Title Quantitative analysis of major elements in igneous rocks with X-ray fluorescence spectrometer “ZSX primus II” using a 1:10 dilution glass bead Author(s) Kusano, Yuki; Umino, Susumu; Kobayashi, Jinya; Mizukami, Tomoyuki; Okuno, Masayuki; Arai, Shoji Citation The science reports of the Kanazawa University = 金沢大学理科報告, 58: 31-44 Issue Date 2014 Type Departmental Bulletin Paper Text version publisher URL http://hdl.handle.net/2297/41282 Right *KURAに登録されているコンテンツの著作権は,執筆者,出版社(学協会)などが有します。 *KURAに登録されているコンテンツの利用については,著作権法に規定されている私的使用や引用などの範囲内で行ってください。 *著作権法に規定されている私的使用や引用などの範囲を超える利用を行う場合には,著作権者の許諾を得てください。ただし,著作権者 から著作権等管理事業者(学術著作権協会,日本著作出版権管理システムなど)に権利委託されているコンテンツの利用手続については ,各著作権等管理事業者に確認してください。 http://dspace.lib.kanazawa-u.ac.jp/dspace/ 32 QuantitativeanalysisofmajorelementsinigneousrockswithXRF 11ntroduction AwavelengthdispersiveX-rayfluorescencespectrometer(XRF)ZSXprimusII (RigakuComoration)hasbeenlaunchedinEarthScienceCourse,SchoolofNatural Systems,CollegeofScienceandEngineering,KanazawaUniversitysinceNovember 2013.TheinstrumentwasusedfOrscientificstudiesbyresearchersofKanazawa University(Otsukaetal.,2014a;Hamadaetal.,2014)andvisitors,andfOreducationof undergraduatestudentsinthefirstyear.Becausesamplepreparationishandyandthe originalprogramsofqualitativeandsen-quantitativeanalysesinstalledintheZSX primusllareeasyfOrabeginnertouse,theinstrumenthasbeen廿equentlyusedfOr researchesinmaterialengineeringandarcheology.However,theresultsofthesemquantitativeanalysesofsomeultramaficrockglassbeadsgivetwiceashighNiandCr contentsastherecommendedvalues.Becausetheseelementsarecriticalinthefieldof earthsciences,theanalyticalproceduresarerequiredtobemoreaccuratefOr g e o c h e m i c a l s t u d i e s . W h o l e r o c k m a j o r e l e m e n t c o m p o s i t i o n s g i v e t h e f i m d a m e n t a l g e o l o g i c a l i n f O n n a t i o n t h a t c h a r a c t e r i z e s r o c k s a m p l e s . R e c e n t l y , w h o l e r o c k p o w d e r s a m p l e s a r e d i r e c t l y f U s e d toaglassbeadonaniridiumfOil(Ichiyamaetal.,2013),andsuchaglassbeadis utilizedfOrmajorelementanalysisbyanElectronProbeMicroAnalyzer(EPMA)and fOrtraceelementanalysisbyaLaser-AbrasionInductivelyCoupledPlasmaMass S p e c t r o m e t r y ( L A I C P M S ) ( O t s u k a e t a l . , 2 0 1 4 b ) . H o w e v e r , t h e r e p r o d u c i b i l i t y a n d p r e c i s i o n o f m a j o r e l e m e n t a n a l y s e s o f a d o l e r i t i c s a m p l e a r e r e l a t i v e l y l o w c o m p a r e d withthosebyXRF(datasource廿omOtsukaetal.,2014a,bandKusanounpublished d a t a ) . I n v i e w o f t h e e a s e o f s a m p l e p r e p a r a t i o n , a c c u r a c y a n d p r e c i s i o n o f a n a l y s e s , g l a s s b e a d s w i t h l : 1 0 d i l u t i o n o r l o w e r d i l u t i o n ( 1 : 2 a n d l : 5 ) h a v e b e e n u s e d f b r m a j o r e l e m e n t a n a l y s e s o f i g n e o u s a n d s e d i m e n t a r y r o c k s b y m a n y l a b o r a t o r i e s a n d i n s t i m t e s (e.g.TsuchiyaandHasenaka,1995;KimuraandYamada,1996;Gotoetal.,2002;Seno andMotoyoshi,2004;ShinjoandMiyamoto,2007;Nakanoetal.,2012;Yamasaki, 2 0 1 4 ) . T h e r e f b r e , w e h a v e e s t a b l i s h e d q u a n t i t a t i v e a n a l y t i c a l p r o c e d u r e s o f m a j o r e l e m e n t s o f i g n e o u s r o c k s a m p l e s u s i n g l : 1 0 d i l u t i o n g l a s s b e a d s . W e p r e s e n t a n a l y t i c a l p r o c e d u r e s b a s e d o n t h e c a l i b r a t i o n l i n e s u s i n g l : 1 0 d i l u t i o n g l a s s b e a d s , a n d t h e c o n d i t i o n s a n d p r e c i s i o n o f t h e q u a n t i t a t i v e a n a l y s i s o f a n d e s i t i c andbasalticrocks,andultramaficrocks. 34 QuantitativeanalysisofmajorelementsinigneousrockswithXRF ●勺■■ユ e a Cm ロューロロ口︾口IJI口IJI■た口一乍一三弐三口口店 Otgetft 36 QuantitativeanalysisofmajorelementsinigneousrockswithXRF SAnalyticalConditions 3、1InstrumentCondition Aglassbeadissetonastainlesssteelsampleholderwiththemeasurementsurfaceup. Thebeadisscreweduptobeincontactwithasamplemaskwithahole30nnnin diameterinthecenter.Afterpassingthroughtheheightchecker,thesampleholderisset onthesamplestage.48sampleholderscanbesetonthestage.Weusuallysetasample usedfbrcalibrationofthePulseHeightAnalyzer(PHA)onthestageno.H-1.Unknown samplesaresetonother47stages. TheZSXprimusllisequippedwithanend-windowX-raytubeandarhodiumanode, andiscontrolledbyZSXsoftwarerunonawindows7personalcomputer.AsZSXis runandX-rayistumedon,ZSXautomaticallysetstheaccelerationvoltageandelectric currentto50kVand50mA,respectivelyandadjuststheX-raycounterbymeasuring thecalibrationsampleonthestageno.H-1. 3.2MeaSuringbasaltandandesitewith66Majorl2'' 3.2.1Calibrationlines TenmajorelementsSi,Ti,Al,Fe,Mn,Mg,Ca,Na,KandPareanalyzedbyan applicationprogram"Majorl2''inlOnnutes.The加strumentconditionsofeach elementarelistedinTable3. ElevenGSJstandardandonesyntheticsamplesareusedtomakecalibrationlines.A regressioncalculationwasdonebytheZSXsoftware.KUlinesofSi,Fe,Mg,CaandK aremeasuredfbr40secondsatpeakpositionsonlybecausepeaktobackgroundX-ray countratiosarelargesothatthedifferencesofthegrossandnetpeakcountsare negligible.BothpeakandbackgroundX-rayintensitiesaremeasuredfOrKUlinesofTi, Al,Mn,NaandP,basedonwhichbackgroundcorrectionsaremade.Thegrossandnet countratesarelinearlycorrelatedwiththemass廿actiOnofoxides,yieldinglinear calibrationlinesofallmajorelements(Figurel).However,JG-2showshigherPKq intensitythanthatexpectedfbrtheP205concentrationofthereconnnendedvalue.Since repeatedmeasurementsofJG-2showhigherPintensities,JG-2wasexcludedfromP205 c a l i b r a t i o n i n t h i s r e p o r t . C o r r e l a t i o n c o e f f i c i e n t s ( R 2 ) o f X r a y i n t e n s i t i e s a n d m a s s fiactionsofmajorelementoxidesarebetterthanO.99fOrallelements.Asshowninthe enlargedplotsofA1203andMgO,X-rayintensitiesandthemass廿actionsofoxidesare w e l l c o r r e l a t e d a r o u n d t h e r a n g e o f a l a r g e n u m b e r o f s t a n d a r d s a m p l e s . ThecalibrationrangesandaccuracyofeachelementareshowninTable4.The accuracyofacalibrationlineisgivenby
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