# US 5,705,816 A · Process and device for analyzing traces of impurities in a gas sample by means of a diode laser

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- Number: US 5,705,816 A
- Document ID: US5705816A
- Status: Granted
- Kind: A
- Application number: 08/634,725
- Filed: 1996-04-19
- Granted: 1998-01-06
- Earliest claimed: 1995-04-21
- Assignees: L'Air Liquide, Societe Anonyme pour l'Etude et l'Exploitation des Procedes Georges Claude
- Inventors: Catherine Ronge; Fabrice Bounaix; Patrick Mauvais; Frederic Stoeckel
- Web page: https://patentgrep.com/patent/US5705816A

## CPC

- G01N 21/39: using tunable lasers
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

The invention relates to a process for analyzing traces of at least one impurity in a gas sample, by absorption by the impurity to be detected of a light beam emitted by a semiconductor diode laser, the beam emitted by the diode being split into at least two branched beams, one called the measurement beam which passes through the gas sample to be analyzed in a multipassage cell before being focused onto a measurement photodetector, another branched beam, called the reference beam, being along a reference path and directly focused onto a reference photodetector without encountering the gas sample, in which process the gas sample is at a pressure at least equal to atmospheric pressure, and a modulation of the supply current of the diode has been introduced, which comprises at least one function of the exponential type.

## Claims

### Claim 1

A process for analyzing traces of at least one impurity in a gas sample by means of a tunable diode laser comprising the steps of:
measuring absorption, by the impurity to be detected, of a light beam emitted by a diode laser, wherein said diode laser is supplied with a supply current comprising a continuous component and a variable component effective to introduce a modulation of the emitted wavelength in order to describe all or part of a profile of at least one absorption line of said impurity,
splitting the beam emitted by the diode laser into at least two branched beams comprising (i) a measurement beam along a measurement path directed toward the gas sample to be analyzed, which passes through said gas sample in a multipassage cell before being focused onto a measurement photodetector and (ii) a reference beam along a reference path and directly focused onto a reference photodetector without encountering the gas sample,
wherein (a) the measurement and reference paths, respectively have optical path lengths between the diode laser and the measurement photodetector and between the diode laser and the reference photodetector, which have been equalized in air, (b) said gas sample is at a pressure at least equal to atmospheric pressure, and (c) said introduced modulation comprises at least one function of the exponential type.

### Claim 2 (depends on 1)

The process as claimed in claim 1, wherein said gas sample has a pressure which does not exceed 3.times.10.sup.5 Pa absolute.

### Claim 3 (depends on 2)

The process as claimed in claim 2, wherein said pressure of said gas sample ranges between 10.sup.5 Pa and 3.times.10.sup.5 Pa absolute.

### Claim 4 (depends on 1)

The process as claimed in claim 1, further comprising the step of flushing a space contained between the diode laser and each photodetector with a protective gas.

### Claim 5 (depends on 4)

The process as claimed in claim 4, wherein said flushing is carried out in laminar flow.

### Claim 6 (depends on 1)

The process as claimed in claim 1, wherein said impurity analyzed is water.

### Claim 7 (depends on 6)

The process as claimed in claim 6, wherein the modulation introduced in the emitted wavelength extends around one of the following two wavelengths: 1.37 .mu.m or 1.9 .mu.m.

### Claim 8

Device for analyzing traces of at least one impurity in a gas sample comprising,
a semiconductor diode laser which emits a beam;
at least one splitter system effective to split the beam emitted by the diode laser into at least two branched beams comprising, a measurement beam and a reference beam;
a multipassage cell containing the gas sample to be analyzed;
an optical device effective to send the branched measurement beam output by the splitter system along a measurement optical path onto the multipassage cell;
a measurement photodetector which generates a signal;
an optical device effective to direct the measurement beam output by the multipassage cell onto the measurement photodetector;
a reference photodetector which generates a signal;
a device effective to direct the reference branched beam output by the splitter system along a reference optical path onto the reference photodetector;
element for acquisition and processing of the signals generated by the measurement and reference photodetectors;
means for equalizing optical path lengths of the measurement and reference paths, respectively between the diode laser and the measurement photodetector, and between the diode laser and the reference photodetector, and
supply current of the diode laser and means for modulating the supply current of the diode laser, effective to introduce a modulation comprising at least one function of the exponential type.

### Claim 9 (depends on 8)

The device as claimed in claim 8, wherein said means for equalizing the optical path lengths comprises systems of mirrors present on the reference path between the splitter system and the reference photodetector.

### Claim 10 (depends on 8)

The device as claimed in claim 8, further comprising means for stabilizing the temperature of the diode laser.

### Claim 11 (depends on 8)

The device as claimed in claim 8, wherein at least one of the diode laser and the measurement and reference photodetectors is without a window.

### Claim 12 (depends on 8)

The device as claimed in claim 8, wherein an assembly comprising the diode laser, the measurement and reference photodetectors and the multipassage cell comprising the gas to be analyzed is isolated from a surrounding atmosphere by being located in an inert gas flow.

### Claim 13 (depends on 12)

The device as claimed in claim 12, wherein the means for injecting a gas flow is dimensioned in such a way that said gas flow is substantially laminar.

### Claim 14 (depends on 8)

The device as claimed in claim 8, wherein the cell is made from a single-piece metal block.

### Claim 15 (depends on 8)

The device as claimed in claim 8, wherein the cell further comprises a means for inlet of the gas to be analyzed into the cell, and for outlet of the gas to be analyzed from the cell, effective to establish a substantially laminar flow regime of the gas inside the cell.
