US2009184039A1PendingUtilityA1

Monolithic column

Assignee: DIONEX CORPPriority: Jun 26, 2002Filed: Dec 30, 2008Published: Jul 23, 2009
Est. expiryJun 26, 2022(expired)· nominal 20-yr term from priority
Inventors:Shaofeng Xie
G01N 30/56B01J 2220/82B01J 19/0013B01D 15/206B01J 2220/58G01N 30/52B01J 41/20B01J 20/285B01J 2219/00162B01J 2220/54B01J 20/261G01N 2030/567B01J 19/18B01J 20/283G01N 2030/528B01J 39/26Y10T29/49604G01N 30/6091B01J 20/28052B01D 15/20B01J 8/0005B01J 20/28042G01N 30/54G01N 2030/525
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Claims

Abstract

Permeable polymeric monolithic materials are prepared in a plastic column casing. In one embodiment, the permeable polymeric monolithic materials are polymerized by the application of heat from an external source starting at a low temperature such as 40 degrees centigrade, depending on the mixture and size of the column, and continuing at a higher temperature, such as 60 degrees centigrade. The temperature at the start of the polymerization is low enough so as not to cause exothermal run-away conditions and to avoid high heat of reaction that would prevent a substantially constant temperature across the cross-section of the column. The higher temperature is used after sufficient monomer depletion has occurred and steric interference has increased so the polymerization reaction is sufficiently slow to avoid heat of reaction generation high enough to cause significant reduction in the homogeneousness of the pore sizes.

Claims

exact text as granted — not AI-modified
1 - 9 . (canceled) 
     
     
         10 . A method of making a disposable chromatographic column comprising the steps of:
 putting a polymerization mixture in a column casing wherein the polymerization mixture comprises a functional monomer containing a sulfonic group; and   directly polymerizing the mixture to provide a strong cation exchanger.   
     
     
         11 . A method in accordance with  claim 10  wherein the step of putting a polymerization mixture in the column casing comprises the steps of hydrolyzing a polymer in the polymerization mixture and modifying a hydroxyl formed in the step of hydrolyzing the polymer with chlorosulfonic acid. 
     
     
         12 . A method in accordance with  claim 10  wherein the step of putting a polymerization mixture in the column casing comprises the steps of hydrolyzing a polymer in the polymerization mixture and modifying a hydroxyl formed in the step of hydrolyzing the polymer with a pyridine salt solution of chlorosulfonic acid. 
     
     
         13 . The method of  claim 12  in which the step of putting a polymerization mixture in the column casing includes the step of inserting at least one vinyl monomer, an initiator, and a porogen. 
     
     
         14 . A method of forming a chromatographic column comprising the steps of:
 putting a polymerization mixture in a column casing with a polymerization mixture comprising a functional monomer containing a sulfonic group; and   directly polymerizing the mixture to provide a strong cation exchanger.   
     
     
         15 . A method in accordance with  claim 14  wherein the step of putting a polymerization mixture in the column casing comprises the steps of hydrolyzing a polymer in the polymerization mixture and modifying a hydroxyl formed in the step of hydrolyzing the polymer. 
     
     
         16 . A method in accordance with  claim 15  wherein the step of putting a polymerization mixture in the column casing comprises the steps of hydrolyzing a polymer in the polymerization mixture and modifying a hydroxyl formed in the step of hydrolyzing the polymer with a pyridine salt solution of chlorosulfonic acid. 
     
     
         17 . The chromatographic column of  claim 14  in which said column casing is disposable and made of plastic. 
     
     
         18 . A method of controlling polymerization of a porous medium of a predetermined shape and size suitable for use in a separating device comprising the steps of:
 establishing a polymerization mixture including a porogen in the porous medium; and   controlling the polymerization with radiation that penetrates the medium to input energy throughout the medium of the predetermined shape.   
     
     
         19 . A method in accordance with  claim 18  in which said polymerization mixture includes a polymer, a cross-linking reagent and a cross-linking monomer, whereby rigidity, capacity and separation-effective opening distribution are controlled by the amount of cross-linking reagent and cross-linking monomer. 
     
     
         20 . A method in accordance with  claim 18  in which the step of controlling the polymerization with radiation includes the step of applying pressure to a polymerization mixture in a temperature controlled reaction chamber with a movable member. 
     
     
         22 . A method in accordance with  claim 18  in which the step of controlling the rate of the polymerization with radiation includes the step of applying pressure to a polymerization mixture in a temperature controlled reaction chamber with a movable member has a smooth surface positioned to contact said polymerization mixture as pressure is applied during polymerization. 
     
     
         22 . A method of controlling polymerization of a porous medium suitable for use in a separating device comprising the steps of:
 establishing a polymerization mixture including a monomer and a porogen; and   polymerizing said monomer in the presence of irradiation to control said polymerization.   
     
     
         23 . A method in accordance with  claim 22  in which said mixture is polymerized to form a solid support suitable for use in a separating device and said irradiation is throughout said mixture to avoid chromatographic nonuniformity in the distribution of separation effective openings. 
     
     
         24 . A method in accordance with  claim 23  in which the radiation is applied axially to an elongated mixture. 
     
     
         25 . A method in accordance with  claim 23  in which the radiation is visible light. 
     
     
         26 . A method in accordance with  claim 23  in which the radiation is ultraviolet light. 
     
     
         27 . A method in accordance with  claim 23  wherein the mixture comprises an initiator that is activated by light and a photoinitiator. 
     
     
         28 . A method in accordance with  claim 23  in which said irradiation is with x-rays.

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