(U, Pu)O2 Powders and sintered pellets - Determination of chlorine and fluorine (ISO 21613:2015)

ISO 21613:2015 describes a method for determining chlorine and fluorine in mixed (U,Pu)O2 powders and sintered pellets. It is applicable for the analysis of samples containing 5 µg.g−1 to 50 µg.g−1 of chlorine and 2 µg.g−1 to 50 µg.g−1of fluorine.
For UO2 powder and sintered pellets, refer to ISO 22875.

(U, Pu)O2-Pulver und gesinterte Pellets - Bestimmung von Chlor und Fluor (ISO 21613:2015)

Diese Internationale Norm beschreibt ein Verfahren zur Bestimmung von Chlor und Fluor in (U,Pu)O2 Pulvern und gesinterten Pellets. Es ist für die Analyse von Proben anwendbar, die 5 µg ∙ g−1 bis 50 µg ∙ g−1 Chlor und 2 µg ∙ g−1 bis 50 µg ∙ g−1 Fluor enthalten.
Für UO2 Pulver und gesinterte Pellets, siehe ISO 22875.

Poudres et pastilles frittées (U,Pu)O2 - Détermination du chlore et du fluor (ISO 21613:2015)

L'ISO 21613:2015 décrit une méthode de dosage du chlore et du fluor dans les poudres et les pastilles frittées d'oxyde mixte (U,Pu)O2. Elle s'applique à l'analyse d'échantillons contenant de 5 µg.g−1 à 50 µg.g−1 de chlore et de 2 µg.g−1 à 50 µg.g−1 de fluor.
En ce qui concerne les poudres et les pastilles frittées d'UO2, voir la norme ISO 22875.

Prah in sintrani peleti (U, Pu)O2 - Ugotavljanje klora in fluora (ISO 21613:2015)

Standard ISO 21613:2015 opisuje metodo za ugotavljanje klora in fluora v mešanem prahu in sintranih peletih (U, Pu)O2. Uporablja se za analizo vzorcev, ki vsebujejo od 5 μg.g-1 do 50 μg.g-1 klora in od 2 μg.g-1 do 50 μg.g-1 fluora.
Za prah UO2 in sintrane pelete glej standard ISO 22875.

General Information

Status
Published
Publication Date
17-Oct-2017
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
18-Oct-2017
Completion Date
18-Oct-2017

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SLOVENSKI STANDARD
SIST EN ISO 21613:2018
01-februar-2018

Prah in sintrani peleti (U, Pu)O2 - Ugotavljanje klora in fluora (ISO 21613:2015)

(U, Pu)O2 Powders and sintered pellets - Determination of chlorine and fluorine (ISO

21613:2015)
(U, Pu)O2-Pulver und gesinterte Pellets - Bestimmung von Chlor und Fluor (ISO
21613:2015)

Poudres et pastilles frittées (U,Pu)O2 - Détermination du chlore et du fluor (ISO

21613:2015)
Ta slovenski standard je istoveten z: EN ISO 21613:2017
ICS:
27.120.30 Cepljivi materiali in jedrska Fissile materials and nuclear
gorivna tehnologija fuel technology
SIST EN ISO 21613:2018 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 21613:2018
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SIST EN ISO 21613:2018
EN ISO 21613
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2017
EUROPÄISCHE NORM
ICS 27.120.20
English Version
(U, Pu)O2 Powders and sintered pellets - Determination of
chlorine and fluorine (ISO 21613:2015)

Poudres et pastilles frittées (U,Pu)O2 - Détermination (U, Pu)O2-Pulver und gesinterte Pellets - Bestimmung

du chlore et du fluor (ISO 21613:2015) von Chlor und Fluor (ISO 21613:2015)
This European Standard was approved by CEN on 13 September 2017.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 21613:2017 E

worldwide for CEN national Members.
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SIST EN ISO 21613:2018
EN ISO 21613:2017 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 21613:2018
EN ISO 21613:2017 (E)
European foreword

The text of ISO 21613:2015 has been prepared by Technical Committee ISO/TC 85 “Nuclear energy,

nuclear technologies, and radiological protection” of the International Organization for Standardization

(ISO) and has been taken over as EN ISO 21613:2017 by Technical Committee CEN/TC 430 “Nuclear

energy, nuclear technologies, and radiological protection” the secretariat of which is held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by April 2018, and conflicting national standards shall be

withdrawn at the latest by April 2018.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,

France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,

Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and the United Kingdom.
Endorsement notice

The text of ISO 21613:2015 has been approved by CEN as EN ISO 21613:2017 without any modification.

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SIST EN ISO 21613:2018
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SIST EN ISO 21613:2018
INTERNATIONAL ISO
STANDARD 21613
First edition
2015-06-15
(U, Pu)O2 Powders and sintered
pellets — Determination of chlorine
and fluorine
Poudres et pastilles frittées (U,Pu)O2 — Détermination du chlore et
du fluor
Reference number
ISO 21613:2015(E)
ISO 2015
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SIST EN ISO 21613:2018
ISO 21613:2015(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
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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
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SIST EN ISO 21613:2018
ISO 21613:2015(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Principle ........................................................................................................................................................................................................................ 1

4 Reagents ........................................................................................................................................................................................................................ 1

5 Equipment ................................................................................................................................................................................................................... 4

5.1 Standard laboratory equipment............................................................................................................................................... 4

5.5 Ion analysis measuring with selective electrode equipment .......................................................................... 5

5.6 Ion-exchange chromatography system .............................................................................................................................. 5

5.7 Mortar ............................................................................................................................................................................................................. 5

6 Operating procedure ........................................................................................................................................................................................ 6

6.1 Sample pyrohydrolysis ..................................................................................................................................................................... 6

6.1.1 Blank test ................................................................................................................................................................................ 6

6.1.2 (U,Pu)O powder sample .......................................................................................................................................... 6

6.1.3 (U,Pu)O pellet sample ............................................................................................................................................... 6

6.1.4 Pyrohydrolysis ................................................................................................................................................................... 6

6.2 Measurement of pyrohydrolysis solutions...................................................................................................................... 8

6.2.1 Measurement by selective electrode .............................................................................................................. 8

6.2.2 Measurement by ionic chromatography ..................................................................................................... 9

6.3 Expression of results .......................................................................................................................................................................... 9

6.3.1 Calculation ............................................................................................................................................................................. 9

6.3.2 Validation limits .............................................................................................................................................................10

6.3.3 Determination limits .................................................................................................................................................10

6.3.4 Determination uncertainty ..................................................................................................................................11

7 Test report ................................................................................................................................................................................................................11

Bibliography .............................................................................................................................................................................................................................12

© ISO 2015 – All rights reserved iii
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SIST EN ISO 21613:2018
ISO 21613:2015(E)
Foreword

ISO (the International Organization for Standardization) 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

organizations, 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 standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).

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. Details of any

patent rights identified during the development of the document will be in the Introduction and/or on

the ISO list of patent declarations received (see www.iso.org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers

to Trade (TBT) see the following URL: Foreword - Supplementary information

The committee responsible for this document is ISO/TC 85, Nuclear energy, nuclear technologies, and

radiological protection, Subcommittee SC 5, Nuclear fuel cycle.
iv © ISO 2015 – All rights reserved
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SIST EN ISO 21613:2018
INTERNATIONAL STANDARD ISO 21613:2015(E)
(U, Pu)O2 Powders and sintered pellets — Determination
of chlorine and fluorine
1 Scope

This International Standard describes a method for determining chlorine and fluorine in mixed (U,Pu)

O powders and sintered pellets. It is applicable for the analysis of samples containing 5 µg.g to 50 µg.

−1 −1 −1
g of chlorine and 2 µg.g to 50 µg.g of fluorine.
For UO powder and sintered pellets, refer to ISO 22875.
2 Normative references

The following documents, in whole or in part, are normatively referenced in this document and are

indispensable for its application. For dated references, only the edition cited applies. For undated

references, the latest edition of the referenced document (including any amendments) applies.

ISO 3696, Water for analytical laboratory use — Specification and test methods

ISO 22875, Nuclear energy — Determination of chlorine and fluorine in uranium dioxide powder and

sintered pellets

ISO 9892, Uranium metal, uranium dioxide powder and pellets, and uranyl nitrate solutions — Determination

of fluorine content — Fluoride ion selective electrode method
3 Principle

The samples are pyrohydrolyzed at 850 °C – 1 000 °C in a tubular furnace with steam or moist oxygen.

Chlorine and fluorine are trapped as halogenated acids and entrained in an aqueous solution. Chloride

and fluoride ions are measured using selective electrodes or another appropriate method, for instance,

ionic chromatography.
4 Reagents
Use only reagents of recognized analytical grade.

4.1 Demineralised water, complying with at least grade 1 in accordance with ISO 3696 is recommended.

4.2 Anhydrous sodium chloride (NaCl), analytical grade.
4.3 Anhydrous sodium fluoride (NaF), analytical grade.

4.4 Concentrated sodium hydroxide solution, w(NaOH) = 32 %, relative density approximately

1,35 g.ml .

Concentrated sodium hydroxide solution (4.4) is used to prepare sodium hydroxide solutions (4.4.1,

4.4.2, and 4.4.3). Concentrations of solutions (4.4.1, 4.4.2, and 4.4.3) are examples of reference solutions

that are acceptable for use.
4.4.1 Sodium hydroxide solution, c(NaOH) = 5 mol.l .

This reagent can also be prepared by using solid sodium hydroxide in various ways.

© ISO 2015 – All rights reserved 1
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SIST EN ISO 21613:2018
ISO 21613:2015(E)
For example, the procedure can be as follows.

Pour 460 ml of concentrated sodium hydroxide solution (4.4) into 1 000 ml volumetric flask, dilute to the

mark using demineralised water (4.1), and mix.

This reagent can also be prepared by dissolving solid sodium hydroxide (4.5) in solution using

demineralised water (4.1).
4.4.2 Sodium hydroxide solution, c(NaOH) = 0,5 mol.l .

Pour 46 ml of concentrated sodium hydroxide solution (4.4) into 1 000 ml volumetric flask, dilute to the

mark using demineralised water (4.1), and mix.
4.4.3 Sodium hydroxide solution, c(NaOH) = 0,05 mol.l .

Pour 100 ml of 0,5 mol/l sodium hydroxide (4.4.2) into 1 000 ml volumetric flask, dilute to the mark

using demineralised water (4.1), and mix.
−4 −1
4.4.4 Sodium hydroxide solution, c(NaOH) = 10 mol.l (or pH 10).

The concentration of solution (4.4.4) is an example of a receiver solution that can be used for a

measurement by chromatography.
4.5 Anhydrous sodium hydroxide (NaOH), granules.
4.6 Glacial acetic acid, (CH COOH), relative density approximately 1,06 g.ml .
4.7 Sodium acetate, (CH COONa) analytical grade.
4.8 Buffer solution.

Using the following buffer solution is recommended in order to ensure that the absorbing solution

remains alkaline. An example of the procedure to prepare the buffer solution is as follows.

Pour 15 ml of acetic acid (4.6) into 1 000 ml polyethylene volumetric flask and dissolve 50 g of sodium

acetate (4.7). Adjust the solution volume to about 900 ml with demineralised water (4.1). Adjust the pH

to 5,3 with the 5 mol.l sodium hydroxide solution (4.4.1), for example, then dilute to the mark using

demineralised water (4.1) and mix.

pH adjustment can be performed with a different sodium hydroxide solution concentration.

Another reagent such as NaOH solution with phenolphthalein can also be used.
4.9 Chloride reference solution.
- −1
4.9.1 Primary chloride reference solution, c(Cl ) = 0,5 g.l .

Dissolve 166 mg of dry anhydrous sodium chloride (4.2) in demineralised water (4.1). Pour into a 200 ml

volumetric flask, then dilute to the mark using demineralised water (4.1) and mix.

Primary chloride reference solution (4.9.1) is used to prepare chloride reference solutions (4.9.2, 4.9.3,

4.9.4, 4.9.5, and 4.9.6). Concentrations of solutions (4.9.2, 4.9.3, 4.9.4, and 4.9.5) are examples of reference

solutions that can be used for calibration of selective electrodes. Exact concentrations of calibration

solutions should be determined by the user based upon the expected concentration of analyte in the

NaOH buffer solution.
2 © ISO 2015 – All rights reserved
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SIST EN ISO 21613:2018
ISO 21613:2015(E)
- −1
4.9.2 Chloride reference solution, c(Cl ) = 35 mg.l .

Pipette 70 ml of the primary reference solution (4.9.1) into 1 000 ml flask. Dilute to the mark with the

0,05 mol.l sodium hydroxide solution (4.4.3) and mix.
- −1
4.9.3 Chloride reference solution, c(Cl ) = 8 mg.l .

Pipette 16 ml of the primary reference solution (4.9.1) into 1 000 ml flask. Dilute to the mark with the

0,05 mol.l sodium hydroxide solution (4.4.3) and mix.
- −1
4.9.4 Chloride reference solution, c(Cl ) = 2,5 mg.l .

Pipette 5 ml of the primary reference solution (4.9.1) into 1 000 ml flask. Dilute to the mark with the

0,05 mol.l sodium hydroxide solution (4.4.3) and mix.
- −1
4.9.5 Chloride reference solution, c(Cl ) = 2 mg.l .

Pipette 25 ml of the reference solution (4.9.3) into a 100 ml flask. Dilute to the mark with the 0,05 mol.

l sodium hydroxide solution (4.4.3) and mix.
- −1
4.9.6 Chloride reference solution, c(Cl ) = X mg.l .

Other chloride reference solution concentrations may be used. For example, a reference solution can

be prepared by diluting the reference solution of 4.9.1 with the 0,05 mol.l sodium hydroxide solution

(4.4.3) to obtain the reference solution (4.9.6).
4.10 Fluoride reference solution.
- −1
4.10.1 Primary fluoride reference solution, c(F ) = 0,5 g.l .

Dissolve 221 mg of dry anhydrous sodium fluoride (4.3) in demineralised water (4.1). Pour into a 200 ml

volumetric flask, dilute to the mark using demineralised water (4.1), and mix.

Primary fluoride reference solution (4.10.1) is used to prepare fluoride reference solutions (4.10.2, 4.10.3,

4.10.4, 4.10
...

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