Gas analysis system comprising a gas spectrometer equipped with a micro-reflectron

Patent metadata

Field	Value
Publication number	US-9696285-B2
Application number	US-201314419108-A
Country	US
Kind code	B2
Filing date	Aug 5, 2013
Priority date	Aug 3, 2012
Publication date	Jul 4, 2017
Grant date	Jul 4, 2017

Abstract

The invention relates to a gas analysis system comprising, from upstream to downstream:
a module (SEP) for separating at least a portion of the species contained in the gas to be analysed, comprising at least one microcapillary column (GC) for gas phase chromatography, and a time-of-flight mass spectrometer (TOFMS) coupled to said separation module, said spectrometer comprising a ion source (MS 1 , MS 2 ) adapted to ionise at least a portion of said species and to emit a ion beam, and a free-flight zone (MS 4 ) for said ions,

said mass spectrometer (TOFMS) being arranged in the volume of at least one substrate and comprising a micro-reflectron (R) arranged between the source (MS 1 , MS 2 ) and the free-flight zone (MS 4 ), a wall (R 1 ) of said micro-reflectron comprising a layer made from a resistive material designed to be polarised between at least two regions so as to create a continuous electrostatic field gradient in said reflectron.

First claim

The invention claimed is:

1. A gas analysis system comprising, from upstream to downstream:
a module for separating at least a portion of the species contained in the gas to be analysed, comprising at least one microcapillary gas phase chromatography column, and
a time-of-flight mass spectrometer coupled to said separation module, said spectrometer comprising a source of ions adapted to ionise at least a portion of said species and to emit a beam of ions, and a free-flight zone for said ions,
said mass spectrometer being arranged in the volume of at least one substrate and comprising a micro-reflectron arranged between the source of ions and the free-flight zone, a wall of said micro-reflectron comprising a layer made from a resistive material designed to be polarised between at least two regions of said layer in such a way as to create a continuous electrostatic field gradient in order to deviate the trajectory of the ions in said micro-reflectron.

2. The system of claim 1 , wherein the micro-reflectron is arranged in such a way as to be passed through by the ions in a longitudinal direction parallel to the direction of the beam of ions at the outlet of the source and the resistive layer is designed to be polarised in such a way that the continuous electrostatic field gradient is oriented transversally to the trajectory of the ions in the micro-reflectron.

3. The system of claim 2 , wherein the micro-reflectron comprises at least two polarising electrodes of the resistive layer in contact with said regions of the resistive layer, said electrodes extending in the longitudinal direction of the micro-reflectron, in such a way as to generate in said resistive layer a potential gradient in the transverse direction of the micro-reflectron.

4. The system of claim 1 , wherein the mass spectrometer is arranged in such a way that the trajectory of the ions in the mass spectrometer is included in a channel extending between two planes parallel to a main face of said at least one substrate, with the height of said channel being less than 1 mm and with the length of said channel being at least ten times greater than said height.

5. The system of claim 1 , wherein said resistive layer of the micro-reflectron extends in a plane parallel to a main face of said at least one substrate.

6. The system of claim 1 , wherein the beam of ions is emitted by the ion source in a direction orthogonal to the direction of introduction, in the spectrometer, of the gas coming from the separation module.

7. The system of claim 1 , wherein the spectrometer comprises, between the source of ions and the micro-reflectron, a zone for accelerating the ions.

8. The system of claim 7 , wherein the zone for accelerating the ions and the free-flight zone are arranged along a longitudinal wall of the micro-reflectron in such a way as to be adjacent.

9. The system of claim 8 , wherein the micro-reflectron comprises a first opening that communicates with the acceleration zone for the inlet of the ions into the reflectron and a second opening that communicates with the free-flight zone for the outlet of the ions, said first and second openings being adjacent in the same wall of the micro-reflectron.

10. The system of claim 7 , wherein the acceleration zone comprises two electrodes extending parallel to the direction of the beam of ions emitted by the ion source, said electrodes being able to be polarised in such a way as to generate an electrostatic field able to deviate the ions in a direction orthogonal to that of the ion beam at the outlet of the ion source in order to have said ions penetrate into the micro-reflectron.

11. The system of claim 10 , wherein said electrodes of the acceleration zone are polarised by a pulse device, in such a way as to have the accelerated ions sequentially enter the micro-reflectron.

12. The system of claim 1 , wherein the free-flight zone of the spectrometer is a zone that is separate from the micro-reflectron and that is devoid of any electrostatic field.

13. The system of claim 1 , wherein the substrate in the volume of which said spectrometer is arranged is housed in a sealed case coupled to a vacuum pump in such a way as to apply a vacuum in said case.

14. The system of claim 1 , wherein said at least one microcapillary chromatography column is arranged in the volume of at least one substrate.

15. The system of claim 14 , wherein the separation module comprises at least one non-destructive micro or nano-detector in said at least one microcapillary chromatography column.

16. The system of claim 1 , wherein the separation module comprises at least two microcapillary gas phase chromatography columns coupled in series and each one comprising a different stationary phase, and a flow modulator in order to regulate the flow of gas successively through each one of said columns.

17. The system of claim 14 , wherein the separation module comprises at least two microcapillary gas phase chromatography columns coupled in series and each one comprising a different stationary phase, each one of said microcapillary columns comprising at least two non-destructive micro or nano-detectors arranged in said columns.

18. The system of claim 1 , further comprising, upstream of the mass spectrometer, at least one non-destructive micro or nano-detector, said detector being arranged in a duct with a cross section equal to that of a microcapillary chromatography column to which it is connected in such a way as to not modify the cross section of passage of the gas.

19. The system of claim 18 , wherein said spectrometer is arranged in the volume of a substrate, said substrate being housed in a sealed case coupled to a vacuum pump in such a way as to apply a vacuum in said case, wherein said non-destructive detector is an electromechanical nano-system comprising a resonator and wherein said detector is arranged in the vacuum pressurising case of the mass spectrometer.

20. The system of claim 1 , further comprising, upstream of the separation module, a circuit for preconcentrating the gas to be analysed comprising a preconcentrator.

Assignees

• Commissariat Energie Atomique
• Analytical Pixels Tech-Apix Tech

Inventors

• Duraffourg Laurent
• Andreucci Philippe
• Tassetti Charles-Marie
• Colinet Eric
• Puget Pierre
• Whiting Joshua
• Stevens Peter Thomas
• Petitjean Mélanie

Classifications

• H01J49/405

  characterised by the reflectron, e.g. curved field, electrode shapes · CPC title

• G01N30/7206 Primary

  interfaced to gas chromatograph (interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04) · CPC title

• H01J49/0018

  Microminiaturised spectrometers, e.g. chip-integrated devices, Micro-Electro-Mechanical Systems [MEMS] · CPC title

• G01N2030/025

  Gas chromatography · CPC title