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6/30/2015

ANALYTICALMETHODS

ANALYTICALMETHODS
Agedeterminationsbylaser40Ar/39Aranalysiswereperformedonsinglecrystalsof
plagioclase,amphibole,andbiotite,whichwerehandpickedfromcrushedand
sievedsplitsofSamples161977A60X1,07cm,61X1,07cm,62X1,1319
cm,and978A47R1,06cm.Mineralseparateswereetchedin15%hydrofluoric
acid(plagioclaseandamphibole)andcleanedusinganultrasonicdisintegrator(all
separates).Sampleswereirradiatedfor72hoursataneutroncurrentof2.1x1012
N/cm2atthe5MWreactoroftheGKSSResearchCenter(Geesthacht,Federal
RepublicofGermany),withcrystalsinaluminumtraysandirradiationcans
wrappedin0.7mmcadmiumfoil.
Analysesof40Ar/39ArwereconductedattheGeomarTephrochronologyLaboratory.
Plagioclaseandamphibolecrystalswerefusedinasinglestep,whereasanalysesof
biotitewereperformedbylaserstepheating(40mW2000mW).Purifiedgas
sampleswereanalyzedusingaMAP216seriesnoblegasmassspectrometer.Raw
massspectrometerpeakswerecorrectedformassdiscrimination,background,and
blankvalues(determinedeveryfifthanalysis).Theneutronfluxwasmonitored
usingTCRsanidine(TaylorCreekRhyolite,27.92MaDalrympleandDuffield,
1988DuffieldandDalrymple,1990)andinternalstandardSAN6165(0.470Ma
vandenBogaard,1995).VerticalvariationsinJvalueswerequantifiedbyacosine
functionfit.LateralvariationsinJwerenotdetected.Correctionsforinterfering
neutronreactionsonCaandKarebasedonanalysesofopticalgradeCaF2and
highpurityK2SO4saltcrystalsthatwereirradiatedtogetherwiththesamples.
Correctionfactorsweredeterminedas36Ar/39ArCa=0.4650.00137Ar/39ArCa
=977238Ar/39ArK=0.02220.0001and40Ar/39ArK=0.0020.001.
Analyticalerrorsarequotedas1 .

Formajorandtraceelementanalyses,thevolcanicpebbleswerecleaned,crushed
to0.5cmsize,handpicked,andthenwashedwithdistilledwater.Wholerockchips
weregroundtorockpowderinanagatemill.BothH2OandCO2contentswere
determinedusingaRosemountInfraredPhotometerCSA5003.Bulkrockanalyses
ofmajorandtraceelements(Ba,Rb,Sr,Zr,V,Cr,Co,Ni,Cu,Zn,andGa)were
performedonfusedtablets.ThetabletswereanalyzedattheGEOMARResearch
CenterusingaPhilipsXuniquePW1480Xrayfluorescencespectrometer.
InternationalreferencestandardsRGM1(rhyolite),BM(basalt),SY2(syenite),
andSDC1(micaschist)werealsoanalyzedandareusedtoevaluatetheprecision
andaccuracyofthemeasurements(Table2).Themaximumstandarddeviationof
thestandardsis0.20wt%forSiO2and0.02wt%forallothermajorelements
exceptNa2O(0.10wt%).ForthetraceelementsmeasuredbyXRF,themaximum
standarddeviationis5ppm,withtheexceptionofBa,forwhichitis14ppm.
Additionaltraceelements(Pb,Th,U,Hf,Nb,Ta,Y,andallrareearthelements
[REE])wereanalyzedusinganupgradedVGPlasmaquadPQ1ICPMSatthe
GeologicalInstitute,UniversityofKiel,afterthemethodofGarbeSchoenberg
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ANALYTICALMETHODS

(1993).TwoblanksandinternationalstandardsBHVO1(basalt),RGM1(rhyolite),
andSTM1(syenite)wereanalyzedwiththesamples.Resultsarepresentedin
Table3.Precisionoftheresultswasestimatedfromduplicatedigestionsand
duplicatemeasurementsandwasfoundtobe<2%5%relativestandarddeviation
inmostcases.

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