1、BSI Standards PublicationBS ISO 13167:2015Water quality Plutonium,americium, curium andneptunium Test methodusing alpha spectrometryBS ISO 13167:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 13167:2015.The UK participation in its preparation was entruste
2、d to TechnicalCommittee EH/3/8, Radioactivity measurements methods.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication
3、. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 83928 3ICS 13.060.60; 17.240Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Commi
4、ttee on 31 December 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 13167:2015 ISO 2015Water quality Plutonium, americium, curium and neptunium Test method using alpha spectrometryQualit de leau Plutonium, americium, curium et neptunium Mthode dessai par spectro
5、mtrie alphaINTERNATIONAL STANDARDISO13167First edition2015-12-15Reference numberISO 13167:2015(E)BS ISO 13167:2015ISO 13167:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publicatio
6、n 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 ISOs member body in the country of
7、 the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 13167:2015ISO 13167:2015(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols 25 P
8、rinciple 26 Chemical reagents and equipment 36.1 Chemical reagents 36.2 Equipment . 37 Procedure. 47.1 Sampling . 47.2 Concentration step and valence cycle . 47.3 Chemical separation . 47.4 Preparation of the source to be measured 47.4.1 General 47.4.2 Electrodeposition method . 47.4.3 Co-precipitat
9、ion method . 47.5 Background determination 57.6 Counting efficiency determination 57.7 Measurement 58 Expression of results 58.1 Calculation of the activity concentration 58.2 Standard uncertainty . 68.3 Decision threshold . 68.4 Detection limit . 68.5 Confidence limits. 79 Quality assurance and qua
10、lity control programme . 79.1 General . 79.2 Influence quantities 79.3 Instrument verification and calibration 89.4 Method verification . 89.5 Demonstration of analyst capability 810 Test report . 8Annex A (informative) Chemical separation of actinides on anionic resin .10Annex B (informative) Chemi
11、cal separation of actinides by specific resins 13Annex C (informative) Preparation of the source by electrodeposition .16Annex D (informative) Preparation of the source by co-precipitation 19Bibliography .21 ISO 2015 All rights reserved iiiContents PageBS ISO 13167:2015ISO 13167:2015(E)ForewordISO (
12、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 commi
13、ttee 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 electrotec
14、hnical 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
15、 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
16、. 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
17、 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 informationThe committe
18、e responsible for this document is ISO/147, Water quality, Subcommittee SC 3, Radioactivity measurements.iv ISO 2015 All rights reservedBS ISO 13167:2015ISO 13167:2015(E)IntroductionRadioactivity from several naturally-occurring and anthropogenic sources is present throughout the environment. Thus,
19、water bodies (e.g. surface waters, ground waters, sea waters) can contain radionuclides of natural, human-made, or both origins. Natural radionuclides, including potassium 40, and those originating from the thorium and uranium decay series, in particular radium 226, radium 228, uranium 234, uranium
20、238, lead 210, can be found in water for natural reasons (e.g. desorption from the soil and wash-off by rain water) or can be released from technological processes involving naturally occurring radioactive materials (e.g. the mining and processing of mineral sands or phosphate fertilizer production
21、and use). Human-made radionuclides, such as transuranium elements (americium, plutonium, neptunium, curium), tritium, carbon 14, strontium 90 and some gamma emitting radionuclides, can also be found in natural waters as a result of authorized routine releases into the environment in small quantities
22、 in the effluent discharged from nuclear fuel cycle facilities. They are also released into the environment following their used in unsealed form for medical and industrial applications. They are also found in the water as a result of past fallout contamination resulting from the explosion in the at
23、mosphere of nuclear devices and accidents such as those that occurred in Chernobyl and Fukushima.Drinking water may thus contain radionuclides at activity concentrations which could present a risk to human health. In order to assess the quality of drinking water (including mineral waters and spring
24、waters) with respect to its radionuclide content and to provide guidance on reducing health risks by taking measures to decrease radionuclide activity concentrations, water resources (groundwater, river, lake, sea, etc.) and drinking water are monitored for their radioactivity content as recommended
25、 by the World Health Organization WHO and as may be required by some national authorities.An international standard on a test method for isotopes of plutonium, americium, curium and neptunium activity concentrations in water samples is justified for test laboratories carrying out these measurements,
26、 which are sometimes required by national authorities, as laboratories may have to obtain a specific accreditation for radionuclide measurement in drinking water samples.238Pu, 239Pu, 240Pu, 241Am, 242Cm, 243Cm, 244Cm, 237Np activity concentrations can vary according to any local effluent authorized
27、 discharges from nuclear plant and environmental characteristics. The guidance level for 238Pu, 239Pu, 240Pu, 241Am, 242Cm, 243Cm, 244Cm, 237Np in drinking water as recommended by WHO is 1 Bq/l for all of those isotopes, except for 242Cm (10 Bq/l) WHO-Guidelines for drinking waters quality, 2011, Ge
28、neva.NOTE The guidance level is the activity concentration (rounded to the nearest order of magnitude) with an intake of 2 l/day of drinking water for 1 year, that results in an effective dose of 0,1 mSv/year for members of the public, an effective dose that represents a very low level of risk that
29、is not expected to give rise to any detectable adverse health effect.This International Standard is one of a set of International Standards on test methods dealing with the measurement of the activity concentration of radionuclides in water samples. ISO 2015 All rights reserved vBS ISO 13167:2015BS
30、ISO 13167:2015Water quality Plutonium, americium, curium and neptunium Test method using alpha spectrometry1 ScopeThis International Standard specifies a test method for measuring actinides (238Pu, 239+240Pu, 241Am, 242Cm, 243+244Cm and 237Np) in water samples by alpha spectrometry following a chemi
31、cal separation.The method can be used for any type of environmental study or monitoring.The volume of the test portion required depends on the assumed activity of the sample and the desired detection limit.The detection limit of the test method is 5 103to 5 104Bq/l for a volume of the test portion o
32、f 0,1 l to 5 l with a counting time of two to ten days.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 cited applies. For undated references, the latest e
33、dition of the referenced document (including any amendments) applies.ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes and sampling techniquesISO 5667-3, Water quality Sampling Part 3: Preservation and handling of water samplesISO 11929, Determination of the ch
34、aracteristic limits (decision threshold, detection limit and limits of the confidence interval) for measurements of ionizing radiation Fundamentals and applicationISO 80000-10, Quantities and units Part 10: Atomic and nuclear physicsISO/IEC 17025, General requirements for the competence of testing a
35、nd calibration laboratories3 Terms and definitionsFor the purposes of this document, the terms, definitions and symbols given in ISO 80000-10 and ISO 11929 apply. INTERNATIONAL STANDARD ISO 13167:2015(E) ISO 2015 All rights reserved 1BS ISO 13167:2015ISO 13167:2015(E)4 SymbolsThe following symbols a
36、pply.A Activity of tracer added at the date of measurement, in becquerelscAActivity concentration of the actinides isotopes in becquerels per litrecA* Decision threshold, in becquerels per litrecA# Detection limit, in becquerels per litreccAAtrianglerighttriangleleft,Lower and upper limits of the co
37、nfidence interval, in becquerels per litre Counting efficiencyrg, rgTGross count rate per second from measured actinides isotopes and tracer, respec-tivelyrr00,TBackground count rate per second from actinides isotopes and tracer, respectivelyR Total measurement yieldRcChemical yieldt0Background coun
38、ting time, in secondstgSample counting time, in secondsuc()AStandard uncertainty associated with the measurement result, in becquerels per litreUExpanded uncertainty, calculated by Ukuc=()Awith k = 1, 2, in becquerels per litreV Volume of test sample, in litresf Correction factor for possible bias f
39、or curium isotopes using 243Am as a tracer or for 237Np using 236Pu as a tracer. For plutonium isotopes or for 241Am, f is equal to 1.5 PrincipleActinide isotopes are deposited as a thin source for measurement by alpha spectrometry using a grid chamber or semi-conductor detector type equipment. The
40、sources are usually prepared by electrodeposition or co-precipitation after chemical separation and purification of the actinide isotopes present in the test portion.1234Specific chemical separation and purification procedures are required in order to avoid interference from the presence of other em
41、itters, and stable nuclides in the sample, in quantities that are often larger than the actinide isotopes of interest.2 ISO 2015 All rights reservedBS ISO 13167:2015ISO 13167:2015(E)These procedures allow the main sources of interference to be removed: the salt content of the water sample, especiall
42、y hydrolysable elements, in order to prepare the thinnest deposited source; other emitting radionuclides, such as uranium and thorium isotopes, whose emissions may interfere with those of actinide isotopes of interest.The total yield for each analysis (product of chemical separation yield and detect
43、ion efficiency) is determined by adding a standard solution of tracer: 236Pu can be used for plutonium isotopes and 237Np, 242Pu can be used for plutonium isotopes only and 243Am can be used for americium and curium isotopes.As a result, the procedure shall include a reduction/oxidation cycle to adj
44、ust the tracer and the analytes to the same oxidation state.It is possible to quantify curium isotopes on the basis of 243Am tracer behaviour. This may lead to a potential bias that shall be quantified using a standard solution and/or participation in inter-laboratory comparison tests.It is possible
45、 to quantify neptunium on the basis of 236Pu tracer behaviour. This may lead to a potential bias that shall be quantified using a standard solution and/or participation in inter-laboratory comparison.NOTE 235Np, 236Np, 238Np and 239Np can be used as a yield tracers for 237Np (if available), and 245C
46、m as a yield tracer for other Cm isotopes but the test method of this International Standard does not cover these measurements.6 Chemical reagents and equipment6.1 Chemical reagentsThe chemical reagents and equipment are described in Annexes A and B for chemical separation and in Annexes C and D for
47、 the preparation of the deposited source.Except for the certified standard solutions, all the chemical reagents needed to carry out this procedure shall be analytical grade.6.2 EquipmentUsual laboratory apparatus and in particular the following equipment.6.2.1 Alpha-spectrometer, of the grid chamber
48、 (with higher detection efficiency, but lower resolution) or semiconductor type (with lower detection efficiency, but higher resolution). Operation at constant temperature is recommended. Follow the manufacturers instructions.For semiconductor-type equipment, the measurements using alpha-spectrometr
49、y depend on the interaction of alpha-particles with an ion-implanted silicon detector. This interaction instantly changes the conductivity of the silicon, proportional to the energy of the incoming alpha-particle. If a well-resolved spectra is required, the detection system should be maintained at a pressure 10 Pa. Resolution can be further enhanced through increasing distance between source and detector.6.2.2 Pipette, suitable for the accurate transfer of (for example 100 l) tracer solution with a to
