PD CEN TR 103772023.docx

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1、PDCEN/TR10377:2023Guide1.inesforthepreparationofstandardroutinemethodswithwave1.ength-dispersiveX-rayf1.uorescencespectrometrybsi.Nationa1.forewordThisPub1.ishedDocumentistheUKimp1.ementationofCEN/TR10377:2023.TheUKparticipationinitspreparationwasentrustedtoTechnica1.CommitteeISE102rMethodsofChemica

2、1.Ana1.ysisforIronandStee1.1.jaV9forganizitt)roiprnngf5nthiscommitteecanbeobtainedon-49Contractua1.and1.ega1.considerationsThispub1.icationhasbeenpreparedingoodfaith,howevernoimp1.ied)bemade,andnoUndertaking1.1.abi1.ityis埠网闻岫施Hnwrtw%dfwwHfiswa碑钟确*四防Wmbereasonab1.enessofthispubfication,11andanysuchre

3、sponsibi1.ityandMm1JtybiiexpoMyrtiwUediedtoahdfttteusmbfcdbythe1.aw.recipientsownrisk.Thetoitsisofthisconsiderrqsectrccpicntuseadvscdub1.ication.scekingprpfessina1.udancewithhrspuDcatonisnotintendedcoconstituteaContract.USe纤are酣飒ns4te00MwtWdupp1.ton1.od.asaBritishStandard.ThebyBSI1.imited名械加Wb1g的564

4、躯ndardDnStitUtiOn2023ICS77.040.30Comp1.iancewithaPub1.ishedDocumentcannotconferimmunityfrom1.ega1.ob1.igations.ThisPub1.ishedDocumentwaspub1.ishedundertheauthorityoftheStandardsPo1.icyandStrategjfCommitteeon30June2023.AmendmentS/corrigendaissuedsincepub1.icationTechnischerreportJune2023SupersedesCR1

5、0299:1998Eng1.ishVersionspectrometryThisTcchnica1.ReportwasapprovedbyCENon12June2023.IthasbeendrawnupbytheTechnica1.CommitteeCEN/TC459/SCCENmembersarcthenationa1.standardsbodiesofAustria,Be1.gium,Bu1.garia,Croatia,Cyprus,CzechRepub1.icDenmarkEstonia,UnitedKingdom.EUROPEANMMIEEFORSTANDARDIZATIONPDC秘翻

6、断用砌施3ECEN*CENE1.ECManagementCentre：RuedeIaScience23.B-1040Brusse1.s02023CEN1.1.rightsofexp1.oitationinanyformandbyan)meansreservedTechnica1.reportRAPPORTTECHNIQUE77.04030Guide1.inesforthepreparationofstandardroutinemethodswithwave1.ength-dispersiveX-rayf1.uorescence2.Fin1.and,France,Germany,Greece.1

7、1.unAry,Icehnd.Irdnnd.Ita1.y.I.tvinvUthiiania.1.uxembourgMa1.u.Ncthcrhndx,Norway,Po1.and.Portuga1.Repuh1.icofNorthMacedonia.Rnanh.Serbia.S1.ovakia,S1.ovenia.Spuin1.Sweden.Switzer1.and,TiirkiycandBCoMrT忘E1.1.ROFtENDENORMAI.SAKXCuropaiSCHCSKOMrTEEFORM)RMUNGwor1.dwideforCENat1.ru1.Members，ContentsEuro

8、peanforewordItrodiict1.onNormativereferencesTermsanddenitionsIMMPrincip1.e.123456.7.8955.5.5.5.5.s.5.5.InstrumentsGenera1.TubesVacuumsystemSamp1.espinnerFi1.tersCo1.1.iinatorsMaMaaaMMMM77.17.27.37.488.18.28.38.48.58.68.78.88.91010.110.210.310.4Crysta1.sDetectors1010101011Sequentia1.-simu1.taneousInS

9、trUmentSSan】P1.ingandSamP1.ePreParat1.onE、a1.Uat1.OnkcChocis1Deadtimecorecton13Backgroundcorrection131.IneInte1.eference,COrreCtIOnmode1.s13Inter-c1.ementeffects,correctionmode1.s.1411tjrato11Stratejy(1.na1.aaWWMMMMMa01)t11z112Se1.ectingtheoptimumconditionsfordetectorsSe1.ectingtheoptimumtubevo1.tag

10、eandcurrentSe1.ectingtheminimummeasuringtimes.Se1.ectingtheca1.ibrationsamp1.esSe1.eCtIngthereca1.ibrationsan】P1.eSMeasuringofca1.ibrationSamP1.CSRegressionca1.cu1.ationsVa1.idationofmethod(truenessandprecision)17Performancecriteria(CCra1.aMMMMCheckingtheprecisionPerformancemonitoringMaintenanCe,17M

11、MMMMM(:Tocompensatefortheday-to-dayvariationsoftheinstrumentasetofrecahbrationsamp1.esismeasured；eitheronewitha1.owandonewithahighcontentforeache1.ement(twopontreca1.ibration)oronewithhighcontenton1.yfareachdement(one-pointreca1.ibration).Theintensitiesarccomparedtotheinitia1.intensitiesrecordedduri

12、ngtheca1.ibrationprocedureandHXrW1.ibratiOncocffidcntsarcca1.1.atcd.Ca1.ibration用手rantsarcnotchanged.backgroundequiva1.entconcentrationBECquantityofana1.ytewhich,whensubjectedtoexcitation,providesanetintensityequa1.tothespectra1.background3.41.imitofdetection1.ODminimumcontentatwhichthesigna1.genera

13、tedbyagivene1.ementcanbepositive1.yrecognisedaboveanybackgroundsigna1.svrithaspecifieddegreeofcertainty3.51.ower1.imitofdetection1.1.Dminimumcontentatwhichthesigna1.generatedbyagivene1.ementcanbepositive1.yrecognisedaboveanybackgroundsigna1.swithaspecifieddegreeofcertaintyNote1toentry:Therehtcdca1.c

14、u1.ationsareon1.yonthecountingIerror3.71.imitofquantification1.OQsma1.1.estcontentthatcanbedeterminedwithaspecifieddegreeofcertainty3.8repeatabi1.ityconditionsconditionswhereindependenttestresu1.tsareobtainedwiththesamemethodonidentica1.testitemsinthesame1.aboratorybythesameoperatorusingthesameequip

15、mentwithinshortinterva1.softimeSOURCE:ISO5725-1:19943.9reproducibi1.ityconditionsconditionswheretestresu1.tsareobtainedwiththesamemethodonidentica1.testitemsindifferent1.aboratorieswithdifferentoperatorsusingdifferentequipmentSOURCE:ISO5725-1.:1994|3.10accuracyc1.osenessofagreementbetweentestresu1.t

16、andacceptedreferenceva1.ueNote1toentry:Thetermaccuracy,whenapp1.iedtoasetoftestresu1.ts,invo1.vesacombinationofrandomcomponentsandacommonsystematicerrororbiascomponent.OURCE:ISO5725-1.:1994|truenessc1.osenessofagreementbetweentheaverageva1.ueobtainedfroma1.argeseriesoftestresu1.tsandanacceptedrefere

17、nceva1.ueNote1toentry：Themeasureoftnenessisusua1.1.yexpressedIntermsofbias.Note2toentry:Truencx*;hahcenreferredtoasaccuracyofthemean*.Thisuxcisnotrecommended.OURCE:ISO5725-1:1994)sensitivity,Sdifferenceinintensitiesbetweenasamp1.ewithahighcontentandonewitha1.owcontentdividedbythedifferenceincontentN

18、ote1toentry:Sensitivityisexpressedascountspcrsecondpcrpercent.4Princip1.eThesamp1.eispreparedtoac1.eanuniformsurfaceandthenirradiatedbyanX-raybeamOfhighenergy.ThesecondaryX-raysproducedaredispersedbymeansofcrysta1.sandtheintensitiesaremeasuredbydetectorsatse1.ectedcharacteristicwave1.engths.Themeasu

19、ringtimeissettoreachbe1.owaspecifiedstatistica1.countingerror.Contentsofthee1.ementsareca1.cu1.atedbyre1.atingthemeasuredintensitiesoftestsamp1.estoca1.ibrationcurvesestab1.ishedwithcertifiedreferencemateria1.s(CRMs)andreferencemateria1.s(RMs).5Instruments5.1 Genera1.Theprincip1.eoftwodifferentconce

20、ptsofX-rayI1.uorcscencespectrometerisshowninFigures1andSamp1.eSpinnerDetectorTubeCrysta1.Primaryco1.1.imatorsecondary嘲Spectrometergeometryofsequentia1.instrumentsortheX-raytubeused.Theuseofacce1.erationvo1.tagesabove60kVison1.yofadvantageinafewcasese.g.fordeterminingthetracee1.ementsinheavymateria1.

21、s.Theradiationfromthesamp1.eisemitteduniform1.yina1.1.directions.Thesamp1.evo1.ume,fromwhereDuringthemeasurement,thesamp1.eismovedtothespectrometerchamber.Itisimportantthat1.ighte1.ements(Z20)aremeasuredinvacuumastheabsorption1.ossesinairaresohighthatameaningfu1.measurementisno1.ongerpossib1.e.Forth

22、eana1.ysisofmeta1.a1.1.oys,itisrecommendedtomeasurea1.1.Mostinstrumentsareequippedwithasamp1.espinnerinordertoavoideffectsfromgrindingstriations.Ifthatisnotthecaseritissuggestedthatthesamp1.esareorientedinsuchawaythatthere1.ationbetweentheX-raybeamandthegrindingstriationsarea1.waysthesamefrommeasure

23、ment里5盅U恪IWn1.Iftheanodeconsistsofane1.ementidentica1.tooneofthee1.ementstobedeterminedafi1.terhastobeinsertedinfrontoftheexitwindowonthetubeinordertoe1.iminatethecharacteristic1.inesfromthetube.Theefficiencyofafi1.terdependsonthemateria1.andthickness.fi1.termadeOftitaniumora1.uminiumisoftenusedtoe1

24、iminatethecharacteristic1.inesfromachromiumtube.Whenafi1.terisused,thesensitivityofthee1.ementtobedeterminedWn1.decreasesevera1.times.Sometimesafi1.tercou1.dbeusedtoincreasethepeaktobackgroundratioforheavye1.ementsin1.owconcentrations.ManynstCtffiFSsuppIiedwithafi1.terchangercontainingfi1.tersofdif

25、ferentmateria1.sandthicknesses.Inthef1.atcrysta1.system(Figure1)on1.yaportionofthesecondaryradiationisse1.ectedbyaprimaryco1.1.imatorandthepara1.1.e1.beamfa1.1.sintothep1.anesurfaceofthecrysta1.Thereso1.utionofthespectrometerisaffectednoton1.ybythecrysta1.sused,buta1.sobytheco1.1.imationoftheradiati

26、on.Thefinertheco1.1.imatorse1.ected,thebetteristhereso1.ution,hutthe1.oweristheintensitymeasured.Mostsequentia1.spectrometersofthistypearesupp1.iedwithat1.easttwoco1.1.imators,coarseandfine.Inacurvedcrysta1.geometry(Figure2)theuseofco1.1.imatorsisnotnecessarysincethe1.ightisfocusedS1.,7the,Jtfsbyas1

27、itsystem.Inordertoiso1.ateindividua1.characteristic1.inesemittedbythesamp1.e,1.argesing1.ecrysta1.sareusedasdispersionmedia.Tocovertheusua1.wave1.engthrange(0,2Ato15A),crysta1.switndifferentInterp1.anarspacing(d-va1.ue)areused.Crysta1.1.atticep1.anes2(1va1.uesForthemeasurementoftheKa-Iinesof5.8DMtt

28、MQyecrystaI-Variab1.eE1.ementsZVTTThese1.ectedf1.uorescentradiationintensityinthespectrometerisrecordedbymeansOfappropriatecounters(f1.owcounter,gascounter,andscinti1.1.ationcounter).sthesensitivityofthevariouscountersisafunctionoftheenergyoftheradiationtobemeasured,itisimportantthatthemostsuitab1.e

29、counterisusedfortheparticu1.are1.ement1.ineinsimu1.taneousapparatus.Withsequentia1.apparatus,f1.owandscinti1.1.ationcountersaregenera1.1.yusedatthesametimeandareconnectedinseries(tandemconnection).Fore1.ementswithatomicnumber1.essthan25thef1.owcounterisusedandforatomicnumberhigherthan30thescinti1.1.

30、ationcounterisused.Foratomicnumbersbetween25and30bothcountersareusedintandem,ifpossib1.e.Insimu1.taneousinstrumentsgascountersfi1.1.edwithkryptonorxenonareoftenusedforatomicnumbersbetween20and40.Counterscanrecordon1.ya1.imitednumberofpu1.sesperunitoftime,becausethemeasuringprocessforeachpu1.serequir

31、esafixedamountoftimewhichisintheorderof1sto100s.Otherpu1.sescannotbede1.ectedinthistime.Itisdefinedasdeadtimer.Therefore,itisimportantthatcareistakentoensurethatthemaximumpre-setpu1.serateisnotexceeded.Thisispossib1.e,forexamp1.e,byconnectingattenuationfi1.ters(insimu1.taneousequipment)ordecreasingt

32、hetubecurrent.Otherwise,therewi1.1.beno1.inearitybetweentheintensityoftheX-rayradiationandthepu1.seratemeasured.Thedeadtimeofthecounterscanhaveaneffectfromapu1.serateofapproximate1.y10；pu1.sespersecond.However,higherpu1.seratescanbeusediftheinstrumentissupp1.iedwithane1.ectronicdeadtimecorrector.The

33、countersusedregisterpu1.sesatdifferentintensitiesasafunctionoftheenergyoftheX-ray瑞池假麻e靴曲渤蒯觎撕r愉怫R哪沿快停俯居4f川加曲用侬瞄睢怫陋picTheX-rayf1.uorescenceapparatuscanbesubdividedintotwocategories：sequentia1.andsimu1.taneous.Simu1.taneousapparatushassevera1.fixedgoniometers(channe1.s)arrangedaroundthesamp1.esothatthe

34、individua1.c1.ementintensitiesaremeasuredatthesametimewiththesameexcitationconditions.Eachchanne1.isoptimizedforeache1.ement.Sequentia1.instrumentsofferthef1.exibi1.itytooptimizethemeasuringconditionsindependent1.yforeachofthese1.ectede1.ementsandthecorrespondingbackground.Thegoniometercanhesettoapre-definedang1.e(50to150o)andtheexcitationconditionscanbeoptimizedseparate1.yforeache1.ement.Simu1.taneousapparatusisoftenusedinaPr(X1.UetiOnenvironm