1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Nuclear 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)BS EN ISO 15651:2
2、017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15651 October 2017 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
3、15651:2015) nergie nuclaire - Dosage de la teneur totale en hydrogne de poudres de PuO2 et UO2, et de pastilles frittes dUO2, (U,Gd)O2 et (U,Pu)O2 - Mthode dextraction par gaz inerte et mthode de mesure de la conductivit (ISO 15651:2015) Kernenergie - Bestimmung des totalen Wasserstoffgehalts in PuO
4、2- und UO2-Pulvern und UO2-, (U,Gd)O2- und (U,Pu)O2-gesinterte Pellets - Trgergasheiextraktion und Leitfhigkeitsbestimmungsverfahren (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 stipu
5、late 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 S
6、tandard 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
7、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,
8、 Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form an
9、d by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15651:2017 ENational forewordThis British Standard is the UK implementation of EN ISO 15651:2017. It is identical to ISO 15651:2015. It supersedes BS ISO 15651:2015, which is withdrawn.The UK participation in its preparation
10、 was entrusted to Technical Committee NCE/9, Nuclear fuel cycle technology.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct
11、application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 96933 1ICS 27.120.30Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy
12、Committee on 28 February 2015.Amendments/corrigenda issued since publicationDate Text affected31 March 2018 This corrigendum renumbers BS ISO 15651:2015 as BS EN ISO 15651:2017BRITISH STANDARDBS EN ISO 15651:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15651 October 2017 ICS 27.120.3
13、0 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) nergie nuclaire - Dosage de la teneur totale en hydrogne de poudres de PuO2 et
14、UO2, et de pastilles frittes dUO2, (U,Gd)O2 et (U,Pu)O2 - Mthode dextraction par gaz inerte et mthode de mesure de la conductivit (ISO 15651:2015) Kernenergie - Bestimmung des totalen Wasserstoffgehalts in PuO2- und UO2-Pulvern und UO2-, (U,Gd)O2- und (U,Pu)O2-gesinterte Pellets - Trgergasheiextrakt
15、ion und Leitfhigkeitsbestimmungsverfahren (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 wit
16、hout 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
17、 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, D
18、enmark, 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. EUROPEA
19、N COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR 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 worldwide for CEN national Members. Ref. No. EN ISO 15651:2017 EBS
20、EN ISO 15651:2017EN ISO 15651:2017 (E) 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 1
21、5651:2017 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 lat
22、est 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.
23、 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, Ge
24、rmany, 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 I
25、SO 15651:2017 without any modification. BS EN ISO 15651:2017ISO 15651:2015(E)Contents PageForeword iv1 Scope . 12 Normative references 13 Principle 14 Interference . 15 Reagents and materials . 16 Apparatus . 27 Sampling 27.1 Sampling procedure . 27.1.1 Powders . 27.1.2 Pellet . 37.2 Preparation 37.
26、2.1 Powder 37.2.2 Pellet . 38 Procedure. 38.1 Blank test . 38.2 Calibration 38.2.1 Calibration of the analyser 38.2.2 Check of the calibration . 38.3 Determination . 49 Calculation 410 Precision . 411 Test report . 5 ISO 2015 All rights reserved iiiBS EN ISO 15651:2017ISO 15651:2015(E)ForewordISO (t
27、he 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 commit
28、tee 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 electrotech
29、nical 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
30、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.
31、 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
32、an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT), see the following URL: Foreword Supplementary information .The committe
33、e responsible for this document is ISO/TC 85, Nuclear Energy, Subcommittee SC 5, Fuel Technology.iv ISO 2015 All rights reservedBS EN ISO 15651:2017Nuclear energy Determination of total hydrogen content in PuO2and UO2powders and UO2, (U,Gd)O2and (U,Pu)O2sintered pellets Inert gas extraction and cond
34、uctivity detection method1 ScopeThis International Standard describes a procedure for measuring the total hydrogen content of UO2and PuO2powders (up to 2 000 g/g oxide) and of UO2and (U,Gd)O2and (U,Pu)O2pellets (up to 10 g/g oxide). The total hydrogen content results from adsorbed water, water of cr
35、ystallization, hydrocarbon, and other hydrogenated compounds which can exist as impurities in the fuel.2 Normative referencesThe 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 cit
36、ed applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO/IEC Guide 98-3:2008, Uncertainty of measurement Part 3: Guide to the expression of uncertainty in measurement (GUM: 1995)3 PrincipleThe total hydrogen content is determined using
37、a hydrogen analyser. The hydrogen analyser is based on the carrier gas method using argon or nitrogen as carrier gas. The samples to be analysed are heated up to a temperature of more than 1 770 C in a graphite crucible. At that temperature, all volatile components are removed. The hydrogen containi
38、ng compounds are cracked and released as hydrogen, oxygen, nitrogen, and carbon monoxide. The released gas is purified in the carrier gas stream, for example by oxidation and adsorption columns. The hydrogen is separated by chromatographic means and analysed in a thermal conductivity cell.4 Interfer
39、enceThe temperature of 1 770 C should be reached in a short time, within approximately 5 s; if not, the decomposition of the released water to hydrogen and oxygen might not be complete.At temperatures of more than 2 200 C, carbon dioxide is released because of a reduction of UO2by graphite according
40、 to the reaction below; carbon dioxide will interfere with the thermal conductivity measurement.UO2+ C UO2-x+ x/2 CO25 Reagents and materialsUse reagents of recognized analytical grade. The reagents and materials below serve as examples to be used according to manufacturer recommendation.5.1 Carrier
41、 gas. Use argon with a purity of a volume fraction 99,995 % or nitrogen with a purity of a volume fraction 99,998 %.INTERNATIONAL STANDARD ISO 15651:2015(E) ISO 2015 All rights reserved 1BS EN ISO 15651:2017ISO 15651:2015(E)5.2 Calibration gas. If calibration is performed with gas, use Argon or nitr
42、ogen with certified hydrogen content or carrier gas mixed with a known amount of hydrogen with a purity of a volume fraction 99,999 %.5.3 Reference material.1)If calibration or calibration check is performed with a standard material, use a reference material with certified hydrogen content (e.g. tit
43、anium or zirconium).5.4 Copper(II) oxide, CuO purifies the carrier gas (Ar/N2), converting H2to H2O.5.5 Absorption media for H2O. After converting H2to H2O (5.4), anhydrone Mg(ClO4)2 is used to trap H2O.5.6 Oxidation reagent for CO, Schutze reagent (iodine pentoxide over silica gel) preceded by Hopc
44、alite manganese oxide/copper(II) oxide oxidizes CO to CO2present in the carrier gas or extracted during measurement.5.7 Absorption media for CO2,sodium hydroxide over clay or equivalent will then absorb the CO2.5.8 Flux reagents for reference material. Tin, copper, or nickel granules are used as flu
45、x to accelerate the melting of reference material.6 Apparatus6.1 Hydrogen analyser. It will consist in a furnace capable to reach temperature of at least 2 200 C, a thermal conductivity cell and gas purifying systems.6.2 High purity graphite crucible, suitable for the appropriate sample types.The im
46、purity content should not exceed 2 g/g.6.3 Hydrogen free tin, copper, or nickel capsules.6.4 Balance, with precision of 1 mg.7 Sampling7.1 Sampling procedure7.1.1 PowdersSampling is done with a tube shaped powder sampler having an inner diameter of more than 2,5 times of the maximum powder particle
47、size. The sample shall be exposed to ambient conditions for not longer than 5 min because alterations of the powder sample due to moisture adsorption or desorption or oxidation have to be avoided. The sample has to be stored in tight containers. The gas volume in the container should be as low as po
48、ssible. In case the analysis is not performed immediately after the sampling, the sample mass has to be controlled before and after storage period prior to the analysis. These precautions can be relaxed if the analysis process is made under controlled gas environment (glove box environment).1) Refer
49、ence materials are available for example from “National Institute of Standard and Technology (NIST)” or “LECO Corporation”. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of these products.2 ISO 2015 All rights reservedBS EN ISO 15651:2017ISO 15651:2015(E)7.1.2 PelletWhen sampling the fuel pellets, ensure that pellets are not contaminated with H2; use metal forceps or pincers for sampling pellets. The sample should be representative for the m
