ICS77.080.01CCSH11

團(tuán)體標(biāo)準(zhǔn)

T/CSTM00012E—2021

Ironandsteel--Characterizationof

distributionofmulti-elementcontentsand

status--Originalpositionstatisticdistributionanalysismethodoflaserinducedbreakdown

spectroscopy

鋼鐵多元素成分及狀態(tài)分布表征

激光誘導(dǎo)擊穿光譜原位統(tǒng)計分布分析方法(EnglishTranslation)

Issueddate:2021-11-10Implementationdate:2022-02-10

IssuedbyChineseSocietyforTesting&Materials，Zhongguancun

T/CSTM00012E—2021

Foreword

ThisEnglishdocumentwastranslatedfromT/CSTM00012-2017byCSTM/FC99(TheintegratedfieldtechnicalcommitteeofChineseSocietyforTesting&Materials).Incaseofanydoubtaboutthe

contentsofEnglishtranslation,theChineseoriginalshallbeconsideredauthoritative.

ThisdocumentisdraftedrefertotherulesgivenintheGB/T1.1-2020(Directivesforstandardization-Part1:Rulesforthestructureanddraftingofstandardizingdocuments).

Attentionisdrawntothepossibilitythatsomeoftheelementsofthisstandardmaybethesubjectofpatentrights.Theissuingbodyofthisdocumentshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.

ThisdocumentwasproposedbyCSTM/FC99(TheintegratedfieldtechnicalcommitteeofChineseSocietyforTesting&Materials).

ThisdocumentwaspreparedbyCSTM/FC99(TheintegratedfieldtechnicalcommitteeofChineseSocietyforTesting&Materials).

T/CSTM00012E—2021

Ironandsteel--Characterizationofdistributionof

multi-elementcontentsandstatus--Originalpositionstatisticdistributionanalysismethodoflaserinducedbreakdownspectroscopy

Warning—Peopleusingthisdocumentshouldhavepracticalworkexperienceinformallaboratory.Inthisdocument,notallpossiblesafetyissuesarepointedout.Theuserisresponsiblefortakingappropriatesafetyandhealthmeasures,andensuringcompliancewiththeconditionsstipulatedbyrelevantnationallawsandregulations.

1Scope

Thisdocumentspecifiesamethodtocharacterizethemulti-elementcontentsandstatusinironandsteelbyoriginalpositionstatisticdistributionanalysismethodoflaser-inducedbreakdownspectroscopy.

Thisdocumentisapplicabletocharacterizethecontentdistribution,locationdistributionandstatedistributionofmulti-elementinironandsteel.Thecontentfrequencystatisticaldistribution,segregationstatisticaldistribution,apparentdensitystatisticaldistribution,statisticfittingdegreestatisticaldistributionandthetype,contentandparticlesizestatisticaldistributionofinclusionscanbecharacterized.

2Normativereferences

Thefollowingdocumentisreferredtointhetextinsuchawaythatsomeoralloftheircontentconstitutesrequirementsofthisdocument.Fordatedreferences,onlytheeditioncitedapplies.Forundatedreferences,thelatesteditionofthereferenceddocument(includinganyamendments)applies.

GB/T21834-2008Mediumandlowalloysteel-Determinationofthedistributionofmulti-elementcontents-Originalpositionstatisticdistributionanalysismethod

3Theory

Theoriginalpositionstatisticdistributionanalysisisperformedbylaser-inducedbreakdownspectroscopy(LIBS)ontherelativemotionsample.Theexcitedemissionspectraaredispersedintocharacteristicspectralline.Theemissionlineintensitiesoftheselectedreferencelineandtheanalysislinearemeasured.Thecalibrationcurveissetupbythestandardsamples.Accordingtotheintensitiesandthecalibrationcurve,theelementscontentofthescanningareaisobtained.Theexcitationlocationinformationissynchronouslyobtained.Bystatisticaldistributionanalysis,variousinformationusedtoevaluatethedistributionofelementswithinthescanningareaisobtained,suchascontent

two-dimensioncontourmap,contentthree-dimensionviewmap,contentlinedistributionmap,content-frequencydistribution,apparentdensitydistribution,maximumsegregationdegree,statisticsegregationdegree,statisticfittingdegree,averageapparentdensity,andthedistributionofthetypes,contentandparticlesizeofinclusions,etc.

4Apparatus

4.1

lasersource

Asystemcanprovideacontinuousandstablelaserwhichcanrealizeenergycontrolandfrequentadjustment;

4.2

laserfocusingopticalpath

Focusingtheemittedlaseronthesamplesurface,whichismainlycomposedofacollimatinglens(group),adiaphragm,andafocusinglens(group);

4.3

three-dimensionalmobilesampleplatform

Amechanicalmobileplatcansupportthesamplewhileexcitingandprovidingcontinuousmovementofthesample.Ifneeded,low-pressurehigh-purityargoncanbeusedforatmosphereprotection;

4.4

lightsplittingsystem

Consistsofcollimatinglens,incidentslit,grating,etc,thelightenterstheincidentslitthroughthecollimatinglens,slitbythegrating.Andthecharacteristicspectrallightofeachelemententersthephotomultipliertube(PMT),orchargecoupleddevice(CCD)orotherspectradetector;

Thereciprocaloftheprimaryspectraldispersionofthespectroscopicsystemshouldbelessthan0.6nm/mm,andthewavelengthrangeshouldbebetween170.0nmand420.0nm.IfC,P,Sandothershort-waveelementsneedtobeanalyzed,aninertgassystemoravacuumsystemshouldbeused.Andthevacuumlevelofthespectrometershouldbelessthan3Pa;

4.5

signalacquisitionsystem

Collectingandstoringallspectralsignalswithintheexcitationareawithhighprecision;

4.6

scanningsystem

Thelineorsurfacescanninganalysisinthesampleareaisrealizedbyscanningthesampleaccordingtothepresetroute;

4.7

dataprocessingsystem

Thelaserpulsesignalisrelatedtothestateofitsexcitationposition.Considerablequantitiesofspectrumsignalsarecollectedbythehigh-precisionacquisitionsystemandtheintensitiesarestored.Bymathematicalstatisticalanalysis,theinformationofthepositioncontentdistributionoftheelementsandtherelateddefectstatedistributionrelatingtotheoriginalpositioncanbeobtained;

Inthissystem,thedistributionpatternoftheelementsmeasuredaredirectlycharacterizedbycontenttwo-dimensioncontourmap,contentthree-dimensionviewmap,contentlinedistributionmap,content-frequencydistribution,apparentdensitydistributionmap,inclusiondistributionmap.Andaveragecontent,maximumsegregationdegree,statisticsegregationdegree,statisticfittingdegree,averageapparentdensity,andthetype,contentandparticlesizeofinclusionsareappliedtoexpressthedistributiontoo;

5Standardsamples,standardizationsamplesandcontrolsamples

5.1Standardsamples

Standardsamplesareusedtodrawcalibrationcurvesintheoriginalpositionstatisticaldistributionanalysisoflaser-inducedbreakdownspectroscopy.Thestandardsampleshouldbeacertifiedstandardsampleorsubstance,andthecontentofeachanalysiselementshouldbegradeddistributionandcovertherangeoftheelementcontentofthemeasuredsample.Theselectedstandardsampleshouldbeclosetothetypeofmeasuredsample.Thenumberofsamplingspotsforthestandardsample'ssurfacescanisnotlessthan9.

5.2Standardizationsamples

Standardizationsamplesareusedtocorrectthedriftoftheinstrument,whichshouldbeuniform.Whentwosamplesareusedforstandardization,thecontentsofeachelementshouldbetakenclosetotheupperandlowerlimitsofthecalibrationcurve.Theanalysisconditionsshouldbethesameasthestandardsamples.

5.3Controlsamples

Thecontrolsampleshavesimilarmetallurgicalprocessandchemicalcompositionwiththeanalysissample,andthecompositionsareevenlydistributed.Whennecessary,itcanbeusedtocalibratetheresultstocontroltheaccuracyofthemeasurement.Theanalysisconditionsshouldbethesameasthestandardsamples.

6Samples

6.1Sampletype

Thesamplesaredividedintodirectanalysissamplesandsamplesthatneedtobeprepared.

6.2Sampling

Thesampleshouldbecutandpreparedeasy-to-holdwithregularshape.Thesampleanalysissurfaceusuallycoverscertaincharacteristicareassuchasthecentralareaoftheslaborthebillet.ThespecificsamplingmethodisshowninAnnexB.1ofGB/T21834-2008.

6.3Preparation

Normallycuttingandsurfacetreatmentareneeded.Wirecuttingorsawingisusedforcuttingtothesuitablesize.Thesurfaceofthesampleshouldbeassmoothaspossible.

Agrinderormillingmachineisusedtotreatthesurface.Thesamplesurfaceshouldbesmoothandclean.ThesurfaceroughnessRaofthesampleshouldbelessthan0.3μm.Whenthegrinderormillingmachineisunavailable,othergrindingequipmentareneededtofittheanalysisrequirements.Itisrecommendedthattheparticlesizeofthegrindingmaterialshouldbelessthan48μm.Thegrindingmaterialisusuallyalumina,zirconiaorsiliconcarbide.Thecontaminationofthegrindingmaterialstothemeasuredelementsistriedtobeavoidedaspossiblewhengrindingsamples.

7Preparationoftheapparatus

Thelaboratoryofthelaser-inducedbreakdownspectroscopyoriginalpositionstatisticaldistributionanalyzershouldbeshockproofandclean.Generally,theindoortemperatureshouldbekeptat25℃±2℃,andtherelativehumidityshouldbe40%~70%.

7.1Stabilizationoftheinstrument

Tomaketheinstrumentworkstably,thelasershouldbepre-poweredforanappropriatetime.Theopticalsystemshouldbepre-heatedtoaconstanttemperature.Whenavacuumopticalsystemisused,thevacuumlevelshouldbelessthan3Pa.

Whenrestartinginstrumentafteralongshutdown,generallythepower-ontimeshouldnotbelessthan4hoursbeforeanalyzing.

Atestsampleshouldbepre-excitedbeforetheanalysistoensurethattheinstrumentisstableandtheanalysiscanbedone.

7.2Inspectionoftheopticalsystem

Thecollimatinglensshouldbecleanedregularly,andtheopticalpathshouldbecalibratedperiodically.

8Stepsofanalysis

8.1Selectionofstandardsamplesandworkingconditions

Accordingtothetypeandchemicalcompositionofthesample,standardsamplesandstandardizedsamplesareselected.

T/CSTM00012E—2021

Accordingtotheanalysiselementandtheircontentrange,thereferenceline,analysisline,excitationparametersandotherworkingconditionsareselected.

8.2Setupofthecalibrationcurve

Undertheselectedworkingconditions,aseriesofstandardsamplesarescannedandanalyzed.Thecalibrationcurveisdrawnbasedontheabsoluteorrelativeintensityofeachmeasuredelementandthecontentgivenbythestandardsample.

8.3Standardizationofthecalibrationcurve

Standardizationsamplesshouldbeusedtostandardizethecalibrationcurveperiodically,andthestandardizationintervaldependsonthestabilityoftheinstrument.Ifnecessary,controlsampleswhicharesimilartothecompositionandmetallurgicalprocessofthemeasuredsamplescanbeused.

8.4Controlofthemeasurementresults

Thestandardsamplesarescannedandmeasuredtodeterminetheaccuracyandreliabilityoftheanalysisresults.

8.5Sampleanalysis

Thesamplingareaandscanningareaofthesamplearedeterminedaccordingtoneeds.Thesameworkingconditionswiththecalibrationcurveareusedtoexcitethesampleandtheresultsaresaved.

9Expressionofresults

Accordingtotheabsoluteorrelativeintensity,thecontentofeachelementinthescanningareaiscalculatedfromthecalibrationcurve.Thestatisticaldistributionanalysiscanprovidevariousinformationtoevaluateelementdistribution:contenttwo-dimensioncontourmap,contentthree-dimensionviewmap,contentlinedistributionmap,content-frequencydistribution,apparentdensitydistributionmap,maximumsegregationdegree,statisticsegregationdegree,statisticfittingdegree,averageapparentdensity,andthedistributionofthetype,contentandparticlesizeofinclusions.

Themethodoforiginalpositionstatisticdistributionanalysismethodoflaser-inducedbreakdownspectroscopyappliedtocharacterizecontentdistributionandlocationdistributionisshowninAnnexA.

Themethodoforiginalpositionstatisticdistributionanalysismethodoflaser-inducedbreakdownspectroscopyappliedtocharacterizethequantitativerelationshipbetweenthestatisticalsegregationdegreeandthesulphurprintratingisshowninAnnexB.

Themethodoforiginalpositionstatisticdistributionanalysismethodoflaser-inducedbreakdownspectroscopyappliedtocharacterizestatedistributionisshowninAnnexC.

T/CSTM00012E—2021

Note:Fordifferentsteelgrades,differentprocesses,anddifferenttypesofinclusions,targetedexperimentsarenecessaryandcorrespondingrulesneedtobeformulated.

10Testreport

Thetestreportshouldincludeatleastthefollowingcontents:

a)Alltheinformationneededtoidentifythesamples;

b)Theusedstandard(includingtheyearofpublication);

c)Testresults(includingeverytestresultandtheaverage);

d)Abnormalphenomenaobservedinthemeasurement;

e)Anyoperationnotspecifiedinthispartoranyoperationthatmayaffecttheresults;

f)Dateoftest.

AnnexA

(Normative)

Explanationoforiginalpositionstatisticdistributionanalysismethodof

laser-inducedbreakdownspectroscopyonthecharacterizationresultsofcontent

distributionandlocationdistribution

Characterizationmethodsofcontentdistributionandlocationdistributionbyoriginalpositionstatisticdistributionanalysismethodoflaser-inducedbreakdownspectroscopyinclude:specificpositioncontent,maximumsegregationdegree,statisticsegregationdegree,statisticfittingdegree,contentlinedistributionmap,contenttwo-dimensioncontourmap,contentthree-dimensionviewmap,content-frequencydistribution,statisticindifferentcontentrange,contentconfidenceintervalandregionalstatisticaldistribution,etc.

A.1Specificpositioncontent

Theelementcontentwhichareobtainedonthespecificpositionofthesamplebylaserspectroscopyanalysis.

A.2Maximumsegregationdegree(M)

Withinthescanningarea,therearetwowaystocalculatethemaximumsegregationdegreeofanelement,themaximumdegreeofpoint-segregationM(x,y)andmaximumdegreeofmicro-zoneM(s).

Themaximumdegreeofpoint-segregationisexpressedbytheratioofthecontentatthehighestcontentpositionofaspecificelementcmtotheoverallaveragecontentc,asshownasformulaA.1:

M(x,y)=cm/c…………（A.1）

Themaximumsegregationdegreeofthemicro-zoneM(s)isexpressedbytheratioofthemaximumaveragecontentofaspecificelementinanareaof1mm2cstotheaveragecontentc,asshownasformulaA.2:

M(s)=cs/c…………（A.2）

A.3Statisticsegregationdegree（S）

Withinthescanningarea,thecontentdistributionofaspecificelementisanalyzedbymathematicalstatistics,andstatisticalsegregationdegreeSisobtainedat95%confidencelevel,whichiscenteredonthemedianvaluewithintheconfidenceinterval[c1,c2].SiscalculatedasformulaA.3:

S=(c1-c2)/2c0…………（A.3）

Where:

c0------themedianvalue;

c1,c2-----theupperandlowerlimitsofthecontentconfidenceinterval

Thelargerthestatisticalsegregationdegree,themoreseriousthesegregationis.Whenthereisnosegregation,thestatisticalsegregationdegreeis0.

[Source:GB/T24213-2009]

A.4Statisticfittingdegree（Cf）

Withinthescanningarea,thepercentageofconsistencybetweenthecontentofanelementatallpositionsandthespecifiedcontent(orcontentrange).

[Source:GB/T24213-2009]

A.5Contentlinedistributionmap

Thegraphthatshowsthecontentchangesalongx(ory)directionofaspecificelement,wheny(orx)isfixed(asshowninFigureA.1).

[Source:GB/T24213-2009]

Fig.A.1LinedistributionalongtheXdirection

A.6Contenttwo-dimensioncontourmap

Themapthatshowsthecontentdistributionofspecificelementcorrespondingtocoordinates(X,Y)withinthescanningarea.Differentcolorsorgraylevelsindicatethecorrespondingcontent(asshowninFigureA.2).

[Source:GB/T24213-2009]

Fig.A.2Contenttwo-dimensioncontourmap

A.7Contentthree-dimensionviewmap

Basedonthecontenttwo-dimensioncontourmap,thevaluesofZaxisareusedadditionallytorepresentthecontentsofelements(asshowninFigureA.3).

[Source:GB/T24213-2009]

Fig.A.3Contentthree-dimensionviewmap

A.8Content-frequencydistribution

Withinthescanningarea,thegraphthatusethecontentofaspecificlocationastheabscissa,andtheratioofthecontentofthespecificlocationtothetotallocationcontentastheordinate(asshowninFigureA.4).

[Source:GB/T24213-2009]

Fig.A.4Content-frequencydistribution

A.9Statisticresultsindifferentcontentrange

Basedonaspecifiedcontentrange,theratiosofthepositioncontentindifferentcontentrangeintheentirescanningareatoallthepositioncontentintheentirescanningareaarerecorded(asshowninFigureA.5).Theresultsofstatisticindifferentcontentrangeshowthemedianvalueandtheconfidenceintervalat95%confidencelevelatthesametime.

[Source:GB/T24213-2009]

Fig.A.5Statisticresultsindifferentcontentrange

A.10Contentconfidenceinterval

Acontentintervalwhichiscenteredbythemediancontentvalueunderacertaindegreeofconfidence(asshowninFigureA.6).[Source:GB/T24213-2009]

T/CSTM00012E—2021

Fig.A.6Contentconfidenceinterval

A.11Regionalstatisticaldistributioncharacterization

Inanygivenareawithinthescanningrange,content-frequencystatisticalcalculationscanalsobeperformed.Thatis,thelocationcontentistakenastheabscissa,andtheratioofthecontentofaspecificpositiontothecontentofallpositionintheareaistakenastheordinate(asshowninFigureA.7).

Fig.A.7Regionalcontent-frequencydistribution

T/CSTM00012E—2021

AnnexB

(Informative)

Thequantitativerelationshipbetweenthestatisticalsegregationdegreeof

originalpositionstatisticdistributionanalysismethodoflaserinduced

breakdownspectroscopyandthesulphurprintrating

B.1Sample

Theselectedsamplesshouldbeaseriesofrepresentativesampleswithobviousdifferencesinthedegreeofsulfursegregationundercertainprocesscondition,atleastnotlessthan4pieces(Thesulfurprintratingis0.5,1,2,and3respectively).

Eachsampleissubjectedtobothoriginalpositionstatisticaldistributionanalysisandsulfurprinttest.Andthescanningareafortheoriginalpositionanalysisshouldbeascloseaspossibletothesulfurprintcorrosionarea,thatis:thesurfaceofthesampleusedforsulfurprinttestshouldbethesameasthesurfaceburnedfororiginalpositionanalysis.Theprocessingthicknessisabout0.3-0.5mm.Then,thesamplewouldbereadytocarryoutthesulphurprinttest.

B.2Originalpositionstatisticaldistributionanalysistest

Theanalysisconditionsandexperimentsoforiginalpositionarecarriedoutinaccordancewiththisdocument.

B.3Sulfurprinttest

SamplepreparationandsulphurprintexperimentarecarriedoutaccordingtoGB/T4236,andsulphurprintratingiscarriedoutaccordingtoYB/T4002andYB/T4003.

B.4Thequantitativerelationshipbetweenthestatisticalsegregationdegreeandthesulphurprintrating

Makealistofthestatisticalsegregationdegreeandthesulfurprintratingresultsoftheseriesofsulphursamples.Thestatisticalsegregationdegreeofsulfuristakenastheabscissaandthesulfurprintratingresultistakenastheordinatetoperformlogarithmicregressionandtodeterminetheconstanttermskandbinthelogarithmicequation,y=klnS+b(yisthesulfurprintgrades,keepingonedecimalplace;Sisthestatisticalsegregationdegreeofsulfur).

Accordingtothisequation,thestatisticalsegregationdegreeofsulfurinanysamplecanbeconvertedintotheresultofsulfurprintrating.

T/CSTM00012E—2021

AnnexC

(Informative)

Explanationoftheoriginalpositionstatisticalstatedistributioncharacterization

resultsoflaser-inducedbreakdownspectroscopy

Theoriginalpositionstatisticalstatedistributioncharacterizationmethodoflaser-inducedbreakdownspectroscopyincludes"totalintensityoftestelements,thresholdintensity,netsignalintensityofinclusions,compositionofinclusions,particlesizeofinclusions"andsoon.

C.1Totalintensityoftestelement(It)

Thesumofthespectralintensitiesgeneratedbyalllaserpulsesofthetestelementsinanalysisarea.

It=

Where:

n——Thenumberoflaserpulsesinanalysisarea;

Ii——Th