DIN EN ISO 11704-2015 Water quality - Measurement of gross alpha and beta activity concentration in non-saline water - Liquid scintillation counting method (ISO 11704 2010) German .pdf

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1、November 2015 English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 13.060.60; 17.240!%I;6“2382419w

2、ww.din.deDIN EN ISO 11704Water quality Measurement of gross alpha and beta activity concentration in Liquid scintillation counting method (ISO 11704:2010);English version EN ISO 11704:2015,English translation of DIN EN ISO 11704:2015-11Wasserbeschaffenheit Bestimmung der Gesamt-Alpha- und Gesamt-Bet

3、a-Aktivitt in nicht-salzhaltigem Wasser Verfahren mit dem Flssigszintillationszhler (ISO 11704:2010);Englische Fassung EN ISO 11704:2015,Englische bersetzung von DIN EN ISO 11704:2015-11Qualit de leau Mesurage des activits alpha globale et bta globale des eaux non salines Mthode de comptage par scin

4、tillation liquide (ISO 11704:2010);Version anglaise EN ISO 11704:2015,Traduction anglaise de DIN EN ISO 11704:2015-11www.beuth.deDocument comprises 19 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.non-saline water 11.15 DIN E

5、N ISO 11704:2015-11 2 National foreword The text of ISO 11704:2010 has been prepared by Technical Committee ISO/TC 147 “Water quality” and has been taken over as EN ISO 11704:2015 by Technical Committee CEN/TC 230 “Water analysis” (Secretariat: DIN, Germany). The responsible German body involved in

6、its preparation was DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Committee NA 119-01-03 AA Wasseruntersuchung. Designation of the method: Measurement of gross alpha and beta activity concentration in non-saline water - Liquid scintillation counting method (C 32):

7、 Method DIN EN ISO 11704 C 32 The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 5667-1 DIN EN ISO 5667-1 ISO 5667-3 DIN EN ISO 5667-3 ISO 5667-14 DIN ISO 5667-14 ISO 11929 DIN ISO 11929 ISO 80000-10 DIN EN ISO 80000-

8、10 ISO/IEC 17025 DIN EN ISO/IEC 17025 A comma is used as the decimal marker. DIN EN ISO 11704:2015-11 3 Expert assistance and specialized laboratories will be required to perform the analyses described in this standard. Existing safety requirements are to be observed. Depending on the objective of t

9、he analysis, a check shall be made on a case-by-case basis as to whether and to what extent additional conditions will have to be specified. This standard has been prepared by Measurement of gross alpha and beta activity concentration in non-saline water Liquid scintillation counting method (C 32).

10、Standard methods published as DIN Standards are obtainable from Beuth Verlag GmbH, either individually or grouped in volumes. The standard methods included in the loose-leaf publication entitled Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published b

11、y Beuth Verlag GmbH and Wiley-VCH Verlag GmbH 13.060.60 English Version Water quality - Measurement of gross alpha and beta activity concentration in non-saline water - Liquid scintillation counting method (ISO 11704:2010) Qualit de leau - Mesurage des activits alpha globale et bta globale des eaux

12、non salines - Mthode de comptage par scintillation liquide (ISO 11704:2010) Wasserbeschaffenheit - Bestimmung der Gesamt-Alpha- und Gesamt-Beta-Aktivitt in nicht-salzhaltigem Wasser - Verfahren mit dem Flssigszintillationszhler This European Standard was approved by CEN on 30 July 2015. CEN members

13、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 references concerning such national standards may be obtained on application t

14、o 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 CEN member into its own language and notified to the CEN-CENELEC Management

15、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 Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lith

16、uania, Luxembourg, 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

17、-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 11704:2015 E(ISO 11704:2010) Contents Page 3 1 Scope4 2 Normative references4 3 Symbols, definitions and units 5 4 Principle5 5 Reagents and equipment6 6 Sampl

18、ing.7 7 Procedure.7 7.1 Direct counting 7 7.2 Thermal preconcentration 8 7.3 Sample preparation .7.4 Liquid scintillation measurement 8 8 Expression of results10 8.1 Calculation of activity per unit of mass 10 8.2 Standard uncertainty.11 8.3 Decision threshold 11 8.4 Detection limit12 8.5 Confidence

19、 limits.12 8.6 Quality control .13 9 Interference control.13 9.1 Contamination .13 9.2 Ingrowth of radon13 9.3 Loss of polonium.13 10 Test report13 Bibliography15 European foreword EN ISO 11704:2015 (E) 8 2 DIN EN ISO 11704:2015-11 European foreword The text of ISO 11704:2010 has been prepared by Te

20、chnical Committee ISO/TC 147 “Water quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 11704:2015 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 nati

21、onal standard, either by publication of an identical text or by endorsement, at the latest by February 2016, and conflicting national standards shall be withdrawn at the latest by February 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of pa

22、tent rights. CEN and/or CENELEC shall not be held responsible for identifying 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, C

23、roatia, 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, Switzerland, Turkey an

24、d the United Kingdom. Endorsement notice The text of ISO 11704:2010 has been approved by CEN as EN ISO 11704:2015 without any modification. EN ISO 11704:2015 (E) 3 DIN EN ISO 11704:2015-11 WARNING Persons using this International Standard should be familiar with normal laboratory practice. This stan

25、dard 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

26、nducted according to this International Standard be carried out by suitably trained staff. 1 Scope This International Standard specifies a method for the determination of gross alpha and gross beta activity in waters for radionuclides which are not volatile at 80 C. Radon isotopes and their decay pr

27、oducts of short half life are not included in the determination. The method is applicable to raw and potable waters with a dry residue less than 5 g/l and when no correction for colour quenching is necessary. 2 Normative references The following referenced documents are indispensable for the applica

28、tion 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 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples ISO/IEC 17025,

29、General requirements for the competence of testing and calibration laboratories ISO 80000-10, Quantities and units Part 10: Atomic and nuclear physics EN ISO 11704:2015 (E) 4 DIN EN ISO 11704:2015-11 3 Symbols, definitions and units For the purposes of this document, the definitions, symbols and abb

30、reviations defined in ISO 80000-10, as well as the following symbols, definitions and units, apply. a,aAlpha and beta activity per mass Bq g1a* Decision threshold Bq g1#a Detection limit Bq g1,aaLower and upper limits of the confidence interval Bq g1A,AActivity of the alpha and beta emitter certifie

31、d reference solution used for the and calibration sources Bq m Mass of the test sample g m1Mass of initial sample subject to heating or possibly concentration g m2Mass of heated or concentrated sample g m3Mass of heated or concentrated sample transferred in the vial g mS, mSMass of alpha and beta em

32、itters certified reference solutions, respectively g rg, rgSample gross count rate, from the alpha and beta windows, respectively s1r0, r0, r0TBlank count rate, from the alpha, beta and total windows, respectively s1rS, rS, rS,TCount rate of the alpha calibration source in the alpha, beta and total

33、window s1rS, rS, rS,T Count rate of the beta calibration source in the alpha, beta and total window s1tgSample counting time s t0Blank counting time s ts, tsCounting time of and calibration sources s u (a) Standard uncertainty associated with the measurement result Bq g1U Expanded uncertainty, calcu

34、lated from U = ku (a), where k = 1, 2 Bq g1()uaStandard uncertainty of aas a function of its true value Bq g1, Counting efficiency for alpha and beta, respectively ()Alpha interference Fraction of counts observed in the beta window withrespect to the total number of counts measured by the counter wh

35、en analpha emitter is measured ()Beta interference Fraction of counts observed in the alpha window withrespect to the total number of counts measured by the counter when a betaemitter is measured 4 Principle Gross alpha and beta activity concentrations are determined by using liquid scintillation co

36、unting of a water sample mixed with a scintillation cocktail. Gross alpha and beta determinations are not absolute determinations of the sample radioactive contents, but relative determinations referred to a specific alpha or beta emitter which constitutes the standard calibration sources. These typ

37、es of determinations are also known as the alpha and beta index. EN ISO 11704:2015 (E) N1)N2)N1)National footnote: Denoting the decision threshold relative to the mass. N2)National footnote: Denoting the detection limit relative to the mass. 5 DIN EN ISO 11704:2015-11 The aqueous sample is acidified

38、 using nitric acid and heated. Subsequently, water with low salt content can be thermally concentrated by slow evaporation to improve the method sensitivity. An aliquot of sample is transferred into a liquid scintillation vial with scintillation cocktail; scintillations from the vial are then counte

39、d by equipment with an alpha and beta discrimination device. The counter is previously optimized with respect to an alpha and beta discriminator setting and then calibrated against alpha and beta emitter certified reference solutions. In data evaluation, no correction for chemical quenching is appli

40、ed, since the procedure is designed to provide samples with a constant quenching level. The method does not account for 222Rn and its daughters of short half life and it is not suitable for 3H and 14C measurement. When suspended matter is present in significant quantities, a filtration step is requi

41、red before acidification. 5 Reagents and equipment All reagents shall be of recognized analytical grade, except for the scintillation cocktail, and shall not contain any detectable alpha and beta activity, except for the radioactive certified reference solutions. 5.1 Nitric acid, c(HNO3) = 15,8 mol/

42、l, = 1,42 g/ml, mass fraction w(HNO3) = 70 %. 5.2 Water, ISO 36961, grade 3. Deionized water can contain detectable amounts of 222Rn and short half-life decay products. It is therefore strongly recommended to boil water under vigorous stirring and let it stand for one day before use. Alternatively,

43、use nitrogen flushing for about 1 h for a 2 l sample. 5.3 Scintillation cocktail. Commercially available scintillation cocktails suitable for alpha and beta discrimination (e.g. diisopropylnaphthalene-based cocktails). 5.4 Volatile organic solvents. Methanol or ethanol. 5.5 Certified reference solut

44、ions. A calibration laboratory establishes traceability of its own calibration sources and measuring instruments to the International System of Units (SI) by means of an unbroken chain of calibrations or comparisons linking them to relevant certified reference solutions of the SI units of measuremen

45、t. The link to the SI units may be achieved with respect to national certified reference materials. These may be primary realizations of the SI units, or agreed representations of SI units based on fundamental physical constants, or they may be secondary materials which are materials certified by an

46、other national metrology institute. When using external calibration services, traceability of measurement shall be assured by the use of calibration services from laboratories that can demonstrate competence, measurement capability, and traceability. The calibration certificates issued by these labo

47、ratories shall contain the measurement results, including the measurement uncertainty and/or statement of compliance with an identified metrological specification. NOTE Calibration laboratories fulfilling the requirements of this International Standard are considered to be competent. A calibration c

48、ertificate bearing an accreditation body logo from a calibration laboratory accredited to this International Standard, for the calibration concerned, is sufficient evidence of traceability of the calibration data reported. In general, the experimental parameters (efficiency, alpha and beta optimum discrimination) depend on alpha and beta energies, thus the choice of alpha and beta emitter certified reference solutions will depend on knowledg