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1、Designation:E2626?081StardGuidefSpectrometricAnalysisofReactiveRefractyMetals1ThisstardisissuedunderthefixeddesignationE2626thenumberimmediatelyfollowingthedesignationindicatestheyearofiginaladoptioninthecaseofrevisionth

2、eyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.1NOTE—EditialcrectionsweremadethroughoutinOctober2009.1.Scope1.1Thisguidecove

3、rsavarietyofanalyticaltechniquesthathaveproventobeacceptableftheanalysisofthereactiverefractymetalstitaniumzirconiumniobiumhafniumtantalummolybdenumtungstenvanadium.1.2TheprinciplestechniquesinthisguidecanbeusedbyISO1702

4、5compliantlabatiesthatneedtoimplementotherperfmancebasedtestmethodsneedtodocumentvalidateextensionsofstardtestmethodsnonstardtestmethods.1.3ThevaluesstatedinSIunitsaretoberegardedasstard.Nootherunitsofmeasurementareinclu

5、dedinthisstard.1.4Thisstarddoesnotpurpttoaddressallofthesafetyconcernsifanyassociatedwithitsuse.Itistheresponsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthpracticesdeterminetheapplicabilityofregulatylimit

6、ationspritouse.2.ReferencedDocuments2.1ASTMStards:2D1193SpecificationfReagentWaterE50PracticesfApparatusReagentsSafetyConsiderationsfChemicalAnalysisofMetalsesRelatedMaterialsE135TerminologyRelatingtoAnalyticalChemistryf

7、MetalsesRelatedMaterialsE539TestMethodfAnalysisofTitaniumAlloysbyXRayFluescenceSpectrometryE882GuidefAccountabilityQualityControlintheChemicalAnalysisLabatyE1097GuidefDeterminationofVariousElementsbyDirectCurrentPlasmaAt

8、omicEmissionSpectrometryE1184PracticefDeterminationofElementsbyGraphiteFurnaceAtomicAbsptionSpectrometryE1479PracticefDescribingSpecifyingInductivelyCoupledPlasmaAtomicEmissionSpectrometersE1552TestMethodfDeterminingHafn

9、iuminZirconiumZirconiumAlloysByDirectCurrentPlasma—AtomicEmissionSpectrometryE1601PracticefConductinganInterlabatyStudytoEvaluatethePerfmanceofanAnalyticalMethodE1621GuidefXRayEmissionSpectrometricAnalysisE1770PracticefO

10、ptimizationofElectrothermalAtomicAbsptionSpectrometricEquipmentE2371TestMethodfAnalysisofTitaniumTitaniumAlloysbyAtomicEmissionPlasmaSpectrometryE2437PracticefDesigningValidatingPerfmanceBasedTestMethodsftheAnalysisofMet

11、alsesRelatedMaterialsE2438PracticefImplementingStardPerfmanceBasedTestMethodsftheAnalysisofMetalsesRelatedMaterials2.2ISOStards:3ISO17025GeneralRequirementsftheCompetenceofTestingCalibrationLabatiesISOGuide32Calibrationi

12、nAnalyticalChemistryUseofCertifiedReferenceMaterials3.Terminology3.1Definitions—FdefinitionsoftermsusedinthisguiderefertoTerminologyE135.3.2DefinitionsofTermsSpecifictoThisStard:3.2.1reactivemetaln—ametalsuchastitaniumzi

13、rconiumthatreadilyreactswiththeenvironment.Ithasastrongaffinityfoxygennitrogenfmsverystablecompoundsthatpassivateinthinlayers.Whenthereactivecoatingisdamageditselfhealsbyreactionwiththeatmosphere.1Thisguideisunderthejuri

14、sdictionofASTMCommitteeE01onAnalyticalChemistryfMetalsesRelatedMaterialsisthedirectresponsibilityofSubcommitteeE01.06onTiZrWMoTaNbHfRe.CurrenteditionapprovedJune152008.PublishedJuly2008.DOI:10.1520E262608E01.2Freferenced

15、ASTMstardsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummarypageontheASTMwebsite.3AvailablefromAmericanNationalStardsInstitute(ANSI)25W.43rdSt

16、.4thFloNewYkNY10036:www.ansi.g.Copyright?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates1solution.DCPAESisunabletoachievethenecessarydetectionlimitsfelementssuchasboncadmiuminazirconium

17、sampleatthelevelsrequiredbymostspecifications.TestMethodE1552givesdetailsftheanalysisofhafniuminzirconiumzirconiumalloysusingtheDCPAEStechniqueTestMethodE2371describestheanalysisoftitaniumtitaniumalloys.GuideE1097discuss

18、esthetechniqueinmegeneralterms.6.2.3InductivelyCoupledPlasmaAtomicEmissionSpectrometry(ICPAES)—PracticeE1479describesthecomponentsofanICPAESthatarebasictoitsoperationtothequalityofitsperfmance.ICPAESICPMSrepresenttheinst

19、rumentsmostcommonlyusedftheanalysisofreactiverefractymetals.Thesesolutionbasedtechniquescomplementeachothertoprovideareliablemeansofanalysisofreactiverefractymetals.Caremustalwaysbetakentoavoidseriousspectralinterference

20、sduetothelinerichnatureofreactiverefractymetals.Theadventofsolidstatedetectshasprovidedmuchflexibilityintheionofwavelengths.Section8.3givesguidanceinwavelengthselection.TestMethodE2371givesdetailsftheanalysisoftitaniumti

21、taniumalloyswhilePracticeE1479discussesthetechniquesinmegeneralterms.6.2.4InductivelyCoupledPlasmaMassSpectrometry(ICPMS)—ThistechniqueisdistinguishedfromICPAESbythedetectionsystemusedtoanalyzethespeciesexcitedbyaplasma.

22、Amassspectrometerisutilizedinthiscase.MuchoftheinfmationinPracticeE1479isapplicabletoICPMS.Thistechniqueiscapableofanalyzingthemajityofthemetalelementsnecessarytosatisfythematerialspecificationsfreactiverefractymetals.Th

23、ehighsensitivityofICPMSmayrequiresignificantdilutionofthesamplesolutionindertoanalyzeelementsatconcentrationsabove0.1%bymass.6.3GlowDisgeSpectrometry—Theissuementionedaboveinsecuringsolidreferencematerialsisaconcernthatm

24、ustbeaddressedwiththistechnique.GlowDisgeinstrumentationisnmallydividedintotwotypesofinstrumentation.6.3.1GlowDisgeMassSpectrometry(GDMS)—Inthistechniquethesurfaceofasolidsampleissputteredwithargongas.Ionizedspeciesareth

25、ensubjectedtohighresolutionmassspectrometricanalysis.Thisresultsinthehighsensitivityanalysisofallelementsintheperiodictableexcepthydrogenatthetracelevel.GDMShasbeenusedfthemultielementsurveyanalysisfthesemetalsincludedin

26、thescopeofthisguide.Caremustbetakenintheinterpretationoftheresultshoweverduetothenonhomogeneityofthesamplesurface.Reactiverefractymetalstypicallyexhibitarelativelylargegrainsizecomparedtothesmallareasampledbytheconventio

27、nal“pin”sampleusedbytheGDMS.Itisalsopossibletosampleaflatsurfacewhichmayhelpalleviatethegrainsizeproblem.Oneshouldkeepinmindthatonlyafewhundredmicrogramsofmaterialaresampledwhichunderscestheimptanceofhomogeneity.Duetothe

28、highcostcomplexityoftheinstrumentationGDMSisfoundinveryfewcaptivelabaties.Commercialanalysisisavailablethroughalimitednumberoflabaties.6.3.2GlowDisgeAtomicEmissionSpectrometry(GDAES)—Theglowdisgeexcitationsourceisadevice

29、thatproducesluminousplasma.Solidsamplesaresputteredusingthelowpressureargonplasma.Theargonionsetchatomssmallatomicclustersfromthesamplesurfacemakingthemavailablefdissociationexcitationintheplasma.Metallurgicalhistyisredu

30、cedbecausesamplingexcitationtakeplaceinseparatelocations.Calibrationrequirestheuseofreferencematerialswhereavailableitispossibletodeterminethealloyingminconstituentssimultaneously.6.4XrayEmissionSpectrometry(XRF)—SeeGuid

31、eE1621fdetailsoftheinstrumentation.Againtherequirementfasetofhomogeneoussolidreferencematerialslimitstheuseofthistechnique.Thelowdetectionlimitrequirementsfmanyoftherequiredelementsinthesematerialswillnotbeachievedbythis

32、technique.TheanalysisofironchromiumnickeltininzirconiumalloyszirconiuminhafniumhavebeendemonstratedtowkwellbyXray.TestMethodE539GuideE1621givevaluableguidance.7.Calibration7.1Setuptheinstrumentfcalibrationasrecommendedby

33、themanufacturer.ThepublicationslistedinSection2aswellasintextstheanalyticalliteratureotherstardsganizationswillalsoprovidevaluableguidance.8.Interferences8.1GuideE1097PracticeE1184PracticeE1479GuideE1621PracticeE1770desc

34、ribesomeoftheinterferencesencounteredduringanalysis.Theuserisresponsiblefensuringtheabsenceofcompensatingfinterferencesthatmaybiastestresultsobtainedusingtheirstardoperatingprocedures.8.2Thephysicalinterferencesresulting

35、fromvariationsinsamplecalibrationsolutionaerosoltransptratesmaybecompensatedfbytheuseofaninternalstardinsometechniques.8.3Table1listswavelengthsthathavebeenusedtoanalyzethelistedelementsinthegivenmetalsaresuggestedftheus

36、erofatomicemissionspectrometers.Duetotheresolutionofindividualinstrumentsconfirmationofthesesuggestionswillberequired.Dependingonthespecificspectrometerotherwavelengthswillbefoundtobeapplicable.9.ReferenceMaterials9.1Sta

37、rdReferenceMaterial(SRM)Zircaloy4SRM360bisavailablefromNationalInstituteofStardsTechnology4othercommercialsuppliers.ThreezirconiummaterialsknownasZr20Zr30Zr40areavailablefromseveralcommercialsuppliers.Duetononhomogeneity

38、theyarerecommendedfXrayfluescenceuseonly.BCR098isaZircaloy4alloythatiscertifiedfchromiumhafniumirontin.4AvailablefromNationalInstituteofStardsTechnology(NIST)100BureauDr.Stop1070GaithersburgMD208991070:www.nist.gov.E2626

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