Molecular separation column and use thereof

• US 4,384,957 A
• Filed: 07/28/1981
• Issued: 05/24/1983
• Est. Priority Date: 09/08/1980
• Status: Expired due to Term

• Current Assignee: Specialty Minerals Incorporated (Minerals Technologies Incorporated)
• Original Assignee: AMFM Incorporated
• Inventors: Ostreicher, Eugene A., Hou, Kenneth C., Marinaccio, Paul J., Fiore, Joseph V., Dailey, Nils L., Crowder, Alvin L. III
• Primary Examiner(s): Adee, John
• Application Number:
  US06/287,609
• Time in Patent Office: 665 Days
• Field of Search: 210/198.2, 210/502, 210/489, 210/503, 210/504, 210/656
• US Class Current: 210/656
• CPC Class Codes: B01D 15/22 relating to the construction of the column
• CPC Class Codes: B01J 20/28004 Sorbent size or size distribution, e.g. particle size
• CPC Class Codes: B01J 20/28028 Particles immobilised within fibres or filaments
• CPC Class Codes: B01J 20/28033 Membrane, sheet, cloth, pad, lamellar or mat
• 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 20/282 Porous sorbents ion exchange B01J39/00 - B01J41/00
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: G01N 2030/527 sorbent material in form of a membrane
• CPC Class Codes: G01N 30/56 Packing methods or coating methods

Abstract

A molecular separation chromotography column for effecting the differential distribution, between two phases, of the components of a sample flowing therethrough. The column contains a substantially homogeneous solid stationary phase which comprises a porous matrix of fiber having particulate immobilized therein, wherein at least one of said fiber or particulate is effective for molecular separation. The column is characterized by a reduced pressure drop, increased axial dispersion, more uniform peak shapes and better separations at high sample loading.

Claims

1. A chromatography column for effecting differential distribution, between two phases, of the components of a sample flowing therethrough, said column containing a solid stationary phase substantially homogeneous with respect to each component thereof, which comprises a porous matrix of fiber having particulate immobilized therein, at least one of said fiber or particulate therein having chromatographic functionality and being effective for chromatographic separation, wherein said solid stationary phase comprises a plurality of sheets of said solid stationary phase elements, the edges of said elements cooperating with the interior wall of the column to form a substantially fluid tight seal therewith, preventing any appreciable skewing or by-pass of fluid around the edges of the elements.

2. The chromatography column of claim 1, wherein the particulate has chromatographic functionality and is effective for chromatographic separation.

3. The chromatography column of claim 2, wherein the fibers are cellulose.

4. The chromatography column of claim 3, wherein the matrix comprises a major amount of long self bonding structural fiber and a minor amount of refined pulp fiber whose Canadian Standard Freeness is in the range of about +100 to -600 ml.

5. The chromatography column of claim 4, wherein the ratio of structural fiber to refined pulp fiber is 2:

1 to 10;

1.

6. The chromatography column of claim 5, wherein the ratio is 3:

1 to 5;

1.

7. The chromatography column of claims 1, 2, 3, 4, 5 or 6, wherein the amount of particulate is at least 10 weight percent of said solid stationary phase.

8. The chromatography column of claim 7, wherein the amount of particulate is from 10 to 80 weight percent of said solid stationary phase.

9. The chromatography column of claims 1, 2, 3, 4, 5 or 6, wherein said particulate has a mean particle size of about 5-100 microns.

10. The chromatography column of claim 4, wherein said structural fiber is cellulose having a Canadian Standard Freeness of +400 to +800 ml.

11. The chromatography column of claim 1, 2, 3, 4, 5 or 6, wherein said column is cylindrical and said sheets are discs.

12. The chromatography column of claim 11, wherein said solid stationary phase is hydrophilic swellable.

13. The chromatography column of claim 12, wherein said elements form a fluid-tight seal with the interior wall of the cylinder by water swellable fit therewith.

14. The chromatography column of claim 13, wherein said particulate has a mean particle size of from about 5 to 100 microns and is about 10 to 80 weight percent of said solid stationary phase, said structural fiber is cellulose having a Canadian Standard Freeness of +400 to +800 ml and a ratio of said structural fiber and refined pulp fiber is 3:

1-5;

1.

15. The chromatography column of claim 1, 2, 3 or 4, wherein said elements form a fluid-tight seal with the interior wall of the cylinder by compression friction fit therewith.

16. In a method of effecting a chromatographic separation by effecting a differential distribution of a sample'"'"'s components between two phases by passing a mobile phase through a chromatography column containing a solid stationary phase, the improvement which comprises employing as said stationary phase a porous matrix of fiber having particulate immobilized therein, at least one of said fiber or particulate having chromatographic functionality and being effective for chromatographic separation, said solid stationary phase being substantially homogeneous with respect to each component thereof, wherein said solid stationary phase comprises a plurality of sheets of said solid stationary phase elements, the edges of said elements cooperating with the interior wall of the column to form a substantially fluid tight seal therewith, preventing any appreciable skewing or bypass of fluid around the edges of the elements.

17. The method claim 16, wherein the particulate has chromatographic functionality and is effective for chromatographic separation.

18. The method of claim 16, wherein the mobile phase is liquid.

19. The method of claim 17, wherein the fibers are cellulose.

20. The method of claim 19, wherein the matrix comprises a major amount of long self bonding structural fiber and a minor amount of refined pulp fiber whose Canadian Standard Freeness is in the range of about +100 to -600 ml.

21. The method of claim 20, wherein the ratio of structural fiber to refined pulp fiber is 2:

1 to 10;

1.

22. The method of claim 21, wherein the ratio is 3:

1 to 5;

1.

23. The method of claims 16, 17, 18, 19 or 20 wherein the amount of particulate is at least 10 percent of said solid stationary phase.

24. The method of claim 23, wherein the amount of particulate is from 10 to 80 weight percent of said solid stationary phase.

25. The method of claims 16, 17, 18, 19 or 20, wherein said particulate has a mean particle size of about 5 to 100 microns.

26. The method of claim 20, wherein said structural fiber is cellulose having a Canadian Standard Freeness of +400 to +800 ml.

27. The method of claim 16, 17, 18, 19, 20, 21 or 22, wherein said column is cylindrical and said sheets are discs.

28. The method of claim 27, wherein said solid stationary phase is hydrophilic swellable.

29. The method of claim 28, wherein said elements form a fluid-tight seal with the interior wall of the cylinder by water swellable fit therewith.

30. The method of claim 29 wherein said particulate has a mean particle size of from about 5 to 100 microns and is about 10 to 80 weight percent of said solid stationary phase, said structural fiber is cellulose having a Canadian Standard Freeness of +400 to +800 ml and the ratio of said structural fiber and refined pulp fiber is 3:

1-5;

1.