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AbstractAbstract
[en] The purpose of this work is to use the radiofrequency glow discharge optical emission spectrometry in order to quantitatively determine carbon, nitrogen, oxygen and hydrogen at low concentration (in the ppm range) in nuclear materials. In this study, and before the definitive contamination of the system, works are carried out on non radioactive materials (steel, pure iron, copper and titanium). As the initial apparatus could not deliver a RF power inducing a reproducible discharge and was not adapted to the analysis of light elements: 1- The radiofrequency system had to be changed, 2- The systems controlling gaseous atmospheres had to be improved in order to obtain analytical signals stemming strictly from the sample, 3- Three discharge lamps had to be tested and compared in terms of performances, 4- The system of collection of light had to be optimized. The modifications that were brought to the initial system improved intensities and stabilities of signals which allowed lower detection limits (1000 times lower for carbon). These latter are in the ppm range for carbon and about a few tens of ppm for nitrogen and oxygen in pure irons. Calibration curves were plotted in materials presenting very different sputtering rates in order to check the existence of a 'function of analytical transfer' with the purpose of palliating the lack of reference materials certified in light elements at low concentration. Transposition of this type of function to other matrices remains to be checked. Concerning hydrogen, since no usable reference material with our technique is available, certified materials in deuterium (chosen as a surrogate for hydrogen) were studied in order to exhibit the feasibility the analysis of hydrogen. Parallel to these works, results obtained by modeling a RF discharge show that the performances of the lamp can be improved and that the optical system must be strictly adapted to the glow discharge. (author)
[fr]
L'objet de ce travail est l'utilisation d'un spectrometre d'emission optique a decharge luminescente radiofrequence pour l'analyse quantitative des elements carbone, azote, oxygene et hydrogene a faible concentration (de l'ordre de la ppm massique) dans les materiaux nucleaires. Dans cette etude, et avant de contaminer le systeme, les essais sont realises sur des matrices non radioactives (acier, fer pur, cuivre et titane). L'appareil initialement a notre disposition n'etant pas capable de delivrer une puissance RF assurant une decharge reproductible et n'etant pas adapte a l'analyse des elements legers, nous avons du: 1- modifier le systeme de puissance, 2- ameliorer les systemes de controle des atmospheres gazeuses pour obtenir des signaux analytiques ne provenant que de l'echantillon, 3- tester trois lampes a decharge et comparer leurs performances, 4- optimiser le systeme optique de collecte de lumiere. Les modifications apportees ont ameliore les stabilites et les intensites des signaux ce qui a pemis d'abaisser les limites de detection (d'un facteur 1000 pour le carbone). Ces dernieres sont dans les fers purs l'ordre de la ppm pour le carbone et de quelques dizaines de ppm pour l'azote et l'oxygene. Pour remedier au manque d'etalons certifies en elements legers a faible concentration, l'existence 'fonction de transfert analytique' entre les droites d'etalonnage obtenues avec des materiaux de vitesses de pulverisation tres differentes a ete verifiee. La transposition a d'autres materiaux de ce type de fonction reste a verifier. Quant a l'hydrogene, aucun materiau de reference utilisable avec notre technique n'etant disponible, des materiaux certifies en deuterium (pris comme 'fantome' de l'hydrogene) ont ete utilises pour montrer la faisabilite de l'analyse de l'hydrogene. Enfin, les resultats obtenus par simulation d'une decharge RF montrent la possibilite d'ameliorer les performances de la source et l'importance de l'adequation du systeme optique a la dechargeOriginal Title
Adaptation d'un spectrometre d'emission optique a decharge luminescente radiofrequence (RF-GD-OES) pour l'analyse des elements legers (carbone, azote, oxygene et hydrogene) dans les solides. Integration en boites a gants pour l'analyse des materiaux nucleaires
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30 Jan 2001; 172 p; 187 refs.; Available from the INIS Liaison Officer for France, see the 'INIS contacts' section of the INIS website for current contact and E-mail addresses: http://www.iaea.org/inis/Contacts/; Also available from Service Commun de la Documentation Bibliotheque universitaire de sciences-economie, 6 rue Sully, 21000 Dijon (France); Chimie Physique
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