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UThPbanalyticalmethodsforZircon

(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.

Age offset from ID-TIMS age (%)


-4

-3

-2

-1

U-Pb ages of standards


Fish Canyon Tuff (28.5 Ma)
9435 (55.5Ma)

Ecstall (91.5 Ma)

49127 (136.6Ma)

Plesovice (337.2 Ma)

Temora (416.8 Ma)

R33 (419.3Ma)

Peixe (564 Ma)

91500 (1065Ma)

FC1 (1099 Ma)

Oracle (1434 Ma)

Isoprobe: 35 micron beam, faradays


Isoprobe: 15 micron beam, channeltrons

Nu: 40 micron beam, faradays


Nu: 30 micron beam, faradays
Nu: 18 micron beam, ion counters
Nu: 14 micron beam, ion counters
Nu: 10 micron beam, ion counters

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

data-point error symbols are 1

102

101

100

99

98

97
Final Age = 100.0 1.4%

Weighted Mean Error = 0.7% Ma


Total External Error = 1.2%

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

~96 Ma igneous zircon


(high U, has Pb loss)

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

Pb/ U age (Ma)

100

110
120

130
140
150
160
170

Magmatic flux curve

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

Zircon age (Ma)

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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