1、BSI Standards PublicationBS ISO 9698:2010Water quality Determinationof tritium activityconcentration Liquidscintillation counting methodBS EN ISO 9698:2015BS EN ISO 9698:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 9698:2015.It is identical to ISO 96
2、98:2010. It supersedes BS ISO 9698:2010 whichis withdrawn.The UK participation in its preparation was entrusted by TechnicalCommittee EH/3, Water quality, to Subcommittee EH/3/8, Radioactivitymeasurements methods.A list of organizations represented on this subcommittee can beobtained on request to i
3、ts secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 88453 5 ICS 13.060.60; 13.280 Compliance with a British
4、 Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the StandardsPolicy and Strategy Committee on 31 March 2011.Amendments/corrigenda issued since publicationDate Text affected31 July 2015 This corrigendum renumbers BS ISO 9698:2010 asBS
5、 EN ISO 9698:2015EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 9698 July 2015 ICS 13.080; 13.060.60 English Version Water quality - Determination of tritium activity concentration - Liquid scintillation counting method (ISO 9698:2010) Qualit de leau - Dtermination de lactivit volumique du
6、 tritium - Mthode par comptage des scintillations en milieu liquide (ISO 9698:2010) Wasserbeschaffenheit - Bestimmung der Aktivittskonzentration von Tritium - Verfahren mit dem Flssigszintillationszhler (ISO 9698:2010) This European Standard was approved by CEN on 16 July 2015. CEN members are bound
7、 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 references concerning such national standards may be obtained on application to the CEN
8、-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 CEN member into its own language and notified to the CEN-CENELEC Management Centre ha
9、s 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 Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Lu
10、xembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Bru
11、ssels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 9698:2015 EEN ISO 9698:2015 (E) 3 European foreword The text of ISO 9698:2010 has been prepared by Technical Committee ISO/TC 147 “Water quality” of the International O
12、rganization for Standardization (ISO) and has been taken over as EN ISO 9698:2015 by Technical Committee CEN/TC 230 “Water analysis” the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endo
13、rsement, at the latest by January 2016, and conflicting national standards shall be withdrawn at the latest by January 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for iden
14、tifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugo
15、slav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 9698:2010 has
16、 been approved by CEN as EN ISO 9698:2015 without any modification. BS EN ISO 9698:2015EN ISO 9698:2015 (E)BS ISO 9698:2010ISO 9698:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Symbols, definitions and units 2 4 Principle .3 5 Re
17、agents and equipment3 6 Sampling and samples5 7 Procedure.6 8 Expression of results8 9 Test report10 Annex A (informative) Numerical applications .12 Annex B (informative) Distillation of large volume sample .14 Annex C (informative) Internal standard methods .17 Annex D (informative) Distillation o
18、f small volume sample.19 Annex E (informative) Screening method for wet matrices.22 Bibliography24 BS EN ISO 9698:2015ISO 9698:2010(E)BS ISO 9698:2010ISO 9698:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of nationa
19、l 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 committee has been established has the right to be represented on that committee. Internation
20、al 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 electrotechnical standardization. International Standards are drafted in accordance with the rules
21、 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 to the member bodies for voting. Publication as an International Standard requires approval by at le
22、ast 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 identifying any or all such patent rights. ISO 9698 was prepared by Technical Committee ISO/TC 147
23、, Water quality. This second edition cancels and replaces the first edition (ISO 9698:1989), which has been technically revised. BS EN ISO 9698:2015ISO 9698:2010(E)BS ISO 9698:2010ISO 9698:2010(E) ISO 2010 All rights reserved vIntroduction The tritium present in the environment is of natural origin
24、and man made. As a result of atmospheric nuclear weapon testing, emissions from nuclear engineering installations, and the application and processing of isotopes, relatively large amounts of tritium have been released to the environment. Despite the low dose factor associated to tritium, monitoring
25、of tritium activity concentrations in the environment is necessary in order to follow its circulation in the hydrosphere and biosphere. BS EN ISO 9698:2015ISO 9698:2010(E)BS ISO 9698:2010BS EN ISO 9698:2015BS ISO 9698:2010INTERNATIONAL STANDARD ISO 9698:2010(E) ISO 2010 All rights reserved 1Water qu
26、ality Determination of tritium activity concentration Liquid scintillation counting method WARNING 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 prac
27、tices 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 Scope This International Standard specifies the conditions for the determination of t
28、ritium activity concentration in samples of environmental water or of tritiated water (3HH2O) using liquid scintillation counting. The choice of the analytical procedure, either with or without distillation of the water sample prior to determination, depends on the aim of the measurement and the sam
29、ple characteristics (see References 1, 2, 3). Direct measurement of a raw water sample using liquid scintillation counting has to consider the potential presence of other beta emitter radionuclides. To avoid interference with these radionuclides when they are detected, the quantification of tritium
30、will be performed following the sample treatment by distillation (see References 4, 5, 6, 7). Three distillation procedures are described in Annexes B, D and E. The method is not applicable to the analysis of organically bound tritium; its determination requires additional chemical processing (such
31、as chemical oxidation or combustion). With suitable technical conditions, the detection limit may be as low as 1 Bq l1. Tritium activity concentrations below 106Bq l1can be determined without any sample dilution. A prior enrichment step can significantly lower the limit of detection (see References
32、8, 9). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 5667-1, Water q
33、uality Sampling Part 1: Guidance on the design of sampling programmes and sampling techniques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples ISO 5667-14, Water quality Sampling Part 14: Guidance on quality assurance of environmental water sampli
34、ng and handling ISO 80000-10, Quantities and units Part 10: Atomic and nuclear physics ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories BS EN ISO 9698:2015BS ISO 9698:2010ISO 9698:2010(E) 2 ISO 2010 All rights reservedISO/IEC Guide 98-3:2008, Uncertainty
35、 of measurement Part 3: Guide to the expression of uncertainty in measurement (GUM:1995) ISO/IEC Guide 99:2007, International vocabulary of metrology Basic and general concepts and associated terms (VIM) 3 Symbols, definitions and units For the purposes of this document, the definitions, symbols and
36、 units defined in ISO 80000-10, ISO/IEC Guide 98-3 and ISO/IEC Guide 99, as well as the following symbols, apply. maxMaximum energy for the beta emission, in kilo-electronvolts V Volume of test sample, in litres m Mass of test sample, in kilograms Mass density of the sample, in grams per litre cAAct
37、ivity concentration, in becquerels per litre a Activity per unit of mass, in becquerels per kilogram A Activity of the calibration source, in becquerels t0Background counting time, in seconds tgSample counting time, in seconds tsCalibration counting time, in seconds n Number of repetitions r0iBackgr
38、ound count rate in the repetition i, per second r0Mean background count rate for i repetitions, per second rgiSample count rate in the repetition i, per second rgMean sample count rate for i repetitions, per second rsCalibration count rate, per second Detection efficiency qEfficiency measured for ea
39、ch of the working standards to elaborate the quench curve fqQuench factor u(cA) Standard uncertainty associated with the measurement result, in becquerels per litre U Expanded uncertainty, calculated by U = k u(cA) with k = 1, 2, in becquerels per litre *Ac Decision threshold, in becquerels per litr
40、e #Ac Detection limit, in becquerels per litre ,A Acc#AcNg210 225 390 tgs 3 600 3 600 3 600 rgs10,058 3 0,062 5 0,108 3 N0180 180 180 t0s 3 600 3 600 3 600 r0s10,050 0,050 0,050 V l 0,010 0,010 0,010 u(V) l 0,002 5 0,002 5 0,002 5 0,25 0,25 0,25 urel() 0,035 0,035 0,035 , , % 5 5 5 w l1400 400 400 u
41、rel(w) 0,252 0,252 0,252 0,922 0 0,974 2 0,999 8 p 0,898 9 0,949 9 0,974 9 q 0,977 0 0,975 6 0,975 0 kp 1,275 1,644 1,957 kq 1,994 1,971 1,960 cABq l13,33 5,00 23,33 u(cA) Bq l12,35 2,57 6,46 *Ac Bq l13,47 3,47 3,47 #Ac Bq l18,74 8,74 8,74 AcBq l18,02 10,06 36,00 Ngand N0are the number of the counte
42、d impulsions for the sample and for the background, respectively. BS EN ISO 9698:2015ISO 9698:2010(E)BS ISO 9698:2010ISO 9698:2010(E) ISO 2010 All rights reserved 13For example, functions to calculate , kp, kq, in Excel1)are: = NORMSDIST ( ()Auc / ) Ackp= NORMSINV (p) kq= NORMSINV (q) 1) Microsoft E
43、xcel is an example of a suitable product available commercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product.BS EN ISO 9698:2015ISO 9698:2010(E)BS ISO 9698:2010ISO 9698:2010(E) 14 ISO 2010 All rig
44、hts reservedAnnex B (informative) Distillation of large volume sample B.1 Principle Samples of volume from 100 ml to 500 ml are considered as large volume samples. Before the distillation of the water sample, oxidizing and suitable alkaline agents are added to degrade organic matter and transform io
45、dine into iodide. An aliquot of the distillate is then mixed with the scintillation solution in a counting vial (see Reference 14). NOTE The majority of the interfering compounds, which quench the scintillation process, remain in the residue of the distillation together with any interfering radionuc
46、lides (radioactive iodine, carbon 14, caesium 137, etc.). B.2 Reagents and equipment During the analysis, use only reagents of recognized analytical grade. B.2.1 Reagents For the oxidant/alkaline medium use either of those given in B.2.1.1. B.2.1.1 Sodium thiosulfate, anhydrous, Na2S2O3, and sodium
47、carbonate, anhydrous, Na2CO3, or potassium permanganate, KMnO4and sodium hydroxide, NaOH. The sodium hydroxide shall be free of tritium. B.2.1.2 Tritium standard solution. B.2.1.3 Scintillation solution. B.2.1.4 Blank water. B.2.1.5 Carborundum or glass beads. B.2.2 Equipment Use usual laboratory eq
48、uipment and the following. B.2.2.1 Cooling system, consisting of cooler, circulating bath (5 C); Dewar flask, adapted to the receiver flask. B.2.2.2 Heating system, consisting of heater, adapted to the distillation flask; air gun heater. BS EN ISO 9698:2015ISO 9698:2010(E)BS ISO 9698:2010ISO 9698:20
49、10(E) ISO 2010 All rights reserved 15B.2.2.3 Distillation equipment, consisting of the following. B.2.2.3.1 Distillation flask, with a capacity of 500 ml. B.2.2.3.2 Splash head. B.2.2.3.3 Distillation column, length 40 cm. B.2.2.3.4 Condenser. B.2.2.3.5 Adapter, bent type. The equipment shall be dried before use. B.2.2.3.6 Borosilicate glass or polyethylene bottles, of capacity about 100 ml. B.3 Distillation Place the test sample in the dis
