ASTME415-2008

StandardTestMethodfor

AtomicEmissionVacuumSpectrometricAnalysisofCarbonandLow-AlloySteel1ThisstandardisissuedunderthefixeddesignationE415;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval.

1.Scope

1.1Thistestmethodcoversthesimultaneousdeterminationof20alloyingandresidualelementsincarbonandlow-alloysteelsintheconcentrationrangesshown(Note1).

ElementAluminumArsenicBoronCalciumCarbonChromiumCobaltCopperManganeseMolybdenumNickelNiobiumNitrogen

PhosphorousSiliconSulfurTin

TitaniumVanadiumZirconium

AConcentrationRange,%

QuantitativeRange,%BApplicableRange,%A0

0000000000000000000totototototototototototototototototototo0.0750.10.0070.0031.12.250.180.52.00.65.00.0850.0150.0851.150.0550.0450.20.30.05

0.02to0.0750.05to0.10.002to0.0070.001to0.0030.08to1.10.02to2.250.008to0.180.04to0.50.10to2.00.03to0.60.02to5.00.02to0.0850.004to0.0150.02to0.0850.07to1.150.01to0.0550.01to0.0450.004to0.20.004to0.30.02to0.05

1.3Thistestmethodcoverstheroutinecontrolanalysisinironandsteelmakingoperationsandtheanalysisofprocessedmaterial.Itisdesignedforchill-cast,rolled,andforgedspecimens.Betterperformanceisexpectedwhenreferencematerialsandspecimensareofsimilarmetallurgicalconditionandcomposition.However,itisnotrequiredforallapplica-tionsofthisstandard.

1.4Thisstandarddoesnotpurporttoaddressallofthesafetyconcerns,ifany,associatedwithitsuse.Itistheresponsibilityoftheuserofthisstandardtoestablishappro-priatesafetyandhealthpracticesanddeterminetheapplica-bilityofregulatorylimitationspriortouse.

2.ReferencedDocuments2.1ASTMStandards:3E135TerminologyRelatingtoAnalyticalChemistryforMetals,Ores,andRelatedMaterials

E158PracticeforFundamentalCalculationstoConvertIntensitiesintoConcentrationsinOpticalEmissionSpec-trochemicalAnalysis4E305PracticeforEstablishingandControllingAtomicEmissionSpectrochemicalAnalyticalCurves

E350TestMethodsforChemicalAnalysisofCarbonSteel,Low-AlloySteel,SiliconElectricalSteel,IngotIron,andWroughtIron

E406PracticeforUsingControlledAtmospheresinSpec-trochemicalAnalysis

E1019TestMethodsforDeterminationofCarbon,Sulfur,Nitrogen,andOxygeninSteelandinIron,Nickel,andCobaltAlloys

E1329PracticeforVerificationandUseofControlChartsinSpectrochemicalAnalysis

E1601PracticeforConductinganInterlaboratoryStudytoEvaluatethePerformanceofanAnalyticalMethod

E1763GuideforInterpretationandUseofResultsfromInterlaboratoryTestingofChemicalAnalysisMethodsE1806PracticeforSamplingSteelandIronforDetermi-nationofChemicalComposition

ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandardsvolumeinformation,refertothestandard’sDocumentSummarypageontheASTMwebsite.4Withdrawn.

3ApplicablerangeinaccordancewithGuideE1763forresultsreportedinaccordancewithPracticeE1950.BQuantitativerangeinaccordancewithPracticeE1601.

NOTE1—Theconcentrationrangesoftheelementslistedhavebeenestablishedthroughcooperativetesting2ofreferencematerials.Included,inadditiontotheoriginaldataofTestMethodE415–71,aredatafromcooperativetestingofabroaderrangeofreferencematerialstoexpandtheelementconcentrationranges.

1.2Thistestmethodcoversanalysisofspecimenshavingadiameteradequatetooverlaptheboreofthesparkstandopening(toeffectanargonseal).Thespecimenthicknesscanvarysignificantlyaccordingtothedesignofthespectrometerstand,butathicknessbetween10mmand38mmhasbeenfoundtobemostpractical.

ThistestmethodisunderthejurisdictionofASTMCommitteeE01onAnalyticalChemistryforMetals,OresandRelatedMaterialsandisthedirectresponsibilityofSubcommitteeE01.01onIron,Steel,andFerroalloys.

CurrenteditionapprovedJune1,2008.PublishedJuly2008.Originallyapprovedin1971.Lastpreviouseditionapprovedin2005asE415–99a(2005).2SupportingdatahavebeenfiledatASTMInternationalHeadquartersandmaybeobtainedbyrequestingResearchReportRR:E2-1004.

1Copyright©ASTMInternational,100BarrHarborDrive,POBoxC700,WestConshohocken,PA19428-2959,UnitedStates.

1

E415–08

E1950PracticeforReportingResultsfromMethodsofChemicalAnalysis

3.Terminology

3.1Fordefinitionsoftermsusedinthistestmethod,refertoTerminologyE135.

4.SummaryofTestMethod

4.1Acapacitordischargeisproducedbetweentheflat,groundsurfaceofthediskspecimenandaconicallyshapedelectrode.Thedischargeisterminatedatapredeterminedintensitytimeintegralofaselectedironline,oratapredeter-minedtime,andtherelativeradiantenergiesoftheanalyticallinesarerecorded.Themostsensitivelinesofarsenic,boron,carbon,nitrogen,phosphorus,sulfur,andtinlieinthevacuumultravioletregion.Theabsorptionoftheradiationbyairinthisregionisovercomebyevacuatingthespectrometerandflush-ingthesparkchamberwithargon.

5.SignificanceandUse

5.1Thistestmethodforthespectrometricanalysisofmetalsandalloysisprimarilyintendedtotestsuchmaterialsforcompliancewithcompositionalspecifications.Itisassumedthatallwhousethistestmethodwillbeanalystscapableofperformingcommonlaboratoryproceduresskillfullyandsafely.Itisexpectedthatworkwillbeperformedinaproperlyequippedlaboratory.

6.Apparatus

6.1SamplingDevices:

6.1.1RefertoPracticeE1806fordevicesandpracticestosampleliquidandsolidironandsteel.

6.2ExcitationSource,capableofprovidingelectricalpa-rameterstosparkasample.See11.1fordetails.

6.3SparkChamber,automaticallyflushedwithargon.Thesparkchambershallbemounteddirectlyonthespectrometerandshallbeprovidedwithasparkstandtoholdaflatspecimenandalowercounterelectrodeofrodform.

NOTE2—Followthemanufacturer’srecommendationsforcleaningtheexcitationchamber(duringcontinuousoperation,thistypicallyshouldbedoneevery24h).Followthemanufacturer’srecommendationsforcleaningtheentrancelensorwindow(verifierdataorotherreferencesampleintensitydatacantypicallyindicatewhenthisisnecessary).

orindirectly,andthenecessaryswitchingarrangementstoprovidethedesiredsequenceofoperation.

6.6VacuumPump,capableofmaintainingavacuumof3.33Pa(25µmHg)orless.

NOTE3—Apumpwithadisplacementofatleast0.23m3/min(8ft/min)isusuallyadequate.

36.7GasSystem,consistingofanargonsupplywithpressureandflowregulation.Automaticsequencingshallbeprovidedtoactuatetheflowatagivenrateforaspecifictimeinterval.Theflowratemaybemanuallyorautomaticallycontrolled.TheargonsystemshallbeinaccordancewithPracticeE406.7.ReagentsandMaterials

7.1CounterElectrodes—Thecounterelectrodescanbesilverorthoriatedtungstenrods,orothermaterial,provideditcanbeshownexperimentallythatequivalentprecisionandbiasisobtained.Therodscanvaryindiameterfrom1.5mmto6.5mm(dependingontheinstrumentmanufacturer)andtypicallyaremachinedtoa90°or120°angledtip.

NOTE4—Ablackdepositwillcollectonthetipoftheelectrode.Thisdepositshouldberemovedbetweenspecimens(typicallywithawirebrush).Ifnotremoved,itcanreducetheoverallintensityofthespectralradiationortransferslightamountsofcontaminationbetweenspecimens,orboth.Thenumberofacceptableexcitationsonanelectrodevariesfromoneinstrumenttoanother,andshouldbeestablishedineachlaboratory.Ithasbeenreportedthatthousandsofexcitationscanbeperformedonathoriatedtungstenelectrodebeforereplacementisnecessary.

7.2InertGas,Argon,inaccordancewithPracticeE406.8.ReferenceMaterials

8.1CertifiedReferenceMaterials(CRMs)—Theseareavail-ablefromtheNationalInstituteofStandardsandTechnology(NIST)andothersourcesandspanallorpartoftheconcen-trationrangeslistedin1.1.Theyareusedtocalibratethespectrometerfortheelementsofinterestortovalidatetheperformanceofthetestmethod.ItisnotrecommendedtouseCRMsasverifiersortoestablishtherepeatabilityofthechemicalmeasurementprocess.DifferencescanoccurbetweenCRMsandproductionsamplespreparedbythesamplingproceduresrecommendedinthistestmethod.Certainel-ement’s(forexample,sulfur)calibrationsmayneedtobecorrectedwithvaluesfromreferencematerialsmadebynormalproductionsamplingtechniquesandanalyzedbyTestMethodsE350andE1019.

NOTE5—CertifiedReferenceMaterialsmanufacturedbyNISTaretrademarkedwiththename,“StandardReferenceMaterials,SRMs.”

6.4Spectrometer,havingareciprocallineardispersionof0.60nm/mm,orbetter,inthefirstorderandafocallengthof0.75mto3m.Itsapproximaterangeshallbefrom120.0nmto400.0nm.Masksshallbeprovidedinthespectrometertoeliminatescatteredradiation.Thespectrometershallbepro-videdwithanairinletandavacuumoutlet.Thespectrometershallbeoperatedatavacuumof3.33Pa(25µmofmercury)orbelow.Theprimaryslitwidthcanrangefrom20µmto50µm.Secondaryslitwidthscanvary(normallybetween37µmand200µm)dependingontheelementwavelengthandpossibleinterferingwavelengths.

6.5MeasuringSystem,consistingofphotomultipliershav-ingindividualvoltageadjustments,capacitorsinwhichtheoutputofeachphotomultiplierisstored,avoltagemeasuringsystemtoregisterthevoltagesonthecapacitorseitherdirectly

2

8.2ReferenceMaterials(RMs)—Theseareavailablefrommultiplesuppliersorcanbedevelopedinhouse.RMsaretypicallyusedtocontrol(verifiers)anddriftcorrect(standar-dants)thespectrometer.Thesereferencematerialsshallbehomogenousandcontainappropriateconcentrationsofeachelementtobecontrolledordriftcorrected,orboth.

9.PreparationofSpecimensandReferenceMaterials9.1Thespecimensandreferencematerialsmustbepreparedinthesamemanner.Aspecimencutfromalargesamplesectionmustbeofsufficientsizeandthicknessforpreparation

E415–08

andtoproperlyfitthespectrometerstand.A10mmto38-mmthickspecimenisnormallymostpractical.

9.2Ensurethespecimensarefreefromvoidsandpitsintheregiontobeexcited(Note6).Initiallygrindthesurfacewitha50-gritto80-gritabrasivebeltordisc(wetordry).Performthefinalgrindwithadryabrasivebeltordisc.Afinerabrasivegrindingmedia(forexample,120-grit)maybeusedforthefinalgrind,butisnotessential(Note7).

NOTE6—Specimenporosityisundesirablebecauseitleadstotheimproper“diffuse-type”ratherthanthedesired“concentrated-type”dis-charge.Thespecimensurfaceshouldbekeptcleanbecausethespecimenistheelectronemitter,andelectronemissionisinhibitedbyoily,dirtysurfaces.

NOTE7—Referencematerialsandspecimensmustberefinisheddryonanabrasivebeltordiscbeforebeingre-excitedonthesamearea

TABLE1InternalStandardandAnalyticalLines

ElementAluminumArsenicBoronCalciumCarbonChromiumCobaltCopperIron(IS)ManganeseMolybdenum

Wavelength,nm

394.40308.22197.20193.76182.182.59396.85193.09298.92267.72345.35228.62327.40213.60271.44273.07293.31255.86379.83277.54386.41231.60227.02319.50149.26

Line

ClassificationAIIIIIIIIIIIIIIIIIIIIIIIIIIIIIIIIIIIIII

PossibleInterferenceBV,Mn,Mo,NiV,MnMo,WMn

S,Mn,MoW,Mn,CuNbAl

Mn,V,Ni,Nb,MoMn,Mo,WCr,MoNi,CrNbMo,Cr

Co

Cr,Mo,NiZrMn

Cu,V,Co,MnV,CrCo,TiNb,WMo,Al,V

Fe,Ti,Si,Mn,Cu,NiandnitrideformingelementssuchasTiMo

Mo,Cr,WFe,VMn

Mn,Mo,AlNbNb

Fe,Mo,Nb,NiMn,Ti,FeW

10.PreparationofApparatus

NOTE8—Theinstructionsgiveninthistestmethodapplytomostspectrometers;however,somesettingsandadjustmentsmayneedtobevaried,andadditionalpreparationoftheequipmentmayberequired.ItisnotwithinthescopeofanASTMtestmethodtoprescribetheminutedetailsoftheapparatuspreparation,whichmaydiffernotonlyforeachmanufacturer,butalsofordifferentequipmentfromthesamemanufac-turer.Foradescriptionofandfurtherdetailsofoperationofaparticularspectrometer,refertothemanufacturer’shandbook.

NickelNiobiumNitrogen

PhosphorusSiliconSulfurTin

TitaniumVanadiumZirconium

A10.1ProgramthespectrometertoaccommodatetheinternalstandardlinesandoneoftheanalyticallinesforeachelementlistedinTable1.Multiplelinesmaybeusedforagivenelement(forexample,nickel)dependingontheconcentrationrangeandtheindividualspectrometersoftware.

NOTE9—ThelineslistedinTable1haveprovensatisfactoryfortheelementsandconcentrationrangesdescribedinthescope.Otherinternalstandardandanalyticallines,suchasthoselistedinTable2,maybeusedprovidedthatitcanbeshownexperimentallythatequivalentprecisionandaccuracyareobtained.

178.29288.16251.61180.731.99337.28324.20310.23311.07343.82IIIIIIIIIIIIIIII

ThenumeralsIorIIinthelineclassificationcolumnindicatethatthelinehasbeenclassifiedinatermarrayanddefinitelyassignedtothenormalatom(I)ortothesinglyionizedatom(II).BInterferencesaredependentuponinstrumentdesign,spectrumlinechoices,andexcitationconditions,andthoselistedrequireconfirmationbaseduponspecimensselectedespeciallytodemonstratesuspectedinterferences.

10.2Testthepositioningofthespectrometerentranceslittoensurethatpeakradiationisenteringthespectrometercham-ber.Thisshallbedoneinitiallyandasoftenasnecessarytomaintainproperentranceslitalignment.Followthemanufac-turer’srecommendedprocedures.Thelaboratorywilldeter-minethefrequencyofpositioningthealignmentbasedoninstrumentperformance.

10.3Exitslitpositioningandalignmentisnormallyper-formedbythemanufactureratspectrometerassembly.Undernormalcircumstances,furtherexitslitalignmentisnotneces-sary(Note10).

NOTE10—Themannerandfrequencyofpositioningorcheckingthepositionoftheexitslitswilldependonfactorssuchas:thetypeofspectrometer,thevarietyofanalyticalproblemsencountered,andthefrequencyofuse.Eachlaboratoryshouldestablishasuitablecheckprocedureutilizingqualifiedserviceengineers.

TABLE2OtherAnalyticalLines

ElementArsenicCarbonCopper

Wavelength,nm

1.04165.81224.26324.75202.03281.62212.415

Line

ClassificationAIIIIIIIIIII

Ni

Mn,Nb

PossibleInterferenceBV,Cr

Molybdenum

Mn

Mo,Ni,V,Cu,Nb

Silicon

AThenumeralsIorIIinthelineclassificationcolumnindicatethatthelinehasbeenclassifiedinatermarrayanddefinitelyassignedtothenormalatom(I)ortothesinglyionizedatom(II).BInterferencesaredependentuponinstrumentdesign,dispersion,spectrumlinechoices,andexcitationconditions,andthoselistedrequireconfirmationbaseduponspecimensselectedespeciallytodemonstratesuspectedinterferences.

11.ExcitationandExposure

11.1ElectricalParameters(Note11):

11.1.1Excitationparametersarenormallyestablishedbythespectrometermanufacturer.Thefollowingrangesarehis-toricalguidelinesandnewerinstrumentsmayvaryfromthese.

3

Capacitance,µFInductance,µHResistance,VPotential,V

TriggeredCapacitorDischarge

10to1550to703to5

940to1000

E415–08

Current,A,r-f

Numberofdischarges

0.3to0.860

NOTE11—Whenparametervaluesareestablished,maintainthemcarefully.Thevariationofthepowersupplyvoltageshallnotexceed65%andpreferablyshouldbeheldwithin62%.

11.1.2InitiationCircuit—Theinitiatorcircuitparametersshallbeadequatetouniformlytriggerthecapacitordischarge.Thefollowingsettingsarehistoricalguidelinesandnewerinstrumentsmayvaryfromthese:

Capacitance,µFInductance,µHResistance,VPeakvoltage,V

0.0025residual2.518000

11.1.3OtherElectricalParameters—Excitationunits,onwhichthepreciseparametersgivenin11.1.1and11.1.2arenotavailable,maybeusedprovidedthatitcanbeshownexperi-mentallythatequivalentprecisionandaccuracyareobtained.11.2ExcitationConditions(Note12)—Thefollowingrangesarenormallyadequate:

Argonflushperiod,sPreburnperiod,sExposureperiod,sArgonflow(Note13)FlushPreburnExposure

5to155to203to30

ft3/h

5to455to455to30

2.5to252.5to252.5to15

L/min

NOTE12—Selectpreburnandexposureperiodsafterastudyofvola-tizationratesduringspecimenexcitations.Onceestablished,maintaintheparametersconsistently.

NOTE13—Ahigh-purityargonatmosphereisrequiredattheanalyticalgap.Moleculargasimpurities,nitrogen,oxygen,hydrocarbons,orwatervapor,eitherinthegassystemorfromimproperlypreparedspecimensshouldbeminimized.

requiredconcentrationrange.Exciteeachcalibrant,standar-dant,andverifiertwotofourtimesandusetheaveragevalue.Ifthespectrometersystemandsoftwarepermits,repeatwithdifferentrandomsequencesatleasttwotimes.Usingtheaveragesofthedataforeachpoint,determineanalyticalcurvesasdirectedinPracticesE158andE305.

12.2Standardization—Followingthemanufacturer’srec-ommendations,standardizeonaninitialsetuporanytimethatitisknownorsuspectedthatreadingshaveshifted.Makethenecessarycorrectionseitherbyadjustingthecontrolsonthereadoutorbyapplyingarithmeticcorrections.Standardizationwillbedoneanytimeverificationindicatesthatreadingshavegoneoutofstatisticalcontrol.

12.3Verification—Verifythattheinstrument’sstandardiza-tionisvalidimmediatelyaftereachstandardizationandasrequiredinaccordancewith12.3.2.

12.3.1AnalyzeverifiersinaccordancewithSection13.Ifresultsdonotfallwithinthecontrollimitsestablishedin12.4,runanotherstandardizationorinvestigatewhytheinstrumentmaybemalfunctioning.

12.3.2Eachlaboratoryshalldeterminethefrequencyofverificationnecessarybasedonstatisticalanalysis.Typicallyevery4hto8hispracticalandadequate.Iftheresultsarenotwithinthecontrollimitsestablishedin12.4,performastan-dardizationandrepeatverification.Repeatstandardizationasnecessarysoverificationsarewithincontrollimitsorinvesti-gatefurtherforinstrumentproblems.

12.4QualityControl—Establishcontrollimitsinaccor-dancewithMNL7A,5PracticeE1329,orotherequivalentqualitycontrolprocedure.

13.ExcitationandRadiationMeasurements

13.1Placethepreparedsurfaceofthespecimenontheexcitationstandsothatexcitationwillimpingeonalocationapproximately6mm(1⁄4in.)fromtheedgeofthespecimen.

NOTE15—Withcertainspectrometers,aproperlyexcitedspecimenusuallyexhibitsadarkringaroundthepittedsparkedarea.Withthatequipment,asmooth,white,textureburnwithoutthecharacteristicdarkringindicatesanimproperlyexcitedspecimen.However,ifboronnitridedisksareusedtomechanicallyrestricttheexcitedareaofthesample,aproperlyexcitedspecimenmaynotexhibitadarkring.

11.3ElectrodeSystem—Thespecimen,electricallynega-tive,servesasoneelectrode.Theoppositeelectrodeisathoriatedtungstenorsilverrod,thetipofwhichhasbeenmachinedtoa90°or120°angledcone.Useeithera3mm,4mm,or5-mm(60.1-mm)analyticalgap.Conditionafreshcounterelectrodewithtwotosixexcitationsusingtheoperat-ingconditionsdescribedin11.1and11.2.

11.4PhotomultiplierPotentials—Thesensitivityofthephotomultipliersisnormallyestablishedandsetbythespec-trometermanufacturerbasedontheparticularwavelengthsselected.

NOTE14—Therangeofanodetocathodepotentialsforagiventubeshouldbespecified,thatis650Vdcto1000Vdc.Ifwithinthepotentialrangethetubeiseithertoosensitiveortooinsensitivefortheelementconcentrationrange,selectanotherphotomultiplier.Thepotentialsonthecapacitorsmaybereaddirectly,oranumberofdifferentreadoutsystemsmaybeemployed,whichyieldlinearorlogarithmicfunctionsofthepotentialsandwhichmaybedisplayedasrelativenumbersorasnumberscalibrateddirectlyintermsofpercent.

13.2Excitespecimensinduplicateandreporttheaverageoftheduplicateresults.

14.Calculation

14.1Usingtheaverageresultsobtainedin13.2,calculatetheconcentrationoftheelementsfromtheanalyticalcurvesdevelopedin12.1.

15.PrecisionandBias

15.1Precision—Uptoeightlaboratoriescooperatedinperformingthistestmethodandobtainedthestatisticalinfor-mationsummarizedinTable3.Additionaldataforwithin-laboratoryvariabilityofresults,obtainedbyanalyzingthreespecimensofonematerialinsevenlaboratoriesinaccordance

MNL7AManualonPresentationofDataandControlChartAnalysis,ASTMManualSeries,ASTMInternational,7thed.,2002.

512.Calibration,Standardization,andVerification

12.1Calibration—Usingtheconditionsgivenin11.1-11.3,excitecalibrantsandpotentialstandardantsinarandomse-quence,bracketingthesewithexcitationsofanymaterialsintendedforuseasverifiers.(Averifiermaybeusedasacalibranteventhoughitisburnedonlyasaverifier.)Thereshallbeatleastthreecalibrantsforeachelement,spanningthe

4

E415–08

withsourceconditionsspecifiedinthismethod,aregiveninTable4.Otherspecimensmayexhibitgreaterorlessvariabilityusingthesameinstrumentandexcitationconditions.

TABLE3StatisticalInformation(TestMethodE415ExtensionStudy)

ElementAluminum

AverageConcentration

0.06690.06250.02120.00380.04150.01440.00630.00380.00061.0540.5070.0331.5741.3072.1280.1180.0930.1570.1140.00860.4350.1500.0541.31.4940.5590.3160.5610.3250.1474.7962.2080.1800.1080.05780.0760.00840.00780.07750.03790.01241.0630.3910.1760.05050.02090.01460.0400.0240.00560.190

NumberofLaboratories

757266777777767774787777777777676777557777777777777

Repeatability,R1A0.0040.0030.0050.00070.0050.0070.00070.00070.00030.0530.0250.0250.0430.1230.0570.0030.0030.0080.0110.00070.0250.0090.0080.0520.0520.0230.0130.0120.0080.0050.2750.1120.0120.0060.0030.0070.0030.0030.0050.0030.0030.0310.0150.0060.0060.0050.0020.0020.0020.0010.024

RelativeRepeatability,%

5.984.8023.618.412.048.611.118.450.05.034.9375.83.3.412.682.543.235.109.658.145.756.0014.82.753.484.114.112.142.463.405.735.076.675.565.199.2135.738.56.457.9224.22.923.843.4111.928.913.75.008.3317.912.6

Reproducibility,R2A0.0250.0230.0110.0010.02720.02470.00110.00420.00090.1080.0610.0420.1760.1240.2320.0110.0080.0570.0230.0040.0390.0260.0220.1810.1410.0740.0510.1680.0370.0160.6910.10.0220.0100.0150.0100.0180.0140.0170.0120.0090.1070.0990.0350.0150.0070.0050.0240.0110.0070.045

Relative

Reproducibility,%

34.736.851.926.365.6172.17.5110.150.10.212.0127.13..4910.99.328.6036.320.246.58.9717.340.79.569.4413.216.129.911.410.914.17.4312.29.2626.013.2214.179.21.931.772.610.125.319.929.733.541.160.045.8125.23.7

AntimonyArsenic

Boron

Carbon

Chromium

Cobalt

Copper

Manganese

Molybdenum

Nickel

Niobium

Phosphorus

Silicon

Sulfur

Tin

Titanium

5

E415–08

TABLE3

Element

AverageConcentration

0.0290.0019

Vanadium

0.2790.0910.00260.04390.00750.0025

NumberofLaboratories

77777555

Repeatability,R1A0.0040.00070.0070.0020.00020.0060.0020.001

Continued

RelativeRepeatability,%

13.836.82.512.207.6913.726.740.0

Reproducibility,R2A0.0170.0020.0410.0150.0020.0090.0120.008

Relative

Reproducibility,%

58.6105.14.716.576.920.5160.320.

Zirconium

AR1isequivalenttor,PracticeE1601;R2isequivalenttoR,PracticeE1601.

TABLE4VariabilityofResultsWithinIndividualLaboratories(NBS1262)

ElementNBS

ValueAluminum0.095

AverageCon-centration,%0.0870.09360.08230.09920.09990.0950.090.0125novaluenovaluenovaluenovalue0.0110novalue0.060novalue0.1085novalue0.07180.08710.07840.00260.001740.00300.002570.003030.002420.00280.1600.10.1580.1620.1590.1590.1620.2960.3000.3090.3020.3000.3040.2980.2990.3020.252

Labo-ratory123456712345671234567123456712345671234567123

StandardRelativeStandard

ADeviation,%Deviation,RSD

%B0.00320.00470.00830.00300.00190.00150.00120.0018novaluenovaluenovaluenovalue0.00031novalue0.0024novalue0.0045novalue0.00290.002430.00210.000400.000430.00030.000090.000140.000070.00010.00800.00940.00460.00220.0070.00370.00380.00480.00380.00390.00150.00320.002200.00200.00540.00440.0137

3.705.0310.103.011.901.581.3614.40novaluenovaluenovaluenovalue2.85novalue4.00novalue4.16novalue4.002.792.15.4024.6810.133.504.602.2.235.005.762.921.374.402.292.241.621.281.260.491.100.720.681.801.455.45

ElementNBS

ValueMolybdenum0.068

AverageCon-centration,%

0.0680.06810.06630.0690.0680.0690.05...0.5970.5600.50.6060.50.5560.2900.2920.3210.2920.20.2830.26360.04140.03550.04140.03940.0400.03690.03420.4030.3920.3930.3980.30.437

Labo-ratory1234567123456712345671234567123456

StandardDeviation,%A0.00120.00400.001730.0000.00110.000680.0005novalue0.00780.00690.00220.00970.004430.00270.01200.01080.00980.00370.01370.00590.00420.00220.001440.00120.000390.00140.000630.00040.00460.00580.01260.00300.00590.0032

RelativeStandardDeviation,RSD%B1.465.912.600.921.600.980.73novalue1.311.220.361.600.750.494.103.693.061.2.702.081.585.304.042.851.003.501.721.301.141.493.210.751.500.73

Antimony0.012Nickel0.59

Arsenic0.076Niobium0.29

Boron0.0025Phosphorus0.042

Carbon0.16Silicon0.39

Chromium0.30Sulfur0.038

0.03760.04040.03630.03870.03920.03760.03750.010.01570.0207

1234567123

0.00200.002390.001180.001030.00140.001320.00140.000670.000480.00046

5.305.942.852.653.503.513.783.753.082.21

Cobalt0.30Tin0.016

6

E415–08

TABLE4

ElementNBS

Value

AverageCon-centration,%0.304novalue0.2990.3038

Copper0.50

0.4990.5020.4940.5050.4960.4990.5341.0561.001.101.0501.0381.0161.0380.192novalue0.3050.187

Labo-ratory4567123456712345671234

StandardRelativeStandardDeviation,%ADeviation,RSD

%B0.0020novalue0.005970.00290.01160.00980.02120.003460.0120.008520.00990.00920.00810.01430.00720.0150.01170.00870.00novalue0.01770.0048

0.66novalue2.000.972.321.954.280.692.401.711.850.870.811.290.691.501.150.844.70novalue5.812.58

Titanium0.084

Continued

ElementNBS

Value

AverageCon-centration,%

0.01780.01580.0160.01750.0790.00.090.0910.08820.0850.10730.0400.04020.04100.04130.03870.0390.04580.1910.1730.1941

Labo-ratory456712345671234567567

StandardDeviation,%A0.000720.00260.000440.00040.00430.00250.0003240.00110.00050.001350.00170.000370.000540.00100.000220.00050.000360.00040.00810.004950.0070

RelativeStandardDeviation,RSD%B4.042.902.772.275.442.813.601.171.301.591.550.921.342.430.521.300.920.784.202.8633.611

Manganese1.04Vanadium0.041

Zirconium0.19Zirconium0.19

AStandardDeviation(s)wascalculatedasfollows:

s5

Œ(d2N21where:

d=differenceofdeterminationfrommean,andN=numberofdeterminations.

BRelativeStandardDeviation(RSD)wascalculatedasfollows:

RSD5

s

100!x¯~

where:

s=standarddeviation,andx¯=averageconcentration,%.

15.1.1PrecisionforCalciumandNitrogen—UptoeightlaboratoriescooperatedinperformingthistestmethodandobtainedtheprecisioninformationsummarizedinTable5.6Anapproximatevaluefortheexpectedreproducibilityindex,R,intherangeof0%to0.0030%calciumcanbecalculatedfromthefollowingequationinwhichCa%istheexpectedcalciumlevel:

R5=@0.0004821~Ca%30.30!2#

(1)

NOTE16—TheinterlaboratorytestdatasummarizedinTables5and6hasbeenevaluatedinaccordancewithPracticeE1601.

15.1.2Fornitrogen,thereproducibilityindex,R,hastheapproximatevalueof0.0020throughouttherangeof0%to0.015%nitrogen.

SupportingdatahavebeenfiledatASTMInternationalHeadquartersandmaybeobtainedbyrequestingResearchReportRR:E01-1022.

615.2Bias—Atleastthreespecimensthatpreviouslyhadbeenanalyzedbychemicaltechniquesinmorethanonelaboratorywereanalyzedfollowingtheconditionsofthistestmethod.ThedataaregiveninTable7(Note16).

15.2.1BiasforCalciumandNitrogen—Thebiasofthistestmethodatcertainconcentrationlevelsmaybejudgedbycomparingtheacceptedreferencevalueswiththearithmeticaverageobtainedbyinterlaboratorytesting(seeTable6).16.Keywords

16.1carbonsteel;low-alloysteel;opticalemission;spec-trometricanalysis

7

E415–08

TABLE5StatisticalInformationforCalciumandNitrogen

TestMaterialCalciumCGHFDJAIBENitrogen

CE

FHGDBAI

NumberofLaboratories

6788888888

Found,%

MinimumSD(SM,PracticeE1601)

0.0000210.0000250.0000750.0001340.0001350.0001290.0001190.00000.0001820.000258

ReproducibilitySD(SR,ReproducibilityIndex

(R,PracticeE1601)PracticeE1601)

0.000175

0.0001810.0002100.0002490.0002310.0002980.0002180.0001810.0003280.000436

0.000490.000510.000590.000700.000650.000830.000610.000510.000920.00122

Rrel%25013955.759.043.345.030.324.434.442.5

0.000200.000360.001060.001180.001490.001860.002010.002070.002670.00288

888888888

0.001250.004000.004780.005090.007510.008170.009770.0120.013

0.0001430.0001690.0001750.0001570.0002470.0002180.00020.0002390.0002

0.0007810.0007870.0007790.0006840.0007150.0006500.0005870.0006030.000813

0.002180.002200.002180.001920.002000.001820.0010.001690.00228

17555.745.637.626.722.216.813.116.7

TABLE6BiasInformationforCalciumandNitrogen

TestMaterialCalciumCGHFDJAIBENitrogen

CE

FHGDBAI

AssumedTrueValue,

%

0.000270.00040.00110.00140.00160.00210.00180.00220.00290.0033

AverageSpectrometer

Value,%

0.000200.000360.001060.001180.001490.001860.002010.002070.002670.00288

Difference,%

MaterialIdentification,Uncertainty

LowAlloySteelDescription

or(SD)BSCA4ABSCCS1ST06BS58GBS54DST08BSCA1AST07BSCA2ABSCSN2D

0.00004(0.00005)(0.00013)(0.00019)(0.00015)(0.00014)(0.0003)(0.0002)(0.0003)(0.0003)

chill-castwroughtwroughtwroughtwroughtwroughtchill-castwroughtchill-castwrought

−0.00007−0.00004−0.00004−0.00022−0.00011−0.000240.00021−0.00003−0.00023−0.00042

0.00110.00360.00440.00560.00740.00870.01060.01350.0136

0.001250.004000.004780.005090.007510.008170.009770.0120.013

0.000150.000400.00038−0.00051−0.00009−0.00053−0.00083−0.000610.00004

BS54DBSXAASBSXCCSBSXCCVBSXCCTBS56GBSCA4ABSCA1ABS46A

(0.0003)(0.00025)(0.00025)(0.00024)(0.0002)(0.0004)(0.0007)(0.00075)(0.00038)

wroughtwroughtwroughtwroughtwroughtwroughtchill-castchill-castwrought

8

E415–08

TABLE7BiasData

Element

AssumedTrueValue,%0.040.0580.0070.0730.220.500.670.050.080.370.851.510.120.170.0160.0560.0700.1010.440.570.981.430.0080.100.140.330.340.0340.10

AverageSpectrometerValue,%

0.0380.0620.0060.0720.210.510.660.050.090.350.851.570.110.160.0170.0540.0650.0980.430.580.941.490.0120.100.150.330.360.0380.11

NumberofLaboratories

44755755753774373355574477357

DeviationfromAssumedTrueValue,%

0.00+0.004−0.001−0.001−0.01+0.01−0.010.00+0.01−0.020.00+0.06−0.01−0.01

Sulfur

Copper

+0.001−0.002−0.005−0.003

Tin

Manganese

−0.01+0.01−0.04+0.06+0.0040.00+0.010.00+0.02+0.004+0.01

TitaniumNiobiumElement

AverageAssumed

TrueValue,SpectrometerNumberof

Value,%Laboratories%0.35

0.560.0230.100.0050.0090.0360.0460.00.0240.180.190.350.400.0080.0320.0340.0530.0040.0080.0240.0280.0440.0020.0270.0020.0120.1350.27

0.340.540.0240.110.0050.0090.0380.0420.0780.0290.180.180.360.390.0060.0280.0380.0510.0050.0080.0250.0240.0400.0020.0290.0020.0120.1380.28

53225575737557453755577772227

DeviationfromAssumedTrueValue,%

−0.01−0.02+0.001+0.010.0000.000+0.002−0.004−0.011+0.0050.00−0.01+0.01−0.01−0.002−0.004+0.004−0.002+0.0010.000+0.001−0.004−0.0040.000+0.0020.0000.000+0.003+0.01

Aluminum

BoronCarbon

Phosphorus

Chromium

Silicon

Cobalt

Molybdenum

Vanadium

Nickel

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9