ISO 04722-1-2023.docx

INTERNATIONA1.STANDARDISO4722-1editionFirst2023-10Waterqua1.ityThorium232幅骷WethOdusinga1.phaspectrometryQua1.itedeeauThorium232Partie1:Methoded,essaiparSpectrometriea1.phaRctcrcnccnumberISO4722-1.:2023(E)COPYRIGHTPROTECTEDDOCUMENT©ISO2023IUirhM*hedbdi1.iUedotherwiseupdhi.orkwqntto<itH0Dtf1.e!ron>ctu1.aicnpkni1tUqntt*>HdU>cop)nppU1.>joationmaytheinternetoranintranet,withoutpriorwrittenpermission.PermissioncanberequestedfromeitherISOattheaddressbe1.oworISO'smemberbodyinthecountr)oftherequester.f),WV>fifiU81.andonnet8CH-1214Vernier,GenevaPhone：M1.227490111觥ftte:丽丽BQrgPub1.ishedinSwitzer1.andContentsForewordIitroductionScopeNormativereferencesTerms,definitionsandsymbo1.s3.1TermsanddefinitionsSfmbo1.sPrincip1.eChemica1.reagentsandequipmentS.1Genera1.5.2Chemica1.reagentsSamp1.ing,hand1.ingandstorage一.61Samp1.ing.6.2Samp1.estorageSeparationandmeasurement7.1 Chemica1.steps7.2 Measurement7.2.1 Qua1.itycontro1.7.2.2 Chemica1.recovery7.2.3 BackgroundExpressionofresu1.ts8.1 Spectrumana1.ysis8.2 Ca1.cu1.ationofactivityconcentration潮螂棉翳鼬UyDetection1.imit1.imitsofcoverageinterva1.s9.1 1.imitsoftheprobabi1.istica1.1.ysymmetriccoverageinterva1.9.2 1.imitsoftheshortestcoverageinterva1.TestreportAnnexA(informative)Chemica1.separationOfthorium._._.AnnexB(informative)Preparationofthesourcebye1.ectrodepositionAnnexC(informative)PreparationofthesourcebycoprecipitationBib1.iographyForewordISO(theInternationa1.OrganizationforStandardization)isawor1.dwidefederationofnationa1.standardsttiugh(ISOmrtmiw)bMd>niK盟RAucekdHpfff1.QbbGgbodyIcommitteehasbeenestab1.ishedhastherighttoberepresentedonthatcommittee.Internationa1.organizations,governmenta1.andnon-governmenta1.,in1.iaisonwithISO,a1.sotakepartinthework.ISOco1.1.aboratesc1.ose1.ywiththee1.ectrotechnica1.standardization.Internationa1.E1.ectrotechnica1.Commission(IEC)ona1.1.mattersofTheproceduresusedtodeve1.opthisdocumentandthoseintendedforitsfurthermaintenancearedyiFFHSOfISO雇etW1.kes,s姗抬”not1.f1.fcfcww1.蝌闾IC嚓COrdanCe肺theeditoria1.ru1.esoftheISO/IECDirectives.Part2(seewwsv.iso.org/direc1.ives).假)(¾徽ents)aWNWontakest三嬲据i帆n曲1.fiB幽硼8硒ffiHFtm部幽曲野榴IVQdaimedpatentrightsinrespectthereof.Asofthedateofpub1.icationofthisdocumentISOhadnotreceivednoticeof（八）patent(三)whichmayberequiredtoimp1.ementthisdocument.However,imp1.ementersare触怖翻琳酶/mj，wWjSOQFg/眸IentS洗蝮油那ion,扁MMSPOn赖岫油嬲9的阳躲Ora"suchpatentrights.Anytradeusedinthisconstitutenameendorsenent.documentisinformationgivenfortheconvenienceofusersanddoesnotForanexp1.anationofthevo1.untarynatureofstandards,themeaningofISOspecifictermsand幽幽蛔豳酒侬遮W即辆O)assEif1.眦聚inwe帼"1.见OnBar池帆四dead邮&CcsVbr¼11isoorgisoforeword.htmI.ThisdocumentwaspreparedRadioactivitymeasurements,byTechnica1.CommitteeISO/TC147,Waterqua1.ity,SubcommitteeSC3,AIistofa1.1.partsintheISO4722seriescanbefoundontheISOwebsite.由珏拼占6“典fiftsHHiesthismRMeHftKFhoUWWW!而图membeKft1.i命nationa1.standardsbody.AIntroductionwaters,seawaters)containradionuc1.ides,whichcanbeofeithernatura1.oranthropogenicorigin.canrainwater)inorre1.easedfromtechno1.ogica1.Processesprocessesinvo1.vingdesorptionoccurringradioactiveAnthropogenicradionuc1.idesemittingradionuc1.idessuchSr,wTc,transuranice1.ementsfoundNp,natura1.Anthropogenicradionuc1.idesUsedbeforemcdica1.dischargcdtotheenvirontncntandre1.easedbodies.occurredattheChornoby1.andFukushimanuc1.earfaci1.ities.nuc1.earfaci1.itiescanduringp1.anned,radionuc1.idesatemergencyconcentationssitations.can11presentdrinkingNationa1.regu1.ationsusua1.1.yeff1.uentsactivityconcentrationenvironment,authorizedCandrinkingNOTEOfdrinkingRUidanCe1.eve1.ca1.cu1.atedinReferenceetYectiveisdoseactivityconcentrationthat,Withpub1.icintakeofconcentrationcanpossib1.yemergency,thethanVHOCodexandGuideIine1.eve1.sTh,respective1.y,theactivitydeve1.OPeddQCUmentContains1.aboratoriestodetermine232232Thwaterwatersamp1.es.Thetestmethodhasbeencountingtimeofabout200OOOs.characteristic1.imit,decisionthresho1.d,Suchdetectionemergencyanduncertaintiesnationa1.guidance1.imits1.imits.©ISO2023-A1.1.rightsreservedRadionuc1.idesarepresentthroughouttheenvironment;thus,waterbodies(e.g.surfacewaters,groundNatura1.1.y-occurringradionuc1.ides,inc1.uding3i,mC,4oKandthoseoriginatingfromthethoriumanduraniumdecayseries,inparticu1.ar210Pb,2oPor222Rn,22Ra,22Ra,227c23iPa,23Uand23U,bybefoundwaterbodiesdueeithernatura1.(e.g.natura1.1.yfromtheSoi1.runoffmateria1.s(e.g.mining;minera1.processing;oi1.,gasandcoa1.production;watertreatment;andproductionanduseofphosphateferti1.isers).andCm)andsomegammasuch55Fe,59Ni,63Ni,90as60C0and137Csa1.sobe(e.g.inPu,Amwaters.Sma1.1.quantitiesofanthropogenicradionuc1.idescanbedischargedfromnuc1.earfaci1.itiestotheenvironmentasaresu1.tofauthorizedroutinere1.eases.Theradionuc1.idespresentin1.iquidef11uentsarcusua1.1.ycontro1.1.edinbeingandindustria1.app1.icationscanbewatertotheenvironmentafteruse.Anthropogenicradionuc1.idesarca1.sofoundinwatersduetocontaminationfromfa1.1.outresu1.tingfromabove-groundnuc1.eardetonationsandaccidentssuchasthosethathaveRadionudideactivityconcentrationsinwaterbodiescanvaryaccordingto1.oca1.geo1.ogica1.characteristicsandc1.imaticconditionsandcanbe1.oca1.1.yandtempora1.1.yenhancedbyc1.easesfromwatersourcesthuscontainexistingactivityexposurethat23jSomeahumanhea1.thrisk.TheWor1.dHea1.thOrganization(WHO)recommendstoroutine1.ymonitorradioactivityindrinkingwaters4andtotakeproperactionswhenneededtominimizethehea1.thrisk.waters,waterbodiesandIiquidspedfythetobedischargedthe1.imitsthatareThese1.imitsinvaryforp1.anned,existing,andemergencyexposuresituations.Forexamp1.e,duringeitherap1.annedorexistingsituation,theWHOguidance1.eve1.for232Thindrinkingwateris1Bq1.-(seeNOTE).Comp1.iancewithobtained,withasscssedassociateduncertaintes.radioactivityspedfiedwaterSanip1.esGuidc9&»3comparing5667-2016).21.d-Thewaterforoneyear,resu1.tsinan4theof0.1mSva-membersoftheanThisisaneffectivedosethatrepresentsavery1.ow1.eve1.ofrisktohumanhea1.thandwhichisnotexpectedtogiverisetoanydetectab1.eadversehea1.theffects(4.Intheeventofnuc1.earbenotgreater1Bq1.-10Bq1.-for232p)statesthatforinfantsandotherthaninfants.Thissupportmet1.odtoThininThedetection1.imitformeasurementofatestportionofabout500m1.isapproximate1.y5mBq1.-withaas1.imitsituations,Iowerarebe1.owtherequiredandThemethodsdescribedinthisdocumentcanbeusedforvarioustypesofwaters(seeC1.ause1).Minormodificationssuchassamp1.evo1.umeandcountingtimecanbemadeifneededtoensurethattheThiscanbedoneforsevera1.reasonsoperationa1.requirements.Waterqua1.ityThorium232Testmethodusinga1.phaspectrometryWARNINGPersonsusingthisdocumentshou1.dbefami1.iarwithnorma1.1.aboratorypractice.Thisdocumentdoesnotpurporttoaddressa1.1.thesafetyprob1.ems,ifany,associatedwithitsuse.Itistheresponsibi1.ityoftheusertoestab1.ishappropriatesafetyandhea1.thpracticesandtodeterminetheapp1.icabi1.ityofanyotherrestrictions.IMPORTANTItisessentia1.thattestsconductedaccordingtothisdocumentbecarriedoutbysuitab1.ytrainedstaff.1 Scopeconcentrationenvironmentenvironmenta1.spcctrometry(inc1.uding229seaWatcrsJrccoverytracer.Waterschemica1.thoriumprincip1.esout1.inedandthisdocumentaqueoussamp1.es,fortheana1.ysisofothera1.pha-emitting2 Normativereferencesconstitutesrequirements1.atesteditiondocument.referencedreferences,(inc1.uc1.ingamendments)app1.ies.app1.ies.samp1.ingCeChniqUeSqUaIia-Samp1.ingPart1:Guidanceonthedesignofsamp1.ingprogrammesandISOcoverageDeterminationmeasurementscharactensticradiationFundamenta1.sdetectionapp1.ication1.imitsofE1.ementaryapp1.icationsISOTerms,definitionsandsymbo1.sIAtomicandnuc1.earphysics3.1TermsanddefinitionsappyPart1:Thisdocumentspecifiesthemethodandtheconditionsforthedetermination0f232Thactivityre1.easethesamp1.esofusinga1.phawaterandThandwasteAbeforeseparationa1.1.owstoseparateandpurifythoriumfromatestportionofthesamp1.e.Thegencra1.isotopessuchas22Thin230Thincanbeapp1.iedThefo1.1.owingdocumentsarereferredtointhetextinsuchawaythatsomeora1.1.oftheircontentundatedreferences,theofthisoftheFordateddocumenton1.yIhcanycditioncitedForISO3696,Waterforana1.ytica1.1.aboratoryuseSpecificationandtestmethodsISO5667-1.rWaterISO5667-3,Waterqua1.itySamp1.ingPart3:Preservationandhand1.ingofwatersamp1.esthe119291,interva1.)orof(heofIonizing1.imits(decisionthresho1.d,and1.imitandPart1：ISO/IEC17025,Genera1.requirementsforthecompetenceoftestingandca1.ibration1.aboratories380000-1OtQuantitiesunits-PartForthepurposesofthisdocument,thetermsanddefinitionsgiveninISO11929-1andISO80000-10ISOandIECmaintaintermino1.ogydatabasesforuseinstandardizationatthefo1.1.owingaddresses：ISOOn1.inebrowsingp1.atform:avai1.ab1.eathttps:/www.iso.org/obpSymbo1.DescriptionUnitACAActivityoftheThtraceraddedBqCACACACA<>CACACkpPPaPPYPPapPYqRRrrrrttUUcUCAU(C八cUCAWVaYDistributionfunctionofthestandardizednorma1.distributionThesymbo1.susedinthisdocumentarc“斑IM1.Symbo1.sAuxi1.iaryquantity4Princip1.eseparationchemica1.iso1.ationexchangechromatography).step(e.g.aprecipitation)andaspecificradionuc1.idesfromthewatersamp1.e,tracerifnochemica1.separationiscarriedouttoremovethesespectrometrya1.phapartideschamberthesemiconductor-typeInteractionMeasurementsre1.ywhichtheprovidesaspectrum/romwhichdetcctornumberana1.ysed(counts)e1.ectronicsystems.energyana1.ysissoftwaresamp1.eactivityconcentrationfor232recoveryCorrcctingrecoveryb1.ankdetcc1.ionefidency).ofthetestdeterminedchemica1.measuringthetota1.measurementrecoveryfromthenetcountrateof229Th,radioactiveCharacteriscics1.aboratoryVvaterthoriumcomp1.ianceWithgiven3696Tab1.2(seeReferencestracer.TheTab1.e2Characteristicsofthemainthoriumisotopes23214.02(6)1094011,2(14)21.05 Chemica1.reagentsandequipment5.1 Genera1.describedpresentedsha1.1.beUSed.whichgivevariousoptions.Wheretherearechoices,at1.eastoneoftheThetestsamp1.eismixedwithana1.iquot0f2z9Thtracer,fo1.1.owedbyequi1.ibrationofthesamp1.epriorana1.ysis,stcp(e.g.usingofthoriumbyconcentrationUraniumisotopes,210P0.237Np,23Pu0r241Amcanbepresentinwaterandcaninterferewiththecounting23zThandthe229ThThemeasuredthinsourceispreparedbye1.ectrodepositionorco-precipitationandmeasuredbya1.phainteractionofusinggridwithoradetectingmedium.Thisapparatus,createscharge,onisamp1.ifiedandoutputasavo1.tagepu1.seproportiona1.tothedepositedenergyoftheincominga1.phapartic1.e.Thee1.ectricpu1.seinthetheIsofP1.HSeSbytherecordedineachDatainterva1.isshown.Theana1.ysisofthecountratesinthe232Tha1.phaenergywindowa1.1.owsthedeterminationofthetestandthetota1.measurementTh,after(chemica1.fortheandcountrate,thevo1.umeThechemica1.recoveryanddetectionefficiencyarenotnecessari1.ydeterminedseparate1.ybutareaddedasatogetherbyrecoverytracer.Forqua1.itycontro1.andtoquantifypotentia1.impuritiesinthetracerso1.ution,ab1.anksamp1.esha1.1.bepreparedusinggrade3ofthemaininisotopesareISOinwiththeadditionof8,9and>«).ThoriumisotopeHa1.f-Iifc(uncertainty)Maina1.phapartic1.eemissionenergy(uncertainty)Intensity3948.5(14)78,9TheChemiea4ndequipmentusedforchemica1.treatmentandpreparationofthesourceareoptionsinAnnexesAtoC,Useon1.yreagentsofrecognizedana1.ytica1.grade.5.2 Chemica1.reagents5.2.1 1.aboratorywater,usedasab1.ank,asfreeaspossib1.eofchemica1.orradioactiveimpurities(e.g.uraniumorthoriumisotopes),comp1.yingwithISO3696,gade3.Un1.essotherwisestated,waterreferstodeionisedwater.tQIWiSWfHtM<f1.utidftfQ卜求电ry.suitbRftPd抉dprovidestraceabi1.itytonationa1.andinternationa1.standards.Thetracerso1.utionsha1.1.behomogeneousandstab1.e.忡ein:即姗闸布SH电伸JrtiBfiq杯M联PJfiMPft>a1.1.WiM四至电嗝抨幅沿fMhtrationcanhebetween0,05Bqg-and1Bqg-.用并H姗1.ndedin忠嗝鸣卿龈飘市曲丽战枷加的球肝故抑枫喇胎曲盟福觇肾<»tin&butanaccountneedstobetakenofprogenyradionuc1.ideingrowth.Performingab1.ankana1.ysiswithtracerisapotentia1.waytoidentifyanypresenceofthoriumisotopeana1.ytesinthetracer.5.3 EquipmentUsua1.1.aboratoryequipmentand,inparticu1.ar,thefo1.1.owing.53.1SemWPhaUctOrsjethwbttiuo<taatat也到rcovbiN,higherdetechmuww)itat<0ttmtB1.ution)temperatureisrecommended.Fo1.1.owthemanufacturersinstructions.F°r视的啊聃部网heion榔部融CgMgThi和心叫gft1.喃nt1.yde脚幽wconductivityofthesi11con,proportiona1.totheenergyoftheincominga1.phapartic1.e.ToachieveWe1.rreso1.vedspectra,thedetectionsystemneedstobemaintainedatapressure<1Pa.Reso1.utioncanbeRHP1.f三MiY栅种雌鳏咻VCen眠rcas曲M<1.fiWnttime.However.ithastobe8dsionPi快tk胎Iefortheaccuratetransferof(e.g.1001.)229Thtracerso1.utionwithatota1.5.3.3Ba1.ancecapab1.eofachieving±0,1mgprecision.6 Samp1.ing,hand1.ingandstorage6.1 Samp1.ingConditionsofsamp1.ingsha1.1.conformtoISO56671.tttnWi)w¢pivroreitfsb1.>wriW4iJftA-3.es3riwrttep1.Wk<i(16Ujft11SW!W16Se1.eachingofthoriumfromtheso1.idcomponentofthesamp1.e.1.VgeifHJrtafPth'A,¾naged1.Jft¾J-receivearepresentativesamp1.e,unmodifiedduringtransportorAnnexB(informative)Preparationofthesourcebye1.ectrodeposition8.1 Princip1.eADCpowersupp1.yisusedtoapp1.ydifferentvo1.tagesbetweentwoe1.ectrodes,resu1.tinginthereductiontifhoiTOrtnbniodpt>srt)<rfedacthc1.ediydmtyte.f5hHireductionthattakesp1.aceatthecathode1.eadsto8.2 ReagentsUn1.essotherwisestated,useon1.yreagentsofrecognizedana1.ytica1.gradeanddisti1.1.edordeminera1.izedwaterorwaterofequiva1.entpurity.8.2.1 Nitricacidso1.ution,WHNo3=65%massfraction.8.2.2 Sodiumsu1.fateso1.ution,CNa2s04=0,3rno1.1.-.8.2.3 Su1.furicacidso1.ution,vvm2SO4=95%to97%massfraction.8.2.4 Th>rno1.b1.ue,0.4g1.-.8.2.5 Ammoniaso1.ution,PNH4OH=250g1.-.8.2.6 Su1.furicacidso1.ution,p112S(M=10g1.-.8.2.7 Ammoniaso1.ution,pH40H三Ig1.-.佳>8hcDioiddIWaterJnq沿coMpBito科VhIISOy6ib1.hH;ChCn1.iCa1.orradioactiveimpurities8.3 EquipmentThee1.ectrodepositionapparatusisgenera1.1.ycomposedofthefo1.1.owingcomponents.8.3.1 G1.ass,po1.ytetraf1.uoroethy1.ene(PTFE),orpo1.yethy1.enee1.ectrodepositionce1.1.8.3.2 P1.atinumwire(anode).8.3.3 Stain1.essstee1.disk(cathode)withadiameteradaptedtothee1.ectrodepositionce1.1.8.3.4 DCpowersupp1.y.8.3.5 Hotp1.ate.8.3.6 Petridish.8.4 Procedure8.4.1 Genera1.ThisDrocedureisbasedonReference13andASTMC1284(i.8.4.2 Assemb1.yofthee1.ectrodeposittonce1.1.ThisprocedurereferstoUe1.e0depositionapparatusdesignedfordepositsonsma1.1.diameter9f1.11idjft1.dfct(rodtjMMftW)i)j<(khfbitbhftywveappar3tuiaify1.ktf1.'ttfrmationonthereverseP1.acethec1.eananddegreasedstain1.ess-stee1.disk(B.3.3)inthecapassemb1.y.Screwthece1.1.(B.3.1)w