Device for producing gaseous CO2 from carbonates for isotopic analysis (δ13C and δ18O) in situ, and associated method

Patent metadata

Field	Value
Publication number	US-12152971-B2
Application number	US-202017597175-A
Country	US
Kind code	B2
Filing date	Jun 30, 2020
Priority date	Jul 1, 2019
Publication date	Nov 26, 2024
Grant date	Nov 26, 2024

Abstract

A device for preparing a gaseous sample obtained from a solid sample. The device includes a laser source arranged to emit a laser beam which is capable of generating calcination and/or combustion of a portion of the solid sample, a collector arranged to collect a gaseous sample of a gas emitted during the calcination and/or combustion of the portion of the solid sample; the laser beam has an irradiance less than 5 MW/cm 2 in a given impact zone on a surface of the sample, and including an optical fibre for propagating the laser beam between the laser source and the given impact zone on the surface of the sample.

First claim

The invention claimed is:

1. A device for preparing a gaseous sample obtained from a solid sample, said device comprising:
a laser source arranged to emit a laser beam generating calcination and/or combustion of a portion of the solid sample and said laser beam not causing a laser ablation;
a means arranged to collect a gaseous sample of a gas emitted during the calcination and/or combustion of the portion of the solid sample;
the laser beam has an irradiance less than 5 MW/cm2 in a given impact zone on a surface of the sample; and
an optical fibre for propagating the laser beam between the laser source and the given impact zone on the surface of the sample.

2. The device according to claim 1 , wherein an optical/electrical efficiency of the laser source is greater than 30%.

3. The device according to claim 1 , wherein the laser source comprises a laser diode.

4. The device according claim 3 , wherein:
the laser source is a laser diode, or
the laser source is an optically pumped doped fibre.

5. The device according to claim 1 , wherein the laser source is arranged to emit a laser beam with a wavelength greater than 0.3 μm and/or less than 5 μm.

6. The device according to claim 1 , wherein a diameter of a core of the optical fibre has a value greater than 2 μm and/or less than 800 μm.

7. The device according to claim 1 , wherein a numerical aperture of the optical fibre is greater than 0.1 and/or less than 0.5.

8. The device according claim 1 , comprising means for shaping and focusing the laser beam being arranged such that the device has a focal distance greater than 5 mm.

9. The device according to claim 8 , wherein the laser source, the optical fibre and the shaping and focusing means are arranged such that the laser beam has a Rayleigh length greater than 0.5 mm and/or less than 10 mm.

10. The device according to claim 1 , comprising a movement means arranged to move the laser beam and/or the impact zone relative to one another.

11. The device according to claim 1 , wherein the optical beam has an M2 factor greater than 2 and/or less than 200.

12. The device according claim 1 , comprising:
a light source arranged to illuminate at least the impact zone; and
an optical sensor arranged to image the illuminated impact zone and/or to measure one or more optical parameters of light reflected by the illuminated impact zone of the solid sample.

13. The device according to claim 12 , comprising a processing unit arranged and/or configured and/or programmed to determine, from the optical parameter(s) measured by the optical sensor, a luminous flux to be applied to the impact zone.

14. The device according to claim 1 , comprising a means arranged to deposit material on the impact zone of the solid sample, said material being arranged to initiate the calcination and/or combustion of the portion of the solid sample adjacent to the deposited material.

15. The device according to claim 1 , comprising an enclosure arranged:
to cooperate with the means arranged to collect the gaseous sample,
such that the solid sample is arranged inside it, or
to be brought into direct contact with the surface of the solid sample.

16. The device according to claim 1 , comprising an optical element situated on a path of the laser beam at the output of the means for shaping and focusing the laser beam, said optical element being arranged to protect said means for shaping and focusing the laser beam.

17. A portable device for the analysis of carbon and/or oxygen isotopic compositions contained in carbonate rocks, said device for the analysis of isotopic compositions comprising:
the device for preparing a gaseous sample according to claim 1 ; and
an optical spectrometer or a mass spectrometer arranged to carry out isotopic analyses of elements contained in gaseous samples prepared by said device for preparing a gaseous sample.

18. A use of the device for preparing a gaseous sample according to claim 1 , for the analysis of carbon and/or oxygen isotopic compositions contained in carbonate rocks.

19. A method for preparing a gaseous sample obtained from a solid sample, said method comprising:
emission, by a laser source, of a laser beam generating calcination and/or combustion of a portion of the solid sample and said laser beam not causing a laser ablation;
collection, by a collection means, of a gaseous sample of a gas emitted during the calcination and/or combustion of the portion of the solid sample;
an irradiance of the laser beam emitted is less than 5 MW/cm2 in a given impact zone on a surface of the sample; and
propagation, by an optical fibre, of the laser beam between the laser source and the given impact zone on the surface of the sample.

Assignees

• Univ Bourgogne
• Centre Nat Rech Scient
• Univ Bretagne Occidentale

Inventors

• Musset Olivier
• Thomazo Christophe
• Sans Jofre Pierre
• Cocquerez Théophile
• Lalonde Stefan

Classifications

• G01N2001/045

  Laser ablation; Microwave vaporisation · CPC title

• G01N2001/028

  Sampling from a surface, swabbing, vaporising · CPC title

• G01N33/24 Primary

  Earth materials (G01N33/42 takes precedence) · CPC title

• G01N1/02

  Devices for withdrawing samples {(sampling of foundation soil E02D1/04; collecting or conveying radioactive samples G01T7/00, e.g. G01T7/02, G01T7/08)} · CPC title

• G01N1/44 Primary

  Sample treatment involving radiation, e.g. heat · CPC title