Separation system, components of a separation system and methods of making and using them
First Claim
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.
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Accused Products
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.
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Citations
113 Claims
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1. A chromatographic system comprising:
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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. - View Dependent Claims (2, 3, 4, 5)
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6. A chromatographic system comprising:
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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. - View Dependent Claims (7, 8, 9)
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10. A chromatographic system comprising:
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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. - View Dependent Claims (11, 12, 13, 14, 15, 16, 17, 18)
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19. A separating system comprising:
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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. - View Dependent Claims (20, 21, 22, 23)
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24. A method of performing chromatography comprising the steps of:
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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. - View Dependent Claims (25, 26, 27, 28, 29)
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30. A method of performing chromatography comprising the steps of:
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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. - View Dependent Claims (31, 32, 33, 34, 35)
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36. A chromatographic column comprising:
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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. - View Dependent Claims (37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54)
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55. Apparatus for making a chromatographic column comprising:
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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. - View Dependent Claims (56, 57, 58)
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59. Apparatus for making a chromatographic column comprising:
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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.
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60. An apparatus for polymerizing chromatographic columns comprising:
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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. - View Dependent Claims (61)
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62. A method comprising the steps of:
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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. - View Dependent Claims (63)
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64. A method comprising the steps of:
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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. - View Dependent Claims (65, 66)
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67. A method of making a monolithic chromatographic column comprising the steps of:
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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. - View Dependent Claims (68, 69, 70)
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71. A method of making a monolithic chromatographic column comprising the steps of:
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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. - View Dependent Claims (72)
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73. A method of making a monolithic chromatographic column comprising the steps of:
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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.
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74. A method of making a weak cation column, comprising steps of:
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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. - View Dependent Claims (75, 76, 77, 78, 79, 80)
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81. A method of making a weak cation column, comprising steps of:
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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. - View Dependent Claims (82, 83, 84, 85)
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86. A method of making a strong anion column, comprising steps of:
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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. - View Dependent Claims (87, 88, 89, 90, 91)
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92. A method of making a strong anion column, comprising steps of:
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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. - View Dependent Claims (93, 94, 95, 96, 97)
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98. A method of making a monolithic permeable device for separating components of a sample, comprising the steps of:
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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.
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- 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.
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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.
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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.
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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.
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104. A method comprising the steps of:
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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. - View Dependent Claims (105, 106)
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107. A monolithic permeable device for separating components of a sample comprising:
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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.
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108. A method of making a monolithic permeable device for separating components of a sample, comprising the steps of:
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putting a polymerization mixture in a container;
polymerizing the polymerization mixture in the container using temperature-time moderation.
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109. A method of controlling polymerization of a porous medium comprising the steps of:
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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. - View Dependent Claims (110, 111, 112)
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113. A method of controlling polymerization of a porous medium comprising the steps of:
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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.
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Specification