Method and device for vacuum chromatography

• US 4,713,963 A
• Filed: 06/26/1986
• Issued: 12/22/1987
• Est. Priority Date: 06/26/1986
• Status: Expired due to Fees

• Current Assignee: Daryl Sharp
• Original Assignee: Daryl Sharp
• Inventors: Sharp, Daryl
• Primary Examiner(s): Tokar, Michael J.
• Assistant Examiner(s): Williams, Hezron E.
• Application Number:
  US06/879,022
• Time in Patent Office: 544 Days
• Field of Search: 73/23.1, 73/61.1 C, 55/270, 55/386, 210/656, 210/198.2
• US Class Current: 73/23.37
• CPC Class Codes: G01N 2030/165 retention gaps
• CPC Class Codes: G01N 2030/7226 OWTC, short capillaries or transfer line used as column
• CPC Class Codes: G01N 30/7206 interfaced to gas chromatograph interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04
• CPC Class Codes: G01N 30/728 Intermediate storage of effluent, including condensation on surface

Abstract

A method and device for analyzing samples containing mixtures of organic compounds using vacuum chromatography is disclosed. The method and device are particularly useful for obtaining mass spectra for identification purposes. The method involves passing a sample dissolved in a solvent through a column with a carrier gas and depositing a thin layer of the sample in the interior of a short column. The short column is then attached to an MS interface. The device comprises a combination of a variable molecular separator and a column alignment component. The alignment component may also be used as a direct probe injector. This device and method allow the separation and MS analysis of mixtures of intermediate molecular weight compounds.

Claims

1. A device for analysis of a sample using a mass spectrometer and a sample introduction column, said sample introduction column having a first end and a second end, said sample being deposited in a thin film on an adsorbent coating on the interior of the first end of the sample introduction column comprising:

(a) an MS transfer column having a bore greater in diameter than the exterior of said sample introduction column;

said bore having a chromatographic surface;

said MS transfer column having a first end and a second end;

said first end of said MS transfer column being insertable into the mass spectrometer source;

(b) a means for connecting the second end of said sample introduction column to a carrier gas source;

(c) an enclosed chamber into which the second end of said MS transfer column and the first end of said sample introduction column may be inserted;

(d) a means for axially aligning the sample introduction column and MS transfer column;

(e) a means for applying a vacuum source to said enclosed chamber;

(f) a means for supporting said sample introduction column at a point outside of said enclosed chamber; and

(g) a means for moving said sample introduction column along its axis so that the extent to which it is inserted into the MS transfer column may be controlled.

2. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 1, wherein the means for moving the sample introduction column along its axis comprises a bellows/micrometer drive mechanism.

3. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 1, wherein the means for applying a vacuum source to said enclosed chamber comprises a vacuum outlet having a bore greater in diameter than the bore of the MS transfer column, said vacuum outlet being connected to a vacuum pump.

4. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 3, wherein the MS transfer column is thirty cm or less in length and shorter than the sample introduction capillary.

5. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 3, wherein the means for moving the sample introduction column along its axis comprises guide rods connected to guide rod supports.

6. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 5, wherein the means for connecting the second end of the sample introduction column to a carrier gas source comprises a flow column and the means for supporting the sample introduction column comprises a union, said flow column having a first flow end and a second flow end, said union having a hollow cylindrical bore extending therethrough between a first union end and a second end, said first flow end being inserted into the second union end and said second end of the sample introduction capillary being inserted into the first union end, and said union being slidably movable along the guide rods such that movement of the union results in axial movement of the sample introduction capillary within the MS transfer column.

7. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 6, wherein the flow column, the enclosed chamber, the union and the MS transfer column are aligned in a line of sight path and the sample is not exposed to a chemically active surface in the device.

8. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 7, wherein the diameters of the flow column and the sample introduction column are different and the bore of the union is tapered so that the inner diameter of the second union end matches the inner diameter of the first flow end and the inner diameter of the first union end matches the inner diameter of the second end of the sample introduction column.

9. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 8, wherein the union comprises a single piece.

10. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 9, wherein the union is made of nickel and is enclosed by a polyimide resin coating which does not come into contact with the sample during analysis.

11. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 10, wherein the union is permanently attached to the sample introduction column.

12. A device for analysis of a sample using a mass spectrometer and a sample introduction column, said sample introduction column having a first end and a second end, said sample being deposited in a thin film on an adsorbent coating on the interior of the first end of the sample introduction column comprising:

(a) an MS transfer column having a bore greater in diameter than the exterior of said sample introduction column;

said bore having a chromatographic surface;

said MS transfer column having a first end and a second end;

said first end of said MS transfer column being insertable into the mass spectrometer source;

(b) a flow column for connecting the second end of said sample introduction column to a carrier gas source, said flow column having a first flow end and a second flow end;

(c) an enclosed chamber into which the second end of said MS transfer column and the first end of said sample introduction column may be inserted;

(d) a means for axially aligning the sample introduction column and MS transfer column;

(e) a means for applying a vacuum source to said enclosed chamber;

(f) guides rods and guide rod supports for moving said sample introduction column along its axis so that the extent to which the sample introduction column is inserted into the MS transfer column may be controlled; and

(g) a union for supporting said sample introduction column at a point outside of said enclosed chamber, said union having a hollow cylindrical bore extending therethrough between a first union end and a second union end, said first flow end being inserted into the second union end and said second end of the sample introduction capillary being inserted into the first union end, and said union being slidably movable along the guide rods such that movement of the union results in axial movement of the sample introduction capillary within the MS transfer column.

13. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 12, wherein the flow column, the enclosed chamber, the union and the MS transfer column are aligned in a line of sight path and the sample is not exposed to a chemically active surface in the device.

14. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 13, wherein the means for applying a vacuum source to said enclosed chamber comprises a vacuum outlet having a bore greater in diameter than the bore of the MS transfer column, said vacuum outlet being connected to a vacuum pump.

15. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 14, wherein the MS transfer column is thirty cm or less in length and shorter than the sample introduction capillary.

16. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 15, wherein the diameters of the flow column and the sample introduction column are different and the bore of the union is tapered so that the inner diameter of the second union end matches the inner diameter of the first flow end and the inner diameter of the first union end matches the inner diameter of the second end of the sample introduction column.

17. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 16, wherein the union comprises a single piece.

18. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 17, wherein the union is made of nickel and is enclosed by a polyimide resin coating which does not come into contact with the sample during analysis.

19. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 18, wherein the union is permanently attached to the sample introduction column.

20. A devie for analysis of a sample using a mass spectrometer and a sample introduction column, said sample introduction column having a first end and a second end, said sample being deposited in a thin film on an adsorbent coating on the interior of the first end of the sample introduction column comprising:

(a) an MS transfer column having a bore greater in diameter than the exterior of said sample introduction column;

said bore having a chromatographic surface;

said MS transfer column having a first end and a second end;

said first end of said MS transfer column being insertable into the mass spectrometer source;

(b) a flow column for connecting the second end of said sample introduction column to a carrier gas source, said flow column having a first flow end and a second flow end;

(c) an enclosed chamber into which the second end of said MB transfer column and the first end of said sample introduction column may be inserted;

(d) a means for axially aligning the sample introduction column and MS transfer column;

(e) a vacuum outlet having a bore greater in diameter than the bore of the MS transfer column by a factor of forty or more, said vacuum outlet being connected to a vacuum pump;

(f) a means for moving said sample introduction column along its axis so that the extent to which it is inserted into the MS transfer column may be controlled; and

(g) a union for supporting said sample introduction column at a point outside of said enclosed chamber, said union having a hollow cylindrical bore extending therethrough between a first union end and a second union end, said first flow end being inserted into the second union end and said second end of the sample introduction capillary being inserted into the first union end, said union being slidably movable such that movement of the union results in axial movement of the sample introduction capillary within the MS transfer column, and said flow column, said enclosed chamber, said union and said MS transfer column being aligned in a line of sight path.

21. The device for analysis of a sample using a mass spectrometer and a sample introduction column as recited in claim 20, wherein the MS transfer column is thirty cm or less in length and shorter than the sample introduction capillary and the sample is not exposed to a chemically active surface in the device.