BS 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 conductivit.pdf

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1、BSI Standards PublicationBS ISO 15651:2015Nuclear energy Determination of total hydrogen content in PuO2and UO2powders and UO2, (U,Gd)O2and (U,Pu)O2sintered pellets Inert gas extraction and conductivity detection methodBS ISO 15651:2015 BRITISH STANDARDNational forewordThis British Standard is the U

2、K implementation of ISO 15651:2015.The UK participation in its preparation was entrusted to TechnicalCommittee 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 n

3、ecessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 75462 3 ICS 27.120.30 Compliance with a British Standard cannot confer immunity from legal obligations.This British Stand

4、ard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e d ISO 2015Nuclear energy Determination of total hydrogen content in PuO2and UO2powders and UO2, (U,Gd)O2and (U,Pu)O2sinter

5、ed pellets Inert gas extraction and conductivity detection methodnergie nuclaire Dosage de la teneur totale en hydrogne de poudres de PuO2et UO2, et de pastilles frittes dUO2, (U,Gd)O2et (U,Pu)O2 Mthode dextraction par gaz inerte et mthode de mesure de la conductivitINTERNATIONAL STANDARDISO 15651Fi

6、rst edition 2015-02-15Reference number ISO 15651:2015(E)BS ISO 15651:2015ISO 15651:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any mea

7、ns, 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 ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 2

8、0Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 15651:2015ISO 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 pr

9、ocedure . 27.1.1 Powders . 27.1.2 Pellet . 37.2 Preparation 37.2.1 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

10、reserved iiiBS ISO 15651:2015ISO 15651:2015(E)ForewordISO (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 memb

11、er 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 Ele

12、ctrotechnical 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

13、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 hel

14、d 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

15、 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 ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT), see the fol

16、lowing URL: Foreword Supplementary information .The committee responsible for this document is ISO/TC 85, Nuclear Energy, Subcommittee SC 5, Fuel Technology.iv ISO 2015 All rights reservedBS ISO 15651:2015Nuclear energy Determination of total hydrogen content in PuO2and UO2powders and UO2, (U,Gd)O2a

17、nd (U,Pu)O2sintered pellets Inert gas extraction and conductivity 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

18、hydrogen content results from adsorbed water, water of crystallization, 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 it

19、s application. For dated references, only the edition cited 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

20、 PrincipleThe total hydrogen content is determined using 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, a

21、ll volatile components are removed. The hydrogen containing 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 mea

22、ns and analysed in a thermal conductivity cell.4 InterferenceThe 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 re

23、leased because of a reduction of UO2by graphite according 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

24、used according to manufacturer recommendation.5.1 Carrier 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 ISO 15651:2015ISO 15651:2015(E)5.2 Calibration gas. I

25、f calibration is performed with gas, use Argon or nitrogen 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 refere

26、nce material with certified hydrogen content (e.g. titanium 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 reage

27、nt (iodine pentoxide over silica gel) preceded by Hopcalite 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 mat

28、erial. Tin, copper, or nickel granules are used as flux 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 cruc

29、ible, suitable for the appropriate sample types.The impurity 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

30、of more than 2,5 times of the maximum powder particle 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.

31、The gas volume in the container should be as low as possible. 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 contr

32、olled gas environment (glove box environment).1) Reference 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 t

33、hese products.2 ISO 2015 All rights reservedBS ISO 15651:2015ISO 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 manufacturing process (e.g. stora

34、ge of the pellets).7.2 Preparation7.2.1 PowderPowder samples can be filled into capsules (6.3) which are subsequently closed. Alternatively, the powder samples can be inserted as pressed bodies (“green pellets” prepared without additives).NOTE A compromise solution between precision and sustainable

35、development (wastes recycling) is to delete the use of capsules.7.2.2 PelletSintered fuel pellets can be analysed without any preparation step. If the pellets are dried before the rod filling in the rod fabrication process, the sample should be dried before analysis to be representative of manufactu

36、ring conditions.8 Procedure8.1 Blank testThe analyser is checked by performing blank measurements proving the integrity of the purifying units and the tightness of the equipment. Blank values exceeding the analyser detection limit require adequate measures of correction.8.2 Calibration8.2.1 Calibrat

37、ion of the analyserHydrogen analyser shall be calibrated before sample measurement. There are two possibilities of calibration: calibration with gas; calibration with certified standards.The calibration will depend on the type of analyser, it can be performed by the analyser manufacturer and/or the

38、final user. The calibration range and the number of standards will depend on the equipment, the final use, and the range of available standards.In case of calibration with gas, a well-defined volume of the calibration gas (5.2), which is corrected on standard conditions, is inserted and analysed. Th

39、is calibration is performed three times.In the case of calibration with certified standards, they are weighed to the nearest 1 mg accuracy.8.2.2 Check of the calibrationTo check the calibration of the equipment, reference material (5.3) is weighed to the nearest 1 mg accuracy flux reagents (5.8) can

40、 be used to help for fusion. The released hydrogen is determined. The measured values can differ from the certified values by not more than the total uncertainty of the analysis process. If not, the calibration is repeated. ISO 2015 All rights reserved 3BS ISO 15651:2015ISO 15651:2015(E)8.3 Determin

41、ationWeigh the sample to the nearest 1 mg.The empty graphite crucible is purified in a carrier gas stream during at least 30 s by heating at a temperature above the analysis temperature.Insert sample (sintered pellet, green pellet, encapsulated powder) into the analyser.Purge with carrier gas during

42、 at least 30 s.The sample is dropped into the crucible and heated up to at least 1 770 C.The hydrogen content is measured, during at least 60 s to extract H2from all the hydrogenated compounds.9 CalculationCalculate the hydrogen mass fractions (g/g sample) using Formula (1):wmmHH22= (1)wherewH2is th

43、e hydrogen mass fractions, in g/g sample;mH2is the mass of the hydrogen in g, corrected of the blank;m is the mass of the sample, in g.If a result expressed as g hydrogen per g U, g hydrogen per g(U+Pu), or g hydrogen per g(U+Gd) is required, the results are converted as follows:wggMHgoxideMcontent

44、of sampleHM2100= /(/)%(2)wherewHM2is the hydrogen mass fractions, in g /gM;M is U or (U+Pu) or (U+Gd).10 PrecisionThe repeatability standard deviation, Sr, of the hydrogen detection system can reach sr= 0,18ppm RSD = 15 % relative in the following conditions: 10 measurements of a reference material;

45、 same calibration with H2-gas during the 10 measurements; and reference material of about 10 g with 1,2 g/g of H2;The total uncertainty, taking into account the accuracy of the reference material and the precision error of the calibration (mainly influenced by the kinetics of moisture release and of

46、 H2O-reduction on the 4 ISO 2015 All rights reservedBS ISO 15651:2015ISO 15651:2015(E)hot graphite crucible), can reach 35 % relative or more if the measurement result is very close to the detection limit.11 Test reportThe test report shall include the following information:a) identification of samp

47、le;b) the method used by reference to this International Standard, (i.e. ISO 15651);c) the results and the form in which they are expressed;d) the detection limit;e) any deviations from the procedure;f) any unusual features observed;g) the location and date of the test. ISO 2015 All rights reserved

48、5BS ISO 15651:2015ISO 15651:2015(E) ISO 2015 All rights reservedICS 27.120.30Price based on 5 pagesThis page deliberately left blankBSI is the national body responsible for preparing British Standards and other standards-related publications, information and services.BSI is incorporated by Royal Cha

49、rter. British Standards and other standardization products are published by BSI Standards Limited.British Standards Institution (BSI)BSI Group Headquarters389 Chiswick High Road London W4 4AL UKAbout usWe bring together business, industry, government, consumers, innovators and others to shape their combined experience and expertise into standards -based solutions.The knowledge embodied in our standards has been carefully assembled in a dependable format and refined through our open c