1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 26062:2010Nuclear technology Nuclearfuels Procedures for themeasurement of elementalimpurities in uranium- andplutonium-based materials byinductively coupled plasmamass sp
2、ectrometryBS ISO 26062:2010 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 26062:2010.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 beo
3、btained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 55786 6ICS 27.120.30Compliance with a British Standard cannot confer immunity fromlegal obligations.Thi
4、s British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 October 2010.Amendments issued since publicationDate Text affectedBS ISO 26062:2010Reference numberISO 26062:2010(E)ISO 2010INTERNATIONAL STANDARD ISO26062First edition2010-09-15Nuclear technolog
5、y Nuclear fuels Procedures for the measurement of elemental impurities in uranium- and plutonium-based materials by inductively coupled plasma mass spectrometry Technologie nuclaire Combustibles nuclaires Modes opratoires pour le mesurage des impurets lmentaires des matriaux base duranium et de plut
6、onium par spectromtrie de masse avec plasma couplage inductif BS ISO 26062:2010ISO 26062:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded
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9、relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2010 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including
10、 photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published i
11、n Switzerland ii ISO 2010 All rights reservedBS ISO 26062:2010ISO 26062:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Principle1 4 Reagents and materials 2 4.1 Water.2 4.2 Acids and other reagents .2 4.3 Standards .3 4.4 Matrix ma
12、terial .3 4.5 Calibration standards for instrumental analysis3 4.6 Quality control standards for instrumental analysis .3 4.7 Quality control standards for the method control .3 4.8 Recovery control standard.3 4.9 Internal standard .4 5 Apparatus.4 5.1 Mass spectrometer4 5.2 Radioactivity containmen
13、t4 5.3 Dissolution containers and process apparatus .5 6 Procedure.5 6.1 Interferences 5 6.2 Test portion7 6.3 Preparation of test portion .7 6.4 Instrumental analysis8 6.5 Instrument and method calibration .9 7 Calculation .11 8 Precision.11 9 Quality assurance and control.11 9.1 Instrument perform
14、ance .11 9.2 Method performance .12 10 Test report12 Annex A (informative) Table of elements measurable by ICP-MS .13 Annex B (informative) Specific examples of dissolution and extraction procedures .15 Annex C (informative) General information19 Bibliography21 BS ISO 26062:2010ISO 26062:2010(E) iv
15、ISO 2010 All rights reservedForeword 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 intereste
16、d 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 Com
17、mission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the techni
18、cal 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 sh
19、all not be held responsible for identifying any or all such patent rights. ISO 26062 was prepared by Technical Committee ISO/TC 85, Nuclear energy, Subcommittee SC 5, Nuclear fuel cycle. BS ISO 26062:2010ISO 26062:2010(E) ISO 2010 All rights reserved vIntroduction The technique presented in this Int
20、ernational Standard is capable of being used to perform quantitative measurements of elements with the specific exceptions of H, He, C, N, O, F, Cl, Br, and the noble gases. The measurement of other elements such as Si, P, S, K and I will require specialized sample introduction options, specialized
21、solutions, mass analysers or in-line systems for the measurement. This International Standard is presented in general terms for actinide samples because of the complexity and variation of the ICP-MS technique and its sample introduction accessories. Sufficient and appropriate method development shou
22、ld be undertaken to ensure that the procedure used for the determination of impurities in uranium and plutonium matrices is validated. It is assumed that the user of this International Standard has a basic understanding of standard sample control, chemical extraction techniques and operation of ICP-
23、MS instrumentation. Blank control is critical when undertaking ICP-MS analysis. Assessment of reagents and standards may be required when undertaking ultra trace analysis. BS ISO 26062:2010BS ISO 26062:2010INTERNATIONAL STANDARD ISO 26062:2010(E) ISO 2010 All rights reserved 1Nuclear technology Nucl
24、ear fuels Procedures for the measurement of elemental impurities in uranium- and plutonium-based materials by inductively coupled plasma mass spectrometry 1 Scope This International Standard specifies a procedure for the determination of trace impurities in uranium- or plutonium-based, or mixed uran
25、ium- and plutonium-based, materials by inductively coupled plasma mass spectrometry (ICP-MS). It provides both guidelines and specific options for the determination of an element or group of elements. It is applicable to solutions such as uranyl or plutonium nitrate, solids such as the oxides and to
26、 mixed actinide materials such as unirradiated mixed oxide material in either solid or dissolved forms. It is not directly suitable for the analysis of uranium or plutonium matrices containing significant quantities of other elements such as uraniumgadolinium mixtures. It may nevertheless form the b
27、asis of a process for analysing this type of matrix, provided that the impact of the gadolinium component is ascertained. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undate
28、d references, the latest edition of the referenced document (including any amendments) applies. ISO 3696, Water for analytical laboratory use Specification and test methods 3 Principle The method is based upon the dissolution of solid samples, the use of an optional chemical treatment to remove the
29、actinide matrix, followed by the spectroscopic determination of the analytes using inductively coupled plasma mass spectrometry (ICP-MS). In principle, the ICP-MS technique relies on the introduction of the sample in an aerosol form into the inductively coupled plasma. In the plasma, the sample atom
30、s are ionized then extracted from the plasma through a series of differential pumping chambers into the analyser region. The ionized species are mass separated using a mass analyser and then measured using an appropriate detection system. Quantitative measurements can be performed using a number of
31、techniques, including standard addition and isotope dilution analysis; however, the generation of calibration graphs from measured standards is the conventional technique. To provide an indication of the application of the technique, Table A.1 lists the elements commonly measured in uranium, plutoni
32、um and mixed actinide materials. The table includes the optimum isotope to be measured, the mass analyser options and comments regarding the measurement of that element. BS ISO 26062:2010ISO 26062:2010(E) 2 ISO 2010 All rights reservedThe process is presented in a series of stages, as given in the f
33、ollowing list. For each stage a series of criteria or principles that require consideration is presented. Annex B gives summaries of specific procedures for the dissolution and optional chemical extraction stages. a) Dissolution to dissolve solid samples: general details provided for hot plate and m
34、icrowave oven based dissolution; b) Optional chemical extraction procedure to remove the sample matrix: general details provided for solvent extraction process and chromatography process; c) Direct analysis of samples in the actinide matrix: general principles to be considered if using this option;
35、d) Analysis of the extracted sample: general principles of calibration, quality control and sample measurement are provided. No details are provided for the specific instrumental set up, owing to the significant range of options available from the variety of instruments currently available commercia
36、lly, for example, quadrupole mass analyser vs. magnetic sector mass analyser vs. time-of-flight mass analyser, conventional nebulisation sample introduction vs. specialised applications e.g. flow injection or ultra sonic nebuliser, the use of “collision/reaction cell” or “cool plasma” systems, quant
37、itative techniques. A brief description of the relative merits of these options is provided in Annex C. However, detailed information should be obtained from textbooks, journals or from manufacturers manuals. 4 Reagents and materials Use only reagents of recognized analytical grade, unless otherwise
38、 specified. 4.1 Water Normal industry practice is to use high purity water designated 18 Mcm, judged as being suitable for this guideline. Water complying with better than grade 2 as defined in ISO 3696:1987 is the recommended water quality. 4.2 Acids and other reagents High purity reagents shall be
39、 used for all ICP-MS analysis. The quality of the reagents used in the process shall be validated by undertaking suitable blank measurements before use. Procedural blanks should be used at the sample preparation, sample extraction (where applicable) and instrument measurement stages. 4.2.1 Nitric ac
40、id, 16 M 4.2.2 Hydrofluoric acid, 40 % BS ISO 26062:2010ISO 26062:2010(E) ISO 2010 All rights reserved 34.2.3 Nitric acid/hydrofluoric acid cleaning solution Fill a 2,5 l plastic bottle with approximately 2 l of the high purity water. Add 470 ml of 16 M nitric acid slowly to the water, swirl gently
41、to mix. Add 5 ml of hydrofluoric acid with a mass fraction of 40 %. Dilute the acid mixture to 2,5 l and mix. 4.3 Standards Suitable certified and reference standards traceable to a certifying authority shall be used for all quantitative analysis. Use standards from different suppliers for calibrati
42、on and quality control standards to monitor for preparation problems. 4.4 Matrix material The use of matrix-matched standards is required to ensure a high level of quality control. Ensure that a suitable material is used that does not affect the measurement. Undertake appropriate and sufficient meth
43、od development to validate the procedure. 4.5 Calibration standards for instrumental analysis The ICP-MS instrument shall be calibrated to allow quantitative analysis, for example external calibration, using the conventional technique described in 6.4. Suitable standards can be prepared from commerc
44、ially available elemental standards. Matrix matching the standards is required for direct analysis of analytes in strong actinide solution to correct for the impact of the sample matrix on signal intensities (i.e. signal suppression or possible enhancement). 4.6 Quality control standards for instrum
45、ental analysis A suitable quality control standard shall be measured to ensure that the calibration has been performed correctly. Prepare quality control standards by diluting commercially available elemental standards down to suitable concentrations for the application. Matrix matching the standard
46、s may be required for direct analysis of analytes in strong actinide solution. 4.7 Quality control standards for the method control A suitable quality control standard shall be processed alongside the samples to monitor the performance of the analytical method. Prepare a suitable quality control sta
47、ndard that contains the desired analytes at levels appropriate for the material being analysed. The quality control standard should be prepared in a suitable matrix to reflect the concentration of the matrix in the sample solution produced after the dissolution phase. Ideally, a certified reference
48、material should be used. In the absence of a suitable reference material, the alternative approach is to prepare a standard from an appropriate dilution of a commercial elemental standard in a matrix that matches the samples being analysed. 4.8 Recovery control standard Where a chemical extraction i
49、s used, the recovery through the process shall be monitored and, if necessary, appropriate correction of the analytical result should be made, ensuring that appropriate uncertainty associated with recovery correction is taken into account. Prepare a suitable standard that contains the desired analytes at levels appropriate for the material being analysed. The matrix of the standard should reflect the concentration of the matrix in the sample solution produced after the dissolution phase. Ideally, a certified refe
