1、BSI Standards PublicationBS ISO 13163:2013Water quality Lead-210 Test method using liquidscintillation countingBS ISO 13163:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 13163:2013.The UK participation in its preparation was entrusted to TechnicalCommitt
2、ee EH/3/8, Radioactivity measurements.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. The British Standards Insti
3、tution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 72183 0ICS 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 Committee on 31 October 2013.Amend
4、ments issued since publicationDate Text affectedBS ISO 13163:2013 ISO 2013Water quality Lead-210 Test method using liquid scintillation countingQualit de leau Plomb 210 Mthode dessai par comptage des scintillations en milieu liquideINTERNATIONAL STANDARDISO13163First edition2013-10-15Reference numbe
5、rISO 13163:2013(E)BS ISO 13163:2013ISO 13163:2013(E)ii ISO 2013 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2013All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, includin
6、g 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 20Tel. + 41 22 749 01 11Fax + 41 22 749
7、 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 13163:2013ISO 13163:2013(E) ISO 2013 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Symbols 24 Principle 35 Reagents and equipment . 46 Sampling and storage 56.1 Sampling . 5
8、6.2 Sample storage 57 Procedure. 57.1 Sample preparation 67.2 Preconcentration . 67.3 Separation of 210Pb . 77.4 Measurement 88 Quality assurance and quality control programme . 98.1 General . 98.2 Influencing variables . 98.3 Instrument verification. 108.4 Contamination 108.5 Method verification 10
9、8.6 Demonstration of analyst capability . 109 Expression of results .109.1 General 109.2 Yield determination . 119.3 Calculation of activity concentration 129.4 Decision threshold 139.5 Detection limit 139.6 Confidence interval limits. 1310 Test report 14Annex A (informative) Spectra examples 15Bibl
10、iography .17BS ISO 13163:2013ISO 13163:2013(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. www.iso.org/directivesAttention 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 resp
14、onsible 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. www.iso.org/patentsAny trade name used in this document is information given for t
15、he convenience of users and does not constitute an endorsement.The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 3, Radioactivity measurements.iv ISO 2013 All rights reservedBS ISO 13163:2013ISO 13163:2013(E)IntroductionRadioactivity from several naturally occ
16、urring and anthropogenic sources is present throughout the environment. Thus, water bodies (e.g. surface water, groundwater, seawater) can contain the following radionuclides of natural or human-made origins: natural radionuclides, including potassium-40, and those originating from the thorium and u
17、ranium decay series, particularly radium-226, radium-228, uranium-234, uranium-238, and 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 (
18、e.g. the mining and processing of mineral sands or the production and use of phosphate fertilizer); human-made radionuclides, such as transuranium elements (americium, plutonium, neptunium, curium), tritium, carbon-14, strontium-90, and gamma-emitting radionuclides, can also be found in natural wate
19、rs as a result of authorized routine releases into the environment in small quantities of the effluent discharged from nuclear fuel cycle facilities. They are also released into the environment following their use in unsealed form for medical and industrial applications. They are also found in the w
20、ater as a result of past fallout contamination resulting from the explosion in the atmosphere 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. I
21、n order to assess the quality of drinking water (including mineral waters and spring 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,
22、etc.) and drinking water are monitored for their radioactivity content as recommended by the World Health Organization WHO and required by some national authorities.An International Standard on a test method for lead-210 activity concentrations in water samples is justified for test laboratories car
23、rying out these measurements, required sometimes by national authorities, as laboratories may have to obtain a specific accreditation for radionuclide measurement in drinking water samples.Lead-210 activity concentration can vary according to local geological and climatic characteristics and usually
24、 ranges from 2 mBql-1to 300 mBql-1(References 1213). The guidance level for lead-210 in drinking water, as recommended by WHO, is 100 mBql-1(Reference 14).NOTE The guidance level is the activity concentration with an intake of 2 lday-1of drinking water for 1 year that results in an effective dose of
25、 0,1 mSvyear-1for members of the public, an effective dose that represents a very low level of risk that is not expected to give rise to any detectable adverse health effect. ISO 2013 All rights reserved vBS ISO 13163:2013BS ISO 13163:2013Water quality Lead-210 Test method using liquid scintillation
26、 countingWARNING Persons using ISO 13163 should be familiar with normal laboratory practice. ISO 13163 does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure comp
27、liance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests conducted according to ISO 13163 be carried out by suitably trained staff.1 ScopeISO 13163 specifies the determination of lead-210 (210Pb) activity concentration in samples of all types of water using liqu
28、id scintillation counting (LSC). For raw and drinking water, the sample should be degassed in order to minimize the ingrowth of 210Pb from radon-222 (222Rn).Using currently available liquid scintillation counters, this test method can measure the 210Pb activity concentrations in the range of less th
29、an 20 mBql-1to 50 mBql-1. These values can be achieved with a counting time between 180 min and 720 min for a sample volume from 0,5 l to 1,5 l.Higher 210Pb activity concentrations can be measured by either diluting the sample or using smaller sample aliquots or both.It is the laboratorys responsibi
30、lity to ensure the suitability of this test method for the water samples tested.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
31、 references, the latest edition of the referenced document (including any amendments) applies.ISO/IEC Guide 98-3, Uncertainty of measurement Part 3: Guide to the expression of uncertainty in measurement (GUM:1995)ISO/IEC Guide 99, International vocabulary of metrology Basic and general concepts and
32、associated terms (VIM)ISO/IEC 17025, General requirements for the competence of testing and calibration laboratoriesISO 5667-3, Water quality Sampling Part 3: Preservation and handling of water samplesISO 11929, Determination of the characteristic limits (decision threshold, detection limit and limi
33、ts of the confidence interval) for measurements of ionizing radiation Fundamentals and applicationISO 80000-10, Quantities and units Part 10: Atomic and nuclear physicsINTERNATIONAL STANDARD ISO 13163:2013(E) ISO 2013 All rights reserved 1BS ISO 13163:2013ISO 13163:2013(E)3 SymbolsFor the purposes o
34、f this document, the symbols and designations given in ISO 80000-10, ISO 11929, ISO/IEC Guide 98-3, and ISO/IEC Guide 99 and the following apply.Ccoeffcoefficient of 210Bi ingrowth to equilibrium in the sample between the end of bismuth elu-tion and time of countingcAactivity concentration in the sa
35、mple, in becquerel per litrecA0activity concentration of the standard, in becquerel per litrecA*decision threshold, in becquerel per litrecA#detection limit, in becquerel per litreccAAtrianglerighttriangleleft,lower and upper limits of the confidence interval, in becquerel per litreRcchemical yieldr
36、bcount rate of the reagent blank, in reciprocal secondrgsample count rate, in reciprocal secondrscalibration count rate, in reciprocal secondr0background count rate, in reciprocal secondS1 eluted solution containing leadtgsample counting time, in secondtscalibration counting time, in secondt0backgro
37、und counting time, in secondU expanded uncertainty, calculated by U = ku(cA) with k = 1, 2, in becquerel per litreu(cA) standard uncertainty associated with the measurement result, in becquerel per litreV volume of the eluted phase, in litreVetotal volume of the test sample plus the carrier, in litr
38、eVsvolume of the standard test sample, in litreVsamplevolume of the sample, in litreV1volume of the aliquot from S1 for 210Pb counting, in litreV2volume of the aliquot from S1 for the determination of the chemical yield of lead, in litre detection efficiency related to 210Pb concentration of lead of
39、 the eluate, in milligram per litreeconcentration of lead in the sample after the addition of the carrier, in milligram per litre2 ISO 2013 All rights reservedBS ISO 13163:2013ISO 13163:2013(E)4 Principle210Pb is a natural beta-emitting radionuclide with a maximum beta-energy of 63,9 keV and a half-
40、life of 22,23 years (References 1516). It appears in the 238U decay series (4n+2) as a long-lived decay product of 222Rn (see Figure 1).210Pb is separated from its daughters, bismuth-210 and polonium-210, by extraction chromatography and its activity is measured by liquid scintillation counting, eit
41、her directly after its separation or indirectly after ingrowth of its progeny bismuth-210. Other separation methods exist (Reference 17).To avoid the possible interferences of the isotopes lead-211 and lead-214 and their progenies during the liquid scintillation counting, it is recommended to wait a
42、t least 3 h between elution of lead and the sample counting to allow these radionuclides to fully decay.For radioisotopes with longer half-lives such as lead-212 and its progenies, their interferences are avoided by choosing appropriate counting windows as their energies are much higher than the ene
43、rgy of 210Pb (see 7.4.2).For samples with high activity concentration, dilution of the sample is required to avoid resin and detector saturation during the separation and counting steps, respectively.Suspended material is removed prior to analysis by filtration using 0,45 m filters. The analysis of
44、the insoluble fraction requires a mineralization step that is not covered by ISO 13163.NOTE A suitable mineralization step is specified in ISO 18589-2.10Figure 1 Uranium-238 and its decay products (see ISO 13164-1)It is necessary to know the concentration of the stable lead in the sample in order to
45、 determine the mass of the lead carrier to add and to calculate the chemical yield for the separation of 210Pb.It is possible to confirm the radiopurity of the 210Pb fraction by monitoring 210Bi ingrowth activity up to equilibration via repeated counting over an appropriate period of time. ISO 2013
46、All rights reserved 3BS ISO 13163:2013ISO 13163:2013(E)5 Reagents and equipmentUse only reagents of recognized analytical grade.5.1 Reagents5.1.1 Nitric acid, HNO3, concentrated, i.e. 700 gl1.5.1.2 Hydrochloric acid, HCl, concentrated, i.e. 370 gl1.5.1.3 Hydrochloric acid solution, 2 moll1HCl.5.1.4
47、Nitric acid solution, 1 moll1HNO3.5.1.5 Nitric acid solution, 0,1 moll1HNO3.5.1.6 Solution of Fe(III), approximately 1 gl1in 0,1 moll1HNO3or 0,5 moll1HCl.5.1.7 Standard solution of Pb(II), approximately 1 gl1in 0,1 moll1HNO3or 2 moll1HCl.5.1.8 Ammonia, NH4OH, concentrated, e.g. 280 gl1.5.1.9 Ammoniu
48、m citrate or citric acid solution, 0,01 moll1to 0,1 moll1or EDTA solution, 0,01 moll1.5.1.10 Chromatographic extraction resin, e.g. a crown ether 18C6-type resin.5.1.11 Liquid scintillation cocktail, chosen according to the characteristics of the sample to be analysed and the properties of the detec
49、tion equipment. The characteristics of the scintillation cocktail shall allow the mixture to be homogeneous and stable.5.1.12 Laboratory water, distilled or deionized, complying with ISO 3696,1grade 3.Deionized water can contain detectable amounts of 222Rn and its short-lived daughters. It is therefore strongly recommended that water be boiled under vigorous stirring and allowed to stand for 1 day before use; otherwise, degassing with nitrogen for about 1 h per 2 l
