IP Library › Granted Patent US 12,306,078
Granted Patent B2
US 12,306,078 · App. 17/428,820 · Granted May 20, 2025

Dynamic headspace vacuum transfer “in trap” extraction method and apparatus

Inventors: Pascal Fuchsmann (Torny-le-Grand, CH); Fabian Wahl (Buchs, CH); Patrick Bischoff (Münsingen, CH); Mireille Tena Stern (Fribourg, CH)
Assignee: CTC Analytics AG
G01N1/2226G01N1/405G01N30/06G01N2001/2229G01N2030/884
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Quick Facts
Patent No.
US 12,306,078
App. No.
17/428,820
Granted
May 20, 2025
Kind
B2
Abstract

A headspace extraction and analysis method for volatile compounds can be performed in automatic mode in a HS-ITEX apparatus adapted to be additionally connectable to a vacuum source. The method includes extracting the headspace by sucking volatile compounds into a sorbent-containing trap followed by desorption into the injector of a GC-MS analyzer.

Claims (38)

1. A headspace extraction and analysis method for volatile compounds, wherein a continuous flow of volatile compounds is forced by applying reduced pressure conditions, the method comprising:

(i) inserting a needle of a sampling means via a septum into a headspace above a solid or liquid sample contained in a container closed by said septum, wherein said sampling means has a trap filled with at least one sorbent, said trap has a first end and a second end, at the first end the trap is connected to the needle, and at the second end the trap is connected with at least one flow channel connected to a valve that is switchable between a vacuum source and an inert gas source, the valve being fluidly connected to a gas distribution block having a first port connected to the at least one flow channel, a second port connected to the vacuum source and a third port connected to the inert gas source,

(ii) connecting the vacuum source to the sampling means on the side of the second end of the trap via the valve and the gas distribution block, so that volatile compounds in the headspace are sucked out from the container into the trap,

(iii) removing the sampling means from the container,

(iv) connecting the inert gas source to the sampling means via the valve and the gas distribution block to dry the sampling means by flowing an inert gas supplied by the inert gas source through the sampling means from the second side,

(v) inserting the needle into an injector of a gas chromatography apparatus,

(vi) desorbing the volatile compounds from the trap by flowing the inert gas supplied by the insert gas source through the at least one sorbent from the second side,

(vii) analyzing the volatile compounds and

(viii) cleaning the trap and needle by flushing with the inert gas supplied by the inert gas source.

2. The method of claim 1 , wherein the temperature of the trap during steps (i) to (iii) is in the range of 0 to 100° C.

3. The method of claim 1 , wherein the temperature of the trap during step (ii) is in the range from 10° C. to 40° C.

4. A headspace extraction and analysis method for volatile organic compounds, wherein a continuous flow of volatile organic compounds is forced by applying reduced pressure conditions, the method comprising:

(i) inserting a needle of a sampling means through a septum into a headspace above a solid or liquid sample contained in a container closed by the septum, wherein the sampling means includes a trap filled with at least one sorbent, the trap has a first end and a second end, the first end of the trap is connected to the needle, and the second end of the trap is connected with at least one flow channel connected to a valve that is switchable between a vacuum source and an inert gas source,

(ii) connecting the vacuum source to the second end of the trap via the valve, wherein volatile organic compounds in the headspace are suctioned out from the headspace of the container and are adsorbed by the at least one sorbent in the trap,

(iii) removing the needle of the sampling means from the septum and the container,

(iv) connecting the inert gas source to the second end of the trap via the valve, wherein organic compounds adsorbed by the sorbent are dried by flowing an inert gas supplied by the inert gas source through the trap, the inert gas and moisture exiting the trap via the needle,

(v) inserting the needle into an injector of a gas chromatography apparatus,

(vi) desorbing the volatile organic compounds from the sorbent and conveying the desorbed organic volatile compounds through the needle to an injector of a gas chromatography apparatus by flowing the inert gas supplied by the insert gas source via the valve and second end of the trap through the at least one sorbent while the needle is inserted in the injector of the gas chromatography apparatus,

(vii) analyzing the volatile organic compounds in the gas chromatography apparatus, and

(viii) cleaning the trap and needle by flushing by supplying the inert gas from the inert gas source to the second end of the trap via the valve.

5. The method of claim 4 , wherein the temperature of the trap in steps (i) to (iii) is lower than the temperature of the trap in steps (vi) and (viii).

6. The method of claim 4 , wherein:

the sampling means further includes a body defining said at least one flow channel,

in step (ii), the at least one flow channel is connected to the vacuum source via the valve, and

in the steps (iv), (vi) and (viii), the at least one flow channel is connected to the inert gas source via the valve.

7. The method of claim 4 , wherein the inert gas is nitrogen.

8. The method of claim 4 , wherein the sampling means further comprises a heating means for heating the trap or a cooling means for cooling the trap.

9. The method of claim 4 , wherein the temperature of the solid or liquid sample is in the range of 0 to 100° C. during step (ii).

10. The method of claim 4 , wherein the pressure in the headspace in step (ii) is below 100 mbar.

11. The method of claim 4 , wherein the temperature of the injector in steps (v) and (vi) is in a range of −10 to 20° C.

12. The method of claim 4 , wherein the at least one sorbent in the trap is a combination of at least two sorbents present in the trap in mixed or layered form.

13. The method of claim 4 , wherein the temperature in the trap in step (iv) is between 150 to 450° C.

14. The method of claim 4 , wherein the flow of the inert gas in step (iv) is 100 to 250 mL min−1.

15. The method of claim 4 , wherein the trap is at a temperature in the range from 10° C. to 40° C. during step (ii).

16. The method of claim 15 , wherein:

the pressure in the headspace in step (ii) is below 100 mbar,

the temperature in the trap in step (iv) is between 150 to 450° C., and

the flow of the inert gas in step (iv) is 100 to 250 mL/min.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 1, 2021
From: FUCHSMANN, PASCAL; WAHL, FABIAN; BISCHOFF, PATRICK; TENA STERN, MIREILLE
To: SCHWEIZERISCHE EIDGENOSSENSCHAFT HANDELND DURCH AGROSCOPE
Reel/Frame 057666/0324 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 1, 2021
From: SCHWEIZERISCHE EIDGENOSSENSCHAFT HANDELND DURCH AGROSCOPE
To: CTC ANALYTICS AG
Reel/Frame 057666/0403 →
Continuity (1)
Related Publication 20220018740A1 · Jan 20, 2022
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