersible pump power-gas line for each well and a flow meter (to check Spargepoint® flow rates). Model Series 3500 & 3600 control modules have been successfully deployed outdoors in benign and moderate environments for prolonged periods of time. The control module must be firmly mounted vertically on 4×4 posts or on a building wall near the wells.
The actual placement depths, separations, number/size of wells and overall remediation system geometry are highly variable. Differences in specific pollutant, spill, soil, groundwater and climate characteristics can greatly influence the design and geometry of the overall remediation system. Monitoring wells are usually also needed. In short, specific circumstances and conditions are often critical, however, a generic or typical overall system is shown on FIG. 1 .
FIG. 13 provides the basic specification for the Series 3500 & 3600 systems. The drawing shows a single well system Series 3600 (M-3601). The Series 3500 does not have the lower Spargepoint® multiple well models (3502, 3503, 3602 & 3603), rather multiple M-3601 well units use a single control module. FIG. 2 shows a piping schematic. FIG. 3 shows an electrical schematic for a three well system (Model 3503 or 3603). Current production 3500 and 3600 Series models have an internal ground fault interrupter and surge buffers incorporated into various electrical components. FIG. 4 shows an internal layout of the control module box for a three well system (M-3503 or M-3603). FIG. 5 shows the geometry of the bottom panel on the control module identifying the external connections and ports for three well units (M-3503 & 3603). FIGS. 3 and 4 also illustrate fuses and their locations.
The Unique Use of Microfine Bubbles for Simultaneous Extraction/Decomposition.
The use of microporous Spargepoint® diffusers to create fine bubbles, which easily penetrate sandy formations to allow fluid flow, has unexpected benefits when used with multiple gas systems. Microfine bubbles accelerate the transfer rate of PCE from aqueous to gaseous state. The bubble rise transfers the PCE to the vadose zone. The ten-fold difference in surface-to-volume ratio of Spargepoint® diffuser microbubbles compared to bubbles from well screens results in a four-fold improvement in transfer rates. To block the gaseous state from reverting to a surface dissolved state in the vadose (unsaturated) zone, a microprocessor system shuttles an oxidizing gas through the vadose zone to chemically degrade the transported PCE.
Gaseous Exchange
If gaseous exchange is proportional to available surface area, with partial pressures and mixtures of volatile gases being held constant, a halving of the radius of bubbles would quadruple (i.e. 4×), the exchange rate. If, in the best case, a standard well screen creates air bubbles the size of a medium sand porosity, a microporous diffuser of 20 micron size creates a bubble one tenth ( 1/10) the diameter and then times the volume/surface ratio (Table 1).
TABLE 1
Diameter
Surface Area
Volume
Surface
(microns)
(4 πr 2 )
(4/3 r 3 )
Area/Volume
200
124600
4186666
.03
20
1256
4186
.3
Theoretically, the microporous bubbles exhibit an exchange rate of ten times the rate of a comparable bubble from a standard ten slot well screen.
Partitioning Enhancement
Soil Vapor concentrations are related to two governing systems: water phase and (non-aqueous) product phase. Henry's and Raoult's Laws (DiGiulio, 1990) are commonly used to understand equilibrium-vapor concentrations governing volatization from liquids. When soils are moist, the relative volatility is dependent upon Henry's Law. Under normal conditions (free from product) where volatile organic carbons (VOC's) are relatively low, an equilibrium of soil, water, and air is assumed to exist. The compound, tetrachloroethene (PCE), has a high exchange coefficient with a high vapor pressure (atm) and low aqueous solubility (μmole/l). By enhancing the exchange capacity at least ten fold, the rate of removal should be accelerated substantially.
Ozone is an effective oxidant used for the breakdown of organic compounds during water treatment. The major problem in effectiveness is ozone's short half-life. If ozone is mixed with sewage-containing water above-ground, the half-life is normally minutes. However, if maintained in the gaseous form, the half-life of ozone can be extended up to 15 hours. Microbubbles can be used as extracting agents by pulling chlorinated solvents out of solution into the gaseous ozone as they enter the microbubble. The small bubble's high surface-to-volume ratio increases the exchange area and accelerates the consumption of HVOC within the bubble maximizing the concentration of gas transferred into the bubble (C S −C). The rate-limiting process is the area-specific diffusion (dominated by Henry's Constant), while the decomposition reaction occurs rapidly (assuming sufficient ozone).
Ozone reacts quickly and quantitatively with PCE to yield breakdown products of hydrochloric acid, carbon dioxide, and water.
Using microporous diffusers to inject ozone-containing bubbles may offset ozone's relatively short half-life. By encapsulating the ozone in fine bubbles, the bubbles would preferentially extract volatile compounds like PCE from the mixtures of soluble organic compounds they encountered. The ozone-mediated destruction of organics may then selectively target volatile organics pulled into the fine air bubbles. Even in a groundwater mixture of high organic content like diluted sewage, PCE removal could be rapid.
The unique combination of microbubble extraction and ozone-mediated degradation can be generalized to render volatile organic compounds amenable to rapid removal. The efficiency of extraction is directly proportional to Henry's Constant which serves as a diffusion coefficient for gaseous exchange (Kg).
In wastewater treatment the two-film theory of gas transfer (Metcalf and Eddy, Inc, 1991) states the rate of transfer between gas and liquid phases is generally proportional to the surface area of contact and the difference between the existing concentration and the equilibrium concentration of the gas in solution. Simply stated, if the surface-to-volume ratio of contact is increased, the rate of exchange will increase. If the gas (volatile organic compound, hereinafter “VOC”) entering the bubble (or micropore space bounded by a liquid film) is consumed, the difference is maintained at a higher entry rate than if the VOC is allowed to reach saturation equilibrium. In the present case, the consumptive gas/gas reaction of PCE to by-products of HCl, CO 2 , and H 2 O drives the transfer of PCE into the bubble.
The normal equation for the two-film theory of gas transfer is (Metcalf and Eddy, 1991):
Vm=KgA(C S −C)
where:
Vm=rate of mass transfer Kg=coefficient of diffusion for gas A=area through which gas is diffusing C S =saturation concentration of gas phase in bubble C=initial concentration of gas phase in bubble volume
Table 2 gives Henry's Constants (H c ) for a selected number of organic compounds and the second rate constants (R c ) for the ozone radical rate of reaction. The fourth column presents the product of both H c and R c (RRC) as a ranking of effectiveness. In actual practice diffusion is rate-limiting, resulting in the most effective removal with PCE (tetrachloroethylene).
TABLE 2 REMOVAL RATE COEFFICIENTS FOR THE MICROBUBBLE/OZONE PROCESS - C-SPARGE Ozone K 2 Second order K 1 Rate Organic Rate Constant a Henry's Removal Compound (M −1 SEC −1 ) Constant b Coefficient Benzene 2 5.59 × 10 −3 .0110 Toluene 14 6.37 × 10 −3 .0890 Chlorobenzene 0.75 3.72 × 10 −3 .0028 Trichloroethylene 17 9.10 × 10 −3 .1540 Tetrachloroethylene 0.1 2.59 × 10 −2 .026 Ethanol .02 4.48 × 10 −5 .0000008 R c · H c = RRC a From Hoigne and Bader, 1983 b From EPA 540/1-86/060, Superfund Public Health Evaluation Manual
Elimination of the Need for Vapor Extraction
The need for vapor control exists when vapors of VOC's partitioned from the dissolved form into the microbubbles, reach the unsaturated zone, releasing vapors. Without reaction with a decomposing gas, such as ozone, a large mass can be transmitted in a short time, creating potential health problems near residential basement areas.
The combined extraction/decomposition process has the capacity to eliminate the need for vapor capture. If the ozone-mediated decomposition rate exceeds the vertical time-of-travel, vapors will either not be produced or their concentration will be so low as to eliminate the requirement for capture. By controlling the size of microbubbles and matching them to suitable slow rise times, the need for vapor control is eliminated.
The rise time of bubbles of different sizes was computed for water, producing the upwards gravitational velocity (Table 3). The upwards velocity provides the positive pressure to push the bubbles through the porous media, following Darcy's equation. By determining the rise rate in the field, the rise time, proportional to upwards pressure, can be calculated. The bubble size is very important. Once a bubble exceeds the pore cavity size, it is significantly retarded or trapped. Pulsing of the water phase provides a necessary boost to assure steady upwards migration and reduction of coalescence.
TABLE 3 TIME (MINUTES FOR UPWARD UPWARDS MIGRATION BUBBLE VELOCITY (3 METERS) (Coarse DIAMETER IN WATER Sand and Gravel) 10 mm .25 m/s 19 min 2 mm .16 m/s 30 min .2 mm .018 m/s 240 min
Elimination Rate of PCE Relative to Ozone Content
The reaction of ozone with tetrachloroethene (PCE) will produce degradation products of hydrochloric acid, carbon dioxide, and water. By adjusting the ozone concentration to match the dissolved PCE level, the PCE can be removed rapidly without excess ozone release to the air or release of PCE vapor into the unsaturated zone.
Accordingly, the object and purpose of the present disclosure is to provide microporous diffusers for removal of contaminants from soil and associated subsurface ground water aquifer, without applying a vacuum for extraction or relying on biodegradation processes.
Another object of the present disclosure is to provide multi-gas systems to be used in combination with the microporous diffusers to promote an efficient removal of poorly biodegradable organics, particularly dissolved chlorinated solvents, without vacuum extraction.
A further object of the present disclosure is to provide that remediation occurs by destroying organic and hydrocarbon material in place without release of contaminating vapors to the atmosphere.
The instrumentalities will be described for the purposes of illustration only in connection with certain embodiments; however, it is recognized that those persons skilled in the art may make various changes, modifications, improvements and additions on the illustrated embodiments all without departing from the spirit and scope of the present disclosure.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross sectional schematic illustration of a soil formation showing an apparatus according to an embodiment.
FIG. 2 is an enlarged piping schematic of the apparatus of FIG. 1 showing the unique fine bubble production chamber.
FIG. 3 is an electrical schematic for a three well system (Model 3503 or 3603) of the apparatus of FIG. 1 .
FIG. 4 shows an internal layout of a control module box for a three well system (M-3503 or M-3603) of FIG. 1 .
FIG. 5A shows the geometry of a bottom panel on the control module identifying external connections and ports for three well units (M-3503 & 3603) of the apparatus of FIG. 1 .
FIG. 5B is a left side view of FIG. 5A .
FIG. 6 is a schematic illustration of a soil formation showing the apparatus of FIG. 1 .
FIG. 7 is a perspective view of a bubbler sparge unit for groundwater treatment shown partly in section.
FIG. 8 is a front view of the bubbler sparge unit of FIG. 7 .
FIG. 9 is a top elevational view of the bubbler sparge unit of FIG. 7 .
FIG. 10 is a bottom elevational view of the bubbler sparge unit of FIG. 7 .
FIG. 11 is a front elevational view of the bubbler sparge unit of FIG. 7 ; the broken line shows the bubbler sparge unit in situ for groundwater treatment.
FIG. 12 is an alternate embodiment of a microporous Spargepoint® assembly of the apparatus of FIG. 1 .
FIG. 13 describes Series 3500 & 3600 systems.
DETAILED DESCRIPTION
The present instrumentalities are directed to sparging apparatus for injection of an oxidizing gas in the form of small bubbles into aquifer regions to encourage in situ remediation of subsurface leachate plumes. In particular, microporous diffusers inject multi-gas bubbles into aquifer regions to encourage biodegradation of leachate plumes which contain biodegradable organics, or Criegee decomposition of leachate plumes containing dissolved chlorinated hydrocarbons.
Referring to FIGS. 1 through 6 , there is shown a C-Sparger® System ( 10 ) consisting of multiple microporous diffusers ( 26 ) in combination with an encapsulated multi-gas system, the system ( 10 ) consists of a master unit ( 12 ) and one or more in-well sparging units ( 14 ). Each master unit ( 12 ) can operate up to a total of three wells simultaneously, and treat an area up to 50 feet wide and 100 feet long. Actual performance depends upon site conditions. Vapor capture is not normally necessary.
In an embodiment, as shown in FIG. 1 and FIG. 2 , master unit ( 12 ) consists of the following: a gas generator ( 16 ), a gas feed line ( 15 ), a compressor ( 18 ), a power source ( 19 ), a pump control unit ( 20 ), and a timer ( 2 ). Master unit ( 12 ) must be firmly mounted on 4×4 posts ( 40 ) or a building wall ( 42 ) near in-well sparging units ( 14 ). A heavy-duty power cable ( 44 ), not over 50 feet in length, may be used to run from the power source to master unit ( 12 ).
Referring to FIGS. 1 and 2 , in-well sparging unit ( 14 ) consists of a casing ( 56 ), an inlet screen ( 50 ), an expandable packer ( 52 ), an upper site grout ( 54 ), an outlet screen ( 58 ), and lower grout ( 62 ). Each in-well unit ( 14 ) includes a fixed packer ( 24 ), at least two microporous diffusers ( 26 ), a water pump ( 28 ), ozone line ( 30 ), check valve ( 32 ), and fittings ( 34 ). As shown in FIGS. 1 and 2 , diffuser ( 26 ) employs a microporous diffuser in place of a standard slotted well screen to improve dispersion of bubbles ( 60 ) through soil shown at ( 84 ) and to improve rate of gaseous exchange. A normal 10-slot PVC well screen contains roughly twelve percent (12%) open area. Under pressure most air exits the top slits and radiates outward in a star-like fracture pattern, evidencing fracturing of the formation.
Referring to FIG. 2 there is shown a fine bubble production chamber ( 46 ) positioned in the well casing ( 56 ) between the upper well screen ( 50 ) positioned immediately below fixed packer ( 24 ) consisting of a removable closure plug and the lower plug ( 48 ) consisting of the fine bubble production chamber ( 46 ) containing bubbles ( 60 ) including upper Spargepoint® ( 26 ) positioned above lower well screen ( 58 ) including pump ( 28 ) and check valve ( 32 ). Referring to FIG. 4 there is shown the internal layout of the control module box ( 12 ) including an AC/DC power converter ( 71 ), and ozone generator ( 72 ), well gas relays ( 73 ) (three wells shown), a compressor ( 74 ), a master relay ( 75 ), a main fuse ( 76 ). There is also shown a programmable timer controller ( 77 ), a power strip ( 78 ), a gas regulator and pressure gauge ( 79 ), together with a solenoid manifold ( 80 ), a ground fault interrupter ( 81 ) and a cooling fan ( 82 ).
Spargepoint® diffusers include several unique configurations as follows:
a. A direct substitute for a well screen comprising 30% porosity, 5-50 micron channel size and resistance to flow from 1 to 3 PSI. This configuration can take high volume flow and needs a selective annular pack (sized to formation). The use of high density polyethylene or polypropylene is light-weight, rugged and inexpensive.
b. A microporous diffuser can be placed on the end of a narrow diameter pipe riser KVA 14-291. This reduces the residence time in the riser volume.
c. A shielded microporous diffuser which is injected with a hand-held or hydraulic vibratory hammer. The microporous material is molded around an internal metal (copper) perforated tubing and attached to an anchor which pulls the Spargepoint® out when the protective insertion shaft is retracted. The unit is connected to the surface with 3/16 or ¼ inch polypropylene tubing with a compression fitting.
d. A thin Spargepoint® with molded tubing can be inserted down a narrow shaft for use with push or vibratory tools with detachable points. The shaft is pushed to the depth desired, then the Spargepoint® is inserted, the shaft is pulled upwards, pulling off the detachable drive point and exposing the Spargepoint®.
e. A microporous diffuser/pump combination placed within a well screen in such a manner that bubble production and pumping is sequenced with a delay to allow separation of large bubbles from the desired fine “champagne” bubbles. The pressure from the pump is allowed to offset the formation back pressure to allow injection of the remaining fine bubbles into the formation.
Improvements
In the present apparatuses an improvement comprises several new equipment designs associated with the Spargepoint® diffusers. Most important is the submittal for HDPE porous material with well fittings and pass-through design which allows individual pressure and flow control as shown in FIGS. 7-11 .
Secondly, the push-probe points have been developed for use with pneumatic tools, instead of drilling auger insertion.
Improvements on C-Sparger®/microporous Spargepoint® diffuser. One of the major pass-through Spargepoint® problems in horizontal sparging is the even distribution of air bubbles. If an inlet is attached to the end of a screen, the pressure drops continuously as air is released from the screen. The resulting distribution of flow causes most bubbles to be produced where the connection occurs with flow alternating outwards. The end of the screen produces little or no bubbles.
To allow even distribution of bubbles, either individual Spargepoints® are bundled (spaghetti tube approach) or the Spargepoints® are constructed in a unique way which allows interval tubing connections with flow and pressure control for each Spargepoint® region within the proposed arrangement. Tubing connected to a Spargepoint® passes through the Spargepoint® internally without interfering with the function of producing small bubbles on a smooth external surface. The tubing penetration reduces the internal gas volume of the Spargepoint®, thereby reducing residence time for oxidative gases (important since ozone has a certain half-life before decomposition), and allows three to four Spargepoints® to be operated simultaneously with equal flow and pressure. Each Spargepoint® can also be programmed to pulse on a timed sequencer, saving electrical costs and allowing certain unique vertical and horizontal bubble patterns. Spargepoint® diffusers can be fitted with an F480 thread with internal bypass and compression fittings, FIG. 12 . Some advantages are as follows:
(1) fits standard well screen;
(2) allows individual flow/pressure control;
(3) reduces residence time; and
(4) allows for casing/sparge instead of continuous bubbler.
Use of injectable points configured as molded, 18 Inch×40 inch HDPE molded into ¼ inch pp tubing or HDPE tubing allows a smooth tube to be inserted into a push probe with a detachable point. Use of “Bullet” prepacked Spargepoint® diffusers with a KVA “hefty system” prepacked sand cylinder and bentonite cylinder placed over tubing and porous point is advantageous. Also use of a porous point reinforced with inner metal tube (perforated) to allow strength throughout tubing resists disintegration of plastic during insertion.
Use of pressure/flow headers: Rotameter/mirror: A mirror placed at an angle in a well hole to allow site of a flowmeter reading scale to a point.
It is well recognized that the effectiveness of treatment is dependent upon the uniformity of gas dispersion as it travels through the formation. A porous structure, with appropriate packing, matches the condition of the pores of the soil with thirty percent (30%) pore distribution. The dispersion of bubbles as a fluid can be checked using Darcy's equation.
The use of microporous materials in the Spargepoint® to inject gases into groundwater saturated formations has special advantages for the following reasons:
1. Matching permeability and channel size; 2. Matching porosity; 3. Enhancing fluidity, which can be determined in situ.
The most effective range of pore space for the diffuser material selected depends upon the nature of the unconsolidated formation to be injected. The following serves as a general guide:
1. Porosity of porous material: thirty percent (30%); 2. Pore space: 5-200 microns;
a. 5-20 very fine silty sand; b. 20-50 medium sand; c. 50-200 coarse sand and gravel.
The surrounding sand pack placed between the Spargepoint® and natural material to fill the zone after drilling and excavation should also be compatible in channel size to reduce coalescing of the produced bubbles.
The permeability range for fluid injection function without fracturing would follow:
1. 10 −2 to 10 −6 cm/sec, corresponding to 2 to 2000 Darcy's; or 2. 10 −2 to 10 −6 cm/sec; or 3. 100 to 0.01 ft/day hydraulic conductivity.
Permeability is defined as a measure of the ease of movement of a gas through the soil. The ability of a porous soil to pass any fluid, including gas, depends upon its internal resistance to flow, dictated largely by the forces of attraction, adhesion, cohesion, and viscosity. Because the ratio of surface area to porosity increases as particle size decreases, permeability is often related to particle size see Table 3.
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Apparatuses for removal of volatile organic compounds in a soil formation include a microporous diffuser for injecting air and gaseous ozone as bubbles into water in the soil formation. The gaseous ozone is present at concentrations to effect removal of volatile organic compounds by the gaseous ozone reacting with the volatile organic compound(s). Injection of air and gaseous ozone is controlled by a timer to allow separation of bubbles by size. In various embodiments, a plurality of microporous diffusers may be controlled by a single timer or each of the plurality of microporous diffusers may be controlled by one of a plurality of timers.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of Korean Application No. 2005-99152, filed Oct. 20, 2005, in the Korean Intellectual Property Office, the disclosure of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] Aspects of the present invention relate to a hinge unit and an image forming apparatus having the same. More particularly, aspects of the present invention relate to a hinge unit capable of smoothly operating by applying a resilience that varies according to an open angle of a hinge unit, and an image forming apparatus having a cover connected to a main body of the image forming apparatus by the hinge unit.
[0004] 2. Description of the Related Art
[0005] Generally, image forming apparatuses that include a scanning function, such as, for example, copiers, scanners, and multifunction apparatuses, scan a document and store an image read from the document as data or print out the image on a print medium such as paper.
[0006] FIG. 1 shows a conventional multifunction apparatus as an example of an image forming apparatus. Referring to FIG. 1 , the multifunction apparatus comprises a scan unit 2 formed at a main body 1 thereof to read images from a document placed on the scan unit 2 , a cover 3 covering the document, and a hinge unit 10 connecting the scan unit 2 and the cover 3 . An automatic document feeder (ADF) 4 may be further mounted to the cover 3 to automatically supply a plurality of sheets of the document to the scan unit 2 . In a high-speed multifunction apparatus or copier, a duplex ADF may be mounted to the cover 3 . However, a cover 3 having a duplex ADF is typically so heavy that a user cannot conveniently lift and lower the cover 3 .
[0007] In a general image forming apparatus, the cover is typically able to pivot by approximately 80°. The moment generated by pivoting the cover does not regularly increase according to the open angle of the cover. As the cover is becomes more and more closed, in other words, as the open angle of the cover with respect to a scan unit becomes close to 0°, the moment and resilience for balancing increase. Therefore, it is hard to maintain the moment equilibrium according to the open angle with a typical hinge unit containing only one spring. Although a single spring is generally mounted to the hinge unit, a pair of springs may be mounted in parallel when greater force is required. However, when using one or two parallel springs, the design freedom of the apparatus is poor. An over-spec spring needs to be employed in order to apply spring forces differently according to various opening angles. However, an over-spec spring does not offer the user a good feeling in opening and closing the cover. In order to provide a favorable opening and closing operation of the cover requiring only a minor force when performing scanning or copying work, configuration of the spring of the hinge unit connecting the cover with the scan unit of the main body becomes an essential issue.
[0008] FIG. 2 is a sectional view showing the structure of a hinge unit 10 mounted in the conventional image forming apparatus, as disclosed in Japanese Patent Publication No. 2003-129739. In the hinge unit 10 , two springs 11 and 12 are serially connected.
[0009] Referring to FIG. 2 , the hinge unit 10 comprises a cam base 30 connected to a cover 3 , a plunger 21 received in a hinge housing 20 to move back and forth and having a slanted face 22 , first and second springs 11 and 12 received in the hinge housing 20 and pushing the plunger 21 , and first and second cams 31 and 32 pivoting in association with the cam base 30 and contacting the slanted face 22 . In the above-structured hinge unit 10 , a resistant force as a reaction by the first cam 31 is applied to the slanted face 22 of the plunger 21 in the direction of a common normal of the point of contact with the first cam 31 . Therefore, the resistant force operates as a moment inclining the plunger 21 to the rotational direction (illustrated by an arrow) so that the plunger 21 may swerve from the first cam 31 , thereby increasing the torque in the open direction around a hinge shaft P. Accordingly, enough force can be obtained for popping up the cover 3 , and also for preventing the cam base 30 and the plunger 21 from deforming. However, the hinge unit 10 may become worn along the first and the second cams 31 and 32 and the slanted face 22 of the plunger 21 . The user still has to apply a great force to open and close the cover 3 , especially a heavy cover, and accordingly, the cover 3 cannot be smoothly pivoted.
SUMMARY OF THE INVENTION
[0010] An aspect of the present invention is to solve the above and/or other problems and disadvantages and to provide at least the advantages described below. Accordingly, an aspect of the present invention is to provide a hinge unit enabling a user to smoothly open and close a cover of an image forming apparatus with only a minor force, by applying resilience of different degrees according to an open angle of the cover.
[0011] Another aspect of the present invention is to provide an image forming apparatus having the above-mentioned hinge unit.
[0012] According to an aspect of the present invention, there is provided a hinge unit comprising a lower frame connected to a scan unit of a main body of an image forming apparatus; an upper frame engaged with the lower frame through a hinge shaft and connected to a cover of the image forming apparatus; and first and second resilient members serially arranged within the upper frame, wherein, when the cover pivots toward the scan unit, the first resilient member displaces first and then the second resilient member displaces.
[0013] According to an aspect of the present invention, the upper frame comprises a fixed holder mounted at one end thereof to receive the first resilient member; a first movable holder mounted to be opposed to the fixed holder, receiving the second resilient member, and moving along a length direction of the upper frame; and a second movable holder disposed between the first and the second resilient members to move along the length direction of the upper frame.
[0014] According to an aspect of the present invention, the upper frame comprises a guide rail that guides sliding movement of the first and the second movable holders along the length direction of the upper frame.
[0015] According to an aspect of the present invention, the upper frame further comprises a fixed member that prevents the fixed holder from being pushed outward.
[0016] According to an aspect of the present invention, the lower frame comprises a link fixed in front of the hinge shaft to contact with the first movable holder.
[0017] According to an aspect of the present invention, at least one of the fixed holder and the second movable holder comprises sidewalls on surfaces thereof opposite to each other. The fixed holder may have a sidewall that extends downward, that is, in the direction of the second movable holder. The second movable holder may have a sidewall that extends upward and/or downward, that is, in the direction of the fixed holder and/or in the direction of the first movable member. The total height of the sidewalls of the fixed holder and sidewalls of the second movable holder extending toward the fixed holder is equal to or greater than length of the first resilient member when the first member is completely compressed. In addition, the respective holders may include mounting parts for seating the first and second resilient members therein.
[0018] Preferably, but not necessarily, the first and the second resilient members are springs, and the spring constant K 1 of the first resilient member is smaller than the spring constant K 2 of the second resilient member.
[0019] An image forming apparatus according to another aspect of the present invention may comprise a main body including a scan unit, and a cover connected with a scan unit of the main body by the above-described hinge unit.
[0020] According to another aspect of the present invention, a hinge unit of an image forming apparatus having a cover and a main body with a scan unit, comprises a lower frame connected to a scan unit of a main body of an image forming apparatus; an upper frame engaged with the lower frame through a hinge shaft and connected to a cover of the image forming apparatus; and a plurality of resilient members serially arranged within the upper frame, wherein an overall resilience of the hinge unit is controlled by selecting a resilience of individual resilient members of the plurality of serially arranged resilient members.
[0021] According to another aspect of the present invention, an apparatus has a main body and a cover, wherein the cover is connected with the main body through a hinge unit, wherein the hinge unit comprises, a lower frame connected to the main body; an upper frame engaged with the lower frame through a hinge shaft and connected to the cover, and first and second resilient members serially arranged within the upper frame, wherein the first resilient member displaces before the second resilient member when the cover pivots toward the scan unit.
[0022] Additional aspects and/or advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] These and/or other aspects and advantages of the invention will become apparent and more readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
[0024] FIG. 1 is an exterior view of a conventional multifunction apparatus;
[0025] FIG. 2 is a sectional view showing the structure of a conventional hinge unit;
[0026] FIG. 3 is a perspective view showing the hinge unit as assembled;
[0027] FIG. 4 is an exploded perspective view of FIG. 3 ;
[0028] FIG. 5 is a longitudinal-sectional view of FIG. 3 ;
[0029] FIG. 6 is a front view showing the detailed structure of resilient members of FIG. 3 ;
[0030] FIG. 7 is a view showing the structure of a hinge unit according to another embodiment of the present invention;
[0031] FIGS. 8A through 8D are views showing the operation of the hinge unit of FIG. 7 ; and
[0032] FIG. 9 is a graph illustrating relationships between loads and open angles of the cover with respect to the hinge unit.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0033] Reference will now be made in detail to the present embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the like elements throughout. The embodiments are described below in order to explain the present invention by referring to the figures. Well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail.
[0034] FIGS. 3 through 6 are an assembled view, an exploded perspective view, a longitudinal-sectional view, and a front view, respectively, for showing a hinge unit according to an embodiment of the present invention. Referring to the drawings, the hinge unit 100 comprises a lower frame 110 , and an upper frame 120 connected to the lower frame 110 through a hinge shaft P.
[0035] The hinge unit may connect a cover of an image forming device with the scan unit of the main body of an image forming device. Aspects of the image forming device may be the same as those shown in FIG. 1 , with respect to the main body 1 , the scanning unit 2 , the cover 3 and optional automatic document feeder 4 , except that the hinge unit according to embodiments of the present invention described herein replaces the conventional hinge unit 10 shown in FIGS. 1 and 2 . The lower frame 110 of the hinge 100 is connected to a scan unit 2 mounted to a main body 1 ( FIG. 1 ) of an image forming apparatus. The lower frame 110 may comprise a fastening hole 114 a on a bottom surface 114 thereof, to be connected with the scan unit 2 by a fastening member (not shown). The hinge shaft P is mounted to the lower frame 110 through a shaft hole formed in front of the hinge shaft P. In other words, the link 112 is placed so that it is offset from the hinge shaft P within the angle of rotation of the hinge 100 . The hinge shaft P and the link 112 may be formed as cylindrical bars. The link 112 , contacts and engages with a first movable holder 121 of the upper frame 120 .
[0036] The upper frame 120 is connected to the cover 3 ( FIG. 1 ) of the image forming apparatus and coupled with the lower frame 110 by the hinge shaft P passing through a connection hole 120 a formed at one side thereof. The upper frame 120 may be fixedly mounted to the cover 3 through a connection member 125 .
[0037] The upper frame 120 comprises first and second resilient members 131 and 132 that are serially arranged. Although the number of the resilient member is not limited, it is preferable to serially arrange two resilient members 131 and 132 .
[0038] The upper frame 120 has a fixed holder 123 formed at an upper side and a first movable holder 121 formed at a lower side opposite to the fixed holder 123 . As used herein, the term “lower side” of the upper frame 120 refers to the portion of the frame that is adjacent to the hinge shaft P and the term “upper side” of the upper frame 120 refers to the opposite portion of the upper frame 120 , that is, the portion that is farthest away from the hinge shaft P. The fixed holder 123 supports the first resilient member 131 so that the first resilient member 131 is not pushed out of the upper frame 120 . In addition, fixed members 126 a and 126 b may be provided to the upper frame 120 or the connection member 125 in order to prevent the fixed holder 123 from being pushed out of the upper frame 120 . Alternatively, the fixed holder 123 may be attached directly to the upper frame 120 or to the connection member 125 .
[0039] The first and the second resilient members 131 and 132 are serially arranged between the fixed holder 123 and the first movable holder 121 . Preferably, but not necessarily, the first movable holder 121 has a mounting part 121 e constructed by sidewalls of a bottom portion thereof to receive therein an end of the second resilient member 132 . Therefore, the second resilient member 132 can be stably received in the first movable holder 121 by the mounting part 121 e of the first movable holder 121 . The fixed holder 123 may also have such a mounting part.
[0040] In addition, a second movable holder 122 is formed between the first and the second resilient members 131 and 132 .
[0041] The upper frame 120 may include guide rails 124 a and 124 b at both flanks along a length direction thereof that allow the first and the second movable holders 121 and 122 to slide in the length direction. The first and the second movable holders 121 and 122 comprise first guide grooves 121 a and 121 b and second guide grooves 122 a and 122 b, respectively, that allow the first and the second movable holders 121 and 122 to smoothly slide along the guide rails 124 a and 124 b.
[0042] In the hinge unit 100 of this embodiment, springs are employed for the first and the second resilient members 131 and 132 . According to this embodiment, it is preferred that a spring constant K 1 of the first resilient member 131 is less than a spring constant K 2 of the second resilient member 132 so that the first resilient member 131 operates first and the second resilient member 132 operates next.
[0043] To ensure the orderly operation of the first and the second resilient members 131 and 132 , and to prevent the resilient members from popping out of the upper frame 120 , the fixed holder, and first and second movable holders may further include sidewalls. Holders having sidewalls are shown as the first movable holder 221 , second movable holder, 222 and fixed holder 223 in the embodiment shown in FIG. 7 . In the embodiment shown in FIG. 7 , the other structures are the same as those of the hinge unit 100 of FIG. 3 except that the holders 221 to 223 include sidewalls, respectively. For convenient explanation, only the holders 221 to 223 and the resilient members 131 and 132 are illustrated in FIG. 7 .
[0044] In the hinge unit 200 according to the embodiment of FIG. 7 , one or both of the second movable holder 221 and the fixed holder 223 may comprise sidewalls on surfaces thereof opposite to each other. As shown in FIG. 7 , sidewalls 222 c and 223 c may be formed on circumferences or perimeters of both the second movable holder 222 and the fixed holder 223 to be opposed to each other. Preferably, a total height of the fixed holder sidewall 223 c and the movable holder sidewall 222 c is equal to or greater than a height of the first resilient member when the first resilient member 131 is completely compressed, so that the operation of the first resilient member 131 is followed by that of the second resilient member 132 . More particularly, when the first resilient member 131 is compressed, the movable holder sidewall 222 c and the fixed holder sidewall 223 c come into contact with each other, thereby restraining the operation of the first resilient member 131 and promoting the operation of the second resilient member 132 .
[0045] Sidewalls 221 c to 223 c of the respective holders 221 to 223 comprise mounting parts 221 e to 223 e, respectively, to stably receive the resilient members 131 and 132 . The second movable holder 222 may further comprise another sidewall 222 ' c formed on a lower part thereof.
[0046] The above-structured hinge unit is applicable to various devices mounting a cover, such as the image forming apparatus having the cover 3 hingedly connected to the main body 1 comprising the scan unit 2 and to the scan unit 2 of the main body 1 . Especially, the hinge unit according to embodiments of the present invention may be used for an image forming apparatus having a relatively heavy cover mounting an automatic document feeder (ADF) 4 ( FIG. 1 ) thereon. The hinge unit may be used with other apparatuses having a heavy cover, such as, for example, a chest freezer.
[0047] Hereinbelow, the operations and effects of the hinge unit according to embodiments of the present invention will be described with reference to the accompanying drawings.
[0048] FIGS. 8A through 8D show the operation of the hinge unit applied to the image forming apparatus according to the embodiment of FIG. 7 . For convenient explanation, only the holders 221 to 223 and the two springs 131 and 132 are illustrated. It is to be understood that the upper frame 120 of the hinge unit 200 is fixed to the cover of the image forming apparatus, and the lower frame 110 is fixed to the scan unit of the main body and that the remaining features of the hinge unit 200 may be as shown, for example, in FIGS. 3-5 . Moreover, it is to be understood that aspects of the image forming device may be the same as those shown in FIG. 1 , with respect to the main body 1 and the cover 3 , except that the hinge unit according to FIGS. 3-8 replaces the conventional hinge unit 10 shown in FIGS. 1 and 2 .
[0049] Generally, the cover 3 of the image forming apparatus is opened and closed pivoting by approximately 80°. The moment generated by pivot of the cover 3 is not regularly increased according to an open angle of the cover 3 . As the cover 3 is being closed, in other words, as the open angle of the cover 3 with respect to a scan unit is becoming 0°, the moment and resilience for balancing increase. In the hinge unit of FIG. 8 , the two springs 131 and 132 are arranged in a serial manner so as to balance the moment according to the open angle of the cover 3 .
[0050] Presuming that ‘K1’ denotes a spring constant of the first spring 131 and ‘K2’ denotes a spring constant of the second spring 132 , the springs wherein K 1 is smaller than K 2 are used so that the first spring 131 is displaced ahead of the second spring.
[0051] In FIG. 8A , the state is shown in which the cover 3 is completely open so that no force is applied to the movable holders 221 and 222 . When the cover 3 begins to be closed, the second movable holder 222 and the fixed holder 223 are pushed in an angular direction by the rotation of the upper frame 120 about the hinge shaft P. The cover 3 begins to generate a large moment with respect to the hinge shaft P due to its own weight. Correspondingly, resilience is generated by the link 112 ( FIG. 3 ). The link 112 restrains the movement of the first movable holder 221 in the angular direction, thereby hindering closing of the cover and pushes the first movable holder 221 in the direction of the fixed member 223 . Since the spring constant K 1 of the first spring 131 is smaller than the spring constant K 2 of the second spring 132 , the second movable holder is also pushed in the direction of the fixed member 223 . The second spring 132 remains uncompressed while the first spring begins to be compressed, as shown in FIG. 8B . Since the springs 131 and 132 are serially arranged, the total spring constant in the state of FIG. 8B can be expressed as (K tot )=(K1×K2)/(K1+K2).
[0052] When the cover 3 is closed by more than a predetermined angle, the first spring 131 becomes compressed completely, and the fixed holder sidewall 223 c and the movable holder sidewall 222 c are brought into contact with each other, as shown in FIGS. 8C and 8D . As a result, the first spring 131 cannot compress any more and only the second spring 132 can generate resilience. The total spring constant (K tot ) in the state of FIG. 8D is equal to K 1 .
[0053] As described above, in the operation of the hinge unit according to aspects of the present invention, the first spring 131 is operated when the open angle of the cover is more than a predetermined angle and then the second spring 132 is operated when the open angle is less than the predetermined angle. Accordingly, the moment caused by the weight of the cover 3 can be properly offset. The resilience of the hinge unit is illustrated in FIG. 9 according to the open angle of the cover 3 .
[0054] FIG. 9 is a graph for showing the relationships between loads and the open angles of the cover with respect to the hinge unit wherein the two springs are serially arranged. As shown in FIG. 9 , when a pivoting angle of the cover is relatively large, for example, at the beginning of closing the cover, a minor force needs to be applied to the cover. However, when the pivoting angle of the cover is relatively small, for example, when the cover is almost closed, a greater force should be applied to the cover.
[0055] Therefore, according to embodiments of the present invention, since the spring constants of the resilient members of the hinge unit are properly applied, the cover can be prevented from closing spontaneously or from slamming down too hard when it is closed. Also, the user can comfortably open and close the cover during scanning and copying of works.
[0056] As can be appreciated from the hinge unit according to embodiments of the present invention, extent of resilience of the resilient members can be controlled according to the open angle of the cover by serially connecting a plurality of the resilient members, thereby properly offsetting the moment by the weight of the cover. In addition, the feeling to the user when opening and closing the cover is improved.
[0057] Although a few embodiments of the present invention have been shown and described, it would be appreciated by those skilled in the art that changes may be made in this embodiment without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents. For example, a plurality of other resilient members may be applied instead of the first and the second resilient members between the fixed holder and the first movable holder. Furthermore, more movable holders may be added in order to securely mount the plurality of resilient members. Therefore, technical protection range of the invention should be defined by the appended claims.
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A hinge unit applies resilience differently according to the angle at which the hinge unit is opened, and an image forming apparatus has a cover attached by the hinge unit. The hinge unit includes a lower frame connected to a scan unit of a main body of an apparatus; an upper frame engaged with the lower frame through a hinge shaft and connected to a cover; and first and second resilient members serially arranged within the upper frame. When the cover pivots toward the scan unit at less than a predetermined angle, the hinge unit provides relatively minor resistance, whereas when the cover pivots toward the scan unit at the predetermined angle or greater, the hinge unit provides relatively greater resistance, thereby appropriately coping with the moment by weight of the cover. As a result, the improved hinge unit may enable a user to open and close the cover more comfortably.
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This application is a continuation of Ser. No. 705,135 filed 07/14/1976 now abandoned.
BACKGROUND OF THE INVENTION
In the field of furniture construction, there is a continuing need for devices with which springs may be attached to the wooden framework of chairs, couches and other pieces of furniture. In the past, various clip-like devices have been used, generally comprising a bent portion with which to engage the spring and the remaining portion with which to provide a base for attaching the clip to the framework. In most cases, the base was perforated with one or more holes through which securing means such as nails, screws or staples were passed for fastening to the frame.
More recently, improved clip designs have been provided which eliminate the need for the additional hardware, i.e. the nails, screws or staples by incorporating in the body of the clip its own means for being secured to the frame. Such a clip is described in U.S. Pat. No. 3,720,960 by J. J. Bond. Bond's clip utilizes a pair of sharp prongs formed at the end opposite the spring attachment end, the prongs being adapted to be driven into the wooden frame.
By eliminating the need for the additional hardware, the clip provided by Bond is an improvement over the prior art materially reducing the difficulty and the time required for attaching the clip to the frame.
While the clip provided by Bond comprised a substantial improvement over the prior art since it can not be pulled out of the furniture frame while in use and carries its own means for being secured to the frame also incorporating an integral means for noise reduction it does not lend itself to multiple formation in strips from which individual clips may be separated and secured by automatic means.
SUMMARY OF THE INVENTION
In accordance with the invention claimed, an improved clip is provided for the attachment of springs to the framework of furniture, the clip comprising a one-piece device specially configured to facilitate the automatic attachment of the clips to furniture frames. The clip requires no auxilliary hardware such as nails, screws or staples for attachment to the frame and means are integrally incorporated to reduce or eliminate audible noise due to the relative motion of the springs relative to the clips which may be selectively applied to strategic areas only for cost reduction purposes.
It is, therefore, one object of the present invention to provide an improved clip for the attachment of springs to the framework of furniture.
Another object of this invention is to provide such a clip which requires no auxiliary hardware for the attachment to the furniture frame.
A further object of this invention is to provide such a clip in a one-piece configuration while incorporating means for substantially reducing or eliminating audible noise as ordinarily produced by the working of the spring against the clip and in strategic areas only for cost reduction purposes.
A still further object of this invention is to provide such a clip in a configuration which is amenable to fabrication in large quantities at low cost in a punch press operation.
A still further object of this invention is to provide such a clip configuration which lends itself to the production of large numbers of such clips joined together in continuous strips which may be readily separated and secured to the furniture frame by automatic equipment.
A still further object of this invention is to provide such a clip in a form which will remain firmly anchored to the frame and which will sustain a firm grip on the attached spring throughout the normal life of the furniture in which it is installed.
A still further object of this invention is to provide such a clip which incorporates a sound deadening means which has improved durability relative to similar means provided in the past.
Yet another object of this invention is to provide the spring engaging end of the clip with ridges along its edges to reinforce these edges to remain firm under spring tension thereby avoiding the necessity of stapling them closed.
Further objects and advantages of the invention will become apparent as the following description proceeds and the features of novelty which characterize this invention will be pointed out with particularity in the claims annexed to and forming a part of this specification.
BRIEF DESCRIPTION OF THE DRAWING
The present invention may be more readily described by reference to the accompanying drawing, in which:
FIG. 1 is a perspective view of a spring clip of this invention;
FIG. 2 is a perspective view of the clip of the invention as viewed from a different angle;
FIG. 3 is a perspective view of a number of the clips of the invention joined by interconnecting fragile webs into a continuous strip of clips;
FIG. 4 is a simplified representation of such a strip of clips formed into a coil or roll from which it may be unwound as it is fed into an automatic machine for attachment to a furniture frame member;
FIG. 5 is an enlarged view of segment 5 of FIG. 4 showing a more detailed plan view of a section of the coiled strip of clips;
FIG. 6 is an enlargement of segment 6 of FIG. 5 showing details of the web joining adjacent clips in the strip of FIGS. 3-5;
FIG. 7 is a perspective view showing the clips of the invention secured to a furniture frame member;
FIG. 8 is a perspective view of an automatic machine and associated fixtures arranged for the automatic securing of the clips to furniture frame members, the clips being dispensed from a coil of clips as defined by FIGS. 3-6;
FIG. 9 is a perspective view of a working member of the automatic machine included in the arrangement of FIG. 8;
FIG. 10 is a plan view of the working member of FIG. 9 shown in operation with motion indicated relative to a stationary furniture frame member;
FIG. 11 is an enlarged perspective view of an automatic hand held device for securing the clips of the invention to a furniture frame member, the device dispensing clips from a continuous strip of clips as shown in FIG. 3.
FIG. 12 is a perspective view of a modification of the spring clip shown in FIGS. 1-6;
FIG. 13 is a cross-sectional view of a modification of the non-metallic liner shown in FIGS. 1 and 2';
FIG. 14 is a partial perspective view of a modification of the spring clips shown in FIGS. 1, 2 and 12 with the liner shown in FIG. 13 held in place by punch-out fingers of the spring clip;
FIG. 15 is a cross-sectional view of a clip showing a modified way of anchoring the clip insert to the clip U-shaped spring engaging end;
FIG. 16 is a cross-sectional view of FIG. 15 taken along the lines 16--16; and
FIG. 17 is a perspective view of a further modification of the spring clips of this invention formed to provide an additional resiliency when used in the supporting frame of cushion held furniture.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring more particularly to the drawing by characters of reference, FIGS. 1 and 2 disclose a spring clip 10 of this invention which is formed from a piece of sheet metal such as steel having one end 11 bent over on itself into a U-shaped configuration. The U-shaped end 11 is designed with a radius such that it will receive a spring of the type commonly employed as a resilient support in furniture such as chairs, sofas or the like, the spring usually having a circular cross-sectional configuration. The remaining portion of the sheet metal is bent 90 degrees at two points 12 and 13 so that it too forms a U-shaped portion having square corners whereby the overall configuration of clip 10 may be thought of as representing in profile an S-shaped device. An outer table having one or more legs 14 of the square-shaped U may be pointed or notched as shown. In operation base 15, defined as that portion of clip 10 comprising the common leg to both U-shaped portions and also defined as that portion generally aligned with the force exerted by the spring it is intended to secure, is also aligned with a top horizontal surface 16 of a furniture frame member 17 to which it is attached. Side 18 of member 17 is oriented to the outside of the furniture frame. The outside leg 14 is driven by an impact tool into frame member 17 until base 19 of the square U-shaped configuration of the clip is in contacting relationship with side 18 of member 17 to act as a flange with respect to base portion 15. Clip 10 is thus firmly attached to frame member 17 by its two contacting sides 15 and 19 and by the third embedded side 14. The disclosed clip is so designed that it cannot be pulled out of the frame.
In terms of the features described thus far, clip 10 is similar to the Bond clip of U.S. Pat. No. 3,720,960. The incorporation of certain relatively subtle modifications yet to be described, however, provides important enhancements which constitute the subject matter of the present invention.
The U-shaped end 11 of clip 10 is modified in two ways to reduce audible noise produced by the working action between clip 10 and an attached spring. A non-metallic liner 21 covers the inside surface of U-shaped end 11 with liner 21 serving as a resilient interface between clip 10 and the attached spring. In addition, to prevent the abrasive action of the attached spring from cutting through liner 21 at the edges of clip 10, the edges 22 are bevelled outwardly the entire length of the U-shaped configuration to form a ribbed surface. The rib on the ridge reinforces the clip edges to prevent spring pressure from opening up the U-shaped configuration. This is in contrast to prior art practice which only provided a bevel along the base of the U and permitted wear and eventual noise as the spring later rubbed directly against the metal at the sides of the U-shaped configuration.
Two other features of the configuration of clip 10 are non-functional in its end use, but they are involved in another important feature of the invention having to do with its fabrication and its automatic installation into a wooden frame member.
The first additional feature is a hole 23 in the center of side 19 which serves as a locator or registration hole for the fabrication of clip 10 in an automatic punch press. The hole 23 also may have utility in the proper positioning of clip 10 in an automatic installation device to be described later.
The second and more significant feature involves four tabs 24, two of which are located on each of the outer edges of side 19. The tabs 24 are vestiges of the original fabricated form of clip 10. As illustrated most clearly in FIG. 3, clips 10 are mass-produced in a continuous strip 25. To those skilled in the art of punch press operation, it will be apparent that strip 25 may be readily produced by an automatic punch press. The individual clips 10 in strip 25 are held together by narrow webs 26. When the clips are later separated by an automatic device which also secures the clips in a wooden frame, the remnants of web 26 at each clip become tabs 24 of FIGS. 1 and 2.
The flexibility of strip 25 at web 26 permits the strip to be coiled into a roll 27 as shown in FIG. 4. For clarification of the axis about which the flexing occurs, an enlargement of section 5 of FIG. 4 is shown as FIG. 5. FIG. 5 is recognized as a top plan view of strip 25 from which it is apparent that the deformation is limited by web 26. Further enlargement of the web area defined as segment 6 of FIG. 5 is shown as FIG. 6 where a small wedge 28 is seen to be cut into the center of web 26 to promote bending at the desired point. Wedge 28 also facilitates the cutting operation to be performed by the automatic device yet to be described.
The adaptability of clip 10 as fabricated in the form of strip 25 and coiled into a roll 27 is illustrated in FIG. 8, FIG. 8 showing an automated assembly station 29 in which the clips 10 are attached to wooden frame members 17 by a suitable driver 32. Driver 32 and a circular cartridge 33 which holds the coiled strip 25 are mounted on a frame 34 resembling a horizontal ladder supported by vertical legs 35. The wooden frame members 17 are carried along one edge of frame 34 by a conveyor means 36 and are prevented from falling over the edge by a rail 37, shown as an example, running along the edge of frame 34 just outboard of conveyor means 36.
Driver 32 is mounted on a plate 38 spanning the two opposite side rails of frame 34 with hammerhead 39 of the driver directed toward the inboard edge of the passing frame member 17.
Cartridge 33 lies horizontally across frame 34 in a position such that as strip 25 of clips 10 is unreeled the clips are appropriately aligned with the edge of frame member 17 so that a blow from the hammerhead 39 will sever the end clip 10 from the strip and drive the pointed outer leg of clip 10 into the bottom of the inboard edge of frame member 17. As clip 10 moves into position directly in front of driver 32, end 11 of clip 10 rides over the top surface of frame member 17. Strip 25 is guided to this position by a fixed rail obscured from view in FIG. 8 and running parallel to frame member 17 along its inboard edge, the rail assuring clearance between the pointed end 14 of clip 10 and frame member 17.
Driver 32, as illustrated in FIG. 8, and in part in FIGS. 9 and 10, comprises a compressed air cylinder 41 with a compressed air delivery line 42, a fixed ram chamber 43 and hammerhead 39. Hammerhead 39 has a rectangular cross-section which mates snugly with a rectangular opening through chamber 43, the opening through chamber 43 being in direct communication with the inside of air cylinder 41 so that as air pressure inside cylinder 41 is abruptly raised hammerhead 39 is driven sharply outward as indicated by the broken line position shown in FIG. 10. As the air pressure is reduced, hammerhead 39 is returned either by spring action or by a suitable pressure applied inside of cylinder 41.
Working in cooperation with driver 32 to sever clip 10 from strip 25 and to secure it to frame member 17 is a heavy metal anvil 45 which backs up the guide rail 37 opposite driver 32 and the obscured fixed rail that guides strip 25 into position. The end of this fixed rail has a shearing edge aligned with one of the sharpened projecting edges 44 of hammerhead 39, the aligned shearing edge being positioned just behind clip 10 so that as hammerhead 39 is driven forward, its edge 44 strikes wedge 28 in web 26 which secures clip 10 to strip 25. Edge 44 in cooperation with the aligned shearing edge of the obscured guide rail severs clip 10 from strip 25 and carries it forward toward frame member 17 so that the pointed ends 14 are driven firmly into the wooden frame member 17 until clip 10 comes to rest secured in the position shown in FIG. 7. Thus, the clip is firmly attached to the frame without chance of being pulled out or worked loose.
When clip 10 has been thus secured, the frame members 17 are advanced to the left as indicated by the arrows in FIG. 8. The length of travel for each advancement of members 17 is of course equal to the spacing 46 between the attached clips 10'.
Thus, it has been shown that a relatively simple arrangement may be contrived for a completely automatic operation in which clips 10 are dispensed in the form of a coiled strip 25 from a cartridge 33 and secured to frame members 17. Expensive manual operations are thus eliminated and furniture of better quality can be made available to the consumer at reduced cost.
Where such a totally automatic system is not practical or warranted, a semi-automatic attachment means may be employed. As suggested by FIG. 11, a hand-held pneumatic gun 47 may be adapted to carry a strip 25 of clips 10 on a spring-fed carrier 48.
Gun 47 has an air cylinder 50, a pistol grip handle 51, a trigger 52, a ram chamber 53, a compressed air delivery line 54 and a concealed hammerhead. The ram chamber 53 is slotted to the contour of clip 10 so that the clip may be moved into position therein prior to the severing and driving operation.
In the use of gun 47, the forward end of ram 53 with a clip 10 appropriately positioned therein is held against the edge of wooden frame member 17. Trigger 52 is then pulled, admitting air under pressure to chamber 53 thereby driving the concealed hammerhead forward severing the end clip and driving it into frame member 17. The trigger 52 is then released, air pressure inside chamber 53 falls to atmospheric and the hammerhead is returned by spring action. As the hammerhead returns rearward, the next clip 10 is moved into position inside the slotted end of chamber 53 in preparation for the ensuing operation.
The improved clip 10 and its fabrication in strip form are thus seen to have enhanced utility both in the end use of the clip and through the assembly operation by automatic or semi-automatic means.
FIG. 15 illustrates a modification of the clip shown in FIGS. 1 and 2 wherein clip 57 is similar to clip 10 and contains the same reference characters for like parts thereof but differs primarily in the width of the clip at the spring engaging U-shaped end 11'. The reason for this modification is to adapt the clip for easy assembly with different types of springs.
FIG. 13 discloses a cross-sectional view of a liner 58 which may be formed of a plastic such as, for example, polyethylene, extruded with the cross section as shown in FIG. 13. Such an extrusion of, for example, 10,000 feet, rolled on a reel may be fed into a special arrangement in a die where it could be crimped onto a clip formed as shown in FIG. 14.
The clip 60, only a part of which is shown in FIG. 14, comprises at its spring-engaging end 61 one or more tabs or fingers such as fingers 62, 62A punched out of their end of the clip which are arranged to hold the liner 58 in place in end 61 of the clip.
The internal shape of the extrusion is rounded out at 63 to permit a round wire of an engaging or mating spring (not shown) to slide through the tapered legs 64, 64A of liner 58 and be retained therein by U-shaped end 61 of the clip 60 and to keep it in there, i.e. locked therein, so that it can not snap back out of these tapered legs when the clip is in actual use.
The use of such an extrusion is less costly, uniformly more consistent and can be assembled at a faster rate of speed than the prior art use of tape pressure fitted on the clip. Further, the wear resistance of the extruded surface of the liner inside of the U-shaped clip is superior to the wear resistance of tape and other known noise control means used on furniture clips.
It should be noted that in place of the liner being extruded and then placed in the U-shaped end of the clip, the plastic material in this U-shaped end of the clip may be molded therein, one example of which is shown in FIGS. 16 and 17, by the clip cross-sectional view of a clip configuration 63. This could involve a multi-piece mold (not shown) which would surround the clip with molten polythylene 64 forced through appropriate openings in the mold into areas of the clip wherein the extruded liner is shown in FIG. 14. This procedure could save manufacturing costs over the extruded liner of FIGS. 13 and 14.
As shown in FIG. 15, the clip may be provided with an aperture 65 through which the polyethylene 64 may be extruded to form a locking plug 66 for holding the liner in place in the clip.
FIG. 17 illustrates a further modification of the spring clip disclosed in FIGS. 1, 2, 12 and 13 wherein a spring clip 67 is shown comprising a clip configuration similar to that shown in FIGS. 1 and 2. Like reference characters are used for like parts; however, the structure differs in end 11" having its leg 68 being curved back on itself and again bent back on itself at 69 to form a further extension 70 of leg 68 for a given distance. A further U-shaped configuration 71 is formed with a continuing leg 72 thereof extending to a point where leg 72 terminates in a U-shaped channel configuration 73, the outer edge 74 of which lies above surface 19 in substantially the same plane therewith.
This structure is intended to have its legs 14 clamped onto a furniture rail member in the same way as heretofore described with the remaining ribbon-like spring configuration positioned thereabove. When a number of these spring clips are spacedly mounted along a rail the opposite channel-like ends 73 are loosely interconnected by a wire or cord extending longitudinally of the rail member to which the legs 14 are attached and along the length of each channel configuration 73.
Thus, if a chair or couch cushion support was formed by internal structure comprising a plurality of clips 65 extending along a rail, the upper leg 70 of clip 65 and the cord extending along channel configuration 71 thereof the clips could form a soft top and front edge of the box cushion support in a manner understandable by people skilled in the art.
Although but a few embodiments of the invention have been illustrated and described, it will be apparent to those skilled in the art that various changes and modifications may be made therein without departing from the spirit of the invention or from the scope of the appended claims.
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A spring attachment clip for the fastening of springs to furniture frames, the clip carrying its own means for being secured to the frame and having in addition means for reducing or eliminating audible noise as ordinarily caused by the action of the spring working against the clip. The clip configuration is adapted to permit its multiple formation in long strips intended to be fed into an automatic device which separates the individual clips from the strips and secures them to the frame. Additionally, the U-shaped edges of the spring engaging end of the clips are bevelled outward to strengthen the clip rendering it unnecessary to close the clip to prevent its opening under spring tension.
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BACKGROUND OF THE INVENTION
Field of the Invention
[0001] The invention relates to a device for guiding signatures, particularly in the region of a wedge-shaped outlet of a cutting-cylinder device in a folder of a rotary printing machine.
[0002] Folders of rotary printing machines, particularly of web-fed rotary offset printing machines, are beset by a problem that, after a longitudinal folding operation on a continuous paper web, signatures severed therefrom by revolving cutting blades do not undergo any defined guidance during and after the cutting operation. This may result in disruptions during the subsequent transportation of the signatures, if the latter enter, for example, onto endless transporting belts arranged downline in the cutting-cylinder arrangement, above and below the transporting path of the signatures, in order for the latter to be fed to a further-processing device, in particular a folder.
[0003] One of the most common causes of disruption occurring as the signatures enter onto the downline transporting belts is that the leading corners of the signatures fold over and form so-called “dog ears” as the signatures enter onto the transporting belts. This results not only in the printed products being unusable as such, and having to be separated out in corresponding downline devices, for example, in reject or waste paper diverters, but rather also, there arises a risk that the damaged signatures, during subsequent folding operations, result in a paper build-up which may frequently be associated with production failures or even damage to the folder.
[0004] It has become known heretofore from U.S. Pat. No. 4,385,537, to provide, in the region of the wedge-shaped outlet of a cutting-cylinder arrangement, an upper and a lower transporting belt which are guided, respectively, over a deflecting roller which is displaceable within the wedge-shaped outlet. This U.S. patent offers no indication or suggestion of providing, in the region of the wedge-shaped outlet of the cutting-cylinder arrangement, any further guide devices which avoid the situation wherein the leading corners of the signatures fold or crease over as the signatures enter onto the transporting belt.
[0005] The published German Non-prosecuted Patent Application (DE-OS) 27 43 801 A1 describes a rotary cross cutter in which there is provided in the region of the wedge-shaped outlet, between the two cutting cylinders, a table which extends over the entire width of the cutting cylinders and is accommodated on a resiliently elastic mounting support which is displaceable in the transporting direction of the signatures. The resiliently elastic mounting support is provided so as to ensure that a signature build-up in the region of the wedge-shaped outlet does not result in damage to the table or to the transporting belts arranged downline from the table, above and below the transporting path of the signatures. Despite the high-outlay resiliently elastic mounting support of the table, the leading ends of the signatures are not prevented by the table from folding over as the signatures enter into the downline transporting belts.
SUMMARY OF THE INVENTION
[0006] Accordingly, it is an object of the invention of the instant application to provide a device for guiding signatures in the region of a web-shaped outlet of a cutting-cylinder device in a folder of a rotary printing machine, which is of straightforward and cost-effective construction, in case of a paper buildup, is not prone to damage, or in the case of damage can be replaced cost-effectively, and allows the signatures to be guided reliably in a downline transporting device.
[0007] With the foregoing and other objects in view, there is provided, in accordance with the invention, a device for guiding signatures, in a folder of a rotary printing machine, comprising at least one guide belt disposed near a transporting path of the signatures, and extending transversely to a transporting direction of the signatures, the at least one guide belt being formed with guide surfaces defining the transporting path.
[0008] In accordance with another feature of the invention, the signature-guiding device is in combination with a cutting-cylinder device having a wedge-shaped outlet within a region of which, the signature-guiding device is disposed.
[0009] In accordance with a further feature of the invention, the at least one guide belt is an endless guide belt extending over two first and second deflecting rollers arranged on mutually opposite sides of the signature-guiding device, so that the guide surfaces are formed by respective mutually opposite inner sides of the endless guide belt, between which the signatures run through the signature-guiding device.
[0010] In accordance with an added feature of the invention, the signature-guiding device includes at least another guide belt, the one and the other guide belts being arranged on mutually opposite sides of the transporting path of the signatures so that respective outer sides of the one and the other guide belts form the guide surfaces.
[0011] In accordance with an additional feature of the invention, the guide surfaces face towards the signatures, and are disposed at an angle to the transporting path of the signatures, so as to produce a funnel-like inlet region into which the signatures enter by leading edges thereof.
[0012] In accordance with yet another feature of the invention, the angle between at least one of the one and the other guide belt, on the one hand, and the transporting path of the signatures, on the other hand, is variable.
[0013] In accordance with yet a further feature of the invention, the at least one guide belt is disposed in a region between a cutting-cylinder pair and a transporting-belt device located downline therefrom, as viewed in the transporting direction of the signatures, in a folder of a web-fed rotary printing machine.
[0014] In accordance with yet an added feature of the invention, the signature-guiding device includes at least another guide belt, each of the guide belts having a tensioning device assigned thereto.
[0015] In accordance with yet an additional feature of the invention, the tensioning device includes a lever arm, an actuating device for pivoting the lever arm about a pivot pin, and a deflecting roller whereover a respective guide belt extends, the deflecting roller being rotatably secured on the lever arm.
[0016] In accordance with still another feature of the invention, the actuating device includes a spring for acting on the lever arm, and a cam assigned to the lever arm, the spring and the cam cooperating with one another so that, by rotation of the cam, the lever arm is movable from a first and tensioning position into a second position, wherein the respective guide belt is not tensioned.
[0017] In accordance with still a further feature of the invention, the actuating device for acting on the lever arm is at least one of a pneumatic cylinder and an electrical actuator, respectively, by which the lever arm is pivotable from a first and tensioning position into a second position, wherein the guide belt is not tensioned.
[0018] In accordance with still an added feature of the invention, the distance between the guide belts, on the one hand, and the transporting path of the signatures, on the other hand, is variable.
[0019] In accordance with still an additional feature of the invention, the guide belts extend over deflecting rollers which have a characteristic selected from the group of characteristics consisting of being eccentrically mounted and non-round, respectively, the distance between the guide belts, on the one hand, and the transporting path of the signatures, on the other hand, being variable due to rotation of the deflecting rollers.
[0020] In accordance with a concomitant feature of the invention, the guide surfaces face towards the signatures and are provided with a friction-reducing coating.
[0021] According to the invention, the device for guiding signatures in the region of a wedgeshaped outlet of a cutting-cylinder device in a folder of a rotary printing machine is distinguished in that, arranged in the vicinity of the transporting path of the signatures, are one or more flat guide belts which extend virtually transversely to the transporting direction of the signatures, the flat or planar belt surfaces forming guide surfaces which bound or define the transporting path of the signatures and are arranged at least on one side of the transporting path of the signatures, but preferably on both sides of the signature-transporting path. The guide belts, which may be formed, for example, of metal, plastic, rubber or some other suitable material, may have a width which is adapted to the respective construction of the folder and may be, for example, in the range between a few cm to 0.4 m. The thickness of the metal belts is likewise dependent upon the respective dimensioning of the cutting-cylinder device and may be, for example, 0.2 to 2.5 mm.
[0022] Using the guide belts according to the invention in the region of the wedge-shaped outlet of a cutting-cylinder device offers the advantage that, even in the case of cutting cylinders with a very small diameter, the upline edges of the belts can be advanced very closely up to the cutting region, with the result that the region wherein the leading edges of the signatures are not guided after the cutting operation can be kept extremely small. In addition, the guide belts according to the invention provide the advantage that, in the case of a paper build-up, they yield automatically due to their own elasticity, as a result of which, damage like that which may occur, in particular, in the case of fixedly installed guide plates is ruled out from the outset. Should, however, a paper build-up result in damage to one of the guide belts according to the invention, then this guide belt can be exchanged straightforwardly and cost-effectively in an extremely short period of time, because the belt material which is to be replaced may be supplied, for example, in the form of supply reels and drawn into the machine by the machine operator himself or herself. In contrast with solid fixedly installed guide devices, in the case of which, damage to the device as a result of a paper build-up usually results in the printing machine being at a standstill for a relatively long period of time, use of the signature-guiding device according to the invention allows the printing operation to be resumed after an extremely short period of time.
[0023] According to a preferred embodiment of the invention, an endless guide belt is guided over two, first and second deflecting rollers arranged on mutually opposite sides, preferably outside the transporting path of the signatures. The guide surfaces, which are directed toward the top side and underside of the signatures, are formed here by the mutually opposite inner sides of the endless guide belt, between which the signatures run. The described embodiment provides the advantage that reliable guidance of the signatures takes place by using only a single endless guide belt.
[0024] Instead of using two guide rollers, it is likewise conceivable for an open-ended guide belt to be correspondingly extended over just one deflecting roller, which may be fastened, for example, on one of the side walls of the folder, and for the two ends of the open-ended guide belt to be fastened, for example, on the opposite side wall of the folder, preferably via a resiliently elastic device.
[0025] According to a further embodiment of the invention, a first and a second open-ended guide belt are arranged separately from one another on mutually opposite sides of the transporting path of the signatures. The first and/or the second guide belt may advantageously be arranged here at an angle to the transporting path of the signatures, so as to produce a somewhat funnel-like inlet region into which the signatures enter by way of the leading edges thereof. This offers the advantage that the formation of “dog ears” is avoided in a particularly effective manner. Furthermore, the angle at which the two separate guide belts are arranged in relation to the transporting path of the signatures may advantageously be adjustable, as a result of which it is possible to achieve adaptation to different signature thicknesses, signature formats, printing materials and machine speeds.
[0026] According to a further embodiment of the invention, each of the guide belts preferably has a separate tensioning device assigned thereto, which, in the simplest case, may be formed, for example, by a tension spring which has adjustable prestressing and acts on one end or both ends of a guide belt according to the invention and is supported, for example, on the frame of the folder.
[0027] According to a preferred embodiment of the invention, however, the tensioning device is formed by a lever arm which can be pivoted about a pivot pin via an actuating device. Fastened onto the lever arm is a deflecting roller, over which a respective guide belt extends. The actuating device advantageously includes here a spring, subjecting the lever arm to a resiliently elastic force, for example, a helical tension spring or a helical compression spring, and a rotatable cam, which is assigned to the lever arm, and on which the lever arm is supported. The cam and the spring cooperate with one another here so that, by rotation of the cam, the lever arm can be moved from a first, tensioning position, wherein the guide belt according to the invention is subjected to a predetermined resiliently elastic force, into a second position, wherein the guide belt remains untensioned and can be fastened onto the lever arm, for example by hand, via corresponding hooks or similar fastening elements. The embodiment just described allows the tensioning of the guide belt to be changed by rotating the cam, with the result that, depending upon a printing order which is to be processed in each case, the signature-guiding device can be adapted to the respective conditions, for example, by manual or motor-driven rotation of the cam.
[0028] In the same way, provision may be made for the actuating device to be formed by a pneumatic cylinder acting on the lever arm, or an electrical actuator, which pivots the lever arm, for the purpose of tensioning the guide belt, into a first, tensioning position and, for example, for the purpose of fastening the belt end on the lever arm, into a second position, wherein the guide belt is in a non-tensioned state. It is conceivable here for the tensioning of one or more of the guide belts to take place in dependence upon the operating state of the printing machine so that, when the printing machine is at a standstill or during an emergency stop, the lever arm is automatically pivoted into the second position, wherein the guide belt is not tensioned. As a result, it is possible, for example, for the operation of threading a new paper web in the region of the wedge-shaped outlet of the cutting-cylinder device after a web break, or prior to a new printing order with a different paper width, to be simplified to a considerable extent and, in the case of a web break or paper build-up in the region of the wedge-shaped outlet, further risk of damage to be reduced to a considerable extent. Furthermore, it is also possible, for adapting to different printing orders or operating conditions of the printing machine, to change the distance between the guide belts and the transporting path of the signatures. For this purpose, provision may be made, for example, for the guide belts to be guided over eccentrically mounted deflecting rollers or over non-round, in particular over elliptically shaped, deflecting rollers, with the result that a change in the distance between the guide belts and the transporting path of the signatures is made possible by virtue of the eccentrically mounted or non-round deflecting rollers being rotated. The rotation of the eccentrically mounted deflecting rollers or non-round deflecting rollers can take place here either manually or via corresponding actuators, for example via electric motors or pneumatic cylinders, automatically and preferably in dependence upon the operating state of the printing machine, in particular in dependence upon the printing order and the machine speed.
[0029] In order to reduce friction and, furthermore, also to reduce smearing of the signatures, which were previously printed in the printing machine, on the guide surfaces of the guide belts according to the invention, it is possible, in particular, for the guide surfaces, which are directed towards the signatures, to be provided with a corresponding coating, for example, with PTFE (Teflon® or polytetrafluorethylene) or chromium, and so forth.
[0030] Other features which are considered as characteristic for the invention are set forth in the appended claims.
[0031] Although the invention is illustrated and described herein as embodied in a device for guiding signatures, particularly in the region of a wedge-shaped outlet of a cutting-cylinder device in a folder of a rotary printing machine, it is nevertheless not intended to be limited to the details shown, since various modifications and structural changes may be made therein without departing from the spirit of the invention and within the scope and range of equivalents of the claims.
[0032] The construction and method of operation of the invention, however, together with additional objects and advantages thereof will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings, wherein:
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] [0033]FIG. 1 is a diagrammatic side elevational view of a signature-guiding device according to the invention having a first and a second guide belt arranged at least approximately parallel to a transporting path of the signatures;
[0034] [0034]FIG. 2 is a view similar to that of FIG. 1 of a further embodiment of the signature-guiding device according to the invention, wherein, above and below the transporting path of the signatures, the first and the second guide belts are arranged at an angle to the transporting path and form a funnel-shaped inlet region for leading edges of the signature into a downline section of the transporting belts;
[0035] [0035]FIG. 3 is a cross-sectional view of the first embodiment of the signature-guiding device according to the invention, facing in the direction of the signature-transporting path, wherein an endless guide belt is guided over two deflecting rollers located outside the transporting path; and
[0036] [0036]FIG. 4 is a view like that of FIG. 3 of a further embodiment of the signature-guiding device according to the invention, wherein an open-ended belt is guided over a deflecting roller fastened to a tensioning lever, both ends of the belt being fastened by hooks to an opposite side wall of the folder.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0037] Referring now to the drawings and, first, particularly to FIG. 1 thereof, there is shown therein a signature-guiding device 1 according to the invention provided for guiding signatures 2 in the region of a wedge-shaped outlet 4 of a cutting-cylinder device 8 having a cutting blade 6 , which is included in an otherwise non-illustrated folder of a web-fed rotary printing machine, the signature-guiding device 1 having one or more flat guide belts 10 , 12 according to the invention which are arranged on both sides of a signature-transporting path 14 . The guide belts 10 and 12 have respective guide surfaces 16 and 18 which are directed towards the outer sides of the signatures 2 and guide leading ends 20 of the signatures 2 in the region of the wedge-shaped outlet 4 and, as the signatures enter onto a transporting-belt device 26 formed by transporting belts 22 and 24 , in order to prevent the leading ends 20 of the signatures 2 from creasing or folding over as the signatures enter the transporting-belt device 26 .
[0038] As is illustrated in FIG. 3, the signature-guiding device 1 according to the invention includes two deflecting rollers 28 and 30 , one deflecting roller 28 of which is arranged on a first side wall 32 of the printing machine, and the other deflecting roller 30 is fastened rotatably on a tensioning device 34 , which is movable relative to a second side wall 38 . The tensioning device 34 here includes a lever arm 36 which is pivotable about a rotary pin 40 which is preferably stationary relative to the second side wall 38 of the folder. The lever arm 36 is forced, by a spring 44 which can be prestressed by an adjusting screw 42 , against a rotatable eccentrically mounted or non-round cam 46 so that, by rotating the cam 46 , the lever arm 36 can be pivoted from the tensioning position for the guide belts 10 and 12 , which is illustrated in FIG. 3, into a non-illustrated position wherein the guide belts 10 and 12 according to the invention are in a non-tensioned state and are removable, for example, easily from the deflecting rollers 28 and 30 . As can also be concluded from FIG. 3, the signatures 2 are guided through, between the inner sides 16 and 18 , respectively, of the endless guide belts 10 and 12 , those inner sides 16 and 18 being providable with a coating which reduces friction, or prevents smearing of the signatures 2 , and forming guide surfaces.
[0039] Instead of using a deflecting roller 28 locally fixed to the first side wall 32 of the folder, it may also be advantageous, as shown in FIG. 4, to use an open-ended guide belt 110 , the ends 111 and 113 of which are fastened to the first side wall 32 of the folder with the aid of a fastening device, in particular by hooks 115 and 117 , respectively, which engage in the respective ends 111 and 113 of the open-ended guide belt 110 .
[0040] According to the further embodiment of the invention, which is illustrated in FIG. 2, the guide belts 10 and 12 are preferably inclined at an angle α and β, respectively, relative to the transporting direction 14 of the signatures 2 and form a conical or funnel-like inlet region 50 . As is indicated by the double-headed arrows 52 and 54 , the guide belts 10 and 12 , respectively, which may be formed like the guide belts of the embodiment of the invention which is illustrated in FIG. 3 and in FIG. 4, are arranged so as to be displaceable relative to the transporting path 14 of the signatures 2 , so that it is possible to vary the distance between the guide surfaces 16 and 18 of the belts 10 and 12 , on the one hand, and the transporting path 14 of the signatures, on the other hand.
[0041] As is also apparent from FIG. 2, the deflecting rollers 56 and 58 for the transporting belts 22 and 24 , respectively, of the transporting-belt device 26 may be arranged within the interspace defined by the guide belts 10 and 12 , respectively, due to which a particularly compact arrangement is achieved.
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A device for guiding signatures in a folder of a rotary printing machine includes at least one guide belt disposed near a transporting path of the signatures, and extending transversely to a transporting direction of the signatures, the at least one guide belt being formed with guide surfaces defining the transporting path.
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BACKGROUND OF THE INVENTION
This invention relates to a power converter apparatus for converting A.C. power into D.C. power.
FIGS. 3-6 are diagrams showing a prior-art voltage converter apparatus disclosed in, for example, the official gazette of Japanese Patent Application Laid-open No. 194697/1984. FIG. 3 is the diagram of the main circuit of an A.C. elevator, FIG. 4 is the block diagram of a control circuit for a converter, FIG. 5 is the block diagram of a current controlling minor loop, and FIG. 6 is the diagram of voltage/current waveforms.
In FIG. 3, numeral 1 designates a three-phase A.C. power source, numeral 2 a converter which is constructed of transistors capable of forced commutation and diodes parallel thereto and which is connected to the A.C. power source 1 so as to convert A.C. power into D.C. power, numeral 3 a smoothing capacitor which is connected to the D.C. side of the converter 2 so as to smooth the D.C. power, numeral 4 a D.C. bus, and numeral 5 an inverter which is constructed similarly to the converter 2 and which is connected to the D.C. bus 4 so as to invert the D.C. power into A.C. power and to perform a variable-voltage and variable-frequency control. Shown at numeral 6 is an induction motor which is connected to the A.C. side of the inverter 5 so as to drive the elevator.
In a case where the motor 6 carries out power running, energy for driving the motor 6 is fed from the A.C. power source 1 through the converter 2 and the D.C. bus 4 to the inverter 5, and this inverter produces the A.C. power of variable voltage and variable frequency, which is supplied to the motor 6. Accordingly, the motor 6 is controlled to a torque and a revolution speed as desired and drives the cage (not shown) of the elevator.
On the other hand, in a case where the motor 6 carries out regenerative running, regenerative energy is fed to the converter 2 through the inverter 5 and the D.C. bus 4 by the function of the flywheel diodes of the inverter 5 and is given back to the A.C. power source 1 by the converter 2. That is, the A.C. power source 1 is regarded as an A.C. machine which rotates at a fixed frequency (here, the commercial frequency of the power source), in opposition to the D.C. voltage source, and the electric power is supplied to the A.C. power source 1 by the converter 2.
In FIG. 4, numeral 9 indicates an A.C. reactor which is inserted in each phase of the A.C. power source 1. Alternating-current detectors 10A-10C detect the currents of lines connecting the A.C. reactors 9 and the converter 2 and deliver alternating-current signals 10a-10c as outputs, respectively. A D.C. voltage detector 11 detects the voltage of the D.C. bus 4, and delivers a D.C. voltage signal 11a as an output. A voltage command value-setting unit 12 issues a D.C. voltage command value 12a, which is set at, for example, a value corresponding to the D.C. voltage of the D.C. bus 4 during the stop (no load) of the motor 6. Numeral 13 indicates a voltage-controlled amplifier, and symbol 13a the output thereof. A three-phase sinusoidal-wave generator 14 generates three-phase sinusoidal-wave reference signals 14a-14c which are synchronous to the A.C. power source 1. Symbols 15A-15C denote multiplier units, which produce respective outputs 15a-15c being three-phase sinusoidal-wave current command values. Current-controlled amplifiers 16A-16C produce outputs 16a-16c, respectively. A saw-tooth wave generator 17 generates an output 17a being an output modulation signal. A comparator 18 produces outputs 18a-18f. A base drive circuit 19 for the transistors of the converter 2 produces outputs 19a-19f which are the switching signals of the transistors.
In FIG. 5, numeral 21 designates an adder. Numeral 22 indicates the transfer function of the current-controlled amplifiers 16A-16C, numeral 23 that of the comparator 18, and numeral 24 that of the converter 2. Shown at numeral 25 is an adder. Numeral 26 indicates the transfer function of the A.C. reactors 9, and numeral 27 that of the alternating-current detectors 10A-10C. Symbol V 2ac denotes a voltage on the A.C. side of the converter 2, and symbol I 2ac a current on the A.C. side thereof.
The prior-art voltage converter apparatus is constructed as described above. The D.C. voltage signal 11a corresponding to the voltage of the D.C. bus 4 is checked with the D.C. voltage command value 12a by the voltage-controlled amplifier 13, and the resulting deviation is delivered as the output 13a. Subsequently, the three-phase sinusoidal-wave reference signals 14a-14c are multiplied by the output 13a in the respective multiplier units 15A-15C. That is, the output 13a serves as a value which determines the amplitudes of the three-phase sinusoidal-wave reference signals 14a-14c. The three-phase sinusoidal-wave current command values 15a-15c and the corresponding alternating-current signals 10a-10c negatively fed back are respectively checked by the current-controlled amplifiers 16A-16C, and the resulting deviations are respectively issued as the outputs 16a-16c. The outputs 16a-16c are compared with the output modulation signal 17a by the comparator 18, whereupon the signal 18a-18f which determine the switching timings of the respective transistors of the converter 2 are output to operate the base drive circuit 19. Then, this base drive circuit applies the switching signals 19a-19f to the bases of the respective transistors so that the D.C. voltage of the smoothing capacitor 3 may equalize to the D.C. voltage command value 12a and that the currents may be controlled into the form of sinusoidal waves. That is, the converter 2 is controlled as a sinusoidal-wave pulse-width-modulation inverter of constant frequency.
FIG. 6 shows the voltage/current waveforms of one phase. In a case where the motor 6 has performed the power running until the D.C. voltage of the smoothing capacitor 3 has become lower than the D.C. voltage command value 12a, the current waveform becomes in phase with the sinusoidal waveform of the power source voltage so as to supply electric power from the A.C. power source 1 to the D.C. bus 4. In contrast, in a case where the motor 6 has performed the regenerative running until the D.C. voltage of the D.C. bus 4 has risen above the D.C. voltage command value 12a, the current waveform comes to have the opposite phase to the phase of the sinusoidal waveform of the power source voltage so as to regenerate electric power from the D.C. bus 4 to the A.C. power source 1.
Even in the sinusoidal-wave pulse-width-modulation control, a ripple component corresponding to a pulse-width-modulation frequency is contained in the current due to the saw-tooth wave voltage. However, the A.C. reactor 9 of comparatively great reactance is inserted in each phase of the A.C. power source 1, and it relieves the ripple so as to obtain a smooth sinusoidal current.
By the way, the voltage-controlled amplifier 13 is usually constructed of an integrator in order to improve the response of the control system.
With the prior-art voltage converter apparatus as stated above, when the voltage-controlled amplifier 13 of the A.C. voltage feedback circuit is constructed of the integrator, the output 13a thereof becomes null at the start of the converter 2 because the integrator needs to be reset at that time. Consequently, the three-phase sinusoidal-wave current command values 15a-15c become null. Since the current on the A.C. side of the converter 2 is null at the start thereof, the alternating-current signals 10a-10c become null. Therefore, the outputs 16a-16c of the current-controlled amplifiers 16A-16C become null, and the transistors are switched so as to render the voltage of the A.C. side of the converter 2 null. As a result, an inrush current expressed by V ac /(jωL) (V ac : the voltage of the A.C. power source 1) flows on the A.C. side of the converter 2, to incur such a problem that the smoothing capacitor 3 and the voltage converter elements are destroyed due to the rise of the voltage of the D.C. bus 4.
SUMMARY OF THE INVENTION
This invention has been made in order to solve the aforementioned problem, and has for its object to provide a power converter apparatus which can prevent an inrush current at the start of a converter and which can stably control the voltage of a D.C. bus.
The power converter apparatus according to this invention comprises an initial voltage-setting circuit by which a signal for generating a predetermined voltage on the A.C. side of a converter is applied to a current negative-feedback circuit at the start of the converter.
In this invention, the predetermined voltage is generated on the A.C. side of the converter at the start thereof, so that the difference between the voltage of the A.C. side of the converter and the voltage of an A.C. power source becomes small, and a current on the A.C. side of the converter becomes low.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 2 are diagrams showing an embodiment of a power converter apparatus according to this invention, in which FIG. 1 is the block diagram of a control circuit for a converter, while FIG. 2 is the block diagram of a current controlling minor loop in FIG. 1; and
FIGS. 3-6 are diagrams showing a power converter apparatus in a prior art, in which FIG. 3 is the diagram of the main circuit of an A.C. elevator, FIG. 4 is the block diagram of a control circuit for a converter in FIG. 3, FIG. 5 is the block diagram of a current controlling minor loop in FIG. 4, and FIG. 6 is the diagram of voltage/current waveforms.
Throughout the drawings, the same symbols indicate identical portions.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIGS. 1 and 2 are diagrams showing an embodiment of this invention, in which FIG. 1 is the block diagram of a control circuit for a converter, while FIG. 2 is the block diagram of a current controlling minor loop, and in which the same portions as in the prior-art apparatus are indicated by identical symbols.
In FIG. 1, numeral 31 designates a voltage-controlled amplifier which is contructed of an integrator and which produces an output 31a. An A.C. voltage detector 32 is connected to an A.C. power source 1 and detects A.C. voltages, which are delivered as outputs 32a-32c. Adders 33A-33C produce outputs 33a-33c, respectively.
In FIG. 2, numeral 35 indicates an adder, and numeral 36 the transfer function of the A.C. voltage detector 32.
Next, the operation of this embodiment will be described.
The voltage-controlled amplifier 31 is reset during the stop of a converter 2, and the reset of the voltage-controlled amplifier 31 is released simultaneously with the start of the converter 2. Since the output 31a of the voltage-controlled amplifier 31 is null immediately before the start, three-phase sinusoidal-wave current command values 15a-15c are null. In addition, since the current I 2ac of the A.C. side of the converter 2 is null, the outputs 16a-16c of current-controlled amplifiers 16A-16C become null. Since, however, the outputs 32a-32c of the A.C. voltage detector 32 are added by the respective adders 33A-33C, the outputs 33a-33c of these adders 33A-33C equalize to the corresponding outputs 32a-32c of the A.C. voltage detector 32, respectively. Accordingly, the voltage V 2ac of the A.C. side of the converter 2 becomes a voltage equal to the voltage V ac of the power source 1 through the transfer function 23 of a comparator 18 and the transfer function 24 of the converter 2. As a result, when the converter 2 is started, the potential difference between the primary side and secondary side of each A.C. reactor 9 vanishes, and current flowing through the A.C. reactor 9 becomes null. That is, when the converter 2 is started, the current I 2ac of the A.C. side thereof is null. Thereafter, the converter 2 is controlled so that currents corresponding to the three-phase sinusoidal-wave current command values 15a-15c may flow.
As described above, in this invention, an initial voltage-setting circuit which generates a predetermined voltage on the A.C. side of a converter is disposed. Therefore, the invention brings forth the effect that an inrush current from an A.C. power source can be prevented at the start of the converter, to avoid the destruction of a smoothing capacitor, power converter elements, etc. and to provide an apparatus of low cost and high precision.
|
A power converter apparatus comprising an initial voltage-setting circuit by which a signal for generating a predetermined voltage on the alternating (A.C.) side of a converter is applied to a current negative-feedback circuit at the start of the converter.
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FIELD OF THE INVENTION
The present invention relates to development of an electronic level sensor and timer based falling head soil permeameter.
BACKGROUND AND PRIOR ART OF THE INVENTION
Soil permeameter is a device in the field of hydraulics, used to measure the permeability property of soil/rock. Permeability is an index of interconnectivity of pores. The coefficient of permeability is a constant of proportionality relating to the ease with which fluid passes through a porous medium. This parameter is very critical in understanding the fluid flow process in porous media and has a wide application in hydraulic engineering and fluid transport modeling studies.
Soil hydraulic conductivity has been historically measured in the laboratory, utilizing a falling or constant head of water applied to soil core samples retrieved from the field or on remolded soil samples. Laboratory measurements are often significantly at variance with in-situ field measurements because of the differing methodologies and the inherent difficulty of obtaining undisturbed soil samples. The hydraulic conductivity of soils at different depths is highly variable due to heterogeneous textural arrangement of soil particles.
It is desirable to have the capability to conduct hydraulic conductivity tests in laboratory by having the undisturbed soil in the form of a core of any desired depth above the permanent water table. Such depths may range from zero to many meters below the ground surface. In addition, it is desirable to have adequate flow capacity for maintaining flow equilibrium in a wide range of soils. Clay soils often have low permeability, whereas sandy or gravelly soils often have high permeability and, therefore, a greater accuracy is necessary in the measurement of time in case of falling head permeameter where the time reflects the permeability characteristics of soil under testing.
Prior art instruments developed for measuring hydraulic conductivity of soils generally fall into two major categories, namely- the lab measurements and in-situ field measurements. In the first type, the soil is collected from the field and subjected to permeability measurement in the lab. The second type is of measuring the permeability of soil at in-situ condition. For the first category of lab measurements, two types of permeameters are available, out of which one applies a constant head and the other a falling head. Both these types apply in principle Darcy's Law for calculation of coefficient of permeability. The second category applied for in-situ measurement of permeability utilizes various methodologies, which include electrical resistivity procedures and gas or liquid injection into the soil through penetrating probes and measuring permeability of unsaturated & saturated regime and complex analysis procedures.
The laboratory measurement of permeability is simpler, but requires collection of soil from the site, safe transportation to the lab, careful setting of lab experiment, and accuracy of measurements and reproducibility of experimental results. Among these two methods of measuring the permeability, namely the constant head has been reported, to be suitable for measuring the permeability of higher ranges, i.e, for coarser soil of more than 200 microns, while the falling head permeameter is for soils less than 200 microns having lower permeability.
The continuing physico-chemical processes ultimately disintegrate the rock into a fine soil texture and deposit in a suitable environment. In most of the semi arid environmental conditions, witnessing regular monsoon cycle, quick removal of the disintegrated rock materials and transport them to places of farther away from place of origin making them further finer particles and gets deposited as low permeable soil layers.
Reference may be made to U.S. Pat. No. 4,072,044 (Farwell et al 1976), U.S. Pat. No. 4,099,406 (Fulkerson, et al 1977) and U.S. Pat. No. 4,969,111 (Merva et al 1990) and scientific literature cited, indicating that the falling head permeameter is preferable for low permeability ranges and several errors/constraints that could affect the test results as reported are:
air trapped in sample; accuracy on measuring the elapsed time of test; uniform supply of water at the head soil core sample; disturbed soil conditions while loading the sample in apparatus; measurement error in head at beginning and at the end of test and area of specimen.
OBJECTS OF THE INVENTION
The main object of the present invention is to develop an electronic level sensor and timer based falling head soil permeameter, which obviates the drawbacks as detailed above.
Another object of present invention is to collect the soil core samples from various depths without disturbing the natural condition, of the same size of permeameter soil core chamber through coring process using the soil recovery pipe made up of seamless carbon steel tubes of various lengths by hammering process for recovering the soil as a core of particular length and depth section.
Still another object of the present invention is to have an accurate head level of start and end of test by using optical level sensors, which is of front mounting type at pre-determined heights in the burette tube.
Yet another object of present invention is to have an electronic timer unit interfaced with the level sensor to monitor the elapsed time between two pre-set levels automatically and more precisely to a level of 1/100 th of a second.
Further object of present invention is to conduct permeability test effectively by applying water uniformly over the soil surface and collecting the soil drained water without any hindrance, achieved by designing a three tubular cylinders assembly.
Still further object of the present invention is that the levels of placement of liquid level sensor can be chosen prior to the experiment by drilling a hole in the burette and fixing dome of the sensor with water leak proof condition using suitable adhesive. In the present case, the top level sensor was fixed at ‘0’ and the bottom level sensor was fixed at 20 cm levels.
SUMMARY OF THE INVENTION
Accordingly, the present invention provides an electronic level sensor and timer based falling head soil permeameter for measuring precisely the soil permeability which comprises, a glass burette ( 7 ) with two liquid level sensors ( 8 ) fixed at 0 and 20 cm graduated positions attached to a burette stand ( 9 ) and connected to top cylinder of soil permeameter assembly through a rubber hose, the said stand further attached to an electronic timer ( 10 ) unit interfaced with the level sensor ( 8 ), the said burette ( 7 ) connected to three cylindrical copper tube chambers to receive water from burette by top chamber ( 5 ) with a perforated Teflon disc at the bottom chamber ( 3 ) and middle chamber ( 4 ), these chambers further connected to soil core recovery tubes ( 11 ), which is attached to a conical flask ( 2 ) with a discharge tube and a measuring jar ( 1 ).
In an embodiment of the present invention, the depth core soils from field sites are collected in an undisturbed condition using a carbon steel seamless tube of various lengths.
In another embodiment of the present invention, a glass burette with two liquid level sensors fixed at 0 and 20 cm graduated positions attached to a burette stand and connected to top cylinder of soil permeameter assembly through a rubber hose is used to achieve the precise detection of water level cross over at selected levels.
In a further embodiment of the present invention, the elapsed time between the liquid level-change from 0 to 20 cm is precisely measured to an accuracy of 1/100 th of a second.
In yet another embodiment of the present invention, the drained out water from the bottom cylindrical chamber is collected and a constant rate of discharge is achieved through the outlet of the conical flask during the course of experiments.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings accompanying this specification
FIG. 1 represents complete setup of an Electronic level sensor and timer based falling head soil permeameter
FIG. 2 represents technical specifications of soil core recovery pipes
FIG. 3 represents optical sensor with front mounting type circuit diagram.
FIG. 4 represents circuit diagram of interface used for electronic timer.
FIG. 5 represents permeameter with three cylinders assembly.
FIG. 6 represents technical specifications of top chamber, which supplies water uniformly to the soil core surface
FIG. 7 represents technical specifications of middle chamber housing test soil core sample
FIG. 8 represents technical specifications of bottom chamber, which collects the drained water
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides an electronic level sensor and timer based falling head soil permeameter for measuring precisely the soil permeability which comprises, soil core recovery tubes of various lengths for collecting the different depth core soils from field sites, a glass burette with two liquid level sensors fixed at 0 and 20 cm graduated positions attached to a burette stand and connected to top cylinder of soil permeameter assembly through a rubber hose to detect precisely the water level crossovers, an electronic timer unit interfaced with the level sensor to monitor the elapsed time between two preset levels automatically and more precisely to a level of 1/100 th of a second, three cylindrical copper tube chambers ( FIG. 5 ) to receive water from burette by top chamber ( FIG. 6 ) with a perforated Teflon disc at the bottom and middle chamber ( FIG. 7 ) to hold the soil core with a perforated Teflon disc at bottom and bottom chamber ( FIG. 8 ) to receive drained water with an outlet rubber hose to channel drain water, a conical flask with a discharge tube to receive the water draining through the rubber hose and a measuring jar to collect constant discharge coming out of outlet of conical flask.
In accordance with the embodiment of the present invention, an electronic level sensor and timer based falling head soil permeameter is developed for measuring precisely coefficient of permeability of soil.
In accordance with the embodiment of the present invention, a process is provided for collection of soil cores from various depths in an undisturbed condition, thus facilitating in determination of permeability to almost nearer to the natural physical condition of the soil.
In accordance with yet another embodiment of the present invention, water level crossing is detected at the chosen heights in burette by using electronic sensors and activating the timer. Two liquid level sensors fixed at ‘0’ and ‘20’ ml position to sense the water level crossing at these two fixed intervals and produce a pulse to the timer. The sensor uses an Opto-Schmitt trigger and principle of total internal reflection. An integral LED and photo-sensor are so arranged that when a liquid does not cover the sensor, a light path is established between them. These two components are housed in a polysulphone body for compatibility with any liquid. Total absence of any moving part in the sensor ensures high reliability even in fast cycling applications. The liquid level sensor used incorporates the principle of total internal reflection. An integral LED and photo-sensor are so arranged that when a liquid does not cover the sensor, a light path is established between them. LED and Opto-Schmitt chips are sealed into the base of a clear plastic dome in such a position that light normally totally internally reflected from the dome boundary to the Opto-Schmitt. When liquid covers the dome, the change in the refractive index occurs at the boundary and some of the light escapes into the liquid, thus less light reaches the Opto-Schmitt, which thus turns off. Direct current supply of 5 Volts is required to power the output amplifier and 30-50 mA is for the operation of internal Light Emitting Diode (LED), which is obtained by using a single current limiting resistor. The output from these two sensors is given to the interface circuit embedded in timer unit.
Sensor 1 and Sensor 2 are mounted on the burette as shown in the diagram at 0 and 20 cm mark. The counting in the electronic timer is initiated by the output of the Sensor 1 and later on the counting is stopped by the output of the Sensor 2 .
In still another embodiment of the present invention a Borosil glass burette of 10 mm dia fitted with optical sensors at ‘0’ and ‘20’ cm levels with a facility of controlling the flow through a knob at the bottom and end tip of the burette which is connected to the top chamber through a rubber hose tightly to avoid the air entry for monitoring falling head.
In accordance with the further embodiment of the present invention, an electronic timer is provided to receive signals from the level sensors and to register the elapsed time taken to a level of 1/100 th of a second for water to cross between chosen two preset levels. The electronic timer is used here for the function of a stopwatch. An interface circuit is used here to take the input from the sensors and initiate as well stop the counting of the electronic timer. The interface circuit consists of all CMOS ICs. The electronic timer is also a CMOS based LCD display unit. The time is displayed in units of 1/100 second, 1/10 second, seconds and minutes. As the water column crosses the Sensor 1 , a low-to-high level transition signal is obtained at the sensor output. This is given to a positive trigger input of a CMOS CD 4047(pin- 8 ), used as a mono-stable multi-vibrator. The output of this mono-stable is a pulse. This pulse is given to an EX-OR gate of a CMOS CD 4030 (pin- 1 ) as one of the input. The moment it receives the input pulse it transfers it to the output of this EX-OR gate, which in turn, is connected to the input of the electronic timer to start the counting process. The counting is instantly shown in the LCD display. The moment the water column crosses the Sensor 2 , a low-to-high level transition is obtained at the sensor output. This is given to a positive trigger input of a second CMOS CD 4047(pin- 8 ), used as a mono-stable multi-vibrator. The output of this mono-stable is a pulse, which is given to the second input of the EX-OR(pin- 2 ) gate. This is instantly transferred to the output, which in turn is connected to the electronic timer, to stop the counting process and to display the total time taken for the water column of 20 ml, which is preset. The second CMOS CD 4047 (pin- 10 ) output is connected to a buzzer circuit. The buzzer gives the tone output to indicate to the operator that the counting is over on the electronic timer. The power supply to CMOS ICs and the Electronic timer is derived from the Regulator IC 7805, giving a constant 5 Volt supply. The instrument runs on the 230 Volt line supply, hence a step-down transformer and a rectifier is used in the front end of the 5 volt regulator.
In accordance with a further embodiment of the present invention, a design is evolved facilitating to house soil core collected from the field in the middle chamber and fitting the same with top chamber of water supply and bottom chamber for collecting the drain water with provision of perforated Teflon discs above and below of soil chamber for application of water uniformly at top surface of soil core and collecting permeated water uniformly draining from the bottom of soil core.
The present invention of Electronic level sensor and timer based falling head soil permeameter setup is schematically shown in FIG. 1 .
The first step of the process is to collect soil core samples from different depths using carbon steel seamless tubes of various lengths used as per technical specifications mentioned in FIG. 2 . The tubes are marked with desired sampling interval of 5 cms and driven into soil by hammering process and soil cores of various depth ranges are retrieved from inner part of the tube and marked with an arrow indicating top end of the soil core and then packed in a polythene sample bag with labeling giving site name, depth range, date of collection and transported safely to the laboratory. The samples are preserved in the laboratory according to site numbers and arranged depth wise and due care being taken to prevent disturbance to the core and as well to avoid direct sunlight falling on sample bags. The soil cores of various depth ranges of a particular site are taken for permeability test using the present invention. Each core sample is taken out from polythene bag and measured for its length and inserted in to middle chamber and then dressed at top and bottom with a knife for leveling up to chamber length. In order to avoid movement of water through contact between the soil core wall and chamber wall, silicon grease is applied inside part of chamber wall before insertion of soil core. The middle chamber holding the soil core is fitted with top chamber and bottom chamber tightly and placed inside chamber holder assembly and obtained verticality nature of chamber assembly with respect to working bench through adjustment of nuts provided in holder assembly and spirit level. The entire assembly is placed over a foldable plastic stool with a hole at the center. The outlet of bottom chamber connected with a rubber hose passes through the hole of plastic stool to drain water in to the conical flask.
The burette with two optical sensors as per specifications mentioned in FIG. 3 is fixed at ‘0’ and ‘20’ Cm levels and burette assembly is clamped to a stand placed on a working bench in such a way that the outlet of burette is above inlet of the top chamber of soil core assembly. The outlet of burette is connected to inlet of top chamber through a rubber hose in such a way that connection is made airtight at both the ends. Similarly, outlet of bottom chamber is connected with a rubber hose and other end of rubber hose is let into the conical flask placed below plastic stool. The outlet of the conical flask is further connected through a rubber hose for carrying the overflow water from the conical flask to the measuring jar placed near the conical flask.
The output from optical liquid level sensor is connected to a housing unit of interface circuit and timer. The interface circuit and timer unit assembly as shown in FIG. 4 is connected to power supply of 230 Volts (AC).
Once the entire setup is made, the level of conical flask output with respect to ‘0’ mm level of the burette tube is measured in terms of height (h o ). De-ionized water or double distilled water is added continuously to the burette keeping full open of the control knob of burette enabling water to enter the top chamber to fill the volume and allow the water to saturate the soil core sample and start draining into the bottom chamber and comes into the conical flask. The addition of water into the burette is continued till the conical flask started draining excess water and then by adjusting outlet control knob of burette, the overflow from the conical flask remains constant, i.e., constant discharge with time. Once the level of constant outflow is achieved, the addition of water to the burette is stopped such that the water level in the burette is above the ‘0’ mm level and the timer unit is started simultaneously. When the water level in the burette crosses the ‘0’ mm level, timer unit starts the clock and the time count is seen on the liquid crystal diode display. As soon as the water level crossed ‘20’ mm level, timer stops and display total time elapsed from head falling from ‘0’ to ‘20’ mm. The elapsed time is recorded. Water is added to the burette to have a level more than ‘0’ mm and the timer unit is reset for making a repeat measurement. The experiment was repeated three to four times. The process is repeated for all soil core samples of a particular site, recorded and tabulated.
The calculation of coefficient of permeability (cm/sec) is done by using the following formula:
k
=
a
·
L
A
·
t
·
ln
h
0
h
t
Where k=Coefficient of permeability (cm/sec)
a=area of burette standpipe (cm 2 ) L=length of specimen (cm) A=area of specimen (cm 2 ) t=elapsed time of test (sec) h 0 =head at beginning (time=0) of test (cm) h t =head at end (time=t) of test (cm)
The following examples are given by way of illustration and therefore should not be construed to limit the scope of the present invention:
In order to test the function of the designed soil permeameter, sieved sand samples of various ranges of size were subjected for permeability determination. Each sample was tested number of times and time elapsed between 0-20 cm of each test was considered for permeability calculation. After ascertaining the performance of permeameter, field samples collected to a depth of 8 m from alluvium at 0.5 m interval was subjected for determination of coefficient of permeability. The various experiments conducted are briefly illustrated as examples.
River sand was sieved to various sizes of 250, 500, 1000 and 2000 microns using sieve shaker. The sieved samples were collected representing samples of having sizes between 250-499 microns, 500-999 microns, 1000-1999 microns and above 2000 microns and then subjected for permeability test using the developed apparatus.
EXAMPLE-1
The first test was carried out using the sand sample having 250-499 micron size and the test was repeated 5 times and for each test the time registered in the timer as elapsed time (t) for the head to drop or falling from ‘0’ to ‘20’ cm level was recorded. The height from ‘0’ level at the beginning of the test up to the conical flask over flow level (h 0 ) was measured and recorded. The head at the end time (t) was estimated by deducting 20 cm from h 0 and noted as (h t ). The length of specimen (L) and area of the specimen (A) measured with the help of middle soil sample holder. The area of burette (a) was calculated by finding the diameter of the burette with the help of Vernier Caliper.
Area of burette (a)=0.785 cm 2 Length of specimen (L)=6.0 cm Area of specimen (A)=19.002 cm 2 Time elapsed (t)=(Refer Table-1) Head at beginning of test (h 0 )=104.5 cm Head at end of test (h t )=84.5 cm
TABLE 1
Size of
Electronic Timer Reading
Coefficient of
sample in
1/100 th of
Permeability K
micron range
Minutes
Seconds
Seconds
In cm/sec
250-499
0
18
93
0.0027815
0
19
01
0.00276981
0
19
10
0.00275676
0
19
13
0.00272819
0
19
12
0.00275379
EXAMPLE-2
The observed elapsed time and calculated Coefficient of Permeability for each test were tabulated and given in Table-2. The other parameters such as area of burette, area of specimen, length of specimen, Head at beginning and at the end being remained unchanged with that of the example 1. The same was used for estimation of coefficient of permeability.
TABLE 2
Size of
Electronic Tinner Reading
Coefficient of
sample in
1/100 th of
Permeability K
micron range
Minutes
Seconds
Seconds
In cm/sec
500-999
0
15
34
0.00343247
0
15
50
0.00339704
0
15
41
0.00341688
0
15
54
0.00338829
0
15
19
0.00346637
0
15
18
0.00346865
0
15
15
0.00347552
EXAMPLE-3
The permeability test was conducted for the sand specimen of size range 1000-1999 microns by loading the specimen in middle chamber without disturbing other set up. The experiment was conducted for four times and elapsed time for each test was noted and used in the calculation. The following tabulation provides the observed elapsed time for each test and permeability evaluated.
TABLE 3
Size of
Electronic Timer Reading
Coefficient of
sample in
1/100 th of
Permeability K
micron range
Minutes
Seconds
Seconds
In cm/sec
1000-1999
0
10
25
0.00513699
0
10
22
0.00515207
0
10
20
0.00516217
0
10
23
0.00514703
EXAMPLE-4
In order to validate the performance of soil permeameter designed, soils were collected from natural condition. Depth samples from 0-8 m with sampling interval of 0.5 m were collected from coastal alluvium using an auguring tool. As the coastal alluvium was loose we could not collect through soil recovery pipes and therefore auguring method was adopted and depth sample interval was kept at 0.5m. The collected samples were packed carefully and brought to the lab for testing. The following Table-4 presents the time elapsed and Coefficient of Permeability determined for all the depth samples.
TABLE 4
Depth of soil
Electronic Timer Reading
Coefficient of
samples in
1/100 th of
Permeability ‘K’
cm range
Minutes
Seconds
Seconds
In cm/sec
0-50
0
17
59
0.002993
0
17
41
0.003024
50-100
0
26
33
0.001999
0
26
37
0.001997
100-150
0
13
56
0.003883
0
13
53
0.003892
150-200
0
19
56
0.002692
0
19
75
0.002666
200-250
0
12
15
0.004333
0
12
19
0.004319
250-300
0
08
48
0.006209
0
08
56
0.006151
300-350
0
34
75
0.001515
0
34
78
0.001514
350-400
0
29
56
0.001781
0
29
53
0.001783
400-450
0
08
12
0.006485
0
08
09
0.006509
450-500
0
14
06
0.003745
0
14
15
0.003721
500-550
0
19
23
0.002738
0
19
28
0.002731
550-600
0
18
32
0.002874
0
18
29
0.002879
600-650
0
18
45
0.002854
0
18
39
0.002863
650-700
01
05
00
0.00081
01
03
82
0.00082
700-750
01
38
05
0.000537
01
37
04
0.000542
750-800
01
16
45
0.000792
01
16
32
0.000793
In all the examples, repetitive measurement of Coefficient of Permeability did not vary and thus establishing the sensitivity of electronic level sensor and timer based falling head soil permeameter developed.
Advantages of the Invention:
The main advantage of the present invention is that the permeability is measured to a maximum undisturbed condition of soil; the falling head level is monitored by an electronic eye avoiding human error; the time elapsed is accurately measured by timer activated by the incoming pulse from liquid level sensor and following a fixed head level change reduces the error in estimating head at beginning (h 0 ) and head at end (h t ). The present invention is capable of measuring all ranges of permeability.
The main advantages of the present invention are:
1. The falling water levels are sensed precisely 2. The elapsed time between two levels is measured accurately to a level of 1/100 th of a second 3. The application of water uniformly over the entire surface area of the soil core was achieved
REFERENCES
Amoozegar, A. W. Warrick, Hydraulic Conductivity of Saturated Soils: Field Methods, Soil Science Soc AM, Madison, Wis., 1986, pp 735-770.
Ankeny et al., 1991. Method for determining Unsaturated Hydraulic Conductivity. Soil Science Society of Americal Journal. 55:467-470
ASTM, 1998. Standard method D 5126-90-Standard Guide for Comparison of Field Methods of determining hydraulic conductivity in the vadose zone, Annual Book of ASTM Standards 2001, Section 4: Construction. Vol.04.08 Soil and Rock (1):D 420-D 5779, pp. 1055-1064.
R. Allan Freeze, J. A. Cherry, Groundwater, Prentice-Hall, Inc., Enalw. Cliffs, N.J., 1979 pp 15-77.
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Determination of hydraulic properties such as porosity and permeability of soil is of paramount importance in hydrology and civil engineering. In order to achieve greater accuracy in determination of permeability of soil using falling head permeameter, the two important known constraints of human monitoring error in noting the falling water level between two selected levels and elapse time between these two levels had overcome through electronically sensing the levels between two selected points and activating the timer clock automatically by the pulses coming from senor. The precision in measurement of time lapse in 1/100 th of a second enables greater accuracy in estimation of permeability. Provision of perforated Teflon disc above and below the soil core facilitates in application of water uniformly over the entire surface area of soil core at top and similar way permeated water leaving the soil core uniformly without any obstruction. The use of carbon steel seamless tube while collecting soil core facilitated in undisturbed soil core recovery from desired depth section. The permeability test was conducted for various sorted sands of different size ranges and each sample was subjected to repetitive tests and elapsed time for each test was recorded from timer unit. Coefficient of Permeability was calculated for each test. The lab experiment conducted for sorted and unsorted sediments has yielded a consistent performance of Electronic level sensor and timer based falling head soil permeameter.
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CROSS-REFERENCE TO A RELATED APPLICATION
[0001] This application is a continuation-in-part application of co-pending U.S. application Ser. No. 12/208,896, filed Sep. 11, 2008; which claims the benefit of U.S. provisional patent application Ser. No. 60/971,451, filed Sep. 11, 2007, which are incorporated herein by reference in their entirety.
BACKGROUND OF THE INVENTION
[0002] The rapid and accurate detection of visible and invisible substances, including target molecules and microorganisms is critical for many areas of research, environmental assessment, food safety, medical diagnosis, air quality assessment, homeland security, illicit drug identification, and warfare. In fact, diagnostic assays of biological compounds have become routine for a variety of applications, including medical diagnosis, forensic toxicology, pre-employment, insurance screening, and foodborne pathogen testing.
[0003] Industrial demand for low-cost, sensitive, rapid assays with the potential for screening multiple analytes simultaneously or in rapid succession has caused the development of many testing systems and formats. Most systems can be characterized as having three key components: a probe that recognizes the target analyte(s) with a high degree of specificity; a reporter that provides a signal that is qualitatively or quantitatively related to the presence of the target analyte; and a detection system capable of relaying information from the reporter to a mode of interpretation.
[0004] To ensure accuracy, the probe (e.g., antibody or nucleic acid sequence) should interact uniquely and with high affinity to the target analyte, but be non-reactive to non-targets. In order to minimize false positive responses, the probe should be non-reactive with and have no cross-reaction to non-target analytes.
[0005] Often, a label is directly or indirectly coupled (conjugated) to the probe. The label provides a signal that is related to the concentration of analyte upon completion of the assay. Ideally, the a label is not subject to signal interference from the surrounding matrix, either in the form of signal loss from analyte extinction or by competition from non-specific signals (noise) from other materials in the system.
[0006] A detector is usually a device or instrument used to determine the presence of the reporter (and therefore the analyte) in a sample. Some devices utilize a detector that provides an accurate and precise quantitative scale for the measurement of the analyte. Other devices, such as rapid on-site tests, such as pregnancy tests, utilize a detection instrument that provides the test results as a qualitative (positive or negative) signal. This signal may be visual.
[0007] Immunochromatographic assays have been known in the art for some time. These include, but are not limited to, lateral flow tests (e.g., lateral flow strips), for detecting analytes of interest. A typical lateral flow test utilizes the concept of lateral liquid or suspension flow in order to transport a given sample to the test. The benefits of lateral flow tests include a user-friendly format, rapid results, long-term stability over a wide range of climates, and relatively low cost to manufacture. These features make lateral flow tests well-suited for applications involving drug testing in urine and saliva in the workplace or retail markets, rapid point-of-care testing in hospitals and doctor's offices, as well as testing in the field for various environmental and agricultural analytes.
[0008] Most lateral flow tests are directed to fluid samples and may require several separate materials or parts in a kit in order to perform and/or optimize detection of a target analyte. Current lateral flow tests require some means for collecting the sample and then a means of exposing the sample to probes specific to the target analyte. Urine samples for drug testing are normally collected into a container and then the lateral flow strip is dipped into the sample. The sample travels up the lateral flow strip and if a drug is present binds to available antibodies which causes a reaction that can be visually detected on the strip. Applying this technology to surface, air and fluid testing has been problematic resulting in cumbersome testing procedures that have limitations. For example, applying the sample to be tested directly to the lateral flow strip disturbs the flow of the materials on the strip and hence the results of the test. Applying the sample directly to the lateral strip also limits the areas available to be tested to clean dry areas where there no grease or other debris is present to interfere with the flow on the strip. Also, the material supplied to initiate the reaction, distilled water droplets from a separate water dropper, freezes and as such the test can not be performed in below freezing climates. Moreover, having a separate device for dropping water to initiate the lateral flow reaction is cumbersome, costly and difficult to use.
[0009] Additional materials that can be provided with the lateral flow test include a separate vial containing a buffer solution or water to start the lateral flow reaction, a wick to transport the sample to the test; a filtration material to remove unwanted particles; a conjugate release pad where the detection reagent(s) is immobile when dry but mobilized when wet; and a reaction matrix where the capture reagents are immobilized. Unfortunately, in all of these cases, at least two separate devices (i.e., one device for collecting the sample and another device for detecting target analytes) and multiple steps are required to perform the test. Our invention simplifies and improves upon the previous inventions in this field.
[0010] Further, lateral flow tests are frequently subject to flow problems due to the nature of the chemistry and flow of reagents and sample. Any alteration of the test strip can alter the dynamics of the chemistry and reaction of the strip in the present of a target analyte. These tests usually require complex, multipart assays performed on a series of overlapping pads of different types of materials aligned on a test strip. Problems arise from, for example, material incompatibility, contact issues, and imperfect material characteristics. Boundaries found between segments can adversely affect flow characteristics. Different materials may have widely different flow, or wicking, rates, which have different effects on molecules flowing through them. Other problems that exist include contamination of the sample by interfering materials in the matrix, by contact with collector/operator; insufficient sample size due to inadequate “washing”; and operator/collector error when utilizing devices that require multiple devices/parts and steps necessary to test a surface for a target analyte.
[0011] Thus, it would be desirable to have a single self-contained device for collecting, extracting, testing, and a system of shipping the original untested material under forensic chain of custody a sample collected from a surface, powder, pill or fluid or sample of air that is easy to operate and not limited by dirty, greasy or wet contaminates and is stable under a wide variety temperatures and field conditions. The subject invention solves the above limitations in a self-contained device by first collecting samples on a built-in, specially treated swab and then washing the target analytes off the swab into a temperature stable buffer solution prior to testing. This approach does not limit the type of sample tested as the target analyte does not overload or disrupt standard lateral flow technology and is applicable to a wide variety of analytes and detection technologies. While the subject invention has been optimized for the drugs of abuse market, it is not limited or intended to just testing for drugs of abuse and can be used to test for a wide variety of substances such as explosives, WMD's, food toxins and industrial waste in dusts, powders, air, biological and non biological liquids with the same basic device.
BRIEF SUMMARY OF THE INVENTION
[0012] The present invention provides a single self-contained device for collecting, extracting, testing, and transferring, under forensic chain of custody, a sample from a medium (e.g., surfaces (hard or soft), air, or powders and fluids) in order to determine the presence or absence of target analytes present on or in the medium. In specific embodiments, the self contained device of the invention is used to test for the presence of illicit drugs; biohazards; food toxins; biologicals; weapons; or explosives in a variety of samples.
[0013] In preferred embodiments, the subject invention enables an operator to detect, on the spot, target analytes present on or in a medium in a simple manner and without additional technical support (e.g., laboratory equipment or manpower). Preferably, the device of the subject invention provides an observable signal for use in instant testing or continuous monitoring of an analyte in samples taken from a medium. If the target analyte (e.g., illicit drug) is indicated to be present by the subject device and confirmation is required by a laboratory, the entire device (or the cap) is designed for sealing and shipping under forensic chain of custody. The sample will then be tested by the laboratory to confirm in the existence of the substance within the sample and, thus, from the sample.
[0014] In one embodiment, the devices and methods of the subject invention can be used for detecting illegal drugs that are being smuggled or trafficked. This embodiment would be useful, for example, for Customs and Border Patrol to monitor activity at land crossings, airports, shipyards, and any other time people or items are crossing a border and require clearance. Analytes can be detected on passports, luggage, airplanes, ships, and in containers. Specifically, the subject device can detect in surface, powder, fluid, or air samples visible, invisible, microscopic, and minute amounts of marijuana, cannabis sativa, cocaine, heroin, amphetamines, MDMA (a.k.a., Ecstasy) and other scheduled and non-scheduled Drug Enforcement Agency drugs of abuse. It is also able to detect a wide variety of prescription drugs and veterinary drugs.
[0015] In certain embodiments of the invention, a self-contained device is used to locate the presence of illicit drugs present on solid surfaces such as office furniture, computer keyboards, lockers, trunks of cars, steering wheels, shipping containers, forklifts, work clothing, door knobs, hazmat supplies/protective gear, shipping containers, freight trains, trucking equipment, passports, and baggage. Solid surface detection of drugs of abuse can occur in a wide variety of settings, including, but not limited to employment settings, border crossings, airports, schools, colleges, courts, athletic contests, home inspections for the sale of a home, home inspections for prospective adoptions, and many other forums.
[0016] Alternatively, the subject self-contained device system can be used to detect target analytes, such as parent drugs and/or metabolites present in air or biofluid samples (such as blood, saliva and urine). The device can be designed to test for one specific drug of abuse or one specific explosive or biologicals; multiple drugs or multiple explosives or biologicals; or even a combination of drugs and explosives or drugs and biologicals. Air and fluid detection can occur in all the same settings as solid surface detection. The single self-contained device can be applied to a wide range of analytes where complex testing is now used that involves several components to complete the test.
[0017] In one embodiment, the single self contained device comprises a housing unit, wherein the housing unit has a main body. The main body is hollow and comprises (a) collection materials or a swab for collecting a target analyte (e.g., from a solid surface and/or air or removed to test fluid samples); (b) an analysis material (such as, but not limited to, a lateral flow testing system) that performs the function of providing a surface upon which labeled probes are affixed to provide a detectable response when a target analyte is detected; (c) a solution contained inside of the device which is sealed and is punctured by “firing” the cap, e.g. pressing it down, and then the solution releases into (d) a wash retention well, preferably in the cap; and e) a results area that enables the operator to ascertain whether a target analyte has been detected on the analysis material.
[0018] An advantage of the device of the subject invention over previous designs is that in certain embodiments it collects the material from a surface on a specially treated swab and then washes the material off the swab with a custom solution. This wash solution containing the material collected from the surface can be tested using a wide variety of detection technologies including, for example, lateral flow and similar systems. This process allows the device to be used on wet, greasy or dirty surfaces as the material is not directly deposited on the lateral flow strip. This allows for a wider application of the device into a number of environments and facilitates testing of visible, as well as invisible, material.
[0019] In addition to assaying for drugs of abuse, explosives, biologicals or other materials on surfaces, air and fluids this invention can be used to identify the medications in pills and capsules or to test unknown powders and fluids. In one embodiment, the unknown pill, capsule or powder can be placed into the cap of the device and a solution released into the cap by pushing a plunger. The pill will dissolve as the device is shaken or agitated and medication will be released into the solution. The plunger mechanism can be rotated and the test strip lowered into the solution thereby sampling the medication in the pill that is now dissolved in the solution. In another embodiment, a pill crushing device is placed into the cap to accelerate the dissolution of the pill or capsule.
[0020] In a preferred method of use, see FIGS. 6A-D , an operator utilizes the self-contained invention to detect a target analyte (such as an illicit drug) on or in a matrix (surface, powder, air or fluid) by (a) removing the cap (b) rubbing the swab across the surface or item to be tested or alternatively leaving it exposed to collect target analytes in air (c) replacing the cap (d) rotating a dial on the top of the device to position “1” and “firing” the device, thus pressing it to puncture a foil (or other membrane) sealed compartment inside the device, thereby allowing the swab fluid to be released into the cap (e) shake or agitate the invention to rinse the material on the swab into the fluid (f) rotating the dial on the top of the device to “2” and press to introduce the lateral flow strip or other detection technology into the fluid in the cap and (g) reading the results of the test by visually discerning the presence of a line, indicator or a digital display within the main body of the housing unit.
[0021] In certain embodiments, the device emits a sound, light or digital readout when the reaction is finished or a positive result is found. The device is designed with sufficient space to accommodate additional electronic or sensing materials to be imbedded allowing these and other functions to be incorporated into the device. This additional space can be used, for example, to incorporate additional test strips to expand the detection capability of the device.
[0022] In certain embodiments, see FIG. 1 , the single self-contained device includes a removable cap. This cap can be located at one end of the device and collects the wash solution, such as, for example, a buffer, which is mixed with the collection substance. This cap can be removed, sealed with a lid, wrapped with evidence tape and shipped back to a laboratory under chain of custody to confirm results. In one embodiment, the self-contained device comprises a housing unit, wherein the housing unit has a main body and a cap that is adapted to be removably coupled to the main body. The main body is hollow and comprises a) a swab or collection material for collecting a target analyte (i.e., from a solid surface and/or air or fluid samples); an analysis material (such as a lateral flow testing system) that performs the function of providing a surface upon which labeled probes are affixed to provide a detectable response when a target analyte is detected and b) a results area that enables the operator to view whether a target analyte has been detected on the analysis material.
[0023] In one embodiment, see FIG. 1 , the main body includes a wash retention well having a puncturable self-sealing membrane through which a swab can pierce. The method of use is similar to that described above for testing a sample solid surface. Specifically, in a method of use, (a) the swab pierces the puncturable self-sealing membrane of the retention well within the main body to wet the swab; (b) the swab is then removed, causing the membrane to self-seal and prevent any release of wash from the cap; (c) the wetted swab is brought in contact with a solid surface to be tested, such as by swabbing on the surface to collect a sample or it can be left for a specific time exposed to collect target analytes in the air; (d) the swab is then replaced into the main body where it repunctures the self-sealing membrane and is immersed in the wash; (e) inverting the device several times to remove the sample from the swab into the wash; (f) through capillary action, moving the sample fluid to a lateral flow based test housed in the main body; and (g) reading the result of the test visually or on a digital display when a target analyte in the sample is detected using the lateral flow based analysis test situated within the main body of the housing unit.
[0024] In other embodiments, the cap includes a wash retention well having a) at least one opening; b) at least one moveable sealing mechanism over the opening that prevents the wash in the retention well from escaping and coming into contact with the collection/analysis material when the cap is placed over the main body of the housing unit; and c) a release mechanism coupled to the sealing mechanism(s) that, when acted upon by the operator, causes the sealing mechanism(s) to move from the opening and allow the wash in the retention well to flow through the opening(s) and come into contact with the collection/analysis material.
[0025] Alternatively, the cap includes a wash retention well and a moveable release mechanism. The moveable release mechanism or removable vapor proof foil is preferably the method of releasing the wash so it can flow freely from the retention well for purposes as described herein.
[0026] In a method of use for the embodiments described above, an operator utilizes the self-contained device system of the invention to detect a target analyte (such as an illicit drug) on a solid surface by (a) releasing the wash from the retention well by activating the release mechanism(s) on the cap to wet the swab; (b) deactivating the release mechanism to seal remaining wash in the retention well; (c) removing the cap from the main body of the housing unit; (d) bringing the wetted swab in contact with a solid surface to be tested and swabbing the area to collect a sample or leaving it exposed to collect target analytes in the air; (e) placing the cap over the collection/analysis material and the main body of the housing unit; (f) releasing the wash from the retention well by activating the release mechanism(s) on the cap; (g) inverting, shaking, or otherwise agitating the device several times to wash the sample into the wash; (h) deactivating the release mechanism to seal remaining wash within the retention well; and (i) reading the result of the test visually or on a digital display when a target analyte in the sample is detected using a lateral flow based analysis technology situated within the main body of the housing unit.
[0027] In certain embodiments, the swab is treated with a water soluble adhesive that captures residue from the surface and immediately dissolve in the wash, thus eliminating steps (a) and (b) above. Alternatively, there may be more than one retention well with appropriate amounts of wash dedicated for use with step (a) and/or (f) so that it is not necessary to deactivate the releasing mechanism and ensure remaining wash is delivered back into the retention well. As understood by the skilled artisan, the release mechanism can be automated, where upon activation by the operator, the release mechanism is automatically deactivated after a specific time period to ensure appropriate amounts of wash are released from and/or returned to the retention well.
[0028] The subject invention further provides a method for manufacturing a self-contained device for collecting, transferring, extracting, and testing for the presence of a target analyte from a sample taken from a solid surface, air or powder or fluid samples. In one embodiment, the method comprises providing a housing unit comprising a main body and cap that can be removably coupled to the main body; disposing a collection/analysis material in the housing; disposing a retention well within the cap; and disposing a wash within the retention well within the cap, wherein the cap includes a means for allowing the wash to be released from the retention well upon action by the operator.
[0029] In particular embodiments, the collection and analysis materials are one and the same, where the single collection/analysis material includes in series, a number of zones (predefined areas): a collection (receiving) zone; a conjugate zone; a reaction zone (also referred to as a detection zone); and optionally, a control zone. A medium is contacted with the collection/receiving zone (e.g., by wiping the collection zone on a solid surface), then filtered to remove any excess dirt, grease or moisture that would interfere with the test, the collection/receiving zone is contacted with the wash via operator manipulation of the releasing mechanism on the cap, where the target analyte is washed from the collection/receiving zone into the wash.
[0030] The wash carries the target analyte through the conjugate zone, which contains free (non-immobilized) probes (e.g., monoclonal antibodies or DNA aptamers) specific for target molecules. Preferably, the probes are labeled with nanoparticles doped or otherwise associated with differently colored dyes (e.g., red and blue dyed nanoparticles) or conductive particles to effect an electrical signal if positive results are detected. All of these components (potentially including probe-target molecule complexes and excess, and unbound probes) flow onto the reaction zone, which contains immobilized binding agents (e.g., polyclonal or monoclonal antibodies) specific for the target molecules. Preferably, the binding agents immobilized in the reaction zone are present in known amounts, such as in a 1:1 ratio, to facilitate quantification of the reaction, as will be described below.
[0031] In certain embodiments of the invention the conjugate and detection zone are one and the same, where probes specific for a target analyte are labeled and bound to collection and/or analysis material. Thus, in certain embodiments, the swab incorporates the analysis material by use of a filter system to ensure the analysis is not compromised by dirty, greasy or moist material. In other embodiments, a separate analysis material comprising both the conjugate and detection zones are provided separately from the swab.
[0032] In certain embodiments, a control zone is provided that contains immobilized binding agents specific for unbound probes, and will serve as a positive control to show that the probes were present in the solution.
[0033] The device system of the invention can collect, transfer, extract, and test for the presence of a target analyte on a solid surface, and/or air or fluid samples, and additionally, be sealed to allow the sample and test to be sent to a laboratory for further testing under forensic chain of custody.
[0034] Addition embodiments and advantages of the invention will become apparent from the following detailed description.
[0035] The detector in this invention relates a positive or negative test result that is read by the human eye or an optical reading that can be digitally read and emit a sound or light.
[0036] It should be noted that the device can be adapted to hold a wide variety of detection devices and is not limited to lateral flow strips.
BRIEF DESCRIPTION OF THE DRAWINGS
[0037] In order that a more precise understanding of the above recited invention be obtained, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. Understanding that these drawings depict only typical embodiments of the invention and are not therefore to be considered as limiting in scope, the invention will be described and explained with additional specificity and detail through the use of the accompanying drawings in which:
[0038] FIG. 1 is an illustration of one embodiment of a self-contained device of the invention, where a removable cap is coupled to the main body of the housing unit.
[0039] FIG. 2 is an illustration of a self-contained device of the invention, where the cap has been detached from the main body of the housing unit.
[0040] FIGS. 3A-C are illustrations of one embodiment of a self-contained device of the invention, where a removable cap includes a retention well with one form of release mechanism.
[0041] FIGS. 4A-B are illustrations of one embodiment of a self-contained device of the invention, where a removable cap includes a retention well with another form of release mechanism.
[0042] FIGS. 5A-B are illustrations of alternative embodiments of a self-contained device of the invention.
[0043] FIGS. 6A-D are cross-sectional illustrations of a specific design embodiment of a self-contained device of the subject invention. Shown in these figures are the use of a nested lid, an inner tube with fluid retention tube therein, being puncturable with a prong when advanced by the button.
[0044] FIGS. 7A-C illustrate an alternative embodiment of a button, with FIG. 7C being a cross-sectional diagram.
[0045] FIG. 8 shows one example of the internal housing assembly utilizing various sleeve inserts for labeling and viewing test results.
[0046] FIGS. 9A and 9B show a further specific design embodiment wherein the button is surrounded by a collar that can be rotated to the proper alignment before allowing the button to be depressed or “fired.”
[0047] FIGS. 10A-D are side views and a top view ( FIG. 10D ) of several design embodiments of the subject invention, using different button and cap configurations.
[0048] FIGS. 11A and 11B illustrate yet another embodiment of a button design, similar to that of FIGS. 7A-C , but utilizing a rounded button.
[0049] FIGS. 12A-12C illustrate alternative embodiments of a cap and nested lid arrangement. FIG. 12A shows a lid configured to fit into the end of the cap. FIG. 12B shows a lid configured to fit on the outside of the cap. FIG. 12C illustrates how the lid, when disengaged from the cap can be used to cover and seal the cap for storage and/or transport.
[0050] FIG. 13 is an illustration of a specific design embodiment of the subject invention.
DETAILED DESCRIPTION OF THE INVENTION
[0051] The present invention provides a self-contained device, and materials and methods for manufacturing and using the device, for collecting, transferring, extracting, and testing for the presence of target analytes from a sample taken from a solid surface and/or from air or powder or fluid samples. Preferably, the single self-contained device is used to detect illicit drug residues (such as residues from marijuana, cannabis sativa, cocaine, heroin, and the like) from solid surface, air, or other fluid samples and incorporating the ability to send the device or part of the device for further analysis under forensic chain of custody.
[0052] The invention is described herein by reference to several embodiments selected for illustration in the drawings. It should be understood that the spirit and scope of this invention is not limited to the embodiments shown in the drawings or the specific embodiments in the following description. Also, it should be understood that the drawings are not necessarily to scale and that any reference to dimensions or indication of colors in the drawings or the following description are provided for illustrative purposes only and are not intended to limit the scope of the invention in any way.
[0053] As used herein, the term “analyte” generally refers to a substance to be detected. For instance, analytes may include, but are not limited to, biological materials, explosives, and illicit and therapeutic drugs. More specifically, analytes include, but are not limited to, toxins, explosive materials, organic compounds, proteins, peptides, microorganisms, amino acids, nucleic acids, hormones, steroids, vitamins, both illicit and therapeutic drugs, drug intermediaries or byproducts, biologicals, virus particles and metabolites of or antibodies to any of the above-substances.
[0054] In certain embodiments, the target analytes that the subject device detects include, but are not limited to, explosives such as HMX, RDX, NG, TATB, Tetryl, PETN, TNT, DNT, TNB, DNB, and NC; and biological materials such as antibodies to rubella (including rubella-IgG and rubella IgM), antibodies to toxoplasmosis (including toxoplasmosis IgG (Toxo-IgG) and toxoplasmosis IgM (Toxo-IgM), hepatitis B virus surface antigen (HBsAg), antibodies to hepatitis B core antigen (including anti-hepatitis B core antigen IgG and IgM (Anti-HBC)), human immune deficiency virus 1 and 2 (HIV 1 and 2), human T-cell leukemia virus 1 and 2 (HTLV), hepatitis B e antigen (HBeAg), antibodies to hepatitis B e antigen (Anti-HBe), and influenza virus and biologicals such as drug resistant biologicals, including MRSA.
[0055] Preferred embodiments of the invention are directed to the detection of illicit drugs on solid surfaces, pills, capsules, powders, and fluids (including air). Illicit drugs (including drugs of abuse or controlled substances) that can be detected using the subject invention include, but are not limited to: amphetamine, methamphetamine, MDMA (a.k.a., Ecstasy), barbiturates (such as amobarbital, butalbital, pentobarbital, phenobarbital, and secobarbital), benzodiazepines (such as alprazolam and diazepam); cannabinoids (such as hashish and marijuana), cocaine, fentanyl, LSD, methaqualone, opiates (such as heroin, morphine, codeine, hydromorphone, hydrocodone, methadone, oxycodone, oxymorphone, and opium), phencyclidine, and propoxyphene. In certain embodiments detection of prescription drugs, which are commonly abused, such as pain killers (oxycodone, percocet, etc.) or erectile dysfunction drugs (Viagra™, Cialis™ etc.) may be detected as well as prescription drugs not commonly subject to abuse.
[0056] As used herein, the term “sample” generally refers to a material suspected of containing the analyte. The sample preferably contains materials obtained directly from a source or medium. The sample may be derived from a solid or semi-solid surface, pill, capsule, powder, fluids, air, or from a biological source, such as a physiological fluid (including blood, interstitial fluid, saliva, vitreous humor, cerebral spinal fluid, sweat, urine, breast milk, vaginal fluid, menses, and the like).
[0057] Preferred samples for testing for illicit drugs are derived from solid surfaces because this form of testing is less intrusive, requires a lower legal standard to test, and because the device is not used directly on humans, FDA clearance is not required. Surface testing for drugs of abuse has been largely ignored in favor of more invasive blood, saliva or urine tests. Surface testing can provide many benefits that biological testing cannot duplicate. In some embodiments, the sample is material derived from wiping residues from a solid surface. Examples of solid surfaces from which a sample may be taken include, but are not limited to, surfaces on office furniture, computer keyboards, lockers, trunks of cars, steering wheels, shipping containers, forklifts, work clothing, door knobs, hazmat supplies/protective gear, shipping containers, freight trains, trucking equipment, fork lifts, passports, and baggage.
[0058] The self-contained device preferably contains a swab and an analysis material based on lateral flow analysis technology. The swab is a solid support of any absorbent material useful in sample collection including, but not limited to, fabric (such as fleece), porous matrices (such as sponge or foam), gel, fiber (such as fiber glass or paper fiber fleeces), cotton, cellulose, rayon, and other synthetic materials. The swab can optionally include materials useful in providing and/or improving solid support of the swab, such as synthetic or semisynthetic polymers (i.e., polyvinyl chloride, polyethylene, polymethyl methacrylate and other acrylics, silicones, polyurethanes, etc.). In certain embodiments, it is preferred that the swab include such supportive materials in order to ensure the swab has the ability to properly penetrate membranes located in certain embodiments of the device. A preferred embodiment is a polyester swab made from 100% unbounded polyester which is treated with Solution (C) containing sodium textraborate 0.1 molar in 1% triton×100 buffer at a PH of 8.6. A preferred embodiment for the wash inside the tube of the device, which is punctured and released into the cap, is a wash solution of 0.10% triton×100 with a pH of 7.4 in 10% ETOH. It is a phosphate buffer saline in a preferred embodiment of the water inside the tube inside the body of the device.
[0059] The analysis material includes at least one probe that is able to specifically bind to a target analyte such as an illicit drug. The illicit drug must interact with, react to, or bind with the probe (e.g., an aptamer or antibody specific for the illicit drug), which creates some measurable change (temperature, color, current, voltage, etc.). This change is then detected visually or by some transduction mechanism. The degree of change is usually proportional to the illicit drug concentration in the sample taken using the self-contained device. Analysis material of the invention includes both the detection and transduction mechanisms. For instance, when an illicit drug binds with an antibody specific for the drug labeled with a conductive material (i.e., the probe) and closes an open circuit, the combined materials for the probe and circuit are provided on the analysis material. The closure of an open circuit and flow of current is the transduction mechanism. Colorimetry, reflectance photometry electrical resistance and electrochemistry can be either transduction mechanisms or both binding materials and transduction mechanisms.
[0060] In certain embodiments, the probe is labeled so as to communicate to the operator when a target analyte has been bound to the probe. For example, with colorimetric techniques, a labeled enzyme (the label is a compound that is capable of generating a colored product or dye upon binding of the enzyme to a target analyte, such as an illicit drug) is provided on the analysis material. The labeled enzyme is reacted with a target analyte. The amount of colored product generated is directly proportional to the amount of target analyte, such as an illicit drug, present in the sample. Thus, the more illicit drug present in the sample, the more intense the color; whereas the less illicit drug present, the less intense the color.
[0061] In certain embodiments, probes of the invention are labeled with chromogenic nanoparticles, which can be produced using known methods (Santra et al., Advanced Materials, 2005, 17:2165-2169, which is incorporated herein by reference in its entirety).
[0062] Highly chromogenic nanoparticles can be generated by a reverse microemulsion method followed by sizing of the particles to select particles with desired diameters (e.g., in the range of 100 nanometers to 400 nanometers). The nanoparticles can be coupled to the binding agents using various chemical groups (—NH 2 being the preferred nucleophile). The capture zone can contain immobilized target-specific binding agents in a predetermined amount or ratio (e.g., a 1:1 mixture of two target-specific binding agents). As the concentration of nanoparticles fixed in the capture zone increases, a color indication will be formed that is proportional to the concentration of the captured nanoparticles. If two or more nanoparticles are captured, the resultant color and intensity can be utilized to determine what type of nanoparticles were captured and in what amount.
[0063] Reflectance photometry quantifies the intensity of the colored product generated by the enzymatic reaction. A light source, such as a light-emitting diode (LED) emits light of a specific wavelength onto a test strip that includes the colored product (generated as described above). Since the colored product absorbs that wavelength of light, the more a target analyte is present in a sample (and thus the more colored product on the test strip), the less reflected light. A detector captures the reflected light, converts it into an electronic signal, and translates that signal to its corresponding illicit drug concentration.
[0064] In certain instances, the probe is coupled to a conductive label to enable electronic signaling to the operator about the presence or absence of a target analyte (such as an illicit drug) in a sample. “Electronic signaling” includes, but is not limited to, a “sensor electrode” or “sensing electrode” or “working electrode,” which refers to an electrode that is monitored to determine the amount of electrical signal at a point in time or over a given time period, where the signal is then correlated with the concentration of a target analyte, such as an illicit drug.
[0065] The conductive label of the probe can be any of numerous electrically conductive materials such as, but not limited to, platinum-group metals (including, platinum, palladium, rhodium, ruthenium, osmium, and iridium), nickel, copper, silver, and carbon, as well as, oxides, dioxides, combinations or alloys thereof. Some conductive labels and conductive labeled probes and fabrication technologies suitable for the construction of amperometric sensors are known to the skilled artisan and are commonly used in conductive lithography techniques.
[0066] According to certain embodiments of the invention, an open circuit is provided with electrodes located at opposite sides of a detection zone on an analysis material. The detection zone consists of immobilized binding agents that have a high specificity and selectivity for the probes of the invention. Preferably, the probes are conjugated to electrically conductive labels. Should a target analyte (i.e., illicit drug) be present in the sample, it will be bound to the conductively labeled probe (i.e., an antibody specific for the illicit drug conjugated to a conductive particle), travel to the detection zone where it will be immobilized by the binding agents, creating a band of conductive-labeled probes/target analyte across the analysis material (such as, for example, a lateral flow test strip). On each side of the lateral flow strip, in the area of the detection zone are two electrodes with a small electrical potential, 0.1-1.0 Volts. The circuit is powered at the beginning of the tests, but no current is able to flow to the electrodes across the detection zone creating an open circuit. Once the test is completed and target analytes, bound to conductively labeled probes, travel to the detection zone, a closed circuit is created. This generates a digital positive signal for the operator to read.
[0067] In certain embodiments, a secondary subcircuit is provided. If no target analytes are present in the sample the circuit will not close and after the specific time for the reaction a secondary subcircuit will close indicating a digital negative signal for the operator to read. These signals can be further processed into printed readout, stored in memory or transmitted to a local computer for further signal processing, storage, analysis and reporting. This signal generating process can be done using a variety of lateral flow chemistries, such as, by way of example, competitive binding assays, double antibody and other techniques all generating unique signal patterns for positive and negative findings. The embodiments of the subject invention can be configured to provide space for the above circuitry and other on-board electronics in the main body of the device.
[0068] The electrode can be, for example, a platinum (Pt)-comprising electrode configured to provide a geometric surface area of about 0.1 to 3 cm 2 , preferably about 0.5 to 2 cm 2 , and more preferably about 1 cm 2 . This particular configuration is scaled in proportion to the analysis material and housing unit used in the testing system of the present invention. The electrode composition is formulated using analytical- or electronic-grade reagents and solvents, which can ensure that electrochemical and/or other residual contaminants are avoided in the final composition, significantly reducing the background noise inherent in the resultant electrode. In particular, the reagents and solvents used in the formulation of the electrode are selected so as to be substantially free of electrochemically active contaminants and the solvents in particular are selected for high volatility in order to reduce washing and cure times. Some electrode embodiments are described in European Patent Publication 0 942 278 A2, published Sep. 15, 1999, herein incorporated by reference in its entirety.
[0069] Any suitable electrode system can be employed; an exemplary system uses a silver or silver/silver chloride (Ag/AgCl) electrode system. Reference and counter electrodes are formulated typically using two performance criteria: (1) the electrodes are capable of operation for extended periods, preferably periods of up to 24 hours or longer in cases where repeated measurements are necessary, as might be the case in open areas; and (2) the electrodes are formulated to have high electrochemical purity in order to operate within the present system, which requires extremely low background noise levels. The electrodes must also be capable of passing a large amount of charge over the life of the electrodes. With regard to operation for extended periods of time, Ag/AgCl electrodes are capable of repeatedly forming a reversible couple, which operates without unwanted electrochemical side reactions (which could give rise to changes in pH, and liberation of hydrogen and oxygen due to water hydrolysis). The Ag/AgCl electrode is thus formulated to withstand repeated cycles of current passage in the range of about 0.01 to 1.0 mA per cm 2 of electrode area. With regard to high electrochemical purity, the Ag/AgCl components are dispersed within a suitable polymer binder to provide an electrode composition, which is not susceptible to attack (e.g., plasticization) by components in the wash sample. The electrode compositions are also typically formulated using analytical- or electronic-grade reagents and solvents, and the polymer binder composition is selected to be free of electrochemically active contaminants, which could diffuse to the sensor to produce a background current. Suitable exemplary sensing electrodes that can be used in accordance with the present invention are described in PCT Publication Nos. WO 97/10499, published 20 Mar. 1997 and WO 98/42252, published 1 Oct. 1998, both of which are incorporated by reference in their entirety.
[0070] In one embodiment, the analysis material includes labeled probes that are specific for a target analyte (present in the conjugate zone) and binding agents specific for the bound probes immobilized on the analysis material (present in the reaction zone). When in solution, the labeled probes bind with target analytes and diffuse along the analysis material to react with a line of binding agents immobilized on the analysis material. The binding of the labeled probes with the binding agents provides a line of color or conductively closes an open electrical circuit that provides a visual indication in the results area that communicates to the operator that the target analyte is present. If no target analytes are present in the sample, the colored or conductive probes are not captured by the predisposed immobilized binding agents and no color or closed electrical circuit is on the analysis material, thereby communicating to the operator that the target analyte is not present in the sample.
[0071] In another embodiment, the analysis material comprises labeled probes that are immobilized along an area of the analysis material that is visible under the results area. The immobilized labeled/conductive probes are specific for a target analyte and are not visible to the operator when unbound. Upon binding to a target analyte, the labeled probes are visible to the operator or close an electrical circuit via the results area as described above.
[0072] The analysis material can be any known test pad containing one or more chemicals, adapted to come into contact with a fluid sample to be tested for an illicit drug. Conventional analysis materials that can be used in combination with the subject invention include, but are not limited to, chemical strip tests used to test for amphetamines, barbiturates, benzodiazepines, cannabinoids, cocaine, opiates and phencyclidine. In specific embodiments of the invention, the parent compound of the illicit drugs such as THC (Δ 9 -tetrahydrocannabinol), cocaine and heroin are detected using the device to indicate the presence of the drug in the area tested.
[0073] As illustrated in FIGS. 2 and 3 A-B, a housing unit 20 is provided, wherein the housing unit has a main body 2 . In certain instances, a detachable cap 7 is provided that is adapted to be removably coupled to the main body. In a specific embodiment, the housing unit has the following dimensions: 12 cm×2.5 cm×1 cm. In another specific embodiment, shown, for example, in FIGS. 6A-12 , the entire unit is approximately 6.0 inches to approximately 6.5 inches in length.
[0074] In a further embodiment, the cap can be removed and sealed with a lid 16 , wrapped with evidence tape and shipped back to a laboratory to confirm results. In a particular embodiment, the lid 16 can be form-fitted or capable of nesting with the cap so that it is easily transportable with the device of the subject invention and readily accessible to seal the cap. FIGS. 6A-D , 8 , and 12 A-C illustrate a specific embodiment having a lid 16 nested within the cap 7 for storage.
[0075] In one embodiment, the main body 2 is, in general, a hollow tubular container that can have therein or attached thereto a) a swab 11 used for obtaining a sample (i.e., from a solid surface and/or air or fluid samples); b) an analysis material 3 that performs the function of providing a surface or material upon which labeled probes (and in certain instances, binding agents) are affixed or embedded to provide a detectable response when a target analyte is present; and c) a results area 12 FIGS. 2 and 3 that enables an operator to visually determine whether a target analyte has been detected by the labeled probes or binding agents present on the analysis material.
[0076] In one embodiment, the swab 11 in FIG. 2 is removable from the main body 2 when used in testing fluid samples. In a further embodiment, removing the swab H exposes at least a portion of the analysis material 3 . In a specific embodiment, the analysis material functions on the basis of lateral flow technology or capillary action. In one embodiment, the analysis material can be brought into contact with a fluid to be tested, such as, for example, by dipping the appropriate end of the housing into the fluid sample. In a further embodiment, the detachable cap 7 shown in FIG. 5B , comprises is sufficiently hollow or is designed with a depression or retention well 8 therein, such that a fluid sample can be placed into the cap 7 . The main body 20 can be affixed to the cap, which would cause the fluid sample to be placed into contact with the analysis material 3 , particularly by inverting the complete housing unit 20 . The results of the test can then be observed in the results area on the main body 2 . In one embodiment, the test results are provided by use of a direct visual indicator, such as, for example, target analyte activated color or shape indicators. In an alternative embodiment, test results can be displayed on a digital display apparatus triggered when a target analyte in the sample is detected using the analysis material 3 .
[0077] To facilitate the collection of certain types of samples, it can be helpful if the swab 11 FIG. 5A-B is wet or at least damp. In one embodiment, the main body contains a retention chamber or inner tube from which a wetting fluid can be released from a puncturable container onto the swab to assist in collecting a sample. Thus, the swab can be dry for obtaining certain types of samples (e.g., from a surface). But, if necessary or desirable, the wetting fluid can be released from the main body to wet the swab. Alternatively, as will be discussed in more detail below, a retention well 8 FIG. 5B within the cap 7 can be designed to contain a wetting fluid. In one embodiment, the wetting fluid can be released by puncturing a seal on the retention well. In a further embodiment, the swab is designed to puncture the seal. In another embodiment the collection swab is moistened and sealed in a foil pouch. When ready to be placed in an area for air or other collection the foil is removed exposing the swab to the air or material to be tested.
[0078] In certain embodiments, the main body can be sealably coupled to the cap to prevent fluid leakage. In a specific embodiment, the main body includes a rectangular collar 6 that corresponds to rectangular openings in the cap 7 . When the main body is joined to the cap, the collar engages with the openings, so as to form a seal that prevents liquid from leaking out of the housing unit. In a further embodiment, the rectangular collar 6 prevents the cap 7 from rotating about the main body.
[0079] In a related embodiment, the cap 7 FIGS. 4A-B includes an wash retention well 8 having a) at least one opening; b) at least one moveable sealing mechanism 10 over the opening that prevents the wash in the retention well from escaping and coming into contact with the collection/analysis material when the cap is placed over the main body of the housing unit; and c) a release mechanism 9 coupled/to the sealing mechanism(s) that, when acted upon by the operator, causes the sealing mechanism(s) to move from the opening and allow the wash in the retention well to flow through the opening(s) and come into contact with the collection/analysis material.
[0080] In certain embodiments, as illustrated in FIGS. 3A-C , the sealing mechanism 10 is a disc disposed over an opening 13 offset to one side of the wash retention well 8 . The disc has an opening 14 therethrough that corresponds to the opening in the wash retention well 8 and a release mechanism that is a latch 9 attached to the disc. Utilizing the latch, the disc, being positioned sealably against the wash retention well 8 , can be rotated from between approximately 30° to approximately 180°, such that in a “closed” position, the disc 10 is positioned so that the opening 14 unaligned with the opening in the retention well 8 . When desirable to release the eluent, such as, for example, after a sample has been taken, the latch 9 can be slideably rotated, such that the opening in the disc 14 aligns with the retention well opening 13 allowing the release of the wash.
[0081] In another embodiment, as illustrated in FIGS. 4A-B , the wash is contained within a bag, pouch, balloon, or similar flexible or otherwise puncturable sealed receptacle 15 comprising a penetrable material or membrane. In one embodiment, the sealed receptacle 15 fills approximately ¼ to approximately ¾ the volume of the retention well 8 in the cap 7 . In a more specific embodiment, the sealed receptacle 15 fills approximately ½ the volume of the retention well 8 with the cap 7 .
[0082] In an alternative embodiment, the bag, pouch, balloon, or similar flexible or puncturable sealed receptacle comprising a penetrable material is contained within the housing. In a still further alternative embodiment, shown, for example, in FIGS. 6A-D , an inner tube 50 is contained within the housing that has disposed therein a fluid tube 55 having portion thereof comprising a penetrable material. In a specific embodiment, the end of fluid tube 55 nearest the swab comprises a penetrable material.
[0083] In a further embodiment, also shown, for example, in FIG. 4A-B , the cap 7 includes a release mechanism 10 capable of puncturing the sealed receptacle 15 . In one embodiment, the release mechanism 10 comprises a stylet, needle, prong, or similar elongated, sharpened implement for puncturing the sealed receptacle 15 and releasing the wash into the retention well 8 . FIGS. 4A-B , 7 A-C, and 8 illustrate an embodiment wherein a plunger or button 9 on the exterior of the cap 7 can be depressed, turned, pressed, or otherwise activated by an operator, causing the sharp ended release mechanism 10 to be pushed into the sealed receptacle 15 , puncturing the sealed receptacle and releasing the wash into the retention well 8 . In alternative embodiment, an example of which is shown in FIGS. 6A-D , the button 9 can be pressed or “fired” to advance the inner tube 50 towards an inner ring 42 having a sharpened prong 54 thereon for puncturing the penetrable material of the sealed receptacle, or on the inner tube 50 (as mentioned above), within the housing so that the wash therein washes over the swab and into the cap 7 . In a further embodiment, the button 9 is aligned to an appropriate position prior to being fired. And in a still further embodiment, an example of which is shown in FIGS. 7A-C and 9 A-B, the button can be surrounded by a collar 58 that can aid in aligning the button to the appropriate position. As seen in the examples in FIGS. 1 , 5 A-B, 6 A-D, 7 A-C, and 11 A-B, a variety of styles and configurations can be employed for the plunger or button 9 utilized with the subject invention. It would be well within the skill of a person trained in the art to create alternative button or plunger styles or configurations that can be utilized with the devices of the subject invention. Such variations are considered to be within the scope of the subject invention.
[0084] In certain other embodiments, the main housing includes additional aspects to assist the operator in using the single device system. For example, the housing can further include a timer 1 that is activated by a pressure switch located on the main body of the housing unit and/or reporting means for communicating the time to the operator. In a further embodiment, a conductive labeled probe, as described above, will close an open circuit triggered by the operator when the timer is started. Once the timer is triggered, if the test is positive the conductive labels will close the open circuit indicating a digital readout of positive or negative. Also, in certain applications quantitative results can be obtained if standards of known quantities are tested along with the unknown analyte.
[0085] In a method of use, an operator would utilize the single self-contained device system of the invention to detect the presence of an analyte on a solid surface by a) removing the cap from the main body of the housing unit; b) obtaining a sample analyte by bringing the collection/analysis material in contact with a solid surface to be tested; c) replacing the cap over the collection/analysis material and the main body of the housing unit; and d) releasing the wash from the retention well by triggering the release mechanism(s) on the cap.
[0086] In a more specific embodiment of a method of use, one embodiment of the device of the subject invention can be used to detect the presence of an illicit drug on a solid surface by:
[0087] a) removing the cap from the main body of the housing unit;
[0088] b) obtaining a sample analyte by bringing the swab attached to the device in contact with a solid surface to be tested and wiping an area of the surface. Instructions included with specific devices of the subject invention can provide information about the size of area to be wiped, such as a few inches, the approximate number of times to wipe an area, such as ten times, and other procedural details;
[0089] c) replacing the cap over the swab and securing it to the main body of the housing unit;
[0090] d) turning a button, as described above, to a first position;
[0091] e) depressing the button to puncture a tube or other receptacle containing an wash within the housing, causing it to wash over the swab and into the cap;
[0092] f) agitating the sealed device vigorously for at least 5 seconds;
[0093] g) turning the button to a second position;
[0094] h) depressing the button again to introduce an analysis material within the housing to the analyte/wash mixture for a pre-determined period of time, such as, for example, 5 seconds;
[0095] g) observing the results area on the housing after a pre-determined period of time, such as, for example, 3 minutes, to visually ascertain the results of the test.
[0096] In certain embodiments, one or several lateral flow strips (2-5 or more) are lined up in the housing unit on a platform 46 that is moveable by pressing down on a release button with the operators thumb. FIGS. 6A-D illustrate one embodiment utilizing a platform 46 for holding at least one lateral flow strip. The cap retention well has the wash retained by a foil seal. In operation the cap would be removed revealing the swab. The area to be tested would be swabbed and then the foil seal removed from the cap and the cap replaced on the device. It is shaken or agitated to release the material from the swab then the lateral flow strips are introduced to the elution fluid by the operator pushing the release button on the platform and sliding the platform with the strips into the cap with the elution fluid.
[0097] In other embodiments of the invention, the housing unit comprises a removable cap 7 that includes a retention well 8 in which wash is contained; a swab 11 on a moveable, solid support 30 ; an analysis material 3 ; and a results area 12 . As illustrated in FIG. 5B , the retention well can include a self sealing membrane 40 that is positioned such that the swab 11 and moveable solid support 30 can penetrate through the membrane and access the wash. The housing unit preferably includes a means for limiting the movement of the solid support 50 , such that following penetration through the self-sealing membrane, the swab cannot be moved beyond the retention well. The means for limiting movement 50 can include any of a variety of devices and techniques known to the skilled artisan for preventing further manual manipulation of a device following activation. For example, those systems used in hypodermic needles or other syringe devices that limit the plunger in order to prevent an operator from withdrawing and/or re-administering fluids after use of the needle or syringe can equally be applied to the device of the subject invention.
[0098] Self-sealing membranes are well known in the art. Examples of self-sealing membranes that can be used in accordance with the subject invention include those that are used with intravenous bags including, but not limited to, U.S. Pat. Nos. 5,400,995 and 6,805,842. In one embodiment of the invention, the self sealing membrane consists of an “O”-ring that enables the swab to penetrate there through and also has the ability to seal shut following removal of the swab. The size of the “O”-ring will depend up on the amount of target analyte the device is manufactured to test and thereby the size of the swab. The “O”-ring can be made of rubber, encapsulated, PTFE, VITRON®, Kalrez Silicone or other standard materials used by those familiar with art.
[0099] In a method of use FIGS. 5A-B , the swab 11 is moved by the operator, so as to puncture the self sealing membrane 40 and enable the swab 11 to be immersed in the wash. The cap 7 is then removed and the wetted swab is swiped over a solid surface to be tested. Due to the nature of the self sealing membrane 40 , following removal of the swab, the membrane 40 becomes sealed shut to ensure no release of the wash from the retention well 8 . Following sampling of a solid surface, the cap 7 is replaced over the swab 11 and the swab 11 re-pierces the self sealing membrane 40 to allow any target analytes (such as illicit drugs) to be washed into the eluent. Through capillary action the analyte laden wash is carried through the swab, and exposed to the analysis material 3 within the main body of the housing unit, and the results of that interaction are provided to the operator in the results area of the housing unit.
[0100] In yet another embodiment of the invention, as illustrated in FIG. 5A , the housing unit does not include a removable cap. In this embodiment, main body of the housing unit includes the retention well 8 in addition to the swab on a movable solid support, the analysis material, and the results area. The retention well houses the wash and includes two repuncturable self sealing membranes 40 , 45 . The two repuncturable self sealing membranes 40 , 45 are located such that the swab can easily puncture there through.
[0101] With the above embodiment, as illustrated in FIG. 5A , the device is activated and used by puncturing a proximal self-sealing membrane 40 using the solid support 30 of the swab 11 . The swab 11 is wetted by the wash within the retention well 8 . The solid support 30 of the swab 11 is then advanced further so as to cause the swab 11 to penetrate a distal, repuncturable, self sealing membrane 45 to expose the swab to the outside of the housing unit. The wetted swab can then be swiped over a solid surface for testing or left exposed to collect target analytes in air. The solid support 30 is then moved to withdraw the swab 11 back into the retention well 8 and to allow the wash to wash any target analytes from the swab. As with the other embodiments described herein, through capillary action, the sample-wash is exposed to the analysis material within the main body of the housing unit and results are provided to the operator in the results area.
[0102] The wash can include, but is not limited to, distilled, sterile water or buffer solution that is conventionally used in immunoassays and familiar with those skilled in the art.
[0103] In preferred embodiments, as illustrated in FIG. 1 , the collection and analysis materials are one and the same, where the single collection/analysis material includes in series, a number of zones (predefined areas): a collection (receiving) zone 11 ; a conjugate zone 5 ; a reaction zone (also referred to as a detection zone) 4 ; and optionally, a control zone. A medium is contacted with the collection/receiving zone (e.g., by wiping the collection zone on a solid surface), the collection/receiving zone is contacted with the wash via operator manipulation of the releasing mechanism on the cap, where the target analyte is washed from the collection/receiving zone into the wash to form a solvent.
[0104] As the solvent front migrates along the solid support, it carries the sample through the conjugate zone, which contains free probes specific for target analytes. Preferably, the probes are labeled with nanoparticles associated with differently colored dyes (e.g., red and blue dyed nanoparticles) and/or conductive particles. All of these components (potentially including bound labeled probes, and unbound probes) flow onto the capture zone, which contains immobilized binding agents (e.g., polyclonal antibodies) specific for the target analytes. Preferably, the binding agents immobilized in the capture zone are present in a 1:1 ratio. The nanoparticles will become fixed in the capture zone, and the shade of color can be read to indicate the presence of the target analyte or an open circuit closed by conductive particles.
[0105] In a further embodiment, one or more binding agents are immobilized in the reaction zone of the solid support. The binding agents may be immobilized by non-specific adsorption onto the support or by covalent bonding to the support, for example. Techniques for immobilizing binding agents on supports are known in the art and are described for example in U.S. Pat. Nos. 4,399,217, 4,381,291, 4,357,311, 4,343,312 and 4,260,678, which are incorporated herein by reference. Such techniques can be used to immobilize the binding agents in the invention. In one embodiment, the solid support is polytetrafluoroethylene, which makes it possible to couple hormone antibodies onto the support by activating the support using sodium and ammonia to aminate it and covalently bonding the antibody to the activated support by means of a carbodiimide reaction (yon Klitzing, Schultek, Strasburger, Fricke and Wood in “Radioimmunoassay and Related Procedures in Medicine 1982”, International Atomic Energy Agency, Vienna (1982), pages 57-62.).
[0106] The analysis material upon which the probes and binding agents are provided include, but are not limited to, cellulose, polysaccharide such as SEPHADEX™, and the like, and may be partially surrounded by a housing for protection and/or handling of the solid support. The solid support can be rigid, semi-rigid, flexible, elastic (having shape-memory), etc., depending upon the desired application. The selection of an appropriate inert support is within the competence of those skilled in the art, as are its dimensions for the intended purpose.
[0107] Preferably, the analysis material is of a solid support that has an absorbent pad or membrane for lateral flow of a liquid medium to be assayed, such as those available from Millipore Corp. (Bedford, Mass.), including but not limited to Hi-Flow Plus™ membranes and membrane cards, and SureWick™ pad materials.
[0108] The amount of probe deposited on the analysis material will be selected so as to meet the requirement for use of a trace amount relative to the wash, as explained above. The binding agent must, as stated above, be one that is specific to the analyte as compared to all other materials it is likely to encounter in use, so that no interfering reaction or in-activation occurs, but this obstacle is no different in principle from those faced in in vitro assays of body fluids and successfully solved. The choice of a probe satisfying these criteria is thus within the general competence of those skilled in the art.
[0109] In certain embodiments, a control zone is provided that contains immobilized binding agents (e.g., immobilized polyclonal antibody) specific for the probe (e.g., goat anti-mouse IgG) used to label one of the target molecules, and will serve as a positive control to show that active material (e.g., monoclonal antibody) was carried the full distance to the analysis material.
[0110] The subject invention further includes a method for manufacturing a single device system for collecting, transferring, extracting, and testing for the presence of an illicit drug from a sample taken from a solid surface area and/or air or fluid samples. The method comprises providing a housing unit comprising a main body and cap that can be removably coupled to the main body; disposing a collection/analysis material in the housing; disposing a retention well within the cap; and disposing a wash within the retention well within the cap. FIGS. 9-13 illustrate various specific design embodiments of the devices of the subject invention that incorporate the various components and features described herein.
[0111] It will be further appreciated by the skilled artisan that more than one collection and analysis material can be included in the main body to form a multi-test system. Further, the single device systems and methods of the invention may be utilized in research and various industries, such as environmental management (e.g., water and wastewater treatment systems), bioremediation (e.g., to determine optimum conditions for microbial growth), public health (e.g., identification of rapidly growing infectious microbes), and homeland security (e.g., identification of rapidly growing bioterrorism agents, WMD and explosive agents.).
[0112] The device and method of the invention can be used in the area of chemical warfare, to assess the extent of exposure to sulfur mustard in the eyes, skin, and respiratory tract (e.g., lungs). The molecule(s) targeted for detection and/or measurement can be sulfur mustard reaction products such as alkylated serum proteins (e.g., albumin), alkylated hemoglobin, alkylated tear proteins (e.g., lactoferrin), alkylated epidermal proteins (keratins), alkylated lung fluid proteins, hydrolysis products of sulfur mustard in urine (thiodiglycol).
[0113] The device and method of the invention can be used to assess the presence of respiratory infection. The molecule(s) targeted for detection and/or measurement can be those associated with viruses, fungi, or biologicals (e.g., viral, fungal, or biologicals1 antigens) that cause pulmonary infections, such as respiratory syncytial virus influenza virus, and pseudomonas.
[0114] In certain embodiments, a system is provided that incorporates the use of the device of the invention. The detection system includes a reporting means capable of tracking the presence and/or concentration of detected target analyte(s) as determined from the single self-contained device analysis. In related embodiments, the single self-contained device described herein includes a computerized means for reporting and tracking target analyte qualitatively or quantitative levels of concentrations. Preferably, the computerized means is capable of communicating remotely or proximately as well as being capable of providing the necessary outputs, controls, and alerts to the operator.
[0115] In a preferred embodiment, the single self-contained detection devices are provided as small, handheld portable equipment. It can be used by an operator in the home, at work, in airports or other security checkpoints. In certain embodiments, such devices can be designed for continuous monitoring, such as at the office, in the operating room, etc. where this capability would be valuable.
[0116] According to the subject invention, an illicit drug testing kit is provided for testing a solid surface area for illicit drug residues. A kit of the invention contains the necessary material for performing the methods described herein. This kit may contain any one or combination of the following, but is not limited to, a single self-contained testing device, which includes a housing unit having a main body, a swab, an analysis material based on, but not limited to, lateral flow analysis technology, and a results area a set of subject instructions for its use; and optionally a means for forensic sealing the device for transport to a laboratory for further confirmatory testing also envisioned is a wireless computer device for keeping track of, storing, displaying, and/or communicating monitored results. In certain related embodiments, the device can calculate and display the concentration of detected illicit drugs present in the matrix tested e.g. surfaces, pills, capsules, unknown powders, air or fluids.
[0117] All patents, patent applications, provisional applications, and publications referred to or cited herein, supra or infra, are incorporated by reference in their entirety, including all figures and tables, to the extent they are not inconsistent with the explicit teachings of this specification.
[0118] It should be understood that the examples and embodiments described herein are for illustrative purposes only and that various modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the spirit and purview of this application.
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The present invention provides a single self-contained device for collecting, extracting, on-site testing, and transferring for forensic confirmatory analysis, a wide variety of substances including, but not limited to, drugs of abuse, explosives, weapons of mass destruction, food toxins and industrial wastes. Samples can be obtained from a surface by swabbing a suspect area or the testing of solid materials (pills, capsules, powders), air samples and biological and non-biological fluids by placing the substance in the device. The device includes a swab, a retention well including a wash, and analysis technologies that can be, for example, a lateral flow testing system. The swab is rinsed with a wash prior to testing thereby not compromising the chemistry of the detection technologies and allowing for a wide variety of applications under a number of field conditions. Also, the device is a single self-contained unit instead of having a separate reagent droppers or sprays, making it compact and easy to use. Moreover, the device is designed to not only collect and test samples but to seal the originally target analyte, not affected by testing procedures, in a specially designed cap for shipping under chain of custody documentation to a forensic laboratory for confirmatory testing.
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TECHNICAL FIELD
The present invention relates to ceramic products, and in particular it relates to ceramic products with high unfired, or "green", strength, especially for use in buildings.
BACKGROUND OF THE INVENTION
It is known to produce fire resistant products for use in buildings and many of these comprise inorganic material such as asbestos bound together into a board or duct. Asbestos is no longer recommended for many applications. These products may take the form of board for use in partitioning or in cladding steel structures. It is important that this material is itself non-flammable and must exhibit poor thermal conductivity so that the temperature of the flame is dropped across the thickness of the material to an acceptable level. This is particularly important when encasing steel structures since in some cases the steel can reach a temperature where it will soften and deform.
As ceramic products are fire resistant (although not necessarily having the low thermal conductivity of fireboard) they are useful as cladding products. However the green strength of most ceramic material limits the size and complexity of shape that can be made owing to handling problems before firing and/or glazing.
It is an object of the present invention to provide a ceramic material which can be formed into boards or other products which have good fire resistance, and to provide a method of making the same.
SUMMARY OF THE INVENTION
According to the first aspect of the present invention there is provided a method of producing a ceramic product comprising the steps of preparing an aqueous slurry of a silica sol with a refractile material comprising a calcium silicate and/or zirconium silicate, causing the slurry to gel by physical or chemical means to form a solid structure, and drying said structure to form a porous ceramic product.
The gelation may be induced by means of a chemical gelling agent, but it is currently preferred to use physical means such as pressure moulding and, in particular, freeze moulding to set the slurry.
Preferably the refractile material, which should be insoluble in water, is a calcium meta-silicate. Preferably, the material includes both calcium and zirconium silicates.
The product can be tailored, or explained more fully hereinafter, to produce a relatively lightweight fireboard or a high green strength ceramic board in large or complex shapes suitable for subsequent firing into a `tilc` (which term is to include moulded three-dimensional shapes as well as simple square or rectangular sheets).
When the resultant product is a ceramic board, it has been found to have unexpectedly high green (unfired) strength and, in addition, the surface of the product produced using this method is particularly suitable for application of ceramic glaze, due to its smoothness, porosity and the absence of materials in the composition which would damage the glaze when burned out during firing. Preferred products are large flat or cornered tiles primarily, but not exclusively, for use as internal or external decorative architectural wall cladding material.
We believe, although the utility of the invention does not depend on the variety of this belief, that the high green strength may be due to one or a combination of the following factors: a) the introduction of divalent, as opposed to trivalent (such as Al 2 O 3 ), cationic refractile material; b) the change in pH caused by the addition of acid-neutral zirconium silicates into the alkaline sol; and c) the range of refractile particle sizes used, and the total specific surface area of these particles in relation to the silica particles, available for bonding. These may all or in part contribute to the formation of stronger bonds between the silica particles during the gelation process and confer the enhanced green strength properties of the product.
Where a fireboard is required, the product may be of relatively low density, advantageously no more than 850 kg/m 3 , ideally 500 or even 250 kg/m 2 .
The step of drying may be carried by firing the structure or by allowing the structure to dry under conditions substantially close to ambient.
The slurry is preferably frozen at a temperature in the range -5° C. to -150° C., advantageously in the region of -40° C. to -70° C.
The slurry comprises a colloidal sol of silica advantageously having an average particle size less than 30 nanometers.
The step of freezing said slurry may be carried out in a mould with an element of high thermal conductivity. In this case, the mould may be of a metal, or heat conductive material, such as aluminium, or a resin, such as an epoxy resin, filled with a metal powder, such as aluminium powder.
To produce a fireboard, the slurry may contain void forming material, such as particles of sawdust, polystyrene or the like, and which is burnt out during the step of firing, or a gas-forming agent. In addition, thermally resistant materials or strengthening fibres/materials comprising such as glass fibres, perlite, vermiculite, inorganic lumina, pulverise fuel ash, flake-like materials such as mica, or chopped fibres, e.g. mineral fibres, or such other materials as will give added strength to the structure, e.g. carbon fibres, may be present. The latter may be in the form of individual fibres, platelets or a mat thereof. As well as improving thermal resistance, the lower density makes the products lighter and easier to handle and install.
According to a second aspect of the present invention there is provided a ceramic product produced in accordance with the above described first aspect.
The product of the invention can be fired prior to use and will then assume the strength characteristics typical of ceramics in general. No loss of strength is observed, indeed strength is increased. This is significant in that calcium silicates are used in the production of fireboards and other products but, although the strength of these materials in the green state is relatively high, their strength is reduced or lost upon exposure to very high or sustained temperatures. It is a unique advantage of the products of the invention that they can be used in the green state, and their strength actually increases if subjected to heat, e.g. in the case of a fire. It is preferred to use zirconium silicate (e.g. Zirconsil) in fireboard products as this enhances strength in conditions of extreme heat for prolonged periods. Since no organic binder is employed there is none to burn out and weaken the product, and the ability to mould or cast means that more complex shapes than the simple flat boards of hitherto can be made.
The enhanced green strength means that much larger ceramic tiles/boards can be produced and improves pre-fired handleability to include sawing, routering, sanding and general cutting to required size or shape and ease of transportation. The fireboard products have enhanced green strength but the ceramic boards have even greater green strength and may be used unfired or partly fired in situations of heat exposure, where the heating will enhance the strength of the product prolonging its life, but will normally be fired and glazed. In this case the inclusion of void-forming products should be avoided as these will mar the glaze during firing. Very large glazed tiles can be produced which have many advantages over existing wall-cladding systems including the ability to produce cornered or three-dimensional shapes and to cast-in fixings.
Where firing and/or glazing is carried out the temperature should be sufficiently high to at least sinter the product and preferably cause crystallisation of the silica. Temperatures in the range of 700° to 1200° C., preferably of 1000° C. or more, may be employed.
Notwithstanding the product's exposure to heat in its untreated green state the ceramic board is weather resistant. Thus the increased green strength of the product, its stability on firing and ability to glaze, broadens the scope of product applications and will open up new markets to ceramic products.
The use of calcium or zirconium silicate refractile material fillers (most preferably acicular in nature) in combination with a colloidal silica sol such as SYTON X30 and gelation by either chemical or physical (pressure) means enables the production of large complex three-dimensional ceramic bodies with green (unfired) strength of at least 5 MPa and fired strengths in the range of 10 MPa to 30 MPa as determined by a modulus of rupture test.
A preferred refractile material is Wollastonite (calcium metasilicate), which is a mineral whose natural form is acicular (spiny), with length:diameter ratios from 3:1 to 20:1. The acicular nature of this material is believed to contribute to the green strength of the product.
It is preferred to employ at least 30% silica sol, especially where a calcium silicate is not used. Overall proportions of components may be within the following range:
______________________________________Silica sol 30-75%Silicates 8-70%Other ingredients 8-40%______________________________________
Within this, the proportion of calcium metasilicate should preferably not exceed 65% (by weight) of the total slurry, and may conveniently be in the range 20-40%. More than one metasilicate may be used, e.g. Wollastonite G and Wollastonite 400, in which case each should be in the range 10-30%. If zirconium silicate, e.g. Zirconsil, is employed it should preferably be in the range 20-30%.
The ceramic product produced may have a density as high as 2,500 kg/m 3 but, for a fireboard, preferably has a density below 1500 kg/m 3 , for example in the ranges around 250, 500 or 800 kg/m 3 .
Two or more such products may be joined together at edges thereof by applying ceramic slip between them, refreezing the combination, and then drying them to form a unitary product.
According to a third aspect of the present invention there is provided a fire-resistant board, tile or casting comprising a ceramic product according to the second aspect above.
The casting may be provided with depressions of such depth as to accommodate ceramic glaze material.
The invention will now be more particularly described by way of example and with reference to the accompanying drawings, in which:
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a diagram of a mould suitable for use in the method of the invention; and
FIG. 2 is a graph of thermal resistance data of products of the invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawing, FIG. 1 shows a mould comprising an insulated lid A and an insulated base B surrounding a lower C and upper D mould plate separated by spacers E. Slurry F in accordance with the invention is enclosed between plates C and D. Reservoirs G receive liquid nitrogen in order rapidly to freeze the slurry F.
One preferred step in the method of the present invention is that the ceramic slurry is frozen. The freezing temperature may typically be minus 70° C. Since the ceramic slurry contains a freeze-sensitive sol, the volume of the water component of the sol increases on its freezing to ice. This increased volume produces an internal pressure which densifies the ceramic particles of the slurry. Subsequently, when the material is warmed back up to room temperature, the ice melts and remains as water within the structure but the structure is now solid with good green strength.
The water is then dried off, to leave a ceramic material which is porous. The amount of porosity in the material is determined by the rate of freezing and the particle size and distribution of particles. The material may then be fired, if so desired.
One advantage of this freezing step is that there is virtually no dimensional change between the wet and dried products. Many ceramics produced by conventional routes such as pressing or slip casting shrink by up to twenty five percent of the original green state ceramic dimensions. Freeze coating eliminates this shrinkage to a very major degree. The material may also be moulded, possibly continuously to produce an elongate board.
As stated above, the material is porous and control of the pore size and distribution is affected by the particle size of the original slurry and by the rate of freezing. The preferred average particle size in the sol is less than 30 nanometers. The rate of freezing may be increased by providing moulds which have high thermal conductivity, such as those made of aluminium or an aluminium powder filled epoxy resin. The mould can either be immersed in a cryogenic tank or a cryogenic liquid, such as liquid nitrogen or solid carbon dioxide, from a freezing unit and can be pumped around channels within the mould. A mould release agent is generally used.
Use of the above procedures enables ceramics to be produced between 25% and 85% dense.
The use of particle sizes in the sol of less than 30 nanometers has a further advantage in that it enables the ceramic to be fired at relatively low temperatures because of the reactivity of the high surface area particles. If it is desired further to reduce the density of the material, e.g. to produce a fireboard, it is possible to add sacrificial materials as described hereinabove.
Fireboards produced in the above manner have extremely low thermal conductivity due to the high porosity but show excellent strength and integrity at temperatures up to 1200° C. They also have high thermal shock resistance, mechanical integrity and dimensional stability.
Because the freezing step gives a green state product which is itself strong or which can be fired without appreciable shrinkage, it is possible to produce very complex geometries, possibly three-dimensional, of insulation fireboard and ducting using the above method. Also, since the system is totally inorganic, and contains no organic binders, the material has better temperature stability since there are no binder systems that can burn out when the material is heated.
The ability to cast complex shapes may be used in the formation of decorative tiles. A series of progressively deeper depressions or profiles may be formed in a surface of the tile, which in use is intended to be outermost. Each depression or profile may be coated or filled with a glaze so that, when the tile or article is fired, the finish of the tile shows variation in colour depending on the depth and colour of the glazes used.
If it is desired to produce a larger product, tiles or other articles produced by the method may be joined by applying between them a bonding layer of ceramic slip, and refreezing the conjoined articles.
It is also possible to incorporate fittings of fixings, such as nuts or trunking, into the mould so that they become part of the cast article. This enables articles such as tunnel linings, cladding or ceramic glazed building panels to be produced for ease of use at a later date.
The invention is further illustrated in the following non-limiting Examples:
EXAMPLE 1
Composition (wt %):
73% Sodium stabilised silica sol
11% Precipitated silica
8% Zirconium silicate (Zirconsil)
8% Perlite (2JL)
36 ml of polystyrene spheres (3-5 mm) in 100 g of above slurry.
The precipitated silica is first mixed thoroughly into the colloidal silica until it is completely dispersed. Next, zirconsil powder is dispersed by continuous stirring until a uniform suspension is obtained. Finally, the perlite and polystyrene are spheres are added and mixed in.
The slurry is poured into a mould to produce the required shape, the mould sealed and then frozen with liquid nitrogen to -70° C. Upon warming back up to room temperature a solid structure has formed. When dry, the product is subjected to a low temperature `firing` step at 800° C. for one hour which produces a porous ceramic having a density of 400 kg/cu.m. The temperature used in below that at which sintering takes place and does not contribute to the strength of the board. It is employed to burn out the heat labile ingredients in order to produce voids in the fireboard.
EXAMPLE 2
Composition (wt %):
71% Sodium stabilised colloidal silica sol
14% Zirconsil powder
7% Quartz sand
8% Perlite (2JL)
The Zirconsil powder is first dispersed in the sol and then the other ingredients mixed in.
A mat of inorganic fibres is introduced into the mould and the above slurry poured in. A second mat of inorganic fibre is then introduced on top of the slurry. A board was then freeze cast as described in Example 1, except that it was dried at 200° C. and fired at 850° C. for one hour. The board so obtained had a density of 560 kg/cu.m and appeared to have greater mechanical strength than that of Example 1.
The board was strong enough to be handled and was tested for thermal insulation by exposing one surface of the board to the face of an oven heated to 1000° C. and recording the temperature on the other surface over time. The results appear in FIG. 2. After the test the board retained its integrity and showed no visible dimensional change after exposure to 1000° C. for eight hours.
EXAMPLE 3
Composition (wt %):
56.3% Colloidal silica sol (sodium stabilised)
3.8% Precipitated silica
7.0% Quartz sand
36.3% Zirconsil powder (ZrO 2 .SiO 2 )
6.1% Perlite (2JL)
0.5% Chopped glass fibre
The precipitated silica was first dispersed in the colloidal silica sol followed by the other products.
The board was then freeze cast as described in Example 1 except that the board was dried at room temperature for several hours before further drying at 100° C. and firing at 800° C. for one hour. The board had a final density of 800 kg/cu.m. The thermal insulation test results are shown in FIG. 2.
EXAMPLE 4
Composition (wt %):
53.3% Syton X30 (silica sol)
13.3% Wollastonite (NYAD G)
13.3% Wollastonite (NYAD 400)
13.3% Zirconsil
6.6% Vermiculite (fine)
The designations NYAD G or 400 refer to the supplier's (Cooksons, Stoke on Trent) designation of the grade.
The Wollastonite C, followed by the Wollastonite 400, the zirconsil and finally the vermiculite were added to the sol in that order and mixed in. The board was freeze cast as described in Example 1 except that it was dried at room temperature and then at 100° C. overnight. No `firing` was carried out. The board had a final density of 920 kg/cu.m and was thermally tested as in Example 3. Test results are shown in FIG. 2 and after 1 hour at 1000° C. no damage was visible to either surface of the board. The board was strength tested using a standard modulus of rupture test and the results are shown in Table 1 below together with comparative tests on proprietary fireboards Supalux and Promatect.
EXAMPLE 5
Composition (wt %):
______________________________________Silica Sol (SYTON X30) 33.5%Calcium Metasilicate (Wollastonite NYAD G) 16.5%Calcium Metasilicate (Wollastonite NYAD 400) 25%Zirconium Silicate (Zirconsil) 25%______________________________________
The Syton X30 was weighed and placed in a mixing container. The other ingredients were individually stirred into the Syton in the following order: Wollastonite G, Wollastonite 400 and Zirconsil. An industrial whisk-type mixer was used to combine the ingredients.
Once combined the slurry is stable at room temperature for 24 hours, however some sedimentation does occur requiring the slurry to be restirred before use.
An aluminium mould was constructed such that the internal dimensions were 1200×1300×9 mm (see FIG. 1).
The slurry was poured into the mould to slight excess volume such that when the sixth side was bolted on, the excess slurry was separated out. This ensured that no air pockets were created.
The mould was then subject to cooling using liquid nitrogen which was poured into a bath containing the mould. The freezing process was allowed to continue for a minimum of 6 minutes and temperature maintained at -30°--40° C. for a minimum further 6 minutes.
The ceramic board was removed from the mould and dried at a temperature of 150° C. for 2.5 hours. This produces a board with a high green strength (see Table 1).
Boards were either fired whole at 1190° C. or cut into smaller pieces and fired with or without glaze, and then strength tested on a universal testing machine (100 centres and 1.5 mm/min) and the MPa required to fracture the tile recorded, as above. The results are given in Table 1.
EXAMPLE 6
37.7% Syton X30 (silica sol)
18.6% Wollastonite NYAD G
43.7% Wollastonite NYAD 400
The wollastonite G and 400 were added to the sol in that order as described in Example 4. The slurry was poured into a mould and freeze cast as in example 5. Samples were tested in the green state and after firing both with and without glaze. The results are in Table 1.
TABLE 1______________________________________SAMPLE STRENGTH MPa______________________________________Supalux (Cape) Av. 6.325 N = 4Promatec L (Eternit) Av. 3.1 N = 4Example 4 Av. 2.24 N = 4Example 5 (Green State) Av. 8.5 N = 2Example 5 (Fired) Av. 12.6 N = 3Example 5 (Glazed) Av. 16.8 N = 3Example 6 (green state) Av. 5.7 N = 2Example 6 (Fired) Av. 11.33 N = 2Example 6 (Glazed) Av. 11.5 N = 2______________________________________
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A method of producing a ceramic product comprising the steps of preparing an aqueous slurry of a silica sol with a refractile material comprising a calcium or zirconium silicate, causing the slurry to gel by physical or chemical means to form a solid structure, and drying said structure to form a porous ceramic product. The product has a high green strength which nevertheless increases on heating, and may be used in building applications.
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BACKGROUND
[0001] 1. Field of Invention
[0002] The invention relates to chemical-mechanical polishing and more particularly to methods and products for replenishing a polishing slurry in a chemical-mechanical polishing apparatus.
[0003] 2. Description of Related Art
[0004] The chemical-mechanical polishing (“CMP”) process is used in the manufacture of optical lenses and microelectronic devices to remove material from a workpiece such as a plastic or glass lens blank or a wafer and thereby create a very smooth, scratch-free surface. In a typical CMP process, a polishing slurry is introduced between the workpiece and a polishing pad that is pressed against the workpiece. One or both of the polishing pad and the workpiece are moved relative to the other so as to cause the polishing pad to wipe against the surface of the workpiece with the polishing slurry disposed therebetween. The polishing slurry typically comprises abrasive particles that are dispersed and suspended in a carrier fluid. The carrier fluid typically comprises one or more chemical compounds that influence the rate at which material can be physically abraded from the surface of the workpiece via the polishing pad and/or the abrasive particles.
[0005] FIG. 1 schematically illustrates a polishing apparatus 10 such as is typically used in plastic lens product polishing applications. The apparatus 10 comprises a polishing machine 20 which supports a workpiece 30 such as a plastic lens blank. The polishing machine 20 presses a polishing pad 40 into contact with a surface 50 of the workpiece 30 . A polishing slurry 60 is provided between the polishing pad 40 and the surface 50 of the workpiece 30 . The polishing slurry 60 is supplied to the polishing machine 20 via a supply line 70 that is in fluid communication with a slurry tank 80 . A pump 90 typically conveys the polishing slurry 60 from the slurry tank 80 to the polishing machine 20 through the supply line 70 .
[0006] In some applications, only one polishing machine 20 is fluidly connected to the slurry tank 80 . In other applications, a plurality of polishing machines 20 are connected to the same slurry tank 80 via supply lines 70 . In FIG. 1 , both possibilities are illustrated by use of brackets, where reference character “n” represents a whole number equal to or greater than 1. It will be appreciated that one pump 90 or a plurality of pumps could be utilized.
[0007] The capacity of the slurry tank 80 can vary from a few liters to hundreds of liters or more. The slurry tanks 80 in many commercial plastic lens polishing applications have a capacity of from about 35 to about 120 liters of polishing slurry 60 . The slurry tank 80 is typically fitted with a mixing device 100 , which helps prevent abrasive particles in the polishing slurry 60 from falling out of suspension and collecting as sludge in the slurry tank 80 . The mixing device 100 can be a mechanical stirrer or pump or a combination of thereof.
[0008] The slurry tank 80 typically comprises a cover 110 , which can be selectively opened or closed. The cover 110 , when closed, keeps unwanted matter from entering the slurry tank 80 and reduces the evaporation rate of the polishing slurry 60 . The cover 110 , when opened, permits an operator to replenish the polishing slurry 60 in the slurry tank 80 .
[0009] A polishing slurry 60 typically comprises abrasive particles that are dispersed and suspended in a carrier fluid. The carrier fluid typically comprises one or more chemical compounds that influence the rate at which a material on the surface 50 of the workpiece 30 can be physically abraded from the surface 50 of the workpiece 30 via the polishing pad 40 and/or the abrasive particles in the polishing slurry 60 .
[0010] Polishing slurries are a consumable component of the CMP process that must be periodically replenished. Polishing slurries are typically preformulated and then packaged in rigid containers for shipment to end users. When it is time to replenish the polishing slurry in a polishing apparatus, the rigid container containing the preformulated polishing slurry is vigorously shaken while sealed in order to resuspend abrasive particles that have settled within the container during storage. Alternatively, the rigid container is opened and the abrasive particles are resuspended by means of a mechanical mixing or stirring device. Once an attempt has been made to resuspend the abrasive particles that have settled during storage, the cover 110 of the slurry tank 80 is opened and the polishing slurry 60 is poured from the rigid container into a slurry tank associated with the polishing apparatus.
[0011] It can be difficult to resuspend substantially all of the abrasive particles of a polishing slurry that have settled within a rigid container by means of shaking or stirring. Accordingly, residues comprising abrasive particles that were not successfully resuspended are often retained on the walls of the rigid container after the flowable portion of the polishing slurry has been poured into the slurry tank. The retention of abrasive particles in the rigid container can upset the intended weight ratio/balances of abrasive particles in the polishing slurry. Furthermore, the container bearing the residues is typically discarded, which creates waste and disposal concerns.
BRIEF SUMMARY
[0012] In view of the foregoing, the present invention is directed towards methods and products for replenishing a polishing slurry in a chemical-mechanical polishing apparatus that overcome the foregoing problems associated with conventional containers. In accordance with the invention, the preformulated polishing slurry is packaged within a container having flexible walls. In the preferred embodiment of the invention, the container having flexible walls comprises a pouch formed of a flexible film. When it is time to replenish the polishing slurry in a polishing apparatus, an operator manually squeezes the sealed container, which causes deformation of the container walls. The deformation of the container walls leads to the rapid and substantially complete resuspension of the abrasive particles into the polishing slurry. Once the abrasive particles have been sufficiently resuspended, the container having flexible walls is unsealed and the polishing slurry is poured into a slurry tank associated with the polishing apparatus. The present invention substantially reduces the amount of abrasive particle residue remaining within the container once the polishing slurry has been poured into the slurry tank. The present invention also substantially reduces the amount of waste.
[0013] The foregoing and other features of the invention are hereinafter more fully described and particularly pointed out in the claims, the following description setting forth in detail certain illustrative embodiments of the invention, these being indicative, however, of but a few of the various ways in which the principles of the present invention may be employed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is a schematic representation of a polishing apparatus used in a CMP process.
[0015] FIG. 2 is front plan view of a preferred embodiment of a sealed flexible pouch containing a polishing slurry according to the invention.
[0016] FIGS. 3-5 are front plan views showing alternative embodiments of sealed flexible pouches containing polishing slurries according to the invention.
DETAILED DESCRIPTION
[0017] FIG. 2 shows a preferred embodiment of a sealed flexible pouch 120 containing a polishing slurry 60 in accordance with the invention. The polishing slurry 60 comprises abrasive particles 130 and a carrier liquid 140 . FIG. 2 b schematically illustrated an enlarged portion of the pouch 120 bounded by a circular area. The size and spacing of the abrasive particles 130 illustrated in FIG. 2 b is grossly exaggerated for the purpose of illustrating the invention. Conventionally, the abrasive particles 130 will have a very small diameter, which depending upon the particular application can range from a few nanometers to as large as several hundred microns. The composition of the abrasive particles 130 will depend upon the material to be removed from the workpiece 30 . Abrasives used in CMP include, for example, alumina, silica, ceria, copper oxide, iron oxide, nickel oxide, manganese oxide, silicon carbide, silicon nitride, tin oxide, titania, titanium carbide, tungsten oxide, yttria, zirconia, and combinations thereof.
[0018] The abrasive particles 130 are adapted to be suspended in the carrier liquid 14 such as, for example, water. However during shipment and storage of the pouch 120 , at least a portion of the abrasive particles 130 will settle out and no longer be suspended in the carrier liquid 140 . The settled abrasive particles 150 tend to collect in the corners, along the seams and/or within creases of the pouch 120 . Settling is generally considered to be a time-dependent factor. Thus, the longer the polishing slurry 60 contained within the pouch 120 is at rest, the more settling of the abrasive particles that is likely to occur.
[0019] As noted above, polishing slurries are conventionally packaged, shipped and stored in containers having substantially rigid walls (e.g., buckets, plastic jugs, jars etc.). It can be very difficult to resuspend and thus redisperse the settled abrasive particles in such containers via shaking and stirring. In many cases, a portion of the abrasive particles cannot be resuspended, and remains as a residue within the container. This residue is discarded together with the container.
[0020] In accordance with the present invention, the polishing slurry 60 is contained within a sealed flexible pouch 120 having walls that are adapted to be repeatedly deformed (e.g., by squeezing or kneading using one's hands). In order to facilitate deformation of the pouch 120 , at least a portion of the pouch 120 is preferably formed of a flexible polymeric film. More preferably, most of the pouch 120 is formed of a flexible polymeric film. The composition of the polymer or polymers used to form the polymeric film is not per se critical. Examples include polymeric films comprising polyethylene (e.g., linear low density polyethylene—“LLDPE”), ethylene vinyl acetate (“EVA”) polyesters and various other flexible film-forming polymers, copolymers and blends of polymers. The films can be formed of a single layer of one polymer, or can be formed as laminates of two or more layers of different film materials. It is preferable for at least a portion of the flexible polymeric film to be transparent, which allows for visual confirmation that substantially of the settled abrasive particles have been substantially resuspended via repeated deformation of the sealed flexible pouch.
[0021] In the embodiment of the invention illustrated in FIG. 2 , the sealed flexible pouch 120 contains a polishing slurry 60 within a cavity 160 bounded substantially entirely by polymeric film. In the embodiment shown in FIG. 2 , the pouch 120 has been formed by folding a polymeric film on itself and welding the folded polymeric film to itself along weld lines 170 so to define the cavity 160 . The pouch 120 shown in FIG. 2 further comprises an opening 180 bounded entirely by weld lines, which can be used as a handle to lift the sealed flexible pouch 120 . The sealed flexible pouch 120 also further comprises a notch 190 , which facilitates tearing of the polymeric film at the weld line 170 to allow the polishing slurry 60 contained within the cavity 160 to be poured from the pouch 120 . The notch 190 can be provided proximal to a narrowed portion 200 of the cavity, which facilitates pouring the polishing slurry 60 from the pouch 120 .
[0022] FIGS. 3-5 show alternative embodiments of pouches 120 containing polishing slurries 60 according to the invention. The same reference numbers utilized in FIG. 2 are used to identify similar structures in FIGS. 3-5 . The pouch 120 shown in FIG. 3 includes a rigid spout 210 , which is welded into pouch 120 . The spout 210 is covered by a cap 220 , which is threadingly received on the spout 210 . The cap 220 can be removed to unseal the pouch 120 and then replaced to reseal the pouch 120 .
[0023] The pouch 120 shown in FIG. 4 includes weld lines 170 that completely surround the cavity 160 . The pouch 120 shown in FIG. 4 differs in this respect from the pouches 120 shown in FIGS. 2 and 3 , which include a base portion 230 that is created by folding the flexible polymeric film and not by welding. The pouch 120 shown in FIG. 4 also does not include a spout or notch. Instead, the pouch 120 shown in FIG. 4 is provided with indicia 240 , which indicates where the pouch 120 should be cut or sliced in order to allow for the polishing slurry 60 to be poured from the cavity 160 . The pouch 120 shown in FIG. 4 also includes an opening 180 bounded by weld lines 170 , which can serve as a handle.
[0024] The pouch 120 shown in FIG. 5 includes a spout 210 and a cap 220 . Furthermore, the pouch 120 shown in FIG. 5 includes a cavity 160 that is bounded entirely by weld lines 170 , except for the portion containing the spout 210 . It will be appreciated that there are literally unlimited configurations (size, handles, spouts, closures, markings for volume, shapes, stand-up, pillows, labels, color, etc.) of pouches that can be utilized in accordance with the invention.
[0025] The cavity 160 of a sealed flexible pouch 120 preferably contains more than 1 liter but less than 10 liters of the polishing slurry 60 . It is preferable for the cavity 160 not to be entirely filled to capacity with the polishing slurry 60 . This allows the walls of the pouch 120 to be deformed by squeezing or kneading, which causes the polishing slurry 60 within the cavity to mix and become homogeneous. This also helps dislodge settled particles 150 , which can more easily become resuspended in the carrier liquid 140 . For ease of handling, pouches 120 containing from about 1.0 to about 3.0, or most preferably about 1.9 liters, are preferred.
[0026] The pouches 120 can be pre-manufactured and simply filled with preformulated polishing slurry 60 and sealed. Alternatively, the pouches 120 can be formed immediately prior to being filled with a polishing slurry 60 . The pouches 120 can be filled using rotary or in-line filling machines, which are well know. Alternatively, the pouches 120 can be filled manually and sealed using a heated platen or RF welding equipment.
[0027] As noted, the sealed flexible pouches advantageously allow settled particles to be resuspended in the carrier liquid by squeezing, kneading or tilting the pouch back and forth. The manipulation or massaging of the pouch loosens the settled particles and thoroughly mixes the polishing slurry to form a substantially homogeneous mixture, which can then be easily poured into the slurry tank of a polishing apparatus. Little to no residue is left behind in the pouch, which is a significant improvement as compared to the use of conventional containers having rigid walls. After the polishing slurry has been poured from the pouch, the pouch can be discarded.
[0028] Pouches containing polishing slurries according to the invention are substantially more environmentally friendly than conventional polishing containers having rigid walls. They take up less warehouse/storage space. They produce less waste volume at the time of disposal. They reduce shipping costs due to weight reductions. They can be formed using <40% of the polymer necessary to form convention rigid containers.
[0029] In addition, they provide advantages to the end user. The pouches are easy to handle during the filling operation. Substantially all of the abrasive particles are resuspended, leaving virtually no residue in the pouch after the filling operation. This preserves the desired balance or ratio of abrasive particles to carrier liquid.
[0030] Thus, the present invention provides a method for replenishing a polishing slurry in a chemical-mechanical polishing apparatus having a slurry tank. The method comprises:
providing a sealed flexible pouch containing a polishing slurry comprising abrasive particles and a carrier liquid, wherein the abrasive particles are adapted to be suspended in the carrier liquid but at least a portion of the abrasive particles are not suspended in the carrier liquid; repeatedly deforming the sealed flexible pouch for a time sufficient to suspend substantially all of the abrasive particles in the carrier fluid;
[0033] unsealing the repeatedly deformed flexible pouch; and
[0034] pouring at least a portion of the polishing slurry from the unsealed flexible pouch into the slurry tank of the chemical-mechanical polishing apparatus.
[0035] The repeatedly deforming step can be performed manually by repeatedly squeezing and releasing less than the entire sealed flexible pouch in one's hands so as to cause the polishing slurry contained in the cavity of the pouch to pulse back and forth between squeezes. The contents of the pouch can also be mixed by repeatedly tilting the sealed flexible container back and forth to thoroughly mix the polishing slurry contained therein. Automatic mixing equipment (shakers etc.) and sonic devices can also be utilized, if desired.
[0036] In a preferred application, the polishing slurry dispensed between a polishing pad and a blank used to form a plastic optical lens. In such applications, a central slurry tank (also known in the art as a “process tank”) is connected through distribution lines to a plurality of polishing apparatus. When the polishing slurry volume in the slurry tank drops to a predetermined level, the tank volume can be replenished in accordance with the method of the invention.
[0037] Additional advantages and modifications will readily occur to those skilled in the art. Therefore, the invention in its broader aspects is not limited to the specific details and illustrative examples shown and described herein. Accordingly, various modifications may be made without departing from the spirit or scope of the general inventive concept as defined by the appended claims and their equivalents.
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Methods and products for replenishing a polishing slurry in a chemical-mechanical polishing apparatus. A preformulated polishing slurry is packaged within a container having flexible walls. When it is time to replenish the polishing slurry in a polishing apparatus, an operator manipulates the sealed container by hand, which causes deformation of the container walls. The deformation of the container walls leads to the rapid and substantially complete resuspension of the abrasive particles into the polishing slurry. Once the abrasive particles have been sufficiently resuspended, the container having flexible walls is unsealed and the polishing slurry is poured into a slurry tank associated with the polishing apparatus.
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FIELD OF INVENTION
[0001] The invention relates to a method to protect against manipulated charging signaling data in IMS networks.
SUMMARY OF THE INVENTION
[0002] More recent communication architectures provide for the separation of switching networks into connection-service-related units and for the transportation of the user information (bearer control). This results in a decomposition/separation of connection setup and medium or bearer setup. The user information (switching of the user channel) can in this case be transmitted using various high-bitrate transportation technologies such as ATM, IP or Frame Relay.
[0003] Such a separation enables telecommunications services currently conducted in narrowband networks to also be implemented in broadband networks. In this case the users are connected either directly (e.g. using a DSS1 protocol) or via exchanges designed as media gateway controllers (MGC) (e.g. using the ISUP protocol). The user information itself is converted into the transportation technology used in each case via media gateways (MG).
[0004] The media gateways are controlled by media gateway controllers (MGC) assigned in each case. In order to control the media gateways the media gateway controllers use standardized protocols, e.g. the MGCP protocol or the H.248 protocol. To communicate with each other the media gateway controllers use a BICC (Bearer Independent Call Control) protocol standardized by the ITU, which is formed from a plurality of standardized protocols and thus comprises a protocol family.
[0005] A protocol suitable for the BICC protocol has emerged from the IETF standardization committee in the shape of the SIP protocol (RFC3261) or the add-on SIP-T (RFC3204). The latter—unlike the SIP protocol—enables ISUP messages to be transmitted. The ISUP messages are generally transmitted through tunnels, i.e. through transparent transfer.
[0006] The connection setup between two or more SIP users is effected with the aid of SIP protocol elements. Among other things, SDP (Session Description Protocol) data is exchanged here. SDP data is (bearer) end-point-related data containing information on codecs, IP port, IP address, etc. If a connection is to be set up between an SIP user and an H.323 or TDM/ISDN user, these SIP protocol elements must be converted accordingly into H.323, TDM or ISDN protocol elements in the participating media gateway controllers. For example, for a TDM user called from the SIP environment this means that the ISUP messages used in the TDM environment, such as the ISUP message IAM (Initial Address Message) for example, must be created and forwarded thereto.
[0007] Initial basic considerations resulted in the standard Q.1912.5 “Interworking SIP and BICC/ISUP” in the ITU-T. Nothing is said there about charging. The function of the BGCF ( FIG. 2 ) is described in section 4.6.4 of the 3GPP specification 3GPP TS 23.228 V6.8.0 (2004-12) and in 3GPP TS 23.002 V6.5.0 (2004-06). In particular an architecture as shown in FIG. 3 is laid down in the IMS (IP multimedia sub-system). This describes how a connection to the terminal of another network operator is established by the SIP terminal UE (User Equipment) of a network operator with the aid of a plurality of functionalities such as for example the BGCF function. CDR-relevant signaling information (charging data record, charging data) is exchanged to this end between the various functionalities.
[0008] The CDR information (CDR tickets) contains information on sender and recipient, in other words which users and operators are involved, which network elements are included in the connection path, etc.
[0009] The problem is now that exchanging the CDR tickets by intentionally changing the data contained therein represents a potential risk. This possible misuse can arise in that the charging data is manipulated.
[0010] The object of the invention is to specify a way in which the risk of misuse when setting up a connection for an SIP terminal across network boundaries can be minimized.
[0011] The object is achieved by the claims.
[0012] The advantage of the invention is that the charging information (CDR tickets) as per TS 24.229 is not automatically accepted by the BGCF function on receipt. Instead this is made dependent on which unit the SIP signaling message was received from.
[0013] The invention is described in greater detail below on the basis of an exemplary embodiment represented in the figures.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 shows the basic relationship between two PSTN users, between whom an internet network is arranged,
[0015] FIG. 2 shows the description of the BGCF function as per standard TS24.229, and
[0016] FIG. 3 shows the IM subsystem as per standard TS24.229.
DETAILED DESCRIPTION OF THE INVENTION
[0017] FIG. 1 shows a network configuration on which the inventive method is executed. Two PSTN networks are disclosed here by way of example, in each of which a plurality of PSTN users is arranged in known fashion. These are routed to local exchanges LE, which in turn are connected to transit exchanges TX.
[0018] The separation between signaling information and user information is now effected in the transit exchanges TX. The signaling information is fed from the transit exchange TX directly via an ISUP protocol to a media gateway controller MGC (MGC A or MGC B) assigned in each case. The user information is transmitted to an (input-side) media gateway MG (MG A or MG B), which acts as an interface between TDM network and an ATM or IP transmission network and is transmitted in packet-oriented form via the relevant transmission network. The media gateway MG A is controlled by the media gateway controller MGC A in the same way as the media gateway MG B is controlled by the media gateway controller MGC B. If the user information is transmitted from the media gateway MG A to the media gateway MG B the user information is again converted into a TDM data stream under the control of the media gateway controller MGC B assigned to the media gateway MG B and is fed to the PSTN user in question. The data transmitted between the media gateway controller MGC and the media gateway assigned in each case is supported by a standard protocol. This can be the MGCP or the H.248 protocol, for example. The SIP is preferably used between the two media gateway controllers MGC A, MGC B in accordance with the present exemplary embodiment. Further devices such as SIP proxies or SIP units SIP E can be inserted into the signaling path.
[0019] FIG. 2 shows the definition and tasks of the BGCF (breakout gateway control function) functionality as per the 3GPP TS 23.002 V6.5.0 (2004-06) standard. This function is executed on a configuration which is shown in FIG. 3 . The device CSCF here represents with the device P-CSCF an SIP proxy, as shown in FIG. 1 , while the MGCF functionality is executed in a media gateway controller MGC.
[0020] The BGCF function (Breakout Gateway Control Function) selects the network (domain, e.g. PSTN) to which the call outgoing from an SIP terminal UE should be routed. If the BGCF function ascertains that the destination is in its own network, i.e. in the network in which the BGCF function is arranged, the BGCF function selects an MGCF functionality which is responsible for interworking with the PSTN network. If the destination is in another network, the BGCF function forwards the signaling to the other network.
[0021] The BGCF function thus has the following tasks:
1. Receipt of the acknowledgement from the serving function S-CSCF to select suitable PSTN networks (domains). 2. Selection of the interconnection point at which the interworking with the PSTN network should take place. If the interworking should take place at another interconnection point, the BGCF function forwards the SIP signaling to the BGCF function of this network. 3. Selection of the MGCF functionality in the network in which the interworking with the PSTN network takes place and forwarding the SIP signaling to this MGCF functionality. 4. Creating the CDR (Charging Data Record, charging data).
[0026] The BGCF function can here use either information which it obtains from other protocols or administration information if it determines in which network the interworking should take place.
[0027] The invention now provides for the BGCF function to be enhanced such that it additionally does not automatically accept the charging information (CDR tickets) as per TS 24.229 on receipt, but instead carries out a check as a function of which unit the SIP signaling message was received from. The following method steps are performed:
1) The BGCF function receives the charging-relevant signaling data, 2) The BGCF function has a database (local or external) containing entries: [Entry attribute 1 ] [Entry attribute 2 ] attribute 1 [origin address (IP address/domain name/subdomain) of the interconnection point (which here would be MGCF of another network)] attribute 2 [IOI of the operator belonging to the origin address] 3) The BGCF function extracts the origin of the signaling message, e.g. from the SIP VIA header, 4) The BGCF function uses this to search the entries in Entry attribute 1 (i.e. address) in the database, 5) The BGCF function finds an entry and in this line fetches the entry attribute 2 (i.e. IOI (interoperator identifier)), 6) The BGCF function compares e.g. the IOI signaled in SIP with the entry attribute 2 (i.e. IOI).
[0037] If the comparison is positive, no manipulation is ascertained (the data in the CDR is interpreted as correct) and the message is sent onward unchanged (as regards charging-relevant data). If the comparison is negative, a manipulation is assumed and an attempt at manipulation exists (if the data has not been/is not being incorrectly administered). The BGCF function then overwrites the received signaling information, here for example IOI, by the entry in attribute 2 and sends this overwritten signaling information internally to the CDR software system with the indication that manipulation had taken place. Externally the correspondingly amended signaling information is forwarded via SIP, so that other units likewise receive the correct information. Alternatively the connection can be cleared down when manipulation is identified.
[0038] In this way the receiving operator/network operator is protected against incorrect charging tickets. The proposed solution prevents the relevant network operators from receiving invalid CDRs when using Com Version FMC2.0 (fixed mobile conversion). In particular the checking function described above by way of example is not restricted to a BGCF and interworking with the PSTN, but should also be logically possible for IMS/IMS calls.
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Method to protect against manipulated charging signaling data in IMS networks In the prior art CDR tickets are exchanged between devices/functionalities of an IMS system. This can result in manipulations. The invention reduces the likelihood of manipulation, in that the BGCF function of the IMS system is enhanced such that it accepts the charging-relevant signaling data as per TS 24.229 from the sender only if this was sent by the correct sender.
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BACKGROUND
The present invention relates to a cooling device with an air guide for a vehicle engine radiator and notably to a device that can incorporate a shut-off device with moving flaps.
Various cooling devices comprising moving flaps, of the venetian blind type, the closure of which is controlled so as to be able to manage CO 2 emissions, are known. This is because it is known that letting air in over a front bumper impairs the aerodynamic drag coefficient SC x and therefore increases the CO 2 emissions of the vehicle. Motor manufacturers have therefore sought to position moving flaps on the air circuit, but the positioning of these moving flaps presents numerous problems in the compact environment of the front end of a vehicle where there are numerous other requirements that have to be met, notably in terms of impact protection, notably pedestrian impact. Thus, a moving flap positioned in or too close to the air intake grille is unsatisfactory: there is a risk that the flap will be damaged in the slightest impact, with high replacement costs involved in the repair. A flap borne by or incorporated into the technical front panel of the vehicle presents problems of fragility and what is more does not lend itself well to a construction that is standardized across various models given that the technical front panel is very closely tied to the design of the vehicle, made entirely of sheet metal and expensive.
Document EP 2080658 discloses a radiator cooling device intended to be mounted at the front of a motor vehicle between a radiator and a bumper skin equipped with an air inlet, of the type comprising from said air inlet as far as said radiator, an air guide fixed to structural parts of the vehicle and housing a device with flaps for shutting off the air arriving at the radiator as required. According to that document, the air guide and its shut-off means are designed to contribute in the absorption of energy in the event of an impact, which they have to do given that the shut-off means are positioned more or less at the level of the air inlet made in the bumper, with nowhere to retreat to in the event of an impact. The shut-off device is incorporated into the walls of the air guide, and the latter bears against the inside of the front bumper skin and has surfaces intended, in the event of an impact, to rest on the front and on the top of the transverse impact beam that forms part of the structure of the vehicle. This construction has the disadvantage of being specifically tied to each model of vehicle and of leaving the shut-off flaps exposed to all impacts, including low-speed impacts.
BRIEF SUMMARY
It is an object of the invention to propose an improved radiator cooling device, with an air guide construction that allows easier adaptation to suit various models of vehicle.
The invention achieves its goal through the use of a radiator cooling device intended to be mounted at the front of a motor vehicle between a radiator and a bumper skin equipped with an air inlet, of the type comprising from said air inlet as far as said radiator, an air guide fixed to structural parts of the vehicle, a device with mobile flaps for shutting off the air arriving at the radiator as required being housed as appropriate in the air guide, characterized in that the air guide comprises at least one front part and a rear part, in that said rear part is fixed to said structural parts and comprises an accepting zone designed to accept, as appropriate, said shut-off flaps device, and in that means are provided for fixing said shut-off flaps device in said rear part.
In a particularly advantageous version, the two, respectively front and rear, parts are separate and fitted with means of attaching one to another, by virtue of which it is easier to access the accepting zone in order, as appropriate, to fit the shut-off flaps device.
Advantageously, the shut-off flaps device is in the form of a removable standalone cassette that can be positioned inside the air guide or not, as desired, when the vehicle is being built, according to the cooling requirements. The cassette comprises a flaps actuator, advantageously laterally offset away from the air inlets, allowing maximum intake of air and limiting the risks of collision between the actuator and the radiator situated behind it. The rear part of the air guide therefore advantageously comprises an opening on the side through which to pass the actuator supply cable.
Advantageously, said means of attaching said shut-off flaps device into said rear part are coincident with the means of attachment of the rear part and of the front part one to the other, so that once the shut-off flaps device has been positioned in the rear part, all that is required is for the front part to be positioned and attached and the shut-off flaps device will itself become locked in position. In other words, attachment of the front and rear parts of the air guide traps the controlled-flaps cassette between the two parts via end stops.
These means of attachment may notably be by screw-fastening or by clip-fastening.
In a practical way, a bearing zone against which the shut-off flaps device can abut when the front part of the air guide is being attached to the rear part is provided in the rear part of the air guide, said front part likewise comprising a zone for bearing against the shut-off flaps device.
Advantageously, the rear part of the air guide which houses the shut-off flaps device comprises, at the front, a bearing zone for the rear of the front part, which is more or less aligned with the front face of the shut-off flaps device so that if the shut-off flaps device is not present, the position in which the front part is assembled with the rear part is substantially the same as it is when the shut-off flaps device is present. It is thus possible to use the same rear part and the same front part of air guide, whether the choice has been made to fit or not to fit the shut-off flaps device.
Advantageously, the rear part of the air guide and the shut-off flaps device are the same for several models of vehicle having a similar engine architecture, this standardization being made possible by the two-part structure of the air guide. By contrast, the front part of the air guide may be specific to each model, according to the design of the vehicle.
Advantageously, the front part of the air guide comprises sealing lips for pressing against the skin of the bumper.
Advantageously, the rear part of the air guide comprises two box sections, respectively a lower and an upper box section, opening into a manifold suited to the size of the radiator, the two sections straddling the impact beam.
Advantageously, the shut-off flaps device is positioned in the lower box section, because this is in theory the main air inlet, and substantially in vertical alignment with the impact beam, giving it good resistance to impacts, notably front end impacts at under 16 km/h (Danner impacts).
Advantageously, the rear part of the air guide is fixed to the transverse impact beam and/or to the lower part of the bumper.
The invention makes it possible to improve the CO 2 emissions of a vehicle by using an optional mobile-flaps module that can be incorporated into an existing architecture, using a solution that is economical insofar as the rear part of the air guide and the flaps cassette are standardized. The cassette is optional and it is possible for vehicles intended to be marketed in countries where the regulations do not set a tax on CO 2 emissions not to be fitted with it: however, in such a case, the air guide is used with its front and rear parts, simply plugging the lateral control cable outlet hole; the overall fluidtightness of the air guide according to the invention is improved in relation to conventional vehicles without controlled flaps.
Moreover, because the mobile flaps module is prepared at the preparation workshop, installing it does not make any appreciable difference to the production time on the main assembly line.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features and advantages of the invention will become apparent from the following description of a number of exemplary embodiments. Reference will be made to the attached drawings in which:
FIG. 1 is a cut-away perspective view of the front of a vehicle in which the invention can be fitted,
FIG. 2 is a perspective view of the rear air guide according to the invention and of the mobile flaps cassette it houses in its lower part,
FIGS. 3 and 4 are perspective views of the rear air guide and of the cassette of FIG. 2 , respectively,
FIG. 5 is a schematic view in longitudinal vertical section of an alternative form of embodiment of the device according to the invention,
FIG. 6 shows an exploded view of one particular embodiment of how the mobile flaps cassette is installed in the air guide,
FIG. 7 is a cross section of another particular embodiment of how the mobile flaps cassette is installed in the air guide.
DETAILED DESCRIPTION
FIG. 1 illustrates the front of the engine compartment at the front of a vehicle of a conventional type to which the invention may be applied. From the rear forward, there are:
The technical front end 1 which acts as a vertical support for a certain number of components and is fixed securely to structural elements of the chassis, for example to components connected to the chassis frame side rails 2 . The vertical radiator 3 , fixed with overhang on the technical front end 1 . The transverse impact beam 4 which is connected in a way that has not been depicted to structural elements of the chassis, theoretically to the front of the chassis frame side rails 2 . The impact beam cuts across the space in front of the radiator 3 . The shock absorber 5 of the bumper 6 , here in the form of two, lower and upper, transverse section pieces. The upper section piece here is situated in front of the impact beam 4 . The bumper 6 comprises, in the usual way, a front face, wrap-around ends and a lower spoiler part which continues rearward under the front of the vehicle.
In the bumper 6 , an opening (at least), and in this instance two openings 7 . 1 and 7 . 2 , allow cooling air to enter, which air is then directed toward the radiator 3 by a suitable air guide 8 . In practice, the inlet 7 . 1 may be the main inlet and the inlet 7 . 2 may or may not be used.
As can be seen clearly in FIGS. 2, 3 and 5 , because of the presence of the impact beam 4 , the air guide 8 is advantageously, in the vicinity of said beam, in the form of a U-shaped box section straddling the beam and having a lower passage part in the form of a box section 8 . 1 and an upper passage part in the form of a box section 8 . 2 these lying respectively below and above the beam 4 and both opening downstream into a common manifold 9 suited to the surface area of the radiator 3 in front of which it is positioned with suitable sealing contrivances. These box sections 8 . 1 , 8 . 2 and the manifold 9 form the rear part of the air guide of the invention, which is supplemented upstream by a front air guide intended to contain the air in a substantially fluidtight manner between the air inlets 7 . 1 and 7 . 2 and the rear part 8 . 1 , 8 . 2 , 9 , for example in the form of box sections 10 . 1 and 10 . 2 , provided with a suitable seal toward the front (cf. FIGS. 2 and 3 ).
According to the invention, the air guide 8 , particularly the lower part 8 . 1 thereof, which corresponds to the main air inlet 7 . 1 , may, thanks to suitable positioning and immobilizing means, house a cassette 20 of mobile shut-off flaps which are controlled by a lateral control device 21 ( FIGS. 2, 4 and 5 ). Such a cassette may be in the form of a rectangle as can be seen in FIG. 4 . It is also possible to provide another cassette in the upper part 8 . 2 but the lower flow rate passing through that does not necessarily justify such an approach. The lateral control device 21 is supplied by a cable, not depicted, passing through a lateral opening, likewise not depicted in the lower box section 8 . 1 of the air guide.
FIG. 5 schematically depicts a slightly different embodiment again showing the beam 4 and the lower box section 8 . 1 situated under the beam and opening into a manifold 9 of the size of the radiator 3 . In this solution, the upper box section has simply been omitted. The mobile flaps cassette 20 is housed in the single lower box section 8 . 1 against a peripheral end stop 22 sealed against air. Lines 23 , 24 indicate the potential regions at which the air guide can be attached to the beam 4 (lines 23 ) and/or, in the lower part, to the spoiler of the bumper 6 (lines 24 ).
FIG. 6 shows the rear part of a preferred embodiment of air guide of the invention, intended to straddle the impact beam, not depicted, and made up of an upper and a lower box section 8 . 1 and 8 . 2 and of the rear manifold 9 . This assembly may be of a single piece or as several assembled pieces. As has been seen, the box section 8 . 1 accommodates the cassette 20 the shape of which is designed to fit exactly into said box section and press against a continuous peripheral end stop arranged on the internal surface of the box section 8 . 1 , all of this being so as to achieve airtightness simply by pressing. The cassette 20 is held in position, more or less in vertical alignment with the impact beam, by closing the assembly using the front part 10 . 1 of the air guide which is attached to the assembly by four self-tapping fixing screws 25 which go through lugs 26 ′ on the front part 10 . 1 and screw into barrels 26 made of soft material formed on the exterior surface near four corners of the peripheral internal end stop of the box section 8 . 1 . This attachment keeps the front guide 10 . 1 , the cassette 20 and the rear guide 8 . 1 all pressed against one another in an airtight manner. According to the invention, the rear part of the air guide 8 . 1 , 8 . 2 , 9 is intended to be the same for all engines of the same range of vehicles and, as required, will either house or not house a mobile flaps cassette 20 . The front part 10 . 1 on the other hand is a component specific to each model of car because it is dependent on the design of said car.
FIG. 7 shows a solution using clip-fastening rather than screw-fastening. Again, it shows the rear part of the air guide 8 . 1 , 9 facing the radiator 3 , with the cassette 20 pressed in an airtight manner against the internal end stop 22 . The front part of the box section 8 . 1 on its edge 31 comprises flexible snap-fixing tabs 27 with hooks 28 pointing forward and able to clip into openings 29 provided on a transverse rim 33 formed at the rear of the front component 10 . 1 . The edge 31 also comprises, on each side, end stops 32 intended to block the rearward movement of the transverse rim 33 of the front component 10 . 1 of the air guide so that this component will maintain substantially the same position along the X axis regardless as to whether or not the cassette 20 is present. What is more, the component 10 . 1 comprises, at the front, a flexible lip 30 intended to press against the inside of the skin of the bumper 6 , around the air inlet opening 7 . Once again, the front part 10 . 1 is a component specific to each model of car, whereas the rear part is a part that is common to an entire range of models having the same engine architecture.
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A device for cooling a radiator, including an air guide attached to structural portions of a vehicle and a device having movable air-blocking flaps, the air guide includes at least two separate portions: a front portion and a rear portion, respectively, which include a mechanism for mutual attachment, the rear portion being attached to the structural portions and including a receiving area configured to receive the device having blocking flaps, the entire assembly being held in place by an attachment mechanism of the front portion onto the rear portion.
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This application is a continuation of application Ser. No. 919,223, filed Oct. 15, 1986, now abandoned.
BACKGROUND OF THE INVENTION
This invention relates to an apparatus for treating a dyed or printed textile web with a liquid such as a washing or rinsing solution.
German Patent No. 830 040 discloses in principle a technique of spraying a treatment solution onto a moving textile web at several points spaced one behind the other along the direction of transport of the web, most of the solution applied at any particular spray station being removed from the fabric by suction before additional solution is applied to the web at a further point. In German Patent No. 830,040, the textile web is conducted freely, under small looping angles, along successive spray and suction pipes or over a suction drum, over the circumference of which drum spray pipes acting radially inwardly are distributed. Such a treatment of a fabric requires that the web have a minimum textile strength. Accordingly, the treatment is unsuitable for material such as knitted fabrics.
As disclosed in German Patent Document (Offenlegungsschrift) No. 23 62 109, an endless sieve belt passes over a pair of guide drums disposed at the same horizontal level, the cloth being spread out on an upper section or segment of the belt so that the cloth can be guided on the belt while the cloth is lying flat and completely slack. Above the upper section of the sieve belt, spray pipes are arranged for applying a washing or rinsing liquid to the cloth lying on the belt. Subsequently, the applied liquid, laden with dirt or dye residues, is removed by suction through the cloth and through the sieve belt.
The distance between the point of application of the liquid and the suction point is relatively short, with the consequence that the liquid has little time to act on the substances which are to be removed from the web.
German Petty Patent (Gebrauchsmuster) No. 17 40 815 discloses a boot-like water-filled washing chamber in which chamber the fabric is placed in a stacked configuration in order to lengthen the contact time of the washing liquid with the substances to be removed from the fabric web. This procedure, however, is unsuitable for many applications, exemplarily in the case of knitted materials, such knitted materials being difficult to draw out of the stack because of the sensitivity of the material to tension. The solution of the Gebrauchsmuster is also unsuitable in the case that the web is provided with printed matter, smudges in the printed matter arising upon stacking of the web.
An object of the present invention is to provide an improved apparatus of the above-described type.
Another, more particular, object of the present invention is to provide such an apparatus in which a washing or rinsing may be adequately effectuated without maintaining the textile web in a stacked configuration.
SUMMARY OF THE INVENTION
An apparatus for treating a dyed or printed textile web with a liquid comprises, in accordance with the present invention, a conveyor, a liquid applicator, a suction device and a dwell stretch. The conveyor includes an endless sieve belt for transporting the textile web along a predetermined substantially horizontal path. The applicator is disposed at a first station along a path for applying the liquid to the web during motion thereof along the path. The suction device is disposed at a second station along the path at a point downstream of the first station for removing the liquid from the web by a suction process during motion of the web along the path. The suction device preferably extends transversely to the web and to the belt and is disposed below and substantially juxtaposed to an upper section of the belt. The dwell stretch is disposed between the applicator and the suction device for conducting the textile web in a spread-out condition and in a single layer through at least one dwell loop.
In a fabric treatment apparatus in accordance with the present invention, the action time of the applied liquid on the substances to be removed from a fabric or textile web is lengthened. In one kind of application, a printing thickener has more time to swell. Because of the greater time that the washing or rinsing liquid has to act on the substances to be removed from the web, a surprising improvement of the washing effect can be achieved. Moreover, owing to the spread-out condition and the single-layer configuration of the textile web in the dwell loop, the tension in the textile web can be maintained at a small level.
In the case of printed material, a fabric treatment apparatus in accordance with the present invention is especially advantageous in that effective washing is possible without soiling a white background, inasmuch as the washing solution is spread onto the textile web and the cloth is neither placed into a stacked configuration nor run through a vat or the like.
A preferred area of application of the invention is so-called "soilage washing," because considerable amounts of soilage can be removed at relatively little expense. A fastness treatment as such may follow a washing operation in accordance with the invention.
In a particular embodiment of a fabric treatment apparatus in accordance with the present invention, the dwell stretch device is formed by an air pass, wherein the textile web is completely free of support or guiding elements at least along major portions of the dwell stretch or loop and is accordingly accessible to the atmosphere at all sides. An air pass may be formed in a known manner by a plurality of freely rotatable rollers arranged in two planes above the upper section of the sieve belt for guiding the web in a plurality of vertically extending loops above the upper section of the belt.
In an alternative embodiment of a fabric treatment apparatus in accordance with the present invention, the dwell stretch includes at least one freely rotatable drum disposed above the upper section of the sieve belt. The dwell loop extends around the drum. The dwell stretch further includes at least two rollers disposed laterally adjacent to one another below the drum for guiding the web to and from the drum. This particular embodiment of the fabric treatment apparatus in accordance with the invention is especially suitable for certain less resistant materials such as knitted fabrics. The web is conducted along a meander path from the belt path and back to the belt. The drum and rollers enable the textile web to be guided with particularly little tension.
A fabric treatment apparatus in accordance with the present invention can have a compact construction, particularly if the textile web is guided back from the dwell loop to the sieve belt at a point downstream and closely adjacent to the point where the web leaves the belt.
The suction device is advantageously disposed near the point of return of the web to the sieve belt. The suction device causes the textile web to adhere to the belt and to be entrained thereby. This entrainment of the textile web by the belt is sufficient to guide the web over several rollers not exhibiting any buoyance, or over drums, without any appreciable longitudinal tensile stresses occuring in the web.
Advantageously, in the second embodiment, the drum is made of a sieve material. However, other drum designs such as slats may also be utilizable in accordance with the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partially schematic side elevational view of a fabric treatment apparatus in accordance with the present invention.
FIG. 2 is a partially schematic side elevational view of another fabric treatment apparatus in accordance with the present invention.
DETAILED DESCRIPTION
As illustrated in FIG. 1, a fabric treatment apparatus 100 comprises a scaffold type machine frame 1. A first guide drum 2 is rotatably mounted to machine frame 1 at an inlet side thereof, while a second guide drum 3 is rotatably mounted to machine frame 1 at an outlet side thereof. Guide drums 2 and 3 have essentially the same diameter and are arranged at approximately the same height above a floor base. An endless sieve belt 4 partially surrounds guide drums 2 and 3, sieve belt 4 having an upper section 4' extending approximately horizontally from guide drum 2 to guide drum 3. Guide drum 3 is driven to move upper section 4' of belt 4 from left to right in the drawing. Guide drum 2 is adjustable for tensioning sieve belt 4, as indicated by an arrow.
A gas-permeable textile web 10, arriving at fabric treatment apparatus 100 from a pretreatment apparatus such as a dying unit or a printing unit (not illustrated), is guided via a tension-compensating roller 5 into apparatus 100 over a full-width roller 6 and immediately thereafter onto sieve belt 4. Textile web 10 is guided in a single layer in a spread-out state and lies tensionless on upper section 4' of sieve belt 4. Textile web 10 then passes a spray pipe 7 having spray nozzles 8 distributed over the width of web 10, a washing or rinsing liquid being applied via nozzles 8 to the top side of textile web 10 substantially uniformly over the width thereof.
Subsequently, while being maintained in a single-layer spread-out state, textile web 10 passes through a dwell stretch W in the form of a so-called air pass 9. Air pass 9 includes a trio of lower rollers 11 closely juxtaposed to but not engaging each other and a pair of upper rollers 12 arranged at a distance 13 above lower rollers 11. Textile web 10 is guided between the lower rollers 11 and upper rollers 12 to form a pair of vertically extending dwell loops. Rollers 11 and 12 are all rotatably mounted to machine frame 1 and are entrained by textile web 10. In the short horizontal distance between the outer rollers of the lower trio of rollers 11, textile web 10 traverses a considerable dwell stretch corresponding to a multiple of distance 13, depending on the number of vertical dwell loops 14. Distance 13 is advantageously 1 to 2 meters.
As soon as textile web 10 again rests horizontally on upper section 4' of sieve belt 4 after passing the last roller of the lower trio of rollers 11, the web passes a suction device 15 provided with a suction pipe and a suction slit 16. Suction device 15 removes by suction, through textile web 10 and upper section 4' of sieve belt 4, the liquid applied by spray pipe 7 together with the greater part of the substances to be eliminated from the textile web.
Spray pipe or liquid applicator 7, air pass 9 and suction device 15 together form an assembly unit 17. As illustrated in FIG. 1, two further assembly units 17' and 17" are spaced from one another and from assembly unit 17 along the path defined by upper sieve belt section 4'. Assembly unit 17' comprises a liquid applicator 7', a dwell stretch W' in the form of an air pass 9' and a suction device 15'. Air pass 9' includes four lower rollers 11' and 3 upper rollers 12', lower rollers 11' being spaced distance 13 from upper rollers 12'. Assembly unit 17" comprises a liquid applicator 17", a dwell stretch W" in the form of an air pass 9" and a suction device 15". Air pass 9" comprises a set of four lower rollers 11" spaced distance 13 from a set of three upper rollers 12". Textile web 10 passes through three dwell loops 14' and another three dwell loops 14" in assembly units 17' and 17", respectively.
A first set of catch plates 18 are provided below upper sieve belt stretch 4' and another set of catch plates 19 are provided below the lower section of sieve belt 4 for collecting liquid and returning it for recycled usage.
Upon leaving guide drum 3, textile web 10 passes over a tension-compensating roll 20 and is further processed. Further processing may include exemplarily a fastness treatment.
As illustrated in FIG. 2, another fabric treatment apparatus 200 in accordance with the present invention has many of the same elements as fabric treatment apparatus 100. The same elements are designated by the same reference numerals in the drawing. Apparatus 200 differs from apparatus 100 in the design of the dwell stretch.
Apparatus 200 comprises three dwell stretch assemblies 27, 27' and 27" spaced from one another along the horizontal path taken by upper sieve belt section 4'. Assembly 27 includes first liquid applicator or spray pipe 7, dwell stretch W in the form of a sieve drum 21, and suction device 15. Sieve drum 21 is rotatably mounted to machine frame 1 at a distance above the plane of upper sieve belt section 4'. A pair of small-diameter guide rollers 22 are disposed below sieve drum 21 symmetrically with respect to a vertical plane passing through the axis of rotation of drum 21. Guide rollers 22 are spaced from one another along the path taken by upper sieve belt section 4'. Each guide roller 22 is closely juxtaposed on a lower side to upper sieve belt section 4' and on an upper side to drum 21.
The direction of motion of textile web 10 about drum 21 is indicated by arrows. The textile web passes partially around an upstream guide roller 22, whereby the direction of motion of the web is substantially reversed. The web is then guided around sieve drum 21 and deposited again on upper sieve belt section 4' upon passing partially around a downstream guide roller 22 and again reversing its direction of motion. Textile web 10 accordingly travels between guide rollers 22 over a meander path corresponding almost to the entire circumference of sieve drum 21.
Upon being deposited on upper sieve belt section 4', textile web 10 is subjected to suction from suction device 15, as described hereinabove with respect to FIG. 1. By the deposition of textile web 10 on sieve belt 4 and additionally by the action of suction device 15 disposed under upper sieve belt section 4' and closely juxtaposed thereto (suction device 15 causing textile web 10 to adhere to sieve belt 4 by suction), textile web 10 is taken along by sieve belt 4 and in turn entrains sieve drum 21 and guide rollers 22. Guide rollers 22 are rotatably mounted to machine frame 1 and can turn easily so that no appreciable tensions arise in the textile web.
Dwell stretch assembly 27' includes liquid applicator 7', dwell stretch W' in the form of a sieve drum 21', and suction device 15'. Two guide rollers 22' are disposed below sieve drum 21' on opposite sides of a vertical plane passing through the axis of rotation of sieve drum 21'. Guide rollers 22' are closely juxtaposed on a lower side to upper sieve belt section 4' and on an upper side to sieve drum 21'. Drum 21' and guide rollers 22' are rotatably mounted to machine frame 1 so that textile web 10 can travel along a meander path defined by guide rollers 22' and sieve drum 21'.
Assembly 27" comprises liquid applicator 7", dwell stretch W" in the form of a sieve drum 21", and a pair of guide rollers 22", and suction device 15". Sieve drum 21" and guide rollers 22" are rotatably mounted to machine frame 1, rollers 22" being closely juxtaposed on a lower side to upper sieve belt section 4' and on an upper side to sieve drum 21". Guide rollers 22" are closely juxtaposed to but spaced from one another along the path of upper sieve belt section 4' and are located symmetrically with respect to a vertical plane passing through the axis of rotation of sieve drum 21".
Although the invention has been described in terms of particular embodiments and applicaitons, one of ordinary skill in the art, in light of this teaching, can generate additional embodiments and modifications without departing from the spirit of or exceeding the scope of the claimed invention. Accordingly, it is to be understood that the drawings and descriptions herein are proffered by way of example to facilitate comprehension of the invention and should not be construed to limit the scope thereof.
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In a fabric treatment apparatus for applying a washing or rinsing liquid to a dyed or printed textile web, the web is transported by a sieve conveyor belt along a horizontal path. Spaced from one another along that horizontal path are several liquid applicators or spray pipes. Associated with each spray pipe is a respect dwell stretch and a suction device, the dwell stretch being located downstream of the respective liquid applicator and upstream of the respective suction device. The dwell stretch includes either two sets of rotatable rollers spaced a distance from one another or a rotatable sieve drum.
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This application is a continuation-in-part of application Ser. No. 278,203 filed Nov. 30, 1988, now abandoned.
BACKGROUND OF THE INVENTION
This invention relates generally to production of metals by reduction of ores containing their oxides. More particularly, the invention relates to a smelting reduction method in which metal oxide ore, such as iron ore, is subjected in a solid state to a preliminary reduction (hereinafter referred to as prereduction) step in a prereduction furnace and thereafter melted in a smelting reduction furnace thereby to carry out final reduction of the ore. The invention concerns a smelting reduction method by which, particularly, the rate of energy utilization is increased, and the consumption of the reaction materials such as coal, oxygen, and lime is greatly reduced.
In the smelting reduction method, in general, metal oxide ore, such as iron ore (iron oxide), is reduced in a molten state thereby to produce iron or ferroalloy. Because of the promising possibility of its adaptation to coping with the further situations of raw materials and energy, this area of technology has recently attracted much attention, and research and development for its reduction to practice is being carried forward.
The principal advantageous features which this method affords as an iron producing method, in comparison with the blast furnace process, are use of low-price raw materials, reduction of preparatory processing steps such as sintering or pelletizing particulate ore, and miniaturization of necessary equipment. In addition, as a method in the production of ferroalloys, it has almost no dependency on the use of electric energy.
While various processes for practicing this smelting reduction method have been proposed, and the reduction furnaces used therein are of diverse form, the smelting reduction furnace of the metal smelting type is a representative form. In the case of a reducing furnace of this type for producing iron, for example, iron ore, together with coal and oxygen, is charged into molten iron bath, and the ore is thus reduced to obtain molten iron (pig iron). However, the reaction is rapid, it being possible to accomplish reduction at a rate which is 100 times or more rapid than in reduction of the ore in solid state, and the required equipment is of simple type. For these and other reasons, furnaces of this type are widely used in many processes.
On its debit side, a smelting reduction furnace of this type has the disadvantage of an extremely poor rate of utilization of energy. The fundamental reaction formula representing the reduction of iron oxides in a furnace of this type is as follows. ##STR1## Since the applied energy in this formula is the heat quantity of combustion of C (carbon), when it is calculated from the quantity of generated heat of C (8,100 kcal/kg), its value becomes 1.293×8,100=10,470 kcal. On the other hand, the heat quantity which has been effectively utilized is the sum of 1,759 kcal, the quantity of heat for reduction of Fe 2 O 3 (1 kg.), and 239 kcal, the heat quantity for melting Fe, that is, the total value 1,998 kcal.
Therefore, the rate of utilization of the energy applied is 1,998/10,470, that is, only 19 percent. Almost all of the remainder is discharged as exhaust gas. Accordingly, in order to increase the rate of utilization of energy, it is necessary to utilize the energy held by this exhaust gas.
A possible measure for this purpose is the so-called secondary combustion technique in which oxygen (or gas containing oxygen) is blown into the gas space part within the smelting reduction furnace thereby to cause combustion of a portion of the combustible gas issuing from the molten metal surface, and one portion of the heat thus generated is recovered and returned into the molten metal, whereby the energy utilization rate of the reduction furnace is increased. This measure utilizes the fact that, the combustion heat generated in the conversion of CO into CO 2 is 2.5 times the combustion heat generated during the conversion of C into CO.
In the case where the secondary combustion rate is 30%, that is, when 30 % of the CO gas emitted from the melt within the furnace is caused to undergo combustion and thus be converted into CO 2 , and the temperature of the gas within the furnace is set at 1,600° C., the fundamental formula of the reaction within the furnace becomes as follows. ##STR2##
In this case, since the added energy is 0.679×8,100=5,500 kcal, the energy utilization rate becomes 36%. While this is a great improvement over the rate obtainable in the case where secondary combustion is not carried out, it is still insufficient. Elevating the secondary combustion rate to an extreme degree gives rise to an excessive rise in the temperature within the smelting reduction furnace and causes a problem in that the serviceable life of the refractories is shortened. Therefore, in order to further increase the energy utilization rate, the introduction of a newer technology is necessary.
As a consequence, a method wherein the raw-material ore is subjected to preparatory reduction or prereduction has been proposed. As mentioned hereinbefore, this method comprises prereducing the ore in its solid state in a prereduction furnace and then subjecting the ore to final reduction in a smelting reduction furnace as described above. For the reducing gas used in the prereduction furnace, high-temperature gas given off during the final reduction in the smelting reduction furnace is mainly used. For the prereduction furnace, a furnace of the fluidized bed type, in which the ore forms a fluidized bed and thus is contacted by and reacts with the above mentioned gas, is used in many cases. In this furnace, the reaction temperature is set at approximately 800° C. so as to obtain a high reduction efficiency without causing sintering of the ore.
In a smelting reduction method of this character as practiced heretofore, in order to obtain as high reduction rate (prereduction rate) in the prereduction furnace as possible, efforts are being devoted toward development toward this goal. Ordinarily, the prereduction rate has been set at 70% or higher value. The term "reduction rate" as used herein designates the rate of decrease of oxygen on the basis of the metal oxide contained in the raw-material ore as reference. For example, in the case where Fe 2 O 3 is taken as reference (reduction rate 0%), the ore is reduced to Fe 3 O 4 at a reduction rate of 11.1%, to FeO at a rate of 33.3%, and to Fe at a rate of 100%.
The energy utilization rate in a process carried out in apparatus comprising a prereduction furnace and a smelting reduction furnace of this character will now be considered.
The fundamental formula representing the reduction reaction of iron oxide in the prereduction furnace is as follows. ##STR3## However, in order to reduce Fe 2 O 3 at 800° C. to Fe, the CO/(CO+CO 2 ) ratio in the gas at the outlet of the prereduction furnace must be maintained at 65% or higher value in accordance with the known Fe-CO equilibrium diagram (shown in FIG. 4 of the accompanying drawings briefly described hereinafter).
Accordingly, in order to increase the quantity of CO fed into the prereduction furnace in the case where the prereduction rate is to be 100% with this process, excess quantities of C and O 2 must be added into the smelting reduction furnace. In this case, since the reaction within the smelting reduction furnace is an exothermic reaction, it is necessary to add a coolant into the furnace in order to maintain thermal equilibrium. For example, when the case where CO 2 is used as the coolant is considered, the fundamental formulas therefor become as follows. ##STR4## In this case, since the energy added is the combustion heat possessed by C, that is, 0.768×8,100=6,221 kcal, the effective utilization rate of heat is 32%.
In the case where the prereduction rate is 75%, that is, where Fe 2 O 3 is reduced to FeO and Fe in the prereduction furnace, the formulas become as follows. ##STR5## The energy utilization rate is 39%.
In a process employing a prereduction furnace also, the secondary combustion technique is applied in some cases in the smelting reduction furnace as described above. However, since the prereduction rate is of a high value of 70% or more, it is necessary to hold the secondary combustion rate at 30% or less in order to secure the CO quantity in the gas for prereduction.
Thus, in a process employing a prereduction furnace and a smelting reduction furnace, the potential heat and the reductive capacity of the gas given off from the smelting reduction furnace are utilized in the prereduction furnace, and at the same time the sensible heat of the ore prereduced in the prereduction furnace is utilized in the smelting reduction furnace, that is, in the process itself, a portion of the energy is being recycled. In contrast, in the smelting reduction method of the prior art, the surplus energy not utilized in the process has been wasted in the exhaust gas.
The above consideration may be summarized as follows. In the known smelting reduction method employing a prereduction furnace and a smelting reduction furnace, the following characteristic features from the viewpoint of energy utilization were afforded.
(i) A prereduction rate of 70% or more.
(ii) A large quantity of surplus energy not utilized in the process has been wasted in the exhaust gas.
A serious problem accompanying the above described known smelting reduction method is that the rate of consumption of carbon (C) necessary for obtaining metal by reducing the metal ore (metal oxide) is high, that is, the energy utilization rate is low. For example, this value is low even in comparison with that of reduction of iron ore by the blast furnace method. For this reason, it is said that, with respect to the smelting reduction method, extensive commercialization thereof is difficult as long as this problem is not solved.
Because of the large consumption of carbon, the consumption of oxygen becomes large. Therefore, in actual practice, not only do adverse effects on production quantities such as the quantity of slag produced, the consumption of coal, and the loss of extracted metal into the slag arise, but the cost of equipment to cope with these effects also increases.
The energy utilization rates examined above are all based on the fundamental reaction formulas, that is, they are energy utilization rates under ideal conditions. In an actual reduction process, however, C is not pure carbon but is in the form of coal, and Fe 2 O 3 is also an iron ore containing impurities. Moreover, occurrences such as discharge of heat from the furnace structure (heat transmission loss) affect the results, whereby the actual rates become somewhat lower than these ideal rates.
Furthermore, since the prereduction rate is high in the conventional smelting reduction method, a prereduction furnace of large capacity is necessary. Another problem is that since metal iron is formed in the ore (prereduced iron), which tend to adhere to each other, the ore is formed into large lumps, whereby difficulties such as obstruction of reaction and transfer are encountered.
SUMMARY OF THE INVENTION
An object of this invention is to solve the above described problems in providing a smelting reduction method in which the rate of utilization of energy is raised to a maximum limit, and the consumption of materials such as coal, oxygen, and lime is made as low as possible.
According to this invention, in order to solve the above described problems, there is provided a method of smelting reduction of metal oxide ore, which comprises prereducing the ore in solid state in a prereduction furnace, thereafter melting the ore and carrying out final reduction thereof in a smelting reduction furnace, and at the same time introducing gas generated in the smelting reduction furnace and having reductive capability into the prereduction furnace, the rate of prereducing the ore in the prereduction furnace being controlled at a value below 30 percent.
By the practice of the smelting reduction method of this invention, metal ore which has been prereduced at a rate such that it is smaller than 30 percent in the prereduction furnace is positively reduced 100% in the smelting reduction furnace of high reduction rate, but since a high reductivity is not necessary in the reducing gas required in the prereduction furnace, secondary combustion can be amply carried out in the smelting reduction furnace. Therefore the rate of utilization of energy in the entire process rises to a maximum limit.
The nature, utility, and further features of this invention will be more clearly apparent from the following detailed description with respect to preferred embodiments of the invention when read in conjunction with the accompanying drawings, which are briefly described below.
BRIEF DESCRIPTION OF THE DRAWINGS
In the accompanying drawings:
FIG. 1 is a schematic flow diagram indicating a first example of apparatus for practicing one embodiment of the invention;
FIG. 2 is a graph indicating relationships between prereduction rate, secondary combustion rate, and coal consumption in the smelting reduction system shown in FIG. 1;
FIG. 3 is a schematic flow diagram indicating a second example of apparatus for practicing another embodiment of the invention;
FIG. 4 is a reduction equilibrium diagram for reduction of iron due to CO gas;
FIG. 5 is a schematic flow diagram indicating a third example of apparatus for practicing still another embodiment of the invention; and
FIG. 6 is a schematic flow diagram indicating a fourth example of apparatus for practicing a further embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring first to FIG. 1, the principal components of the apparatus shown therein for practicing the smelting reduction method of this invention are a prereduction furnace 1 and a smelting reduction furnace 2. In the mode of operation of the this example apparatus iron ore is first preparatorily reduced or prereduced in the solid state in the prereduction furnace 1 and is thereafter melted and subjected to final reduction in the smelting reduction furnace 2, while high-temperature gas having reducing capability which has been formed in the smelting reduction furnace 2 is introduced as a reducing gas into the prereduction furnace 1.
At the prereduction furnace 1, particulate iron ore is charged thereinto through an ore charging pipe 11, while reducing gas is introduced thereinto upwardly through a gas transfer pipe 25 and through a perforated dispersion plate (rectification plate) 1a at a lower part of the furnace 1, whereupon the particulate iron ore on the dispersion plate 1a forms a fluidized bed 1b which is agitated and mixed (by means not shown). The iron ore in this fluidized state is thereby contacted by the reducing gas, undergoes reaction, and is thereby prereduced.
The iron ore thus prereduced (prereduced iron) passes through the dispersion plate 1a and is discharged out through a discharge pipe 12 disposed below or through a side wall of the furnace 1 through a discharge pipe 13 and is transferred, for example, by gas conveyance, through a transfer pipe 14 to be charged into molten iron 2a in the smelting reduction furnace 2. Into the molten iron 2a (and slag 2b) within the smelting reduction furnace 2, in addition to the above mentioned prereduced iron, coal and lime are blown in through a charging pipe 21. Furthermore, oxygen and, if necessary, carbon dioxide gas (CO 2 ) or process recovery exhaust gas (CO+CO 2 +H 2 +H 2 O) are blown in through a charging pipe 22. In addition, through a charging pipe 23, oxygen is blown into the gas space within the furnace 2, and a portion of the gas emerging from the iron melt surface is caused to undergo secondary combustion. As a result, a gas is generated within the smelting reduction furnace 2, is conducted through a furnace top hood 24 and the aforementioned gas transfer pipe 25, and is introduced into the prereduction furnace 1 to be used in the prereduction step. The resulting exhaust gas in the prereduction furnace 1 is discharged out through an exhaust gas pipe 26.
In the instant example, in order to increase the energy utilization rate of the entire process, the process is so controlled that almost all of the iron ore will be reduced to FeO in the prereduction furnace 1, and the secondary combustion rate in the smelting reduction furnace 2 is 20 to 50% and in the broader reaches of the invention the secondary combustion rate is 25% or more. In the case where the Fe 2 O 3 is reduced to FeO in the prereduction furnace 1, the prereduction rate is smaller than 30%, but in the iron ore actually used as a raw material, some Fe 3 O 4 of slightly lower oxygen content is also contained in addition to Fe 2 O 3 . Moreover, when the economy of the prereduction furnace is considered in view of its characteristics owing to its being of the fluidized bed type, the actual prereduction rate becomes approximately 20 to smaller than 30%.
The reason why the energy utilization rate is made high by setting the prereduction rate and the secondary combustion rate in this manner is as follows.
In a smelting reduction system as indicated in FIG. 1, in the case where the obtaining of a unit quantity of molten iron (ton) is considered, the following relationships are made apparent from a comparison and study of the fundamental reaction formulas (1) to (6) set forth hereinbefore.
(1) On the basis of comparison of (3)·(4) and (5)·(6): by changing the prereduction rate in the prereduction furnace 1, the quantity of CO required in the prereduction furnace 1 is caused to change, whereby the quantity of C required in the smelting reduction furnace 2 changes.
(2) On the basis of comparison of (1) and (2): when the secondary combustion rate in the smelting reduction furnace 2 is changed, the required quantity of C changes.
(3) On the basis of comparison of (1) and (2): when the secondary combustion rate is changed, the quantity of the CO given off from the smelting reduction furnace 2 changes. Since the prereduction rate in the prereduction furnace 1 is caused to change by this CO quantity (reference: FIG. 4), the secondary combustion rate influences the prereduction rate.
From the above points of consideration, it can be thought that, by selecting a suitable prereduction rate and a suitable secondary combustion rate, the required quantity of C can be made a minimum, in other words, the effective utilization rate of energy can be made a maximum. Accordingly, we decided to determine the consumption of C on the basis of fundamental reaction formulas (1) to (6) with respect to various combinations of varying values of the prereduction rate and the secondary combustion rate.
In the calculations, in order to investigate the consumption rate of C (that is, coal) in reduction steps as close as possible to the actual case, factors such as the heat discharged (heat transmission loss) from the furnace structure in each case and the heat transfer efficiency into the molten iron of the heat generated by the secondary combustion were considered on the bases of results of preliminary tests carried out in advance. In addition, after setting variables such as the proportions of the raw materials and the molten iron as described below, the fundamental reaction formulas (1) to (6) were used after corrections.
(a) Raw materials:
Iron ore: composition (%, dry state) . . .
T.Fe: 67.8, FeO: 0.1, LOI: 0.5,
SiO 2 : 0.7, CaO: 0.06, MgO: 0.04
Coal: composition (%, dry state) . . .
T.C: 80.0, S: 0.5, H: O, N: 1.0
O: 10.0
Composition in coal ash (%, dry state)
SiO 2 : 60, CaO: 4, MgO: 15
Lime: composition (%, dry state) . . .
CaO: 53.0, MgO: 1.0, LOI: 42.7
(b) Molten iron: composition (%) . . . Fe: 94.5, C: 4.5 Temperature . . . 1,450° C.
(c) Charging temperature: 500° C. of prereduction iron into smelting reduction furnace
(d) Reaction temperature in prereduction furnace: 800° C.
(e) Gas for cooling smelting reduction furnace interior: CO 2 (25° C.)
(f) CO quantity within prereduction furnace:
On the basis of the equilibrium diagram of FIG. 4, a suitable quantity was added to the value considered to be theoretically necessary for obtaining the specific prereduction rate, and the resulting value was taken as the minimum necessary value. For example, for reducing Fe 2 O 3 to FeO at 800° C., the ratio CO/(CO+CO 2 ) was caused to be 30% or higher, and for further reduction to Fe, this ratio was caused to be 70% or higher.
As a result of the above calculation, and with the consumption quantity of coal necessary for producing a unit quantity (1t) of molten iron expressed as t/t of molten iron, the graph shown in FIG. 2 was obtained. The coal consumption is taken as a value indicating the degree of consumption of the actual energy in place of the energy utilization rate under the ideal conditions as mentioned hereinbefore. This graph indicates the coal consumption in the case wherein the secondary combustion rate is set at increments of 10% from 0%, and the prereduction rate is varied from 0 to 90%. In this graph, cases where the gas temperature at the outlet of the smelting reduction furnace 2 exceeds 1,900° C. because of the secondary combustion are excluded.
As is apparent from FIG. 2, the coal consumption becomes a minimum when the secondary combustion rate is 50%, and the prereduction rate is below 30%. It can also be seen that, in the interval between 50 and 20% of the secondary combustion rate, and with a prereduction rate of approximately 33%, minimum values are indicated. Furthermore, the same graph indicates that, since a great quantity of CO is necessary in the case where the prereduction rate is 30% more, if the secondary combustion rate is made high (30% or higher), the coal consumption will increase tremendously.
When the consumption quantities of the coal, oxygen, and lime (per ton of molten iron) determined by the above calculations are indicated with respect to the points A to D in FIG. 2, the following results are obtained. Secondary combustion rate is abbreviated S.C.R., and prereduction rate is abbreviated P.R.
Point A (S.C.R. 20%, P.R. 9.3%)
Coal 1.73t, oxygen 1,060Nm 3 , Lime 0.31t
Point B (S.C.R. 20%, P.R. 33%)
Coal 1.30t, oxygen 790Nm 3 , lime 0.24t
Point C (S.C.R. 20%, P.R. 75%)
Coal 2.70t, oxygen 1,730Nm 3 , lime 0.47t
Point D (S.C.R. 50%, P.R. 33%)
Coal 0.71t, oxygen 450Nm 3 , lime 0.15t
Thus, at point B or D where the coal consumption is low (and P.R. is 33% in either case), the consumptions of oxygen and lime are also low.
The invention will now be described with respect to a second embodiment thereof and with reference to FIG. 3, in which those parts which are the same as or equivalent to corresponding parts in FIG. 1 are designated by like reference numerals. FIG. 3 illustrates an apparatus for practicing the smelting reduction process for iron production according to the invention which is basically the same as that indicated in FIG. 1. In this apparatus, the energy of gas produced in and discharged from two reduction furnaces is used for another purpose outside of the process thereby to effectively utilize the energy. On the basis of the results of analysis in the first embodiment of the invention, the prereduction rate is set at 33%, and the secondary combustion rate at 50% also in this example.
This example is characterized in that the gas formed in the smelting reduction furnace 2 is caused, in its transfer path to the prereduction furnace 1, to flow through a dust remover 31, a steam generator 32 (No. 1 boiler), and a partial gas combustion device 33, and the exhaust gas from the prereduction furnace 1 is caused to flow through a dust remover 34 and a steam generator 35 (No. 2 boiler). Therefore, these gases are respectively cleaned of dust by the dust removers 31 and 34 and conducted into the steam generators 32 and 35 to be used as heat sources for generating steam. By this utilization of these gases, the heat possessed by these gases is converted into steam energy, which therefore can be used for generating electric power, space heating, and other uses in the iron and steel plant.
The partial gas combustion device 33 operates to reheat the gas the temperature of which has dropped in the No. 1 boiler by blowing into this gas oxygen, or a gas containing oxygen, and burning a portion of the combustible component thereof thereby to raise the gas temperature to the value necessary for the prereduction furnace 1. Since the prereduction rate in the prereduction furnace 1 is low, the resulting gas is amply satisfactory for use as the gas for prereduction, even by this partial combustion wherein one portion of the CO or H 2 in the gas is burned and converted into CO 2 and H 2 O, if the gas temperature rises. For increasing the thermal efficiency of the No. 1 boiler 32, the injection orifice for blowing in the oxygen for this partial combustion may be provided in the gas flow path within the No. 1 boiler 32.
The temperatures and compositions shown in the four tables in FIG. 3 are quantitative values indicating the states of the gases at various points in the gas flow paths. In this second example, these values indicate results of calculations carried out with the prereduction rate and the secondary combustion rate set as indicated above under the conditions (a) to (f) of the preceding first example and the following conditions (A), (B), and (C).
(A) Gas temperature variation in No. 1 boiler 32:
1,700° C. to 600° C.
(B) Partial combustion rate (proportion of conversion from CO.H 2 to CO 2 .H 2 O) at partial burner 33:
15%
(C) Gas temperature variation in No. 2 boiler 35:
800° C. to 400° C.
Among the values in the tables which are significant are those relating to the outlet gas of the partial gas combustion device 33 and the outlet gas of the prereduction furnace 1. The ratio CO/(CO+CO 2 ) of the outlet gas of the partial burner 33 is 38% which is less than 65%. For this reason, when this gas is introduced into the prereduction furnace 1 to carry out prereduction of the iron ore at approximately 800° C., pure iron cannot be produced in the iron ore.
The outlet gas from the prereduction furnace 1 contains CO and H 2 of quantities which are ample for reducing the iron ore to FeO. That is, in the case where C and H 2 exist in the gas, the conditions for obtaining FeO at 800° C. are CO/CO 2 >0.35 and, moreover, H 2 /H 2 O>0.34. These conditions are met since the results of calculation for the outlet gas of the prereduction furnace 1 are CO/CO 2 =0.36 and H 2 /H 2 O=1.18. Furthermore, this gas which is discharged through the No. 2 boiler 35 contains chemical heat of 780 kcal/Nm 3 in terms of its composition, whereby it can be used as fuel within the iron and steel works similarly as in the case of blast furnace gas and the like.
The quantity of steam generated by the steam generators 32 and 35 becomes approximately 1.6t (per ton of molten iron) as a total. If all of this steam is used for generating electric power, it will become approximately 300 kW (perton of molten iron), which means that a great quantity of energy can be utilized outside of the process.
Still another advantageous feature of this example of apparatus is that fluctuations in the temperature and composition of the gas for prereduction arising from fluctuations in the operational conditions of the smelting reduction furnace 2 can be suppressed by varying the partial combustion rate. More specifically, in the operation of the smelting reduction furnace 2, the charging quantity of the coal, oxygen, or lime is varied in accordance with factors such as the degree of progress of the reduction reaction. As a consequence, the temperature and composition of the gas formed in the smelting reduction furnace 2 (that is, the gas for prereduction which is introduced into prereduction furnace 1) also fluctuates. By adjusting the partial combustion rate of the gas in the partial gas combustion device 33 in accordance with this fluctuation, the temperature and composition of the gas can be made to be those desirable for the gas for prereduction. For example, in the case where, as a consequence of a lowering of the secondary combustion rate by reducing the quantity of oxygen blown into the smelting reduction furnace 2, the content of CO in the gas increases and the gas temperature drops, the state of the gas can be corrected to suit a reduction rate below 30% by increasing the partial combustion rate in the partial gas combustion device 33.
The smelting reduction method of the invention described above is not limited to the production of iron by reducing iron ore but is applicable also to the production of other metals by a similar process such as that of obtaining ferrochromium by reducing chrominum ore (Cr 2 O 3 or FeCr 2 O 4 ).
By the practice of the above described smelting reduction method, the following beneficial effects are afforded.
(1) The consumption quantity of coal required for obtaining a specific quantity of a molten metal is greatly reduced.
(2) Together with the above effect (1), the consumption quantities of oxygen and lime are also reduced.
(3) Together with the above effects (1) and (2), the quantity of exhaust gas formed decreases.
(4) Together with the above effects (1) and (2), the quantity of slag formed in the molten metal decreases, whereby the loss of metal is reduced, and the yield of metal in the production thereof is increased.
(5) Together with the above effects (1) through (4), the equipment for conveying materials such as coal and lime, the equipment for supply oxygen, and the equipment for processing the exhaust gas can be reduced in scale and cost and their operation cost can be decreased.
(6) Since the prereduction rate is low, a prereduction furnace of small size can be used.
(7) Since a low reducing capacity (quantity of reductive component) of the gas for prereduction is sufficient, energy can be effectively utilized as, for example, the maximum recovery of sensible heat of the gas in the boilers as demonstrated in the second example.
Still another (third) example of apparatus for practicing the smelting reduction method of this invention is shown in FIG. 5. In this apparatus, the gas obtained after secondary combustion from the smelting reduction furnace 2 is passed through a gas pipe 41 connected to the furnace top hood 24, and a portion of this gas is distributed through a branch gas pipe 41a branched from the gas pipe 41 and, passing through a wettype dust collector 43, a blower 44, and a decarburizing device 45, is joined and admixed in a gas pipe 42 with the gas which has flowed in the other branch gas pipe 41b. The resulting mixed gas is passed through a hot cyclone 46 and a partial combustion device 47 and, as a gas for prereduction, is introduced into the prereduction furnace 1.
The wet-type dust collector 43 is not limited in its type as long as it is a device capable of cooling and removing dust from the gas. The decarburizing device 45 also may be any of various types of gas reforming or modifying devices, for example, a device for reforming CO 2 into CO or H 2 through the use of a hydrocarbon or pulverized coal. In the partial combustion device 47, oxygen (or a gas containing oxygen) is blown into a portion of the gas to cause one portion of its combustible component to undergo combustion thereby to raise the temperature of the gas. In place of this device, a heating device of any type for raising the gas temperature can be used.
In this example, similarly as in the preceding examples, the prereduction furnace 1 is of the fluidized bed type. Iron ore in particulate form which is charged into this furnace 1 through the ore charging pipe 11 is caused by the gas for prereduction introduced into this furnace through the gas pipe 42 as described above to form a fluidized bed on the perforated dispersion plate (rectification plate) 1a and, in this state, is contacted by and reacts with the reduction gas to be prereduced. The iron thus prereduced is discharged through the discharge pipe 12 or 13 and is transferred, for example, by gas conveyance, through the transfer pipe 14 to be charged into the smelting reduction furnace 2. Separately, the above mentioned gas used in the prereduction is discharged out of the prereduction furnace 1 through the exhaust gas pipe 26.
In this third example, in order to increase the energy utilization rate of the entire process, the characteristics of the gas for prereduction are adjusted, and at the same time the secondary combustion rate in the smelting reduction furnace 2 is caused to be 60% or higher so that reduction will be carried out until the iron ore becomes almost FeO in the prereduction furnace 1. In the case where Fe 2 O 3 is reduced to FeO in the prereduction furnace, the prereduction rate is 33.3%. However, the iron ore actually used as a raw material contains, in addition to FeO 3 also, some Fe 3 O 4 of slightly low oxygen content. For this reason, the actual prereduction rate will be below 30%.
In a process as indicated in FIG. 5, by adjusting the characteristics of the gas for prereduction, the prereduction rate and the secondary combustion rate are set in this manner for the following reasons.
As described hereinbefore, the prereduction rate in the prereduction furnace 1 is determined by the quantity (proportion) of CO contained in the gas for prereduction. This CO quantity, in turn, is determined by the quantity of C (coal) charged into the smelting reduction furnace 2 and the secondary combustion rate. Furthermore, the quantity of C varies with the prereduction rate of the iron ore charged into the smelting reduction furnace 2. This trend can be easily understood by a comparative study of the fundamental reaction formulas (2), (5) and (6), a number of reaction formulas which have varied the secondary combustion rate and the prereduction rate, the known reduction equilibrium diagram concerning CO gas and iron shown in FIG. 4, and other data.
From a quantitative study of the above considered points, it appears possible to determine suitable values of the prereduction rate and the secondary combustion rate for reducing the consumption quantity of C for obtaining a unit quantity of molten iron Fe(l) to a minimum, in other words, for obtaining maximum utilization of energy. Accordingly, we determined these rates by calculation after setting realistic conditions (e.g., characteristics of the iron ore and the coal and heat loss from various parts). Then we carried out verification experiments. The results thus obtained were as follows.
(i) The consumption quantity of coal (C) becomes a minimum for a secondary combustion rate of 25% or higher when the prereduction rate is below 30%. These values are less than the minimum coal consumption quantity in the case where the secondary combustion rate is less than 25%. The coal consumption quantity in the case of a prereduction rate of below 30% decreases with increase of the secondary combustion rate over 20%.
(ii) When the secondary combustion rate exceeds 60%, the quantity of CO in the gas generated in the smelting reduction furnace drops. Therefore, unless this gas is reformed or modified, a prereduction rate of 30% and above, i.e., be attained.
To summarize: maintenance of the prereduction rate at below 30% and raising the secondary combustion rate as much as possible result in decreasing the coal consumption. For example, the coal consumption in the case of a secondary combustion rate of 50% and a prereduction rate of 33%, for example, becomes approximately 40% less than that in the aforedescribed example (secondary combustion rate 0% and prereduction rate 75%). This indicates a great degree of improvement.
If, in order to lower the coal consumption, the secondary combustion rate is set at 60% or higher, the generated gas from the smelting reduction furnace 2 cannot be used directly as it is as the gas for prereduction for the reason given in paragraph (ii) above. In this example, by adjusting the characteristics of the gas for prereduction, the prereduction rate was set at a value of the order of below 30% and the secondary combustion rate at 60% or higher for the reasons given above.
Trial calculations relating to the characteristics of the gases at various parts (points A through G in FIG. 5) of the gas piping of the apparatus of the instant example were carried out for the case where, by the use of the apparatus, the process is carried out under the conditions of a secondary combustion rate in the smelting reduction furnace 2 of 65%, a distribution of the generated gas from the gas pipe 41 of 50% to each of the branch pipes 41a and 41b, and combustion of 15% of the combustible component of the gas in the partial combustion device 47, whereupon the following results were obtained.
______________________________________ GasGas composition (%) Temp. quantityPart CO CO.sub.2 H.sub.2 H.sub.2 O N.sub.2 (°C.) (Nm.sup.3)______________________________________A 23.1 42.9 8.1 14.9 11.0 1700 1600B 25.3 40.7 5.8 17.2 11.0 1050 1600C 27.6 44.5 6.4 9.5 12.0 70 733D 45.9 7.5 10.7 15.9 20.0 50 440E 26.3 35.2 13.9 10.4 14.2 700 1240F 23.1 38.4 10.7 13.6 14.2 1100 1240G 16.3 45.1 7.6 16.8 14.2 800 1240______________________________________
In the above mentioned trial calculations, it was assumed that, in the wet-type dust collector 43, 67Nm 3 of H 2 O is removed with the cooling of and dust removal from the gas and that, in the decarburizing device 45, 90% or 293Nm 3 of CO 2 in the gas is removed, and lowering of the temperatures of the gases within the various devices and gas pipes and, further, the accompanying shift reaction were considered.
Among the above quantitative values, the gas composition at point G (the outlet of the prereduction furnace 1) is noticed. In the gas at this point G, CO and H 2 are contained as the reductive component, and the percentage quantities thereof are high, for the following reasons, and ample for attaining a prereduction rate of below 30% (reduction of the iron ore to FeO). That is, when CO and H 2 exist in the gas, the condition for obtaining FeO at 800° C. is CO/CO 2 >0.35, which is satisfied by the trial calculation result of CO/CO 2 =0.36.
When the secondary combustion rate is raised to 65% while the prereduction rate is maintained at a value smaller than 30% by adjusting the characteristics of the gas for prereduction in the above described manner, the consumption of coal is further decreased by several % as compared with that in the above described case of secondary combustion rate of 50%. In this connection, the coal consumption in the case where the secondary combustion rate exceeds 20% increases rapidly when the prereduction rate is 30% or more. On the other hand, since the coal consumption increases only slightly even when the prereduction rate falls below 33%, actual optimum value of the prereduction rate is in a range of from somewhat above 10% to below 30% in actual production.
By the method of this example, the secondary combustion rate can be further raised if a large quantity of gas is reformed by increasing the quantity of gas distributed into the gas pipe 41a. Therefore it is also possible to further decrease the coal consumption. In the case also where the secondary combustion rate is 60% or less, if the gas characteristics are adjusted by this method, the reductivity of the gas for prereduction can be increased. Therefore many advantages, such as the attainment of the same prereduction rate (below 30%) through the use of a prereduction furnace of small capacity, are afforded.
A further (fourth) example of apparatus suitable for use in the practice of this invention will now be described with reference to FIG. 6. Those parts in FIG. 6 which are the same or equivalent to corresponding parts in FIG. 5 are designated by like reference numerals. Detailed description of such parts will not be repeated. This example in FIG. 6 is adapted to the smelting process for iron production similarly as that shown in FIG. 5 but is characterized in that one portion of the cooled and dust-removed exhaust gas from the prereduction furnace 1, after being reformed, is admixed into the gas which has been generated in the smelting reduction furnace 2 and introduced through a gas pipe 51 into the prereduction furnace 1.
More specifically, the exhaust gas which has been discharged from the prereduction furnace 1 and flows through an exhaust gas pipe 58 is cooled and cleaned of dust in a wet-type dust collector 53 and is thereafter distributed into branch gas pipes 58a and 58b. The gas passed through the gas pipe 58b is discharged and disposed of as exhaust gas. The gas flowing through the gas pipe 58a is passed through a blower 54 and a decarburizing device 55 and joins and is admixed with the above described gas in the gas pipe 51. One portion of the resulting mixed gas, similarly as in the preceding example shown in FIG. 5, undergoes partial combustion in a partial combustion device 57 to raise the temperature of the gas and thereafter is introduced as gas for prereduction into the prereduction furnace 1.
In this example, furthermore, in order to adjust the characteristics of the gas for prereduction with even higher accuracy and positiveness, a gas pipe 51c is provided so that one portion of the generated gas from the smelting reduction furnace 2 can be discharged as exhaust gas through this gas pipe 51c when necessary. This gas conducted through the gas pipe 51c may be caused to join the flow of the above mentioned exhaust gas through the gas pipe 58b. Since the gas discharged in this manner contains a combustible component, it can be utilized as fuel within the iron and steel making factory.
In this example, also, the gas compositions and temperatures are so adjusted that the prereduction rate of the iron ore in the prereduction furnace 1 will be 33%. Therefore a high secondary combustion rate in the smelting reduction furnace 2 can be used, and molten iron can be obtained with a coal consumption which is less than in a known process. In this case, however, since the exhaust gas from the prereduction furnace 1 having less CO and H 2 than in the example illustrated in FIG. 5 is reformed, it is necessary to conduct through the gas pipe 58a and decarburize a greater quantity of gas (for example, 70 to 80% of the total exhaust gas quantity).
On the other hand, there is an advantage afforded by this example in that the quantity of the gas for prereduction can be adjusted by increasing or decreasing the quantity of gas distributed to the gas pipe 58a or the quantity of gas discharged out through the gas pipe 51c even in the event of fluctuation in the quantity of gas generation due to fluctuation in the state of operation of the smelting reduction furnace 2. This advantage is especially pronounced in the case where the prereduction furnace 1 is of the fluidized bed type, which requires accurate and positive adjustment of the flow rate of the gas for reduction.
It is to be noted that the above described method of adjusting the characteristics of the gas for prereduction is not limited in application to only the production of iron by reducing iron ore but is suitable also for application to smelting reduction of other metals by similar processes such as, for example, obtaining chromium by reduction of chromium ore (Cr 2 O 3 or FeCr 2 O 4 ).
By the above described method of adjusting the characteristics of the gas for prereduction, the following advantageous effects are afforded.
(1) Since the secondary combustion rate can be increased to a high value, the rate of consumption of coal required for obtaining molten metal is greatly decreased.
(2) It is necessary to reform only one portion of the generated gas from the smelting reduction furnace or the exhaust gas from the prereduction furnace, and therefore the costs of installation and operation of the reforming equipment are relatively low.
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Metal oxide ore is subjected to smelting reduction to obtain the molten metal by a method which comprises prereducing said ore in solid state in a prereduction furnace, thereafter melting said ore and carrying out final reduction thereof in a smelting reduction furnace, and at the same time introducing gas generated in said smelting reduction furnace and having reductive capability into said prereduction furnace, the rate of prereducing said ore in said prereduction furnace being controlled at a value with a maximum of the order of 33 percent for raising the rate of utilization of energy to a maximum limit.
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FIELD OF THE INVENTION
This invention relates to the treatment of wells penetrating subterranean formations and more particularly to the isolation of an interval within a well for the introduction of a treating fluid into an adjacent formation.
BACKGROUND OF THE INVENTION
Various treatment procedures are known in the art for the treatment of a well penetrating a subterranean formation. One common treatment procedure involves the hydraulic fracturing of a subterranean formation in order to increase the flow capacity thereof. Thus, in the oil industry, it is a conventional practice to hydraulically fracture a well in order to produce fractures or fissures in the surrounding formations and thus facilitate the flow of oil and/or gas into the well from the formation or the injection of fluids from the well into the formation. Such hydraulic fracturing can be accomplished by disposing a suitable fracturing fluid within the well opposite the formation to be fractured. The well is open to the formation by virtue of openings in a conduit, such as a casing string, or by virtue of an open completion in which a casing string is set to the top of the desired open interval and the formation face then exposed directly to the well below the shoe of the casing string. In any case, sufficient pressure is applied to the fracturing fluid and to the formation to cause the fluid to enter into the formation under a pressure sufficient to break down the formation with the formation of one or more fractures. Oftentimes the formation is ruptured to form vertical fractures. Particularly, in relatively deep formations, the fractures are naturally oriented in a predominantly vertical direction. One or more fractures may be produced in the course of a fracturing operation, or the same well may be fractured several times at different intervals in the same or different formation.
Another widely used treating technique involves acidizing, which is generally applied to calcareous formations such as limestone. In acidizing, an acidizing fluid such as hydrochloric acid is introduced into the well and into the interval of the formation to be treated which is exposed in the well. Acidizing may be carried out as so-called “matrix acidizing” procedures or as “acid fracturing” procedures. In acid fracturing, the acidizing fluid is injected into the well under a sufficient pressure to fracture the formation in the manner described previously. An increase in permeability in the formation adjacent the well is produced by the fractures formed in the formation as well as by the chemical reaction of the acid with the formation material. In matrix acidizing, the acidizing fluid is introduced through the well into the formation at a pressure below the breakdown pressure of the formation. In this case, the primary action is an increase in permeability primarily by the chemical reaction of the acid within the formation with there being little or no effect of a mechanical disruption of the formation, such as occurs in hydraulic fracturing.
Various other treatment techniques are available for increasing the permeability of a formation adjacent a well or otherwise imparting a desired characteristic to the formation. For example, solvents can sometimes be involved as a treating fluid in order to remove unwanted material from the formation in the vicinity of the well bore.
SUMMARY OF THE INVENTION
In accordance with the present invention, there is provided a method for the treatment of a subterranean formation penetrated by a well. In carrying out the invention, first and second flow paths are established within the well, extending from the wellhead into the vicinity of the subterranean formation. A plugging fluid comprising a suspension of a particulate plugging agent in a carrier liquid is circulated into the first of the flow paths and into the well in contact with the wall of the well within the subterranean formation. The carrier liquid is separated from the particulate plugging agent by circulating the carrier liquid into a second flow path. Circulation of the liquid is accomplished through a set of openings leading to the second flow path, which are dimensioned to allow the passage of the carrier liquid while retaining the particulate plugging agent in contact with the set of openings. The circulation of the plugging fluid continues until the particulate plugging agent accumulates to form a bridge packing within the well. The bridge packing acts similarly as a mechanical packer to form a barrier within the well. Subsequent to establishing the bridge packing, a treating fluid is introduced into the well through the first flow path and in contact with the surface of the formation in the well adjacent to the accumulated plugging agent forming the bridge packing.
In a further aspect of the invention, a treatment procedure is carried out in a section of a well penetrating a subterranean formation and having a return tubing string provided with spaced screened sections at a location in the well adjacent the subterranean formation. A working tubing string opens into the interior of the well intermediate the spaced screen sections. In carrying out the invention, a plugging agent comprising a suspension of particulate plugging agent in a carrier liquid is circulated through the working string into the intermediate interval between the screen sections. The carrier liquid is flowed through openings in the spaced screen section, which are sized to allow the passage of the carrier liquid while retaining the particulate plugging agent in the well in contact with the screen sections. The flow of the plugging agent within the well is continued until the particulate plugging agent in the fluid accumulates in the well adjacent the screen sections to form spaced bridge packings within the well and surrounding the return string. Thereafter, a treating fluid is introduced into the well and into the interval of the well intermediate the spaced bridge packings and introduced into the formation. In a specific application of the invention, the treating fluid is a fracturing fluid introduced into the treating interval under pressure sufficient to hydraulically fracture the formation. In another embodiment of the invention, the treating fluid is an acidizing fluid effective to acidize the formation in either a matrix acidizing or acid fracturing operation. Preferably, subsequent to the introduction of the treating fluid into the well, a clean-up fluid is circulated down the well into the return tubing string to displace the accumulated particulate plugging agent away from the screened sections and disrupt and remove the bridge packings. In carrying out the hydraulic fracturing operations, the fracturing fluid is normally in the nature of a cross-linked gel having a high viscosity. The clean-up fluid can incorporate a breaker to break down the viscosifying agent in the fracturing fluid. For example, where the viscosifier in an aqueous-based fracturing agent takes the form of hydroxethylcellulose, the clean-up fluid can incorporate an acid such as hydrochloric acid, which functions to break the fracturing fluid gel to a liquid of much lower viscosity. Subsequently, the tubing strings can be moved longitudinally through the well to a second location within the well bore spaced from the originally treated location and the operation then repeated to treat a different section of the well bore. The tubing strings employed in carrying out the invention may be parallel tubing strings or they may be concentrically oriented tubing strings in which the working string disposed within the return string provides a return pathway formed by the annulus of the working string and the return string.
In a further application of the invention, a treating process is carried out in a well section that extends in a horizontal orientation within the subterranean formation. The fracturing operation is carried out to hydraulically fracture the formation and form a vertically oriented fracture within the formation extending from the horizontally oriented well bore. Thereafter, the return and working strings are moved longitudinally through the horizontally extending well section to a second location, and the operation is repeated to form a second set of bridge packings followed by hydraulic fracturing to form a second vertically oriented fracture within the well section spaced at some distance from the initially formed vertically oriented fracture. These operations can be repeated as many times as desired in order to produce multiple fractures.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic illustration of a well with parts broken away, showing the formation of spaced bridge packings using concentrically oriented tubing strings.
FIG. 2 is a schematic illustration of a well with parts broken away showing the invention as carried out employing parallel tubing strings.
FIG. 3 is a schematic illustration of a section of a well showing a preferred form of screen section in a parallel string configuration.
FIG. 4 is a schematic illustration of a well with parts broken away showing the application of the invention in a deviated well having a horizontal well section within a subterranean formation.
FIGS. 5 and 6 are schematic illustrations with parts broken away of a horizontal well section showing sequential operations within the well section.
FIG. 7 is a schematic illustration of a well with parts broken away showing the application of the invention in forming a single bridge packing with a concentric tubing string assembly.
FIG. 8 is a schematic illustration of a well with parts broken away showing the application of the invention in forming a single bridge packing with parallel tubing string configuration.
FIG. 9 is a side elevation with parts broken away showing a downhole well assembly suitable for use in carrying out the present invention.
FIG. 10 is a side elevation with parts broken away showing another form of a downhole well assembly suitable for use in carrying out the present invention.
FIG. 11 is a side elevation of a tubing section employed in a preferred screen section for use in the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides for the formation of one or more downhole bridge packings which can be placed at precise locations in a well by fluid circulation techniques in order to permit well-defined access to a formation by a suitable treating agent. The bridge packings can be assembled within the well without the use of special downhole mechanical packings and can be readily removed after the treatment procedure by a reverse circulation technique. The bridge packings are formed by the circulation downhole of a particulate plugging agent which is suspended in a suitable carrier liquid. The plugging fluid is circulated through a downhole screen at a desired location which permits the suspending liquid to readily flow through the screen openings but retards passage of the particulate plugging agent so that it accumulates in the well at the desired downhole location. The plugging agent may take the form of gravel or a gravel/sand mixture as described in greater detail below. Other suitable mixtures of porous permeable materials may be employed. The gravel-plugging agent is suspended within a liquid that may be either oil- or water-based for circulation down the well to the desired downhole location. The carrier liquid typically is treated with a thickening agent in order to provide a viscosity, normally within the range of 10-1,000 centipoises, preferably within the range of 30-200 centipoises, which is effective to retain the plugging agent in suspension as the plugging fluid is circulated through the well. However liquids of low viscosity, for example, water having a viscosity of about 1 cp can be used with low density plugging agents.
The invention may be carried out employing tubing sections suspended down hole from a mechanical packer, which may be equipped with a crossover tool, or it may be carried out employing tubing strings which extend from the wellhead to the downhole location of the well being treated. The invention will be described initially with respect to the latter arrangement, which normally will be employed only in relatively shallow wells, in order to illustrate in a simple manner the flow of fluids in the course of carrying out the invention.
Turning now to the drawings and referring first to FIG. 1, there is illustrated a well 10 , which extends from the earth's surface 12 into a subterranean formation 14 . Formation 14 may be of any suitable geologic structure and normally will be productive of oil and/or gas. The well 10 is provided with a casing string 15 which extends from the surface of the earth to the top of formation 14 . Typically, casing string 15 will be cemented within the well to provide a cement sheath (not shown) between the outer surface of the casing and the wall of the well. It is to be recognized that the well structure of FIG. 1 is highly schematic. While only a single casing string is shown, as a practical matter a plurality of casing strings can be and usually will be employed in completing the well. Also, while FIG. 1 depicts a so-called “open hole” completion, the well may be set with casing and cemented through the formation 14 and the casing then perforated to provide a production interval open to the well.
The well is completed with concentrically run tubing strings comprising an outer tubing 17 and an inner tubing string 18 . The tubing strings 17 and 18 are hung in the well from the surface by suitable wellhead support structure (not shown). A flow line equipped with a valve 20 extends from the tubing 18 to allow for the introduction and withdrawal of fluids. A similar flow line with valve 21 extends from tubing string 17 and allows for the introduction and withdrawal of fluids through the annulus 22 , defined by the tubing strings 17 and 18 . The casing string is provided with a flow line and valve 23 providing access to the tubing-casing annulus. The tubing strings 17 and 18 are both closed at the bottom by closure plugs 17 a and 18 a . The tubing string 17 is provided with spaced screen sections 24 and 25 . The screen sections may be of any suitable type as long as they provide for openings sufficient to permit the egress and ingress of the liquid carrier while blocking passage of all or at least a substantial portion of the particulate plugging agent. In a typical downhole configuration involving a 4-inch diameter tubing set within a well bore having a nominal diameter of about 8-9 inches, the screen sections may be formulated by grid screens having sieve openings within the range of about 0.006-0.01 inch, corresponding generally to a standard sieves of 60-100 mesh. Other configurations can be used. For example, the screen sections can be provided by perforated sections of tubing or tubing which has been slotted vertically or vertically and horizontally, providing openings sufficient to block the passage of plugging agent. Also, sintered metal screens can be employed. The screen sections may be of any suitable dimension. In a well configuration as described above, the screen sections 24 and 25 may each be about 2-30 feet in length with an interval between the screen sections (from the top of the lower section to the bottom of the upper section) of about 5-30 feet. The downhole well assembly is provided with one or more flow ports such as provided by a spider assembly 28 comprised of a plurality of tubes extending from the interior of tubing string 18 to the exterior of tubing string 17 to permit the flow of fluid between the interior of tubing string 18 and the exterior of tubing string 17 .
In carrying out the invention, the slurry of particulate plugging agent in the carrier liquid is circulated through line 20 and down the well through tubing 18 . The slurry flows through the downhole spider assembly 28 into the annular space 30 between the wall of the well and the outer surface of tubing 17 . Within the well annulus 30 , the slurry flows through the screens 24 and 25 into the annulus 22 defined by tubing strings 17 and 18 . If desired, a packer (not shown) may be set in the well annulus above screen 24 in order to direct the flow of fluid into the annulus 22 rather than up the well annulus 30 . However, this often will be unnecessary. The plugging fluid flowing down the well (having a suspension of gravel or the like in the carrier liquid) will have a higher bulk density than the carrier liquid itself. Thus, as the carrier liquid flows through the screens 24 and 25 causing the granular plugging agent to accumulate in the vicinity of the screens, the pressure gradient across the screens will be less than the pressure gradient up the well. Thus, flow will be predominantly through the screen and into the tubing annulus 22 .
At the conclusion of the preliminary circulation step, effective bridge packings 32 and 34 are formed adjacent the screens 24 and 25 . The packings are retained in place by the hydrostatic pressure in the well annulus 30 , and the packings are sufficiently impermeable to prevent any significant migration of fluid from one side of a packing to the other.
At the conclusion of the formation of the bridging plugs, a suitable treating fluid is injected via line 20 into tubing 18 and through the spider assembly 28 into the space between the bridge packings 32 and 34 . By way of example, a fracturing fluid may be injected down tubing 18 and under pressure sufficient to form a fracture 36 in the formation 14 . Alternatively, the treating procedure may take the form of an acidizing procedure or an acid fracturing procedure.
Standard procedures can be employed in carrying out the treating operation. Where a fracturing operation is involved, initial spearhead fluid will be injected in accordance with accepted practice under a sufficient pressure to exceed the breakdown pressure of the formation and fracture the formation. Normally the spearhead fluid will be a viscous fluid, typically having a viscosity within the range of 10-1,000 centipoises which is free of propping agent or has a very low propping agent concentration. In order to insure that the bridge packings remain in place during the initial fracturing procedure, the spearhead fluid can incorporate a bridging agent such as sand employed in relatively low concentration, typically within the range of 1-50 pounds per barrel.
After fracturing is initiated in the formation, a fracturing fluid carrying a propping agent, is pumped down tubing 18 to propagate the fracture in the formation and leave it packed with propping agent. Typically a “sand out” condition will occur, as indicated by an increase in pressure, and the fracturing operation is then concluded.
At the conclusion of the treating procedure, the bridge packings may be removed. In order to remove the bridge packings 32 and 34 , a reverse circulating fluid, which may be the same or different from the fluid employed as the carrier liquid initially, is injected through valve 21 into the tubing annulus 22 . This creates a reverse pressure differential through the screen sections 24 and 25 causes the bridge packings to begin to disintegrate. Ultimately, the bridge packings are removed by the particulate plugging agent becoming suspended in carrier liquid and carried away from the vicinity of the formation. Normally, the particulate plugging agent will be reverse circulated up tubing string 18 to the surface and removed from the well. The suspension of particulate plugging in the carrier liquid can be circulated up the annulus 30 . The reverse circulation fluid may be different from the fluid employed as the initial carrier liquid. The reverse circulation fluid may take the form initially of a lower viscosity fluid to facilitate the initial removal of the particulate plugging agent. Where the carrier liquid incorporates a cross linked gel, the reverse circulation flow may contain a breaking agent to help remove the cross-linked gel from the bridge packing. Suitable gelling agents include guar gum or hydroxyethylcellulose. They may be used in any suitable amounts. Typically, they are used in minimum amounts of about 20-25 to perhaps 30 lbs. per thousand gallons. The gel may be broken through the use of oxydizers or enzymes to effect suitable decomposition reactions. Typically, oxydizers are used. Suitable oxidizers include sodium hypochlorite and ammonium persulfate.
Turning now to FIG. 2, there is illustrated an alternative well structure for use in carrying out the present invention in which parallel tubing strings are employed. In FIG. 2 like elements are designated by the same reference numerals as shown in FIG. 1 and the foregoing description is applicable to FIG. 2 with the exception of the modification involving the use of parallel tubing strings. In FIG. 2, string 38 (analogous in function to tubing string 18 ) and tubing string 40 (analogous in function to tubing string 17 ) are run in a parallel configuration. The tubing strings are dimensioned to take into account the parallel configuration. By way of example, in a well having a nominal diameter of 8-9 inches, each of strings 38 and 40 may be 2-3-inch tubing strings. Tubing string 40 is provided with screen sections 41 and 42 , which may be configured with respect to the size of the openings, similarly as described above with respect to FIG. 1 . Tubing string 40 is closed at its lower end with a suitable plug indicated by reference numeral 40 a . Tubing string 38 is provided with a closure or seal 44 at its bottom end and is provided with a perforated section 45 to allow for the flow of fluid from tubing 38 into the well bore. Alternatively, instead of providing tubing string 38 with a perforated section, the tubing string may be open at its bottom end to provide for flow of fluids from the interior of the tubing string into the well. In this case the lower end of the tubing sting should be located approximately midway between the locations of the screen sections 41 and 42 . The operation of the invention employing the parallel tubing configuration shown in FIG. 2 is similar to the operation employing the concentric tubing strings as shown in FIG. 1. A plugging fluid comprising a suspension of particulate plugging agent is circulated down the well via tubing 38 . The openings in the perforated section 45 of tubing 38 are sufficient to permit the passage of the particulate plugging agent in suspension in the carrier liquid without the plugging agent screening out of suspension and accumulating in the interior of the tubing string 38 .
The plugging fluid is circulated down tubing 38 into the well and through the screen sections 41 and 42 in order to form bridge packings 47 and 48 . As the carrier liquid passes through the screen sections and into tubing string 40 , the bridge packings 47 and 48 are formed similarly as described above. At the conclusion of formation of the bridge packings, the treating fluid is then injected down tubing string 38 and into the interval of the well between bridge packings 47 and 48 to carry out the desired treating operation. At the conclusion of the treating operation, the bridge packings 47 and 48 may be removed by circulation of the viscous carrier liquid down the well in tubing string 40 . Alternatively, a different fluid may be used as described previously.
In carrying out the invention with the parallel tubing configuration of FIG. 2, the lower bridge packing 47 will occupy a substantially greater cross-sectional area of the well bore than in the case of employing concentric tubing strings. In a preferred embodiment of the invention, in order to facilitate removal of the lower screen section in conjunction with dispersion of the bridge packing, the lower screen section can be formed in a tapered configuration. This embodiment of the invention is shown in FIG. 3, in which the tubing 40 is shown to terminate in a tapered screen section 49 . By way of example, where the tubing string 40 is a 3-inch tubing, the screen section may taper downwardly to provide a lower dimension indicated by reference numeral 50 of about half of the dimension of the tubing string.
A preferred application of the present invention is in carrying out multiple treatments in a single wellbore. This is facilitated by the fact that the bridge packings can be readily removed by a reverse circulation technique, the tubing assembly then moved to a new location in the well, and a new set of bridge packings put in place. This mode of operation is particularly advantageous in the operation of wells in which the producing section is slanted substantially from the vertical in some cases to a nominally horizontal orientation. Such horizontal well bores are typically employed in relatively thick gas or oil formations where the slant well follows generally the dip of the formation and especially where the formation permeability is relatively low. Such slant wells or horizontal wells can be formed by any suitable technique. One technique involves the drilling of a vertical well followed by the use of whipstocks to progressively deviate from the vertical in a direction to arrive at the horizontal orientation. Such horizontal wells may also be formed using coiled tubing equipment of the type disclosed, for example, in U.S. Pat. No. 5,215,151 to Smith et al. Turning now to FIG. 4, there is illustrated a well 52 which has been deviated from the vertical into a horizontal configuration to generally follow the dip of subterranean formation 54 . The well is equipped with a concentric tubing arrangement having inner and outer tubing strings 56 and 57 corresponding generally to the tubing strings 17 and 18 of FIG. 1 . The outer tubing string 57 is equipped with upper and lower screen sections 58 and 59 , which are disposed above and below a spider assembly 60 providing for the flow of fluid between the interior of tubing string 56 and the exterior of tubing string 57 . In operation of the system of FIG. 4, the suspension of a particulate plugging agent is circulated down tubing string 56 and through spider assembly 60 into the annulus 62 between the wall of the well 52 and the outer tubing string 57 . The carrier liquid flows through the screen elements 58 and 59 and into the tubing annulus 64 , resulting in the formulation of bridge packings similarly as described above. A tubing fracturing operation is then initiated in order to form one or more vertical fractures as indicated by reference character 65 .
In the stimulation of formations penetrated by horizontal or deviated wells as shown in FIG. 4, it is sometimes desirable to form a series of spaced vertical fractures. This sequence of operation is shown by FIGS. 5 and 6. FIG. 5 illustrates the location of the tubing strings 56 and 57 at a second location moved uphole from the initial location where fracture 65 was formed. The circulation procedure is repeated to again provide spaced bridge packings 67 and 68 followed by a fracturing operation in order to form a second fracture system 70 spaced horizontally from the first fracture system 65 . Thereafter, circulation is reversed as indicated in FIG. 6 with a carrier liquid (without particulate plugging agents) circulated down the annulus 64 to disrupt the bridge packings with return of fluid up the inner tubing string 56 and, if desired, also within the well-tubing annulus 62 . If desired, the process can be repeated by again moving the tubing assembly uphole and forming new bridge packings at yet another location followed by fracturing to produce a third vertical fracture system spaced from the systems 65 and 70 .
Usually in carrying out the invention in deviated wells as depicted in FIGS. 4 through 6, it will be preferred to employ a concentric tubing arrangement rather than a parallel tubing arrangement configuration of the type depicted in FIG. 2 . When using the concentric tubing arrangement, suitable centralizers can be employed along the length of the concentric tubing strings in order to maintain the generally annular spacing shown.
A further embodiment of the invention, as carried out employing only a single bridge packing, is shown in FIG. 7 . In the system of FIG. 7, a concentric tubing arrangement similar to that shown in FIG. 1 is employed with the exception that the interior tubing string 72 extends through the bottom of the exterior tubing string 74 . The exterior tubing string is provided with a suitable closure element 79 in order to seal the annulus 76 between the inner and outer tubing strings at the bottom. In this embodiment of the invention, normally carried out near the bottom of a well, the dispersion of plugging agent in the carrier liquid is circulated down tubing string 72 and into the well bore. The carrier liquid is returned from the well bore through string screen 77 into the tubing annulus 76 to form a bridge packing 78 similarly as described previously. Once the packing is formed, a suitable treating operation can be carried out by the injection of a treating fluid such as a fracturing fluid or an acidizing fluid down the interior tubing string 72 into the well section below the bridge packing 78 . At the conclusion of the treating operation, flow can be reversed by circulating the carrier liquid down the tubing annulus 76 to displace the accumulation of particulate plugging agent away from the screen section 77 .
FIG. 8 illustrates a parallel tubing string configuration employed to provide a single bridge packing. Here, tubing string 80 is open at the bottom, and tubing string 82 is provided with a closure 83 and a screen section 84 spaced upwardly from the lower end of the tubing string. A carrier liquid containing a particulate plugging agent in suspension is circulated down tubing string 80 through the screen section and up tubing string 82 in order to form a bridge packing 86 . The treating operation can be carried out through tubing string 80 , and at the conclusion of the treating operation, reverse circulation down tubing 82 is instituted to disrupt the bridge packing 86 , similarly as described above.
The invention as thus far described involves the use of separate tubing strings run in parallel or concentrical configuration from the wellhead to the vicinity of the formation undergoing treatment. While applications of this nature are useful, particularly in relatively shallow wells, the tubing arrangements involved become relatively cumbersome when the invention is carried out in wells of substantial depth, particularly where the depth of the well to the formation undergoing treatment exceeds about 1,000-2,000 ft. In such cases it will usually be desirable to run a well tool providing separate flow paths as described above on a single tubing string equipped with a packer. If desired, the packer may be equipped with a flow control tool of conventional configuration to permit different flow paths from the surface of the well to the downhole location through a single tubing string and/or through the tubing-casing annulus.
Turning to FIG. 9, there is illustrated a well 10 having a single tubing string 90 extending from the surface of the well (not shown). Supported on the tubing string 90 is a mechanical packer 91 which supports sections of tubings 92 and 93 . Tubing section 93 is equipped with upper and lower screen sections 94 and 95 and is analogous in operation to the tubing string 40 described above with reference to FIG. 2 . Tubing string 92 is provided with a perforated section 96 and is analogous in operation to the tubing string 38 described above with reference to FIG. 2 . The tubing sections 92 and 93 are secured to one another in a fixed space location by the packer 91 and by means of spacing elements 97 extending between the tubing sections. Spacing elements 97 do not, of course, provide fluid passages between the tubing sections. Tubing 92 can be placed in fluid communication with the tubing string 90 through a passageway 99 in the packer, and the interior of tubing string 93 placed in fluid communication with the tubing-casing annulus 98 by means of passageway indicated by broken lines 100 . In operation of the well tool shown in FIG. 9, a suspension of the particulate plugging agent in a suitable carrier liquid is circulated down the well via tubing 90 and exits into the well bore via perforations 96 . The carrier liquid is circulated through screen sections 94 and 95 , which are configured as described previously, to permit the passage of the carrier liquid but retain the particulate plugging agent on the screen sections to form bridge packings (not shown) similarly as described above. Return flow in the configuration shown is through the tubing-casing annulus 98 . The lower screen section 95 is tapered as described previously in order to facilitate removal of the well tool. At the conclusion of the treating operation carried out through tubings 90 and 92 , carrier liquid may be circulated down the tubing casing annulus 98 into tubing section 93 . At the same time, the packer 97 may be released, and upward strain imposed by the working tubing 90 with the tapered screen section 95 facilitating removal from the lower bridge packing as described previously.
FIG. 10 is a side elevation with parts broken away of a downhole tool incorporating concentric tubing sections, which function similarly as described above with reference to FIG. 1 . In FIG. 10, like elements as are shown in FIG. 9 are designated by the same reference numerals as used in FIG. 9 . In the tool of FIG. 10, an outer concentric tubing 101 is provided with upper and lower screen sections 102 and 103 . Also suspended from the packer 91 is a concentric inner tubing section 105 , which is provided with an upper spider section 106 and a lower spider section (not shown) terminating in perforations in the outer tubing section 101 indicated by reference numeral 108 . The spider sections provide flow passages from the interior of tubing section 105 to the exterior of the tubing string 101 . The annulus 109 between the inner and outer tubing strings is placed in fluid communication with the tubing-casing annulus 98 through a passageway 110 in the packer 91 as indicated by broken lines. The interior of the tubing string 105 is placed in fluid communication with the working tubing string 90 as indicated by the broken line passageway 112 . The operation of the well tool shown in FIG. 10 is similar as that described above with reference to FIG. 1 . The carrier liquid containing the particulate plugging agent is introduced into the well through tubing 90 into tubing section 105 and thence outwardly through the spider passageways to the exterior of outer tubing section 101 . Return flow is directed into annulus 109 and then upwardly through the tubing-casing annulus 98 to form bridge packings (not shown) adjacent screen sections 102 and 103 .
As disclosed previously, the screen sections employed in the present invention may be of any suitable type but normally will take the form of a 0.006-0.01 inch mesh screen. FIG. 11 shows a suitable screen section configuration in which the screen section of the tubing 114 is provided with perforations 116 . A wire mesh screen (not shown) is wrapped around the perforated section of pipe 114 . The pipe functions to support the screen element. In addition, by appropriately sizing the perforations 116 when the reverse circulation carrier liquid is pumped down the well flow and flow through the constricted perforations 111 , it exits at a relatively high velocity, thus facilitating disruption of the particulate bridging agent around the screen section.
As described previously, the present invention may be carried out employing treating fluids other than those commonly used in acidizing, fracturing, or acid fracturing operations. A treating fluid may take the form of a solvent, other than an acidizing fluid, in order to remove material immediately adjacent the well bore to facilitate fluid flow between the well bore and the formation. Alternatively, a treating agent in the nature of a plugging agent can be introduced into the well in order to seal a section of the formation intermediate the bridge packings formed adjacent the screen sections. For example, a suspension of a thermoset polymer may be introduced into the well, followed by the introduction of a setting agent to crosslink the polymer and form a seal within a limited portion of the well bore. Suitable materials useful in the embodiment of this nature include crosslinked hydroxyethylcellulose.
The screen sections employed in the various embodiments of the invention may, as noted previously, be relatively short, e.g., on the order of about one or two feet. However, as a practical matter, screen sections will usually be provided ranging in lengths from about 5 to 20 feet. The interval between screen sections may range from a low as 2 feet up to perhaps 60 feet in length, depending upon the formation interval to be treated. However, a typical spacing between the screen sections will be about 10-30 feet from the top of the lower screen section to the bottom of the upper screen section.
From the foregoing description, it will be recognized that the viscosity of the carrier liquid and the particle size range and density of the particulate plugging agent are interrelated. In addition, the size of the screen openings is related to the characteristic of the particulate plugging agent since all or most of the plugging agent should be retained on the screen to form the bridge packing. The particulate plugging agent preferably will take the form of a sand/gravel mixture having a specific gravity of about 1.5-3.5 with a particle size distribution which promotes packing of the relatively fine sand particles within the interstices formed by the somewhat coarser gravel particles. For example, a suitable particulate plugging agent may comprise about 40-60 wt. % gravel having a particle size distribution of about 20-40 mesh and a relatively fine 40-60 mesh size sand portion comprising about 40-60 wt. % of the mixture. For such a particulate plugging agent, the viscosity of the carrier liquid should be within the range of about 20-200 centipoises. The screen section may take the form of a 0.006-0.01 inch mesh screen. Where the screen is wrapped around underlying perforated pipe as shown in FIG. 11, the perforations may have a diameter of about ⅛-⅜ inches with about 2-50 perforations per foot of pipe.
Having described specific embodiments of the present invention, it will be understood that modifications thereof may be suggested to those skilled in the art, and it is intended to cover all such modifications as fall within the scope of the appended claims.
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A method for the treatment of a subterranean formation penetrated by a well in which, first and second flow paths are established from the wellhead into the vicinity of the formation. A plugging fluid comprising a suspension of a particulate plugging agent in a carrier liquid is circulated into the first flow path and into contact with the wall of the well within the subterranean formation. The carrier liquid is separated from the particulate plugging agent by circulating the carrier liquid through a set of openings leading to the second flow path, which are dimensioned to allow the passage of the carrier liquid while retaining the particulate plugging agent in contact with the set of openings. The circulation of the plugging fluid continues until the particulate plugging agent accumulates to form a bridge packing within the well. Subsequent to establishing the bridge packing, a treating fluid is introduced into the well through the first flow path and in contact with the surface of the formation in the well adjacent to the bridge packing. The treating fluid may be a fracturing fluid under or an acidizing fluid. A clean-up fluid is circulated into the second flow path to remove the bridge packing.
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This application is a Divisional of application Ser. No. 10/572,396 filed on Jun. 6, 2007 now U.S. Pat. No. 7,955,991, and for which priority is claimed under 35 U.S.C. §120. Application Ser. No. 10/572,396 is the national phase of PCT International Application No. PCT/JP2004/013678 filed on Sep. 17, 2004 under 35 U.S.C. §371. The entire contents of each of the above-identified applications are hereby incorporated by reference. This application also claims priority of Application No. 2003-327358 filed in Japan on Sep. 19, 2003 under 35 U.S.C. §119.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a producing method of a semiconductor device and a substrate processing apparatus, and more particularly, to a producing method of a semiconductor device and a substrate processing apparatus which use CVD (Chemical Vapor Deposition) processing for reducing fine particles generated in a producing process.
2. Description of the Related Art
In a process for producing a semiconductor device, a film is formed on a substrate to be processed such as a wafer using chemical vapor deposition (CVD) method.
The film is formed in the following manner. That is, a predetermined number of wafers are mounted on a boat. The wafers mounted on the boat are loaded into a reaction furnace. The reaction furnace is evacuated, reaction gas is introduced into the reaction furnace, and films are formed on the wafers.
After the film formation is completed, the pressure in the reaction furnace is returned to the atmospheric pressure, and the boat is unloaded. The boat is cooled in a state in which the boat is completely pulled out from the furnace. At the same time, the temperature in the reaction furnace is lowered, and gas purging (decompression N 2 purging) is carried out. With the gas purging, stress of deposited film adhered to an inner wall of the reaction furnace is increased to allow a cracking to produce in the deposited film, and fine particles generated when the cracking is produced is eliminated by the gas purging (see Japanese Patent Application Laid-open Publication No. 2000-306904).
SUMMARY OF THE INVENTION
In this case, when the temperature in the furnace is lowered in a state where the processed substrates are unloaded from the reaction furnace, the temperature in the furnace is lowered from the film forming temperature to about 150° C. over several tens of minutes, e.g., 50 minutes at natural air cooling temperature lowering rate (≈3° C./min). However, with the temperature lowering rate of about 3° C./min, the particle discharging effect obtained by forcibly generating a cracking in the deposited film (film cracking generated when thermal stress caused by difference of coefficient of thermal expansion between the deposited film and a quartz reaction tube exceeds a tolerance limit value (mechanical disruptive strength of the deposited film)) is low. Especially in processing of φ300 mm wafer, it is found that a large number of particles are generated when the accumulated film thickness exceeds 1.2 μm and in the processing of φ300 mm wafer, the particle reducing effect is extremely low. Further, since about 50 minutes are required for reducing the temperature (≈3° C./min) by natural air cooling, there is a problem that availability rate of the substrate processing apparatus (semiconductor producing apparatus) is lowered and the productivity is deteriorated.
It is a main object of the present invention to provide a producing method of a semiconductor device and a substrate processing apparatus having excellent particle reducing effect and capable of enhancing the productivity.
According to an aspect of the present invention, there is provided a producing method of a semiconductor device, comprising:
loading a substrate into a reaction furnace;
forming a film on the substrate in the reaction furnace;
unloading the substrate from the reaction furnace after the film has been formed; and
forcibly cooling an interior of the reaction furnace in a state where the substrate does not exist in the reaction furnace after the substrate has been unloaded.
According to another aspect of the present invention, there is provided a producing method of a semiconductor device, comprising:
loading a substrate into a reaction furnace;
forming a film on the substrate in the reaction furnace;
unloading the substrate from the reaction furnace after the film has been formed; and
after the substrate has been unloaded and in a state where the substrate does not exist in the reaction furnace, lowering a temperature of the interior of the reaction furnace to a temperature lower than a film forming temperature simultaneously with gas-purging the furnace in a state where a pressure in the furnace is equal to the atmospheric pressure.
According to still another aspect of the present invention, there is provided a producing method of a semiconductor device, comprising:
loading a substrate into a reaction furnace;
forming a film on the substrate in the reaction furnace;
unloading the substrate from the reaction furnace after the film has been formed; and
after the substrate has been unloaded and in a state where the substrate does not exist in the reaction furnace, lowering a temperature of the interior of the reaction furnace to a temperature lower than a film forming temperature, simultaneously with supplying gas into the furnace and exhausting the furnace using an exhaust line which is different from an exhaust line used in the film forming.
According to still another aspect of the present invention, there is provided a producing method of a semiconductor device, comprising:
loading a substrate into a reaction furnace;
forming a film on the substrate in the reaction furnace;
unloading the substrate from the reaction furnace after the film has been formed; and
after the substrate has been unloaded and in a state where the substrate does not exist in the reaction furnace, once increasing a temperature of the interior of the furnace to a temperature higher than a film forming temperature and thereafter lowering the temperature of the interior of the reaction furnace to a temperature lower than a film forming temperature.
According to still another aspect of the present invention, there is provided a substrate processing apparatus, comprising:
a reaction furnace for forming a film on a substrate;
a film-forming gas supply line through which a film-forming gas is supplied into the reaction furnace;
a purge gas supply line through which purge gas is supplied into the reaction furnace;
an exhaust line through which the reaction furnace is exhausted;
a transfer device which loads and unloads the substrate to and from the reaction furnace;
a forcibly cooling device which forcibly cools an interior of the reaction furnace, and
a controller which controls the forcibly cooling device to forcibly cool the interior of the reaction furnace in a state where the substrate does not exist in the reaction furnace after the substrate is unloaded from the reaction furnace.
BRIEF DESCRIPTION OF THE FIGURES IN THE DRAWINGS
FIG. 1 is a schematic longitudinal sectional view for explaining a substrate processing apparatus according to a preferable embodiment of the present invention;
FIG. 2 is a schematic longitudinal sectional view for explaining a substrate processing apparatus according to a preferable embodiment of the present invention;
FIG. 3 is a diagram showing a wafer processing flow according to a preferable embodiment of the present invention;
FIG. 4 is a diagram showing a relationship between a temperature lowering width at the time of a LTP operation according to a first example of the present invention and particles;
FIG. 5 is a diagram showing a relationship between a temperature lowering rate at the time of a LTP operation according to a second example of the present invention and particles; and
FIG. 6 is a diagram showing a relationship between a accumulated film thickness at the time of a LTP operation according to a third example of the present invention and particles.
DETAILED DESCRIPTION OF THE INVENTION
In a an embodiment of the present invention, in a state where a substrate is taken out from the reaction furnace, an interior of the reaction furnace is abruptly cooled by a heater having a quick cooling mechanism at a temperature lowering rate of 10° C./min or more, preferably 20° C./min or more, thereby forcibly generating a cracking in a deposited film formed in the reaction furnace, fine particles generated when the cracking is generated is forcibly discharged by atmospheric pressure gas purge, fine particles adhering to a wafer are reduced, the cleaning frequency of the reaction furnace is reduced, and productivity is enhanced.
An embodiment of the present invention will be explained with reference to the drawings. A semiconductor producing apparatus as a substrate processing apparatus which carries out CVD film forming processing of the embodiment will be explained with reference to FIG. 2 . The semiconductor producing apparatus shown in FIGS. 1 and 2 is a hot wall type batch processing type vertical semiconductor producing apparatus.
FIG. 1 shows a state where a boat 9 on which the wafers 10 are mounted is loaded into the reaction furnace 1 , and a lower opening of a furnace opening flange 2 is closed with a furnace opening seal cap 12 . FIG. 2 shows a state where the boat 9 on which the wafers 10 are mounted is unloaded from the reaction furnace 1 into a transfer chamber 11 , and the lower opening of the furnace opening flange 2 is closed with a furnace opening gate valve 13 .
The reaction furnace 1 of a hot wall type, and includes the metal furnace opening flange 2 , a quartz outer tube 3 which air-tightly stands on the furnace opening flange 2 , a quartz inner tube 4 which stands concentrically within the quartz outer tube 3 , and a heater 5 provided outside of the quartz outer tube 3 such as to surround the quartz outer tube 3 .
A forcibly cooling mechanism 40 is provided such as to cover the quartz outer tube 3 and the heater 5 . The forcibly cooling mechanism 40 includes a thermal insulation cover 41 covering the quartz outer tube 3 and the heater 5 , a supply line 42 which is in communication with an interior space of the thermal insulation cover 41 , and an exhaust line 43 which is in communication with the interior space of the thermal insulation cover 41 through an exhaust hole 44 formed in a ceiling of the thermal insulation cover 41 . The supply line 42 is provided with a shutter 46 and an introduction blower 45 . The exhaust line is provided with a shutter 47 , a radiator 48 and an exhaust blower 49 .
Gas introducing lines 6 and 7 are in communication with an interior of the reaction furnace 1 for introducing reaction gas, and an exhaust line 30 is also in communication with the interior of the reaction furnace 1 . The gas introducing lines 6 and 7 are connected to the furnace opening flange 2 at a location lower than a lower end of the quartz inner tube 4 . The exhaust line 30 is connected to the furnace opening flange 2 at a location lower than a lower end of the quartz outer tube 3 and higher than the lower end of the quartz inner tube 4 . The exhaust line 30 includes a main exhaust line 31 which is in communication with an exhaust apparatus 8 such as a vacuum pump, a HFV (high flow vent) line 32 which is branched off from the main exhaust line 31 , a slow exhaust line (now shown) which is branched off from the main exhaust line 31 , and an overpressure preventing line 33 and a nitrogen gas introducing line 34 which are branched off from the main exhaust line 31 . An APC valve as a main valve is provided on the main exhaust line 31 downstream from the branch point of the flow vent line 32 . A slow exhaust line is provided such as to bypass the APC valve.
The high flow vent line 32 is in communication with an exhaust system of a building service. Exhaust flow rate of the high flow vent line 32 is greater than those of the main exhaust line 31 , the slow exhaust line (not shown) and the overpressure preventing line 33 , and gas of high flow rate can flow through the high flow vent line 32 at atmospheric pressure. An inner diameter of the high flow vent line 32 is smaller than that of the main exhaust line 31 , and is greater than those of the slow exhaust line (not shown) and the overpressure preventing line 33 . The high flow vent line 32 includes a valve 35 . By switching between the valve 35 and the APC valve, the exhaust route can be switched between the main exhaust line 31 and the high flow vent line 32 .
The overpressure preventing line 33 includes a valve 36 and a check valve 37 . If the pressure in the main exhaust line 31 , i.e., in the reaction furnace 1 becomes equal to or higher than the atmospheric pressure, the check valve 37 is opened, atmosphere in the main exhaust line 31 is exhausted through the check valve 37 . Therefore, the pressure in the main exhaust line 31 , i.e., in the reaction furnace 1 is prevented from becoming overpressure higher than the atmospheric pressure.
A boat elevator 15 as boat transfer (vertically moving) means is provided in a substrate transfer chamber 11 below the reaction furnace 1 . The boat is moved upward and downward to load and unload the boat 9 into and out from the reaction furnace 1 . The wafers 10 which are substrates to be processed are mounted in a multi-stacked manner at distances from one another in a horizontal attitude. The boat 9 may be made of quartz.
As shown in FIG. 1 , in a state where the boat 9 is loaded into the reaction furnace 1 and the lower opening of the furnace opening flange 2 is closed with the furnace opening seal cap 12 , the furnace opening gate valve 13 is in a standby status at a standby position 14 . When the boat 9 is unloaded into the transfer chamber 11 from the reaction furnace 1 as shown in FIG. 2 , the lower opening of the furnace opening flange 2 is closed with the furnace opening gate valve 13 .
A control apparatus 20 controls heating operation of the heater 5 , cooling operation of the forcibly cooling apparatus 40 , introducing operation of gas of the gas introducing lines 6 and 7 , selecting operation of the exhaust line by switching between the valves, and exhausting operation of the exhaust line.
A method for forming films on semiconductor silicon wafers using CVD as one process of a producing step of semiconductor devices using the apparatus will be explained with reference to FIGS. 1 to 3 . In the following explanation, operations of various members constituting the apparatus are controlled by the control apparatus 20 .
As described above, the substrate transfer chamber 11 exists below the reaction furnace 1 , and in a state where the boat 9 is lowered into the substrate transfer chamber 11 , a predetermined number of wafers 10 are charged into the boat 9 (Wafer Charge) by a substrate transfer device (not shown). In this state, atmosphere in the reaction furnace 1 is maintained under the atmospheric pressure, and when the wafers 10 are charged into the boat 9 , inert gas, e.g., N 2 is introduced into the reaction furnace 1 at the same time. At that time, the temperature in the reaction furnace 1 is set to 600° C.
Next, the boat 9 is moved upward by the boat elevator 15 , and the boat 9 is loaded into the reaction furnace 1 (Boat Load) whose temperature is set to 600° C. After the boat 9 is loaded into the reaction furnace 1 , the reaction furnace 1 is evacuated slowly (Slow Pump) by the exhaust apparatus 8 through the slow exhaust line. When the pressure in the reaction furnace 1 is lowered to a predetermined pressure, the APC valve is opened, the reaction furnace 1 is evacuated by the exhaust apparatus 8 through the main exhaust line 31 , and the pressure in the reaction furnace 1 reaches a predetermined pressure.
The temperature in the reaction furnace 1 is increased from 600° C. to 730° C. to 800° C., e.g., to the film forming temperature of 760° C. (Ramp Up), and when the wafer temperature reaches the film forming temperature and is stabilized (Pre Heat), reaction gas is introduced into the reaction furnace 1 from the gas introducing lines 6 and 7 , and films are formed on the wafers 10 (Depo). For example, when an Si 3 N 4 film (nitride silicon film, Sin hereinafter) is to be formed on the wafer 10 , gas such as DCS (dichlor silane (SiH 2 Cl 2 )) and NH 3 is used. In this case, the temperature in the reaction furnace 1 is maintained at the film forming temperature of 730° C. to 800° C.
After the film forming processing is completed, gas is exhausted from the reaction furnace 1 while introducing inert gas (e.g., N2) into the reaction furnace 1 , thereby carrying out gas purging in the reaction furnace 1 , and residual gas is purged (Purge). Thereafter, the main valve is closed, the introduction of the inert gas is maintained, and the pressure in the reaction furnace 1 is returned to the atmospheric pressure (Back Fill). Then, the wafers 11 formed with films supported by the boat 9 are lowered by the boat elevator from the reaction furnace 1 , and are unloaded into the substrate transfer chamber 11 (Boat Down).
The temperature in the furnace is lowered from 760° C. to 700° C. before the boat 9 is unloaded for increasing the unloading speed of the boat. If the temperature in the reaction furnace 1 when the boat is unloaded is lower than the film forming temperature (760° C.), a temperature difference or variation over the entire surface of a wafer when the boat is unloaded can be reduced, and a flexure amount of a wafer can be reduced. In such a state, the boat can be moved down swiftly without affecting the wafer. The temperature is slightly lowered also for moderating thermal influence on peripheral members when the boat is unloaded.
After the boat is unloaded, an opening of the reaction furnace (boat in/out opening), the opening of the furnace opening flange 2 is closed air-tightly with the furnace opening gate valve 13 (see FIG. 2 ). Then, wafers 10 after the films are formed are cooled in the substrate transfer chamber 11 (Wafer Cool). The cooling operation of the wafers 10 in the substrate transfer chamber 11 is completed, the wafers 10 are discharged from the boat 9 by a substrate transfer device (not shown) (W/F Discharge)
Together with the cooling operation of the wafers 10 (Wafer Cool) and the discharging operation of the wafers (W/F Discharge), gas purging is carried out using inert gas in a state where the air-tightly closed reaction furnace 1 is brought into the atmospheric pressure. For example, N 2 purging is carried out. When purging is carried out, it is preferable that while supplying N 2 of large flow rate of 20 L/min or more into the reaction furnace 1 , gas is exhausted through the high flow vent line 32 which is branched off from the main exhaust line 31 . In this case, the valve 35 is opened, and the main valve is closed.
Simultaneously with the purging in the furnace in the atmospheric pressure state, the temperature in the reaction furnace 1 is reduced at greater temperature lowering rate (≈3° C./min) than the temperature lowering rate at the time of natural cooling operation by the forcibly cooling mechanism 40 , and the temperature in the furnace is abruptly varied. With this, stress of the deposited film adhered to the reaction furnace 1 is increased as compared with the natural cooling operation to positively generate the thermal stress, and a cracking more than the natural cooling operation is forcibly generated in the deposited film. Fine particles scattered when the cracking is generated are forcibly and efficiently discharged out from the reaction furnace by the purging in the furnace in the atmospheric pressure state. When the temperature in the furnace is lowered by the forcibly cooling mechanism 40 , the shutters 46 and 47 are opened, atmospheric gas of high temperature in the thermal insulation cover 41 is exhausted by the exhaust blower 49 , and cooling medium such as air and N 2 is introduced into the thermal insulation cover 41 by the introduction blower 45 .
It is preferable that the temperature lowering rate is at least 10° C./min or more, and more preferable 20° C./min or more. Concerning the temperature reduction in the furnace, the temperature in the reaction furnace 1 is lowered to about ½ (50%) or lower of at least the film forming temperature. That is, the temperature lowering width (amount) is set to about ½ (50%) or more of at least the film forming temperature. For example, when the film forming temperature is about 730 to 800° C., the temperature in the reaction furnace 1 is lowered from 800° C. to 400° C.
Before the temperature in the reaction furnace 1 is lowered, the temperature in the reaction furnace 1 is once increased higher than the film forming temperature and then, the temperature may be reduced lower than the film forming temperature. In the case of FIG. 3 , after the boat is moved down, the temperature in the reaction furnace 1 is once increased higher than the temperature in the furnace (700° C.) when the boat is moved down and increased to 800° C. which is higher than the film forming temperature (760° C.) at the temperature increasing rate of 40° C./min and then, the temperature in the furnace is reduced to 400° C. which is lower than the film forming temperature at the temperature lowering rate of 20° C./min. If the temperature in the furnace is once increased before it is lowered in this manner, the temperature lowering width (temperature difference) can be increased without lowering the temperature of the temperature-lowering end so much and thus, the temperature increasing time after the temperature is lowered can be shortened.
The temperature in the furnace is increased before the temperature is lowered so as to increase the temperature difference (temperature lowering width) without reducing the temperature-lowering end so much. This operation can be omitted but in such a case, the temperature difference (temperature lowering width) is reduced, and the particle-reducing effect is deteriorated. To prevent the particle-reducing effect from being deteriorated, it is necessary to lower the temperature of the temperature lowering end to increase the temperature difference (temperature lowering width), but in such a case, the temperature increasing time after the temperature is lowered is increased, and the throughput is deteriorated.
Also when the temperature is increased before the temperature in the furnace is lowered, the temperature in the furnace is abruptly varied. Therefore, it is conceived that cracking to some extent is generated in the deposited film which is adhered to the furnace. However, according to the theoretical calculation, it is conceived that stress difference between quartz (furnace wall) and the deposited film is increased when the temperature in the furnace is lowered, and cracking is more prone to be generated.
As an experiment, purging was carried out while lowering the temperature in the furnace from 800° C. to 400° C. slowly without forcibly cooling (abruptly cooling) the furnace. As a result of the experiment, cracking was not generated so much in the deposited film adhered to the furnace, and the effect was insufficient. That is, it was found that sufficient effect could not be obtained only by increasing the temperature difference (temperature lowering width). To obtain sufficient effect, it is necessary to increase both (1) temperature difference (temperature lowering width) and (2) temperature lowering speed.
If the gas purging is carried out simultaneously with the forced cooling in the furnace using inert gas in the reaction furnace 1 under the atmospheric pressure, there is a merit that the particle eliminating effect is greater as compared with the gas purging carried out under a reduced pressure. This is because that the number of molecules and the number of atoms which carry foreign matters under the atmospheric pressure are greater as compared with those under the reduced pressure, and energy for carrying foreign matters is greater.
If N 2 molecules are exhausted by a vacuum pump such as a turbo molecule pump or the like, since the N 2 molecules roughly exist in the gas flow and average free path of the N 2 molecule is large, even if the flow speed of N 2 molecule is increased, it is difficult to discharge particles as molecule flow. This is because that the probability that Brownian moving particles by heat do not collide against the N 2 molecules and drop by gravitation is high.
In the case of exhausting operation under the atmospheric pressure, although the gas flow speed becomes as slow as about 10 cm/min, since N 2 molecules finely exist in the gas flow and collide against particles, it is easy to exhaust the particles. This is because that wind of N 2 gas blows from introducing side toward exhausting side in the furnace, and the wind blows off the particles out from the furnace.
For comparison, gas purging was carried out in a furnace under a reduced pressure and under the atmospheric pressure as experiments, and it was found that the particle eliminating effect of gas purging under the atmospheric pressure is much more excellent as compared with gas purging under the reduced pressure.
In the case of purging under the reduced pressure, a step for returning the pressure in the furnace to the atmospheric pressure after the purging is required and time loss is generated. In the case of purging under the atmospheric pressure, there is a merit that such a step is unnecessary and the purging time can be shortened.
In the case of the purging under the reduced pressure, by-product which is adhered to an exhaust system or periphery thereof sublimes and flows backward into the furnace in some cases, but in the case of the purging under the atmospheric pressure, such a problem is not caused.
When the interior of the furnace is only cooled forcibly and purging is not carried out, generated particles drop onto the furnace opening gate valve 13 . Particles which drop to the furnace opening gate valve 13 are retracted to an evacuation position 14 in a state where the particles are held on the furnace opening gate valve 13 when next films are formed. That is, next films are to be formed, it is possible to create a state where no particles exist in the furnace so that particles do not affect the next film forming operation. The furnace opening gate valve 13 is provided at its upper surface with grooves (recesses), and the dropped particles can be accommodated in the grooves. Therefore, when the furnace opening gate valve 13 is to be moved to the evacuation position 14 , the particles can be prevented from dropping. The evacuation position 14 may be provided with a particle removing mechanism (sucking means or the like), and particles on the furnace opening gate valve may be removed while the furnace opening gate valve 13 is retracted.
In a state where wafers 10 are unloaded from the reaction furnace 1 and the reaction furnace 1 is air-tightly closed, the temperature in the reaction furnace 1 is lowered to about half of the film forming temperature at a temperature lowering rate of at least 10° C./min or more, more preferably 20° C./min or more and in this state, inert gas is purged. This series of operations is carried out while controlling the heater 5 , the forcibly cooling apparatus 40 , the gas supply system, the exhaust system and the like by the control means 20 . The purging in the furnace is called a low temperature purging (LTP).
A preferable temperature increasing rate when the temperature is to be increased before the temperature in the furnace is lowered in the LTP is 3° C./min or more, preferably 10 to 100° C./min, and more preferably 30 to 100° C./min. A preferable temperature lowering rate when the temperature in the furnace is to be lowered is 3° C./min or more, preferably 10 to 100° C./min, and more preferably 20 to 100° C./min.
When the discharging operation of the wafers 10 from the boat 9 in the substrate transfer chamber 11 is completed, a desired number of next wafers 10 are charged into the boat 9 by the substrate transfer device (Wafer charge). At the same time, the temperature in the furnace is increased to a standby temperature, e.g., 600° C. If the wafers 10 are charged into the boat 9 , the boat 9 is moved upward by the boat elevator 15 , the boat 9 is loaded into the reaction furnace 1 (Boat Load), and the next batch processing is continued.
A reason why the temperature in the furnace is increased from 400° C. to 600° C. before the boat is loaded after the LTP is that the temperature in the furnace increasing time after the boat is loaded in next film forming operation is shortened, and total film forming time is shortened. If the temperature in the furnace is held at 400° C. which is the temperature lowering end of the LTP after the LTP, it is necessary to load the boat at 400° C. at the next film forming operation and to increase the temperature in the furnace from 400° C. to 760° C. (by 360° C.), and the temperature increasing time is increased. If the temperature in the furnace is increased to 600° C. after the LTP, the boat can be loaded at 600° C. at the next film forming operation and then, the temperature in the furnace may be increased from 600° C. to 760° C. (by 160° C.), and the temperature increasing time can be shortened. If the temperature in the furnace when the boat is to be loaded is excessively high, the wafer may be warped. The temperature in the furnace is set to 600° C. while taking this problem into consideration.
In the water processing, in a state where the reaction furnace 1 is air-tightly closed after the boat is unloaded (in a state where there is no wafer 10 in the reaction furnace 1 ), N 2 is purged from the reaction furnace 1 under the atmospheric pressure and in this state, air is exhausted under the atmospheric pressure. At the same time, the temperature in the furnace is lowered (reduced) from 800° C. to 400° C. by the forcibly cooling mechanism 40 at a temperature lowering rate of 20° C./min or more. By lowering the temperature in this manner, stress of the reaction by-product deposited film adhered to an inner surface of the reaction furnace 1 is increased as compared with a case of natural air cooling (temperature lowering rate≈3° C./min), the thermal stress is positively generated, and cracking greater than that of the natural cooling is forcibly generated in the deposited film. By purging gas from the reaction furnace 1 under the atmospheric pressure, fine particles scattered by the generated cracking are forcibly and efficiently discharged out from the reaction furnace 1 .
The temperature in the furnace when films are formed is higher than the temperature lowering end temperature (400° C.) in the LTP by several hundred degrees, and stress of a deposited film whose temperature was once lowered (400° C.) is moderated. Therefore, new cracking is prevented from being generated when SiN films of next batch processing are to be formed. It is found that if the temperature is increased, stress of the deposited film is reduced, and since the stress of the deposited film is reduced when films are to be formed, the possibility that a new cracking is generated when films are formed is further reduced.
Cracking is previously generated in a deposited film, and fine particles generated when the cracking is generated is forcibly discharged out from the reaction furnace 1 before a boat is loaded. Therefore, wafers are processed in a state where there are no fine particles. Since particles which are generated by the cracking in the deposited film can efficiently be removed, the reaction furnace 1 may be cleaned before the deposited film is peeled. According to the present invention, time period during which a deposited film is peeled can largely be increased. Therefore, it is possible to largely increase the time interval between cleaning periods of the reaction furnace 1 (time elapsed before thickness of a deposited film becomes 25 μm).
Since the coefficients of thermal expansion of SiC and SiN are close to each other, large stress difference is not generated so much between SiC and SiN. Therefore, when a reaction tube such as the outer tube 3 and the inner tube 4 is made of SiC, excellent effect of the LTP can not be expected so much. Since the coefficients of thermal expansion of SiO 2 (quartz) and SiN are largely different from each other, a stress difference therebetween is large. That is, the LTP is especially effective when a reaction tube made of quartz is used and SiN films are formed.
First Example
Next, an experiment carried out for finding out a relation between a temperature lowering width in the LTP and generated particles will be explained below as a first example.
Using the wafer processing method in the above embodiment, SiN films, especially Si 3 N 4 films whose film thickness of one film-formation was 1500 Å or higher were formed on silicon wafers of φ300 mm. DCS (SiH 2 Cl 2 ) and NH 3 were used as reaction gases and the film forming temperature was 730° C. to 800° C. The temperature lowering rate in the LTP was 20° C./min. The processing was carried out while varying the temperature lowering width between three values, i.e., 300° C., 400° C. and 800° C., and the number of particles after the processing in each case was measured.
FIG. 4 shows a result of the measurement (relation between particles and the temperature lowering width in the LTP). A horizontal axis shows the temperature lowering width (° C.) in the LTP, and a vertical axis shows the number of particles (the number of particles/wafer) which are adhered to a wafer and which is 0.13 μm or greater. In FIG. 4 , T represents a top wafer and B represents a bottom wafer. From FIG. 4 , it can be found that the number of particles is about 60 to 70 when the temperature lowering width is 300° C., and the number of particles is 40 or less when the temperature lowering width is 400° C. That is, if the temperature lowering width is 400° C. (about 50% of film forming temperature) when the film forming temperature is 730° C. to 800° C., the particles can largely be reduced (at least 40 particles or less).
Second Example
Next, an experiment carried out for finding out a relation between a temperature lowering width in the LTP and generated particles will be explained below as a second example.
According to the wafer processing method of the above example, SiN films, especially Si 3 N 4 films whose film thickness of one film-formation was 1500 Å or higher were formed on silicon wafers of φ300 mm. DCS (SiH 2 Cl 2 ) and NH 3 were used as reaction gases and the film forming temperature was 730° C. to 800° C. The temperature lowering width in the LTP was 400° C. The processing was carried out while varying the temperature lowering rate between three values, i.e., 0° C./min, 4° C./min and 20° C./min, and the number of particles after the processing in each case was measured.
FIG. 5 shows a result of the measurement (relation between particles and the temperature lowering rate in the LTP). A horizontal axis shows the temperature lowering rate (° C./min) in the LTP, and a vertical axis shows the number of particles (the number of particles/wafer) which are adhered to a wafer and which is 0.13 μm or greater. In FIG. 5 , T represents a top wafer and B represents a bottom wafer. In FIG. 5 , when the temperature lowering rate is set to 0° C./min (i.e., when the temperature is not lowered), the number of particles of the top wafer is about 460, and the number of particles of the bottom water is about 60. When the temperature lowering rate is set to 4° C./min, the number of particles of the top wafer is about 100 or more, and the number of particles of the bottom water is about 70. When the temperature lowering rate is set to 20° C./min, the number of particles of the top wafer and the number of particles of the bottom water are both 30 or less. That is, if the temperature lowering rate in the LTP is set to 20° C./min or higher, the number of particles can largely be reduced (at least 30 or less). As a result of another experiment, it could be checked that if the temperature lowering rate was set to at least 10° C./min or higher, the number of particles could largely be reduced as compared with the natural cooling.
Third Example
Next, an experiment carried out for finding out a relation between particles and accumulated film thickness at the time of the LTP will be explained below as a third example.
According to the wafer processing method of the above example, SiN films, especially Si 3 N 4 films whose film thickness of one film-formation was 1500 Å (150 nm) or higher were formed on silicon wafers of φ300 mm. DCS (SiH 2 Cl 2 ) and NH 3 were used as reaction gases and the film forming temperature was 730° C. to 800° C. The temperature lowering width in the LTP was 400° C., and the temperature lowering rate was 20° C./min. Wafer cooling time was 15 minutes and wafer collecting time was 15 minutes. Therefore, the LTP was carried out simultaneously with these events within this total time (30 minutes) so that throughput is not lowered. In this example, the total time of the LTP was 30 minutes (temperature increasing time before the temperature is lowered was 10 minutes and the temperature lowering time was 20 minutes). Under such conditions, wafers were subjected to continuous batch processing, and after the batch processing, the number of particles adhered to the wafer was measured.
FIG. 6 shows a result of the measurement (a relation between particles and accumulated film thickness). A horizontal axis shows the number of continuous batch processing (Run No.), a left vertical axis shows the number of particles which adheres to the wafer (the number of particles/wafer), and a right vertical axis shows accumulated film thickness (nm). In FIG. 6 , TOP represents a top wafer and BOTTOM represents a bottom wafer. A bar graph shows the number of particles, and a line graph shows accumulated film thickness. From FIG. 6 , it can be found that the number of particles is about 50 or less until Run No. 119 (119th batch processing) was carried out, i.e., until the accumulated film thickness became 23 μm (23000 nm). The present inventors performed an experiment and could check that the number of particles became 50 or less even if the accumulated film thickness exceeded 25 μm (25000 nm).
When the present invention is not carried out, if the accumulated (cumulative) film thickness exceeds 1 μm (1000 nm), the number of particles is abruptly increased and largely exceeds 200. If the present invention is carried out, however, the number of particles becomes 50 or less even if the accumulated film thickness exceeded 25 μm (25000 nm). In the case of this example, the film thickness accumulated during one batch processing is 0.15 μm (150 nm). Therefore, in the conventional technique, to make it possible to form films while suppressing the number of particles to 50 or less, the continuous batch processing can be carried out only about seven times. If the present invention is carried out, however, the continuous batch processing can be carried out about 167 times. That is, the time interval between the cleaning time periods of the reaction furnace can largely be increased, and the cleaning frequencies of the reaction furnace can largely be reduced.
The entire disclosure of Japanese Patent Application No. 2003-327358 filed on Sep. 19, 2003 including specification, claims, drawings and abstract are incorporated herein by reference in its entirety.
Although various exemplary embodiments have been shown and described, the invention is not limited to the embodiments shown. Therefore, the scope of the invention is intended to be limited solely by the scope of the claims that follow.
INDUSTRIAL APPLICABILITY
As explained above, according to the embodiment of the present invention, cracking is forcibly generated in a deposited film produced in the reaction furnace before films are formed, and fine particles produced when the cracking is generated are discharged out. Therefore, it is possible to restrain fine particles from being generated when films are formed, and films of high quality can be formed. Since the cleaning operation of the reaction furnace may be carried out before the deposited film is peeled, there are excellent effects that time interval between the cleaning time periods is increased, maintenance performance is enhanced, an availability factor is enhanced, and the processing time is not increased as compared with the conventional technique.
As a result, the present invention can preferably be utilized for a producing method of a semiconductor device having a film forming step using the CVD and for a substrate processing apparatus which can preferably carry out the film forming step.
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Disclosed is a producing method of a semiconductor device, comprising: loading a substrate into a reaction furnace; forming a film on the substrate in the reaction furnace; unloading the substrate from the reaction furnace after the film has been formed; and forcibly cooling an interior of the reaction furnace in a state where the substrate does not exist in the reaction furnace after the substrate has been unloaded.
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This is a division of application Ser. No. 116,696, filed Jan. 30, 1980, now U.S. Pat. No. 4,278,663.
DESCRIPTION OF THE INVENTION
The present invention relates to the novel antibiotic X-14868A which has the formula ##STR2## and the pharmaceutically acceptable salts thereof.
As utilized in the structural formulas herein the expression Me stands for the term methyl.
There is further provided according to the present invention a fermentation process for the production of such antibiotic substance together with the isolation techniques utilized to recover the antibiotic compound from the fermentation broth.
The organism producing the antibiotic of the present invention is a new species designated Nocardia sp. X-14868. A culture of the living organism, given the laboratory designation X-14868, has been deposited in the American Type Culture Collection, Rockville, Md. and added to its permanent collection of microorganisms as ATCC 31585. The culture has been identified as a strain of Nocardia.
The new microorganism was isolated from a soil sample collected from beach sand in Colloroy, Australia. A representative strain of Nocardia sp. X-14868 has the following characteristics:
General Characteristics
Nocardia sp. X-14868 is characterized by its lack of aerial spore formation, fragmentation of the Gram positive substrate mycelium after several days of incubation and cell wall composition consisting of meso-diaminopimelic acid, galactose and arabinose.
Growth Characteristics
The organism was cultivated on the standard ISP media (Difco) described by Shirling and Gottlieb "Methods for Characterization of Streptomyces Species", Intern. J. System. Bacteriol., 16, pp 313-340, 1966 as well as various other media used to characterize the culture as listed below:
Yeast extract:
yeast extract, 1.0%; glucose, 1.0%; agar, 1.5%; pH 6.8
Glucose-Yeast extract-peptone:
glucose, 0.3%; yeast extract, 0.5%; peptone, 0.5%; CaCO 3 , 0.75%; agar, 1.5%, pH 7.0
Glucose-asparagine:
glucose 1.0%; asparagine, 0.05%; K 2 HPO 4 , 0.05%; agar, 1.5%; pH 6.8
Sucrose-nitrate:
sucrose, 1.0%; NaNO 3 , 0.2%; K 2 HPO 4 , 0.1%; MgSO 4 7H 2 O, 0.05%; KCl, 0.05%; agar, 1.5%.
Media utilized in other tests were those from the following references:
__________________________________________________________________________ References__________________________________________________________________________A. Sodium Chloride tolerance Gordon and Smith, "Rapidly Growing AcidB. Hydrolysis of casein Fast Bacteria", J. Bacteriol., 66:41-48, 1953C. Reduction of nitrateD. Gelatin (modified with Actinomyces Skerman, "A Guide to the Identification of the broth [Difco] plus 2.0% agar in Genera of Bacteria", William and Williams meat infusion agar) Co., Baltimore, 1967.E. Starch (Actinomyces broth [Difco] plus 0.25% soluble starch and 2.0% agar)F. Action on Litmus Milk (Difco)G. Resistance to Lysozyme Gordon, "Some Criteria for the Recognition of Nocardia..", J. Gen. Microbiol., 45:355-364, 1966.H. Sensitivity to penicillin (10 unit discs)__________________________________________________________________________
Test were run at 28° and 37° C. for almost all media. Color determinations were made after 2 and 4 weeks of incubation.
Carbon utilization was determined by the method of Shirling and Gottlieb (above) using ISP-9 (Difco) medium.
A 48 hour-old ISP-1 broth culture of X-14868 was centrifuged and homogenized to obtain a washed suspension for inoculation.
The ability of the organisms to grow at 10°, 28°, 36°, 45° and 50° C. was investigated by inoculating broth of ISP-1 (Difco) medium. Cell wall analysis of the isomer of diaminopimelic acid was performed by the method of Becker et al., Appl. Microbiol., 12, 421-423, 1964. For sugar content of the cell wall, the method of Lechevalier and Lechevalier, Actinomycetales, Ed. H. Prauser, Gustav Fischer, Jena, p 311-316, 1970 was followed. Nocardomycolic acid analysis was performed by a slight modification of the method of Lechevalier, Lechevalier, and Horan, Can. J. Microbiol. 19:965-972, 1973.
Results
Microscopic Examination
Strain X-14868 produces a substrate mycelium, which fragments after several days allowing extensive mycelial development. It produces an aerial mycelium consisting of rope-like tufts but no spores were found.
Cell Wall Analysis
The cell wall contains the meso-isomer of diaminopimelic acid as well as galactose and arabinose (cell wall type IV of the classification by Lechevalier et al., Adv. Appl. Microbiol., 14, 47-72, 1971). The organism appears to produce nocardomycolic acids. These morphological and chemical criteria assign X-14868 to the genus Nocardia.
Microscopic Examination
Table 1 summarizes the amount of growth, degree of sporulation, aerial mass color, color of reverse substrate mycelium and presence of any soluble pigment produced by Strain X-14868 on various solid media after 4 weeks of incubation at 28° C.
TABLE 1__________________________________________________________________________Cultural Characteristic of Strain X-14868Agar Amount of Growth Color of ReverseMedium and Aerial Mycelium Color of Aerial Mycelium.sup.a Substrate Mycelium.sup.a__________________________________________________________________________Yeast malt moderate to abundant growth; b (oyster white) 2 ie (lt. mustard tan)extract (ISP-2) some aerial mycelium in isolated edges, leathery growthOatmeal moderate growth; moderate aerial b (oyster white) 3 dc (natural)(ISP-3) myceliumInorganic sparse growth; sparse aerial mycelium b (oyster white) 2 dc (natural, string)Salts-Starch(ISP-4)Glycerol aspara- poor growth; nearly no aerial mycelium; b (oyster white) 2 ge (covert tan)gine (ISP-5) substrate myceliumYeast extract abundant growth; sparse aerial b (oyster white) 3 ge (beige) mycelium; leatheryGlucose-Yeast moderate growth; sparse aerial b (oyster white) at edge 3 ge (beige)extract-peptone mycelium at edge; leathery, brown soluble pigmentGlucose-aspara- moderate growth; some aerial 2 dc (natural, string) 3 ge (beige)gine mycelium; leatherySucrose-nitrate sparse growth; moderate aerial b (oyster white) translucent c mycelium (lt. gray)__________________________________________________________________________ Note: No spores were found in the aerial mycelium on any of the media examined after 4 weeks of incubation. .sup.a The color scheme used was Color Harmony Manual, tth ed. 1958 (Container Corporation of America, Chicago).
Physiological Characteristics
Strain X-14868 hydrolyzed gelatin and casein but not starch. The culture was resistant to a 10 unit disk of penicillin as well as 0.005% lysozyme dissolved in broth when tested according to the method of Gordon, J. Gen. Microbiol., 45, 355-364, 1966. The strain completely peptonized litmus milk. No melanin production was detected on ISP 1, 6 or 7.
Table 2 reports the results of carbon utilization on ISP 9 (Difco) by Strain X-14868 at 28° C. after one month incubation.
TABLE 2______________________________________Carbon Utilization by Strain X-14868Carbon Source Response.sup.a______________________________________No carbon control -D-Glucose ++D-Xylose -L-Arabinose -L-Rhamnose -D-Fructose ±D-Galactose +Raffinose -D-Mannitol -i-Inositol -Salicin ±Sucrose -Cellulose -______________________________________ .sup.a -, negative response; ±doubtful response; +more growth than on carbon control but less than on ++positive response, equal to the amount of growth on glucose.
In Table 3 is a list of diagnostically important, mostly metabolic, properties.
TABLE 3______________________________________Characteristics of X-14868Test Result______________________________________ISP 1, darkening -ISP 6, darkening -ISP 7, melanin -Casein hydrolysis ++Gelatin hydrolysis ++Starch hydrolysis -NaCl (%) tolerance 5%Temperature at whichgrowth was observed 28 and 36° C.Reverse side pigment noneSoluble pigment brown on glucose yeast extract-peptonePenicillin (10 unit disk)sensitivity -Nitrate reduction ++Gram strain +Acid fast stain -Catalase +Diaminopimelic acid meso-isomerCell wall sugars galactose, arabinose, riboseProduction ofnocardomycolic acid +______________________________________
The species Nocardia X-14868 described herein includes all strains of Nocardia which produce the antibiotic X-14868A and which cannot be definitely differentiated from the culture Nocardia X-14868 and its subcultures including mutants and variants thereof. The compound X-14868A is structurally identified herein and after this identification is known, it is easy to differentiate the strains producing the antibiotic compound X-14868A from others.
The pharmaceutically acceptable salts of antibiotic X-14868A can be prepared by conventional means. These salts are prepared from the free acid form of the antibiotic by methods well-known in the art, for example, by washing the free acid in solution with a suitable base or salt. Examples of such pharmaceutically acceptable basic substances capable of forming salts for the purpose of the present invention include alkali metal bases such as sodium hydroxide, potassium hydroxide, lithium hydroxide and the like; alkaline earth metal bases such as calcium hydroxide, barium hydroxide and the like; and ammonium hydroxide. Alkali metal or alkaline earth metal salts suitable for forming pharmaceutically acceptable salts can include anions such as carbonates, bicarbonates and sulfates.
Nocardia X-14868, when grown under suitable conditions, produces the compound X-14868A. A fermentation broth containing Nocardia X-14868 is prepared by inoculating spores or mycelia of the organism producing the compound X-14868A into a suitable medium and then cultivating under aerobic conditions. For the production of the X-14868A, cultivation on a solid medium is possible but for production in large quantities, cultivation in a liquid medium is preferable. The temperature of the cultivation may be varied over a wide range, 20°-35° C., within which the organism may grow but a temperature of 26°-30° C. and a substantially neutral pH are preferred. In the submerged aerobic fermentation of the organism for the production of the antibiotic X-14868A, the medium may contain as the source for carbon, a commercially available glyceride oil or a carbohydrate such as glycerol, glucose, maltose, lactose, dextrin, starch, etc. in pure or crude states and as the source of nitrogen, an organic material such as soybean meal, distiller's solubles, peanut meal, cotton seed meal, meat extract, peptone, fish meal, yeast extract, corn steep liquor, etc. and when desired inorganic sources of nitrogen such as nitrates and ammonium salts and mineral salts such as ammonium sulfate, magnesium sulfate and the like. It may also contain sodium chloride, potassium chloride, potassium phosphate and the like and buffering agents such as sodium citrate, calcium carbonate or phosphates and trace amounts of heavy metal salts. In aerated submerged culturing procedures, an anti-foam agent such as liquid paraffin, fatty oils or silicone compounds is used. More than one kind of carbon source, nitrogen source or anti-foam source may be used for production of the antibiotic X-14868A.
The following table sets forth the antimicrobial activity of antibiotic X-14868A and the three minor components X-14868B; X-14868C; and X-14868D.
TABLE 4__________________________________________________________________________ Minimum Inhibitory Concentration (mcg/ml) of AntibioticsMicroorganism X-14868A X-14868B X-14868C X-14868D__________________________________________________________________________G (+) cocciStreptococcus faecium ATCC 8043 0.313 1.57 0.79 0.19Staphylococcus aureus 82 ATCC 6538p 6.25 6.25 62.5 12.5Sarcina lutea PCI ATCC 9341 12.5 12.5 250 62.5G (+) rodsBacillus megaterium 164 ATCC 8011 12.5 7.5 125 61.5Bacillus sp. E ATCC 27859 0.39 0.79 6.25 1.57Bacillus subtilis NRRL 558 12.5 25 250 62.5Bacillus sp. TA ATCC 27860 6.25 12.5 125 25G (+) filamentsMycobacterium phlei 78 ATCC 355 12.5 25 250 62.5Streptomyces cellulosae 097 ATCC 3313 25 25 500 125MoldsPaecilomyces varioti M16 ATCC 26820 250 500 * *Penicillum digitatum 0184 ATCC 26821 1000 1000 * *YeastCandida albicans 155 NRRL 477 250 100 * *Saccharomyces cerevisiae 90 NRRL 4226 1000 * * *__________________________________________________________________________ *Inactive at 1 mg/ml against molds and yeasts tested.
As indicated in Table 4, antibiotic X-14868A and its three minor components possess the property of adversely affecting the growth of certain gram-positive bacteria. They would therefore be useful in wash solutions for sanitary purposes as in the washing of hands and the cleaning of equipment, floors or furnishings of contaminated rooms or laboratories.
The following table sets forth the anticoccidostatic activity versus that of an infected untreated control (IUC) and an uninfected untreated control (UUC) following the test method set forth below.
TABLE 5______________________________________ Weight Mor- Average Degree of InfectionConc., gain, tality Intestinal Lesion ScoreGroup % % % Upper Mid Ceca Avg.______________________________________ UUC 100 0 0.0 0.0 0.0 0.0IUC 37 20 2.7 2.0 3.0 2.6X-14868A, 0.002 39 0 0.0 0.0 0.0 0.0sodium saltLot-1 0.001 81 0 0.2 0.0 0.0 0.07 0.0005 96 0 0.4 0.3 0.0 0.2X-14868A, 0.002 60 0 0.0 0.0 0.0 0.0sodium saltLot-1A______________________________________
Test Method
This test utilizes ten chickens per drug group. Ten chickens are employed as a weight control and ten chickens as an infected control. The drug is given 48 hours in advance of the infection. One gm of the test drug is mixed in a mechanical mixer with a sufficient amount of chicken feed to result in the desired dosage. The infection consists of approximately 300,000 oocysts given orally by pipette of Eimeria acervulina, E. mivati, E. maxima, E. necatrix and E. tenella. The test lasts for six days and then the surviving birds are autopsied and examined for gross lesions in the ceca. The test birds are rated according to the number of survivors and the number of intestinal lesions. The results are expressed as average degree of infection (A.D.I.). An average degree of infection of less than 2.5 is considered significant.
The coccidiostatic compositions of this invention containing as the active ingredient, antibiotic X-14868A or its pharmaceutically acceptable salts or the dried unfiltered broth are prepared by mixing the active ingredient with an inert ingredient. The inert ingredient can comprise a feedstuff, extender materials and the like. By the term "inert ingredient" is meant a material which does not function as an antiparasitic agent, e.g., a coccidiostat, is inactive with respect to the active ingredient and which may be safely ingested by the animals to be treated, and thus, such inert material is one which is inactive for the purpose of the present invention.
The active ingredient when orally administered to coccidiosis susceptible domestic animals, particularly fowl such as turkeys and chickens, as a component of feed, effectively controls the disease by either preventing it or curing it after it occurs. Furthermore, the treated fowl either maintain their weight or actually gain weight when compared to controls. Thus, the compositions of this invention not only control coccidiosis, but also aid in improving the efficiency of conversion of feed to weight gains.
The actual concentration of the active ingredient in animal feed can, of course, be adjusted to the individual needs and may vary over a wide range. The limiting criteria of the concentration are that the minimum concentration is such that a sufficient amount of active ingredient is provided to effect the desired control of coccidiosis and the maximum concentration is such that the amount of composition ingested does not result in any untoward or undesirable side effects.
Thus, for example, a feed premix or complete feed contains sufficient active ingredient to provide from about 0.0003% to about 0.001% by weight of the daily feed consumption. Preferably about 0.0005% to 0.001% by weight is used. Generally, about 0.0005% of the active ingredient is sufficient for the purpose of controlling and combating coccidiosis. Amounts greater than 0.001%, while being effective against coccidiosis, do not generally show improved results over 0.001% and in some cases may adversely affect the growth, feed efficiency and mortality.
Even though amount over 0.001% are efficacious for combatting coccidiosis, this amount is the preferred upper range because of economics, i.e., the cost per unit of effectiveness is lowest within this range. Amounts lower than 0.0003% are not effective for combating coccidiosis. Preferred is a lower limit of 0.0005% because this insures efficaciousness. The most preferred amount, i.e., about 0.0005% by weight of the poultry daily feed consumption is particularly efficacious since it achieves maximum effect with minimum dose.
The optimum dose level will, of course, vary with the size of the animal. When using the antibiotics in accordance with the invention for treating or preventing coccidiosis, it can be first compounded or blended with a feed ingredient or carrier to become a feed additive premix, a feed concentrate, or a feed additive supplement. A feed additive, concentrate or premix is an article intended to be diluted to produce a complete feed, i.e., an article intended to be administered as a sole ration. A feed additive supplement is an article intended for consumption by an animal directly or which can be further diluted to produce a complete feed or can be ingested and used as a supplement to other rations. Feed additive supplements, concentrates and premixes contain a relatively large percentage of coccidiostats, i.e., the active ingredient to a suitable carrier and mixing in a manner to give substantially uniform dispersion of the coccidiostat in the carrier. Suitable carriers are solids that are inert with respect to the active ingredient and which may safely be ingested by the animals to be treated. Typical of such carriers are commercial poultry feeds, ground cereal grains, grain by-products, plant protein concentrates (soy, peanuts, etc.) fermentation by-products, salts, limestone, inorganic compounds, and the like or admixtures thereof. Liquid dispersions can be prepared by using water or vegetable oil preferably including a surface active agent, emulsifying agent, and the like, in the liquid dispersion such as ethylenediaminetetraacetic acid, etc. and solubilizers. Any suitable carrier or extender material can function as the inert ingredient in the solid form of the antiparasitic agent provided that it is inert to the active material and is non-toxic insofar as the animal to which it is to be administered is concerned.
The active ingredient may be blended into a mash, pellet, or any desired configuration with the inert carrier or extender solid material by any convenient technique. For example, compositions can be formed by finely grinding or pulverizing the active ingredient and the inert ingredient using any commercially avaiable grinder or pulverizer with or without the feed material being present. If the feed material is not present when the grinding or pulverizing is effected, the resultant material can be distributed, in accordance with the present invention, in any conveniently available feed material. Typical poultry feeds, which can be medicated with the active ingredient of this invention can contain several ingredients, for example, they can contain high energy grain products such as corn, wheat, wheat red dog flour, milo, oatmeal, or the like; medium and low energy grain products, such as oats, barley, wheat flour, middlings, standard middlings or the like; stabilized fats; vegetable protein such as soybean meal, corn gluten meal, peanut meal, or the like; animal protein such as fish meal, fish solubles, meat scraps or the like; UGF (unidentified growth factor) sources and other B-vitamin carriers such as dried milk products, dried brewers yeast, distillers dried solubles, fermentation solubles, or the like; dehydrated alfalfa meal; and various special additives such as additional riboflavin, vitamin B 12 , calcium pantothenate, niacin, choline, vitamin K and vitamin E or the like, as well as stabilized vitamin A, vitamin D 3 (D-activated animal sterols); calcium and phosphorus supplements such as dicalcium phosphate, steamed bone meal, defluorinated phosphate, limestone, or the like; iodized salt, manganese sulfate, zinc carbonate, an antibiotic feed supplement; methionine or its hydroxy analog, and an antioxidant.
As is evident from the above, the coccidiostat compositions are intended for oral ingestion. They can be added to the normal feed supply of the treated animal or can be administered by other procedures, such as incorporating the same in a tablet, pill or bolus and supplying it forcibly to the animal. The administration of the active ingredient must be considered in terms of the specific animal under the husbandry practices encountered.
The minor components X-14868B, C and D also exhibit anticoccidiostatic activity when tested in vitro. X-14868B also has been shown to be active in vivo.
Antibiotic X-14868A has also been found to exhibit activity as a growth promotant in ruminants, i.e., animals with a rumen function, for example, cattle. A discussion of the mechanism whereby feed is digested, degraded and metabolized in a ruminant animal can be found in U.S. Pat. No. 3,839,557 issued Oct. 1, 1974 which discloses the use of certain antibiotics in improving ruminant feed utilization and is incorporated herewith by reference. Economically important ruminant animals include cattle, sheep and goats.
The effectiveness of antibiotic X-14868A in modifying the ratio of volatile fatty acids produced in the rumen (and thereby improve ruminant feed utilization) is demonstrated by means of the in vitro testing.
Rumen fluid is obtained from a steer with a fistulated rumen. The steer is maintained on the following ration:
Corn: 89.93%
Alfalfa meal: 5.000%
Soy bean oil meal: 3.00%
Limestone: 0.80%
NaCl: 0.60%
Dicalcium phosphate: 0.50%
Trace minerals: 0.025%
Vitamin premix additions: 0.1%
Vitamin A, TIU: 4.0003
Vitamin D 3 , IU: 0.801
Vitamin E, TIU: 3.002
The rumen fluid is immediately strained through a #30 mesh sieve. For each fermentation, 75 ml of the resulting fluid is added to a 250 ml flask containing the following:
1 g of 80%:20% finely ground grain: hay ration;
1 ml of an 18% aqueous glucose solution (1 millimole per flask);
1.5 ml of a 3.1% aqueous urea solution (0.76 millimole per flask);
60 micromoles of each of the 10 essential amino acids (arginine, histidine, leucine, methionine, threonine, valine, lysine, isoleucine, phenylalanine, tryptophan);
1 ml of an aqueous solution of test drug to give either 10 or 25 μg/ml (calculated total volume of fermentation mixture of 80 ml);
Each flask is incubated at 38° C. in a shaking water bath equipped with a gassing hood. Carbon dioxide is continuously passed through the hood. After four hours incubation, a 10 ml quantity of the fermentation fluid is centrifuged at 14,000 rpm (approximately 30,000 xg) for 20 minutes in an International Centrifuge equipped with a No. 874 angle head. Three ml of the supernate is added to 1 ml of a 25% metaphosphoric acid solution containing 23 micromoles 2-methyl valeric acid as an internal standard. The resulting fluid is permitted to sit at room temperature for 30 minutes. The fluid is filtered through a 0.22 millimicron Millipore filter and refrigerated until gas-liquid chromatographic analyses for volatile fatty acids.
Gas-liquid chromatographic (GLC) analyses of four in vitro control fermentations and two fermentations each with 10 and 25 ppm antibiotic X-14868A are set forth in the following table.
TABLE 6______________________________________Ratios of moles of propionate (C.sub.3) to acetate (C.sub.2)plus n-butyrate (nC.sub.4) in vitro rumen fermentations VFA Molar Ratio % PositiveCompound Concentration C.sub.3 /(C.sub.2 + nC.sub.4) Control______________________________________Negative Control 0 0.203 51.8X-14868A 5 ppm 0.323 82.5 50 ppm 0.358 91.2Positive Control 50 ppm 0.392 100.0(Monensin)______________________________________
As shown in Table 6 the ratio of propionate (C 3 ) to acetate and n-butyrate is significantly improved. With the increase of propionates rather than acetates from the carbohydrates, the efficiency of carbohydrate and therefor feed utilization is increased.
Administration of antibiotic X-14868A hereafter "Antibiotic" or "Antibiotic Compound" prevents and treats ketosis as well as improves feed utilization. The causative mechanism of ketosis is a deficient production of propionate compounds. A presently recommended treatment is administration of propionic acid or feeds which preferentially produce propionates. It is obvious that encouraging propionate production from ordinary feeds will reduce incidence of ketosis.
It has been found that antibiotic X-14868A increases the efficiency of feed utilization in ruminant animals when it is administered orally to the animals. The easiest way to administer the antibiotic is by mixing it in the animal's feed.
However, the antibiotic can be usefully administered in other ways. For example, it can be incorporated into tablets, drenches, boluses, or capsules, and dosed to the animals. Formulations of the antibiotic compound in such dosage forms can be accomplished by means of methods well-known in the veterinay pharmaceutical art.
Capsules are readily produced by filling gelatin capsules with any desired form of the desired antibiotics. If desired, the antibiotic can be diluted with an inert powdered diluent, such as a sugar, starch, or purified crystalline cellulose in order to increase its volume for convenience in filling capsules.
Tablets of the antibiotic are made by conventional pharmaceutical processes. Manufacture of tablets is a well-known and highly advanced art. In addition to the active ingredient, a tablet usually contains a base, a disintegrator, an absorbent, a binder, and a lubricant. Typical bases include lactose, fine icing sugar, sodium chloride, starch and mannitol. Starch is also a good disintegrator as is alginic acid. Surface-active agents such as sodium lauryl sulfate and dioctyl sodium sulphosuccinate are also sometimes used. Commonly-used absorbents again include starch and lactose while magnesium carbonate is also useful for oily substances. Frequently-used binders are gelatin, gums, starch, dextrin and various cellulose derivatives. Among the commonly used lubricants are magnesium stearate, talc, paraffin wax, various metallic soaps and polyethylene glycol.
The administration of the antibiotic compound may be as a slow-pay-out bolus. Such boluses are made as tablets except that a means to delay the dissolution of the antibiotic is provided. Boluses are made to release for lengthy periods. The slow dissolution is assisted by choosing a highly water-insoluble form of the antibiotic. A substance such as iron filing is added to raise the density of the bolus and keep it static on the bottom of the rumen.
Dissolution of the antibiotic is delayed by use of a matrix of insoluble materials in which the drug is inbedded. For example, substances such as vegetable waxes, purified mineral waxes, and water-insoluble polymeric materials are useful.
Drenches of the antibiotic are prepared most easily by choosing a water-soluble form of the antibiotic. If an insoluble form is desired for some reason, a suspension may be made. Alternatively, a drench may be formulated as a solution in a physiologically acceptable solvent such as a polyethylene glycol.
Suspensions of insoluble forms of the antibiotic can be prepared in nonsolvents such as vegetable oils such as peanut, corn, or sesame oil, in a glycol such as propylene glycol or a polyethylene glycol; or in water, depending on the form of the antibiotic chosen.
Suitable physiologically acceptable adjuvants are necessary in order to keep the antibiotic suspended. The adjuvants can be chosen from among the thickeners, such as carboxymethylcellulose, polyvinylpyrrolidone, gelatin, and the alginates. Many classes of surfactants serve to suspend the antibiotic. For example, lecithin, alkylphenol polyethylene oxide adducts, naphthalenesulfonates, alkylbenzesulfonates, and the polyoxyethylene sorbitan esters are useful for making suspensions in liquid nonsolvents.
In addition many substances which effect the hydrophilicity, density, and surface tension of the liquid can assist in making suspensions in individual cases. For example, silicone anti-foams, glycols, sorbitol, and sugars can be useful suspending agents.
The suspendable antibiotic may be offered to the grower as a suspension, or as a dry mixture of the antibiotic and adjuvants to be diluted before use.
The antibiotic may also be administered in the drinking water of the ruminants. Incorporation into drinking water is performed by adding a water-soluble or water-suspendable form of the antibiotic to the water in the proper amount. Formulation of the antibiotic for addition to drinking water follows the same principles as formulation of drenches.
The most practical way to treat animals with the antibiotic compound is by the formulation of the compound into the feed supply. Any type of feed may be medicated with the antibiotic compounds, including common dry feeds, liquid feeds and pelleted feeds.
The methods of formulating drugs into animal feeds are well-known. It is usual to make a concentrated drug premix as a raw material for medicated feeds. For example, typical drug premixes may contain from about one to about 400 grams of drug per pound of premix. The wide range results from the wide range of concentration of drug which may be desired in the final feed. Premixes may be either liquid or solid.
The formulation of ruminant feeds containing the proper amounts of antibiotic for useful treatment is well understood. It is necessary only to calculate the amount of compound which it is desired to administer to each animal, to take into account the amount of feed per day which the animal eats and the concentration of antibiotic compound in the premix to be used, and calculate the proper concentration of antibiotic compound, or of premix, in the feed.
All of the methods of formulating, mixing and pelleting feeds which are normally used in the ruminant feed art are entirely appropriate for manufacturing feeds containing the antibiotic compound.
As has been shown, oral administration of the antibiotic beneficially alters the production of propionates relative to the production of acetates in the rumen. It may therefore be postulated that the same treatment would also benefit monogastric animals which ferment fibrous vegetable matter in the cecum since it would be expected that a beneficial change in the propionate/acetate ration would occur upon oral administration of the instant antibiotic. Horses, swine and rabbits are exemplary animals which digest a part of their food by cecal fermentation.
Antibiotic X-14868A also has demonstrated activity as an agent in the treatment or prevention of swine dysentery. The compound was examined for activity against Treponema hyodysenteriae, the etiologic agent of swine dysentery. The results which represent a comparative test following well-known test methods versus a known agent in the treatment and prevention of swine dysentery are set forth in the table below.
TABLE 7______________________________________ Minimum Inhibitory Concentration (mcg/ml)T. hyodysenterial Strain X-14868A Ipronidazole______________________________________H-78 0.05 0.63H 140 0.05 0.63B 169 0.05 0.63SQ 2 0.05 2.5Mean 0.05 1.1______________________________________
Also forming part of the present invention are the novel minor components denominated as X-14868B, C and D. These components exhibit in vitro anticoccidial activity against an E. tenella as set forth below.
______________________________________In vitro activity versus E. tenellaCompound PPM effective against E. tenella______________________________________X-14868B 0.1X-14868C 10.0X-14868D 10.0______________________________________
The structural formula of compound X-14868B is as follows: ##STR3##
The infrared absorption spectra for the respective compounds are as follows:
______________________________________ X-14868A FIG. 1 X-14868B FIG. 2 X-14868C FIG. 3 X-14868D FIG. 4______________________________________
Table 8 sets forth physical constants for the various components produced by fermentation of the Nocardia X-14868.
TABLE 8__________________________________________________________________________Physical constants of X-14868 components [α]D, Specific rotation *Microanalysis foundComponent Number M.P. °C. chloroform methanol % C % H % Na % OMe__________________________________________________________________________X-14868A 193-195 +40.6° +23.8° 60.11 8.54 2.38 12.10X-14868B 172.5-174 +46.1° +34.8° 60.97 8.60 1.23 14.87X-14868C 172-175 +49.6° +30.5° 57.13 8.58 2.36 10.25X-14868D 194-195 +41.1° +29.2° 60.32 8.80 3.40__________________________________________________________________________*Calculated Microanalysisfor compounds A and B M.W. % C % H % Na % OMe__________________________________________________________________________X-14868A: C.sub.47 H.sub.79 O.sub.17 Na 939.25 60.10 8.50 2.45 13.22X-14868B: C.sub.96 H.sub.163 O.sub.34 Na.H.sub.2 O 1902.36 60.61 8.75 1.21 16.54__________________________________________________________________________
The following examples will serve to illustrate this invention without limitating it thereto.
EXAMPLE 1
Shake Flask Fermentation of Nocardia X-14868
The antibiotic X-14868A producing culture is grown and maintained on a starch-casein agar slant having the following composition (grams/liter distilled water):
______________________________________Soluble starch 10.0Casein 1.0K.sub.2 HPO.sub.4 0.5MgSO.sub.4 (anhydrous) 0.5Agar 20.0Adjust pH to 7.4 with NaOH before autoclaving at 15 poundpressure for 20 minutes.______________________________________
The slant is inoculated with Nocardia X-14868 culture and incubated at 28° C. for 7-14 days. A chunk of agar containing mycelia from the well-grown agar slant is then used to inoculate a 500-ml Erlenmeyer flask containing 100 ml sterilized inoculum medium having the following composition (grams/liter distilled water):
______________________________________Tomato pomace 5.0Distillers soluble 5.0OM peptone 5.0Debittered dried yeast 5.0Cornstarch 20.0CaCO.sub.3 1.0K.sub.2 HPO.sub.4 1.0Adjust pH to 7.0 with NaOH before sterilization.______________________________________
The inoculated inoculum medium is incubated at 28° C. for 72 hours on a rotary shaker, operating at 250 rpm with a 2-inch stroke.
A 3 ml portion (3%, v/v) of the resulting culture is then used to inoculate a 500-ml Erlenmeyer flask containing 100 ml sterilized production medium having the following composition (grams/liter distilled water):
______________________________________Glycerol 40.0OM peptone 5.0Cerelose 2.0Potato starch 2.0Defatted soy grit (Archer Daniels Midland Co.) 5.0Debittered dried yeast 5.0NaCl 5.0CaCO.sub.3 0.2Adjust pH to 6.4 before autoclaving.______________________________________
The inoculated medium is incubated at 28° C. for 5 days on a rotary shaker running at 250 rpm with a 2-inch stroke. The potency of the antibiotic X-14868A in the fermentation broth is estimated by assaying against Staphylococcus aureus ATCC 6538P using agar diffusion cup-plate assay.
EXAMPLE 2
Isolation of Antibiotic X-14868A-Na Salt and Antibiotic X-14868B-Na Salt from Shake Flask Fermentation
Step A:
The whole broth from 50 half-liter Erlenmeyer flasks each containing 100 ml, after 5 days of fermentation were pooled (5 liters) and extracted twice with one-half volume of ethyl acetate. After stirring for one-half hour solvent layer was separated and concentrated to an oil (4 g) under reduced pressure. The oil was dissolved in diethyl ether and was chromatographed on a diethyl ether slurry packed 200 g silica gel (Davison grade 62) column. The column was eluted with a gradient between 2 liters of diethyl ether to 2 liters diethyl ether/acetone (9:1) and then 2 liters of diethyl ether/acetone (1:1) and then 2 liters of methylene chloride/ethyl alcohol (7:3). Fractions of 40 ml each were collected and from fraction numbers 18-75 were pooled, solvent was removed under reduced pressure and the (1.66 g) residue thus obtained was dissolved in ethyl acetate and was washed with equal volume of 1 N HCl two times, followed by washing with equal volume of Na 2 CO 3 (saturated at room temperature) two times. The solvent phase was dried over Na 2 SO 4 , and by addition of n-hexane antibiotic X-14868A-Na salt crystals were obtained. Recrystallization from ethyl acetate/n-hexane yielded the analytical sample of antibiotic X-14868A-Na salt. M.P. 193°-194° C.
Step B:
From fraction numbers 161-215 subsequent to the solvent being removed under reduced pressure, and the residue being dissolved in ethyl acetate and washed with 1 N HCl, followed by Na 2 CO 3 (saturated at room temperature) washing and drying over Na 2 SO 4 , after addition of n-hexane antibiotic X-14868B-Na salt crystals were obtained. M.P. 172.5°-174° C.
EXAMPLE 3
Tank Fermentation of Nocardia X-14868
The antibiotic X-14868A producing culture Nocardia X-14868 is grown and maintained on a starch-casein agar slant having the following composition (grams/liter distilled water):
______________________________________Soluble starch 10.0Casein 1.0K.sub.2 HPO.sub.4 0.5MgSO.sub.4 (anhydrous) 0.5Agar 20.0Adjust pH to 7.4 with NaOH before autoclaving.______________________________________
The slant is inoculated with Nocardia X-14868 culture and incubated at 28° C. for 7-14 days. A chunk of agar containing mycelia from the well-grown agar slant is then used to prepare vegetative inoculum by inoculating a 500-ml Erlenmeyer flask containing 100 ml of inoculum medium with the following composition (grams/liter distilled water):
______________________________________Tomato pomace 5.0Distillers soluble 5.0OM peptone 5.0Debittered dried yeast 5.0Cornstarch 20.0CaCO.sub.3 1.0K.sub.2 HPO.sub.4 1.0pH is adjusted to 7.0 before autoclaving.______________________________________
The inoculated medium is incubated for 72 hours at 28° C. on a rotary shaker operating at 250 rpm with a 2-inch stroke.
Sixty ml (3%v v/v) of this culture broth are used to inoculate a 6-liter Erlenmeyer flask containing 2-liters of inoculum medium having the following composition (grams/liter distilled water):
______________________________________Tomato pomace 5.0Distillers soluble 5.0OM peptone 5.0Debittered dried yeast 5.0Cornstarch 20.0CaCO.sub.3 1.0K.sub.2 HPO.sub.4 1.0pH is adjusted to 7.0 before autoclaving.______________________________________
The inoculated medium is incubated for 72 hours at 28° C. on a rotary shaker operating at 250 rpm.
Four liters of this culture are used to inoculate 60 gallons of the following production medium in a 100-gallon fermentor (grams/liter tap water):
______________________________________Glycerol 40.0OM peptone 5.0Cerelose 2.0Potato starch 2.0Defatted soy grit (Toasted Nutrisoy grit, 40-80) 5.0Debittered dried yeast 5.0NaCl 5.0CaCO.sub.3 0.2Sag 4130 antifoam (Union Carbide) 0.1The pH of the medium is adjusted to 6.4 before sterilizationfor 11/4 hours with 60 lb/in.sup.2 steam.______________________________________
The inoculated medium is aerated with compressed air at a rate of 3 cubic feet per minute, and is stirred with agitators at 280 rpm. The fermentation is carried out at 28° C. for 5 days.
The potency of antibiotic X-14868A in the fermentation broth is estimated by assaying against Staphylococcus aureus ATCC 6538P using agar diffusion cup-plate assay.
EXAMPLE 4
Isolation of Antibiotic X-14868-A-; -C; and -D Sodium Salts from Tank Fermentation of Nocardia X-14868
Step A:
To the whole broth from a sixty gallon (227.1 liters) fermentation as set forth in Example 3 was added, after 115 hours growth, an equal volume of ethyl acetate. After stirring for one hour the solvent layer was separated and concentrated to 4.2 liters under reduced pressure. The concentrated solvent extract was washed with equal volume of 1 N HCl two times, followed by washing two times with equal volume of Na 2 CO 3 (saturated at room temperature). The solvent phase was dried over Na 2 SO 4 and concentrated to an oil under reduced pressure. The oil was dissolved in n-hexane and was extracted once with acetonitrile followed by two extractions with acetonitrile/methanol (8:2). The acetonitrile and acetonitrile/methanol (8:2) extracts were pooled, and the solvent was removed under reduced pressure. The resulting oil was dissolved in diethyl ether, treated with charcoal (MCB, activated "Norit A"), filtered and by addition of n-hexane crude antibiotic X-14868A-Na salt crystals were obtained. The crude antibiotic crystals were dissolved in methylene chloride and were subjected to chromatography on a methylene chloride slurry packed 600 g silica gel (Davison grade 62) column. The column was eluted with 4 liters of diethyl ether/acetone/ammonium hydroxide (8/2/0.02). Fractions of 45 ml each were collected and from fraction numbers 13-15 were pooled. The solvent was removed under reduced pressure, the residue was dissolved in ethyl acetate and consecutively washed twice with 1 N HCl and twice with Na 2 CO 3 (saturated at room temperature) dried over Na 2 SO 4 . The ethyl acetate phase was concentrated to an oil and was dissolved in methylene chloride and by addition of n-hexane crystalline antibiotic X-14868A-Na salt was obtained. M.P. 193°-195° C.
Step B:
The mother liquor of the crude antibiotic X-14868A-Na salt crystals (described in above Step A) was chromatographed on a methylene chloride slurry packed 1 kg silica gel (Davison grade 62) column. The column was eluted with 1 liter of n-hexane and then a gradient between 4 liters of diethyl ether/n-hexane (7:3) to 4 liters of diethyl ether/acetone (8:2). Fractions of 40 ml each were collected and fraction numbers 43-80 were pooled. The solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate and washed with 1 N HCl, followed by the aqueous Na 2 CO 3 (saturated at room temperature) wash and charcoal treatment (MCB activated "Norit A"). After filtration, the ethyl acetate phase was concentrated to an oil. The oil was dissolved in diethyl ether and the addition of n-hexane yielded additional antibiotic X-14868A-Na salt. M.P. 193°-195° C.
Step C:
Fraction numbers 22-40 from the silica gel column described above in Step A yielded crystalline antibiotic X-14868C-Na salt. M.P. 172°-175° C.
Step D:
The mother liquor of the crystalline X-14868A-Na salt described in Step B and fractions 16-21 from the silica gel column, described in Step A were pooled, concentrated and subjected to chromatography on a methylene chloride slurry packed 600 g silica gel column. The column was eluted with 4 liters of diethyl ether/hexane (1:1); 4 liters of diethyl ether/acetone/n-hexane/ammonium hydroxide (6:2:2:0.002); 2 liters of diethyl ether/acetone (8:2). Fractions of 40 ml each were collected. Fraction numbers 71-98 were pooled and crystallization yielded additional crystalline X-14868A-Na salt. Fraction numbers 141-172 were also pooled, solvent was removed under reduced pressure and crystallization from diethyl ether/n-hexane yielded antibiotic X-14868D-Na salt. M.P. 194°-195° C.
EXAMPLE 5
Preparation of the thallium salt of antibiotic X-14868A
A solution of 51 mg of antibiotic X-14868A-Na salt in methylene chloride was washed with 1 N HCl, followed by water wash and then four times with an aqueous solution of thallium carbonate. The solvent was separated and concentrated to a small volume under reduced pressure and after the addition of n-hexane crystalline thallium salt of antibiotic X-14868A was recovered. Recrystallization from diethyl ether/n-hexane yielded crystals suitable for X-ray analysis.
EXAMPLE 6
Preparation of the calcium salt of antibiotic X-14868A
A solution of 200 mg of antibiotic X-14868A-Na salt in ethyl acetate was first washed with 1 N HCl, then three times with an aqueous solution of calcium hydroxide (saturated at room temperature). The solvent was separated and removed under reduced pressure. The calcium salt of antibiotic X-14868A was recovered as a white solid foam.
EXAMPLE 7
Shake Flask Fermentation of X-14868
The antibiotic X-14868A producing culture was grown and maintained on a starch casein agar slant having the following composition (grams/liter distilled water):
______________________________________Soluble starch 10.0Casein 1.0K.sub.2 HPO.sub.4 0.5MgSO.sub.4 (anhydrous) 0.5Agar 20.0Adjust pH to 7.4 with NaOH before autoclaving at 15 poundpressure for 20 minutes.______________________________________
The slant was inoculated with Nocardia X-14868 culture and incubated at 28° C. for 7-14 days. A chunk of agar containing mycelia from the well-grown agar slant was then used to inoculate a 500-ml Erlenmeyer flask containing 100 ml sterilized inoculum medium having the following composition (grams/liter distilled water):
______________________________________Tomato pomace 5.0Distillers soluble 5.0OM peptone 5.0Debittered dried yeast 5.0Cornstarch 20.0CaCO.sub.3 1.0K.sub.2 HPO.sub.4 1.0Adjust pH to 7.0 with NaOH before sterilization.______________________________________
The inoculated inoculum medium was incubated at 28° C. for 72 hours on a rotary shaker, operating at 250 rpm with a 2-inch stroke.
A 3 ml portion (3%, v/v) of the resulting culture is then used to inoculate a 500-ml Erlenmeyer flask containing 100 ml sterilized production medium having the following composition (grams/liter distilled water):
______________________________________Cerelose (C.P.C. International Co.) 45.0Eclipse N Starch (A. E. Staley Co.) 20.0Soyalose 105 (Central Soya Co.) 15.0Casein hydrolysate (acid) (General Biochemicals) 1.0Black strap molasses 3.0CaCO.sub.3 2.5Tap water to 1 literpH 7.1______________________________________
The inoculated medium is incubated at 28° C. for 7 days on a rotary shaker running at 250 rpm with a 2-inch stroke. The potency of antibiotic X-14868A in the fermentation broth was estimated by assaying against Staphylococcus aureus ATCC 6538P using agar difussion cup-plate assay.
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Antibiotic X-14868A having the following chemical structure ##STR1## and the pharmaceutically acceptable salts thereof is presented. Also presented is a fermentative method of producing the above antibiotic.
Antibiotic X-14868A exhibits anticoccidiostatic activity.
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FIELD OF THE INVENTION
[0001] The present invention relates to methods and apparatus for detecting and preventing undesirable scale deposition, and more particularly relates, in one embodiment, to methods and apparatus for detecting and preventing undesirable scale deposition that employ electrodes which intentionally cause scale deposition as a diagnostic indicator.
BACKGROUND OF THE INVENTION
[0002] The accumulation of inorganic mineral scales in oil field formation and production equipment is a major problem for the oil industry. Deposition of inorganic mineral scale in oil-bearing formations and on production tubing and equipment causes significant and costly loss of production. Other industries have similar problems with scale deposition. The primary offenders are carbonates and sulfates of calcium, barium and strontium. These compounds may precipitate as a result of changes in pressure, temperature and ionic strength of produced fluids or when connate reservoir waters mix with injected waters during secondary recovery operations. In order to avoid costly losses in production or post-scale treatments, it is necessary to prevent deposition of scale downhole as well as in post production processing. Scale is a particular problem when equipment is in contact with certain brines.
[0003] Current scale probes indicate the onset of scale deposition. However, in order to take preventive action, an advance sensor is required which detects the onset of scaling conditions before actual scale deposition occurs on the surfaces to be protected. The advantage of such a sensor would be that time for preventive measures is gained and the need for remedial work is avoided. It would be advantageous if a scale prediction probe could be devised which would be able to determine conditions just prior to when undesirable scaling would occur.
SUMMARY OF THE INVENTION
[0004] Accordingly, it is an object of the present invention to provide a method and apparatus for preventing scale from forming on surfaces, particularly oil field production equipment.
[0005] It is another object of the present invention to provide a scale prediction probe which would be able to determine conditions just prior to those under which undesirable scaling would occur.
[0006] In carrying out these and other objects of the invention, there is provided, in one form, a method for predicting scale deposition in a general environment which involves providing a localized environment where scale is preferentially formed first (relative to the general environment), where the localized environment is adjacent the general environment, and monitoring the deposition of scale in the localized environment. Preemptive action may thus be taken to prevent scale deposition in the general environment in response to the results obtained from monitoring the deposition of scale. Finally, the intentionally formed scale is removed from the localized environment so the method can be practiced again.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] [0007]FIG. 1 is a schematic diagram of an electrode configuration for a calcium carbonate scale sensor in accordance with the apparatus and method of this invention, where FIG. 1A schematically shows a scale free electrode at time t=0, and where FIG. 1B schematically shows a scaled cathode at a later time t=t;
[0008] [0008]FIG. 2 is a graph of voltage potential v. current density in a current/voltage relationship at the scale sensing electrode of this invention under various conditions; and
[0009] [0009]FIG. 3 is a schematic diagram of an electrode configuration for a barium sulfate or strontium sulfate scale sensor in accordance with the apparatus and method of this invention.
DETAILED DESCRIPTION OF THE INVENTION
[0010] The scale prediction probe of the present invention provides a surface that will preferentially scale over before any other surface in the general area. Stated another way, scale-forming conditions are intentionally caused to be formed in a localized environment adjacent a general environment so that scale forms on that localized environment or surface before any other surface in the general environment has scale deposited thereon. Further, the degree of “over scaling potential” may be controlled and remotely adjusted to suit individual conditions.
[0011] It may thus be understood that the inventive scale prediction probe may be used to predict, and thus prevent, the deposition of undesirable scale in the general environment. It should be recognized that this concept of prediction is different from that used by some researchers where “predict” is used to mean being able to accurately measure the amount of scale formed on a surface.
[0012] Two probe embodiments form the basis of the invention. The first embodiment uses an inert electrode with a controlled surface pH, and the second embodiment is a dual surface probe where one area generates a controlled release of sulfate ions, for example, and the second surface acts as the scale collector. The first embodiment is for the prediction of calcium carbonate scale deposition and the like, in one non-limiting case, while the second embodiment is for barium and strontium sulfate scale deposition prevention, in other non-limiting cases.
[0013] During cathodic protection in sea water and other saline solutions (brines) the cathodic surface becomes coated with scale in preference to nearby non-cathodic surfaces. This scale deposition is induced due to the electrical generation of alkaline conditions at the electrode surface. This high surface pH can be caused as described below. The effect of the localized increased pH is to drive the scaling reaction such as that depicted below:
Ca 2+ +2HCO 3 − ←→CaCO 3 ↓+CO 2 +H 2 O
[0014] The increase in alkalinity of the electrode surface is generated by an applied electric current. This current may be controlled either galvanostatically, potentiostatically, or may have some time-dependent voltage/current control. The electrode may be of the same or different material as the system, but should not generate scaling species. Carbon steel may be appropriate in some conditions due to the cathodic polarization induced by the recording and stimulating equipment. Preferably, the electrode is an inert electrode material such as platinum-plated or platinum-coated titanium. However, the invention is not limited to any particular metal for the electrodes.
[0015] [0015]FIG. 1 provides a schematic diagram of the principal parts of the invention; however, it would be appreciated that the actual configuration used in practice would depend on the individual system in which the sensor would be installed. The electrode configuration or apparatus for the calcium carbonate scale inhibitor of FIG. 1 is generally referred to as 10 , where the reference electrode 12 may be positioned adjacent the cathode 14 which is opposite and adjacent (in another, facing direction) the auxiliary electrode 16 having fluid flow in the direction indicated. Note the cathode 14 and anode 16 are downstream from the reference electrode 12 . The reference electrode 12 is used to measure the electrical potential of the cathodic or working electrode 14 . Measurements taken by reference electrode 12 are used by the instrumentation to control the potential/current applied by the auxiliary electrode 16 on the cathodic (working) electrode 14 . Reference electrode 12 also provides a fixed point of reference for comparison of electrochemical potentials in other systems (where a recognized standard reference electrode is utilized).
[0016] [0016]FIG. 1A shows the apparatus 10 at some initial time, t=0, where cathode 14 is scale-free. FIG. 1B shows the apparatus 10 at some later time, t=t, where the cathode 14 has scale 18 deposited thereon. It will be appreciated that the early detection of carbonate scales other than calcium carbonate could be achieved by the method and apparatus of this embodiment. It will also be appreciated that cathode 14 and anode 16 make up the localized environment in one embodiment of the invention. Generating the applied electric current across cathode 14 and anode 16 conditions the cathode 14 to be slightly more scaling than the bulk fluid.
[0017] The measurement of intentional scale build-up on the electrode depends upon the detection of the diffusion limited current due to the reduction of a suitable species in the electrolyte. For example, in sea water, oxygen is reduced to hydroxyl ion, and diffusion of the gas to the electrode surface is increasingly limited by the build-up of scale. This results in a diffusion-limiting current at the electrode surface. FIG. 2 shows the effect of scale build-up on the current voltage relationship at the electrode surface. The values of the diffusion limiting currents (I lim 1 , I lim 2 , and I lim 3 ) are given at three different times or scale levels, with scale increasing on the cathode in the direction right to left in FIG. 2. That is, I lim decreases with time as scale is formed on the electrode. FIG. 2 is an example of how the curve would move with time.
[0018] The diffusion limited current may be detected by electrochemical methods other than the full potential sweep shown in FIG. 2, such as electrochemical impedence measurements and current potential logging, as non-limiting examples among others. In essence, impedence measures the response of the working electrode to a varying applied potential frequency in terms of electrical impedence. Current potential logging measures the current passing between two electrodes and the potential of the electrodes. This data is then statistically analyzed.
[0019] The surface pH is dependent upon the cathodic current density and the rate of diffusion of alkaline species away from the electrode and the rate of diffusion of acidic species toward the electrode. If the temperature, surface geometry, current density and flow characteristics of the brine or other fluid are known, then by using Fick's laws of diffusion and basic chemical/electrochemical equations, the surface pH may be calculated. Control of the surface pH is less accurate using calculated values from diffusion laws (e.g. Fick's law) due to variability of hydrodynamics, etc., and would only be used as a “sighting shot” or to determine approximate settings for obtaining empirical data. Alternatively, control values may be obtained from experimental data and used for other conditions by interpolation or extrapolation.
[0020] If the auxiliary and working (cathode or sensing) electrode are identical, then they may be interchanged, or the auxiliary may be used as a blank scale reference/normal scaling potential reference. An additional benefit of this technique is that electrode cleaning of a scaled surface is possible by applying a high current density to the electrode that has the effect of generating gas bubbles that disrupt and remove the scale from the electrode surface. Thus, the electrode surface can be used for accurate monitoring again.
[0021] As the presence of scale is detected through reduction in current density as shown, the scale prediction probe can give a signal for the release of a certain, predetermined amount or rate of scale inhibiting chemical or agent into the fluid of the system. This step may be initiated when the current density falls below a certain preset threshold. Such a preset threshold would be individual for each system and could not be specified in general or in advance. By injecting scale inhibiting agents or chemicals only when needed, conservation of the agent and costs associated therewith can be achieved. Scale inhibiting chemicals and agents are well known in the art. Additionally, the use of injection mechanisms such as nozzles, pipes, needles, and the like are also well known in the art. Similarly, the removal of scale by applying a high current density to the electrode as described above could also be triggered or caused once the current density falls below a certain preset threshold.
[0022] In the embodiment for barium and strontium sulfate scale deposition, one change to the above embodiment is there is present an additional surface suitable to generate a controlled release of sulfate ions.
[0023] The formation of sulfate-containing scales is not strongly affected by pH, and thus the above embodiment cannot create an increased scaling tendency for these scale types. However, by the introduction of a local excess of sulfate ion (barium or strontium, for example, where appropriate), over the bulk concentration of these ions, then the local scaling tendency will be increased. This latter technique is the basis of the sulfate scaling tendency embodiment of the invention.
[0024] Shown in FIG. 3 is a schematic diagram of an electrode configuration for a barium sulfate or strontium sulfate scale sensor. The electrode configuration is generally denoted as 20 . The detecting or scaling electrode 22 (corresponding to the cathode 14 in the carbonate scale detection embodiment) is immediately down stream of a sulfate generating electrode 24 , the sole purpose of which is to generate a controlled excess of scaling ion (sulfate, barium, strontium, etc.). This excess ion then drifts over the sensing electrode 22 (i.e. the working electrode, as in the previously described embodiment) and causes deposition when the bulk fluids are close to saturation with respect to the scale being deposited on the sensing/detecting electrode 22 .
[0025] The comparator electrode 26 shown in FIG. 2 is similar to the sensing electrode 22 down stream of the generating electrodes and serve the purpose of determining if the actual system is in a scaling condition without the presence of the excess ions supplied by electrode 24 . Counter electrodes 30 serve the function of auxiliary electrodes 16 in the FIG. 1 embodiment.
[0026] The generation of sulfate, barium or strontium scaling ions for producing an excess scaling tendency is necessary for the second embodiment, for without it, the electrode sensor 22 will only detect scale at the same time the entire system experiences the onset of scaling.
[0027] In the foregoing specification, the invention has been described with reference to specific embodiments thereof. However, it will be evident that various modifications and changes can be made thereto without departing from the broader spirit or scope of the invention as set forth in the appended claims. Accordingly, the specification is to be regarded in an illustrative rather than a restrictive sense. For example, scales other than those specifically mentioned, and electrode configurations other than those specifically shown and described, falling within the claimed parameters, but not specifically identified or tried in a particular application to inhibit scale formation, are within the scope of this invention.
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A method for predicting scale deposition in a general environment has been discovered which involves providing a localized environment where scale would preferentially form, where the localized environment is adjacent the general environment. Monitoring the deposition of scale in the localized environment is performed for the purpose of taking preemptive action to prevent scale deposition in the general environment once scale begins to form, or a certain threshold is reached. Scale is removed from the localized environment so that monitoring can be performed by the probe again. Preemptive action will often be the introduction of a scale inhibiting agent into the general environment. An apparatus for practicing the method of predicting and preventing scale deposition in a general environment is also described.
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BACKGROUND OF THE INVENTION AND RELATED ART STATEMENT
The present invention relates to an SO 2 gas sensor for measuring the sulfur dioxide (SO 2 ) gas concentration in the exhaust gas of a combustion engine, or the like, or in the air. Particularly, the present invention relates to a SO 2 gas sensor which can reduce the influence of coexistent oxygen (O 2 ) on a value obtained by a SO 2 gas measurement and which can operate even at such a high temperatures as 600° C. 900° C.
In boilers for thermal power generation or incineration facilities, there are emission standards on toxic gases that occur in the exhaust gas, such as NO x and SO 2 , which exist for environment protection. Each facility is required to monitor the concentration of these toxic gases in order to prove that the standards are being followed. In thermoelectric power plants or incineration facilities, there is used a measuring apparatus of a nondispersive infrared ray absorption type (NDIR type) to monitor these air-pollutive gases. Since the measuring apparatus is not directly inserted into the exhaust gas, the exhaust gas is sampled by an absorption pump and analyzed in a place separate from the passage for the exhaust gas.
However, in the NDIR type of measuring apparatus, a sampling apparatus is exposed to high temperatures. Therefore, it requires rather frequent maintenance checks, which because of various restrictions are difficult to carry out without stopping the operation of the boiler or the incineration facilities.
Further, the apparatus itself must have gas-pretreatment portions for removing dust and water contained in an exhaust gas, which in combination with the use of an absorption pump, inevitably enlarges the apparatus and raises its price.
Furthermore, because a measurement of the concentration of toxic gases such as SO 2 in an exhaust gas requires the absorption step by the use of an absorption pump, even when such a concentration in an exhaust gas reaches nearly a critical level by, for example, an unexpected extraordinariness of combustion facilities; it is difficult to avoid delay in a response time, and a certain time lag is necessary to cope with the extraordinariness, or the like, which increases the risk of an unexpected accident.
Additionally, since the sensor used in the apparatus sustains interference of CO 2 , hydrocarbons inevitably discharged into an exhaust gas, or the like, a precise measurement cannot be expected.
The other methods for measurement shown in JIS B7981 are (1) an electrolytic conductivity method, (2) an ultraviolet ray absorption method, and (3) controlled potential electrolysis. However, these methods have problems regarding sampling due to the aforementioned nondispersive infrared ray absorption, and each of these methods is influenced by peculiar interferential gases.
SUMMARY OF THE INVENTION
The present invention was made in view of the aforementioned problems and provides a SO 2 gas sensor for appropriately measuring a concentration of SO 2 gas contained in an exhaust gas from thermoelectric power plants or incineration facilities and further provides a SO 2 gas concentration measuring apparatus using the SO 2 gas sensor.
According to the present invention, there is provided a sulfur dioxide gas sensor comprising:
a solid electrolyte having oxygen ion conductivity;
a detecting electrode for measuring sulfur dioxide gas, electrically connected to at least a part of a surface of the solid electrolyte; and
a basic electrode for measuring sulfur dioxide gas, electrically connected to at least a part of a surface of said solid electrolyte;
wherein the detecting electrode contains glass and either gold or a gold alloy.
According to the present invention, there is further provided a sulfur dioxide gas sensor comprising:
a solid electrolyte having oxygen ion conductivity;
a detecting electrode for measuring sulfur dioxide gas, electrically connected to at least a part of a surface of the solid electrolyte;
a basic electrode for measuring sulfur dioxide gas, electrically connected to at least a part of a surface of the solid electrolyte; and
a detecting electrode for measuring oxygen and/or a basic electrode for measuring oxygen;
wherein the detecting electrode for measuring sulfur dioxide gas contains glass and either gold or a gold alloy.
According to the present invention, there is also provided an apparatus for measuring said SO 2 gas equipped with said sensor.
According to the present invention, there is furthermore provided a sulfur dioxide gas sensor comprising:
a solid electrolyte having oxygen ion conductivity;
a detecting electrode for measuring sulfur dioxide gas, electrically connected to at least a part of a surface of the solid electrolyte;
a basic electrode for measuring sulfur dioxide gas, electrically connected to at least a part of a surface of the solid electrolyte;
a detecting electrode for measuring oxygen and/or a basic electrode for measuring oxygen; and
an oxygen pump cell for controlling oxygen content in the atmosphere to be measured;
wherein the detecting electrode for measuring sulfur dioxide gas contains glass and either gold or a gold alloy.
It is preferable that the electrode used for the oxygen pump cell in said SO 2 gas sensor is made of a metal oxide, which does not oxidize SO 2 gas.
Preferably, the SO 2 gas sensor has a gas diffusion rate-determining layer on a surface of the detecting electrode. The sensor may have a structure in which both the detecting electrode for measuring SO 2 gas and the basic electrode for measuring SO 2 gas are disposed on the same surface of the solid electrolyte. Further, the sensor may have a three-electrode structure in which a reference electrode for measuring SO 2 gas is employed next to the detecting electrode for measuring SO 2 gas and the basic electrode for measuring SO 2 gas.
A SO 2 gas sensor of the present invention employs a method of measuring a change of electromotive force caused by adsorption/oxidation of sulfur dioxide gas in the detecting electrode for measuring SO 2 gas when a certain current is applied between the detecting electrode and the basic electrode for measuring SO 2 . This enables improvement of SO 2 detection sensitivity.
Alternatively, an SO 2 gas sensor of the present invention may employ a method in which a SO 2 gas concentration is measured by measuring the change of amperage caused by an oxidation reaction of SO 2 gas on the detecting electrode for measuring SO 2 gas when the voltage is kept constant between the detecting electrode for measuring sulfur dioxide and the basic electrode for measuring sulfur dioxide. This also enables improvement of SO 2 detection sensitivity and assists in conduction of excellent measurement of concentration.
A SO 2 gas sensor of the present invention having electrodes for measuring oxygen, which are separate from the electrodes for measuring SO 2 , employs a method in which a SO 2 gas concentration and an oxygen concentration are measured simultaneously, and the SO 2 gas concentration is amended according to the results of the measurement of the oxygen concentration.
In the SO 2 gas sensor of the present invention having a reference electrode for measuring oxygen, which are seperate from the electrodes for measuring SO 2 , a certain current is applied between the detecting electrode and the basic electrode for measuring SO 2 gas and the voltage between the reference electrode and the detecting electrode is measured, or a current between the detecting electrode and the reference electrode is measured by keeping the voltage constant between the detecting electrode and the reference electrode. This enables measurement with high precision by separating only the reaction of SO 2 gas on the detecting electrode. Therefore, in the present invention, it is possible to improve measurement precision by combining the aforementioned methods with the function of the structure of the SO 2 gas sensor.
It is preferable that a solid electrolyte, which is one of the members constituting the aforementioned SO 2 gas sensor, contains zirconium oxide and a stabilizer. As a stabilizer, there can be suitably used magnesium oxide, calcium oxide, yttrium oxide, cerium oxide, scandium oxide, and a rare earth metal oxide. For electrodes except for the detecting element for measuring SO 2 gas, it is preferable to use a cermet electrode made of porous platinum or a mixture of porous platinum and the same material as the solid electrolyte. When the gas sensor has a structure in which the solid electrolyte can be heated and maintained at a constant temperature of 600° C. to 900° C., by using an element for measuring temperature and a heater installed on the vicinity of solid electrolyte or those installed unitarily with the solid electrolyte, it can cope with a decrease in temperature dependency of a value obtained by the measurement.
When the detecting electrode for measuring SO 2 gas is formed on the solid electrolyte, the solid electrolyte is roughened as shown in FIG. 13 by subjecting the solid electrolyte to chemical etching or the like in advance so as to enhance adhesion between the solid electrolyte and the detecting electrode. Additionally, SO 2 gas detection sensitivity gas is further improved by increasing the area of contact interfaces among the detecting element, the solid electrolyte, and SO 2 gas.
The same effect can be obtained by disposing an electrode film on a layer which is disposed on the solid electrolyte and contains Au or Au alloy fine particles having a certain average diameter.
According to the present invention, in an apparatus for measuring the gas component concentration in an exhaust gas, SO 2 concentration can be measured more precisely by using the aforementioned oxygen gas sensor as a direct inserted type or a direct coupled type of sensor, resulting in more precise control of SO 2 concentration in an exhaust gas. The direct insert type of sensor is disclosed by Japanese Patent Laid-Open 1-250753, where the sensor is directly inserted into a measurement atmosphere. The direct coupled type of sensor is disclosed by Japanese Patent Laid-Open 3-277957, where the sensor is disposed in a periphery of a measurement atmosphere and takes the gas to be measured into the apparatus by using the flow speed of the gas to be measured.
As described above, the present invention employs, as a detecting electrode for measuring SO 2 gas concentration, an electrode made of metallic material such as gold or a gold alloy, which has lower catalytic ability than platinum (which has conventionally been used), and a glass component (for when SO 2 gas concentration in a combustion engine or in the air is measured). This enables a reduction in the influence of O 2 concentration on a value of SO 2 gas concentration and raises the operation temperature of the sensor up to 600° C.-900° C.
An oxidation reaction of SO 2 gas is accelerated in a detecting electrode by applying a certain current between he detecting electrode for measuring SO 2 gas and the basic electrode for measuring SO 2 gas, or by keeping the voltage between the detecting electrode and the basic electrode constant, thereby improving sensitivity of the SO 2 gas sensor to SO 2 gas.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view showing a basic structure of a SO 2 gas sensor of the present invention.
FIG. 2 is a sectional view showing an embodiment of a SO 2 gas sensor of the present invention.
FIG. 3 is a sectional view showing another embodiment of a SO 2 gas sensor of the present invention.
FIG. 4 is a sectional view showing an embodiment of a SO 2 gas sensor of the present invention, which is provided with an electrode for measuring O 2 .
FIG. 5 is a sectional view showing an embodiment of a SO 2 gas sensor of the present invention, which is provided with an O 2 pump.
FIG. 6 is a sectional view showing an embodiment of a SO 2 gas sensor of the present invention, which is provided with a gas diffusion rate-determining layer.
FIG. 7 is a sectional view showing an embodiment of a SO 2 gas sensor of the present invention, which is provided with a reference electrode.
FIG. 8 is a sectional view showing another embodiment of a SO 2 gas sensor of the present invention, which is provided with a reference electrode.
FIG. 9 is a graph showing an improvement of sensitivity of detecting SO 2 gas by a SO 2 gas detecting electrode of the present invention.
FIG. 10 is a graph showing an influence of a CO gas concentration in a gas to be measured on a SO 2 gas detecting electrode of the present invention.
FIG. 11 is a graph showing the influence of the amount of a glass component added to Au (or Au alloy) on SO 2 gas detecting sensitivity.
FIG. 12 is a graph showing the influence of a content of lead oxide in a glass component on a responding property.
FIG. 13 is a schematic sectional view showing the state of the bonding portion between a SO 2 gas detecting electrode and a solid electrode which is formed after roughening a surface, on the side of the SO 2 gas detecting electrode to be mounted, of the solid electrode according to a method for forming a SO 2 gas detecting electrode of the present invention.
FIG. 14 is a sectional view of a SO 2 gas measuring apparatus on which a gas sensor of the present invention is mounted.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention is described on the basis of the preferred embodiments with reference to drawings. However, the present invention is by no means limited to these embodiments.
FIG. 1 is a sectional view showing the basic structure of a SO 2 gas sensor of the present invention. A basic electrode 2 and a detecting electrode 3 , which are a pair of electrodes, are formed on each of the surfaces of a solid electrolyte plate 1 so as to sandwich the solid electrolyte plate 1 . The basic electrode 2 is formed in the side of basic gas, and the detecting electrode 3 is formed in the side of gas to be measured. Leads 4 and 5 are connected to the basic electrode 2 and the detecting electrode 3 , respectively. The solid electrolyte plate 1 is engaged with substrate 6 and serves as a partition between the gas to be measured and the standard gas.
The solid electrolyte plate 1 may be made of any material as long as it has oxygen ion conductivity, such as zirconium oxide, bismuth oxide, or cerium oxide. The present invention preferably employs stabilized zirconia, which is excellent in high temperature stability and chemical stability. The term “stabilized zirconia” means a product whose cubic crystal which is a stabilized phase of zirconium oxide at a high temperature is stabilized at all range of temperatures so as to prevent a martensite-type phase transition. This is done by forming a solid solution with a divalent or trivalent metal oxide, which is called a stabilizer since pure zirconium oxide causes the phase transition at about 1000° C. due to a charge in volume between the monochrinic crystal and the tetragonal crystal thereof, which results in the formation of cracks. The solid solution of such a stabilizer generates an oxygen defect and improves conductivity. As a stabilizer in the present invention, there can be suitably used magnesium oxide (MgO), calcium oxide (CaO), yttrium oxide (Y 2 O 3 ), cerium oxide (CeO 2 ), scandium oxide (Sc 2 O 3 ), and rare earth oxides.
The solid electrolyte plate 1 is produced by subjecting a green sheet obtained by a known method such as press molding, slip casting, extrusion molding, and doctor blading then punching to obtain a compact having a predetermined shape, removing the binder, and firing. As necessary, it is further subjected to grinding and/or sanding to obtain a sample plate.
Then, the basic electrode 2 is to be electrically connected with a solid electrolyte plate 1 . Since the basic electrode 2 is required to serve as an electrode for diffusing/adsorbing a gas, it is preferable for this electrode to be porous. Since the basic electrode 2 is the place for an electrochemical reaction when O 2 in a standard gas is ionized, there is suitably used Pt, which has a characteristic of adsorbing and ionizing O 2 , as a material for the basic electrode 2 . Alternatively, an alloy containing Pt as a main component and Pd, Rd, or the like, or Pt, or a cermet material composed of a Pt alloy and a solid electrolyte material may be used. The reason why a cermet is used as a material for a basic electrode 2 is that it provides many places for the electrochemical reaction and avoids exfoliation, or the like, of the electrode caused by a thermal stress which occurs at high temperatures. It also aims at improvement of adhesion between the electrode and the solid electrolyte and adjustment of the coefficient of thermal expansion since the electrochemical reaction of ionizing O 2 in the standard gas takes place at the interfaces among the three phrases of the gas phase, the metallic electrode, and the solid electrolyte.
The basic electrode 2 is fixed to the solid electrolyte plate 1 by printing a paste made of a cermet of Pt and a solid electrolyte on a surface of a solid electrolyte plate 1 by a method such as screen printing, abutting a Pt mesh to the paste before it is dried, and baking by drying it. Alternatively, there may be employed a method in which a Pt mesh is impregnated with a slurry containing Pt, the Pt mesh is placed on the solid electrolyte plate 1 before the slurry is dried, and they are subjected to baking. These methods are simplest and easiest. Alternatively, the paste may be left unbaked after the screen printing. The baking may be performed simultaneously with the baking of the detecting electrode, which is formed on the surface of the solid electrolyte 1 , opposite to the basic electrode 2 . Alternatively, the baking of the basic electrode 2 may be performed separately from the baking of the detecting electrode 3 . Regarding fixation of the Pt lead 4 to the basic electrode, when the basic electrode is Pt mesh, it is preferable that the Pt lead 4 has previously been welded to the Pt mesh by spot welding, arc welding, or the like, so as to give it high strength in fixation. When only a screen printing is employed for forming an electrode, the Pt lead 4 can be fixed by baking. Alternatively, the electrode may be found by Pt plating, baking of chloroplatinic film, or the like.
On the other hand, a detecting electrode 3 is disposed on the surface, opposite to the basic electrode 2 , of the solid electrolyte plate 1 . The detection electrode 3 is preferably porous since, as a result of an oxidative reaction between an oxygen ion transferred through the solid electrode and SO 3 gas absorbed in the metallic component of the electrode, a function, which on interface between the gas phase, the metallic electrode and the solid electrode, and which is capable of liberating SO 2 gas, is necessary. A material suitable for the detecting electrode 3 preferably has the characteristic of not promoting oxidation of SO 2 gas by coexisting O 2 . That is, it is preferable that a reaction of an adsorbed oxygen (O(ad)) and SO 2 gas, as shown in the following formula 1, is not caused and that an electron (e − ) is generated by the reaction of an oxygen ion (O 2− ) which transferred in a solid electrolyte from the side of the basic electrode and SO 2 gas, as shown in the following formula 2. This electron is applied to a SO 2 gas measurement.
SO 2 +O(ad) SO 3 [Formula 1]
SO 2 +O 2− SO 3 +2 e− Formula 2
From the above, gold (Au) is suitably used as a metal for the detecting electrode in the present invention. It is more preferable to employ an Au alloy in which 1-10 wt % of another noble metal is added to Au. By adding, to Au, another noble metal of 0.1-10 wt %, preferably 0.1-5 wt %, more preferably 0.1-1 wt %, aggregation of Au particles at a high temperature upon producing the detecting electrode is suppressed, which enables maintenance of the porosity and enlarge the surface area of the detecting electrode. As a result, the sensitivity with which SO 2 is detected can be improved.
Incidentally, Rh, Pt, Pd, Ag, or the like, may be used as a metal to be alloyed with Au. Au concentration is 90 wt % or more, preferably 95 wt % or more, more preferably 99 wt % or more. Au concentration is suitably determined depending on the alloys melting point and baking temperature, or depending on the temperature at which the sensor is used.
There can be suitably used a cermet electrode in which the same material as the solid electrolyte plate is mixed with Au or a Au alloy. The reason why a cermet material is used is the same as the case of the basic electrode 2 .
In the case where a layer of Au or fine particles from an Au alloy are formed on the electrolyte and an electrode film is formed on the layer so as to obtain the detecting electrode, a paste in which fine particles are dispersed is applied on the solid electrolyte and fired, or a layer of fine particles and an electrode film are applied on the solid electrolyte in this order and fired simultaneously.
Incidentally, fine particles of Au or an Au alloy have an average particle size of 0.01-10 m, preferably 0.01-1 m, more preferably 0.01-0.1 m. The shapes of particles are not necessarily spherical and may be granules or, for instance, rugby-ball shaped.
Any kind of glass material may be used in combination with gold or a gold alloy upon producing the detecting electrode, as long as it melts at a temperature which is the same as or lower than the melting point of gold or a gold alloy, and lead brosilicate glass is suitably used.
By using a glass component in combination with gold or a gold alloy, a glass phase is precipitated on interfaces among the gas phase, the metal electrode, and the solid electrolyte, thereby further suppressing a reaction of an inflammable gas, such as CO. Therefore, interferential influence caused by inflammable gas can be reduced.
Further, adhesion between a substrate made of solid electrolyte and a detecting electrode is improved.
Improvement of detection sensitivity by addition of a glass component was tested in comparison with a detecting electrode having only an Au electrode. Gases containing sulfur dioxide of 0, 200, 400, 600, 800, or 1000 ppm were used for testing sensitivity of detecting sulfur dioxide. The results are shown in FIG. 9 . As is clear from the results, the use of a glass component improves sensitivity of detecting sulfur dioxide.
In order to test the influence of carbon monoxide on a sulfur-dioxide detecting electrode of the present invention, a detecting electrode of the present invention and a detecting electrode made of only Au without any glass component are tested for an influence on sulfur dioxide by the use of gases containing CO gas of 0, 20, 40, or 80 ppm. The results are shown in FIG. 10 . As is clear from the results, even if 80 ppm of carbon monoxide is contained in a gas to be measured, there was no influence substantially in the case of the detecting electrode of the present invention.
Incidentally, in the case of using a glass component, an amount of a glass component to be added to a sulfur dioxide detecting electrode of the present invention can be selected arbitrarily within the range of 1-10 wt % of the total weight of gold or gold alloy and the glass component.
A detecting electrode can be formed by applying a paste made of a mixed powder, gold or gold alloy, and a glass component on a substrate made of solid electrolyte and then by firing the paste. Alternatively, the mixed powder is dispersed in an adequate solvent to obtain a dispersed liquid, and the dispersed liquid is applied on the substrate made of solid electrolyte and fired.
When the amount of a glass component to be added is less than 1%, adhesion of the detecting electrode to the substrate made of solid electrolyte is not improved, and the effect of reducing interferential influence caused by inflammable gas, for example, CO is not sufficient. When it exceeds 10%, it is not preferable because delay in response or deterioration in SO 2 sensitivity is perceptible. A content (wt/wt %) of lead oxide in glass component has an influence on the sensing property and responding property for detecting SO 2 gas. A content (wt/wt %) of lead oxide in a glass component is 60 (wt/wt) % or more, preferably 60% or more and 90% or less. When it is less than 60%, delay in response is found, although influence on SO 2 sensitivity is not found. When it exceeds 90%, sensitivity to inflammable gas, for example, CO gas becomes slightly higher, although the SO 2 sensing property and responding property are not influenced. Therefore, precision in measuring SO 2 gas is unpreferably influenced.
The lead 5 can be fixed to the detecting electrode 3 by the use of a paste, as a material for an electrode, containing Au or an Au alloy or cermet of Au and a solid electrolyte, an Au mesh or an Au alloy mesh, and an Au lead 5 as in the aforementioned case of the basic electrode 2 .
The solid electrolyte 1 to which an electrode was thus fixed is pressed to the substrate 6 so as to engage with the substrate 6 . The solid electrolyte 1 functions as a partition wall separating the atmosphere of the basic gas from the atmosphere of gas to be measured. For sealing the solid electrolyte plate 1 and the substrate 5 , a glass melting agent, or the like is used. As a standard gas, air is usually employed. When such a partition-type structure is employed, the SO 2 gas concentration in the gas to be measured can be measured by measuring electromotive due to a difference in SO 2 gas partial pressure between the standard gas and the gas to be measured. In this case, the basic electrode 2 may be made of the same material as the detecting electrode 3 .
FIG. 2 shows another embodiment of the present invention. A solid electrolyte substrate 11 having a bottomed cylindrical shape is provided with a basic electrode 12 inside and a detecting electrode 13 outside the end portion. A Pt lead 14 and a Au lead 15 are connected to the electrodes 12 and 13 , respectively. The solid electrolyte substrate 11 having a bottomed cylindrical shape can be easily produced by firing a compact obtained by slip casting, extrusion molding, or injection molding. Each electrode can be produced by applying a paste, or the like, containing an electrode material on the position where an electrode is fixed to, abutting a mesh of an electrode material, and firing as in the description of the embodiment in FIG. 1 . Since the embodiment also shows a structure which separates a gas to be measured and a basic gas, the sensor constitutes a concentration cell. Therefore, the basic electrode 12 may be composed of a material of Au or an Au alloy as well as the detecting electrode 13 .
FIG. 3 shows still another embodiment of the present invention. A basic electrode 22 and a detecting electrode 23 are fixed to the same surface of the solid electrolyte plate 21 . To the basic electrode 22 and the detecting electrode 23 are fixed a Pt lead 24 and a Au lead 25 . In this case, the standard gas is not required, and the whole sensor element is placed in an atmosphere for a gas to be measured. A shape of the solid electrolyte plate 21 is not limited to be laminar, and it may be any shape, for example, a cylinder or a stick.
In the case of this embodiment, the basic electrode 22 is preferably made of a material different from that of the detecting electrode 23 . This is because the SO 2 gas concentration in the gas to be measured can be measured by measuring the electromotive force caused by the difference in electrode reaction of SO 2 gas between the detecting electrode 23 and the basic electrode.
FIG. 4 shows an SO 2 sensor according to the present invention regarding a mode for measuring SO 2 gas concentration. For example, an electrode for measuring O 2 is fixed to an embodiment shown in FIG. 2 . SO 2 gas concentration and O 2 gas concentration are simultaneously measured, thereby removing and amending influence caused by the reaction of O 2 which occurs as a result of measuring SO 2 gas by the use of the result of the measurement of O 2 gas concentration. Thus, SO 2 gas concentration can be measured independently. In this mode, there can be used the same basic electrode 12 and detecting electrode 13 for measuring SO 2 gas as the basic electrode and detecting electrode used in the mode shown in FIG. 2 . The basic electrode 26 and the detecting electrode 27 for measuring O 2 are basically O 2 sensors. Therefore, there is preferably used a porous Pt electrode, which is used as an electrode of a conventional zirconia O 2 sensor. Fixing of these electrodes and a lead 28 can be performed in the same manner as in the case of the electrodes for measuring SO 2 gas. As a lead 28 , there can be preferably used a Pt wire. Incidentally, it can be easily thought that this mode can be applied to a planar element shown in FIG. 1. A basic electrode for measuring SO 2 gas may be used in combination with a basic electrode for measuring O 2 .
FIG. 5 shows an embodiment of sensor using an H-type electrolyte substrate 3 having two depressions. One depression contacts an atmosphere for a basic gas. At the bottom of the depression, a basic electrode 32 made of porous Pt is formed. To the basic electrode 32 is fixed a Pt lead 34 . Another depression contacts an atmosphere for a gas to be measured. At the bottom of the protrusion is provided a detecting electrode 33 of Au or an Au alloy and a glass component. An Au lead 35 is fixed to the detecting electrode 33 . To the side wall of the depression are fixed an O 2 sensor 41 and a O 2 pump cell 42 . One of two electrodes 36 of the O 2 sensor 41 and one of two electrodes 37 of the O 2 pump cell 42 are formed inside the depression, and the other electrodes are formed outside the depression. All the electrodes contact an atmosphere for a gas to be measured. The electrode 37 of the O 2 pump cell preferably has a characteristic of not oxidizing SO 2 gas, and an electrode of a conductive metal oxide such as lanthanum manganite is preferably used.
Incidentally, as leads 38 and 39 fixed to the electrodes 37 and 38 , respectively, Pt wires are preferably used. Since the electrode 37 is a ceramic electrode, a lead 39 cannot be fixed directly by welding. Therefore, generally, a surface of the electrode is metallized, and then the lead 39 is baked.
This structure enables an O 2 pump cell to be driven by controlling a potentiostat 43 so that O 2 concentration in an atmosphere in a gas to be measured is always kept constant by an O 2 measuring sensor. Therefore, the O 2 concentration is kept constant in an SO 2 gas detecting electrode in a gas to be measured, and it is possible to measure SO 2 by easily excluding the O 2 influence generated by a detecting electrode 33 for measuring SO 2 gas to be measured. Thus, measurement precision is further sought.
FIG. 6 shows a structure in which a gas diffusion rate-determining layer 18 is disposed on the surface of a detecting electrode 13 for detecting SO 2 in a mode shown in FIG. 2 . The gas diffusion rate-determining layer 18 can remove inflammable gases such as propane and butane (except for SO 2 gas) sent to the surface of the detecting electrode 13 . Selectivity of SO 2 gas in a sensor of the present invention can be improved by using such a gas diffusion rate-determining layer 18 . Specifically, a zeolite film is used. It can be formed by superposing the film on a surface of the detecting electrode 13 by dipping, or the like, to form a laminate. Alternatively, the gas diffusion rate-determining layer 18 can be formed by a screen printing, or the like, after the detecting electrode 13 is formed on the solid electrolyte substrate 11 . It is needless to say that such a gas diffusion rate-determining layer 18 can be applied to all the aforementioned embodiments.
Regarding the aforementioned method for measuring SO 2 gas concentration in a SO 2 gas sensor, a concentration cell is formed in a structure in which a solid electrolyte plate serves as a partition to separate an atmosphere for a standard gas and an atmosphere for a gas to be measured. Therefore, SO 2 gas concentration can be measured by an electromotive force of the concentration cell. When the whole solid electrolyte having a detecting electrode and a basic electrode is disposed in an atmosphere for a gas to be measured, the detecting electrode for measuring SO 2 gas is made of a material different from that for the basic electrode. Therefore, by measuring a difference in electromotive force generated between each electrode, the SO 2 concentration can be known.
Additionally, in the present invention, a certain current is applied between the detecting electrode and the basic electrode for measuring SO 2 gas in all of the aforementioned embodiments. SO 2 gas can be measured by measuring a change of electromotive force due to adsorption/oxidation of SO 2 gas on the detecting electrode. According to this method, oxidation reaction of SO 2 on the electrode is promoted, and sensitivity of a sensor to SO 2 gas is improved. Further, a similar effect can be obtained by measuring the current, between the detecting electrode and the basic electrode, which is required in order to keep the voltage constant between the detecting electrode and the basic electrode for measuring SO 2 gas.
FIG. 7 shows a structure in which a reference electrode 7 for measuring SO 2 gas is disposed on a SO 2 gas sensor shown in FIG. 1 . The reference electrode 7 is made of porous Pt as in the basic electrode 2 , and a Pt wire is used as a lead 8 . In a SO 2 gas sensor of this structure, the SO 2 gas reaction at the detecting electrode 3 can be separately measured by measuring voltage between the reference electrode 7 and the detecting electrode 3 when a certain current is applied between the basic electrode 2 and the detecting electrode 3 . This enables more precise measurement.
FIG. 8 shows an embodiment in which a reference electrode 16 with a Pt lead 17 is disposed on the embodiment using the solid electrolyte substrate 11 having a bottomed cylindrical shape shown in FIG. 2 . The reference electrode 16 has the same function as the reference electrode 7 shown in FIG. 7 .
FIG. 9 shows results of measuring SO 2 gas concentration by the use of a sensor in which an electrode is made of Au without using any glass component in contrast with a sensor of the present invention. A sensor of the present invention apparently has high sensitivity in detecting SO 2 gas and shows that it is excellent as an SO 2 gas sensor.
FIG. 10 shows results of testing the influence of CO gas, which is one of the inflammable gases contained in the gas to be measured, on a sensor by the use of a sensor in which an electrode is made of Au without using any glass component in contrast with a sensor of the present invention. Influence of CO gas on a sensor of the present invention was not found substantially even with concentration of 80 PPM.
FIG. 11 is a graph showing the influence on sensitivity of detecting SO 2 when a glass component of 3, 6, 12, or 25 (wt/wt) % was added to Au (or an Au alloy). This graph shows that SO 2 sensitivity is lowered when a glass component exceeds 10%.
FIG. 12 is a graph showing the influence on response properties when the lead oxide content in a glass component is controlled to be 55, 68, 74 or 85 (wt/wt) %. This graph shows that the response is slow when the content is less than 60%.
FIG. 13 shows a mode of a method for forming an SO 2 detecting electrode of the present invention.
FIG. 14 shows a schematic view of a basic structure of a direct-coupled SO 2 gas measurement apparatus on which a SO 2 gas sensor shown in FIG. 1 . This apparatus is composed basically of a sensor case 110 having a portion 118 for fixing a sensor apparatus, a sensor cover 114 fixed to the sensor case 110 so that it is attachable and detachable, a SO 2 gas sensor 108 of the present invention installed in a sensor box, a holder 109 to which the sensor 108 is fixed, a pipe 12 for supplying a basic gas, a filter 113 disposed on a front surface of the sensor 108 and made of porous ceramic, a pipe 103 for collecting a gas to be measured, having a dual structure, and a pipe 101 for supplying an ejector gas.
The pipe 103 for collecting the gas to be measured has a dual structure. A path 115 for collecting the gas to be measured is formed in a peripheral portion of the pipe 103 , and a path 104 for discharging a gas to be measured is formed inside the pipe 103 .
An ejector supply port 107 is formed at one end of the pipe 101 for supplying an ejector gas. The pipe 101 for supplying an ejector gas first passes through a heat-insulating material 102 as shown in 101 a , and then reaches an exposed portion of a pipe 101 b for supplying an ejector gas, which is spirally wound around the periphery of the pipe 103 for collecting a gas to be measured and has a dual structure. Then, it is connected to an exposed portion of a linear pipe 101 c for supplying an ejector gas and passes through the heat-insulating material 102 . Then, it is exposed to inside of the pipe 103 and connected to an ejector 106 .
When an ejector gas is supplied from the ejector supply port 107 , the ejector gas passes through an embedded portion 101 a in the heat-insulating material 102 , and the exposed portion 101 b and 101 c and an embedded portion 101 d in the heat-insulating material 102 in this order and spouts out of the ejector discharge port 120 . This reduces pressure in a periphery of the ejector 106 and causes a convection. As a result, the gas to be measured is collected from outside of the apparatus via a collection port 116 and flows along an arrow A in a path 115 for collecting a gas to be measured. The gas reverses to flow along an arrow B in a path 104 for discharging a gas to be measured, and is discharged outside of the apparatus. Meanwhile, SO 2 gas in the gas to be measured is measured by a sensor 108 .
As described above, according to an SO 2 gas sensor of the present invention, when an SO 2 gas concentration in an exhaust gas discharged from various kinds of combustion engines in thermoelectric power plants, incineration facilities, or the like, or in the air, selectivity of SO 2 gas can be improved by employing an electrode containing Au or an Au alloy, which has a lower catalytic ability to SO 2 gas than Pt, which has conventionally been used, and a glass component for the detecting electrode for measuring SO 2 gas. Further, precision in measuring SO 2 gas is improved by compensating a value of SO 2 gas measurement by a value of an O 2 gas measurement by the use of O 2 sensor in combination. Particularly, even if an oxygen gas coexists in an exhaust gas, influence of O 2 concentration on a value of SO 2 gas concentration measurement can be made very small. Additionally, in all the SO 2 gas sensors of the present invention, sensitivity to SO 2 gas can be improved by applying a certain current between electrodes for measuring SO 2 gas or by keeping a voltage constant. Generally, precision in SO 2 gas sensor can be remarkably improved. Further, an area of contact interfaces among a gas phase, a metal electrode, and a solid electrolyte can be enlarged by making rough a surface, on the side of the detecting electrode, of the solid electrolyte by a chemical etching, or the like, or by disposing a layer of a fine particles of gold or gold alloy between the solid electrolyte and the electrode film. Since the sensor can be operated at the high temperature of 600° C.-900° C., an error caused by other interferential gas components contained in a gas to be measured is decreased.
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A sulfur dioxide gas sensor having a high selectivity of SO 2 gas, and an operability at a high temperature which comprises: a solid electrolyte having oxygen ion conductivity; a detecting electrode for measuring sulfur dioxide gas, electrically connected to at least a part of a surface of the solid electrolyte and containing glass and either gold or a gold alloy; and a basic electrode for measuring sulfur dioxide gas, electrically connected to at least a part of a surface of the solid electrolyte and containing Pt.
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TECHNICAL FIELD OF THE INVENTION
[0001] The invention present relates in general to snow melting devices. More particularly, the present invention relates to a portable snow melting device which may be applied to the surface of snow to warm the snow and initiate melting thereof.
BACKGROUND OF THE INVENTION
[0002] A snowfall may be exciting for children—who look forward to fun in the snow, but can be aggravating to adults—who anticipate hours of back-breaking snow removal work. Many individuals are injured each year from slipping on snow covered or icy pathways. Although shoveling can remove the snow from the pathway, it requires a large amount of work which many infirm individuals are unable to perform.
[0003] Snow removal on sidewalks, walkways, driveways, and patios is traditionally carried out with a shovel. The problems with using a shovel are many. First, a lot of labor is involved with repeatedly undermining the shovel beneath a pile of snow, and then physically lifting the snow away from the sidewalk. Second, the shovel cannot always remove all of the snow. On textured sidewalks and brick or cobblestone driveways, it is not possible to scrape off all snow. Third, on such textured sidewalks and driveways, it is extremely difficult to carry out shoveling at all, since the shovel continually snags upon a brick, stone, or the like. The shovel can even chip bricks and stones, creating a weathered appearance after the winter. A similar problem exists with shoveling snow from uneven or broken sidewalks and driveways.
[0004] The removal of snow is generally accomplished by motorized scoops or by shoveling. There are often small snow falls which are not adequately or conveniently dealt with by cumbersome apparatus, and the use of snow shovels becomes heavy work. The snow blower has been around for decades, and provides a less labor intensive snow removal solution for some people. However, the snow blowers typically employ two stroke engines, which are often difficult to start, and require long term storage of gasoline and oil. Further, they are loud and produce the odor of gasoline exhaust as they operate. Thus they are unsuitable for use in tight alleys and near buildings where the fumes could harm people living therein. Furthermore, many of these devices have a large number of moving parts. Such devices are therefore subject to malfunctioning and may require a great deal of upkeep and repair. This will make such devices undesirable for many people.
[0005] The inventor is aware of several have snow melting mats have been proposed for melting snow. However, these devices are only suited for installation upon a walkway or other such area prior to a snowfall, so that they can then be activated following the snowfall to cause the snow to melt. However, none of these devices are suited for portable use wherein the device is brought to a location after a snowfall where snow melting is desired, to effect snow melting at that location.
[0006] While these units may be suitable for the particular purpose employed, or for general use, they would not be as suitable for the purposes of removing snow or ice from an area such as a patio, walkway or the like. The inventor is also aware of devices such as heated snow shovels. However, heated snow shovels may be inadequate to remove large amounts of snow and may not be adequate at all for removing ice. Ice removal using a shovel, even a heated shovel, will be difficult work, time consuming and may still damage the surface if the shovel is used to chip the ice. Accordingly, even heated snow shovels have many disadvantages.
[0007] Since snow falls may create various depths of snow, any device used to remove snow must be adaptable for various snow depths. While shovels will be adaptable, shovels will still have the above-discussed problems. Therefore, there is a need for a device for melting snow or ice which is easy to use and which is adaptable for a wide variety of snow fall depths.
SUMMARY OF THE INVENTION
[0008] The above-discussed disadvantages of the prior art are overcome by an electrically operated snow/ice melter that operates from standard house utility power. The snow/ice melter has adjustable legs whereby different depths of snow and/or ice can be melted.
[0009] Using the snow/ice melter embodying the present invention will permit a user to quickly and easily melt snow and/or ice of nearly any depth. The melter is easy to move and position so even those of limited dexterity or strength can efficiently operate the melter embodying the present invention.
[0010] Other systems, methods, features, and advantages of the invention will be, or will become, apparent to one with skill in the art upon examination of the following figures and detailed description. It is intended that all such additional systems, methods, features, and advantages be included within this description, be within the scope of the invention, and be protected by the following claims.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
[0011] The invention can be better understood with reference to the following drawings and description. The components in the figures are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the invention. Moreover, in the figures, like referenced numerals designate corresponding parts throughout the different views.
[0012] FIG. 1 is a perspective view of a snow/ice melter embodying the present invention.
[0013] FIG. 2 is an end elevational view of the snow/ice melter shown in FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
[0014] Referring to the figures, it can be understood that the present invention is embodied in a snow/ice melter 10 which overcomes the problems discussed above in relation to existing snow clearing devices. Melter 10 comprises a housing 12 which has a first surface 14 that is a top surface when the housing is in a use condition such as shown in FIG. 1 , a second surface 16 that is a bottom surface when the housing is in use and a thickness dimension 18 which extends between the first surface and the second surface. A first end 20 is a forward end when the housing is in use and a second end 22 is a rear end when the housing is in use. A top element 24 is removably mounted on the housing and an interior chamber 26 is defined in the housing.
[0015] A heating unit 30 is located on the housing and functions to melt snow or ice located beneath the housing when activated. The heating unit includes an electrical heater 32 , such as an electrical resistance wire or the like, located on the bottom surface of the housing.
[0016] A power transformer 34 as shown in dotted lines is located in interior chamber 26 and is electrically connected to the electrical heater. Transformer 34 is of the type well known to those skilled in the art and the exact details of the transformer are not important to the present invention and will not be claimed. As such, the details of the transformer will not be discussed. A power cord 36 is electrically connected to power transformer 34 and is adapted, as by including an appropriate plug 38 on one end thereof, to be electrically connected to a utility power source, such as via an electrical outlet in a home.
[0017] A handle 40 has one end 42 connected to the housing and has a hand grip element 44 on a second end 46 thereof. Handle 40 is movable in the manner of any well known handle unit so melter 10 can be pushed using handle 40 . A heating unit control system 50 is located on one end of the housing and includes an on/off switch 52 located on the first end of the housing. Switch 52 is electrically connected to the heating unit. A power level adjustment switch 56 is located on the first end of the housing and is electrically connected to the heating unit. A plug socket 58 is also located on the end of the housing and is electrically connected to the power transformer so power from a utility source can be transferred to the transformer when the cord 36 is electrically connected to a power outlet and to socket 58 . A power cord attachment unit 60 is located on the first end of the housing and is electrically connected to the heating unit.
[0018] Four adjustable legs, such as legs 70 and 72 , are mounted on the housing. The legs are identical and each leg includes a first portion 74 which is fixed to the housing, a second portion 76 that is telescopingly connected to the first portion to move in the direction of thickness dimension 18 of the housing for adjusting the height of the housing above a ground level to accommodate various snow and/or ice thicknesses. A plurality of set pin holes, such as set pin hole 78 , are defined through the first portion and through the second portion, and a set pin, such as set pin 82 , fits through the set pin holes to couple the second portion to the first portion in the selected position. Wheels, such as wheels 84 and 86 , are rotatably mounted on the second portion of two of the adjustable legs. A power cord holder 90 is mounted on the first end of the housing to store a power cord when the melter is being stored.
[0019] Use of melter 10 can be understood from the teaching of the present disclosure and thus will not be discussed in detail. The melter is moved to be located above a patch of ice or snow to be melted. The power cord is connected to the unit and to a power source, the legs are adjusted so the heating unit is located in a desired position, and the unit is activated. The unit is moved as necessary to melt the ice or snow, and can be left on at any desired location to evaporate any water that may remain after the melting step is completed.
[0020] While various embodiments of the invention have been described, it will be apparent to those of ordinary skill in the art that many more embodiments and implementations are possible within the scope of this invention. Accordingly, the invention is not to be restricted except in light of the attached claims and their equivalents.
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A portable electric snow/ice melter has adjustable legs whereby it can be easily used to melt snow and/or ice of varying depths.
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This is a continuation of application Ser. No. 08/568,978, filed Dec. 7, 1995 now U.S. Pat. No. 5,678,871, the disclosure of which is herein incorporated by reference.
FIELD OF THE INVENTION
The present invention relates generally to a security astragal used to secure a door latching mechanism from tampering. More particularly, the present invention relates to an improved astragal device that can be easily installed on and removed from new and existing doors but is also secure against unauthorized removal.
BACKGROUND OF THE INVENTION
Double entrance doorways are commonplace in residential and business settings. Typically, one door in a double doorway remains closed and is referred to as the inactive leaf. The other door, commonly referred to as the active leaf, is used as the main entrance door. Generally, the mating edges of the active and inactive doors do not directly contact each other, but are separated by a slight gap. This gap, when exposed, provides room for tampering with the door latching mechanism.
An astragal's primary function is to cover the gap between double doors and thus secure the door latching mechanism. Typically, an astragal is attached along the exterior edge of the inactive door so as to cover the gap between the active and inactive door leaves.
FIG. 1 depicts a standard double door arrangement employing a prior art astragal 10. As shown, an astragal 10 is affixed to and runs the length of the inactive leaf 12. When the active leaf 14 is in the closed position, the astragal 10 functions to cover the gap between the active 14 and inactive 12 leaves so as to prevent tampering with the door latching mechanism.
FIG. 2 depicts a partial view of a typical inactive door leaf 12 with an attached astragal 10. As shown, the astragal 10 overlaps the edge of the inactive leaf 12. The overlap is large enough to bridge a gap that may exist between the inactive 12 and active 14 leaves when both are in the closed position. By bridging the gap between the door leaves, the astragal protects the latching mechanism from compromise.
A problem not addressed by the prior art is securing the astragal against unauthorized removal while also providing the flexibility for quick and easy authorized removal. One prior art method of attaching an astragal is to drill anchoring screws through the exterior face of the astragal. An astragal attached in this fashion serves the purpose of obstructing attempts to manipulate the latching mechanism between doors. However, an astragal attached with exposed anchoring screws could potentially be removed without authorization by unscrewing the exposed screws. Unauthorized removal of the astragal would leave the latching mechanism exposed to potential tampering.
Another prior art method of securing an astragal is to weld the astragal to the door. Generally, the welded bonds between the door and the astragal are permanent and cannot be broken. Although welding assures against unauthorized removal of the astragal, it also precludes the astragal from being removed so that the door can be reused without the astragal. Similar techniques of permanently affixing an astragal to the door also assure against unauthorized removal but likewise preclude authorized removal and subsequent reuse of the door without the astragal.
Accordingly, a primary goal of the present invention is to provide a security astragal that is secure against unauthorized removal but which permits authorized removal and subsequent reuse of the door without the astragal.
SUMMARY OF THE INVENTION
The present invention provides a security astragal that can be easily installed and removed from a door but which is secure against unauthorized removal. The invention marks a significant improvement over the prior art by providing substantial time savings during installation, assures uncompromising security, and provides the flexibility of reusing the door without the astragal.
In one presently preferred embodiment of the invention, the security astragal 20 comprises a security bar 22 that is fastened with anchoring screws 26 to the exterior door edge. The security bar 22 runs the length of the door, covering the gap between doors. The security bar therefore functions to secure the door latching mechanism from compromise.
The astragal 20 also comprises a protective sheath 24. The protective sheath 24 prevents unauthorized removal of the security bar 22. The protective sheath 24 envelopes the security bar 22 and, by so doing, prevents access to the security bar anchoring screws 26. By controlling access to the anchoring screws 26, the protective sheath 24 functions to protect the security bar 22 from unauthorized removal.
The protective sheath 24 is secured to the security bar 22 with securing screws 28 that are driven from the interior of the door. Because the securing screws 28 are driven from the interior of the door, they are not accessible from the exterior face of the doorway. Therefore, when the double doors are closed, the protective sheath 24 and the underlying security bar 22 cannot be removed by a person with access from the exterior of the doorway.
However, the protective sheath 24 can be removed quickly and easily by a person with access from the interior of the doorway. The protective sheath 24 is removed simply by unscrewing the protective sheath securing screws 28. With the protective sheath 24 removed, the security bar 22 can be easily removed by unscrewing the exposed anchoring screws 26.
The present invention therefore provides a security astragal 22 which prevents compromise of the door latching mechanism and insures that the astragal cannot be removed without authorization. Additionally, the present invention provides the flexibility to easily remove the security astragal 20 so that the door can be subsequently used without the astragal.
Other features of the present invention are described below.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a prior art astragal applied in a standard double doorway.
FIG. 2 is a perspective view of a prior art astragal.
FIG. 3 is an enlarged front view of an astragal in accordance with the present invention.
Fig. 4 is a perspective view of a security bar in accordance with th resent invention.
FIG. 5 is a view of a security bar from a perspective opposite of that depicted in FIG. 4.
FIG. 6 is a sectional view of a security bar.
FIG. 7 is a perspective view of a protective sheath in accordance with the present invention.
FIG. 8 is a sectional view of the protective sheath.
FIG. 9 is a perspective view of the security bar partially enveloped in the protective sheath.
FIG. 10 is a view of the security bar partially enveloped in the protective sheath from a perspective opposite of that depicted FIG. 9.
FIG. 11 is a sectional view of the security bar enveloped within th protective sheath.
Fig. 12 is a sectional view of the assembled protective sheath attached to a standard door.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIGS. 3 through 12 depict one presently preferred embodiment of the invention, distinguish the invention from the prior art, and demonstrate the beneficial characteristics of the invention.
FIG. 3 is a perspective view, partially in section, of a security astragal in accordance with the present invention. As shown, a security bar 22 is anchored to the edge of a standard door 12 with security bar anchoring screws 26. A protective sheath 24 envelopes the exterior portion of the security bar 22 so that the security bar anchoring screws 26 cannot be accessed. Both the protective sheath 24 and the security bar 22 may be made of metal of sufficient strength to obtain a U.L. rating. With the protective sheath 24 in place, the security bar 22 cannot be removed without removing the protective sheath 24.
The protective sheath 24 is secured to the security bar with protective sheath securing screws 28 that are driven from the interior of the doorway. The presently preferred security screws 28 comprise allen screws but other types of screws and entirely different means of securing, such as nuts and bolts, could also be employed to attach the protective sheath 24 to the security bar 22. Because the securing screws 28 are driven from the interior of the door, they are not accessible from the exterior face of the doorway. Therefore, when the double doors are closed, the protective sheath 24 and the underlying security bar 22 cannot be removed by a person with access from the exterior of the doorway.
FIGS. 4, 5, and 6 illustrate additional features of the security bar. FIG. 4 provides a frontal view of a representative portion of the security bar 22. The security bar 22 has multiple securing holes 30 through which the security bar anchoring screws 26 are inserted for the purpose of securing the security bar 22 to the door 12. In the presently preferred embodiment, the securing holes 30 are slightly offset from center so that a portion of the security bar 22 will overlap the edge of a door 12 when attached thereto. Also, multiple protective sheath securing notches 32 are located along the edges of the security bar 22. The protective sheath securing notches 32 accept protective sheath securing screws 28 that extend from the protective sheath 24 when the protective sheath 24 is in place over the security bar 22. With the protective sheath screws 28 inserted in the notches 32, the protective sheath 24 is secure and cannot be removed.
FIG. 5 depicts a representative portion of the security bar 22 as shown from the side opposite that depicted in FIG. 4. The illustrated surface abuts the door when the security bar 22 is attached thereto. FIG. 4 shows the security bar securing holes 30 and protective sheath securing notches 32 that are described above. Also shown is a clearance offset 34 which is slightly raised from the surrounding surface of the security bar 22. When the security bar 22 is attached to a door 12, the clearance offset 34 directly contacts the door 12 surface, leaving a gap between the door 12 and the remaining surface of the security bar 22. An insulating strip 36 that functions to dampen the impact between the double doors is likewise shown.
FIG. 6 depicts a cross sectional view of the security bar 22. As shown, the clearance offset 34 is slightly raised from the remaining portion of the security bar 22 surface. The clearance offset 34 directly contacts the surface of the door to which the security astragal 20 is attached. The insulating strip 36 is also raised from the surface of the security bar 22 but remains exposed when the security astragal 20 is attached to the door.
FIGS. 7 and 8 illustrate characteristics of the protective sheath 24. As shown in FIG. 7, which shows a representative portion of the protective sheath 24, the protective sheath 24 has a length commensurate with, and width slightly greater than, the security astragal 22. The protective sheath securing holes 38 line the edges of the protective sheath 24. When the protective sheath 24 is in place over the security bar 22, protective sheath securing screws 28 can be inserted into the securing holes 38. The screws extend to points within the protective sheath securing notches 32 located on the security bar 22 and function to hold the protective sheath 24 in place.
FIG. 8 provides a sectional view of the protective sheath 24. As shown, the edges of the protective sheath 24 are curved to form channels. The channels function as a guide so that the protective sheath 24 can be slidably moved over the security bar 22. When in place, the protective sheath 24 envelops the exterior of the security bar 22, so that the security bar anchoring screws 26 cannot be accessed.
FIGS. 9, 10, and 11 demonstrate the protective sheath and security bar in tandem. FIG. 9 is a frontal view of the protective sheath 24 partially in place over the security bar 22. The security bar 22 fits snugly within the channels formed by the edges of the protective sheath 24. As shown, the protective sheath 24 covers the security bar anchoring screws 26 so they cannot be compromised.
FIG. 10 provides a view of the protective sheath 24 and security bar 22 from the side opposite that depicted in FIG. 9. As shown, the edges of the security bar 22 fit within the channels formed by the edges of the protective sheath 24. The protective sheath 24 covers the exterior of the security bar 22 but does not interfere with the security bar being secured to the door.
FIG. 11 is a section view of the security bar 22 enveloped within the protective sheath 24. As shown, the edges of the security bar 22 fit within the channels formed by the edges of the protective sheath 24.
FIG. 12 is a cross-sectional view of the security astragal 20 attached to a door 12. As shown, the clearance offset 34 comes in direct contact with the surface of the door 12 to which it is secured. When the security bar is attached in such fashion, the remaining surfaces of the security bar 22 are left at a distance from the door, providing clearance for the protective sheath 24 to be slidably moved over the security bar 22. Also shown is the insulating strip 36. The insulating strip 36 is exposed so that it will contact the second door in the double doorway when the two are closed.
The present invention may be employed in other specific forms without departing from the spirit or essential attributes thereof. For example, a security bar with a different means of attaching to a door or a different shape may be employed. Similarly, a protective sheath, also with a different shape and securing mechanism, could be used. Accordingly, the scope of protection of the following claims is not limited to the presently preferred embodiment disclosed above.
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Disclosed is a security astragal that is secure against unauthorized removal but can be easily removed when authorized so that the door can be subsequently reused without the astragal. The disclosed security astragal includes a security bar that protects against tampering with the door latching mechanism and a protective sheath that secures the security bar from unauthorized removal.
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CROSS REFERENCE TO RELATED APPLICATION
[0001] Priority is claimed to U.S. Provisional Application No. 62/057,780 (filed on Sep. 30, 2014), which is incorporated herein by reference in its entirety.
STATEMENT OF GOVERNMENT INTEREST
[0002] None.
BACKGROUND OF THE DISCLOSURE
Field of the Disclosure
[0003] The disclosure relates to diboron compounds, which can be used as reagents to prepare chemical intermediates that are used in pharmaceutical, agrochemical, and specialty electronics industries. Such diboron compounds currently retail between about $300/kg to $800/kg, and the expense can be attributed to their complicated synthesis, which has not been significantly improved since the 1960s.
SUMMARY
[0004] Diboron reagents are used on metric ton scales for a variety of chemical processes, for example as starting compounds for various pharmaceutical, agrochemical, and specialty electronics compounds. Despite their widespread use, their synthesis involves multiple steps and batch processing, making them costly. The processes and compounds disclosed herein provide simplified syntheses that significantly reduce steps, improve scalability, and minimize costs for producing these diboron reagents.
[0005] In one aspect, the disclosure relates to a boron compound (e.g., in pure or substantially pure form (such as at least 90 wt. %, 95 wt. %, 98 wt. %, or 99 wt. % pure), or in admixture with other components) having a structure according to the following Formula I:
[0000]
[0000] wherein: (i) the W atoms are independently selected from the group consisting of O and S; (ii) the R 1 group is an alkylene group (e.g., linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkylene group joins the two W atoms at its terminal ends or at an intermediate location of its chain); (iii) the X atom is selected from the group consisting of Cl, F, Br, I; (iv) the Y atom coordinated to the boron atom (B) is selected from the group consisting of N and P; and (v) the R 2 groups are independently selected from the group consisting of an alkyl group and an aryl group (e.g., same or different groups for each of the R 2 groups; linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl; aryl or heteroaryl (e.g., N, O, S-containing) groups with 4, 5, or 6 carbon atoms such as phenyl).
[0006] In another aspect, the disclosure relates to a method for forming the boron compound of Formula I, the method comprising: (a) reacting at least one of an alkane diol and an alkane dithiol with a boron trihalide to form a product (e.g., a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) diol or dithiol with 2, 3, 4, 5, or 6 carbon atoms and at least 2 hydroxy groups or at least 2 thiol groups such as ethylene glycol or 1,2-ethanedithiol; the product is a dialkoxyboron halide (when using a diol) or a sulfur-equivalent (when using a dithiol); the three halogen atoms of the boron trihalide can be the same or different); and (b) reacting the product of part (a) with at least one of a tri(alkyl and/or aryl) amine and a tri(alkyl and/or aryl) phosphine to form the boron compound according to Formula I (e.g., such as trimethyl amine and triphenylphosphine; the alkyl and aryl groups of the amine and phosphine can be as described in Formula I as R 2 group alternatives). In a refinement, the alkane diol is used and comprises ethylene glycol. In a refinement, the boron trihalide comprises boron trichloride. In a refinement, the amine comprises trimethyl amine.
[0007] In another aspect, the disclosure relates to a diboron compound (e.g., in pure or substantially pure form (such as at least 90 wt. %, 95 wt. %, 98 wt. %, or 99 wt. % pure), or in admixture with other components) having a structure according to the following Formula II:
[0000]
[0000] wherein: (i) the W atoms are independently selected from the group consisting of O and S; (ii) the R 1 groups are the same or different alkylene groups (e.g., linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkyl group joins the two W atoms at its terminal ends or at an intermediate location of its chain); (iii) the Y atoms coordinated to the boron atoms (B) are independently selected from the group consisting of N and P; and (iv) the R 2 groups are independently selected from the group consisting of an alkyl group and an aryl group (e.g., same or different groups each of the R 2 groups, linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl; aryl or heteroaryl (e.g., N, O, S-containing) groups with 4, 5, or 6 carbon atoms such as phenyl).
[0008] In another aspect, the disclosure relates to a method for forming a diboron compound, the method comprising: (a) reacting the boron compound of Formula I with a metal to form a diboron compound (e.g., diboron compound of Formula II; metal can be an alkali metal such as Na or K, an alkali earth metal, or other metal to additionally form a metal halide salt byproduct in addition to the diboron compound of Formula II; the metal can be combined with silica or other delivery vehicle for the metal). In a refinement, the metal comprises sodium optionally in combination with silica. In a refinement, the method further comprises forming the boron compound of Formula I according to any of the foregoing methods.
[0009] In another aspect, the disclosure relates to a method for forming a tetraalkoxy diboron compound, the method comprising: (a) reacting the diboron compound of Formula II with one or more alkanols having at least one hydroxy group to form the tetraalkoxy diboron compound (e.g., a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) diol with 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 2 hydroxy groups such as pinacol; a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) monoalcohol with 1, 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 1 hydroxy group such as methanol). In a refinement, the one or more alkanols comprises pinacol and the tetraalkoxy diboron compound comprises bis(pinacolato)diboron (B 2 pin 2 ). In a refinement, an alkane diol and/or a tri(alkyl and/or aryl) amine as above are further formed as reaction products in part (a) (e.g., where such additional reaction products can be recovered/separated from the tetraalkoxy diboron compound product and/or recycled as reactants for forming the boron compound). In a refinement, the method further comprises forming the diboron compound of Formula II according to any of the foregoing methods (e.g., in a complete process as illustrated in the top pathway of Scheme 3, with or without removal and recycle of byproducts as an initial reactant).
[0010] In another aspect, the disclosure relates to boron compound (e.g., in pure or substantially pure form (such as at least 90 wt. %, 95 wt. %, 98 wt. %, or 99 wt. % pure), or in admixture with other components) having a structure according to the following Formula III:
[0000]
[0000] wherein: (i) the W atoms are independently selected from the group consisting of 0 and S; (ii) the E group coordinated to the boron atom (B) is selected from the group consisting of an O atom, an S atom, an alkyl amino group, an aryl amino group, an alkyl phosphino group, and an aryl phosphino group (e.g., an amino or phosphino group with a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) group with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl, or an aryl or heteroaryl (e.g., N, O, S-containing) group with 4, 5, or 6 carbon atoms such as phenyl); (iii) the R 1 groups are the same or different alkylene groups (e.g., same or different linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkylene group joins the W atom and E group at its terminal ends or at an intermediate location of its chain); and (iv) the X atom is selected from the group consisting of Cl, F, Br, I.
[0011] In another aspect, the disclosure relates to a method for forming the boron compound of Formula III, the method comprising: (a) reacting a silane compound according to the following Formula IIIA with a boron trihalide to form the boron compound of Formula III (e.g., a boron trihalide where the three halogen atoms are the same or different):
[0000] (R 3 ) 3 Si—W—R 1 -E-R 1 —W—Si(R 3 ) 3 (IIIA)
[0000] wherein: (i) the W atoms are independently selected from the group consisting of O and S; (ii) the E group is selected from the group consisting of an O atom, an S atom, an alkyl amino group, an aryl amino group, an alkyl phosphino group, and an aryl phosphino group (e.g., an amino or phosphino group with a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) group with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl, or an aryl or heteroaryl (e.g., N, O, S-containing) group with 4, 5, or 6 carbon atoms such as phenyl); (iii) the R 1 groups are the same or different alkylene groups joining the W atoms and the E group (e.g., same or different linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkylene group joins the W atom and E group at its terminal ends or at an intermediate location of its chain); and (iv) the R 2 groups are independently selected from the group consisting of an alkyl group and an aryl group (e.g., linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl; aryl or heteroaryl (e.g., N, O, S-containing) groups with 4, 5, or 6 carbon atoms such as phenyl). In a refinement, the E group is an oxygen atom (O). In a refinement, the E group is a methylamino group (NMe). In a refinement, the boron trihalide comprises boron trichloride. In a refinement, part (a) further comprises forming a tri(alkyl and/or aryl)silyl halide (e.g., where such additional reaction product can be recovered/separated from the boron compound product and/or recycled as a reactant for forming the silane compound of Formula IIIA).
[0012] In another aspect, the disclosure relates to a diboron compound (e.g., in pure or substantially pure form (such as at least 90 wt. %, 95 wt. %, 98 wt. %, or 99 wt. % pure), or in admixture with other components) having a structure according to the following Formula IV:
[0000]
[0000] wherein: (i) the W atoms are independently selected from the group consisting of 0 and S; (ii) the E groups coordinated to the boron atom (B) are independently selected from the group consisting of an O atom, an S atom, an alkyl amino group, an aryl amino group, an alkyl phosphino group, and an aryl phosphino group (e.g., an amino or phosphino group with a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) group with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl, or an aryl or heteroaryl (e.g., N, O, S-containing) group with 4, 5, or 6 carbon atoms such as phenyl); and (iii) the R 1 groups are the same or different alkylene groups (e.g., same or different linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkylene group joins the W atom and E group at its terminal ends or at an intermediate location of its chain).
[0013] In another aspect, the disclosure relates to method for forming a diboron compound, the method comprising: (a) reacting the boron compound of Formula III with a metal to form the diboron compound (e.g., an alkali metal such as Na or K, an alkali earth metal, or other metal to additionally form a metal halide salt byproduct in addition to the diboron compound; the metal can be combined with silica or other delivery vehicle for the metal). In a refinement, the metal comprises sodium optionally in combination with silica. In a refinement, the method comprises forming the boron compound of Formula III according to any of the foregoing disclosed methods.
[0014] In another aspect, the disclosure relates to a method for forming a tetraalkoxy diboron compound, the method comprising: (a) reacting the diboron compound of Formula IV with one or more alkanols having at least one hydroxy group to form the tetraalkoxy diboron compound (e.g., a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) diol with 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 2 hydroxy groups such as pinacol; a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) monoalcohol with 1, 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 1 hydroxy group such as methanol). In a refinement, the one or more alkanols comprises pinacol and the tetraalkoxy diboron compound comprises bis(pinacolato)diboron (B 2 pin 2 ). In a refinement, a diol analog of the compound according to Formula IIIA as is further formed as a reaction product in part (a) (e.g., where such additional reaction products can be recovered/separated from the tetraalkoxy diboron compound product and/or recycled as reactants for forming the compound according to Formula IIIA). In a refinement, the method further comprises forming the diboron compound of Formula IV according to the method of any of the foregoing embodiments (e.g., in a complete process as illustrated in the bottom pathway of Scheme 3, with or without removal and recycle of byproducts as an initial reactant).
[0015] In another aspect, the method for forming a diboron compound, the method comprising: (a) reacting a 4-coordinate boron compound with a metal (e.g., an alkali metal such as Na or K, an alkali earth metal, or other metal to additionally form a metal halide salt byproduct; the metal can be combined with silica or other delivery vehicle for the metal) under suitable conditions to form a 4-coordinate diboron compound, wherein: (i) the 4-coordinate boron compound comprises (A) a boron atom, (B) one halogen atom (e.g., F, Cl, Br, I) covalently bonded to the boron atom, (C) two same or different heteroatoms selected from the group consisting of N, O, P, and S covalently bonded to the boron atom, and (D) one heteroatom selected from the group consisting of N, O, P, and S coordinately covalently bonded to the boron atom (e.g., where the three heteroatoms covalently bonded or coordinately covalently bonded to the boron atom can be the same or different from each other, and/or the three heteroatoms can be bonded to any other suitable (hetero)alkyl and/or (hetero)aryl groups are described above); and, (ii) the 4-coordinate diboron compound comprises an adduct of two 4-coordinate boron compound molecules joined by a B—B covalent bond after elimination of their halogen atoms (e.g., each B atom having 3 covalent bonds and 1 coordinate covalent bond as above with each B-halogen covalent bond replaced by the mutual B—B covalent bond). In a refinement, the method further comprises (b) reacting the 4-coordinate diboron compound with one or more alkanols having at least one hydroxy group to form a tetraalkoxy diboron compound (e.g., a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) diol with 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 2 hydroxy groups such as pinacol; a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) monoalcohol with 1, 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 1 hydroxy group such as methanol).
[0016] While the disclosed compounds, methods and compositions are susceptible of embodiments in various forms, specific embodiments of the disclosure are illustrated (and will hereafter be described) with the understanding that the disclosure is intended to be illustrative, and is not intended to limit the claims to the specific embodiments described and illustrated herein.
DETAILED DESCRIPTION
[0017] A current synthesis of the tetraalkoxydiboron reagent B 2 pin 2 (bis(pinacolato)diboron, where “pin” represents the reaction product of pinacol with boron as illustrated) is outlined in Scheme 1. While BCl 3 is a cheap source of boron, the direct route to B 2 pin 2 from ClBpin (1, Scheme 1) fails because the product, which contains 3-coordinate boron atoms, also reacts with Na. While related compounds have been reduced to make B—B bonds, these reactions require Na/Hg amalgams for success. The large volumes of mercury that would be required produce diboron compounds on industrial scales make this route infeasible.
[0000]
[0018] The current route to B 2 pin 2 requires preparation of boron nitrogen compound 2 from BCl 3 and dimethylamine. Compound 2 is then reduced to form boron-boron bonded compound 3. Because compound 3 is unreactive, it must be converted to B 2 pin 2 in a reaction with pinacol and 8 equivalents of hydrochloric acid. The 4-step process for preparing B 2 pin 2 from BCl 3 generates 8 equivalents of NH 2 Me 2 Cl waste for every molecule of B 2 pin 2 produced. Each step requires careful purification of products, and the toxic amine waste stream must be remediated. Under best practices, the yields of B 2 pin 2 are limited to about 30%.
[0000]
[0019] The present disclosure uses dialkoxyboron halides that are stabilized by nitrogen or oxygen donors (Scheme 3, compounds 4-6). Boron-boron bond formation is accomplished by reduction with an alkali metal or alkali metal-silica such as Na or Na-silica, a safe source of Na with improved chemical reactivity. Because the boron atoms in compounds 7-9 are four-coordinate, they will be unreactive towards Na, and unwanted side reactions will be avoided. Compounds 7-9 can be converted to B 2 pin 2 in straightforward fashion. This also will allow other diboron diolate (or alkanolate) reagents to be formed (e.g., by reacting compounds 7-9 or similar analogs with other alkyl or aryl alcohols, diols, triols, or higher polyols other than pinacol as illustrated). The sequence in Scheme 3 uses intermediates that are crystalline solids, which simplifies purifications. Intermediates 5 and 6 are prepared from cheap diols that can be recycled. Lastly, the route in Scheme 3 minimizes, or eliminates, the generation of ammonium salts, which will significantly reduce waste disposal costs.
[0000]
[0020] Various aspects of the disclosure are provided by the following numbered paragraphs.
[0021] 1. A boron compound (e.g., in pure or substantially pure form (such as at least 90 wt. %, 95 wt. %, 98 wt. %, or 99 wt. % pure), or in admixture with other components) having a structure according to the following Formula 1:
[0000]
[0000] wherein: (i) either or both of the oxygen atoms (O) in Formula 1 may be replaced with sulfur (S) atoms; (ii) the O 2 ethylene group joining the two oxygen atoms (O) in Formula 1 alternatively may be replaced with an alkyl group (e.g., linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkyl group joins the two oxygen atoms at its terminal ends or at an intermediate location of its chain); (iii) the chlorine atom (Cl) in Formula 1 may be replaced with a different halogen (e.g., F, Br, I); (iv) the nitrogen atom (N) coordinated to the boron atom (B) in Formula 1 may be replaced with a phosphorous (P) atom; and (v) any or all of the methyl groups (Me) in Formula 1 may be replaced with an alkyl group or an aryl group, which may be the same or different (e.g., linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl; aryl or heteroaryl (e.g., N, O, S-containing) groups with 4, 5, or 6 carbon atoms such as phenyl).
[0022] 2. method for forming the boron compound of paragraph 1, the method comprising: (a) reacting an alkane diol with a boron trihalide to form a dialkoxyboron halide (e.g., a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) diol with 2, 3, 4, 5, or 6 carbon atoms and at least 2 hydroxy groups such as ethylene glycol; a boron trihalide where the three halogen atoms are the same or different); and (b) reacting the dialkoxyboron halide with a tri(alkyl and/or aryl) amine to form the boron compound of paragraph 1 (e.g., where the alkyl and aryl groups of the amine can be as described in paragraph 1 as methyl group alternatives).
[0023] 3. The method of paragraph 2, wherein the alkane diol comprises ethylene glycol.
[0024] 4. The method of paragraph 2, wherein the boron trihalide comprises boron trichloride.
[0025] 5. The method of paragraph 2, wherein the amine comprises trimethyl amine.
[0026] 6. The method of paragraph 2, wherein the alkane diol alternatively may be replaced by or combined with an alkane dithiol (e.g., a thiol analog of the various alkane diols, such as 1,2-ethanedithiol).
[0027] 7. The method of paragraph 2, wherein the tri(alkyl and/or aryl) amine alternatively may be replaced by or combined with a tri(alkyl and/or aryl) phosphine (e.g., a phosphine analog of the various amines, such as triphenylphosphine).
[0028] 8. A diboron compound (e.g., in pure or substantially pure form (such as at least 90 wt. %, 95 wt. %, 98 wt. %, or 99 wt. % pure), or in admixture with other components) having a structure according to the following Formula 2:
[0000]
[0000] wherein: (i) any or all of the oxygen atoms (O) in Formula 2 may be replaced with sulfur (S) atoms; (ii) either or both of the O 2 ethylene groups joining two oxygen atoms (O) in Formula 2 alternatively may be replaced with an alkyl group (e.g., linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkyl group joins the two oxygen atoms at its terminal ends or at an intermediate location of its chain); (iii) either or both of the nitrogen atoms (N) coordinated to the boron atom (B) in Formula 2 may be replaced with a phosphorous (P) atom; and (iv) any or all of the methyl groups (Me) in Formula 2 may be replaced with an alkyl group or an aryl group, which may be the same or different (e.g., linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl; aryl or heteroaryl (e.g., N, O, S-containing) groups with 4, 5, or 6 carbon atoms such as phenyl).
[0029] 9. A method for forming the diboron compound of paragraph 8, the method comprising: (a) reacting the boron compound of paragraph 1 with a metal to form the diboron compound of paragraph 8 (e.g., an alkali metal such as Na or K, an alkali earth metal, or other metal to additionally form a metal halide salt byproduct in addition to the diboron compound of paragraph 8; the metal can be combined with silica or other delivery vehicle for the metal).
[0030] 10. The method of paragraph 9, wherein the metal comprises sodium optionally in combination with silica.
[0031] 11. The method of paragraph 9, further comprising forming the boron compound of paragraph 1 according to the method of any of paragraphs 2 to 7.
[0032] 12. A method for forming a tetraalkoxy diboron compound, the method comprising: (a) reacting the diboron compound of paragraph 8 with one or more alkanols having at least one hydroxy group to form the tetraalkoxy diboron compound (e.g., a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) diol with 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 2 hydroxy groups such as pinacol; a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) monoalcohol with 1, 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 1 hydroxy group such as methanol).
[0033] 13. The method of paragraph 12, wherein the one or more alkanols comprises pinacol and the tetraalkoxy diboron compound comprises bis(pinacolato)diboron (B 2 pin 2 ).
[0034] 14. The method of paragraph 12, wherein an alkane diol and/or a tri(alkyl and/or aryl) amine as recited in paragraph 2 are further formed as reaction products in part (a) (e.g., where such additional reaction products can be recovered/separated from the tetraalkoxy diboron compound product and/or recycled as reactants for forming the boron compound).
[0035] 15. The method of paragraph 12, further comprising forming the diboron compound of paragraph 8 according to the method of any of paragraphs 9 to 11 (e.g., in a complete process as illustrated in the top pathway of Scheme 3, with or without removal and recycle of byproducts as an initial reactant).
[0036] 16. A boron compound (e.g., in pure or substantially pure form (such as at least 90 wt. %, 95 wt. %, 98 wt. %, or 99 wt. % pure), or in admixture with other components) having a structure according to the following Formula 3:
[0000]
[0000] wherein: (i) either or both of the oxygen atoms (O) in Formula 3 may be replaced with sulfur (S) atoms; (ii) the E group coordinated to the boron atom (B) in Formula 3 may be an oxygen atom (0), a sulfur atom (S), an alkyl or aryl amino group, or an alkyl or aryl phosphino group (e.g., an amino or phosphino group with a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) group with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl, or an aryl or heteroaryl (e.g., N, O, S-containing) group with 4, 5, or 6 carbon atoms such as phenyl); (iii) either or both of the O 2 ethylene groups joining the oxygen atoms (O) and E group in Formula 3 alternatively may be replaced with an alkyl group (e.g., same or different linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkyl group joins the oxygen atom and E group at its terminal ends or at an intermediate location of its chain); and (iv) the X group in Formula 3 is a halogen (e.g., F, Cl, Br, I).
[0037] 17. A method for forming the boron compound of paragraph 16, the method comprising: (a) reacting a silane compound according to the following Formula 3A with a boron trihalide to form the boron compound of paragraph 16 (e.g., a boron trihalide where the three halogen atoms are the same or different):
[0000]
[0000] wherein: (i) either or both of the oxygen atoms (O) in Formula 3A may be replaced with sulfur (S) atoms; (ii) the E group in Formula 3A may be an oxygen atom (O), a sulfur atom (S), an alkyl or aryl amino group, or an alkyl or aryl phosphino group (e.g., an amino or phosphino group with a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) group with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl, or an aryl or heteroaryl (e.g., N, O, S-containing) group with 4, 5, or 6 carbon atoms such as phenyl); (iii) the O 2 ethylene groups joining the oxygen atoms (O) and E group in Formula 3A alternatively may be replaced with an alkyl group (e.g., same or different linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkyl group joins the oxygen atom and E group at its terminal ends or at an intermediate location of its chain); and (iv) any or all of the methyl groups (Me) in Formula 3A may be replaced with an alkyl group or an aryl group, which may be the same or different (e.g., linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl; aryl or heteroaryl (e.g., N, O, S-containing) groups with 4, 5, or 6 carbon atoms such as phenyl).
[0038] 18. The method of paragraph 17, wherein the E group is an oxygen atom (O).
[0039] 19. The method of paragraph 17, wherein the E group is a methylamino group (NMe).
[0040] 20. The method of paragraph 17, wherein the boron trihalide comprises boron trichloride.
[0041] 21. The method of paragraph 17, wherein part (a) further comprises forming a tri(alkyl and/or aryl)silyl halide (e.g., where such additional reaction product can be recovered/separated from the boron compound product and/or recycled as a reactant for forming the silane compound of Formula 3A).
[0042] 22. A diboron compound (e.g., in pure or substantially pure form (such as at least 90 wt. %, 95 wt. %, 98 wt. %, or 99 wt. % pure), or in admixture with other components) having a structure according to the following Formula 4:
[0000]
[0000] wherein: (i) any or all of the oxygen atoms (O) in Formula 4 may be replaced with sulfur (S) atoms; (ii) either or both of the E groups coordinated to the boron atom (B) in Formula 4 may be an oxygen atom (O), a sulfur atom (S), an alkyl or aryl amino group, or an alkyl or aryl phosphino group (e.g., an amino or phosphino group with a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) group with 1, 2, 3, 4, 5, or 6 carbon atoms such as methyl, ethyl, propyl, butyl, pentyl, or hexyl, or an aryl or heteroaryl (e.g., N, O, S-containing) group with 4, 5, or 6 carbon atoms such as phenyl); and (iii) any or all of the O 2 ethylene groups joining the oxygen atoms (O) and E group in Formula 4 alternatively may be replaced with an alkyl group (e.g., same or different linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) groups with 2, 3, 4, 5, or 6 carbon atoms such as an ethylene or propylene group, for example where the (hetero)alkyl group joins the oxygen atom and E group at its terminal ends or at an intermediate location of its chain).
[0043] 23. A method for forming the diboron compound of paragraph 22, the method comprising: (a) reacting the boron compound of paragraph 16 with a metal to form the diboron compound of paragraph 22 (e.g., an alkali metal such as Na or K, an alkali earth metal, or other metal to additionally form a metal halide salt byproduct in addition to the diboron compound of paragraph 22; the metal can be combined with silica or other delivery vehicle for the metal).
[0044] 24. The method of paragraph 23, wherein the metal comprises sodium optionally in combination with silica.
[0045] 25. The method of paragraph 23, further comprising forming the boron compound of paragraph 16 according to the method of any of paragraphs 17 to 21.
[0046] 26. A method for forming a tetraalkoxy diboron compound, the method comprising: (a) reacting the diboron compound of paragraph 22 with one or more alkanols having at least one hydroxy group to form the tetraalkoxy diboron compound (e.g., a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) diol with 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 2 hydroxy groups such as pinacol; a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) monoalcohol with 1, 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 1 hydroxy group such as methanol).
[0047] 27. The method of paragraph 26, wherein the one or more alkanols comprises pinacol and the tetraalkoxy diboron compound comprises bis(pinacolato)diboron (B 2 pin 2 ).
[0048] 28. The method of paragraph 26, wherein a diol analog of the compound according to Formula 3A as recited in paragraph 17 is further formed as a reaction product in part (a) (e.g., where such additional reaction products can be recovered/separated from the tetraalkoxy diboron compound product and/or recycled as reactants for forming the compound according to Formula 3A).
[0049] 29. The method of paragraph 26, further comprising forming the diboron compound of paragraph 16 according to the method of any of paragraphs to 17 to 21 (e.g., in a complete process as illustrated in the bottom pathway of Scheme 3, with or without removal and recycle of byproducts as an initial reactant).
[0050] 30. A method for forming a diboron compound, the method comprising: (a) reacting a 4-coordinate boron compound with a metal (e.g., an alkali metal such as Na or K, an alkali earth metal, or other metal to additionally form a metal halide salt byproduct; the metal can be combined with silica or other delivery vehicle for the metal) under suitable conditions to form a 4-coordinate diboron compound, wherein: (i) the 4-coordinate boron compound comprises (A) a boron atom, (B) one halogen atom (e.g., F, Cl, Br, I) covalently bonded to the boron atom, (C) two same or different heteroatoms selected from the group consisting of N, O, P, and S covalently bonded to the boron atom, and (D) one heteroatom selected from the group consisting of N, O, P, and S coordinately covalently bonded to the boron atom (e.g., where the three heteroatoms covalently bonded or coordinately covalently bonded to the boron atom can be the same or different from each other, and/or the three heteroatoms can be bonded to any other suitable (hetero)alkyl and/or (hetero)aryl groups are described above); and, (ii) the 4-coordinate diboron compound comprises an adduct of two 4-coordinate boron compound molecules joined by a B—B covalent bond after elimination of their halogen atoms (e.g., each B atom having 3 covalent bonds and 1 coordinate covalent bond as above with each B-halogen covalent bond replaced by the mutual B—B covalent bond).
[0051] 31. The method of paragraph 30, further comprising (b) reacting the 4-coordinate diboron compound with one or more alkanols having at least one hydroxy group to form a tetraalkoxy diboron compound (e.g., a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) diol with 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 2 hydroxy groups such as pinacol; a linear or branched alkyl or heteroalkyl (e.g., N, O, S-containing) monoalcohol with 1, 2, 3, 4, 5, 6 and/or up to 10 carbon atoms and 1 hydroxy group such as methanol).
[0052] Because other modifications and changes varied to fit particular operating requirements and environments will be apparent to those skilled in the art, the disclosure is not considered limited to the example chosen for purposes of illustration, and covers all changes and modifications which do not constitute departures from the true spirit and scope of this disclosure.
[0053] Accordingly, the foregoing description is given for clearness of understanding only, and no unnecessary limitations should be understood therefrom, as modifications within the scope of the disclosure may be apparent to those having ordinary skill in the art.
[0054] All patents, patent applications, government publications, government regulations, and literature references cited in this specification are hereby incorporated herein by reference in their entirety. In case of conflict, the present description, including definitions, will control.
[0055] Throughout the specification, where the compounds, compositions, methods, and processes are described as including components, steps, or materials, it is contemplated that the compositions, processes, or apparatus can also comprise, consist essentially of, or consist of, any combination of the recited components or materials, unless described otherwise. Component concentrations can be expressed in terms of weight concentrations, unless specifically indicated otherwise. Combinations of components are contemplated to include homogeneous and/or heterogeneous mixtures, as would be understood by a person of ordinary skill in the art in view of the foregoing disclosure.
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The disclosure is directed to diboron compounds, related methods of making, and related intermediate boron and diboron compounds used to make the same. The diboron compounds can be used as reagents to prepare chemical intermediates that are used in pharmaceutical, agrochemical, and specialty electronics industries. The disclosed processes and compounds provide simplified synthetic paths that significantly reduce steps, improve scalability, and minimize costs for producing the diboron reagents.
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[0001] This application is a divisional of U.S. Ser. No. 10/984,216 filed Nov. 9, 2004.
[0002] The U.S. Government may have certain rights in this invention in accordance with Contract Number N00019-02-C-3003 awarded by the United States Navy.
BACKGROUND OF THE INVENTION
[0003] This invention relates generally to a cooling passage for an airfoil. More particularly, this invention relates to a core assembly for the formation of cooling passages for an airfoil.
[0004] A gas turbine engine typically includes a plurality of turbine blades that transform energy from a mainstream of combustion gasses into mechanical energy that rotates and drives a compressor. Each of the turbine blades includes an airfoil section that generates the rotational energy desired to drive the compressor from the flow of main combustion gasses.
[0005] The turbine blade assembly is exposed to the hot combustion gasses exhausted from the combustor of the gas turbine engine. The temperature of the combustion gasses exhausted through and over the turbine blade assemblies can decrease the useful life of a turbine blade assembly. It is for this reason that each turbine blade is provided with a plurality of cooling air passages. Cooling air is fed through each of the turbine blades and exhausted out film holes on the surface of the turbine blade. The position of the film holes on the turbine blade creates a layer of cooling air over the surfaces of the turbine blade. The cooling air insulates the turbine blade from the hot combustion gasses. By insulating the turbine blade from exposure to the hot combustion gasses the turbine blade reliability and useful life is greatly extended.
[0006] Typically, the cooling passages within a turbine blade are formed by a ceramic core that is provided with and surrounded with molted material that is used to form the turbine blade. Once the molten material utilized to form the turbine blade is solidified the core material is removed. Removing the core material leaves the desired cooling air passages along with the desired configuration of film cooling holes.
[0007] As appreciated, each turbine blade assembly represents a dead end or an end of a cooling airflow path. This is so because cooling air flowing from an inner side or platform of the turbine blade flow radially outward to a tip of the turbine blade. The tip of the turbine blade is closed off forming the end of the cooling air passage. Accordingly, the only exit for cooling air through the turbine blade is through the plurality of the film cooling holes disposed about and on the surface of the turbine blade. The configuration and quantity of the film holes for cooling the turbine blade is determined to produce a desired flow rate of cooling air.
[0008] The shape of the turbine blade varies throughout the cross section from a leading edge of the turbine blade to a trailing edge. The leading edge is most often much thicker than the trailing edge. However, the cooling needs in the trailing edge are often greater than those in the leading edge and therefore require cooling passages arranged within a close proximity to the trailing edge. As appreciated, cooling passages within the thinner edge section are much smaller. The smaller cooling passages require smaller core assemblies to form those cooling passages. As the size of the core assemblies are reduced the susceptibility to damage during the molding operation increases. The smaller core assemblies required the desired cooling passage in the thinner sections of the turbine blade and are more susceptible to damage during manufacturing.
[0009] Accordingly, it is desirable to develop a core assembly that is robust enough to provide for reliable manufacturing process results while still providing for the formation of the smaller cooling air passages in the thinner sections of the turbine blade assembly.
[0010] Another concern in the design and configuration of cooling air passages is the direction of cooling air on an inner side of the cooling passage. The cooling passage typically receives air from a main core section. The main core section of the turbine blade is in turn in communication with a cooling air source. The cooling air passage therefore includes an inner surface that is adjacent the main core and an outer surface that is adjacent an exterior surface of the turbine blade. Impingement holes within the cooling air passages communicate air from the main core into the cooling air passage and against the outer surface.
[0011] Accordingly, it is desirable to develop a core assembly to form a cooling air passage within a turbine blade assembly that is both reliable during manufacturing processes and that provides the desirable cooling air flow properties to maximize to heat transfer capabilities applications.
SUMMARY OF THE INVENTION
[0012] A sample embodiment of this invention includes a turbine blade assembly having cooling passages where each of the impingement holes is isolated from at least some of the other impingement holes. The isolation of the impingement holes within the cooling passages provides for the direction of cooling airflow to specific desired areas. Further, the core assembly utilized for forming the cooling air passages provides a series of structures that strengthen and improve manufacturability.
[0013] An example turbine blade assembly of this invention is formed with a cooling air passage that is in communication with a main core. The main core is in turn in communication with cooling air from other systems. The cooling passage is formed through the use of a unique core assembly that includes a plurality of impingement holes that are isolated from each other. Isolating each of the impingement holes from at least some of the other impingement holes prevents cross flow between impingement holes to improve cooling air flow against an outer surface of the cooling passage.
[0014] The core assembly provides the configuration of the cooling passages and includes impingement structures for forming the impingement openings. Each of the impingement structures is isolated from at least some of the other impingement structures by separation structures. The separation structures form the channels within the cooling passages that isolate the impingement openings. Each of the channels formed by the core assembly is in communication with expanded chambers at a side of the cooling passage. Within the expanded chamber are film structures that are provided for creating the film openings between the cooling air passage and an exterior surface of the turbine blade assembly.
[0015] Accordingly, the turbine blade assembly of this invention includes cooling air passages that provide desirable cooling characteristics for the turbine blade.
[0016] These and other features of the present invention can be best understood from the following specification and drawings, the following of which is a brief description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1A is a side view of a turbine blade assembly according to this invention.
[0018] FIG. 1B is a cross-section view of a portion of the turbine blade assembly.
[0019] FIG. 2 is a prospective view of an airfoil assembly.
[0020] FIG. 3 is a prospective view of a portion of a core assembly according to this invention.
[0021] FIG. 4 is a prospective view of an airfoil assembly according to this invention with a portion broken away to illustrate the cooling air passage.
[0022] FIG. 5 is a prospective view of a core assembly according to this invention.
[0023] FIG. 6 is a view of an exterior surface of a cooling passage.
[0024] FIG. 7 is a plan view of a side of a core assembly according to this invention.
[0025] FIG. 8 is a plan view of the other side of a core assembly as shown in FIG. 7 .
[0026] FIG. 9 is a view of one side of a core assembly according to this invention.
[0027] FIG. 10 is a view of an opposite side of a core assembly illustrated in FIG. 9 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0028] Referring to FIGS. 1A and 1B , turbine blade assembly 10 includes an airfoil section 12 , a root section 14 , and a platform section 16 . The root section 14 extends into a hub portion (not shown) as is known in the art. The root section 14 extends to the platform section 16 . The airfoil 12 extends upwardly from the platform section 16 . Turbine airfoil section 12 extends from the platform section 16 to a tip 18 . The turbine blade assembly 10 includes a leading edge 20 and a trailing edge 22 . Between the leading edge 20 and the trailing edge 22 is the exterior surface 24 . The exterior surface 24 is shaped to provide the desired transition or conversion of gas stream flow to rotational mechanical energy. As should be understood, the turbine blade assembly 10 as is shown in FIG. 1A is as is known to a worker skilled in the art. A worker skilled in the art with the benefit of this disclosure would understand that other airfoil configurations utilized in different applications would benefit from the disclosures and cooling passages of this invention.
[0029] The turbine blade assembly 10 includes a cooling passage 30 . The cooling passage 30 is disposed within the turbine blade assembly 10 . Cooling air enters the turbine blade assembly 10 through passages 26 within the root section 14 . Cooling air enters through the passages 26 into a main core 28 ( FIG. 1B ). Main core 28 is a hollow portion within the interior of the turbine blade assembly 10 . Cooling air communicated through the passages 26 and into the main core 28 enters cooling passages 30 disposed within the turbine blade assembly 10 . Cooling air enters the cooling passages 30 from the main core 28 through a plurality of impingement opening 32 .
[0030] Cooling airflow from the impingement openings 32 flows toward expansion chambers 42 disposed opposite the impingement opening 32 . Cooling airflow then proceeds through the walls of the turbine blade assembly 10 through film openings 34 . Cooling air exiting the cooling passage 30 through the film openings 34 flows over the exterior surface 24 of the turbine blade assembly 10 to provide a cooling and insulating layer of air.
[0031] The turbine blade assembly 10 of this invention includes the cooling passage 30 . Each of the cooling passages 30 includes the impingement openings 32 . The impingement openings 32 are isolated from each other by channels 36 . The channels 36 are formed by a series of separating structures 38 . Separation and isolation of each of the impingement openings 32 provides for the separation of cooling flow that is impinged upon an outer surface of the cooling passage 30 . Further, isolation of adjacent impingement opening 32 prevents and reduces cross flow problems encountered with typical conventional prior art impingement opening designs. The flow from the impingement openings 32 passes through the channel 36 to the plurality of film holes 34 . Film holes 34 are in communication with the expanded chamber 42 . The expanded chamber 42 provides a portion of the cooling passage for the accumulation of cooling air that is to be communicated to the film openings 34 . The accumulation of cooling air within the expanded chamber 42 reduces problems associated with back wall strikes corresponding with impingement openings 32 .
[0032] Referring to FIG. 2 , a prospective view of the airfoil 12 is shown to illustrate the configuration of the main core 28 . The main core 28 provides for communication of cooling air up through the central portion of the turbine blade assembly 10 and to communicate with cooling passages 30 . The specific shape and configuration of the turbine blade assembly and the airfoil 12 illustrated in FIG. 2 is as known. A worker with the benefit of the disclosure would understand that many different types of airfoil configurations will benefit from this the cooling passage configuration illustrated and described within this disclosure.
[0033] Referring to FIG. 3 , the cooling passage 30 is formed within the turbine blade assembly 10 through the use of core assembly 44 . The core assembly 44 provides for the formation of the various structures and configuration including openings, channels of the cooling passage during fabrication of the turbine blade assembly 10 . Conventionally, the turbine blade assembly 10 is fabricated through the use of a conventional molding process. The core assembly 44 can be fabricated from known core materials such as specially formulated ceramic and refractory metals. The core assembly 44 is placed within a mold and then surrounded by molten material that will comprise the turbine blade assembly 10 . Upon solidification of the material forming the turbine blade assembly 10 , the core assembly 44 is removed. Removal of the core assembly 44 is as known and can comprise various processes including leeching or oxidation process where a chemical are used to destroy and leech out the core assembly 44 . As appreciated, a worker versed in the art with the benefit of this disclosure would understand that the use of other molding process and materials as are known are within the contemplation and scope of this invention. The type of removal process that is utilized to remove the core 44 from the turbine blade assembly 10 will depend on various factors. These factors include the type of turbine blade material, the type of core material used and the specific configuration of the cooling air passage.
[0034] The core assembly 44 utilized to form intricate cooling air passages required to provide the desired cooling properties within the turbine blade assembly 10 . The core assembly 44 includes impingement structures 46 that extend and provide formation of the impingement openings 32 within a completed turbine assembly 10 . Core assembly 44 also includes separation structures 48 that form the channels and walls that are required for isolating each of the impingement openings 32 from at least another of the impingement openings 32 .
[0035] Referring to FIG. 4 , an airfoil 12 is shown with a portion of the surface removed to illustrate the specific features of the cooling air passage formed therein. The cooling air passage 30 includes the expanded chambers 42 on each side of the cooling air passage 30 . The cooling air passage 30 includes a lead edge side 50 and a trailing edge side 52 . Each side of the cooling air passage 30 includes an expansion chamber 42 . Adjacent impingement openings 32 communicate with an expansion chamber 42 disposed on an opposite side of the cooling air passage 30 . No two adjacent impingement openings communicate cooling air to a common expansion chamber 42 . In this way the specific cooling flow can be controlled and tailored to provide cooling to specific areas and features of the airfoil 12 .
[0036] Referring to FIG. 5 , an example core assembly 44 is shown and includes the impingement structures 46 utilized to form the impingement openings 32 within the airfoil 12 . The impingement openings 32 communicate cooling air from the main core 28 into the cooling passage 30 . The core assembly 44 also includes the separation structures 48 that utilize and provide for the separation of cooling air through each adjacent impingement opening 32 . The core assembly 44 includes a reverse structure from that which will be formed within the completed turbine blade airfoil 12 . The impingement structures 46 therefore are extensions that will extend through and provide the openings through the airfoil 12 to the main core 28 . The structure and space of the core assembly 44 provides for the open spaces within the completed airfoil 12 .
[0037] The core assembly 44 also includes a plurality of heat transfer enhancement features 60 . These heat transfer enhancement features 60 are formed in the core assembly 44 as openings such that within the completed cooling air passage 30 the heat transfer enhancement features 60 will form a plurality of ridges that extend upward within the various of the cooling air passage 30 . A worker with the benefit of this disclosure would understand that different shapes of the heat transfer enhancement features 60 other than the examples illustrated that disrupt or direct airflow are within the contemplation of this invention.
[0038] Referring to FIG. 6 , an outer side 56 is illustrated. The outer side 56 is cut away from the airfoil 12 illustrated in FIG. 4 . The outer side 56 is not typically sectioned as is shown in FIG. 6 but is an integral portion of the airfoil 12 . The outer side 56 is adjacent the exterior surface of the airfoil 12 . FIG. 4 illustrates an inner side 54 of the cooling passage 30 . The inner side is adjacent the main core 28 . It is for this reason that the ridges 62 are provided on the outer side 56 illustrated in FIG. 6 . As appreciated, thermal energy radiates along the exterior surface 24 .
[0039] The outer side 56 that is adjacent the exterior portion of the airfoil 12 is provided on which cooling air flow can most affect desired heat absorption and transfer. Airflow through the impingement openings 32 strikes the outer sides 56 immediately across from the impingement openings 32 . Airflow will then proceed as directed by the channels 36 towards the trailing edge or leading edge side towards the expansion chamber 42 . Through the channels 36 air will be controlled and tailored to create turbulent effects that increase heat transfer and absorption properties. Once air has reached the expansion chambers 42 it is accumulated and exhausted out the film holes 34 . Through the film holes 34 the air will then be exhausted into the main combustion gas stream. The example core assembly 44 is substantially straight. However, the core assembly 44 may include a curved shape to conform to an application specific airfoil shape.
[0040] Referring to FIG. 7 , a portion of the core assembly 44 is shown that provides for the formation of the outer side 56 of the cooling air passage 30 . The core assembly 44 includes the structures that form the channels 36 , film holes 34 , and separating structures 38 . The impingement structures 46 are illustrated in dashed lines to indicate that they do not extend outwardly from this side of the core 44 . Instead the impingement openings are formed from extensions or structures 46 that extend from an opposite side of the core. This side of the core assembly 44 produces these features within the outer side 56 of the cooling air passage 30 of the completed airfoil 12 . In this example core assembly 44 , each impingement structure 46 it opens into a separate channel 36 . Therefore each of the impingement openings 32 are isolated from any of the adjacent the impingement openings 32 . Within each of the channels are a plurality of the heat transfer enhancement structures 60 that will form the desired ridges and heat transfer ridges 62 within the completed channels 36 . The heat transfer structures 60 illustrated in FIG. 7 are cavities that receive material during the molding process to form the outwardly extended ridges.
[0041] Referring to FIG. 8 , an inner side of the core assembly 44 is shown and includes the impingement structures 46 . The separation structures 48 are shown in dashed lines to indicate that they would not extend from this side but would extend from the opposite side. Further, the other structures that would be formed on the outer side 56 from the inner side 54 are not shown for clarity purposes. However, as appreciated those features would extend outwardly from the opposite side and may also be represented by dashed lines in this view.
[0042] Referring to FIGS. 9 and 10 , another example core assembly 70 according to this invention, includes a plurality of impingement structures 46 disposed within separate channels 36 . In this core assembly 70 , three impingement structures 46 are disposed within each of the separation channel 36 . By providing several impingement openings within each chamber the specific air flow requirements and cooling airflow impingement on a specific area can be tailored to accommodate area specific heat transfer and absorption requirements. Although there are several impingement openings 46 disposed within each channel 36 . These are still isolated from at least one impingement opening is isolated from at least another impingement opening. Further, the impingement openings are all disposed about a centerline 40 .
[0043] Although each of the impingement openings 32 are disposed about a common centerline 40 they are still isolated from at least one other impingement opening. Although it is shown in the example core assembly 70 that the impingement openings and impingement structures 46 are disposed about a centerline 40 , other configurations and locations of impingement openings are within the contemplation of this invention. A worker versed in the art will understand that isolation of at least one impingement opening relative to another impingement opening provides the desired benefits of tailoring cooling in a cooling passage.
[0044] Referring to FIG. 10 , the core assembly 70 is shown on the side opposite that shown in FIG. 9 and illustrates the side of the core assembly 70 that would form the outer side 56 of the cooling air passage 30 . This side of the core assembly 70 illustrates the film structures 58 that would form the film holes 34 in the completed airfoil 12 . Further, heat transfer structures 60 are illustrated that would form the heat transfer ridges 64 in the completed cooling passage 30 . Further, as is shown, the impingement structures 46 are shown in dashed lines indicate their location relative to the features formed on the outer side 56 . As can be seen by FIG. 10 the separation structures 48 and the heat transfer structures 60 provide for the creation of a tailored cooling airflow from the impingement openings to the film openings.
[0045] Accordingly, the core assembly 44 and airfoil 12 of this invention provides for the tailoring and improvement of cooling air properties within a turbine blade assembly 10 . Further, the core assembly 44 includes a single core that can provide a plurality of individual channels desirable for separating airflow through each of the impingement hole openings. The isolation of the impingement openings provides improved airflow and tailoring capabilities for implementing and optimizing local cooling and flow characteristics within an airfoil.
[0046] Although a preferred embodiment of this invention has been disclosed, a worker of ordinary skill in this art would recognize that certain modifications would come within the scope of this invention. For that reason, the following claims should be studied to determine the true scope and content of this invention.
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A turbine blade airfoil assembly includes a cooling air passage. The cooling air passage includes a plurality of impingement openings that are isolated from at least one adjacent impingement opening. The cooling air passage is formed and cast within a turbine blade assembly through the use of a single core. The single core forms the features required to fabricate the various separate and isolated impingement openings. The isolation and combination of impingement openings provides for the augmentation of convection and film cooling and provide the flexibility to tailor airflow on an airfoil to optimize thermal performance of an airfoil.
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FIELD OF THE INVENTION
This invention relates generally to the field of waterproofing and sealing rigid structures. In particular, the invention relates to a method of waterproofing and sealing a rigid structural unit using a multilayered system by first coating the unit with a styrene polymeric film cast from an organic solvent and secondly by applying an overcoat or top coat on top of the film where the top coat contains a rubberized asphalt layer or a multi-layer system such as a waterproofing membrane.
BACKGROUND OF THE INVENTION
Masonry and concrete structures are porous and are susceptible to cracking due to distortion caused by movement of their foundation, vibration, and/or drying out subsequent to their construction. In addition, below grade structures are often subjected to hydrostatic pressure from ground water. Therefore, waterproofing and sealing below grade masonry and concrete structures have been major concerns for a number of years. Masonry and concrete structures have been coated with various tar-based and asphaltic compositions. These compositions are relatively inexpensive and can be applied year-round if heated to a pliable state. However, these compositions generally contain leachable components which can contaminate the surrounding soil. In addition, these compositions contain substantial amounts of organic materials which are attacked by soil- and water-borne microorganisms and have a short useful life before decomposition to form substantial pathways through the coatings.
The most difficult questions with respect to the need for waterproofing are related to intermittent hydrostatic pressure. Intermittent hydrostatic pressure has been defined as a varied pressure gradient of short duration that will act on a wall after rain showers, induced irrigations, and snow melt.
Since this condition exists in most buildings except in extremely dry climates or extremely well-drained soils, it can be inferred that waterproofing, not dampproofing, is required for the majority of basement walls.
Numerous synthetic coatings, such as acrylic, polyurethane and rubber-based or rubberized coatings, and more elaborate waterproofing/sealing systems based on polyvinyl and polyethylene sheeting have been developed to address the shortcomings of the tar-based and asphaltic compositions. Many of the coating compositions are aqueous emulsions or latexes of the polymeric resins. The resulting films generally are short-lived as they are subject to degradation caused by soil acids and microorganisms. These compositions have generally resulted in effective application systems only when applied under non-freezing conditions. To reduce attack on acrylic coatings, including rubberized acrylic, antifungal components are often included in the compositions. However, these components can leach into the soil and may be only temporarily effective.
Rubberized coatings generally provide fragile membranes which are easily damaged and ruptured during further work and backfilling around the masonry structures and may be easily oxidized. Rubberized acrylic, water-based coatings are not effective for application at below freezing temperatures, and can suffer from microorganism attack. Other rubberized coatings include rubberized asphalt which suffers from the inclusion of organic impurities which can be attacked and decomposed by microorganisms. In addition, the rubberized coatings cannot easily be applied by brush or roller.
Polyurethane compositions generally result in unstable coatings due to plasticizer migration and exposure to sunlight to result in brittle and friable coatings. Once applied, many polyurethanes continue to evolve formaldehyde vapors which are highly undesirable. These compositions are often foamed and applied as insulating coatings.
The waterproofing/sealing systems based on polyvinyl and polyethylene sheeting generally have open seams and generally require black mastics or metal fasteners such as nails, etc., to adhere the sheeting to the masonry surfaces. The sheets are usually UV-sensitive and can be susceptible to fungus, insect and rodent attack. In addition, the sheets are difficult to form around non-uniform surfaces, and the nails puncture the sheet and will puncture cement blocks to provide a direct water channel into the interior of the block wall.
Beyond the problems discussed above, the state of the art coating compositions are generally fragile, and they must be protected during backfilling of earth around the masonry structures. Without such protection, the sheets or coatings can be ruptured, torn, pulled down along vertical surfaces by the backfill, etc. Further, many of these coating systems require that the masonry structure be dry or contain only a trace of dampness which requires careful protection of the structure before application of the waterproofing/sealing system.
Recently crystallizing waterproofing products have become available from producers such as AKONA, BONDEX, THORO SEAL and Xypex Chemical Corporation. These compositions generally are powders which include Portland cement, silica sand and other active chemicals. The compositions are applied as a slurry in water to concrete surfaces, and they penetrate cracks and pores in concrete and other cementitious structures. When the compositions cure, they generally form crystalline structures within the pores and plug the cementitious surfaces. While these compositions are generally very effective, they require careful application to perform up to their designed specifications. Careful preparation of the surfaces and the use of two or more coats of slightly different layers are necessary to ensure complete waterproofing of the structure. Due to the labor intensive application, the compositions are costly to apply. Thus these systems are of rather limited use where very high performance is required to justify the cost.
Therefore, a new, low cost, waterproof sealant is needed for use in a majority of waterproofing applications which is durable and has a long effective life span. In addition, a new method of waterproofing and sealing subterranean masonry and concrete structures is needed which is useful year round, even in northern latitudes, and which can be applied to damp masonry and concrete surfaces.
Many of the above deficiencies in waterproofing and sealing rigid structural units were overcome by applying a liquid coating composition containing a styrene polymeric resin in an organic solvent to the structural unit. On drying a film having an average water vapor permeability of less than about 1×10 -2 perms/inch was formed. This is described in related co-pending application Ser. No. 08/258,562, now U.S. Pat. No. 5,482,737; Ser. No. 08/258,558, pending, and Ser. No. 08/315,884, now abandoned.
SUMMARY OF THE INVENTION
Elastomeric coatings when applied on concrete or masonry units alone often time fail because they are soft and easily deformed. The capillary action of water can push a coating with elastomeric properties off the surface to which it is applied. The effect of capillary action is called "bladdering". When bladdering occurs, water gets in direct contact with the very surface that was intended to be protected. Bladdering is a major drawback of elastomeric systems.
Accordingly, the present invention provides for a method which solves the "bladdering" problem of elastomeric coatings and improves the styrene polymeric coating composition. The present invention provides for a multilayer combination of a styrene polymeric resin as a first coating in combination with an elastomeric coating. This provides double protection to the structural unit. The styrene polymeric resin reduces the risk of bladdering by the elastomeric coating by providing an adherable surface, a barrier membrane such that water/moisture cannot undermine the elastomeric coating adhered to the styrene resin, and at the same time providing waterproofing protection should the elastomeric adhesion fail. The advantage of using the elastomeric top coat or overcoat provides crack bridging capabilities to the styrene polymeric resin coating.
The present invention thus includes a method of waterproofing and sealing rigid structural units by first applying a liquid coating composition containing a styrene polymeric resin in an organic solvent to the structural unit, drying the liquid composition to form a film then applying on top of the film a second coating by either spraying or applying a rolled sheet of an elastomeric coating such as a rubberized asphalt layer on top of the film.
In one embodiment, the first layer is a liquid coating composition containing a combination of about 100 parts by weight of a styrene polymeric resin binder; about 150 to 400 phr of an organic solvent; about 0 to 50 phr of a plasticizer; about 0 to 200 phr of a filler; and about 0 to 100 phr of a particulate solid selected from the group consisting of an opacifying agent and a pigment.
The application of the first layer coating composition penetrates deep into the pores of the concrete or masonry surface sealing each pore of the concrete and each pore locking on with a mechanical grip. Neither water nor air can come through this membrane from either side.
This first coat application conforms to the surface filling in the low valleys with excess material and thinner on the high peaks leaving a smoother, non-breathing surface, excellent for receiving a properly formulated elastomeric coat as a top-coat or overcoat.
The second coat or overcoat is applied on top of the first coating or film either by means of spraying or by a means similar to paper hanging using manufactured sheets containing one or more thermoplastic layers. The elastomeric coat has the ability to bridge cracks. Water vapor may be able to penetrate the elastomeric membrane but flowing water will not. The elastomeric coat with a multilayer system basically protects itself; the soft pliable coating may be designed with an additional harder surface to protect the coating from back filling and other harmful elements. The harder surface does not require a protection board and can be directly back filled against.
The procedure for applying the first coat is operable over a wide range of temperatures, from well below freezing to in excess of 100° F., and to surfaces which are wet or dry. Further, the resulting coating is tough, and adheres strongly to the masonry or concrete structure. In addition, the waterproofing/sealing composition rapidly dries to a coating layer for application of the second coat.
As used herein the specification and the claims, the phrase "a rigid structural unit" is intended to include the following, non-limiting list of rigid structural materials such as wood, metal, stone and stone products, concrete and concrete products, composite materials, brick, tile, terracotta, and the like. In addition, the term "masonry" is intended to include the following, non-limiting list of inorganic materials such as stone and stone products, concrete and concrete products, clay products, brick, tile, terra-cotta, and the like. The unit of measure "phr" is a weight based measurement of parts of a particular component based on 100 parts by weight of the binder component in the composition.
DETAILED DESCRIPTION OF THE INVENTION
Rigid Structural Units
The present invention is useful in methods for protecting subterranean masonry structures. These masonry structures may be foundations, basement walls, retaining walls, cement posts, and the like. The structures may include poured concrete, block and mortar, brick, stucco and the like. The masonry structures may ultimately be completely buried, or may be partially exposed to the atmosphere. The masonry structures may or may not comprise reinforcing bars, rod, mesh, and the like.
In one embodiment, the masonry or concrete structure comprises the foundation and basement walls of a residential or commercial building. These structures generally are formed in excavations in the earth, and may be built under diverse weather and temperature conditions. Generally, the structures are exposed to all weather conditions prior to backfilling or other protection.
In another embodiment, the masonry or concrete structure comprises pre-cast or cast-in-place horizontal decks or floor, for example, as employed in parking ramps and outside courtyards above habitable spaces.
The structures may also have defects which require filling prior to coating. Such defects can be cracks and fissures, and they can be a result of concrete form ties, cold joints in concrete, and the like.
FIRST COAT
Waterproofing/Sealing Coating Composition
The liquid coating composition comprises a styrene polymeric resin binder in an organic solvent. In a preferred embodiment, the liquid coating composition is a combination of about 100 parts by weight of a binder resin comprising a styrene polymer; about 150 to 400 phr of an organic solvent; about 0 to 50 phr of a plasticizer; about 0 to 200 phr of a filler; and about 0 to 100 phr of a particulate solid selected from the group consisting of an opacifying agent and a pigment.
The resin binder may be a styrene homopolymer (polystyrene), a copolymer including styrene, a mixture of polystyrene and one or more polymers, or a combination of the above. The styrene copolymer may comprise a styrene and a rubbery diene co-monomer including isoprene, butadiene, and the like, or it may comprise co-monomers such as acrylonitrile, acrylates, olefins such as butylene, and the like. These copolymers may be random or block copolymers. The styrene polymeric resin can be a general purpose grade, crystalline, high impact, or moderate impact grade of polystyrene. Increasing amounts of styrene copolymers such as styrene-butadiene and styrene-isoprene tend to increase the difficulty in completely dissolving the binder resin, but it is possible to use high impact polystyrene and moderate impact polystyrene resins in the present invention. Preferably, the styrene resin comprises a general purpose grade or moderate impact grade of polystyrene.
A non-limiting list of other polymers which may be mixed with the styrene polymer to form the binder resin includes polypropylene oxide; vinyl polymers such as polyvinyl chloride, polyvinylpyrrolidone, and ethylenevinyl acetate; polyvinylidene chloride; polyethylene; poly(ethyl ether); acrylics; acrylates, methacrylates, and methacrylate copolymers; and the like.
Preferably the styrene resin forms at least about 85 wt. % of the polymeric binder resin, more preferably, at least about 90 wt. %, and most preferably, at least about 95 wt. % of the polymeric binder resin. If the proportion of styrene resin is too low, it may be difficult to completely dissolve the binder resin in the selected solvent. In addition, too small a proportion of styrene in the binder resin may reduce the remelting of the waterproofing film in repair operations discussed below.
The styrene polymeric resin used in the present invention may be modified by plasticizers, coupling agents, and the like. Such modified resins include high impact polystyrene such as styrene-butadiene modified high impact and medium impact polystyrene.
The resin binder may be virgin resin, reground resin, recycled resins, or a mixture thereof. Again, the styrene polymeric resin may be mixed with other resins such as styrene-butadiene rubbers, and the like, to increase the toughness of the resulting film.
Preferably, the resin binder is a styrene polymeric resin having at least 85 wt. % styrene homopolymer. More preferred, the styrene polymeric resin is a general purpose grade polystyrene, which may be clear virgin resin, reground resin or recycled resin. Most preferably, the resin binder comprises clear reground or recycled general purpose grade polystyrene resin.
About 100 parts by weight of the resin binder is dissolved in a suitable organic solvent in order to carry the coating components uniformly through the composition. The amount of solvent used may be selected by the formulator of the liquid composition in order to provide the desired amount of solids, thickness, drying time, etc., in the formulated composition. Preferably, the solvent is present at about 150 to 400 phr, more preferably, at about 180 to 350 phr, and most preferably at about 250 to 300 phr. Persons skilled in the art will be able to easily select an appropriate solvent for the particular binder resin used. Some solvents which are commonly used include methylene chloride, ethylene chloride, trichloroethane, chlorobenzene, acetone, ethyl acetate, propyl acetate, butyl acetate, isobutyl isobutyrate, benzene, toluene, xylene, ethyl benzene, and cyclohexanone. If acrylics or acrylates are used in a mixture with the styrene polymer, it may be helpful to use a co-solvent such as tetrahydrofuran to increase the solubility of both resins in the liquid composition. Preferred solvents include aromatic hydrocarbons such as chlorobenzene, benzene, toluene, xylene, and ethyl benzene.
The plasticizer may be liquid or solid, and is preferably present in an amount sufficient to increase the toughness and flexibility of the film coating. The film coating is more flexible and elastic than the masonry structure substrate. A non-limiting list of useful plasticizers for the present invention include butyl stearate, dibutyl maleate, dibutyl phthalate, dibutyl sebacate, diethyl malonate, dimethyl phthalate, dioctyl adipate, dioctyl phthalate, butyl benzyl phthalate, benzyl phthalate, octyl benzyl phthalate, ethyl cinnamate, methyl oleate, tricresyl phosphate, trimethyl phosphate, tributyl phosphate and trioctyl adipate. Persons skilled in the art will be able to select the type and requisite combination of properties needed in the plasticizer to modify the binder resin. Preferred plasticizers include liquid phthalate plasticizers such as dioctyl phthalate, diethyl phthalate, butyl benzyl phthalate (SANTICIZER™ 160), benzyl phthalate, and octyl benzyl phthalate (SANTICIZER™ 261).
Preferably, the plasticizer is included in the liquid composition at about 0 to 50 phr, depending upon the nature of the resin binder and the desired toughness, elasticity, and related properties in the dried film. More preferably, the plasticizer is included at about 5 to 30 phr, and most preferably, it is present at about 10 to 20 phr.
The filler component of the composition is useful to increase the strength of the resulting film layer. The filler also decreases the amount of the more expensive binder resin needed in the composition, increases the bulk and weight of the resulting film, and otherwise modifies the physical properties of the film and film forming composition. The major modifications which can be achieved with fillers are changes of color or opacity, changes of density, increase of solids content, change of rheology, increase in stiffness or modulus of the coating, and changes in the affinity of the coating for various adhesives, cements, mortars, and the like. A non-limiting list of useful fillers for the present invention include carbonates, clays, talcs, silicas including fumed silica and amorphous silica, silico-aluminates, aluminum hydrate, oxides (zinc or magnesium), silicates (calcium or magnesium), sand, cement powder, mortar powder, and the like. Preferred fillers include magnesium silicate, fumed silica, sand, and cement powder.
Preferably, the filler is included in the liquid composition at about 0 to 200 phr, depending upon the nature of the resin binder and the desired toughness, elasticity, and compatibility of the dried film. More preferably, the filler is included at about 50 to 150 phr, and most preferably, it is present at about 60 to 100 phr.
Particulate solids useful in the present invention are pigments and opacifying agents. These components are useful to impart color to the composition to allow the user to determine coverage of the structure and to render the film coating relatively impervious to UV light. Thus, the pigments and opacifying agents can help to protect the film from UV degradation. Pigments and opacifying agents can be powders, lakes, metal flakes, and the like. A non-limiting list of useful pigments and/or opacifying agents for the present invention include titanium dioxides; iron lakes; iron oxide such as vermillion red, yellow and black; and the like. Preferred pigments and opacifying agents include titanium dioxide, iron oxides, and iron lakes.
Preferably, the particulate solid pigments and opacifying agents are included in the liquid composition at about 0 to 100 phr. More preferably, the particulate solids are included at about 1 to 25 phr, and most preferably, they are present at about 1 to 10 phr. If the particulate solid pigments and/or opacifiers are present at too great an amount, the film will prematurely skin over and the solids may settle and cake. The resulting film will be of poorer quality.
The liquid composition may be prepared by combining the binder resin and organic solvent in a vessel and allowing the components to rest undisturbed overnight. The resin/solvent combination can then be mixed for about 30 minutes. The mixture should be relatively clear to indicate a high level of dissolution of the resin in the solvent. Increasing opacity of the mixture signals a high level of plasticizer or other polymers in the mixture.
Plasticizers, fillers, etc., can then be added and mixing continued for about 45 minutes or until the liquid mixture appears creamy and all particles within the mixture appear to be uniform when viewed through a falling film of the mixture. Of course, adding mild heat to the mixing vessel will decrease mixing time necessary, and beginning agitation immediately will eliminate the need to allow the resin/solvent combination to rest overnight. However, agitation will generally exceed 30 minutes.
The liquid composition is relatively viscous, preferably passing through a 3/8 inch aperture of a 31/4 ounce full radius viscosity cup in about 12-20 seconds at 60° F. and, more preferably, about 15-20 seconds at 60° F., and has a solids content of about 35 to 65 wt. %, and forms a film having an average water vapor permeability of less than about 1*10 -2 perms-inch. More preferably, the solids content is about 40 to 55 wt. %, and the average water vapor permeability is less than about 8*10 -3 perms-inch. Most preferably, the solids content is about 50 wt. %, and the permeability is less than about 6*10 -3 perms-inch.
Application of the First Coating Composition
The first coating composition can be applied to the exterior of any below grade masonry structure, or it can be applied to the interior of a structure such as below grade masonry walls, ceilings, etc., in basements, tunnels, retaining walls, cement posts, and the like, or elsewhere as discussed above. In coating foundations, the composition is applied on the exterior of the below grade structure prior to backfilling. The exterior coating using the composition of present invention of the structure resists water pressure and provides a waterproof coating to keep the interior of the masonry structure dry and relatively free of aqueous-induced degradation of reinforcing steel structures. In addition, the coating greatly reduces interior humidity in basements of structures. Interior coatings of masonry walls, ceilings, etc., using the composition of present invention strongly adhere to the masonry substrate to resist hydrostatic pressure and effervesce which often destroys paints and coatings on many below grade masonry surfaces.
The liquid coating composition can be applied by rolling, brushing, spraying, spraying and backrolling, etc. Preferably, the coating is applied by transfer pump at about two to three gallons/minute from a container to the surface of the structure followed by rolling or brushing as with standard waterproofing paints. After application, the coating can dry rapidly under average ambient conditions. However, in extreme cold temperatures or high humidity, the drying of the coating can be more prolonged. Generally, under moderate humidity in the shade at about 70° F., a coating having a wet thickness of about 35 mils will dry to a non-tacky, non-fluid state in about 4 hours. At the other extreme, under winter conditions of about 25° F. and low humidity, the same coating will dry in about 12 hours (overnight).
Filler Composition
The filler composition comprises a polystyrene resin binder and an inorganic filler in an organic solvent. The resin binder and organic solvent may be as discussed above. The inorganic filler is preferably added to the composition as a powder or larger particulate solid. A non-limiting list of useful inorganic fillers for the present invention include portland cement, natural cement, mortar, sand, and crushed aggregate. The filler composition generally comprises about 100 parts by weight of the resin binder, about 50 to 200 phr of the inorganic filler and sufficient organic solvent to form a paste. In a preferred embodiment, filler composition comprises about 75 to 150 phr of the inorganic filler and about 80 to 250 phr of the organic solvent, and more preferably, the filler comprises about 100 to 120 phr of the inorganic filler and less than about 180 phr of the organic solvent. The filler composition can be applied by trowel, roller, brush, caulk gun, or other processes normally used for applying heavy mastics and slurries. The filler composition has a solids content of at least about 60 wt. % and more preferably about 80 to 90 wt. %.
In coating the filler composition with the coating composition, the organic solvent can remelt the resin binder to form a strong joint between the filler and coating compositions. The filler composition can be coated with the waterproofing/sealing composition essentially immediately or as soon as the filler composition attains a non-tacky state.
OVERCOAT
The overcoat applied over the first coat or continuous film of the present invention is an elastomeric material. Any elastomer known in the art may be used but those of low to moderate price are preferable. For example, rubber/asphalt elastomers are especially desirable and may be combined with a thermo-plastic rubber to form a hard, durable surface that stretches when applied and long after. Other elastomers capable of being used in the present invention are those such as unvulcanized natural rubber, chlorinated natural rubber, styrene-butadiene rubber, polyisoprene, butadiene polymers, polybutene, isobutylene-isoprene copolymers, ethylene-propylene copolymers and terpolymers, chlorinated butylene-isoprene polymers, chlorosulfonated polyethylene, polychloroprene, polyacrylates, polymethacrylates, polyurethanes, acrylonitrile-butadiene rubbers, hexafluoropropylenevinylidene fluoride rubbery copolymers, epichlorohydrin homopolymers, and epichlorohydrin-propylene oxide rubbery copolymers. These rubbery polymers often contain fillers, such as silica and additives, for example, pigments, plasticizers and stabilizers.
The above elastomers can be used as a sprayable coat or can also be used as part of a waterproofing membrane adhered to a sheet. Such sheeting of layered laminates may be purchased commercially and preferably contain a support structure or sheet made of polyolefin material which the waterproofing membrane is adhered thereto on one face of the sheet. Said waterproofing membrane may comprise an asphalt-rubber type of composition known as a bitumen-rubber composition which has waterproofing pressure-sensitive adhesive properties. The membrane which is adhered on one face of the sheet may be protected on the other side by a removable paper or disposable sheet when purchased commercially. Preferred waterproofing membranes used as an overcoat in the present invention are those described in U.S. Pat. No. 5,316,848 which patent is incorporated herein by reference.
The waterproofing membrane contains one or more layers of an adhesive layer, preferably a waterproofing pressure sensitive adhesive layer, an elastomeric protective coating layer and a carrier layer. The protective coating may consist of one or more layers depending on the needs of the structure to be treated. Thus, for example, a waterproofing membrane may contain protective layers which not only prevent water from leaking but also provide insulation to noise and/or temperature. The elastomeric layers sandwich one or more closed cell layers of a flexible or rigid film coating known in the art to insulate noise and/or temperature as well as being waterproof.
OVERCOAT APPLICATION
One method of applying the overcoat is by spray coating which has the advantages of spray delivery and minimal man power. This coating may be sprayed in the same manner as the first coat is sprayed through a high pressure sprayer and hose delivery system. The system may require temperature control of the materials and may require additional hoses and spray guns and possibly a second pump and/or a heat exchanger. The elastomeric materials may be admixed with mineral spirits or the solvents employed in the first coat for application.
The elastomeric overcoat may be in a form of sheet goods comprising a sheet and waterproofing membrane adhered to one face of the sheet. This type of material has the advantage of controlled thickness, increase stretch, no/or low VOCs and immediate back filling. These sheet goods are manufactured in thin layers, rolled, boxed and available as such. Application merely involves rolling the material at the job site and applying onto the first coat. Application of the product requires techniques similar to paper hanging and may be applied on masonry or concrete materials including foundations below grade. In addition to U.S. Pat. No. 5,316,848 mentioned above, preferred sheeting goods are those described in U.S. Pat. Nos. 3,741,856; 3,853,682; and 3,900,102 which patents are incorporated herein by reference.
The elastomeric overcoat may have a variety of thicknesses from about 1/64 to 3 inches thick depending on the number of layers and materials used. Preferably, the overcoat varies from about 0.125 to about 0.25 inches thick.
EXAMPLES
The following specific examples can be used to further illustrate the invention. These examples are merely illustrative of the invention and do not limit its scope.
FIRST COAT
Example 1
Fifty-five gallons of a liquid coating composition was prepared from the following materials:
______________________________________Component Quantity______________________________________Polystyrene resin (DISCOVER* 100 lbs.GPPS OPS regrind)Xylene 40 gal.Dioctyl phthalate plasticizer 2 gal.(DOP - Eastman Kodak)Magnesium silicate (MISTRON from 50 lbs.Cyprus Industrial Minerals)Titanium dioxide 3 lbs.Iron oxide 4 oz.______________________________________ *Discover Plastics, Inc., Minneapolis, MN
The liquid coating composition was prepared by combining the binder resin and organic solvent in a vessel and allowing the components to rest undisturbed overnight. The next morning, the combination was mixed for about 30 minutes until clear, and the remaining ingredients were added. Agitation continued for about 45 minutes until the liquid mixture appeared creamy. All particles within the mixture appear to be uniform when view through a falling film of the mixture.
The samples were prepared by spraying a test coating to the foil face of polyisocyanurate sheet-type insulation board. Four 2'×2' samples were prepared and identified as "A"-"D".
The actual thickness of the material varied within each individual sheet and within each 3" diameter specimen. Specimens cut from the "A" sample averaged from 5 to 20 mils. Specimens cut from the "B" sample averaged from 10 to 17 mils. Specimens from samples "C" and "D" averaged from 4 to 40 mils.
The specimens tested were selected from three thickness groups: 6 to 7 mil average thickness, 9 to 10 mil average thickness and 38 to 40 mil average thickness.
______________________________________SUMMARY OF RESULTS______________________________________Thickness Average Permeance,Group Perms (Grains/ AveragePerms*in Method (hr*ft.sup.2 * in Hg)) Permeability,______________________________________6-7 mils Desiccant 0.46 0.0030 Water 0.56 0.00369-10 mils Desiccant 0.30 0.0028 Water 0.45 0.004638-40 mils Desiccant 0.14 0.0054______________________________________ Permeance, Perms, Perme-Thickness Specimen (Grains/ ability,Group Method Number (hr*ft.sup.2 in Hg)) Perms*in______________________________________6-7 mils Desiccant 1 0.32 0.0023 2 0.60 0.0036 Average 0.46 0.0030 Water 1 0.53 0.0033 2 0.65 0.0043 3 0.50 0.0033 Average 0.56 0.00369-10 mils Desiccant 1 0.29 0.0028 2 0.27 0.0025 3 0.28 0.0025 4 0.34 0.0034 Average 0.30 0.0028 Water 1 0.45 0.004638-40 mils Desiccant 1 0.15 0.0057 2 0.13 0.0050 Average 0.14 0.0054______________________________________
OBSERVATIONS
The water vapor "permeance", measured in "perms", is the time rate of water vapor transmission through unit area of a flat material induced by a vapor pressure difference between two specific surfaces, under specified temperature and humidity conditions. The thickness of a material is not factored into a measure of "permeance". Thus, the "perms", or the rate of water vapor transfer, is decreased as the specimen thickness is increased.
The water vapor "permeability" is the time rate of water vapor transmission through unit area of flat material of unit thickness induced by unit vapor pressure difference between two specific surfaces, under specific temperature and humidity conditions. "Permeability" is the arithmetic produce of permeance and thickness.
TEST METHODS
The water vapor transmission test was conducted in accordance with ASTM E96-90, "Standard Test Methods for Water Vapor Transmission of Materials." The test was conducted using both the dry-cup and wet-cup methods at conditions of 73° F. and 50% RH. Several 2.8" diameter specimens from each sample group were tested. Each specimen was sealed, suing a rubber gasket or wax, in an aluminum water vapor transmission test cup containing dried anhydrous calcium chloride or deionized water. The test assemblies were placed in a Blue M model FR-446PF-2 calibrated environmental chamber, serial number F2-809, with conditions set at 73°+2° F. and 50+2% RH. Weight gain was monitored daily up until steady-state vapor transfer was achieved. The permeance for each specimen was calculated based on computer-generated graphs of the steady-state vapor transfer.
Example 2
FIRST COAT
Fifty-five gallons of a liquid coating composition are prepared from the following materials:
______________________________________Component Quantity______________________________________Polystyrene resin (DISCOVER* 95 lbs.GPPS OPS regrind)Acrylic resin (ELVACITE™ #2010 5 lbs.dupont)Xylene 38 gal.Tetrahydrofuran 2 gal.Dioctyl phthalate plasticizer 2 gal.(DOP - Eastman Kodak)Magnesium silicate (MISTRON from 50 lbs.Cyprus Industrial Minerals)Titanium dioxide 3 lbs.Iron oxide 4 oz.______________________________________ *Discover Plastics, Inc., Minneapolis, MN
The liquid coating composition is prepared by combining the polystyrene resin and xylene solvent in a vessel and allowing the components to rest undisturbed overnight. The next morning, the combination is mixed for about 30 minutes until clear. The acrylic resin is dissolved in tetrahydrofuran and added to the polystyrenexylene mixture. The remaining ingredients are added under agitation beginning with the plasticizer, and the complete mixture is agitated for about 45 minutes until the liquid mixture appeared creamy. All particles within the mixture appear to be uniform when view through a falling film of the mixture. Viscosity is checked with a 31/4 oz. cup having a 3/8" aperture. The cup empties in about 15-17 seconds at 60° F., and 12-16 seconds at 70° F.
The foregoing description, examples and data are illustrative of the invention described herein, and they should not be used to unduly limit the scope of the invention or the claims. Since many embodiments and variations can be made while remaining within the spirit and scope of the invention, the invention resides wholly in the claims herein after appended.
Example 3
A liquid coating composition was prepared as in Example 1 from the following materials:
______________________________________Component Quantity______________________________________Polystyrene resin (Ex. 1) 100 lbs.xylene 38 gal.Dioctyl phthalate plasticizer 2 gal.(Ex. 1)Chlorinated paraffin 2 gal.Magnesium silicate (Ex. 1) 50 lbs.Micaceous Iron Oxide 3 lbs.______________________________________
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A novel multi-layered system for waterproofing and sealing a rigid structural unit using as a first coat a styrene polymeric film cast from an organic solvent and an elastomeric overcoat applied thereon is described. The first coat is easily maintained as damaged areas and imperfections can be repaired by simply applying additional liquid composition to the damaged area, and the liquid composition remelts the existing film allowing the newly formed film to be continuous. The overcoat adds crack bridging properties to the first coat without bladdering. Novel methods relating to the use of the system are also described.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a method for producing sheet-metal container bodies having a longitudinal seam welded by a laser beam, and to an apparatus for performing the method.
2. Description of the Related Art
Published Federal Republic of Germany Patent Application (Offenlegungsschrift) No. 27 01 427 discloses a method for producing container bodies from sheet metal with straight longitudinal ends joined into a longitudinal seam by abutting the edges of the longitudinal end, followed by laser beam welding of the abutted edges. With this method, satisfactory seams are attainable at welding speeds of up to approximately 30 m/min. At higher welding speeds, irregularities or flaws, such as cracks, shrink holes or pores, have been found to appear in the welded seam. Such irregularities occur in part because of stresses due to a steep temperature drop in the areas of the metal sheet adjoining the abutted edges.
Published Federal Republic of Germany Patent Application (Offenlegungsschrift) No. 29 20 428 discloses a method and apparatus for producing laser beam welded hollow sections (pre-forms) in which both longitudinal ends of the pre-formed section are bent in the same direction and are oriented radially outwardly and pushed together before being welded. In this method, it is accordingly difficult, without further machining, to obtain a smooth welded seam.
Published Federal Republic of Germany Patent Application (Offenlegungsschrift) No. 32 19 252 discloses a method for welding metal parts that have a particularly defined geometric shape which they must retain and a relatively great sheet thickness, for example, a platform and web of a brake shoe. The metal parts in their final shape are urged into contact with one another and are welded together by means of a focused laser beam, electron beam or plasma beam. In order to counteract the strain in the metal parts caused by the heat of welding, an additional force is exerted on the connection of the metal parts in the vicinity of the welding site, for instance by means of a roller.
Published Federal Republic of Germany Patent Application (Offenlegungsschrift) No. 26 47 082 discloses a method in which two strips that each move in their longitudinal extension are joined at an angle to form a mutually overlapping connection in the direction of movement and are pressed together by a pair of pressure rollers. A focused laser beam is aimed at the region in which the two strips run together, effecting a continuous weld of the overlapping seam.
Finally, U.S. Pat. No. 4,237,363 discloses a method for spot welding or line welding together two flat stacked sheets in which an electron beam or laser beam is aimed at the outside of one of the sheet elements. An attendant disadvantage of this method is that the surface of one of the sheet elements is marred by the electron or laser beam.
SUMMARY OF THE INVENTION
It is an object of the present invention to devise a method for producing container bodies from body blanks of sheet metal with longitudinal seams welded by means of a laser beam, with which method a satisfactory seam quality is attainable even at high welding speeds, such as welding speeds in excess of 30 m/min.
It is a further object of the present invention to devise an apparatus for performing the method.
These objects are accomplished by providing a method for laser beam welding of longitudinal seams in container bodies having a predetermined circumferential dimension, characterized in that a metal blank or sheet is used having opposite first and second longitudinal ends and opposing first and second transverse ends, the first and second longitudinal ends each having a length, a longitudinal edge, and an inner face and an outer face, the transverse ends each having a length which exceeds the predetermined circumferential length of the container body. The first and second longitudinal end of the sheet, either during or after the formation of the shape of the container body, are overlapped, i.e., the first longitudinal end is moved toward and over the second longitudinal end into such a position that, as seen in cross section, they form an acute angle and define an angular opening therebetween by orienting the edge of the second longitudinal end toward the inner face of the first longitudinal end. At least one focused laser beam is aimed into the angular opening and relative movement is effected between the at least one focused laser beam and the angular opening along its longitudinal extension. At least a portion of the respective faces of the first and second longitudinal ends that form the acute angle, i.e., the inner face of the first longitudinal end and the outer face of the second longitudinal end, are heated to a temperature above the welding temperature and the first and second longitudinal ends, prior, to dropping below the welding temperature, are pressed together thereby forming a welded longitudinal seam for the container body.
The term "longitudinal ends" as used herein is not intended to mean that these ends are necessarily long ends, such that the container blank is necessarily longer than its width or circumferential dimension. Rather, the term refers to the ends to be joined that are moved "longitudinally" past the laser beam for welding and encompasses ends whose length is shorter than the width or circumferential dimension of the container blank, and visa versa.
The term "circumferential dimension" of the container blank as used herein is not limited to a blank forming a cylindrical container body having a circular cross section, but is intended to refer to the dimension of the blank corresponding to a periphery of the container body, regardless of the shape or cross section of the container body. The container body may have any cross section including, for example, circular, square, rectangular, etc.
By forming an acute angle between the longitudinal ends of the metal sheet, the faces of the sheet that are to be joined together can be heated by the at least one focused laser beam and brought to a dough-like or molten state, while the respective obverse faces of the longitudinal ends continue to have a predominantly solid structure. The immediately ensuing pressing against one another of the longitudinal ends, i.e., the pressing together of the molten face portions of the longitudinal ends, creates a firm seam connection upon cooling.
The materials being pressed together deform. Advantageously, the deformation of the material is not limited merely to the molten or dough-like region, however, the peripheral regions adjacent to the seam site are also deformed. These regions are deformed plastically, that is, permanently, and the deformation preferably takes place at right angles to the pressing force being exerted. Since the deformation is usually permanently effected in and around the area of the welded longitudinal seam, the shrinkage strains that occur with rapid cooling of the molten material and the adjacent regions of the seam site are largely compensated for, that is, reduced. The danger of fissuring in the weld is counteracted in this way.
Further advantageous features of the inventive method are attained as follows. By pressing the second longitudinal end flush with and inwardly against a forming mandrel, and forming the acute angle between the two longitudinal ends by bending the first longitudinal end, good guidance of the longitudinal ends on the forming mandrel is attained. Alternately, the acute angle formed between the longitudinal ends of the sheet may be produced by raising and extending at a tangent the second longitudinal end, which is substantially flat, away from a forming mandrel and moving the first longitudinal end, which is likewise substantially flat, so that its inner face approaches the edge of the second longitudinal end. In this way, the acute angle between the longitudinal ends can be formed without having to bend one longitudinal end. However, the first longitudinal end, prior to having its inner face approach the edge of the second longitudinal end, may be bent outwardly and with the additional bending, the angle of the angular opening can be made larger.
To take into account the various reflective or absorptive capacities of the faces of the longitudinal ends of the container blank that are to be pressed into contact while at or above the welding temperature, the axis of the at least one focused laser beam may be variable. The vertical projection of the axis of the at least one focused laser beam onto a tangential plane through the welded longitudinal seam may form an angle which ranges between 10° and 170°, preferably between 45° and 90°, with the portion of the vertical longitudinal central plane oriented counter to the feed direction of the metal sheet, that is, with the vertical longitudinal central plane when viewed in the feed direction. To attain an optimal distribution of heat to the contact or weld faces, especially when the faces have different properties, the axis of the at least one laser beam also may be pivotable about a horizontal axis.
Thus, the at least one focused laser beam may be caused to meet the faces of the longitudinal ends which are intended to form the longitudinal seam in such a manner that the axis of the at least one focused laser beam is inclined, as viewed from its focal point, by an angle of up to 45° upwardly and by an angle of up to 10° downwardly with respect to a tangential plane passing through the longitudinal seam to be formed.
When the respective faces of the longitudinal ends after having been heated by the at least one focused laser beam are pressed together in such a manner that the remaining thickness of the longitudinal seam is less than the sum of the original sheet thicknesses of the longitudinal ends, the container blanks are simpler to machine in subsequent machining operations, such as flanging or beading.
The objects of the present invention are additionally accomplished by providing an apparatus for performing the inventive method having a pair of pressure rollers by means of which the longitudinal ends are pressed together before they drop below the welding temperature. The clearance space between the pressure rollers is adjusted to an amount in accordance with the inventive method and at least one of the pressure rollers is drivable.
More particularly, the apparatus has an arrangement for guiding and positioning a metal sheet, which may be a preformed container blank, which metal sheet has opposing first and second longitudinal ends that are to be welded. The apparatus has an arrangement for overlapping the first and second longitudinal ends and forming an angular opening therebetween, including a forming mandrel, and has an optical device for supplying at least one focused laser beam, for performing the inventive method. The optical device is angularly variably adjustable with respect to a vertical longitudinal central plane through the longitudinal seam to be welded and through the axis of the forming mandrel and is aimed into the angular opening. The pair of pressure rollers are positioned vertically one above the other and above and below, that is, on either side of, the overlapping first and second longitudinal ends. The resultant thickness of the welded longitudinal seam may be controlled by exerting pressure upon the pressure rollers. In the above apparatus, at least one pressure roller may be movably supported transversely to the feed direction with respect to the other pressure roller and may be acted upon with pressure in a direction toward the pair of pressure rollers by an adjustable force.
In order to raise one longitudinal end of the sheet away from the forming mandrel, a strip positioned along the vertical longitudinal central plane and protruding beyond the surface of the forming mandrel may be provided. In order to form the angular opening, a feed roller may also provided.
One longitudinal end can be bent at an angle if the arrangement for forming the angular opening between the longitudinal ends of the sheet has two pairs of profile rollers having running faces adapted to the container body. The profile roller pair for one longitudinal end has one roller located outside the forming mandrel and has a segment tapering toward the other longitudinal end, and one roller located at least partly in the forming mandrel and having a correspondingly widening flange. Some of the profile rollers can simultaneously act as a conveyor device for the container body if the respective outer rollers are drivable.
In the simplest case, the circumferential faces of the pressure rollers are cylindrical or slightly convex. However, in order to preserve the pre-formed shape, especially for small, cylindrical container blanks, the outer pressure roller may be provided with a concave circumferential face, and the inner pressure roller with a convex circumferential face. Moreover, to reduce their wear, the pressure rollers may be made of a material having high thermal conductivity, and they may have a circumferential ring of heat-resistant material forming the running faces thereof. They may also be provided with hollow spaces for the flow therethrough of coolants.
BRIEF DESCRIPTION OF THE DRAWING
Exemplary embodiments of the invention are schematically shown in the drawing, in some cases with highly exaggerated proportions. Further objects and advantages of the present invention and the structure and operation of the apparatus will become apparent from the following detailed descriptions taken in conjunction with the drawing in which:
FIG. 1 is a fragmentary plan view of the apparatus for laser pressure welding of an overlapping seam of a container blank;
FIG. 2 is a front view, partly in cross section, of the apparatus of FIG. 1 taken along the arrow A of FIG. 1;
FIG. 3 is a fragmentary side view of the apparatus of FIG. 1;
FIG. 4 is a fragmentary cross section of the apparatus during the formation of a V-shaped angular opening or welding gap between the longitudinal ends;
FIG. 5 is a fragmentary cross section of the apparatus during the formation of a V-shaped angular opening with longitudinal ends touching one another;
FIG. 6 is a fragmentary cross section of another embodiment of the apparatus showing an arrangement of the metal sheet for the formation of a V-shaped angular opening having longitudinal ends touching one another;
FIG. 7 is a fragmentary side view of the apparatus of FIG. 6;
FIG. 8 is a fragmentary cross section taken along line VIII--VIII of FIG. 7 showing the location of the metal sheet ends on the forming mandrel after the passage of the arrangement of FIGS. 6 and 7 through the focal point of the focused laser beam;
FIG. 9 is a fragmentary cross section of an apparatus embodiment showing the location of the longitudinal ends of the metal sheet on a forming mandrel provided with an upper strip, the inner or second longitudinal end resting on the strip and the outer or first longitudinal end being bent outwardly;
FIG. 10 is a fragmentary cross section showing one end of the welded longitudinal seam pressed between pressure rollers; and
FIG. 11 is a plan view of an apparatus for laser pressure welding of an overlapping seam with an optical device having three laser apertures, i.e., three focused laser beams.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The apparatus according to FIGS. 1-3 for welding longitudinal seam N, which is an overlapped seam, to form container body 1 has a forming mandrel 2 on the end of which a pressure roller 3 is supported, freely rotatably, in a support arm arrangement 4 which is secured to the forming mandrel 2. The support arm arrangement 4 is adjustable in height (in a manner not shown) relative to the forming mandrel 2, and the pressure roller 3 has an axis of rotation which is disposed behind the forming mandrel 2 as seen in feed direction V of the container body 1 that is to be welded. A counterpart pressure roller 5 that is drivable by a drive means (not shown) is disposed above the pressure roller 3. The axes of rotation of the pressure rollers 3, 5, which are each provided with a respective cylindrical circumferential face 6, 7, are disposed horizontally parallel to one another, and vertically one above the other. The counterpart pressure roller 5 is overhung-mounted in a bearing block 8, which in turn is secured to a base plate 9, which is a frame member of the apparatus. Because of the adjustability in height of the support arm arrangement 4, clearance space a 0 (see FIG. 10) between the cylindrical circumferential faces 6 and 7 of the rollers 3 and 5 is also variably adjustable.
The apparatus shown in FIG. 1 also has an optical device 10, which concentrates or focuses a laser beam 12 into a focused laser beam 15 having a focal point 13. The forming mandrel 2 has a vertical longitudinal central plane S and focal point 13 is located in the vertical longitudinal central planes ahead of a plane E defined by the axes of rotation of pressure rollers 3, 5. Vertical longitudinal central plane S is also defined by the longitudinal seam N and by the axis of each particular container body 1. As viewed in feed direction V of the rounded metal blank or sheet to be welded, into container body 1, the optical device 10 is disposed ahead of the plane E defined by the axes of rotation of the pressure rollers 3, 5, extends perpendicular to the vertical longitudinal central plane S, and is pivotable toward an imaginary horizontal plane H (FIG. 2) by an angle β. The angle β can range between -10° and +45°; that is, the focused laser beam 15 can be inclined up to 10° downwardly and up to 45° upwardly as seen from the optical device 10, with respect to plane H. The imaginary horizontal plane H is parallel to imaginary tangent plane T (FIG. 2) of the container body 1 that extends at right angles to the vertical longitudinal central plane S through the longitudinal seam N.
Optical device 10 is also pivotable within the imaginary horizontal plane H, such that the vertical projection of axis 14 of the optical device 10, or of laser beam 12 focused by the optical device 10 into focussed laser beam 15, onto plane H or T, and the portion of the vertical longitudinal central plane S facing away from the feed direction V, as viewed vertically from above, form an angle α of 60°. In other words, the axis 14, viewed radially toward the prepared, but as yet unwelded, longitudinal seam, is inclined by an angle α with respect to the prepared longitudinal seam. Depending on the reflective or absorptive capacity of faces 16, 17 of longitudinal ends 18, 19, respectively, of the metal sheet, which faces 16, 17, are to be welded together, the angle α can range between 10° and 170°, preferably 45° to 90°.
The optical device of the apparatus of FIG. 11 differs from the above-described exemplary embodiments and has three optical elements 10a, 10b, 10c, each of which transmits one-third of laser beam 12 at an angle α-1, α-2, α-3, respectively, with respect to the vertical longitudinal central plane S in the form of focused laser beams 15a, 15b, 15c, respectively. There may be any positive, finite number of optical device elements, 10a, 10b, . . . , 10n. Depending on the number n of optical device elements, 10a, 10b, . . . , 10n, there are n focal points 13a, 13b, . . . , 13n on the vertical longitudinal central plane S. In FIG. 11, n=3 and there are three focal points 13a, 13b, 13c.
In the exemplary embodiment of FIGS. 4 and 5, the forming mandrel 2 has a strip 20, in the vicinity of its uppermost generating line, which protrudes upwardly beyond the cylindrical outer surface of the forming mandrel 2 and terminates, in the longitudinal direction, with the termination of the mandrel 2. Located next to the strip 20, on one side thereof, is a cylindrical feed roller 21, axis of rotation 22 of which is disposed in an imaginary plane transverse to the longitudinal axis of the forming mandrel 2 and is inclined by an angle φ (hereinafter "angle phi") with respect to horizontal line W.
In another exemplary embodiment shown in FIGS. 6-8, the forming mandrel 2 is shown as completely cylindrical at its end (see FIGS. 7 and 8). Ahead of the plane E formed by the axes of rotation of the pressure rollers 3, 5 and ahead of the focal point 13 of the focused laser beam 15, as seen in the feed direction V, the apparatus has a forming or profile roller arrangement shown generally at 23 positioned at the cylindrical end of forming mandrel 2 for bending or folding one of two longitudinal ends 18, 19, of the metal sheet (see FIGS. 6 and 7 in which longitudinal end 18 still is bent). The profile roller arrangement 23 (FIG. 6) has an upper pair of profile rollers 24, 26, which are freely rotatable and a lower pair of profile rollers 25, 27. The upper pair of profile rollers 24, 26 is overhung-mounted on a bearing block 28 secured to the base plate 9, and the lower pair of profile rollers 25, 27 is supported in a recess 29 of forming mandrel holder 30.
The lower pair of profile rollers 25, 27 have convex circumferential faces 31, 33, respectively, in the form, as seen in cross section, of a circular segment the radius R of which is equivalent to the circular segment of the outer cylindrical face of the forming mandrel 2 (compare FIGS. 6 and 8). The upper profile rollers 24, 26 have concave circumferential faces 32, 34, respectively, the generating lines of which are likewise described by a circular segment having the radius R.
With reference to FIG. 6, the lower profile roller 25 also has a conical widening flange 35 on the side thereof which is oriented toward the roller 27. The generating line of the outer face of the conical flange 35 is, as seen in cross section, inclined outwardly by an angle γ (hereinafter "angle gamma") with respect to the tangent of the convex circumferential face 31 at the common point of contact. Adjoining the concave circumferential face 32 of the upper profile roller 24 in a direction toward the upper profile roller 26 is a conical segment 36. The generating line of the conical segment 36 is inclined inwardly by the angle gamma with respect to the tangent of the concave circumferential face 32 at the common point of contact.
With continuing reference to FIG. 6, between the profile rollers 24, 26 and 25, 27 of the profile roller pairs, two guide strips 37, 38, are provided, as seen in the feed direction V, and are made of a suitable wear-resistant material, such as hardmetal, ceramic or the like. The guide strips 37, 38 are secured to a web plate 39, which in turn is secured via a holder 40 to the base plate 9.
In the exemplary embodiment of FIG. 7, bearing 8' of the upper pressure roller 5 is movably supported in support means shown as a vertical guide 45 and is urged by a compression spring 46 toward the lower pressure roller 3. Deviating from this exemplary embodiment, the support means for upper pressure roller 5 can alternately be a rocker arm (not shown), which is optionally connected to the base plate 9 via a torsion bar (not shown).
With reference to FIG. 10, the pressure rollers 3, 5 each have two roller halves 51, 52 (although only the two roller halves 51, 52 of pressure roller 5 are shown), made of copper, for example, and having defined collectively therein a common circumferential groove 53, in which is fastened a circumferential ring 54 made of, for example, hardmetal or ceramic, that forms running surfaces 6, 7. Between the respective roller halves 51, 52, there is also a partitioning disk 55, which, together with the inside surfaces of the respective rollers halves 51, 52, defines a coolant conduit 56.
In the apparatus of FIGS. 1-3, container bodies 1 are moved one after the other, the metal blank or sheet to become container body 1 being wrapped around the forming mandrel 2 and being, moved longitudinally along the forming mandrel 2. In this process and with reference to FIG. 4, the inner face of the longitudinal end 19 slides on the strip 20, while inner face 16 of the outer longitudinal end 18 is urged by the cylindrical feed roller 21 toward edge 43 of the longitudinal end 19. Depending on the angular position of the axis of rotation 22 of the cylindrical feed roller 21, inner face 16 of the longitudinal end 18 can be spaced apart by a short distance from edge 43 (FIG. 4) or can be pressed firmly against edge 43 (FIG. 5), as a result of which the inner longitudinal end 19 is well retained in its position.
The focused laser beam 15 is aimed into an angular opening 57 that is a welding gap defined between inner face 16 of the outer longitudinal end 18 and outer face 17 of the inner longitudinal end 19 (FIG. 4) or into the intersection point thereof (FIG. 5). The overlapping of longitudinal ends 18, 19 forms an acute angle γ (hereinafter "angle gamma"). The location of the laser beam 15 with respect to faces 16, 17, or their imaginary angle-bisecting plane can be varied by pivoting optical device 10 relative to the imaginary horizontal plane H (FIG. 2) and adjusting it correspondingly in height. As a result, uniform melting of both faces 16, 17 can be attained.
Directly after passing through focal point 13 of laser beam 15, the corresponding segments of longitudinal ends 18, 19 are moved through the clearance space a 0 , i.e., the gap between pressure rollers 3, 5 (see FIG. 10). The clearance space a 0 between circumferential faces 6, 7 of the pressure rollers 3, 5 is preferably less than two sheet thicknesses (2s) compared to metal sheet thickness (s), so that the longitudinal ends 18, 19 are pressed together to form a common, welded longitudinal seam N even before their molten parts have changed to solid state again. The remaining thickness thereof is likewise correspondingly less than two sheet thicknesses (2s).
In the exemplary embodiment of the apparatus and method as shown in FIG. 6, the outer longitudinal end 18 is bent outwardly by profile roller pair 24, 25. Edges 42, 43 of the longitudinal ends 18 and 19, respectively, slide along wear or guide strips 37, 38. Prior to passage through focal point 13 and pressure roller pair 3, 5, the various segments of the container body 1 and, in particular, the longitudinal ends 18, 19, are moved by additional rollers 44 (only one of which is shown in FIG. 7) into the position shown in FIG. 8. In the case of this prepared, but as yet unwelded, longitudinal seam, laser beam 15 must be aimed correspondingly more steeply than for the longitudinal seam being formed in FIG. 5.
With reference to FIG. 9, it is also possible to allow the inner longitudinal end 19 to slide on strip 20 of the forming mandrel 2 and to press an outwardly-bent outer longitudinal end 18 against the edge 43 of the longitudinal end 19. In that case, the angle gamma of the angular opening 57 prepared for welding is particularly large.
The present disclosure relates to the subject matter disclosed in Federal Republic of Germany Patent Application No. P 36 30 889.7, filed Sept. 11th, 1986, the entire specification of which is incorporated herein by reference.
It will be understood that the above description of the present invention is susceptible to various modifications, changes and adaptations, and the same are intended to be comprehended within the meaning and range of equivalents of the appended claims.
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Method and apparatus for laser-beam welding of longitudinal seams in container bodies feature overlapping longitudinal ends of a metal sheet, the length of the transverse ends of which exceeds a predetermiined circumferential dimension for the container body, into such a position relative to one another that they form an acute angle and define an angular opening, and the edge of one longitudinal end is oriented toward the inner face of the other longitudinal end. At least one focused laser beam, which is capable of relative movement with respect to this angular opening and parallel to the longitudinal ends, is aimed into the angular opening and locally melts portions of the longitudinal ends. The locally-molten longitudinal end portions are pressed against one another before they drop below the welding temperature to form a welded longitudinal seam.
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