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An Appraisal of Analytical Methods for Plutonium and their Applications to the Analysis of Nuclear Materials; Evaluation des Methodes Analytiques de Dosage du Plutonium et de Leur Application a l'Analyse des Matieres Nucleaires; Otsenka analiticheskikh metodov opredeleniya plutoniya i ikh primenenie dlya analiza yadernykh materialov; Metodos Analiticos de Determinacion del Plutonio y su Empleo en el Analisis de Materiales Nucleares

Conference:

Abstract

A variety of methods is available for the determination of the plutonium content of nuclear materials. For milligram amounts of plutonium the available methods include differential spectrophotometry using the colour of Pu (III), gravimetry based on PuO{sub 2} gamma counting, and redox methods including potentiometric and amperometric titrations and controlled-potential coulometry. Alpha counting, isotopic dilution, and polarographic methods are suitable for microgram amounts. Some methods are more suitable than others for certain types of sample and the analyst is faced with difficult selection problems to achieve the best results. The advantages and limitations of the above methods are described in the light of a varied experience with them over many years at AERE, together with comments on accuracy, precision, sensitivity and features of special interest. Some of the methods cannot be applied without some separation of the plutonium from other sample constituents, and comments are made from experience in the use of anion exchange and reverse-phase chromatographic techniques for this with emphasis on their suitability for radioactive samples. Consideration is given to the many problems that have arisen in the successful application of these methods to the analysis of plutonium alloys, ceramics and cermets in various systems containing uranium, thorium,  More>>
Authors:
Milner, G. W.C.; Phillips, G. [1] 
  1. Atomic Energy Research Establishment, Harwell, Berks. (United Kingdom)
Publication Date:
Feb 15, 1966
Product Type:
Conference
Report Number:
IAEA-SM-67/51
Resource Relation:
Conference: Symposium on Nuclear Materials Management, Vienna (Austria), 30 Aug - 3 Sep 1965; Other Information: 20 refs., 9 tabs.; Related Information: In: Nuclear Materials Management. Proceedings of the Symposium on Nuclear Materials Management| 905 p.
Subject:
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS; AMPEROMETRY; CARBIDES; CERAMICS; CERMETS; CHROMATOGRAPHY; COST ESTIMATION; GRAVIMETRY; ION EXCHANGE; ISOTOPE DILUTION; MOLYBDENUM; NUCLEAR FUELS; NUCLEAR MATERIALS MANAGEMENT; PLUTONIUM; PLUTONIUM ALLOYS; PLUTONIUM OXIDES; POLAROGRAPHY; POTENTIOMETRY; SPECTROPHOTOMETRY; THORIUM; URANIUM
OSTI ID:
22127258
Research Organizations:
International Atomic Energy Agency, Vienna (Austria)
Country of Origin:
IAEA
Language:
English
Other Identifying Numbers:
Other: ISSN 0074-1884; TRN: XA13M2353082337
Submitting Site:
INIS
Size:
page(s) 691-704
Announcement Date:
Sep 12, 2013

Conference:

Citation Formats

Milner, G. W.C., and Phillips, G. An Appraisal of Analytical Methods for Plutonium and their Applications to the Analysis of Nuclear Materials; Evaluation des Methodes Analytiques de Dosage du Plutonium et de Leur Application a l'Analyse des Matieres Nucleaires; Otsenka analiticheskikh metodov opredeleniya plutoniya i ikh primenenie dlya analiza yadernykh materialov; Metodos Analiticos de Determinacion del Plutonio y su Empleo en el Analisis de Materiales Nucleares. IAEA: N. p., 1966. Web.
Milner, G. W.C., & Phillips, G. An Appraisal of Analytical Methods for Plutonium and their Applications to the Analysis of Nuclear Materials; Evaluation des Methodes Analytiques de Dosage du Plutonium et de Leur Application a l'Analyse des Matieres Nucleaires; Otsenka analiticheskikh metodov opredeleniya plutoniya i ikh primenenie dlya analiza yadernykh materialov; Metodos Analiticos de Determinacion del Plutonio y su Empleo en el Analisis de Materiales Nucleares. IAEA.
Milner, G. W.C., and Phillips, G. 1966. "An Appraisal of Analytical Methods for Plutonium and their Applications to the Analysis of Nuclear Materials; Evaluation des Methodes Analytiques de Dosage du Plutonium et de Leur Application a l'Analyse des Matieres Nucleaires; Otsenka analiticheskikh metodov opredeleniya plutoniya i ikh primenenie dlya analiza yadernykh materialov; Metodos Analiticos de Determinacion del Plutonio y su Empleo en el Analisis de Materiales Nucleares." IAEA.
@misc{etde_22127258,
title = {An Appraisal of Analytical Methods for Plutonium and their Applications to the Analysis of Nuclear Materials; Evaluation des Methodes Analytiques de Dosage du Plutonium et de Leur Application a l'Analyse des Matieres Nucleaires; Otsenka analiticheskikh metodov opredeleniya plutoniya i ikh primenenie dlya analiza yadernykh materialov; Metodos Analiticos de Determinacion del Plutonio y su Empleo en el Analisis de Materiales Nucleares}
author = {Milner, G. W.C., and Phillips, G.}
abstractNote = {A variety of methods is available for the determination of the plutonium content of nuclear materials. For milligram amounts of plutonium the available methods include differential spectrophotometry using the colour of Pu (III), gravimetry based on PuO{sub 2} gamma counting, and redox methods including potentiometric and amperometric titrations and controlled-potential coulometry. Alpha counting, isotopic dilution, and polarographic methods are suitable for microgram amounts. Some methods are more suitable than others for certain types of sample and the analyst is faced with difficult selection problems to achieve the best results. The advantages and limitations of the above methods are described in the light of a varied experience with them over many years at AERE, together with comments on accuracy, precision, sensitivity and features of special interest. Some of the methods cannot be applied without some separation of the plutonium from other sample constituents, and comments are made from experience in the use of anion exchange and reverse-phase chromatographic techniques for this with emphasis on their suitability for radioactive samples. Consideration is given to the many problems that have arisen in the successful application of these methods to the analysis of plutonium alloys, ceramics and cermets in various systems containing uranium, thorium, iron, chromium, molybdenum, cerium and cobalt. Difficulties occurring in the dissolution of samples and in the adjustment of the plutonium to the required valency state are described. The respective merits of dissolving in mixtures of common mineral acids and with the aid of fusion techniques are commented upon with examples. Outlines of procedures, together with analytical results for typical samples, are given for the analysis of Pu-U, Pu-Ce-Co and Pu-U-Mo alloys, Pu-U oxides and carbides, and Pu-U carbide cermets with Fe, Mo and Cr. These materials have arisen from metallurgical research and development programmes for new nuclear fuels. (author) [French] Il existe plusieurs methodes de dosage de la teneur en plutonium des matieres nucleaires. Pour les quantites de l'ordre du milligramme, les methodes utilisables sont la spectro- photometiie differentielle fondee sur la couleur de Pu (III), la gravimetrie fondee sur PuO{sub 2}, le comptage gamma et les methodes de reduction/oxydation comprenant les titrages poientiometriques et amperemetriques et la coulombmetrie a potentiel constant. Pour les quantites de Tordre du microgramme, le comptage alpha, la dilution isotopique et les methodes polarigraphiques sont a utiliser. Certaines methodes conviennent mieux que d'autres a des types determines d'echantillons et l'analyste soucieux d'obtenir les meilleurs resultats se heurte a un choix difficile. Les auteurs exposent les avantages et les inconvenients des methodes citees tels qu'ils se sont degages de l'experience acquise au cours des annees a l'Atomic Energy Research Establishment, et ils discutent l'exactitude, la precision, la sensibilite de ces methodes, et d'autres caracteristiques presentant un interet particulier. Certaines methodes ne peuvent etre utilisees si l'on n'a, dans une certaine mesure, separe le plutonium des autres constituants de l'echantillon et le memoire commente l'experience acquise avec l'echange d'anions et les procedes de chromatographie a phase inversee utilises a cette fin, en insistant surtout sur la mesure dans laquelle cette methode convient aux echantillons radioactifs. Les auteurs etudient en outre les nombreux problemes qui se sont poses lors de l'application (d'ailleurs couronnee de succes) de ces methodes a l'analyse des alliages de plutonium, des ceramiques et des cermets dans differentes combinaisons contenant de l'uranium, du thorium, du fer, du chrome, du molybdene, du cerium et du cobalt. Us exposent les difficultes de la dissolution des echantillons et de la reduction du plutonium a l'etat de valence voulu, ainsi que les avantages respectifs de la dissolution dans des melanges d'acides mineraux courants et de la dissolution faisant appel a des procedes de fusion, avec des exemples a l'appui. Les auteurs decrivent aussi les procedes utilises et les resultats obtenus, pour l'analyse des alliages Pu-U, Pu-Ce-Co et Pu-U-Mo, des oxydes et carbures de Pu-U, et des cermets de carbure de Pu-U contenant Fe, Mo et Cr. Ces matieres sont l'aboutissement de recherches metallurgiques destinees a mettre au point des combustibles nucleaires. (author) [Spanish] Para determinar el contenido de plutonio de los materiales nucleares existen diversos metodos. Si se trata de cantidades del orden del miligramo se pueden emplear la espectrofotometria diferencial por el color del Pu (III), la gravimetria basada en el PuO2{sub ,} si recuento gamma y metodos de oxidorreduccion como las valoraciones potenciometricas o amperimetricas y la culombiometria de potencial controlado. Si se trata de microgramos son preferibles el recuento alfa, la dilucion isotopica o las tecnicas polarograficas. Teniendo en cuenta que unos metodos son mas adecuados que otros para ciertos tipos de muestra, el analista tiene que resolver un dificil problema de seleccion a fin de obtener ios mejores resultados posibles. Los autores exponen las ventajas y las limitaciones puestas de manifiesto por los anos de experiencia en la A.E.R.E. y formulan observaciones acerca de la exactitud y la precision de los metodos, su sensibilidad y otras cuestiones de especial interes. Como algunos de esos metodos exigen la separacion previa del plutonio, los autores estudian el empleo de las tecnicas de intercambio anionico y de cromatografia en fase inversa, y en particular su conveniencia para el analisis de muestras radiactivas. Examinan los muchos problemas que han surgido al analizar por estos metodos, aleaciones, productos ceramicos y cermets de plutonio en diversos sistemas que contenian uranio, torio, hierro, cromo, molibdeno, cerio y cobalto. La memoria trata ademas de las dificultades que se encuentran al disolver las muestras y al llevar el plutonio al estado de valencia deseado. Comenta con ejemplos las ventajas y los inconvenientes de disolver las muestras en mezclas de acidos inorganicos corrientes o mediante tecnicas de fusion. Los autores exponen someramente los procedimientos de analisis y dan los resultados obtenidos con muestras tipicas de aleaciones de Pu-U, Pu-Ce-Co y Pu-U-Mo, oxidos y carburos de Pu-U, y cermets carburados de Pu-U con Fe, Mo y Cr. Estos materiales han ido surgiendo de los programas de investigacion metalurgica y de desarrollo de nuevos combustibles nucleares. (author) [Russian] Sushhestvujut razlichnye metody opredelenija soderzhanija plutonija v jadernyh materialah. Dlja opredelenija milligrammovyh kolichestv primenjajut metody, vkljuchaja differencial'nuju spektrofotometriju s ispol'zovaniem cve'a Pu(III), gravimetriju, osnovannuju na PUO{sub 2}, gamma-schet i metody okislenija-vosstanovlenija s potenciometricheskim i amperometricheskim titrovaniem i kontrol'no-potencial'noj ku- lonmetriej. Al'fa-schet, izotopnoe razbavlenie i poljarograficheskie metody vpolne prigodny dlja vychislenija mikrogrammovyh kolichestv. V svjazi s tem, chto nekotorye metody bolee prigodny po sravneniju s drugimi dlja nekotoryh obrazcov, lico, proizvodjashhee analiz, stalkivaetsja s trudnymi problemami vybora metoda dlja poluchenija nailuchshih rezul'tatov. Preimushhestva i nedostatki vysheukazannyh metodov opisyvajutsja v svete raznoobraznogo opyta, nakoplennogo pri rabote s nimi v techenie mnogih let v atomnom nauchno-issledovatel'skom centre v Harujelle, a takzhe izlagajutsja zamechanija o tochnosti, chetkosti, chuvstvitel'nosti i konstruktorskih osobennostjah, predstavljajushhih osobyj interes. Nekotorye metody nevozmozhno primenit' bez opredelennogo otdelenija plutonija ot drugih sostavnyh chastej obrazca. V svjazi s jetim izlagajutsja zamechanija na osnove opyta po ispol'zovaniju anionnogo obmena i hromatograficheskogo sposoba obratnoj fazy, prichem osoboe vnimanie obrashhaetsja na ih prigodnost' dlja radioaktivnyh obrazcov. Udeljaetsja vnimanie mnogim problemam, kotorye voznikajut pri uspeshnom primenenii jetih metodov dlja analiza splavov plutonija, keramiki i kermetov v razlichnyh sistemah, soderzhashhih uran, torij, zhelezo, hrom, molibden, cerij i kobal't. Opisyvajutsja trudnosti, voznikajushhie pri rastvorenii obrazcov i pri podgonke plutonija k trebuemomu sostojaniju valentnosti. V doklade na primerah kommentirujutsja sootvetstvujushhie preimushhestva rastvorenija v smesjah obychnyh mineral'nyh kislot s pomoshh'ju plavlenija. Izlagajutsja procedury s odnovremennym opisaniem analiticheskih rezul'tatov dlja tipichnyh obrazcov s cel'ju ispol'zovanija ih dlja analizov splavov Pu-U, Pu-Ce-Co i Pu-U-Mo, okisej i karbidov Pu-U karbidnyh kermetov Pu-U s dobavleniem Fe, M.o i Sg. Jeti materialy polucheny na osnove metallurgicheskih issledovanij i programmnyh razrabotok dlja novogo jadernogo topliva. (author)}
place = {IAEA}
year = {1966}
month = {Feb}
}