1、BSI Standards PublicationBS ISO 13165-3:2016Water quality Radium-226Part 3: Test method using coprecipitationand gamma-spectrometryBS ISO 13165-3:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 13165-3:2016.The UK participation in its preparation was entru
2、sted 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 correctapplicat
3、ion. The British Standards Institution 2016. Published by BSI StandardsLimited 2016ISBN 978 0 580 77411 9ICS 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 Co
4、mmittee on 31 March 2016.Amendments issued since publicationDate Text affectedBS ISO 13165-3:2016 ISO 2016Water quality Radium-226 Part 3: Test method using coprecipitation and gamma-spectrometryQualit de leau Radium 226 Partie 3: Mthode dessai par coprcipitation et spectromtrie gammaINTERNATIONAL S
5、TANDARDISO13165-3First edition2016-03-01Reference numberISO 13165-3:2016(E)BS ISO 13165-3:2016ISO 13165-3:2016(E)ii ISO 2016 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduce
6、d 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 the requester.ISO
7、 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 13165-3:2016ISO 13165-3:2016(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols 25 Principle of th
8、e measurement 36 Reagents and equipment . 36.1 Reagents 36.2 Equipment . 47 Sampling 47.1 Sample collection 47.2 Sample transport and storage 48 Procedures 48.1 Blank sample preparation . 48.2 Sample preparation 58.3 Counting procedure 59 Quality assurance and quality control programme . 59.1 Genera
9、l . 59.2 Influence quantities 69.3 Instrument verification 69.4 Method verification . 69.5 Demonstration of analyst capability 610 Expression of results 610.1 General . 610.2 Water-soluble 226Ra activity concentration 710.3 Standard uncertainty of activity concentration 710.4 Decision threshold . 71
10、0.5 Detection limit . 710.6 Limits of the confidence interval . 810.7 Corrections for contributions from other radionuclides and background . 810.7.1 General 810.7.2 Contribution from other radionuclides 910.7.3 Contribution from background 1011 Expression of results .10Annex A (informative) Uranium
11、 and its decay chain .12Bibliography .14 ISO 2016 All rights reserved iiiContents PageBS ISO 13165-3:2016ISO 13165-3:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International
12、 Standards is normally carried out through ISO technical committees. Each member 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, a
13、lso take part in the work. ISO collaborates closely with the International Electrotechnical 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.
14、 In particular the different approval criteria needed for the different types 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 eleme
15、nts of this document may be the subject of patent rights. ISO shall not be held 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
16、 (see www.iso.org/patents).Any trade name used in this document is information 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 adheren
17、ce to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 3, Radioactivity measurements.ISO 13165 consists of the following parts, under the ge
18、neral title Water quality Radium-226: Part 1: Test method using liquid scintillation counting Part 2: Test method using emanometry Part 3: Test method using coprecipitation and gamma-spectrometryiv ISO 2016 All rights reservedBS ISO 13165-3:2016ISO 13165-3:2016(E)IntroductionRadioactivity from sever
19、al naturally occurring and human-made sources is present throughout the environment. Thus, water bodies (surface waters, ground waters, sea waters) can contain radionuclides of natural and human-made origins:Natural radionuclides, including potassium-40, and those of the thorium and uranium decay se
20、ries, in particular 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 releases from technological processes involving naturally occurring radioactive materials (e.g. the mining and p
21、rocessing of mineral sands or phosphate fertilizer production and use).Human-made radionuclides such as transuranium elements (americium, plutonium, neptunium, curium), tritium, carbon-14, strontium-90, and gamma emitters radionuclides can also be found in natural waters as they can be authorized to
22、 be routinely released into the environment in small quantities in the effluent discharge from nuclear fuel cycle facilities and following their use in unsealed form in medicine or industry. They are also found in the water due to the past fallout of the explosion in the atmosphere of nuclear device
23、s and those following the Chernobyl and Fukushima accident.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
24、 releases into the environment in small quantities in 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 water as a result of past fallout con
25、tamination resulting from the explosion in the atmosphere of nuclear devices and accidents such as those that occurred in Chernobyl and Fukushima.Drinking water can thus contain radionuclides at activity concentration which could present a risk to human health. In order to assess the quality of drin
26、king 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, etc.) and drinking water are monitore
27、d for their radioactivity content as recommended by the World Health Organization (WHO) and can be required by some national authorities.The need of a standard on a test method of radium-226 activity concentrations in water samples is justified for test laboratories carrying out these measurements,
28、required sometimes by national authorities, as they may have to obtain a specific accreditation for radionuclide measurement in drinking water samples.Radium-226 activity concentration can vary widely according to local geological and climatic characteristics and ranges from 0,001 Bql1in surface wat
29、ers up to 50 Bql1in natural groundwaters; the guidance level for radium 226 in drinking water as recommended by WHO is 1 Bql1(see Reference 13).NOTE The guidance level is the activity concentration (rounded to the nearest order of magnitude) with an intake of 2 ld1of drinking water for 1 year that r
30、esults in an effective dose of 0,1 mSvy1for 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.This International Standard is one of a series on determination of the activity concentration of rad
31、ionuclides in water samples. ISO 2016 All rights reserved vBS ISO 13165-3:2016BS ISO 13165-3:2016Water quality Radium-226 Part 3: Test method using coprecipitation and gamma-spectrometryWARNING Persons using this part of ISO 13165 should be familiar with normal laboratory practice. This part of ISO
32、13165 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 compliance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests co
33、nducted in accordance with this part of ISO 13165 be carried out by suitably qualified staff.1 ScopeThis part of ISO 13165 specifies the determination of radium-226 (226Ra) activity concentration in all types of water by coprecipitation followed by gamma-spectrometry (see ISO 18589-3).The method des
34、cribed is suitable for determination of soluble 226Ra activity concentrations greater than 0,02 Bq l1using a sample volume of 1 l to 100 l of any water type.For water samples smaller than a volume of 1 l, direct gamma-spectrometry can be performed following ISO 10703 with a higher detection limit.NO
35、TE This test method also allows other isotopes of radium, 223Ra, 224Ra, and 228Ra, to be determined.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
36、applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 5667-3, Water quality Sampling Part 3: Preservation and handling of water samplesISO 10703, Water quality Determination of the activity concentration of radionuclides Method by high
37、resolution gamma-ray spectrometryISO 11929, Determination of the characteristic limits (decision threshold, detection limit and limits of the confidence interval) for measurements of ionizing radiation Fundamentals and applicationISO/IEC 17025, General requirements for the competence of testing and
38、calibration laboratoriesISO 80000-10, Quantities and units Part 10: Atomic and nuclear physics3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 80000-10 and the following apply.INTERNATIONAL STANDARD ISO 13165-3:2016(E) ISO 2016 All rights reserved 1BS
39、ISO 13165-3:2016ISO 13165-3:2016(E)3.1activitynumber of spontaneous nuclear disintegrations occurring in a given quantity of material during a suitably small interval of time divided by that interval of timeSOURCE: ISO 921:1997, 233.2reference standardstandard, generally having the highest metrologi
40、cal quality available at a given location or in a given organisation, from which measurements made there are derived3.3working standardstandard which, usually calibrated against a reference standard (3.2), is used routinely to calibrate or check material measures, measuring instruments or reference
41、materials. It can be used as a solution of known activity (3.1) concentration obtained by precise dilution or dissolution of a reference standard4 SymbolsFor the purposes of this part of ISO 13165, the symbols defined in ISO 11929 and ISO 80000-10, and the following apply.Table 1 List of symbolsV Vo
42、lume of the test sample in litresA Activity of each radionuclide in calibration source, at the calibration time, in becquerelsccAAc,Activity concentration of 226Ra, without and with corrections, expressed in becquerels per litreMsulfateMass of barium sulfate, in gramsMnitrateMass of barium nitrate,
43、in gramsMcarbonateMass of barium carbonate, in gramstgSample spectrum counting time, in secondst0Background spectrum counting time, in secondstsCalibration spectrum counting time, in secondsnn nNN Ns,0Number of counts in the net area of the peak considered, at energy E, in the sample, background and
44、 calibration spectra, respectivelynn ngg gs,0Number of counts in the gross area of the peak considered, at energy E, in the sample, back-ground and calibration spectra, respectivelynn nbb bs,0Number of counts in the background of the peak considered, at energy E, in the sample, back-ground and calib
45、ration spectra, respectivelyEfficiency of the detector at energy E, at actual measurement geometryRCChemical yieldPProbability of the emission of a gamma ray with energy, E, of each radionuclide, per decay, i.e. the branching ratio or the number of -quanta per decayu(cA) Standard uncertainty of acti
46、vity concentration, in becquerels per litreu(x) Standard uncertainty of measurand xurel(x) Relative uncertainty: u(x)xU Expanded uncertainty calculated by U = k u(cA) with k usually equals 2, in becquerels per litrecA*Decision threshold, in becquerels per litre2 ISO 2016 All rights reservedBS ISO 13
47、165-3:2016ISO 13165-3:2016(E)cA#Detection limit, in becquerels per litreCAtriangleright, CAtriangleleftLower and upper confidence limits, of each radionuclide, in becquerels per litre5 Principle of the measurementMeasurement of 226Ra activity concentration in water is carried out in two separate ste
48、ps: a sample preparation step, followed by a measurement by gamma-spectrometry.131415The sample preparation consists of a filtration of the water sample (see ISO 5667-3) to ensure the measurement of the activity concentration of the 226Ra soluble fraction. The filtration is followed by a pre-concent
49、ration, coprecipitation, and accumulation of decay products of 226Ra.After filtration and acidification of the water sample, the 226Ra is coprecipitated into sulfate using a carrier such as barium nitrate or carbonate. The radium and barium sulfates are then washed, dried, and weighed. The chemical yield is obtained gravimetrically.For water samples that may have an existing concentration of soluble barium, another tracer should be used to avoid a chemical yield above 100 %.When a radiometric tracer
