1、BSI Standards PublicationBS EN ISO 13161:2015Water quality Measurementof polonium 210 activityconcentration in water byalpha spectrometryBS EN ISO 13161:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO13161:2015. It is identical to ISO 13161:2011.The UK
2、participation in its preparation was entrusted 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. Use
3、rs are responsible for its correctapplication. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 89462 6ICS 13.060.60; 17.240Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the author
4、ity of theStandards Policy and Strategy Committee on 31 October 2015.Amendments/corrigenda issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13161 October 2015 ICS 13.060.60; 17.240 English Version Water quality - Measurement of polonium 210 activity
5、concentration in water by alpha spectrometry (ISO 13161:2011) Qualit de leau - Mesurage de lactivit du polonium 210 dans leau par spectromtrie alpha (ISO 13161:2011) Wasserbeschaffenheit - Bestimmung der Aktivittskonzentration von Polonium-210 in Wasser mittels Alphaspektrometrie (ISO 13161:2011) Th
6、is European Standard was approved by CEN on 27 September 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical ref
7、erences concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a C
8、EN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedon
9、ia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPI
10、SCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 13161:2015 EBS EN ISO 13161:2015EN ISO 13161:2015 (E) 3 European foreword The text o
11、f ISO 13161:2011 has been prepared by Technical Committee ISO/TC 147 “Water quality” ofthe International Organization for Standardization (ISO) and has been taken over as EN ISO 13161:2015by Technical Committee CEN/TC 230 “Water analysis” the secretariat of which is held by DIN. This European Standa
12、rd shall be given the status of a national standard, either by publication of anidentical text or by endorsement, at the latest by April 2016, and conflicting national standards shall bewithdrawn at the latest by April 2016. Attention is drawn to the possibility that some of the elements of this doc
13、ument may be the subject ofpatent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patentrights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of thefollowing countries are bound to implement this European Standard: Au
14、stria, Belgium, Bulgaria,Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden
15、, Switzerland,Turkey and the United Kingdom.Endorsement notice The text of ISO 13161:2011 has been approved by CEN as EN ISO 13161:2015 without any modification. BS EN ISO 13161:2015ISO 13161:2011(E)Contents PageForeword ivIntroduction v1 Scope 12 Normative references .13 Terms, definitions, symbols
16、 and units 13.1 Terms and definitions .23.2 Symbols, definitions and units 24 Principle .24.1 General .24.2 Treatment .34.3 Principle of alpha spectrometry 35 Reagents and equipment 35.1 Reagents 35.2 Preparation material and treatment 45.3 Alpha spectrometry measuring equipment 46 Sampling and samp
17、les .47 Chemical treatment and deposit process .47.1 General .47.2 Chemical treatment .57.3 Disc cleaning 57.4 Deposition phase .58 Measurement by alpha spectrometry 68.1 General .68.2 Quality control 68.3 Measurement 69 Expression of results .69.1 General .69.2 Total yield 79.3 Activity concentrati
18、on of 210Po in the sample .79.4 Combined uncertainties 89.5 Decision threshold 89.6 Detection limit 89.7 Confidence limits .910 Test report .9Annex A (informative) Cell deposit examples .11Annex B (informative) Spectrum examples .13Bibliography .15 ISO 2011 All rights reserved iiiBS EN ISO 13161:201
19、5ForewordISO (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 t
20、echnical 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 Commission (IEC) on all matters
21、 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 technical committees are circulated
22、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 shall not be held responsible for
23、 identifying any or all such patent rights.ISO 13161 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 3, Radiological methods.ISO 13161:2011(E)iv ISO 2011 All rights reservedBS EN ISO 13161:2015IntroductionThere are different techniques to measure 210Po activity concent
24、ration in water: alpha spectrometry, liquid scintillation counting, alpha proportional counting.This International Standard describes a method for measuring 210Po activity concentration in natural waters by alpha spectrometry.Polonium 210 (210Po) is a natural alpha-emitting radionuclide with a half-
25、life of 138 d. It appears in the natural chain of uranium 238 (238U) (see Figure 1). It is a long-life decay product of radon 222 (222Rn) through lead 210 (210Pb) (see References 5 to 9).Precautions are required when manipulating radioactive materials such as polonium isotopes.The activity concentra
26、tion ranges of 210Po, in drinking waters for example, are generally very low, usually ranging from 1 mBq lnull1to 30 mBq lnull1.This International Standard is applicable to all types of water, including sea water, and usually allows the measurement of 210Po activity concentrations greater or equal t
27、o 5 mBq lnull1.NOTE 206Pb is stable.Figure 1 Uranium 238 and its decay productsISO 13161:2011(E) ISO 2011 All rights reserved vBS EN ISO 13161:2015BS EN ISO 13161:2015INTERNATIONAL STANDARD ISO 13161:2011(E)Water quality Measurement of polonium 210 activity concentration in water by alpha spectromet
28、ryWARNING Persons using this International Standard should be familiar with normal laboratory practice. This International Standard 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
29、 practices and to ensure compliance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests conducted according to this International Standard be carried out by suitably trained staff.1 ScopeThis International Standard specifies the measurement of 210Po activity conce
30、ntration by alpha spectrometry in all kinds of natural waters.The detection limit of this method depends on the volume of the sample, the counting time, the background count rate and the detection efficiency. In the case of drinking water, the analysis is usually carried out on the raw sample, witho
31、ut filtration or other pretreatment.If suspended material has to be removed or analysed, filtration at 0,45 m is recommended. The analysis of the insoluble fraction requires a mineralization step that is not covered by this International Standard (see NF M 60-790-44). In this case, the measurement i
32、s made on the different phases obtained. The final activity is the sum of all the measured activity concentrations.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated refere
33、nces, the latest edition of the referenced document (including any amendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methodsISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes and sampling techniquesISO 5667-3, Water quality
34、 Sampling Part 3: Preservation and handling of water samplesISO 11929, Determination of the characteristic 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:
35、 Atomic and nuclear physicsISO/IEC 17025, General requirements for the competence of testing and calibration laboratoriesISO/IEC Guide 98-3, Uncertainty of measurement Part 3: Guide to the expression of uncertainty in measurement (GUM:1995)3 Terms, definitions, symbols and unitsFor the purposes of t
36、his document, the terms, definitions, symbols and abbreviations given in ISO 80000-10 and the following apply. ISO 2011 All rights reserved 1BS EN ISO 13161:20153.1 Terms and definitions3.1.1certified reference solutionsolution of known concentration traceable to primary or secondary certified refer
37、ence solution standards of radioactivity3.1.2tracer solutionusually a secondary standard or reference material, such as 208Po or 209Po, employed to determine the chemical yield of the analysis3.1.3quality control standardradioactive source used to demonstrate that the measurement equipment employed
38、performs within defined limitsNOTE Quality control is usually carried out by the regular measurement of a suitable radioactive source in accordance with ISO 7870-11, ISO 7870-22, and ISO 78713.3.2 Symbols, definitions and unitsnull activity of the tracer added BqcAactivity concentration of 210Po Bq
39、lnull1cA*decision threshold Bq lnull1cA#detection limit Bq lnull1ccAAtrianglerighttriangleleft, lower and upper limits of the confidence intervalBq lnull1nullcchemical yield 1nullTtotal yield 1null0background count rate in the 210Po region of interest snull1null0Tbackground count rate in the tracer
40、region of interest snull1nullggross count rate of the sample in the 210Po region of interest snull1nullTgross count rate in the tracer region of interest snull1null0background counting time snullgsample counting time snull expanded uncertainty calculated by null null null null null(cA) with null nul
41、l 1, 2 . Bq lnull1null(cA) standard uncertainty associated with the initial measurement result Bq lnull1null volume of the test sample aliquot lnull counting efficiency 14 Principle4.1 GeneralAfter sampling, the test sample undergoes a treatment which leads to an extremely thin deposit of the poloni
42、um on a metal disc, for measurement by alpha spectrometry.ISO 13161:2011(E)2 ISO 2011 All rights reservedBS EN ISO 13161:2015210Po has a half-life of 138,376 d null 0,002 d (see Reference 11).The sample shall be analysed as soon as possible to give an activity concentration on the sampling date. If
43、the time elapsed between sampling and measurement is long, the activity concentration measured requires correction and it is then necessary to know the 210Pb and 210Bi activity concentrations of the sample to adjust the 210Po activity concentration on the sampling date.4.2 TreatmentThe main steps of
44、 the sample treatment are: filtration if necessary; aci dification with concentrated hydrochloric acid or nitric acid and addition of a polonium tracer (208Po or 209Po) solution;NOTE The polonium isotopes 208Po (5,11 MeV alpha emission) or 209Po (4,88 MeV alpha emission) can be used as tracers since
45、 interference with 210Po (5,31 MeV alpha emission) is minimal for sources displaying good resolution (null50 keV FWHM); 209Po is preferred, but 208Po is acceptable. addition of a reducing agent (e.g. ascorbic acid); spontaneous deposition of a thin layer on to a metal disc.The activity concentration
46、 measurement as well as the determination of the total yield is carried out by alpha spectrometry.4.3 Principle of alpha spectrometryThe thin layer deposited on the metal disc allows the detection of alpha particles. The interaction of alpha particles and detector results in a change in (bias) curre
47、nt that is proportional to the energy of the particles.The electronic pulses generated by the detector are amplified, and displayed as an energy spectrum using an analogue-digital converter, multiple channel analyser, and computer processing. The spectrum display enables the radionuclides present in
48、 the source to be identified and integration of counts enables the determination of activity concentration of the test sample, taking into account the background counting rates and/or the blank test and the total yield.A blank test should be carried out with the same reagents replacing the water sam
49、ple by water complying with ISO 3696, grade 3 previously used for the preparation of the reagents without tracer.To ensure the acceptable performance of the detector system, a quality control standard shall be measured.The chemical yield of 210Po measurement is determined by adding a radioactive tracer. The total yield is a product of the chemical yield and the detection efficiency.5 Reagents and equipment5.1 ReagentsDuring chemical treatment and cleaning of the metal disc, use only reagents of recognized analytica
