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

• US 7,922,909 B2
• Filed: 10/31/2007
• Issued: 04/12/2011
• 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:
  US11/932,343
• Publication Number:
  US 20080179773A1
• Time in Patent Office: 1,259 Days
• Field of Search: 961/01, 210/635, 210/656, 210/659, 210/748.01, 210/198.2, 210/502.1, 95/88
• 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 making a monolithic chromatography column, said method comprising the steps of

(a) adding a polymerization mixture containing a porogen to a chamber,

(b) polymerizing the mixture in the chamber under a pressure of at least 80 psi during at least part of said polymerization to form a monolithic polymer plug in the shape of a chromatography column, at least part of said polymerizing being performed by applying sufficient pressure to the polymerization mixture to prevent wall channeling openings in said monolithic polymer plug and during heating of the polymerization mixture to a controlled elevated temperature, and

(c) washing the polymer plug to remove the porogen.

2. The method of claim 1 in which said polymerization is performed under temperature-time moderating conditions, whereby temperature gradients arc controlled to prevent substantial cross sectional variations in the monolithic chromatographic column.

3. The method of claim 1 in which the monolithic polymer plug is formed in a capillary tube chamber.

4. The method of claim 1 in which polymerizing is performed under a pressure of at least 150 psi during at least part of said polymerizing.

5. The method of claim 1 in which polymerizing is performed under a pressure of at least 180 psi during at least part of said polymerizing.

6. The method of claim 1 in which the pressure is applied in intervals of increasing pressures.