EN ISO 15651:2017

Nuclear energy - Determination of total hydrogen content in PuO2 and UO2 powders and UO2, (U,Gd)O2 and (U,Pu)O2 sintered pellets - Inert gas extraction and conductivity detection method (ISO 15651:2015)

ISO 15651:2015 describes a procedure for measuring the total hydrogen content of UO2 and PuO2 powders (up to 2 000 µg/g oxide) and of U02 and (U,Gd)O2 and (U,Pu)O2 pellets (up to 10 µg/g oxide). The total hydrogen content results from adsorbed water, water of crystallization,  hydro-carbon, and other hydrogenated compounds which can exist as impurities in the fuel.

Kernenergie - Bestimmung des totalen Wasserstoffgehalts in PuO₂- und UO₂-Pulvern und UO₂-, (U,Gd)O₂- und (U,Pu)O₂-gesinterten Pellets - Trägergasheißextraktion und Leitfähigkeitsbestimmungsverfahren (ISO 15651:2015)

Diese Internationale Norm legt ein Verfahren zur Messung des Gesamtgehalts an Wasserstoff in UO2- und PuO2-Pulvern (bis zu 2 000 μg/g Oxid) und in UO2- und (U,Gd)O2- sowie (U,Pu)O2-Pellets (bis zu 10 μg)/g Oxid) fest. Der Gesamtgehalt an Wasserstoff ergibt sich aus adsorbiertem Wasser, Kristallwasser, Kohlenwasserstoff und anderen hydrierten Verbindungen, die als Verunreinigungen im Brennstoff vorhanden sein können.

Énergie nucléaire - Dosage de la teneur totale en hydrogène de poudres de PuO2 et UO2, et de pastilles frittées d'UO2, (U,Gd)O2 et (U,Pu)O2 - Méthode d'extraction par gaz inerte et méthode de mesure de la conductivité (ISO 15651:2015)

L'ISO 15651:2015 décrit un mode opératoire permettant de mesurer la teneur totale en hydrogène de poudres d'UO2 et PuO2 (jusqu'à 2 000 µg/g d'oxyde) et de pastilles d'UO2, (U,Gd)O2 et (U,Pu)O2 (jusqu'à 10 µg/g d'oxyde). La teneur totale en hydrogène provient de l'eau adsorbée, de l'eau de cristallisation, et des hydrocarbures et autres composés hydrogénés qui peuvent exister à l'état d'impuretés dans le combustible.

Jedrska energija - Ugotavljanje deleža vodika v PuO2 in praških UO2 ter v sintranih peletih UO2, (U,Gd)O2 in (U,Pu)O2 - Metoda z ekstrakcijo inertnih plinov in ugotavljanjem prevodnosti (ISO 15651:2015)

Standard ISO 15651:2015 opisuje postopek za merjenje deleža vodika v praških UO2 in PuO2 (do 2000 µg/g kisika) ter v peletih U02, (U,Gd)O2 in (U,Pu)O2 (do 10 µg/g kisika). Delež vodika je posledica absorbirane vode, vode kristalizacije, ogljikovodika in drugih hidrogeniranih spojin, ki so lahko prisotne v gorivu kot nečistoče.

General Information

• Status: Published
• Publication Date: 10-Oct-2017
• Withdrawal Date: 29-Apr-2018
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: CEN/TC 430 - Nuclear energy, nuclear technologies, and radiological protection
• Drafting Committee: CEN/TC 430 - Nuclear energy, nuclear technologies, and radiological protection
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 11-Oct-2017
• Due Date: 05-May-2019
• Completion Date: 11-Oct-2017
• Ref Project: SIST EN ISO 15651:2017 - Nuclear energy - Determination of total hydrogen content in PuO2 and UO2 powders and UO2, (U,Gd)O2 and (U,Pu)O2 sintered pellets - Inert gas extraction and conductivity detection method (ISO 15651:2015)

Overview

EN ISO 15651:2017 (identical to ISO 15651:2015) specifies a laboratory method for the determination of total hydrogen content in nuclear fuel materials: PuO2 and UO2 powders and UO2, (U,Gd)O2 and (U,Pu)O2 sintered pellets. The method uses inert gas extraction (argon or nitrogen carrier gas) and thermal conductivity (conductivity) detection with a hydrogen analyser. Reported measurement ranges cover powders (up to 2 000 µg H/g oxide) and sintered pellets (up to 10 µg H/g oxide).

Key topics and technical requirements

• Measurement principle: Rapid high‑temperature decomposition (>1 770 °C) in a graphite crucible to release hydrogen from adsorbed water, water of crystallization, hydrocarbons and other hydrogenated impurities; separation and detection of hydrogen by chromatography and a thermal conductivity cell.
• Temperature control: Heating to >1 770 °C within ≈5 s is required to ensure complete decomposition; avoid temperatures >2 200 °C to prevent CO2 formation from UO2–graphite reactions that interfere with detection.
• Carrier gas and purity: Use argon (≥99.995% v/v) or nitrogen (≥99.998% v/v). Calibration gases or certified mixes with known hydrogen are required for instrument calibration.
• Apparatus & consumables:
  • Furnace and hydrogen analyser with thermal conductivity detector; furnace capable of at least 2 200 °C.
  • High‑purity graphite crucibles (impurities ≤2 µg/g).
  • Hydrogen‑free tin, copper or nickel capsules; analytical balance (1 mg resolution).
  • Purification reagents/columns: CuO, anhydrone (Mg(ClO4)2), Schutze reagent, Hopcalite, NaOH over clay.
• Sampling and sample handling:
  • Powder samplers with diameter >2.5× maximum particle size; exposure to ambient air limited to ≤5 minutes unless handled in a glove box.
  • Store samples in tight containers with minimal headspace; check mass before/after storage when delayed analysis.
• Calibration and quality control: Calibration by gas or certified reference materials (e.g., Ti or Zr standards); blank tests and calibration checks specified. Measurement uncertainty guided by ISO/IEC Guide 98‑3 (GUM).

Applications

• Quality control and acceptance testing of nuclear fuel powders and sintered pellets.
• Fuel manufacturing process monitoring (drying, sintering, storage) to detect hydrogen-related impurities.
• Safety and performance assessments where hydrogen content affects fuel behavior (oxidation, thermal properties).

Who uses it

• Nuclear fuel manufacturers, fuel technologists, R&D laboratories, and regulatory testing facilities involved in nuclear fuel quality assurance, characterization of fissile materials, and material certification.

Related standards

• ISO 15651:2015 (original international text adopted as EN ISO 15651:2017)
• ISO/IEC Guide 98-3:2008 (GUM: uncertainty of measurement)

Standards Content (Sample)

SLOVENSKI STANDARD
01-december-2017
Jedrska energija - Ugotavljanje deleža vodika v PuO2 in praških UO2 ter v
sintranih peletih UO2, (U,Gd)O2 in (U,Pu)O2 - Metoda z ekstrakcijo inertnih plinov
in ugotavljanjem prevodnosti (ISO 15651:2015)
Nuclear energy - Determination of total hydrogen content in PuO2 and UO2 powders and
UO2, (U,Gd)O2 and (U,Pu)O2 sintered pellets - Inert gas extraction and conductivity
detection method (ISO 15651:2015)
.HUQHQHUJLH%HVWLPPXQJGHVWRWDOHQ:DVVHUVWRIIJHKDOWVLQ3X2"XQG82"3XOYHUQ
XQG82"8*G2"XQG83X2"JHVLQWHUWH3HOOHWV7UlJHUJDVKHL‰H[WUDNWLRQXQG
/HLWIlKLJNHLWVEHVWLPPXQJVYHUIDKUHQ,62
Énergie nucléaire - Dosage de la teneur totale en hydrogène de poudres de PuO2 et
UO2, et de pastilles frittées d'UO2, (U,Gd)O2 et (U,Pu)O2 - Méthode d'extraction par gaz
inerte et méthode de mesure de la conductivité (ISO 15651:2015)
Ta slovenski standard je istoveten z: EN ISO 15651:2017
ICS:
27.120.30 Cepljivi materiali in jedrska Fissile materials and nuclear
gorivna tehnologija fuel technology
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 15651
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2017
EUROPÄISCHE NORM
ICS 27.120.30
English Version
Nuclear energy - Determination of total hydrogen content
in PuO2 and UO2 powders and UO2, (U,Gd)O2 and
(U,Pu)O2 sintered pellets - Inert gas extraction and
conductivity detection method (ISO 15651:2015)
Énergie nucléaire - Dosage de la teneur totale en Kernenergie - Bestimmung des totalen
hydrogène de poudres de PuO2 et UO2, et de pastilles Wasserstoffgehalts in PuO2- und UO2-Pulvern und
frittées d'UO2, (U,Gd)O2 et (U,Pu)O2 - Méthode UO2-, (U,Gd)O2- und (U,Pu)O2-gesinterte Pellets -
d'extraction par gaz inerte et méthode de mesure de la Trägergasheißextraktion und
conductivité (ISO 15651:2015) Leitfähigkeitsbestimmungsverfahren (ISO
15651:2015)
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 15651:2017 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
The text of ISO 15651:2015 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 15651:2017 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 15651:2015 has been approved by CEN as EN ISO 15651:2017 without any modification.

INTERNATIONAL ISO
STANDARD 15651
First edition
2015-02-15
Nuclear energy — Determination of
total hydrogen content in PuO and
UO powders and UO , (U,Gd)O and
2 2 2
(U,Pu)O sintered pellets — Inert gas
extraction and conductivity detection
method
Énergie nucléaire — Dosage de la teneur totale en hydrogène de
poudres de PuO et UO , et de pastilles frittées d’UO , (U,Gd)O et
2 2 2 2
(U,Pu)O — Méthode d’extraction par gaz inerte et méthode de
mesure de la conductivité
Reference number
ISO 15651:2015(E)
©
ISO 2015
ISO 15651:2015(E)
© ISO 2015
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
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ii © ISO 2015 – All rights reserved

ISO 15651:2015(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Interference . 1
5 Reagents and materials . 1
6 Apparatus . 2
7 Sampling . 2
7.1 Sampling procedure . 2
7.1.1 Powders . 2
7.1.2 Pellet . 3
7.2 Preparation . 3
7.2.1 Powder . . 3
7.2.2 Pellet . 3
8 Procedure. 3
8.1 Blank test . 3
8.2 Calibration . 3
8.2.1 Calibration of the analyser . 3
8.2.2 Check of the calibration . 3
8.3 Determination . 4
9 Calculation . 4
10 Precision . 4
11 Test report . 5
...