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1、DeterminationofTraceElementsinSteelbyhighsensitivityinductivelycoupledplasmamassspectrometrywithoutmatrixseparationNIELingqing1JIHongling1CHENYingying1LIUXiaoping1WANGYangping2(1.BaosteelResearchInstituteShanghai201900Ch
2、ina2EastChinaUniversityofScienceTechnology200237China)Abstract:Inconnectionwithincreasingqualitydemsinsteelsteelproductiondecreasingchemicalanalysisofthesetraceelementsdowntotheuggrangeisincreasingimptant.Inourstudyafast
3、preciseaccuratemultielementsdeterminationmethodftraceelementsBAlPPbSnSbAsBiintherangeofμgg1subμgg1insteelhasbeenestablishedbyhighsensitivityinductivelycoupledplasmamassspectrometry(HRICPMS)withoutanymatrixseparationanyin
4、ternalstard.IthasgoodprecisionlowlimitofdetectionwithRSD5%LOD0.01μgg1fmostelements.Themeasuredvaluetalliedwiththestardvalve.Therecoveryissatisfied.Keywds:HRICPMSsteeltraceelementswithoutmatrixseparation0IntroductionThepr
5、opertiesqualityofsteelareamongotherthingsaffectedbytramptraceelementswhichareeitheraddedduringthesteelmakingprocesspresentasimpuritiesiginatingfromtherawmaterials1.someelementssuchasPbareunwholesometous.Inconnectionwithi
6、ncreasingqualitydemsinsteelsteelproductiondecreasingchemicalanalysisofthesetraceelementsdowntotheuggrangeisofincreasingimptant2.InrecentyearsHRICPMShasbeenemployedtodeterminingtraceanalysisinvariousfields.Inironsteelfiel
7、dsomepaper34repteddeterminingoftraceamountsofelementsinhighpurityironsteelafterseparatingtheironmatrixbyexchangechromatographybysolidphaseextractionInsomeresearch5traceelementswereanalyzedusingmatrixmatchedstardsolutionc
8、alibrationinternalstard.1EXPERIMENTAL1.1InstrumentationTheICPMSusedinourstudywasElement2(FinniganMATBremenUSA).TheconditionsfICPMSweredailyoptimized.Sotheconditionsspecialtchpositiongasflowwerealittledifferentdaily.Themi
9、crowaveusedinthisstudywasMDS2100(CEMUSA).TheconditionsfGenerallymatrixeffectswerecoursedbyalargeamountofFecomplexcompositionofsteelwhereastheextentofinfluenceisdifferentfromdifferentinstrument.Inourstudyonlyafewminuteswe
10、reneededinourexperimentalprocesscommonlymatrixeffectsareinconspicuousfmostelements(2ngg1)under100μgg1matrixwhenusingshtinjectingtimeasshowninFig.1.Ontheotherhthehigherconcentrationofmatrixistheeasiliertheconeificeisclogg
11、edbydepositofdissolvedmetaloxidesinsolutions.Sowechoose100μgg1matrixwithoutanyinternalstardastheanalyticalsolutioninourstudy.Fig.1signalvarietyfcontinueinjectingtimeIndertovalidateourconclusionthefunctionofinternalstarde
12、lementswasstudy.WedeterminedofBwithwithoutinternalstard.Asshownintable2therewasn’tanyconspicuousdifferencebetweenthedatafrom“withoutinternalstard”methodthedatafrom“withinternalstard”method.Table2themeasurevalueofBwithwit
13、houtinternalstardelement2.3LimitofdetectionRecoveryThelimitofdetectioninsolutionwascalculatedonthebasisofstarddeviationofelevensuccessivemeasurementsofblanksolutioncalculatingasthefollowingfmula(1).Table3showstheLODofmos
14、telementsisunder0.01μgg1inmassexceptPwiththeLODof0.144μgg1perhapspartlyaccdingtolowintensityofit.Recoveryyieldsoftraceelementswereexaminedby1ugg5ugg10ugg50uggofstardsolutionintosamplescontainingveryfewinterestingtraceele
15、ments.Asdemonstratedintable3therecoveryoftraceelementsofsteelswassatisfied.CRMBwithoutISBwithISYBwithISBeCertifiedvalueGBW013230.00230%0.00231%0.00227%0.0023%GBW013270.00094%0.00098%0.00102%0.001%020000040000060000080000
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