Micromachined gas chromatography columns for fast separation of Organophosphonate and Organosulfur compounds and methods for deactivating same

• US 8,152,908 B2
• Filed: 12/18/2008
• Issued: 04/10/2012
• Est. Priority Date: 01/16/2008
• Status: Active Grant

• Current Assignee: Board of Trustees of The University of Illinois
• Original Assignee: Board of Trustees of The University of Illinois
• Inventors: Masel, Richard I., Radadia, Adarsh D.
• Primary Examiner(s): CLEMENTE, ROBERT ARTHUR
• Application Number:
  US12/337,882
• Publication Number:
  US 20090211452A1
• Time in Patent Office: 1,209 Days
• Field of Search: 961/01, 95/82, 95/83, 73/233.9, 210/198.2, 210/656, 427230-239
• US Class Current: 96/101
• CPC Class Codes: G01N 2030/0095 Separation specially adapted for use outside laboratory, e.g. field sampling, portable equipments
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 30/6095 Micromachined or nanomachined, e.g. micro- or nanosize

Abstract

Improved microcolumns and methods for producing microcolumns particularly suitable for use in gas chromatographs are disclosed. In particular, following deposition of the stationary phase coating, the microcolumns are subjected to a postcoating treatment with a molecule that binds to the active sites in the stationary phase column thereby eliminating or reducing loss of gas chromatograph performance associated with those active sites. The postcoating treatment molecule binds to the same active sites as the analytes of interest.

Claims

1. A Gas chromatography (GC) column, comprising:

a plurality of column walls each having a deactivated inner surface;

a stationary phase layer deposited on the deactivated inner surface of said plurality of column walls;

a plurality of binding sites in said stationary phase layer; and

a post-coating molecule bound to at least one of said plurality of binding sites in said stationary phase layer;

wherein the post-coating molecule is one or more compounds selected from the group consisting of a thiol, a phosphine, an amine,

2. The GC column of claim 1, wherein the inner surface of said plurality of column walls has been deactivated with a compound selected from the group consisting of DMDCS, Ah3P, and DPTMDS.

3. The GC column of claim 1, wherein said stationary phase layer has a thickness of about 0.1 μ

M.

4. The GC column of claim 1, wherein said stationary phase layer is uniformly spread over the inner surface of said plurality of column walls.

5. The GC column of claim 1, wherein said plurality of column walls has a serpentine configuration.

6. The GC column of claim 1, wherein said plurality of column walls are rounded.

7. The GC column of claim 1, wherein said post-coating molecule comprises a structure of Formula I:

8. The GC column of claim 1, wherein the post-coating molecule comprises the structure of Formula II:

9. A method for preparing a gas chromatograph (GC) column, said method comprising the steps of

deactivating a plurality of walls of a GC column;

depositing a stationary phase in the GC column; and

treating the GC column with a molecule such that the molecule binds to active sites in the stationary phase of the column;

wherein the molecule is one or more compounds selected from the group consisting of an acid including hydrocarbon ligands, a base including hydrocarbon ligands, a thiol, a phosphine, and an amine.

10. The method of claim 9, wherein the stationary phase in said depositing step is applied at a pressure of about 0.9 psi and at a concentration of about 10 w/v %.

11. The method of claim 9, wherein the deactivating step comprises a method selected from the group consisting of silylation, perisilylation, and deactivation using an organosilicon hydride.

12. The method of claim 11, wherein the silylation is performed using DMDCS, the perisilylation is performed using Ah3P, and the deactivation with the organosilicon hydride is performed using DPTMDS.

13. The method of claim 9, wherein the molecule in said treating step comprises a structure of Formula I:

14. The method of claim 13, wherein the molecule comprises the structure of Formula II:

15. A gas chromatograph (GC) column prepared by the method of claim 9.

16. The GC column of claim 15, wherein the molecule in said treating step comprises a structure of Formula I:

17. The GC column of claim 15, wherein the molecule comprises the structure of Formula II:

18. The GC column of claim 15, wherein the molecule comprises the structure of Formula III: