Separation system, components of a separation system and methods of making and using them

• US 20050061745A1
• Filed: 08/06/2004
• Published: 03/24/2005
• Est. Priority Date: 06/26/2002
• Status: Abandoned Application

• Current Assignee: Dionex Corporation (Thermo Fisher Scientific Incorporated)
• Original Assignee: Teledyne Isco, Inc. (Thermo Fisher Scientific Incorporated)
• Inventors: Xu, Mingcheng, Xie, Shaofeng, Allington, Robert W.
• Application Number:
  US10/914,005
• Publication Number:
  US 20050061745A1
• Time in Patent Office: Days
• US Class Current: 210/656
• CPC Class Codes: B01D 15/20 relating to the conditioning of the sorbent material
• CPC Class Codes: B01D 15/206 Packing or coating
• CPC Class Codes: B01J 19/0013 Controlling the temperature of the process
• CPC Class Codes: B01J 19/18 Stationary reactors having moving elements inside B01J19/08, B01J19/26 take precedence
• CPC Class Codes: B01J 20/28042 Shaped bodies; Monolithic structures
• CPC Class Codes: B01J 20/28052 Several layers of identical or different sorbents stacked in a housing, e.g. in a column
• CPC Class Codes: B01J 20/283 based on silica
• CPC Class Codes: B01J 20/285 based on polymers
• CPC Class Codes: B01J 2219/00162 controlling the pressure
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: B01J 2220/82 Shaped bodies, e.g. monoliths, plugs, tubes, continuous beds
• CPC Class Codes: B01J 8/0005 Catalytic processes under superatmospheric pressure non-catalytic processes B01J3/00
• CPC Class Codes: G01N 2030/522 pressure
• CPC Class Codes: G01N 2030/525 surface properties, e.g. porosity
• CPC Class Codes: G01N 2030/528 Monolithic sorbent material
• CPC Class Codes: G01N 2030/567 coating
• CPC Class Codes: G01N 30/30 of temperature
• CPC Class Codes: G01N 30/52 Physical parameters
• CPC Class Codes: G01N 30/54 Temperature
• CPC Class Codes: G01N 30/56 Packing methods or coating methods

Abstract

Permeable polymeric monolithic materials are prepared in a column casing. In one embodiment, the permeable polymeric monolithic materials 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

1. A chromatographic system comprising:

a pumping system;

a chromatographic column and detector array;

a fraction collector system; and

a controller;

said chromatographic column and detector array including a plurality of chromatographic columns;

each of said chromatographic columns having a diameter size over 10 mm;

each of said chromatographic columns containing a corresponding one of a plurality of polymeric plugs without substantially inhomogeneous pore sizes caused by exotherms;

each of said polymeric plugs having the same characteristics, whereby said chromatographic columns separate sample in a similar manner;

a source of solvent;

said pumping system being arranged to supply solvent from the source of solvent to the chromatographic column and detector array under the control of the controller wherein effluent flows into the collector system from the chromatographic column and detector array under the control of the controller;

said controller being connected to receive signals from detectors in the chromatographic column and detector array indicating bands of solute and to activate the collector accordingly.

2. A chromatographic system according to claim 1 wherein a polymeric monolithic plug that is adjacent to walls of the chromatographic column has smooth walls.

3. A chromatographic system according to claim 1 in which at least some of the plurality of chromatographic columns include a corresponding temperature measuring device within a corresponding one of a plurality of plugs.

4. A chromatographic system according to claim 1 in which said corresponding one of a plurality of polymeric plugs is a temperature-time moderated polymeric plug.

5. A chromatographic system according to claim 4 in which said at least one permeable monolithic polymeric plug is a size-compensated polymeric plug.

6. A chromatographic system comprising:

a pumping system;

a column and detector array;

a fraction collector system; and

a controller;

said column and detector array including a plurality of columns;

each of said columns containing a corresponding one of a plurality of temperature-time moderated polymeric plugs;

each of said temperature-time moderated polymeric plugs having the same characteristics, whereby said columns separate sample in a similar manner;

a source of solvent;

said pumping system being arranged to supply solvent from the source of solvent to the column and detector array under the control of the controller wherein effluent flows into the collector system from the column and detector array under the control of the controller;

said controller being connected to receive signals from detectors in the column and detector array indicating bands of solute and to activate the fraction collector accordingly.

7. A chromatographic system according to claim 6 wherein surfaces of the temperature-developed polymeric plugs adjacent to column walls is smooth.

8. A chromatographic system according to claim 6 in which at least some of the plurality of columns include a corresponding temperature measuring device within a corresponding one of the plurality of plugs.

9. A chromatographic system according to claim 6 in which;

said solvent is supplied to a pump array having a different one of a plurality of pumps in said pump array communicating with a corresponding one of said plurality of columns in said column and detector array; and

a motor driven under the control of said controller to drive the array of pumps.

10. A chromatographic system comprising:

a sample injector;

at least one chromatographic column having a column casing and at least one permeable monolithic polymeric, temperature-time moderated plug inside the column casing positioned to receive a sample from the sample injector;

a solvent system in communication with the chromatographic column for supplying a solvent to the at least one chromatographic column, whereby the sample is separated into its components within the at least one chromatographic column;

said at least one column casing including a column casing wall with an internal column casing surface;

said at least one permeable monolithic polymeric, temperature-time moderated plug with smooth walls without discontinuities in contact with an internal surface of the column walls; and

a utility device for receiving fluid from said chromatographic column.

11. A chromatographic system in accordance with claim 10 in which said at least one chromatographic column comprises a plurality of columns.

12. A chromatographic system according to claim 11 in which at least some of the plurality of columns includes a corresponding temperature measuring device within a corresponding one of a plurality of plugs.

13. A chromatographic system in accordance with claim 10 in which the at least one permeable monolithic polymeric plug includes divinylbenzene.

14. A chromatographic system in accordance with claim 10 in which the at least one permeable monolithic polymeric plug includes glycidyl methacrylate with hydrophobic surface groups.

15. A chromatographic system in accordance with claim 10 in which the at least one permeable monolithic polymeric plug includes urea formaldehyde.

16. A chromatographic system in accordance with claim 10 in which the at least one permeable monolithic polymeric plug includes silica.

17. A chromatographic system in accordance with claim 10 in which the column casing is glass.

18. A chromatographic system according to claim 10 in which the at least one permeable monolithic plug is size compensated.

19. A separating system comprising:

a permeable, temperature-time moderated polymeric support;

a sample injector positioned to inject sample onto the permeable, temperature-time moderated polymeric support;

a solvent system in communication with the permeable, temperature-time moderated polymeric support, whereby the sample is separated into its components within the separating system; and

a utility device positioned to receive fluid from said permeable, temperature-time moderated polymeric support.

20. A chromatographic system according to claim 19 wherein the permeable, temperature-time moderated polymeric support has smooth walls.

21. A chromatographic system according to claim 19 in which the permeable, temperature-time moderated polymeric support includes a temperature measuring device.

22. A chromatographic system according to claim 19 in which said permeable, temperature-time moderated polymeric support is size compensated.

23. A chromatographic system in accordance with claim 19 in which the permeable, temperature-time moderated polymeric support includes divinylbenzene.

24. A method of performing chromatography comprising the steps of:

applying a sample to a chromatographic column having a column casing and a polymeric monolithic packing of over 10 mm diameter without substantially inhomogeneous pore sizes caused by exotherms; and

supplying a solvent to the chromatographic column, whereby the sample is separated into its components within the chromatographic column.

25. A method of performing chromatography in accordance with claim 24 in which the step of applying a sample to a chromatographic column having a column casing and a polymeric monolithic packing comprises the step of applying the sample to a chromatographic column that is size compensated.

26. A method in accordance with claim 24 in which the step of applying a sample to a chromatographic column having a column casing and a polymer monolithic packing includes the step of applying a sample to a permeable monolithic polymeric plug that includes a vinyl group.

27. A method in accordance with claim 24 in which the step of applying a sample to a chromatographic column having a column casing and a polymer monolithic packing comprises the step of applying a sample to a temperature-time moderated permeable monolithic polymeric plug.

28. A method in accordance with claim 24 in which the step of applying a sample to a chromatographic column having a column casing and a polymeric monolithic packing includes the step of applying a sample to a permeable monolithic polymeric plug that includes urea formaldehyde.

29. A method in accordance with claim 24 in which the step of applying a sample to a chromatographic column having a column casing and a polymeric monolithic packing includes the step of applying a sample to a permeable monolithic polymeric plug that includes a silica polymer.

30. A method of performing chromatography comprising the steps of:

applying a sample to a chromatographic column having a column casing and a temperature-time moderated polymer monolithic packing; and

supplying a solvent to the chromatographic column, whereby the sample is separated into its components within the chromatographic column.

31. A method of performing chromatography in accordance with claim 30 in which the step of applying a sample to a chromatographic column having a column casing and a temperature-time moderated polymer monolithic packing comprises the step of applying the sample to a chromatographic column that is size compensated.

32. A method in accordance with claim 30 in which the step of applying a sample to a chromatographic column having a column casing and a temperature-time moderated polymer monolithic packing includes the step of applying a sample to a permeable monolithic polymeric plug that includes a vinyl group.

33. A method in accordance with claim 30 in which the step of applying a sample to a chromatographic column having a column casing and a temperature-time moderated polymeric monolithic packing comprises the step of applying a sample to a size compensated permeable monolithic polymeric plug.

34. A method in accordance with claim 30 in which the step of applying a sample to a chromatographic column having a column casing and a polymeric monolithic packing includes the step of applying a sample to a permeable monolithic polymeric plug that includes urea formaldehyde.

35. A method in accordance with claim 30 in which the step of applying a sample to a chromatographic column having a column casing and a polymeric monolithic packing includes the step of applying a sample to a permeable monolithic polymeric plug that includes a silica polymer.

36. A chromatographic column comprising:

a chromatographic column support having internal column walls;

a permeable monolithic polymeric plug in said column walls;

said permeable monolithic polymeric plug being a polymer having separation-effective openings of a controlled size formed in the polymer by a porogen in a polymerization mixture before polymerization and controlled cross sectional uniformity by temperature-time moderation during polymerization.

37. A chromatographic column according to claim 36 wherein sizes of the separation-effective openings are controlled at least partly by pressure during polymerizations.

38. A chromatographic column in accordance with claim 36 in which the permeable monolithic polymeric plug has smooth walls and is size compensated by pressure.

39. A chromatographic column in accordance with claim 36 wherein there are substantially no pores within the permeable monolithic polymeric plug and the permeable monolithic polymeric plug has smooth walls.

40. A chromatographic column in accordance with claim 36 wherein there are substantially no pores within the permeable monolithic polymeric plug.

41. A chromatographic column in accordance with claim 36 wherein the permeable monolithic polymeric plug is free of channeling openings in the walls of the plug.

42. A chromatographic column in accordance with claim 36 wherein the permeable monolithic polymeric plug is formed principally of methacrylate.

43. A chromatographic column in accordance with claim 36 wherein the permeable monolithic polymeric plug is formed principally of methacrylate with hydrophobic surface groups.

44. A chromatographic column in accordance with claim 36 wherein the permeable monolithic polymeric plug is formed principally of urea formaldehyde.

45. A chromatographic column in accordance with claim 36 wherein the permeable monolithic polymeric plug is formed principally of silica.

46. A chromatographic column in accordance with claim 36 wherein the permeable monolithic polymeric plug is principally formed of polymers of glycidyl methacrylate and of ethylene dimethacrylate in a ratio by weight in the range of from 1 to 1 and 2 to 1.

47. A chromatographic column in accordance with claim 36 wherein the permeable monolithic polymeric plug is principally formed of polymers of glycidyl methacrylate and of ethylene dimethacrylate in a ratio by weight of 3 to 2.

48. A chromatographic column in accordance with claim 36 in which the permeable monolithic polymeric plug includes as its principal component a mixture of divinylbenzene and styrene in a ratio in the range of 3 to 1 and 9 to 1.

49. A chromatographic column in accordance with claim 36 in which the permeable monolithic polymeric plug includes as its principal component a mixture of divinylbenzene and styrene in a ratio in the range of 4 to 1.

50. A chromatographic column in accordance with claim 36 in which the column is in the range of 35 percent and 80 percent by weight divinylbenzene.

51. A chromatographic column in accordance with claim 36 in which the column is 64 percent by weight divinylbenzene.

52. A chromatographic column in accordance with claim 36 in which the column includes a polymeric plug with a temperature measuring device within it.

53. A chromatographic column in accordance with claim 36 having a diameter of over 10 mm.

54. A chromatographic column in accordance with claim 36 in which a volume of pores per square millimeter and mean size of pore openings in the direction of a longitudinal axis of the column per square millimeter does not vary from location to location and does not vary by more than 5 percent.

55. Apparatus for making a chromatographic column comprising:

a temperature controlled reaction chamber adapted to contain a polymerization mixture during polymerization; and

means for varying the temperature during polymerization, whereby the polymerization mixture is temperature-time moderated.

56. Apparatus for making a chromatographic column in accordance with claim 55 further including means for applying pressure to said polymerization mixture in said temperature controlled reaction chamber.

57. Apparatus according to claim 56 wherein said means for applying pressure is a means for applying pressure with a movable member.

58. Apparatus according to claim 57 in which said movable member has a smooth surface positioned to contact said polymerization mixture as pressure is applied during polymerization.

59. Apparatus for making a chromatographic column comprising:

a temperature controlled reaction chamber adapted to contain a polymerization mixture during polymerization to form a plug;

said temperature controlled reaction chamber including means for temperature-time moderation; and

aqueous processing means for applying an aqueous solution to the plug; and

means for applying pressure to said plug to reduce voids in the plug.

60. An apparatus for polymerizing chromatographic columns comprising:

a temperature controlled reaction chamber adapted to contain a polymerization mixture during polymerization to form a plug;

means for conducting heat from outside a column into the column at its surface whereby the rate of polymerization is kept below the self-sustaining temperature but polymerized homogeneously;

radiation means for applying radiation to the plug; and

control means for controlling the radiation.

61. An apparatus in accordance with claim 60 further including means for applying pressure to the plug to reduce voids in the plug.

62. A method comprising the steps of:

putting a polymerization mixture in a column casing;

polymerizing the polymerization mixture in the column casing using a combination of low and high temperature polymerization.

63. A method in accordance with claim 62 in which the step of putting a polymerization mixture in a column casing comprises the step of putting a polymerization mixture in a column casing having a diameter of at least 10 mm.

64. A method 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.

65. A method in accordance with claim 64 wherein the step of putting a polymerization mixture in a 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.

66. A method in accordance with claim 64 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.

67. A method of making a monolithic chromatographic column comprising the steps of:

preparing a polymerization mixture;

performing polymerization under temperature-time moderating conditions, whereby temperature gradients are controlled to prevent spacial cross sectional variations in the monolithic chromatographic column.

68. A method in accordance with claim 67 in which the polymerization is performed under pressure, whereby sufficient pressure is applied to prevent voids from being formed caused by vacuum due to shrinkage during polymerization.

69. The method of claim 67 in which the step of performing polymerization includes the step of inserting a polymerization mixture into the walls of a chromatographic column and polymerizing in a temperature controlled chamber during at least part of the time pressure is being applied to the polymerization mixture.

70. The method of claim 69 in which the step of inserting a polymerization mixture includes the step of inserting at least one vinyl monomer, an initiator, and a porogen.

71. A method of making a monolithic chromatographic column comprising the steps of:

adding a polymerization mixture containing a porogen to a closed container;

polymerizing the mixture under temperature-time moderation to form a size compensated polymer plug; and

washing the polymer plug to remove the porogen.

72. A method according to claim 71 in which the step of polymerizing the mixture includes the step of polymerizing the mixture under pressure to form a polymer plug, whereby sufficient pressure is applied to prevent voids from being formed caused by vacuum due to shrinkage during polymerization.

73. A method of making a monolithic chromatographic column comprising the steps of:

preparing a polymerization mixture including a porogen;

performing polymerization with temperature-time moderation to form a polymer plug;

washing the polymer plug to remove the porogen, wherein the plug tends to swell; and

applying pressure to prevent swelling of the polymer plug and eliminate voids.

74. A method of making a weak cation column, comprising steps of:

mixing GMA, MMA, EDMA, an initiator and a porogen to form a polymerization mixture; and

polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug.

75. A method of making a weak cation column in accordance with claim 74 wherein the step of mixing includes the step of supplying a polymerization mixture comprising 1 part of GMA to between 4 and 6 parts of MMA and 10 and 14 parts of EDMA and an initiator to a container.

76. A method of making a weak cation column in accordance with claim 74 wherein the step of polymerizing includes the step of polymerizing at a gradient temperature starting at the control initiation point at a low temperature and gradually increasing the temperature to a safe point and curing at a a higher temperature wherein temperature run-away is avoided and adequate polymerization and cross linking is obtained.

77. A method of making a weak cation column in accordance with claim 74 wherein the step of polymerizing includes the step of polymerizing at a gradient temperature starting at the control initiation point at a value between 35 and 45°

C. and gradually increasing the temperature to a safe point and curing at a higher temperature.

78. A method of making a weak cation column in accordance with claim 75 wherein the step of polymerizing includes the step of polymerizing at a gradient temperature starting at the control initiation point at and gradually increased to a safe point and curing at a higher temperature.

79. A method in accordance with claim 74 wherein the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug includes the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug without substantial non-uniform characteristics caused by temperature gradients.

80. A method in accordance with claim 74 wherein the step or polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug includes the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug with substantial non-uniform characteristics caused by temperature gradients resulting from exotherms.

81. A method of making a weak cation column, comprising steps of:

applying a polymerization mixture comprising 1 part of GMA to between 4 and 6 parts of MMA and 10 and 14 parts of EDMA and an initiator into a container;

shaking the mixture gently until the mixture becomes a homogeneous solution;

weighing a porogen into the homogeneous solution and shaking until the new mixture is homogeneous to form a polymerization solution;

degassing;

putting the polymerization solution in the column;

polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug; and

washing the plug to remove the porogen.

82. A method in accordance with claim 81, wherein the column includes means for applying pressure to the polymerization solution further comprising the steps of sealing the column and applying pressure to the polymerization mixture.

83. A method in accordance with claim 81 wherein the polymerizing mixture is polymerized at a gradient temperature starting at the control initiation point at a value between 35 and 45°

C. and gradually increased to a safe point in 12 hours and cured at a temperature of between 55 and 65°

C. for 24 hours.

84. A method in accordance with claim 81 wherein the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug includes the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug without substantial non-uniform characteristics caused by temperature gradients.

85. A method in accordance with claim 81 wherein the step or polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug includes the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug with substantial non-uniform characteristics caused by temperature gradients resulting from exotherms.

86. A method of making a strong anion column, comprising steps of:

mixing GMA, ATMS, EDMA, an initiator and a porogen to form a polymerization mixture; and

polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug.

87. A method of making a strong anion column in accordance with claim 86 wherein the step of mixing includes the step of supplying a polymerization mixture comprising between 2 and 4 parts of GMA to between 2 and 4 parts of ATMS to between 7 and 11 parts of EDMA and an initiator into a container.

88. A method in accordance with claim 86 wherein the step of polymerizing includes the step of polymerizing at a gradient temperature starting at the control initiation point at a low temperature and gradually increasing the temperature to a safe point and curing at a a higher temperature wherein temperature run-away is avoided and adequate polymerization and cross linking is obtained.

89. A method in accordance with claim 86 wherein the step of polymerizing includes the step of polymerizing at a gradient temperature starting at the control initiation point at a value between 35 and 45°

C. and gradually increasing the temperature to a safe point and curing at a higher temperature.

90. A method in accordance with claim 87 wherein the step of polymerizing includes the step of polymerizing at a gradient temperature starting at the control initiation point at and gradually increased to a safe point and curing at a higher temperature.

91. A method in accordance with claim 86 wherein the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug includes the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug without substantial non-uniform characteristics caused by temperature gradients.

92. A method of making a strong anion column, comprising steps of:

applying a polymerization mixture comprising between 2 and 4 parts of GMA to between 2 and 4 parts of ATMS to between 7 and 11 parts of EDMA and an initiator into a container;

shaking the mixture gently until the mixture becomes a homogeneous solution;

weighing a porogen into the homogeneous solution and shaking until the new mixture is homogeneous to form a polymerization solution;

degassing;

putting the polymerization solution in the column;

polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug; and

washing the plug to remove the porogen.

93. A method in accordance with claim 92, wherein the column includes means for applying pressure to the polymerization solution further comprising the steps of sealing the column and applying pressure to the polymerization mixture.

94. A method in accordance with claim 92 wherein the polymerizing mixture is polymerized at a gradient temperature starting at the control initiation point at a value between 35 and 45°

C. and increasing gradually to a safe-point at between 55 and 65°

C. in 12 hours and cured at a temperature of between 55 and 65°

C. for 24 hours.

95. A method in accordance with claim 92 wherein the polymerizing mixture is polymerized at a temperature of between 35 and 45°

C. for 72 hours and then cured at a temperature of between 55 and 65°

C. for 24 hours.

96. A method in accordance with claim 92 wherein the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug includes the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug without substantial non-uniform characteristics caused by temperature gradients.

97. A method in accordance with claim 92 wherein the step or polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug includes the step of polymerizing the polymerization solution in the column under temperature-time moderation conditions to form a plug with substantial non-uniform characteristics caused by temperature gradients resulting from exotherms.

98. A method of making a monolithic permeable device for separating components of a sample, comprising the steps of:

preparing a polymerization mixture including a monomer, a porogen and at least one radiation sensitive substance;

said radiation sensitive substance comprising one or more substances selected from a group consisting of photo initiators, solvents, x-ray sensitizers and scintillators; and

irradiating the polymerization mixture; and

temperature-time moderating the polymerization mixture.

99. A method of polymerizing a mixture to form a solid support containing at least one monomer and a porogen comprising the step of irradiating the mixture with x-rays and polymerizing under temperature-time moderation.

101. A method in accordance with claim 99 in which the x-rays are applied axially to an elongated mixture.

100. A method of polymerizing a mixture to form a solid support containing at least one monomer and a solvent comprising the step of irradiating the mixture with x-rays and applying temperature-time moderation.

102. A polymerization mixture comprising 1 part of GMA to between 4 and 6 parts of MMA and 10 and 14 parts of EDMA and an initiator, wherein a temperature-time moderated polymer may be formed having weak cation separating characteristics.

103. A polymerization mixture comprising between 2 and 4 parts of GMA to between 2 and 4 parts of ATMS to between 7 and 11 parts of EDMA and an initiator, wherein a temperature-time moderated polymer may be formed having strong anion separating characteristics.

104. A method comprising the steps of:

putting a polymerization mixture in a column casing with the polymerization mixture comprising a functional monomer containing a sulfonic group; and

directly polymerizing the mixture to provide a strong cation exchanger.

105. A method in accordance with claim 104 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.

106. A method in accordance with claim 104 wherein the step of puffing 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.

107. A monolithic permeable device for separating components of a sample comprising:

a permeable monolithic support;

said permeable monolithic support being a polymer having separation effective openings of a controlled size formed in the polymer by a porogen in a polymerization mixture before polymerization and controlled in cross sectional uniformity by temperature-time moderation during polymerization.

108. A method of making a monolithic permeable device for separating components of a sample, comprising the steps of:

putting a polymerization mixture in a container;

polymerizing the polymerization mixture in the container using temperature-time moderation.

109. A method of controlling polymerization of a porous medium comprising the steps of:

establishing a polymerization mixture including a porogen;

controlling the rate of the polymerization with radiation and temperature-time moderation of at least one substance that is caused by the radiation to affect the polymerization.

110. A method in accordance with claim 109 wherein the at least one substance that is caused by the radiation to affect the polymerization is energized to emit further radiation.

111. A method in accordance with claim 109 in which the further radiation initiates polymerization.

112. A method in accordance with claim 109 wherein at least one of the at least one substance emits radiation that energizes a second substance to emit radiation.

113. A method of controlling polymerization of a porous medium comprising the steps of:

establishing a polymerization mixture including a solvent;

controlling the rate of the polymerization with radiation temperature-time moderation and at least one substance that is caused by the radiation to affect the polymerization.