WO1995017656A1 - Method for determining the surface contamination of a solid, and device therefor - Google Patents

Method for determining the surface contamination of a solid, and device therefor Download PDF

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Publication number
WO1995017656A1
WO1995017656A1 PCT/FR1994/001519 FR9401519W WO9517656A1 WO 1995017656 A1 WO1995017656 A1 WO 1995017656A1 FR 9401519 W FR9401519 W FR 9401519W WO 9517656 A1 WO9517656 A1 WO 9517656A1
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WIPO (PCT)
Prior art keywords
particles
contamination
laser beam
pollutant
solid
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Application number
PCT/FR1994/001519
Other languages
French (fr)
Inventor
Pierre Laffont
Jean-Claude Dumont
Original Assignee
Compagnie Generale Des Matieres Nucleaires
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Publication date
Application filed by Compagnie Generale Des Matieres Nucleaires filed Critical Compagnie Generale Des Matieres Nucleaires
Publication of WO1995017656A1 publication Critical patent/WO1995017656A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
    • G01N2001/045—Laser ablation; Microwave vaporisation

Definitions

  • the present invention relates to a method for controlling the surface contamination of a solid and a device for its implementation.
  • the surfaces of solids are constantly subjected to the effects of pollution which can be of varied nature. It can be dust, fatty substances which cover objects with dirt. They can be microorganisms which develop superficially. Chemical pollution and oxidation can also cause the appearance of a surface layer covering objects. In environments subject to nuclear contamination, the machinery parts and the walls of the installations are covered with a film of metallic oxides or radioactive salts (nitrates, for example).
  • a visual method may consist of examining the color and appearance (matt or shiny) of an object and assessing their degree of alteration.
  • the visual methods are random and do not allow the rate of surface contamination to be quantified. They also require the approach of the solid to be examined.
  • Sampling methods may require sampling by solid vector (by smear), liquid (by washing) or gas (by reaction with a gas). These methods cause the dispersion of the contamination both on the surface of the solid studied and in the surrounding space or the installations and generate secondary waste which can be random (in the case of solids) or which dilute the pollutant making its quantification very difficult if not impossible.
  • patent FR-A-2 641 718 discloses the use of a pulsed laser beam in particular for restoring works of art, dirt being then volatilized.
  • Document EP-A-91 646 discloses the use of the same effect for decontaminating surfaces of nuclear organs. The waste obtained is then sucked up for disposal.
  • document FR-A-2 678 418 a contaminated area is cleaned thanks to the effect generated by a laser beam conveyed by an optical fiber, the waste obtained being aspirated.
  • Other documents disclose the use of this effect for cleaning operations.
  • US-A-4,756,765 a high power laser beam allows the removal of pollutants of low thermal conduction (paints, greases).
  • Document FR-A-2 467 656 proposes to remove rust from metal surfaces by transformation, by means of a laser beam, of rust into magnetite which is then removed mechanically or chemically.
  • document FR-A-2 300 632 an abrupt and intense heating of a surface is caused by means of a laser beam to detach a surface film of oxides therefrom by mechanical, chemical or electrochemical means.
  • the method using the shock effect was the subject of patent application EP-A-380 387 which describes a method of cleaning the surface of materials in which a shock wave generated by a laser beam allows the detachment of the polluting surface layers which are then blown away by a jet of fluid.
  • the present invention has been designed to allow a control of the surface contamination rate of a solid, not having the drawbacks of the visual method or of the sampling method as described above.
  • a laser beam will be used for this purpose to detach a few particles from the contaminated surface which will be transferred for analysis.
  • the laser beam used has characteristics such that, when it is directed at the very surface of the solid, it induces an overpressure between the surface of the solid and the contaminating layer which causes an expulsion of this layer in the form of particles while leaving it intact. the material constituting the solid.
  • the subject of the invention is therefore a method of controlling the state of contamination by a pollutant from the surface of a solid, comprising the removal of particles of this pollutant from an area of the surface to be checked in order to quantify the rate of contamination. of this surface, characterized in that: - there is a sampling device on the surface to be checked and allowing access to said area, this device making it possible to collect said particles,
  • said zone is subjected to the impact of a laser beam of characteristics such that it causes the extraction of said particles
  • a known fraction of the particles extracted is collected using the sampling device, - Estimating the contamination rate of said surface by quantifying the particles collected and taking into account the characteristics of the laser beam and the sampling device.
  • the sampling device may comprise a blade transparent to said beam, arranged on its path and placed so as to receive the extracted particles which are sucked along the laser beam by the plasma effect generated by this beam.
  • the contamination rate can then be estimated by measuring the attenuation of the optical transmission of the slide, by examining it under a microscope or by dissolving the particles collected and physico-chemical analysis of these particles.
  • the sampling device can comprise the passage of a gas flow conveying all or part of the particles extracted, by dissolving the particles conveyed in the gas flow and physico-chemical analysis of these particles, or by a granulometer placed in line with the gas flow. .
  • the contamination rate can also be estimated by stopping the particles on an absolute filter and detecting them, either by microscopic examination of the deposit collected on the filter, or by nuclear measurements if the particles contain radioelements.
  • the invention also relates to a device for sampling particles of a pollutant covering the surface of a solid, comprising an enclosure having an opening intended to cover an area of said surface, the enclosure being provided with a transparent blade to a laser beam intended to extract, by its impact on said zone, said particles, the enclosure also being provided with an inlet orifice and with an outlet orifice allowing the circulation of a gas for the transfer of the particles , characterized in that the gas inlet is located as close as possible to the surface of the solid. This ensures better capture of the particles.
  • Such a device also has the advantage of avoiding the dispersion in the atmosphere or the surrounding environment of pollutant particles.
  • Another gas inlet may be located as close as possible to the blade. This avoids the opacification of the blade if necessary.
  • the device can nevertheless be used regardless of the surface state of the solid.
  • the enclosure has a small diameter, compatible with the diameter of the laser beam ( ⁇ 10 mm) and the surface-inlet opening latitude is large (several cm) since it suffices to adapt the gas flow.
  • the subject of the invention is also an installation for controlling the rate of contamination by a pollutant on the surface of a solid, characterized in that it comprises: a sampling device as defined above,
  • FIG. 1 shows a first variant of a device for sampling particles from a pollutant covering the surface of a solid, according to the invention
  • FIG. 2 shows a second variant of a device for sampling particles of a pollutant covering the surface of a solid, according to the invention
  • FIG. 3 schematically shows an installation for controlling the state of contamination by a pollutant from the surface of a solid, according to the invention.
  • the invention makes it possible to detect, characterize if necessary and quantify, if necessary, polluting materials such as radioelements, fatty substances, salts, bacteria, viruses, etc. on the surface of solid bodies.
  • a zone 3 of this surface is covered by a cylindrical enclosure 4.
  • One of the ends of the cylindrical enclosure is placed opposite zone 3 The other end is closed by a blade 5.
  • the extraction of pollutant particles is carried out by the impact of a laser beam 6 passing through the transparent blade 5 for the wavelength of the laser beam.
  • the extraction of particles can be done, as is well known, by thermal effect or by shock effect.
  • the laser is preferably of the YAG type and operating in pulsed regime.
  • the speed of the gas flow must be adjusted according to the nature of the pollutant to allow the best possible evacuation of the extracted particles. This makes it possible to cancel the fallout of the pollutant extracted.
  • the enclosure 4 can be metallic or plastic. It can be placed a few millimeters from the surface of the substrate to make an inlet port for the particle transport gas.
  • the deposit made on the slide can be examined and characterized under a microscope. This deposit can be dissolved in a suitable solvent for physicochemical analysis of the particles.
  • FIG. 2 shows such an alternative embodiment.
  • the holes 17 provided in the cylinder 4 just under the blade 5 ensure this circulation.
  • FIG. 3 represents a typical installation for the treatment of particles entrained by a gas flow.
  • the laser 11 emits a light beam which is transported to the sampling device for example by a fiber optic system 12, in direct fire or by a set of mirrors.
  • the laser beam 6 can be moved relatively with respect to the surface to be tested to ensure scanning of this surface. This movement can be ensured by a table with crossed movements, in particular for examining flat surfaces, or by a turntable, in particular for surfaces of revolution.
  • a programmed robot can move the optical fiber.
  • the suction duct 8 is connected to an apparatus 13.
  • This apparatus 13 can be a sampling apparatus comprising an absolute filter, a bubbler, etc., according to the known art. It can be an in-line detection device with or without a downstream filter or an in-line measuring device with or without a downstream filter.
  • a flow meter 14 connected to the device 13 allows the speed of the transport gas to be controlled at the inlet and in the sampling device.
  • the flow meter 14 is connected to a fan 15 ensuring the gas flow and rejecting the gas to a ventilation duct, a chimney or, where appropriate, a recycling circuit with possibly a filtration device.
  • an auxiliary gas inlet valve 16 (for example air) makes it possible to adjust the gas flows required.
  • the pollutant entrained by the gas flow can be detected by an online particle detector. It can be detected by stopping particles on an absolute filter followed either by microscopic examination of the deposit on it, or by one or more nuclear measurements in the case where the pollutant contains radioelements. Characterization and quantification of the pollutant can be carried out by dissolving the pollutant deposited and analyzed by conventional physicochemical processes. One can also use an on-line device, for example a granulometer.
  • the sampling circuit is compact and the polluted volume is therefore lower and limited to the sampling device and any filters;
  • the sensitivity is very good, the laser making it possible to remove layers of pollutant of a few ⁇ m and the device used ensuring concentration;
  • the sensitivity is therefore given by the surface explored and the sensitivity of the detection device placed in the circuit;
  • the exploration speed of a contaminated surface is high and can reach several m 2 / h;
  • the invention allows remote sampling which is advantageous when the pollutant or the solid to be tested is dangerous for a worker;
  • the invention allows the exploration of almost closed bodies such as hollow bodies, grooves, cracks, and which may have poor surface conditions;

Abstract

A method for determining the contamination by a pollutant of the surface of a solid (1), wherein a particle sampling device is positioned on the surface portion of interest in order to collect particles, said portion is exposed to an incident laser beam (6) having properties which cause extraction of the particles (7), a known fraction of the extracted particles is collected using the collecting assembly, and the degree of contamination of said surface is estimated by analysing the collected particles with reference to the properties of the laser beam and the sampling device. The sampling device used in said method, and an apparatus for determining the contamination by a pollutant of the surface of a solid, are also disclosed.

Description

PROCEDE DE CONTROLE DE LA CONTAMINATION CONTAMINATION CONTROL PROCESS
SURFACIQUE D'UN SOLIDE ETSURFACIC OF A SOLID AND
DISPOSITIF DE MISE EN OEUVREIMPLEMENTATION DEVICE
La présente invention concerne un procédé de contrôle de la contamination surfacique d'un solide et un dispositif pour sa mise en oeuvre.The present invention relates to a method for controlling the surface contamination of a solid and a device for its implementation.
Les surfaces de solides sont constamment soumises aux effets de la pollution qui peut être de nature variée. Il peut s'agir de poussières, de corps gras qui recouvrent les objets de salissures. Il peut s'agir de micro-organismes qui se développent superficiellement. La pollution chimique et l'oxydation peuvent également causer l'apparition d'une couche superficielle recouvrant les objets. Dans les milieux soumis à la contamination nucléaire, les organes des machines et les parois des installations se recouvrent d'un film d'oxydes métalliques ou de sels (nitrates par exemple) radioactifs.The surfaces of solids are constantly subjected to the effects of pollution which can be of varied nature. It can be dust, fatty substances which cover objects with dirt. They can be microorganisms which develop superficially. Chemical pollution and oxidation can also cause the appearance of a surface layer covering objects. In environments subject to nuclear contamination, the machinery parts and the walls of the installations are covered with a film of metallic oxides or radioactive salts (nitrates, for example).
Pour contrôler l'état de contamination surfacique des solides, on utilise classiquement une méthode visuelle ou une méthode de prélèvement.To control the state of surface contamination of solids, a visual method or a sampling method is conventionally used.
Une méthode visuelle peut consister en l'examen de la couleur et de l'aspect (mat ou brillant) d'un objet et en l'évaluation de leur degré d'altération. Les méthodes visuelles sont aléatoires et ne permettent pas de quantifier le taux de contamination des surfaces. Elles nécessitent en outre l'approche du solide à examiner.A visual method may consist of examining the color and appearance (matt or shiny) of an object and assessing their degree of alteration. The visual methods are random and do not allow the rate of surface contamination to be quantified. They also require the approach of the solid to be examined.
Les méthodes de prélèvement peuvent nécessiter le prélèvement d'échantillons par vecteur solide (par frottis), liquide (par lavage) ou gazeux (par réaction avec un gaz) . Ces méthodes provoquent la dispersion de la contamination tant à la surface du solide étudié que dans l'espace environnant ou les installations et génèrent des déchets secondaires qui peuvent être aléatoires (dans le cas des solides) ou qui diluent le polluant rendant sa quantification très difficile voire impossible.Sampling methods may require sampling by solid vector (by smear), liquid (by washing) or gas (by reaction with a gas). These methods cause the dispersion of the contamination both on the surface of the solid studied and in the surrounding space or the installations and generate secondary waste which can be random (in the case of solids) or which dilute the pollutant making its quantification very difficult if not impossible.
On connaît d'autre part différents procédés de nettoyage de surfaces de solides contaminées. Parmi tous ces procédés, un procédé relativement récent utilise l'impact d'un faisceau laser sur une surface contaminée. On peut utiliser dans ce cas l'effet thermique engendré par le faisceau laser sur la surface à nettoyer ou l'effet de choc engendré par ce faisceau au contact de cette surface.On the other hand, various methods of cleaning contaminated solid surfaces are known. Among all these methods, a relatively recent method uses the impact of a laser beam on a contaminated surface. In this case, the thermal effect generated by the laser beam on the surface to be cleaned or the shock effect generated by this beam in contact with this surface can be used.
Pour illustrer la méthode utilisant l'effet engendré par un faisceau laser, on peut citer le brevet FR-A-2 641 718 qui divulgue l'utilisation d'un faisceau laser puisé en particulier pour restaurer des oeuvres d'art, les salissures étant alors volatilisées. Le document EP-A-91 646 divulgue l'utilisation du même effet pour décontaminer des surfaces d'organes nucléaires. Les déchets obtenus sont alors aspirés pour leur mise au rebut. Selon le document FR-A-2 678 418, une zone contaminée est nettoyée grâce à l'effet engendré par un faisceau laser véhiculé par une fibre optique, les déchets obtenus étant aspirés. D'autres documents divulguent l'utilisation de cet effet pour des opérations de nettoyage. Selon le brevet US-A-4 756 765, un faisceau laser de forte puissance permet l'enlèvement de polluants de faible conduction thermique (peintures, graisses). Le document FR-A-2 467 656 propose d'enlever la rouille de surfaces métalliques par transformation, au moyen d'un faisceau laser, de la rouille en magnétite qui est ensuite retirée mécaniquement ou chimiquement. Selon le document FR-A-2 300 632, on provoque un chauffage brusque et intense d'une surface au moyen d'un faisceau laser pour en détacher une pellicule superficielle d'oxydes par des moyens mécaniques, chimiques ou électrochimiques.To illustrate the method using the effect generated by a laser beam, mention may be made of patent FR-A-2 641 718 which discloses the use of a pulsed laser beam in particular for restoring works of art, dirt being then volatilized. Document EP-A-91 646 discloses the use of the same effect for decontaminating surfaces of nuclear organs. The waste obtained is then sucked up for disposal. According to document FR-A-2 678 418, a contaminated area is cleaned thanks to the effect generated by a laser beam conveyed by an optical fiber, the waste obtained being aspirated. Other documents disclose the use of this effect for cleaning operations. According to US-A-4,756,765, a high power laser beam allows the removal of pollutants of low thermal conduction (paints, greases). Document FR-A-2 467 656 proposes to remove rust from metal surfaces by transformation, by means of a laser beam, of rust into magnetite which is then removed mechanically or chemically. According to document FR-A-2 300 632, an abrupt and intense heating of a surface is caused by means of a laser beam to detach a surface film of oxides therefrom by mechanical, chemical or electrochemical means.
La méthode utilisant l'effet de choc a fait l'objet de la demande de brevet EP-A-380 387 qui décrit un procédé de nettoyage de la surface de matériaux dans lequel une onde de choc générée par un faisceau laser permet le décollement des couches superficielles polluantes qui sont ensuite soufflées par un jet de fluide. La présente invention a été conçue pour permettre un contrôle du taux de contamination surfacique d'un solide, ne présentant pas les inconvénients de la méthode visuelle ou de la méthode de prélèvement telles que décrites plus haut. On utilisera à cet effet un faisceau laser pour détacher de la surface contaminée quelques particules qui seront transférées pour être analysées. Le faisceau laser utilisé a des caractéristiques telles que, lorsqu'il est dirigé sur la surface même du solide, il induit une surpression entre la surface du solide et la couche contaminante qui provoque une expulsion de cette couche sous forme de particules tout en laissant intact le matériau constituant le solide.The method using the shock effect was the subject of patent application EP-A-380 387 which describes a method of cleaning the surface of materials in which a shock wave generated by a laser beam allows the detachment of the polluting surface layers which are then blown away by a jet of fluid. The present invention has been designed to allow a control of the surface contamination rate of a solid, not having the drawbacks of the visual method or of the sampling method as described above. A laser beam will be used for this purpose to detach a few particles from the contaminated surface which will be transferred for analysis. The laser beam used has characteristics such that, when it is directed at the very surface of the solid, it induces an overpressure between the surface of the solid and the contaminating layer which causes an expulsion of this layer in the form of particles while leaving it intact. the material constituting the solid.
L'invention a donc pour objet un procédé de contrôle de l'état de contamination par un polluant de la surface d'un solide, comprenant le prélèvement de particules de ce polluant sur une zone de la surface à contrôler pour quantifier le taux de contamination de cette surface, caractérisé en ce que : - on dispose un dispositif de prélèvement sur la surface à contrôler et permettant d'accéder à ladite zone, ce dispositif permettant de collecter lesdites particules,The subject of the invention is therefore a method of controlling the state of contamination by a pollutant from the surface of a solid, comprising the removal of particles of this pollutant from an area of the surface to be checked in order to quantify the rate of contamination. of this surface, characterized in that: - there is a sampling device on the surface to be checked and allowing access to said area, this device making it possible to collect said particles,
- on soumet ladite zone à l'impact d'un faisceau laser de caractéristiques telles qu'il provoque l'extraction desdites particules,- said zone is subjected to the impact of a laser beam of characteristics such that it causes the extraction of said particles,
- on recueille une fraction connue des particules extraites grâce au dispositif de prélèvement, - on estime le taux de contamination de ladite surface par quantification des particules recueillies et en tenant compte des caractéristiques du faisceau laser et du dispositif de prélèvement.a known fraction of the particles extracted is collected using the sampling device, - Estimating the contamination rate of said surface by quantifying the particles collected and taking into account the characteristics of the laser beam and the sampling device.
Le dispositif de prélèvement peut comprendre une lame transparente audit faisceau, disposée sur son trajet et placée de façon à recevoir les particules extraites qui sont aspirées le long du faisceau laser par l'effet plasma généré par ce faisceau.The sampling device may comprise a blade transparent to said beam, arranged on its path and placed so as to receive the extracted particles which are sucked along the laser beam by the plasma effect generated by this beam.
Le taux de contamination peut alors être estimé par mesure de l'atténuation de la transmission optique de la lame, par son examen au microscope ou par dissolution des particules recueillies et analyse physico-chimique de ces particules.The contamination rate can then be estimated by measuring the attenuation of the optical transmission of the slide, by examining it under a microscope or by dissolving the particles collected and physico-chemical analysis of these particles.
Le dispositif de prélèvement peut comprendre le passage d'un flux gazeux véhiculant tout ou partie des particules extraites, par dissolution des particules véhiculées dans le flux gazeux et analyse physico-chimique de ces particules, ou par un granulomètre placé en ligne avec le flux gazeux.The sampling device can comprise the passage of a gas flow conveying all or part of the particles extracted, by dissolving the particles conveyed in the gas flow and physico-chemical analysis of these particles, or by a granulometer placed in line with the gas flow. .
On peut également estimer le taux de contamination par arrêt des particules sur un filtre absolu et détection, soit par un examen microscopique du dépôt recueilli sur le filtre, soit par des mesures nucléaires si les particules contiennent des radioéléments.The contamination rate can also be estimated by stopping the particles on an absolute filter and detecting them, either by microscopic examination of the deposit collected on the filter, or by nuclear measurements if the particles contain radioelements.
L'invention a également pour objet un dispositif de prélèvement de particules d'un polluant recouvrant la surface d'un solide, comprenant une enceinte présentant une ouverture destinée à recouvrir une zone de ladite surface, l'enceinte étant pourvue d'une lame transparente à un faisceau laser destiné à extraire, par son impact sur ladite zone, lesdites particules, l'enceinte étant également pourvue d'un orifice d'entrée et d'un orifice de sortie permettant la circulation d'un gaz pour le transfert des particules, caractérisé en ce que l'orifice d'entrée du gaz est situé le plus près possible de la surface du solide. Ceci assure une meilleure captation des particules.The invention also relates to a device for sampling particles of a pollutant covering the surface of a solid, comprising an enclosure having an opening intended to cover an area of said surface, the enclosure being provided with a transparent blade to a laser beam intended to extract, by its impact on said zone, said particles, the enclosure also being provided with an inlet orifice and with an outlet orifice allowing the circulation of a gas for the transfer of the particles , characterized in that the gas inlet is located as close as possible to the surface of the solid. This ensures better capture of the particles.
Un tel dispositif a de plus l'avantage d'éviter la dispersion dans l'atmosphère ou le milieu ambiant de particules de polluant.Such a device also has the advantage of avoiding the dispersion in the atmosphere or the surrounding environment of pollutant particles.
Un autre orifice d'entrée du gaz peut être situé le plus près possible de la lame. Ceci évite le cas échéant l'opacification de la lame. Le dispositif est néanmoins utilisable quel que soit l'état de surface du solide. En effet, l'enceinte a un petit diamètre, compatible avec le diamètre du faisceau laser (<10 mm) et la latitude surface-orifice d'entrée est grande (plusieurs cm) puisqu'il suffit d'adapter le débit gazeux.Another gas inlet may be located as close as possible to the blade. This avoids the opacification of the blade if necessary. The device can nevertheless be used regardless of the surface state of the solid. In fact, the enclosure has a small diameter, compatible with the diameter of the laser beam (<10 mm) and the surface-inlet opening latitude is large (several cm) since it suffices to adapt the gas flow.
L'invention a aussi pour objet une installation pour le contrôle du taux de contamination par un polluant de la surface d'un solide, caractérisée en ce qu'elle comprend : - un dispositif de prélèvement tel que défini ci-dessus,The subject of the invention is also an installation for controlling the rate of contamination by a pollutant on the surface of a solid, characterized in that it comprises: a sampling device as defined above,
- un laser émettant un faisceau laser,- a laser emitting a laser beam,
- des moyens pour véhiculer ce faisceau laser jusqu'à la zone de la surface à contrôler, - des moyens permettant d'assurer la circulation du gaz de transfert des particules,means for conveying this laser beam to the area of the surface to be checked, means for ensuring the circulation of the particle transfer gas,
- des moyens permettant l'examen des particules transférées par ledit gaz.- Means for examining the particles transferred by said gas.
L'invention sera mieux comprise et d'autres particularités apparaîtront à la lecture de la description qui va suivre, donnée à titre d'exemple non limitatif, accompagnée des dessins annexés parmi lesquels :The invention will be better understood and other particularities will appear on reading the description which follows, given by way of nonlimiting example, accompanied by the appended drawings among which:
- la figure 1 représente une première variante d'un dispositif de prélèvement de particules d'un polluant recouvrant la surface d'un solide, selon l'invention ;- Figure 1 shows a first variant of a device for sampling particles from a pollutant covering the surface of a solid, according to the invention;
- la figure 2 représente une seconde variante d'un dispositif de prélèvement de particules d'un polluant recouvrant la surface d'un solide, selon 1'invention ;- Figure 2 shows a second variant of a device for sampling particles of a pollutant covering the surface of a solid, according to the invention;
- la figure 3 représente de manière schématique une installation pour le contrôle de l'état de contamination par un polluant de la surface d'un solide, selon 1'invention.- Figure 3 schematically shows an installation for controlling the state of contamination by a pollutant from the surface of a solid, according to the invention.
L'invention permet de détecter, de caractériser le cas échéant et de quantifier, s'il est nécessaire, des matériaux polluants tels que les radioéléments, les corps gras, des sels, des bactéries, des virus, etc.. à la surface de corps solides.The invention makes it possible to detect, characterize if necessary and quantify, if necessary, polluting materials such as radioelements, fatty substances, salts, bacteria, viruses, etc. on the surface of solid bodies.
Sur la figure 1, on a représenté un substratIn Figure 1, a substrate is shown
1 dont la surface est recouverte d'une couche 2 résultant du dépôt d'un matériau polluant. Pour procéder au contrôle de l'état de contamination de cette surface, on recouvre une zone 3 de cette surface par une enceinte cylindrique 4. L'une des extrémités de l'enceinte cylindrique est placée en vis-à-vis de la zone 3. L'autre extrémité est fermée par une lame 5.1, the surface of which is covered with a layer 2 resulting from the deposition of a polluting material. To control the state of contamination of this surface, a zone 3 of this surface is covered by a cylindrical enclosure 4. One of the ends of the cylindrical enclosure is placed opposite zone 3 The other end is closed by a blade 5.
L'extraction de particules de polluant est réalisée par l'impact d'un faisceau laser 6 traversant la lame 5 transparente pour la longueur d'onde du faisceau laser. L'extraction de particules peut se faire, comme il est bien connu, par effet thermique ou par effet de choc. Le laser est de préférence du type YAG et fonctionnant en régime puisé.The extraction of pollutant particles is carried out by the impact of a laser beam 6 passing through the transparent blade 5 for the wavelength of the laser beam. The extraction of particles can be done, as is well known, by thermal effect or by shock effect. The laser is preferably of the YAG type and operating in pulsed regime.
Suivant la nature physico-chimique du polluant, les particules 7 extraites de la couche de polluantDepending on the physicochemical nature of the pollutant, the particles 7 extracted from the pollutant layer
2 peuvent être aspirées le long du faisceau laser par l'effet plasma généré par celui-ci. Les particules remontent alors vers la source laser et se déposent sur la lame 5. Les particules peuvent ne pas être soumises à l'effet d'aspiration du faisceau laser. Pour les collecter, il est alors nécessaire de prévoir une circulation d'un flux gazeux entraînant les particules extraites de la couche 2. Ce flux gazeux peut être simplement causé par l'aspiration du gaz ambiant, en général l'air. Pour cela, l'enceinte 4 est maintenue en position de façon à laisser subsister un orifice d'entrée 10 du fluide ambiant près du substrat 1. En partie haute, le cylindre 4 communique avec un conduit d'aspiration 8 branché sur l'orifice de sortie 9. Cette disposition, c'est-à-dire l'orifice d'entrée près de la couche 2 et l'orifice de sortie plus éloigné, contribue à une bonne évacuation des particules extraites 7.2 can be sucked along the laser beam by the plasma effect generated by it. The particles then go up towards the laser source and settle on slide 5. Particles may not be subjected to the suction effect of the laser beam. To collect them, it is then necessary to provide for the circulation of a gas flow entraining the particles extracted from layer 2. This gas flow can simply be caused by the suction of the ambient gas, generally air. For this, the enclosure 4 is held in position so as to leave an inlet orifice 10 for the ambient fluid near the substrate 1. At the top, the cylinder 4 communicates with a suction duct 8 connected to the orifice outlet 9. This arrangement, that is to say the inlet orifice near the layer 2 and the more distant outlet orifice, contributes to good evacuation of the extracted particles 7.
La vitesse du flux de gaz doit être réglée en fonction de la nature du polluant pour permettre la meilleure évacuation possible des particules extraites. Ceci permet d'annuler les retombées du polluant extrait.The speed of the gas flow must be adjusted according to the nature of the pollutant to allow the best possible evacuation of the extracted particles. This makes it possible to cancel the fallout of the pollutant extracted.
Ces deux modes de collectes des particules extraites ne s'excluent pas mutuellement et le polluant peut se répartir sur la lame et dans le flux gazeux. Il faudra en tenir compte dans le cas d'une pollution complexe où certains constituants vont préférentiellement vers la lame et d'autres sont préférentiellement entraînés par le flux gazeux. Il faudra de même en tenir compte pour la quantification du polluant. L'enceinte 4 peut être métallique ou en plastique. Elle peut être disposée à quelques millimètres de la surface du substrat pour réaliser un orifice d'entrée de gaz de transport des particules.These two modes of collecting the extracted particles are not mutually exclusive and the pollutant can be distributed on the slide and in the gas flow. This will have to be taken into account in the case of complex pollution where certain constituents preferentially go towards the blade and others are preferentially entrained by the gas flow. It will also have to be taken into account for the quantification of the pollutant. The enclosure 4 can be metallic or plastic. It can be placed a few millimeters from the surface of the substrate to make an inlet port for the particle transport gas.
L'examen du dépôt obtenu sur la lame 5 et/ou des particules recueillies par aspiration permet de prendre connaissance de la nature du polluant et de le quantifier par des méthodes d'analyse et de quantification connues. La connaissance des caractéristiques du faisceau laser et du dispositif de prélèvement (dimensions, vitesse du flux de gaz, etc.) et la réalisation d'essais permet un étalonnage du matériel utilisé en fonction de la nature des polluants possibles.Examination of the deposit obtained on the slide 5 and / or of the particles collected by aspiration makes it possible to become aware of the nature of the pollutant and quantify it by known methods of analysis and quantification. Knowing the characteristics of the laser beam and the sampling device (dimensions, speed of the gas flow, etc.) and carrying out tests allows the equipment used to be calibrated according to the nature of the possible pollutants.
Le dépôt réalisé sur la lame peut être examiné et caractérisé au microscope. Ce dépôt peut être dissous dans un solvant approprié pour une analyse physico-chimique des particules.The deposit made on the slide can be examined and characterized under a microscope. This deposit can be dissolved in a suitable solvent for physicochemical analysis of the particles.
Dans le cas où l'extraction du polluant donne naissance à des particules pouvant entraîner une opacification de la lame mince par suite d'un dépôt important ou par impacts, le passage d'un flux gazeux pour véhiculer les particules extraites devient indispensable. On peut améliorer la protection de la lame 5 en créant une circulation de fluide ambiant entre celle-ci et le cylindre 4. La figure 2 représente une telle variante de réalisation. Les orifices 17 prévus dans le cylindre 4 juste sous la lame 5 permettent d'assurer cette circulation.In the case where the extraction of the pollutant gives rise to particles which can cause an opacification of the thin strip as a result of a significant deposit or by impacts, the passage of a gas flow to convey the extracted particles becomes essential. The protection of the blade 5 can be improved by creating an ambient fluid circulation between it and the cylinder 4. FIG. 2 shows such an alternative embodiment. The holes 17 provided in the cylinder 4 just under the blade 5 ensure this circulation.
La figure 3 représente une installation type pour le traitement des particules entraînées par un flux gazeux. Le laser 11 émet un faisceau lumineux qui est transporté vers le dispositif de prélèvement par exemple par un système à fibre optique 12, en tir direct ou par un jeu de miroirs. Le faisceau laser 6 peut être déplacé relativement par rapport à la surface à tester pour assurer un balayage de cette surface. Ce déplacement peut être assuré par une table à mouvements croisés, en particulier pour l'examen de surfaces planes, ou par un plateau tournant, en particulier pour les surfaces de révolution. Pour les surfaces complexes, un robot programmé peut assurer le déplacement de la fibre optique.FIG. 3 represents a typical installation for the treatment of particles entrained by a gas flow. The laser 11 emits a light beam which is transported to the sampling device for example by a fiber optic system 12, in direct fire or by a set of mirrors. The laser beam 6 can be moved relatively with respect to the surface to be tested to ensure scanning of this surface. This movement can be ensured by a table with crossed movements, in particular for examining flat surfaces, or by a turntable, in particular for surfaces of revolution. For the complex surfaces, a programmed robot can move the optical fiber.
Le conduit d'aspiration 8 est relié à un appareil 13. Cet appareil 13 peut être un appareil de prélèvement comprenant un filtre absolu, un barboteur, etc., selon l'art connu. Il peut s'agir d'un appareil de détection en ligne avec ou sans filtre aval ou d'un appareil de mesure en ligne avec ou sans filtre aval. Un débitmètre 14 connecté à l'appareil 13 permet le contrôle de la vitesse du gaz de transport à l'entrée et dans le dispositif de prélèvement. Le débitmètre 14 est relié à un ventilateur 15 assurant le débit gazeux et rejetant le gaz vers une gaine de ventilation, une cheminée ou, le cas échéant, un circuit de recyclage avec éventuellement un dispositif de filtration.The suction duct 8 is connected to an apparatus 13. This apparatus 13 can be a sampling apparatus comprising an absolute filter, a bubbler, etc., according to the known art. It can be an in-line detection device with or without a downstream filter or an in-line measuring device with or without a downstream filter. A flow meter 14 connected to the device 13 allows the speed of the transport gas to be controlled at the inlet and in the sampling device. The flow meter 14 is connected to a fan 15 ensuring the gas flow and rejecting the gas to a ventilation duct, a chimney or, where appropriate, a recycling circuit with possibly a filtration device.
Si le ventilateur n'est pas à vitesse variable, une vanne 16 d'entrée de gaz auxiliaire (de l'air par exemple) permet d'ajuster les débits de gaz nécessaires. Le polluant entraîné par le flux gazeux peut être détecté par un détecteur de particules en ligne. Il peut être détecté par arrêt des particules sur un filtre absolu suivi soit par examen microscopique du dépôt sur celui-ci, soit par une ou plusieurs mesures nucléaires dans le cas où le polluant contient des radioéléments. La caracterisation et la quantification du polluant peuvent être réalisées par dissolution du polluant déposé et analysé par des procédés physico-chimiques classiques. On peut aussi utiliser un appareil en ligne, par exemple un granulomètre.If the fan is not at variable speed, an auxiliary gas inlet valve 16 (for example air) makes it possible to adjust the gas flows required. The pollutant entrained by the gas flow can be detected by an online particle detector. It can be detected by stopping particles on an absolute filter followed either by microscopic examination of the deposit on it, or by one or more nuclear measurements in the case where the pollutant contains radioelements. Characterization and quantification of the pollutant can be carried out by dissolving the pollutant deposited and analyzed by conventional physicochemical processes. One can also use an on-line device, for example a granulometer.
L'invention permet d'obtenir les avantages suivants :The invention provides the following advantages:
- pas de dispersion du polluant sur la surface testée ; - pas de dispersion du polluant dans- no dispersion of the pollutant on the surface tested; - no dispersion of the pollutant in
1*environnement ; - la quantité de déchets induits est très faible : dans le cas d'un prélèvement sur filtre, celui-ci ne fait qu'environ 100 cm2 et dans le cas d'une mesure en ligne, le flux gazeux ne représente que quelques m3/h de prélèvement ;1 * environment; - the amount of waste generated is very low: in the case of sampling on a filter, it is only around 100 cm 2 and in the case of online measurement, the gas flow represents only a few m3 / h of collection;
- le circuit de prélèvement est compact et le volume pollué est donc plus faible et limité au dispositif de prélèvement et aux filtres éventuels ;- the sampling circuit is compact and the polluted volume is therefore lower and limited to the sampling device and any filters;
- la sensibilité est très bonne, le laser permettant de prélever des couches de polluant de quelques μm et le dispositif mis en oeuvre en assurant la concentration ;- the sensitivity is very good, the laser making it possible to remove layers of pollutant of a few μm and the device used ensuring concentration;
- la sensibilité est donc donnée par la surface explorée et la sensibilité de l'appareil de détection disposé dans le circuit ;the sensitivity is therefore given by the surface explored and the sensitivity of the detection device placed in the circuit;
- le coefficient de transfert des particules après évaluation permet une quantification en ligne ;- the particle transfer coefficient after evaluation allows online quantification;
- la vitesse d'exploration d'une surface contaminée est importante et peut atteindre plusieurs m2/h ;- the exploration speed of a contaminated surface is high and can reach several m 2 / h;
- l'invention permet un prélèvement à distance ce qui est avantageux lorsque le polluant ou le solide à tester est dangereux pour un intervenant ;- The invention allows remote sampling which is advantageous when the pollutant or the solid to be tested is dangerous for a worker;
- 1'invention permet 1'exploration de corps quasiment fermés tels que des corps creux, des rainures, des fissures, et pouvant présenter de mauvais états de surface ;- The invention allows the exploration of almost closed bodies such as hollow bodies, grooves, cracks, and which may have poor surface conditions;
- elle permet la détection, la caracterisation, la quantification du polluant suivant le besoin ; - la vérification de la mise en suspension du polluant sous l'effet laser ayant été faite une fois pour toutes, la méthode est rigoureuse et la représentativité en est donc assurée ;- it allows the detection, characterization, quantification of the pollutant according to the need; - the verification of the suspension of the pollutant under the laser effect having been done once and for all, the method is rigorous and the representativeness is therefore ensured;
- il n'y a pas d'altération de la surface du solide à tester. En optimisant les paramètres laser et ventilation dans chaque cas, on a obtenu, dans les expériences menées pour des polluants nucléaires, un taux de récupération des polluants surfacique de 50% sur du béton et de 90% sur des aciers inoxydables, en effectuant une seule passe laser. - there is no alteration of the surface of the solid to be tested. By optimizing the laser and ventilation parameters in each case, in the experiments conducted for nuclear pollutants, a surface pollutant recovery rate of 50% on concrete and 90% on stainless steels was obtained, by performing a single laser pass.

Claims

REVENDICATIONS
1. Procédé de contrôle de l'état de contamination par un polluant de la surface d'un solide (1), comprenant le prélèvement de particules de ce polluant sur une zone de la surface à contrôler pour quantifier le taux de contamination de cette surface, caractérisé en ce que :1. Method for controlling the state of contamination by a pollutant from the surface of a solid (1), comprising sampling particles of this pollutant from an area of the surface to be checked in order to quantify the rate of contamination of this surface , characterized in that:
- on dispose un dispositif de prélèvement sur la surface à contrôler et permettant d'accéder à ladite zone, ce dispositif permettant de collecter lesdites particules,- there is a sampling device on the surface to be checked and allowing access to said zone, this device making it possible to collect said particles,
- on soumet ladite zone à l'impact d'un faisceau laser (6) de caractéristiques telles qu'il provoque l'extraction desdites particules (7), - on recueille une fraction connue des particules extraites grâce au dispositif de prélèvement,- said zone is subjected to the impact of a laser beam (6) with characteristics such that it causes said particles (7) to be extracted, - a known fraction of the particles extracted is collected using the sampling device,
- on estime le taux de contamination de ladite surface par quantification des particules recueillies et en tenant compte des caractéristiques du faisceau laser et du dispositif de prélèvement.- Estimating the contamination rate of said surface by quantifying the particles collected and taking into account the characteristics of the laser beam and the sampling device.
2. Procédé de contrôle selon la revendication2. Control method according to claim
1, caractérisé en ce que le dispositif de prélèvement comprend une lame (5) transparente audit faisceau (6), disposée sur son trajet et placée de façon à recevoir les particules extraites qui sont aspirées le long du faisceau laser par l'effet plasma généré par ce faisceau.1, characterized in that the sampling device comprises a blade (5) transparent to said beam (6), arranged in its path and placed so as to receive the extracted particles which are sucked along the laser beam by the plasma effect generated by this beam.
3. Procédé de contrôle selon la revendication3. Control method according to claim
2, caractérisé en ce que l'on estime le taux de contamination par mesure de l'atténuation de la transmission optique de la lame.2, characterized in that the contamination rate is estimated by measuring the attenuation of the optical transmission of the blade.
4. Procédé de contrôle selon la revendication 2, caractérisé en ce que l'on estime le taux de contamination par examen au microscope de la lame. 4. Control method according to claim 2, characterized in that the contamination rate is estimated by examination of the slide under a microscope.
5- Procédé de contrôle selon la revendication 2, caractérisé en ce que l'on estime le taux de contamination par dissolution des particules recueillies et l'analyse physico-chimique de ces particules.5- Control method according to claim 2, characterized in that the contamination rate by dissolution of the particles collected and the physico-chemical analysis of these particles are estimated.
6. Procédé de contrôle selon l'une des revendications 1 ou 2, caractérisé en ce que le dispositif de prélèvement comprend le passage d'un flux gazeux véhiculant la fraction connue des particules extraites.6. Control method according to one of claims 1 or 2, characterized in that the sampling device comprises the passage of a gas flow conveying the known fraction of the particles extracted.
7. Procédé de contrôle selon la revendication 6, caractérisé en ce que l'on estime le taux de contamination par dissolution des particules véhiculées dans le flux gazeux et analyse physico-chimique de ces particules.7. Control method according to claim 6, characterized in that the contamination rate is estimated by dissolution of the particles conveyed in the gas flow and physico-chemical analysis of these particles.
8. Procédé de contrôle selon la revendication 6, caractérisé en ce que l'on estime le taux de contamination par un granulomètre placé en ligne avec le flux gazeux.8. Control method according to claim 6, characterized in that the contamination rate is estimated by a particle size analyzer placed in line with the gas flow.
9. Procédé de contrôle selon la revendication 6, caractérisé en ce que l'on estime le taux de contamination par arrêt des particules sur un filtre absolu et détection, soit par un examen microscopique du dépôt recueilli sur le filtre, soit par des mesures nucléaires si les particules contiennent des radioéléments. 9. Control method according to claim 6, characterized in that the contamination rate is estimated by stopping the particles on an absolute filter and detection, either by microscopic examination of the deposit collected on the filter, or by nuclear measurements. if the particles contain radioelements.
10. Dispositif de prélèvement de particules d'un polluant recouvrant la surface d'un solide, comprenant une enceinte (4) présentant une ouverture destinée à recouvrir une zone de ladite surface, l'enceinte étant pourvue d'une lame (5) transparente à un faisceau laser (6) destiné à extraire, par son impact sur ladite zone, lesdites particules (7), l'enceinte étant également pourvue un orifice d'entrée (10) et d'un orifice de sortie (9) permettant la circulation d'un gaz pour le transfert des particules, caractérisé en ce que l'orifice d'entrée (10) du gaz est situé le plus près possible de la surface du solide.10. Device for sampling particles of a pollutant covering the surface of a solid, comprising an enclosure (4) having an opening intended to cover an area of said surface, the enclosure being provided with a transparent blade (5) to a laser beam (6) intended to extract, by its impact on said zone, said particles (7), the enclosure also being provided with an inlet orifice (10) and an outlet orifice (9) allowing the circulation of a gas for the transfer of particles, characterized in that the gas inlet (10) is located as close as possible to the surface of the solid.
11. Dispositif selon la revendication 10, caractérisé en ce que l'enceinte est également pourvue d'un autre orifice d'entrée (17) du gaz qui est situé le plus près possible de la lame (5).11. Device according to claim 10, characterized in that the enclosure is also provided with another inlet orifice (17) for the gas which is located as close as possible to the blade (5).
12. Installation pour le contrôle du taux de contamination par un polluant de la surface d'un solide, caractérisé en ce qu'elle comprend :12. Installation for controlling the rate of contamination by a pollutant on the surface of a solid, characterized in that it comprises:
- un dispositif de prélèvement selon l'une des revendications 10 ou 11,- a sampling device according to one of claims 10 or 11,
- un laser émettant un faisceau laser,- a laser emitting a laser beam,
- des moyens pour véhiculer ce faisceau laser jusqu'à la zone de la surface à contrôler,means for conveying this laser beam to the area of the surface to be checked,
- des moyens permettant d'assurer la circulation du gaz de transfert des particules,means for ensuring the circulation of the particle transfer gas,
- des moyens permettant l'examen des particules transférées par ledit gaz. - Means for examining the particles transferred by said gas.
PCT/FR1994/001519 1993-12-23 1994-12-22 Method for determining the surface contamination of a solid, and device therefor WO1995017656A1 (en)

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