Fast gas chromatograph method and device for analyzing a sample

• US 8,591,630 B2
• Filed: 10/06/2010
• Issued: 11/26/2013
• Est. Priority Date: 10/06/2010
• Status: Active Grant

• Current Assignee: Aviv Amirav
• Original Assignee: Aviv Amirav
• Inventors: Amirav, Aviv, Fialkov, Alexander B.
• Primary Examiner(s): CLEMENTE, ROBERT ARTHUR
• Application Number:
  US12/899,288
• Publication Number:
  US 20120085148A1
• Time in Patent Office: 1,147 Days
• Field of Search: 95/82, 95/87, 961/01, 961/03, 961/05, 961/06, 73/233.5, 73/233.9, 73/234.2
• US Class Current: 95/87
• CPC Class Codes: G01N 2030/3061 column or associated structural member used as heater
• CPC Class Codes: G01N 2030/3069 electrical resistance used to determine control temperature
• CPC Class Codes: G01N 2030/3076 using specially adapted T(t) profile
• CPC Class Codes: G01N 30/30 of temperature
• CPC Class Codes: G01N 30/463 for multidimensional chromatography
• 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

Abstract

In a fast gas chromatograph (GC) method and device for obtaining fast gas chromatography analysis, a capillary gas chromatography column is inserted into a resistively heated metal tube located mostly outside a standard gas chromatograph oven, which may serve as a heated transfer line to a flexible column that enters the resistively heated metal tube from its injector and exits into its detector. The fast GC device enables less than one minute full range temperature programming and cooling back analysis cycle time. The fast GC according to one embodiment is combined with mass spectrometry with supersonic molecular beams for the provision of fast analysis cycle time together with highly informative mass spectral information for improved sample analysis and identification.

Claims

1. A method for fast gas chromatography analysis, said method comprising:

injecting a sample to be analyzed into a gas chromatograph injector that is coupled to a gas chromatography capillary column;

transferring said sample in said injector into said capillary column with a carrier gas flow;

transferring said capillary column through a gas chromatograph oven as a flexible non-rigid capillary into a resistively heated metal tube having opposing input and output ends;

locating the input and output ends of said resistively heated metal tube near a hole in the gas chromatograph oven body so that a substantial portion of said column in said heated metal tube is located outside said gas chromatograph oven and so that said input and output ends project a short distance inside said gas chromatograph oven;

introducing an end of said portion of said capillary column that is outside the gas chromatograph oven from said heated metal tube into said gas chromatograph oven as a flexible capillary, wherein the capillary column and the resistively heated metal tube are configured such that transferring the capillary column through the gas chromatograph oven into the resistively heated metal tube and introducing the capillary column from the heated metal tube into the gas chromatograph oven is reversible, without removal of the resistively heated metal tube;

connecting said flexible capillary with a transfer line that leads into a gas chromatograph detector;

connecting both ends of said resistively heated metal tube to a power supply; and

resistively heating said heated metal tube in a time programmed manner to facilitate fast temperature program of said capillary column;

wherein said capillary column is flexibly connected to said gas chromatograph injector and detector.

2. The method according to claim 1, wherein:

said sample in said carrier gas is transferred via a heated transfer line into a supersonic nozzle; and

compounds in said sample expand from said supersonic nozzle into a vacuum system while forming a supersonic molecular beam with vibrationally cold sample molecules which are ionized in said supersonic molecular beams with electrons in a fly through electron ionization ion source followed by mass analysis, ion detection and data analysis of the data obtained from the resulting mass spectral information, for identifying and/or quantifying the chemical content of said sample.

3. The method according to claim 1 wherein said capillary column is freely inserted into said heated metal tube in such a way that both ends of said capillary column protrude from said heated metal tube.

4. The method according to claim 1, including removing the column and inserting a replacement column without replacing the heated metal tube.

5. The method according to claim 1, wherein, during use, said gas chromatograph oven is heated to a temperature similar to that of the detector transfer line so that said gas chromatograph oven serves as a portion of transfer lines of said fast gas chromatograph from the injector and to the detector.

6. The method according to claim 1, wherein said carrier gas flow rate is above 4 ml/min.

7. The method according to claim 1, wherein said capillary column length is below 4 meters.

8. The method according to claim 1, wherein the full analysis cycle time is achieved in under one minute.

9. The method according to claim 1, wherein said capillary column extends from both input and output ends of said heating metal tube.

10. The method according to claim 1, wherein said capillary column is cut from a standard length capillary column without its assembly on a mounting tool or bundling with a heater and/or insulation material.

11. The method according to claim 1, wherein said resistively heated metal tube is located and mounted on top of a standard gas chromatograph oven.

12. The method according to claim 1, wherein said resistively heated metal tube is located in an enclosure and said enclosure further includes a time-programmable air cooling fan.

13. The method according to claim 1, wherein said resistively heated metal tube is interfaced with said gas chromatograph oven in a way to minimize temporary cold spots and hot spots.

14. The method according to claim 1, wherein the fast gas chromatograph is an accessory for the conversion of a standard gas chromatograph into a fast gas chromatograph as an add-on device without the removal of any substantial component from the standard gas chromatograph.

15. The method according to claim 1, wherein said injector is an Open Probe.

16. The method according to claim 1, wherein said fast gas chromatograph serves as a second dimension fast gas chromatograph of a comprehensive GC×

GC or two dimensional GC-GC.

17. The method according to claim 1, wherein said sample is introduced into said gas chromatograph injector from the output of a liquid chromatograph for obtaining fast comprehensive LC×

GC and/or LC×

GC-MS.

18. The method according to claim 1, wherein said capillary column end is connected in a T connected with another capillary column and transfer line for enabling fast switching between standard gas chromatography analysis and fast gas chromatography analysis without a change of hardware.

19. A fast gas chromatograph device for obtaining fast gas chromatography analysis, said device comprising:

a gas chromatograph injector;

a gas chromatograph detector

a capillary gas chromatography column;

a connector for flexibly connecting said capillary column with said gas chromatograph injector;

a source of carrier gas flow for the transferring of sample vapor in said injector into said capillary column;

a metal tube having opposing input and output ends that is adapted to be resistively heated and that is located mostly outside a gas chromatograph oven and that is coupled via a flexible capillary column to said gas chromatograph injector and detector;

a transfer line with a connector for flexibly connecting said flexible capillary column to a gas chromatograph detector;

said input and output ends of said metal tube being located near a hole in the gas chromatograph oven body so that a substantial portion of said column in said metal tube is located outside said gas chromatograph oven;

means for coupling a power supply to both ends of said metal tube for its resistive heating; and

a controller configured for resistively heating said metal tube in a time programmed manner to facilitate fast temperature program of said capillary column in said heated metal tube, wherein the capillary column and the resistively heated metal tube are configured to provide for changing the capillary column without detaching and changing the resistively heated metal tube.

20. The device according to claim 19, further comprising a supersonic nozzle for the formation a supersonic molecular beam with vibrationally cold sample molecules which are ionized in said supersonic molecular beams by electrons in a fly through electron ionization ion source.

21. The device according to claim 19 wherein said heated metal tube enables free insertion of said capillary column into it in such a way that both ends of said capillary column are hanged out from said metal tube.

22. The device according to claim 19, further comprising means for gas chromatography capillary column replacement without the replacement of said metal tube.

23. The device according to claim 19, wherein during use said gas chromatograph oven is heated to a temperature substantially similar to that of the detector transfer line so that said gas chromatograph oven is adapted to serve as a portion of transfer lines of said fast gas chromatograph from the injector and to the detector.

24. The device according to claim 19, further comprising means for the provision of carrier gas flow rate above 4 ml/min.

25. The device according to claim 19, wherein said capillary column length is below 4 meters.

26. The device according to claim 19, wherein the full analysis cycle time can be achieved in under one minute.

27. The device according to claim 19, wherein said capillary column extends before and after said heating metal tube.

28. The device according to claim 19, wherein said capillary column is cut from a standard length gas chromatography capillary column without its assembly on a mounting tool or bundling with a heater and/or insulation material.

29. The device according to claim 19, wherein said metal tube is located and mounted on top of a standard gas chromatograph oven.

30. The device according to claim 19, further comprising an enclosure with an air cooling fan.

31. The device according to claim 19, further comprising means for minimizing thermal cold spots and hot spots near an interface of said flexible capillary column and said metal tube.

32. The device according to claim 19, wherein the fast gas chromatograph device further comprises means for the conversion of a standard gas chromatograph into a fast gas chromatograph without the removal of any substantial component from the standard gas chromatograph.

33. The device according to claim 19, wherein the gas chromatograph injector comprises an open probe.

34. The device according to claim 19, further comprising means for using said fast gas chromatograph as a second dimension fast gas chromatograph of a comprehensive GC×

GC or two dimensional GC-GC.

35. The device according to claim 19, further comprising a liquid chromatograph for the introduction of its eluted sample into said gas chromatograph injector for obtaining fast comprehensive LC×

GC and/or LC×

GC-MS.

36. The device according to claim 19, further comprising a T-connector for the simultaneous connection of said capillary column with another capillary column for enabling fast switching between standard gas chromatography analysis and fast gas chromatography analysis without a change of hardware.