Method and system for analyzing a gaseous fluid comprising at least one rare gas by means of a getterizing substrate

Patent metadata

Field	Value
Publication number	US-9851335-B2
Application number	US-201414220644-A
Country	US
Kind code	B2
Filing date	Mar 20, 2014
Priority date	Mar 25, 2013
Publication date	Dec 26, 2017
Grant date	Dec 26, 2017

Abstract

The invention relates to a method and a system for analyzing rare gases present in a gaseous fluid ( 1 ). According to the invention, initially, the rare gases are extracted from the gaseous fluid by trapping by means of a getterizing substrate ( 5 ), then superconcentration of the rare gases is produced before injection ( 8 ) into the measuring instruments ( 9 ). By virtue of the invention, it is possible to increase the partial pressure of the rare gases in the gases to be analyzed before their injection into the analysis instruments.

First claim

The invention claimed is:

1. Method for analyzing a gaseous fluid comprising at least one rare gas, characterized in that the following steps are carried out:
a) the vacuum is created in an accumulation chamber comprising a getterizing substrate, said getterizing substrate being suitable for trapping the components of said gaseous fluid except for said rare gas;
b) the flow rate of said fluid entering into said accumulation chamber is controlled by means of a flow rate restrictor;
c) said rare gas is extracted and accumulated from said gaseous fluid and separated from other components of said gaseous fluid by the passage of said gaseous fluid into said getterizing substrate of said accumulation chamber;
d) said extracted rare gas, separated from the other components of the gaseous fluid, is compressed such that the pressure and the volume of said compressed rare gas are adapted to the pressure and the volume of said analysis; and
e) said compressed rare gas, separated from the other components of the gaseous fluid, is analyzed.

2. Method according to claim 1 , in which said rare gas is analyzed by gaseous phase chromatography coupled with mass spectrometry.

3. Method according to claim 1 , in which said getterizing substrate is a metal alloy in foam, powder, deposition, rod or ribbon form.

4. Method according to claim 3 , in which said getterizing substrate is a foam or powder of titanium, zirconium, aluminum or an alloy of one of these metals.

5. Method according to claim 1 , in which said getterizing substrate is heated for the step of extraction of said rare gas.

6. Method according to claim 1 , in which, prior to said step of extraction of said rare gas, the vacuum is produced in a chamber incorporating said getterizing substrate.

7. Method according to claim 1 , in which the flow rate of the passage of said gaseous fluid in said getterizing substrate is controlled.

8. System for analyzing at least one gaseous fluid comprising at least one rare gas, characterized in that it comprises:
a flow rate restrictor for controlling the flow rate of said gaseous fluid,
means for extracting and accumulating said rare gas comprising an accumulation chamber incorporating a getterizing substrate, said getterizing substrate being suitable for trapping all the components of said gaseous fluid apart from said rare gas,
vacuum-generating means for said accumulation chamber,
means for compressing said extracted rare gas, separated from the other components of the gaseous fluid, the compression means being suitable for compressing and injecting said rare gas, separated from the other components of the gaseous fluid, for said analysis, and
means for analyzing said compressed rare gas, separated from the other components of the gaseous fluid.

9. System according to claim 8 , in which said gaseous fluid is a sample of gas taken from a geological reservoir.

10. System according to claim 8 , in which said means for analyzing said rare gas comprise a chromatograph coupled with a mass spectrometer.

11. System according to claim 8 , in which said getterizing substrate is a metal alloy in foam, powder, deposition, rod or ribbon form.

12. System according to claim 11 , in which said getterizing substrate is a foam or a powder of titanium, zirconium, aluminum or an alloy of one of these metals.

13. System according to claim 8 , in which said analysis system also comprises means for heating said chamber incorporating said getterizing substrate.

14. System according to claim 8 , in which said analysis system also comprises vacuum-generating means for said chamber suitable for creating a vacuum in said chamber incorporating said getterizing substrate, said vacuum-generating means comprising at least one pump.

15. System according to claim 14 , in which said vacuum-generating means also comprise a second getterizing substrate suitable for trapping the reactive gaseous molecules present in said chamber in a powerful vacuum.

16. System according to claim 8 , in which said means for compressing said rare gas comprise a superconcentration syringe pump comprising a piston whose displacement can be controlled to adapt the volume and the pressure of said rare gas for said analysis.

17. System according to claim 8 , in which said analysis system comprises a transfer syringe pump suitable for picking up said gaseous fluid and for transferring it to said means for extracting said rare gas, said transfer syringe pump comprising a piston whose displacement can be controlled to adapt the injection flow rate of said fluid in said means for extracting said rare gas.

18. System according to claim 8 , in which said analysis system comprises a flow rate restrictor upstream of the means for extracting said rare gas.

19. A method for analysis of a gaseous fluid comprising at least one rare gas, the at least one rare gas being a sample of gas taken from a geological reservoir, comprising:
a) creating a vacuum in an accumulation chamber comprising a getterizing substrate, the getterizing substrate being configured to trapping components of the gaseous fluid except for rare gas;
b) controlling a flow rate of the gaseous fluid comprising the at least one rare gas entering into the accumulation chamber by a flow rate restrictor;
c) extracting and accumulating the at least one rare gas from the gaseous fluid comprising the at least one rare gas by the passage of the gaseous fluid comprising the at least one rare gas into the getterizing substrate of the accumulation chamber;
d) compressing the at least one rare gas that has been extracted and accumulated in the accumulation chamber from the gaseous fluid and that has been separated from the other components of the gaseous fluid such that a pressure and volume of the at least one rare gas are adapted to a pressure and volume of the analysis; and
e) analyzing the at least one rare gas, separated from the other components of the gaseous fluid, at the pressure and volume to which the at least one rare gas has been compressed.

20. The method according to claim 19 , wherein analyzing the at least one rare gas is conducted by gaseous phase chromatography coupled with mass spectrometry.

21. A system for analysis of at least one gaseous fluid comprising at least one rare gas, comprising:
an accumulation chamber incorporating a getterizing substrate, the getterizing substrate being configured to trap all components of the at least one gaseous fluid comprising the at least one rare gas apart from rare gas to separate the at least one rare gas from other components of the at least one gaseous fluid,
a flow rate restrictor for controlling a flow rate of the at least one gaseous fluid comprising the at least one rare gas into the accumulation chamber,
a first pump for creating a vacuum in the accumulation chamber,
a second pump for compressing the at least one rare gas that has been extracted and accumulated in the accumulation chamber from the gaseous fluid and that has been separated from the other components of the at least one gaseous fluid such that a pressure and volume of the at least one rare gas are adapted to a pressure and volume of the analysis, and
at least one analyzer for analyzing the at least one rare gas that has been separated from the other components of the at least one gaseous fluid at the pressure and volume to which the at least one rare gas has been compressed by the pump for compressing the at least one rare.

22. The system according to claim 21 , wherein

Assignees

• Ifp Energies Now

Inventors

• Rouchon Virgile

Classifications

• G01N33/0036

  specially adapted to detect a particular component (physical analysis of gaseous biological material G01N33/497) · CPC title

• C01B2210/004

  Separation of a mixture of noble gases · CPC title

• G01N1/2202

  involving separation of sample components during sampling · CPC title

• G01N33/0014

  by eliminating a gas (by a chemical reaction G01N33/0013; a chemical reaction taking place or a gas being eliminated in one or more analysing channels G01N33/0024) · CPC title

• G01N33/0016 Primary

  by regulating a physical variable, e.g. pressure or temperature · CPC title