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

• US 7,074,331 B2
• Filed: 06/25/2003
• Issued: 07/11/2006
• Est. Priority Date: 06/26/2002
• Status: Active Grant

• Current Assignee: Dionex Corporation (Thermo Fisher Scientific Incorporated)
• Original Assignee: Dionex Corporation (Thermo Fisher Scientific Incorporated)
• Inventors: Jiang, Tao, Xu, Mingcheng, Xie, Shaofeng, Allington, Robert W.
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US10/607,080
• Publication Number:
  US 20040020855A1
• Time in Patent Office: 1,112 Days
• Field of Search: 210/635, 210/656, 210/659, 210/502.1, 210/198.2, 210/748, 95/88, 961/01
• US Class Current: 210/635
• 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 20/283 based on silica
• CPC Class Codes: B01J 20/285 based on polymers
• CPC Class Codes: B01J 20/3064 Addition of pore forming agents, e.g. pore inducing or porogenic agents
• 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 2030/528 Monolithic sorbent material
• CPC Class Codes: G01N 2030/567 coating
• CPC Class Codes: G01N 30/30 of 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 are polymerized while pressure is applied through a piston having a smooth piston head in contact with the polymerization mixture. The pressure eliminates wall effect and changes the structure in the column. Similarly, some columns that have a tendency to swell in the presence of aqueous solutions and pressurized while the solution is applied to prevent swelling and wall effect. This procedure also changes the structure in the column. The size of the separation effective openings can be controlled by the amount of the pressure and pores eliminated. Uniformity in the direction flow is improved by controlling polymerization with radiation rather than with conducted heat.

Claims

1. A method of controlling polymerization of a porous medium of a predetermined shape and size having a radius of more than 10 mm suitable for use in a separating device comprising the steps of:

establishing a polymerization mixture including a porogen in the porous medium;

controlling the polymerization with radiation that penetrates the medium to input energy throughout the medium of the predetermined shape and size and at least a first substance that is caused by the radiation to affect the polymerization.

2. A method in accordance with claim 1 wherein the at least a first substance that is affected by the radiation is energized to emit further radiation.

3. A method in accordance with claim 2 in which the further radiation initiates polymerization.

4. A method in accordance with claim 2 wherein the first substance emits radiation that energizes a second substance to emit radiation.

5. A method in accordance with claim 1 in which the step of establishing a polymerization mixture includes the step of establishing a polymerization mixture that includes divinylbenzene.

6. A method in accordance with claim 1 in which the step of establishing a polymerization mixture includes the step of establishing a polymerization mixture that includes glycidyl methacrylate with hydrophobic surface groups.

7. A method in accordance with claim 1 in which the step of establishing a polymerization mixture includes the step of establishing a polymerization mixture that includes urea formaldehyde.

8. A method in accordance with claim 1 in which the step of establishing a polymerization mixture includes the step of establishing a polymerization mixture that includes silica.

9. A method in accordance with claim 1 in which the step of establishing a polymerization mixture includes the step of establishing a polymerization mixture that includes a vinyl group.

10. A method in accordance with claim 1 in which the step of establishing a polymerization mixture includes the step of establishing a polymerization mixture that includes a 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.

11. A method in accordance with claim 1 in which the step of controlling the rate of the polymerization with radiation and at least a first substance that is caused by the radiation to affect the polymerization includes the step of applying pressure to a polymerization mixture in a temperature controlled reaction chamber.

12. A method in accordance with claim 1 in which the step of controlling the rate of the polymerization with radiation and at least one substance that is caused by the radiation to affect the polymerization includes the step of applying pressure to a polymerization mixture in a temperature controlled reaction chamber with a movable member.

13. A method in accordance with claim 1 in which the step of controlling the rate of the polymerization with radiation and at least one substance that is caused by the radiation to affect the polymerization 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.

14. A method of controlling polymerization of a porous medium suitable for use in a separating device comprising the steps of:

establishing a polymerization mixture having a radius of more than 10 mm including a solvent;

controlling the rate of the polymerization with radiation and at least a first substance that is caused by the radiation to affect the polymerization.

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

preparing a polymerization mixture with a radius of more than 10 mm 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.

16. A method in accordance with claim 15 in which the step of preparing a polymerization mixture including a monomer, a porogen and at least one radiation sensitive substance includes the step of establishing a polymerization mixture that includes divinylbenzene.

17. A method in accordance with claim 15 in which the step of preparing a polymerization mixture including a monomer, a porogen and at least one radiation sensitive substance includes the step of preparing a mixture that includes glycidyl methacrylate with hydrophobic surface groups.

18. A method in accordance with claim 15 in which the step of preparing a polymerization mixture including a monomer, a porogen and at least one radiation sensitive substance includes the step of preparing a mixture that includes urea formaldehyde.

19. A method in accordance with claim 15 in which the step of preparing a polymerization mixture including a monomer, a porogen and at least one radiation sensitive substance includes the step of preparing a mixture that includes silica.

20. A method in accordance with claim 15 in which the step of preparing a polymerization mixture including a monomer, a porogen and at least one radiation sensitive substance includes the step of preparing a mixture that includes a vinyl group.

21. A method of polymerizing a mixture to form a solid support suitable for use in a separating device containing at least one monomer and a porogen comprising the step of irradiating the mixture with x-rays to avoid chromatographic nonuniformity in the distribution of separation effective openings.

22. A method in accordance with claim 21 wherein the porogen includes a mixture of alcohols;

said mixture of alcohols comprising first, second and third alcohols in a ratio of a first value in a range of a value between 2.8 and 3 to a second value in a range of 0.3 to 0.35 and a third value in a range of 0.3 to 0.35, wherein the first alcohol is ethanol, the second alcohol is methanol and the third alcohol is isopropanol.

23. A method in accordance with claim 21 wherein the porogen includes a mixture of alcohols;

said mixture of alcohols comprising first and second alcohols in a ratio of a first value in a range of a value between 1.8 and 2 to a value between 1.25 and 1.35, wherein the first alcohol is ethanol and the second alcohol is butanol.

24. A method of polymerizing a mixture to form a solid support suitable for use in a separating device containing at least one monomer and a solvent comprising the step of irradiating the mixture with x-rays to avoid chromatographic nonuniformity in the distribution of separation effective openings.

25. A method in accordance with claim 24 in which the z-rays are applied axially to an elongated mixture.

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

establishing a polymerization mixture including a solvent with a refractive index substantially the same as that of a polymer being formed;

controlling polymerization with radiation that penetrates the medium to input energy throughout the medium and at least a first substance that is caused by the radiation to affect the polymerization.

27. A method in accordance with claim 26 in which the radiation is visible light.

28. A method in accordance with claim 26 in which the radiation is ultraviolet light.

29. A method in accordance with claim 26 wherein the step of establishing a polymerization mixture includes the step of establishing a polymerization mixture comprising a initiator that is activated by light and a photoinitiator.