Nuclear fuel technology — Controlled-potential coulometric assay of plutonium

ISO 12183:2016 describes an analytical method for the electrochemical assay of pure plutonium nitrate solutions of nuclear grade, with a total uncertainty not exceeding ±0,2 % at the confidence level of 0,95 for a single determination (coverage factor, K = 2). The method is suitable for aqueous solutions containing more than 0,5 g/L plutonium and test samples containing between 4 mg and 15 mg of plutonium. Application of this technique to solutions containing less than 0,5 g/L and test samples containing less than 4 mg of plutonium requires experimental demonstration by the user that applicable data quality objectives will be met. For some applications, purification of test samples by anion exchange is required before measurement to remove interfering substances when present in significant amounts.

Technologie du combustible nucléaire — Dosage du plutonium par coulométrie à potentiel imposé

L'ISO 12183:2016 décrit une méthode analytique pour le dosage électrochimique de plutonium pur dans des solutions nitriques de qualité nucléaire, avec une incertitude ne dépassant pas ± 0,2 % dans un intervalle de confiance de 0,95 pour une simple détermination (facteur d'élargissement, K = 2). La méthode est adaptée aux solutions aqueuses contenant plus de 0,5 g/L de plutonium et à des échantillons d'essai contenant entre 4 mg et 15 mg de plutonium. L'application de cette technique aux solutions contenant moins de 0,5 g/L et d'échantillons d'essai contenant moins de 4 mg de plutonium exige que l'utilisateur démontre expérimentalement que les objectifs relatifs à la qualité des données applicables soient atteints. Pour certaines applications, une purification des échantillons d'essai par échange anionique est nécessaire avant la mesure pour éliminer les substances interférentes présentes en quantités significatives. Se reporter à l'Article 10 qui traite des interférences et des actions correctives. La purification est aussi nécessaire dans les situations où la pureté de l'échantillon d'essai n'est pas connue ou quand elle peut fluctuer de façon imprévisible dans le procédé de fabrication. L'Article 11 traite des changements dans l'application de la méthode et de la méthodologie qui peuvent être appliquées et des considérations importantes pour sélectionner les paramètres de mesure, tout en restant à l'intérieur du domaine d'application du présent document.

General Information

Status
Withdrawn
Publication Date
04-Aug-2016
Current Stage
9599 - Withdrawal of International Standard
Completion Date
07-May-2024
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Standards Content (Sample)

DRAFT INTERNATIONAL STANDARD
ISO/DIS 12183
ISO/TC 85/SC 5 Secretariat: BSI
Voting begins on: Voting terminates on:
2015-09-01 2015-12-01
Nuclear fuel technology — Controlled-potential
coulometric assay of plutonium
Technologie du combustible nucléaire — Dosage du plutonium par coulométrie à potentiel imposé
ICS: 27.120.30
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 12183:2015(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2015

---------------------- Page: 1 ----------------------
ISO/DIS 12183:2015(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2015, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2015 – All rights reserved

---------------------- Page: 2 ----------------------
ISO/DIS 12183
Contents Page
Foreword iv
1 Scope 1
2 Normative References 1
3 Principle 1
4 Reagents 2
5 Apparatus 2
6 Procedure 7
6.1 Plutonium determination 7
6.2 Analysis of subsequent test samples 13
7 Expression of results 14
7.1 Calculation of the electrical calibration factor 14
7.2 Calculation of the blank 14
7.3 Fraction of electrolysed plutonium 15
7.4 Plutonium content 15
7.5 Quality control 16
8 Characteristics of the method 16
8.1 Repeatability 16
8.2 Confidence interval 16
8.3 Analysis time 16
9 Interferences 17
10 Procedure variations and optimisation 20
10.1 Accountability measurements and reference material preparation 20
10.2 Process control measurements 20
10.3 Measurement cell design 21
10.4 Electrolyte and electrode options 21
10.5 Test sample size 22
10.6 Background current corrections 22
10.7 Correction for iron 23
10.8 Control-potential adjustment 23
10.9 Calibration Methodologies 23
Annex A (normative) Purification by anion-exchange separation 25
Annex B (normative) Determination of formal potential, E 27
0
Bibliography 28

© ISO 2015 – All rights reserved iii

---------------------- Page: 3 ----------------------
ISO/DIS 12183
Foreword
ISO (the International Organisation for Standardisation) is a worldwide federation of national standards bodies (ISO
member bodies). The work of preparing International Standards is normally carried out through ISO technical
committees. Each member body interested in a subject for which a technical committee has been established has
the right to be represented on that committee. International organisations, governmental and non-governmental, in
liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardisation.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
The main task of the technical committee is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights.
ISO shall not be held responsible for identifying any or all such patent rights.
ISO 12813 was prepared by Technical Committee ISO/TC 85, Nuclear energy, nuclear technologies, and
radiological protection, Subcommittee SC 5, Nuclear fuel cycle.
This third edition cancels and replaces the second edition (ISO 12183:2005), which has been technically revised.

© ISO 2015 – All rights reserved iv

---------------------- Page: 4 ----------------------
ISO/DIS 12183
Nuclear Energy — Fuel Technology — Controlled-potential
coulometric assay of plutonium
1 Scope
This International Standard describes an analytical method for the electrochemical assay of pure
plutonium nitrate solutions of nuclear grade, with a total uncertainty not exceeding ± 0,2 % at the
confi
...

INTERNATIONAL ISO
STANDARD 12183
Third edition
2016-08-15
Nuclear fuel technology — Controlled-
potential coulometric assay of
plutonium
Technologie du combustible nucléaire — Dosage du plutonium par
coulométrie à potentiel imposé
Reference number
ISO 12183:2016(E)
©
ISO 2016

---------------------- Page: 1 ----------------------
ISO 12183:2016(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved

---------------------- Page: 2 ----------------------
ISO 12183:2016(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 2
7 Procedure. 8
7.1 Plutonium determination . 8
7.1.1 Weighing the test sample, with an uncertainty of ±0,01 %, K = 1. . 8
7.1.2 Preparation of the test sample . 9
7.1.3 Electrode pre-treatment. 9
7.1.4 Electrical calibration of the current integration system .10
7.1.5 Formal potential determination .11
7.1.6 Coulometric blank determination.12
7.1.7 Plutonium measurement .13
7.2 Analysis of subsequent test samples .13
8 Expression of results .14
8.1 Calculation of the electrical calibration factor .14
8.2 Calculation of the blank .14
8.3 Fraction of electrolysed plutonium .
...

NORME ISO
INTERNATIONALE 12183
Troisième édition
2016-08-15
Technologie du combustible
nucléaire — Dosage du plutonium par
coulométrie à potentiel imposé
Nuclear fuel technology — Controlled-potential coulometric assay of
plutonium
Numéro de référence
ISO 12183:2016(F)
©
ISO 2016

---------------------- Page: 1 ----------------------
ISO 12183:2016(F)

DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2016, Publié en Suisse
Droits de reproduction réservés. Sauf indication contraire, aucune partie de cette publication ne peut être reproduite ni utilisée
sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique, y compris la photocopie, l’affichage sur
l’internet ou sur un Intranet, sans autorisation écrite préalable. Les demandes d’autorisation peuvent être adressées à l’ISO à
l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – Tous droits réservés

---------------------- Page: 2 ----------------------
ISO 12183:2016(F)

Sommaire Page
Avant-propos .iv
1 Domaine d’application . 1
2 Références normatives . 1
3 Termes et définitions . 1
4 Principe . 1
5 Réactifs . 2
6 Appareillage . 2
7 Mise en œuvre . 8
7.1 Mesure du plutonium . 8
7.1.1 Pesée de l’échantillon d’essai, avec une incertitude de ± 0,01 %, K = 1. . 8
7.1.2 Préparation de l’échantillon d’essai . 9
7.1.3 Traitement préliminaire de l’électrode . 9
7.1.4 Étalonnage électrique du système d’intégration de courant .11
7.1.5 Détermination du potentiel formel .11
7.1.6 Détermination du blanc coulométrique .12
7.1.7 Mesure du plutonium .13
7.2 Analyse d’échantillons d’essai successifs .14
8 Expression des résultats.14
8.1 Calcul du facteur d’étalonnage électrique .14
8.2 Calcul du blanc .15
8.3 Fraction de plutonium électrolysé .
...

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