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(ArizonaLaserChronCenter,UniversityofArizona)
G.Gehrels(12August,2010)
ZirconisapowerfulmineralforUThPbgeochronologybecauseithasthefollowing
properties:
HighUconcentration(commonly1001000ppm)
ModerateThconcentration(commonly10100ppm)
UandTharetightlyheld[similarsize(0.81.0)andcharge(+4)asZr]
LowcommonPbduringcrystallization(ppt)
Grows@6001100CbutretainsPbto>800C,sogenerallyrecordscrystallization
Commoninfelsic&intermediateigneousrocks
Chemicallyandmechanicallyresistant
Containsotherelementsthatyieldcomplementaryinformation(e.g.,Hf,Li,O,REE,He)
Figure1:Zirconcrystalstypicalofigneousrocks(left)andsedimentaryrocks(right).
TypicalapplicationsofUThPbgeochronologyinclude:
Determinationofcrystallizationageofplutonicandvolcanicrocks
DeterminationofprovenanceofsedimentaryrockbasedonUPbageandU/Thcontent
ofdetritalzircons
Determinationofmaximumdepositionalageofsedimentaryrockbasedonyoungest
age(s)ofdetritalzircons
AnalyticalmethodsforUThPbgeochronologyofzirconbyLAICPMSaremature,with
numeroustechniquepapersfromvariouslabs(Changetal.,2004;Gehrelsetal.,2008;
Horstwoodetal.,2003;Jeffriesetal.,2003;Kosleretal.,2002;Simonettietal.,2005,2006).
Althoughanalyticalmethodsvaryindetail,mostlabsconductanalysesusingmethods
similartothosedescribedherein.
UThPbgeochronologyofzirconisalsomaturebecausenumerouscalibrationstandards
havebeendocumentedandareavailable.Mostlabsuseoneofthesestandardsastheir
primaryreferenceforcalibrationofPb/U,andsomeuseothersassecondarystandardsto
ensurethatfinalagesareaccurate.StandardsinuseattheALCareasfollows:
SriLankazircon:Thisisaninhousestandardthathasbeenusedasourprimary
standardsince2005.ThecrystalwascalibratedoriginallybyIDTIMSinhouse,and
subsequentlybyCATIMSbyJimMattinson(resultsreportedinGehrelsetal.,2008).
Thecrystalhas518ppmUand68ppmTh,206Pb/204Pb=18,000,andaconcordantage
of563.52.3Ma(2).
Oracle:Thisisaninhousestandardthatweuseasasecondarystandardfor
Precambriansamples.ItconsistsofmoderatesizecrystalsthatyieldanIDTIMSageof
14348Ma.SamBowring(MIT)iscurrentlyconductingCATIMSanalysesonthese
crystalstodetermineamorereliableage.
FC52&FC1:ThesearelargezirconcrystalsfromtheDuluthGabbrocomplex,assumed
tobethesameageastheFC1/AS3samples(10992Ma)analyzedbyPacesandMiller
(1993)andSchmitzetal.(2003).
91500:Weusefragmentsofthissinglecrystal,whichhasanIDTIMSageof10655
Ma(Wiedenbecketal.,1995).
Peixe:Thisisaninhousestandardthatweuseasasecondarystandardfor
intermediateagesamples.ItconsistsofalargecrystalthatyieldsanIDTIMSageof
5644Ma.
R33:ThesesmallcrystalsyieldanIDTIMSageof419.30.4Ma(Blacketal.,2004).
Temora2:TheesmallcrystalsyieldanIDTIMSageof416.80.3Ma(Blacketal.,
2004).
Plesovice:Thesemoderatesizecrystalsyieldanageof337.20.4Ma(Slamaetal.,
2008).
Ecstall:Thisisaninhousestandardthatweuseasasecondarystandardforyoung
samples.ItconsistsofmoderatesizecrystalsthatyieldanIDTIMSageof91.51.0Ma
(Butleretal.,2002).
9435:Thisisaninhousestandardthatweuseasasecondarystandardforyoung
samples.ItconsistsoflargecrystalsthatyieldanIDTIMSageof55.51.5Ma(Klepeis
etal.,1998).
FishCanyonTuff:Thesesmallcrystalsyieldanageof28.500.04Ma(Schmitzand
Bowring,2001).Wecommonlyusethisasasecondarystandardforyoungsamples.
FollowingareexamplesofthetypesofUThPbgeochronologicanalysesconductedon
zirconattheALC.
PrecisionandAccuracy
AnalysisofthesestandardsbyLAICPMSprovidesinformationabouttheprecisionand
accuracyof206Pb*/238Uagesavailableusingthetwodifferentcollectorconfigurationsand
usingbothourNuPlasmaICPMSandourolderGVIIsoprobe.Figure2showstheresultsof
analysesofthesestandardsinseveraldifferentsessions.Eachsessionconsistsoften
analyses(nonerejected)ofeachstandardusingourSriLankazirconastheprimary
standard.Theweightedmeanofeachsetoftenanalysesisshownrelativetotheknown
ageofthestandard(inpercentoffset).Theuncertaintyofeachweightedmeanisshownat
the2level.
-3
-2
-1
49127 (136.6Ma)
R33 (419.3Ma)
91500 (1065Ma)
Figure2:AgeoffsetplotofzirconstandardsanalyzedbyLAICPMSusingbothinstrumentsat
theALC,withtwocollectorconfigurationsforeach.Eachboxrepresentstheweightedmean
of10analyses(withnonerejected),shownasthe%offsetofthismeanagefromtheknown
(IDTIMS)age.Theuncertaintyofeachsetisshownatthe2level.PlotfromGehrelsetal.
(2008).
206
Pb*/238U
FordatafromtheNuICPMS,theprecisionofeachsetoftenrangesfrom0.8%to4.0%,with
anaverageof1.9%.Thereisclearlyacorrelationbetweenprecisionandbeamsize(larger
beamsgenerateloweruncertainty),andbetweenprecisionandage(olderageshavelower
uncertainty).Intermsofaccuracy,theaverageoffsetofallanalyseswiththeNuICPMSis
0.11%abovetheIDTIMSages,whereastheaverageabsolutevalueoftheoffsetis1.1%.
Interestingly,severalofthestandardsyieldagesthatareconsistentlyshiftedrelativetothe
knownIDTIMSage.Thisyieldsanaveragereproducibilityof0.6%foreachset,whichis
considerablysmallerthantheaverageoffset.Suchsystematicshiftspresumablyresult
fromvariableconcentrationsoftraceelements(e.g.,Nd;Blacketal.,2004)thatinterfere
with206Pb.Variousexperimentsareinprogresstobetterunderstandthisinterference,
whichisclearlyoneoftheprimarysourcesoferrorinLAICPMSanalyses.
Thebottomlinefromthisanalysisisthat,forasetof10analysesofcogeneticzircons,the
uncertaintyoftheweightedmeanagewillaverage~1.9%,thefinalagewillbewithin1.1%
ofthetrueageonaverage,andtheaveragereproducibilitywillbesomewhatbetterat
0.6%.Theseareaveragevaluesfor206Pb*/238Uagesbetween28and1434Ma,expressed
atthe2level.
AnalysisofIgneousRocksWithSimpleSystematics
Figure3isanexampleofresultsthathavebeengeneratedonyoungzircons,where
206Pb*/238Uagesareusedtodeterminethefinalcrystallizationage.Thezirconsinthis
sampledonotshowevidenceofcomplexities(e.g.,Pblossorinheritance),andtheMSWD
of~1.0suggeststhatthegrainsmaywellbecogenetic.Itisaccordinglyappropriateto
determineanageforthesetofanalysesbycalculatingtheirweightedmeanand
uncertainty.
Asshownonthisplot,theinternalerror(precision)forindividualanalysesistypically0.5
1.5%(1).Theexternalerrorforthissample,1.2%(2),isalsotypical,andthesetogether
yieldatypicalfinaluncertaintyof~1.5%(2)forasetof~20analyses.
103
102
101
100
99
98
97
Final Age = 100.0 1.4%
96
Uncertainties at 2
MSWD = 0.90
95
Figure3:Exampleofanalysesfromanigneoussample,showingscatterandprecisionof
individualanalysesandrelativemagnitudesofinternal,external,andfinalerrors.Plotmade
withIsoplot(Ludwig,2008).
AnalysisofIgneousRocksWithComplexSystematics
UThPbsystematicsofzirconanalysesareinmanycasescomplexduetothepresenceof
Pbloss,inheritance,and/ormetamorphicovergrowths.ThespatialresolutionofLAICPMS
providesapowerfultoolforresolvingthesecomplexities.
Acommonstrategyfortacklingcomplexzirconcrystalsistodecreasethebeamsizetothe
pointwherenumerousanalysescanbeconductedineachagedomain.Figure4provides
anexampleofazircongrainfromtheCoastMountainsbatholiththathasbeenanalyzed
with140different10microndiameterlaserpits.WhencombinedwithaCLimage,this
techniqueofagemappingprovidesarichrecordofthehistoryofzircongrowth.Detailsof
agemappinghavebeenreportedbyJohnstonetal.(2009).
Laser pits
130 Ma inherited
130-160 Ma inherited
igneous core
metamorphic core
96.8 Ma igneous zircon
(high U and U/Th, has Pb loss)
(low U, no Pb loss)
57 Ma metamorphic
rim
100 microns
Figure4:Exampleofacomplexzirconcrystalthathasbeenanalyzedwith140ablationpits.
DatareportedbyGehrelsetal.(2009);CLimageacquiredwithassistancefromAxelSchmitt
(UCLAionprobefacility).
U/Thdataalsoprovidecriticalconstraintsontheconditionsofzircongrowth,withhigh
U/Thindicatingthatzircongrowthmostlikelyoccurredinthepresenceofmetamorphic
fluids(e.g.,Williams,2001;Rubatto,2002;Rubattoetal.,2001;HoskinandSchaltegger,
2003;Harleyetal.,2007).Fortunately,U/ThisgeneratedforeveryUThPbanalysis.
Figure4showstheutilityofU/Thonthescaleofasinglecrystal,withthepresenceof
metamorphicfluidsrecordedbyhighU/Thintheoldestandyoungestdomains.Figure5
showstheutilityofU/Thratiosinalargedataset,inthiscasefor~80plutonsintheCoast
MountainsbatholiththathavebeendatedbyLAICPMS.ThepatternofUPbagesyieldsa
recordofmagmaticfluxofthebatholith,whereasU/Thforthesedeterminationssuggests
thattwoofthehighfluxperiodswereaccompaniedbysignificantregionalmetamorphism.
Increasing flux
40
50
60
70
80
90
U/Th curve
206
238
100
110
120
130
140
150
160
170
180
Undivided core & rim analyses
Core analysis
Rim analysis
190
200
210
220
20
40
60
80
100
120
140
160
180
200
U/Th
Figure5:ExampleoftheuseofU/Thtoresolveperiodswhenmetamorphicfluidswere
generatedduringhighfluxmagmatismintheCoastMountainsbatholith(Gehrelsetal.,
2009).
AnalysisofDetritalZircons
LAICPMSisanidealtechniqueforUThPbgeochronologybecauseoftheabilitytoanalyze
crystalsofvarioussize,andbecausethehighefficiencyofdataacquisitionallowsfor
generationoflargedatasets.Thetwomainapplicationsofthetechniqueatpresentareto
determineprovenanceandmaximumdepositionalage.Fedoetal.(2003)andAndersen
(2005)havepublishedexcellentreviewsofdetritalzirconproceduresandapplications,
andthemethodsusedattheALChaverecentlybeendescribedbyGehrels(2010).
Followingisanexampleofeachofthetwomaintypesofanalyses.
Provenance
Figure6showstheagedistributionofdetritalzirconsthathavebeenanalyzedfrom
NeoproterozoicthroughCretaceoussandstonesexposedintheGrandCanyonandthe
adjacentColoradoPlateauofArizona(fromTimmonsetal.,2005;DickinsonandGehrels,
2003,2008a,2008b,2009a;andGehrelsetal.,inprep.).Showninverticalshadedbarsare
theinterpretedsourceregionsfromwhichdetritalzirconsareinterpretedtohavebeen
shed.Ofcoursesuchinterpretationsneedtobedevelopedandtestedrigorouslyandin
lightofmanyothertypesofinformation,butitisclearthatsuchagedistributionspresent
powerfulinformationabouttheprovenanceofclasticsediments.
Figure6:ExampleofthedetritalzirconagepatternsinsandstonesofMesoproterozoic
throughCretaceousageinnorthernArizona.DataarefromTimmonsetal.(2005),Dickinson
andGehrels(2003,2008a,2008b,2009a),andGehrelsetal.(inprep.).
Maximumdepositionalage
Determinationofmaximumdepositionalageonthebasisofdetritalzirconsisapowerful
tool,especiallyinrocksthatarenotfossiliferous.Suchdeterminationsmustbemadewith
caution,however,becausePblossmayhavecompromisedtheageoftheyoungestzircon
analyzed.Amoreconservativedeterminationisfromtheageoftheyoungestclusterof
ages,asitwouldbeunlikelyforPblosstohaveproducedaclusterofagesthatallaretoo
young(DickinsonandGehrels,2009b).
Figure7isacompilationofmaximumdepositionalagesforPhanerozoicstratafromthe
GrandCanyonandColoradoPlateauregionofthesouthwesternUS(modifiedfrom
DickinsonandGehrels,2009b).Zirconageisplottedagainsttheinterpretedabsoluteage
ofdeposition,whichisbasedonfaunalconstraintsconvertedtoabsoluteageusingtheOgg
etal.(2008)timescale.Theageoftheyoungestgrainisobvious,whereastheageofthe
youngestclusterisdeterminedfromtheweightedmeanageoftheyoungestclusterthat
hasatleastthreeageswhichoverlapatthe2level.Assumingthatthefaunal
determinationsareallaccurate,theyoungestsinglegrainclearlyistooyounginmany
cases,whereastheyoungestclusterconsistentlyprovidesareliablemaximumdepositional
age.
MAX DEPOSITIONAL AGE
350
300
250
200
Youngest Grain
Youngest Cluster
150
100
50
50
100
150
200
250
Depositional age (Ma)
300
350
Figure7:ExampleofthedeterminationofmaximumdepositionalagefromPhanerozoic
sandstonesoftheGrandCanyonandColoradoPlateauregionofthesouthwesternUS.
Acknowledgments:UThPbanalyticalmethodsattheArizonaLaserChronCenterwere
developedincollaborationwithJeffVervoortandVictorValencia.Supportforthis
developmentworkwasprovidedbyNSFEAR0732436.
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