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GoldintheSouthwestoftheIberianPeninsuladuringthe3rd MillenniumBC
F.Nocete a, *,R.Sáez b,M.R.Bayona a,J.M.Nieto b,A.Peramo a,P.López c,J.I.Gil-Ibarguchi d , N.Inácio a,S.García d,J.Rodríguez d
a GrupodeInvestigaciónMIDAS,DepartamentoHistoriaI(Prehistoria),UniversidaddeHuelva,Edif.MarieCurie,CampusdelCarmens/n, 21007Huelva,Spain
b DepartamentodeGeología,UniversidaddeHuelva,CampusdelCarmens/n,21007Huelva,Spain c Arqueólogo,C/PalmadelRíono24,4oB,41008Sevilla,Spain d ServicioGeneraldeGeocronologíayGeoquímicaIsotópica,FacultaddeCienciayTecnología,UniversidaddelPaísVasco,Apdo.644C.P., 48080Bilbao,Spain
articleinfo
Articlehistory:
Received16May2013
Receivedinrevisedform
18September2013
Accepted4October2013
Keywords:
Spain
3rdMillenniumBC
Goldprovenanceandmanufacturing
Laserablation
Leadisotopes
abstract
IntheSouthwestoftheIberianPeninsula,oneofthemaingoldminingregionsinWesternEurope,the presenceofthe firstgoldproductsarenotedinthearchaeologicalrecordsof3rdMillenniumBC megalithictombs,atsomedistancefromtheminingdistricts.Thelackofsystematicprogrammesto analysesucharchaeologicalgold findshasledthemtobeingidentifiedasornamental finds,ofundeterminedchronology,linkedtoasimplemanufacturingtechnologyofhammeringgoldnuggetsofan uncertainoriginorfromtheEasternMediterranean,aswellasitemswithapurelysymbolicor ‘prestige’ valueinthefunerarypracticesofsimplegroup-orientedorcollaborativechiefdoms.Buthowever,the firstdocumentation,radiocarbondatingandsystematicanalysisoftheseproductsinsettlementcontexts hasalteredthisinterpretation.
Thepresenceofgoldmanufacturesduringthethirdquarterofthe3rdMillenniumBC(c.2500 2350cal.BC)inthecontextsofasettlementspecialisedincopperproductionsuchasCabezoJuré,in theSouth-westernminingregion(Huelva,Spain),andinthecontextsofahugecentralsitesuchas ValencinadelaConcepción,intheagrarianregionoftheLowerGuadalquivirBasin(Seville,Spain),points tothewidespreadsocialuseofgoldintheperiodofmaximumexpressionoftheinter-settlement hierarchisationintheSouthwestoftheIberianPeninsula,itslinkwiththesocialspacesofinequality expressionandtheirrelationshipwithacomplexproductionsystem.Geochemicalcharacterizationby LA-ICP-MS,leadisotopesanalysisbyMC-ICP-MSandmetallographicstudysuggesttwodifferentiated andindependentsuppliesofrawmaterialsystems(fluvialplacersvs.minesandlocalvs.regionalscale), withatleastfoursourceareas,theregionalcirculationofrawmaterialorproductsandamanufacturing byametallurgicaltechnologylinkedtothecopperproduction.
2013ElsevierLtd.Allrightsreserved.
1.Introduction
Goldhasbeenasymbolofexcellenceandusedasanexpression ofstatusandpowerinsomemodernandprehistoricsocieties (Clark,1986;MorteaniandNorthover,1995;Tylecote,1987;etc).Its rolewasveryimportantinthereproductionofthe firstinequalities andthe firstpoliticalsystems.SuchisthecaseofPrehistoric WesternEuropeduringthe3rdMillenniumBC,wheregoldproducts,inallcasesinornamentalforms,becamewidespreadinthe burialcontextsofthecentraltombsofthemainsettlements
* Correspondingauthor.
E-mailaddress: nocete@dhis1.uhu.es (F.Nocete).
0305-4403/$ seefrontmatter 2013ElsevierLtd.Allrightsreserved. http://dx.doi.org/10.1016/j.jas.2013.10.006
(Chapman,1990;Eluere,1995;Renfrew,1978),coincidingwiththe emergenceofthe firstinter-settlementhierarchicalsystems (Nocete,2001).However,themainquestionsintheinterpretation ofgoldinthesesocietiesconcernstheabsenceofaprecisechronologyofthisprocess,theabsenceofcontextsinthesettlement linkedtotheuseandproductionofthegoldartefactandaprecise characterizationoftheirmanufacturingtechnologybesidesthe sourceoftherawmaterialanditscirculation.
Sincethe firststudiesby Hartmann(1982),over4000goldobjectsinEuropeanalysedbyopticalemissionspectroscopy,aswell assubsequentdatabases(Pingel,1995),moreprecisescientific methodologieshavebeendevelopedtocharacterizethetechnologicalprocessesandthesourceoftherawmaterialsusing
elementalgeochemistrybyLA-ICP-MSandleadisotopesbyMCICP-MS(Baronetal.,2011;Bendalletal.,2009;Chapmanetal., 2006;Ehseretal.,2011a;GuerraandCalligaro,2003,2004; Guerraetal.,1999;Kovacsetal.,2009).Buthowever,suchmethodologieshaveneverbeenappliedtoarchaeologicalgold finds which,forthemostpart,derivefromsurface findingsordecontextualizedburial.SuchwasthecaseintheSouthwestoftheIberianPeninsula.
Thispaperpresentsthe firstsystematicstudyofgoldproductsin settlementcontextsfromthe3rdMillenniumBCintheSouthwest oftheIberianPeninsula,usingelementalgeochemistrybyLA-ICPMS,leadisotopesbyMC-ICP-MSandmetallographicandchronological(byC14 AMS)analyses.
2.GoldintheSouthwestoftheIberianPeninsuladuringthe 3rdMillenniumBC:archaeologicalbackgroundandnew perspectives
TheSouthwestisaspatialareawherecoincidethehighest concentrationofarchaeologicalgold finds(Chapman,1990; Hernando,1983)andthelargestinter-settlementhierarchicalsystemoftheIberianPeninsuladuringthe3rdMillenniumBC (Chapman,2008;Nocete,2001)andoneofthemostimportantgold miningregionsinWesternEurope(Domergue,1970;Emmons, 1974;Lehrberger,1995;Pingel,1992,1995;Porteretal.,1989).
Goldispresentinprimarymineralizationassociatedwithquartz, suchastheminesofCala(Huelva,Spain)andHornachuelos (Córdoba,Spain)intheOssa-MorenaZone(OMZ)(Lehrberger,1995), inoxidizedfacies(gossan)ofmassivesulphides,suchastheminesof Riotinto,Tharsis,LaLapilla,Sotiel,etc.(Huelva,Spain)intheSouth PortugueseZone(SPZ)(Garcíaetal.,2005;Lehrberger,1995)andin fluvialplacerslinkedtothem,suchastheTintoRiver(Peña,1917;M. Leblanc,personalcommunication).Incontrast,thearchaeological gold findsofthe3rdMillenniumBCderivefromsurfaceordecontextualized findingsofcentraltombsinthelargesettlementsthat hierarchizedagrarianterritoriesatadistancefromtheminingdistricts,suchasinthetomb4ofAlcalar(LeisnerandLeiner,1943,1959; Veiga,1886,1889),the hipogeo ofLosAlgarves(Possac,1975),the tombsofCañadaCarrascal(Harrison,1977),CañadaHonda (Berdichewsky,1964)andLasCanteras(HurtadoandAmores,1984) closetotheElGandulsettlementand,lastly,thetombsofLaPastora (Almagro,1962;LeisnerandLeiner,1943,1959),Matarrubilla (Collantes,1969),LasCabezas(FernándezandRuiz,1978),LosVeinte (Fernández,1984),SeñoríodeGuzmán(ArteagaandCruz-Auñón, 1999;Lacalleetal.,2000)andMontelirio(FloresandAycart,2013) inthehugesettlementinthisarea:ValencinadelaConcepción.
Despitethat,nocomparativeanalyseshaveeverbeenconducted ontheregionaloredepositsandarchaeologicalgold finds,while thecharacterizationofthelatterhasbeenlimitedtogeochemical informationleadingtosemi-quantitativeconcentrationsofboth majorandminoralloycomponents(Au,Ag,CuandoccasionallySn) byopticalemissionspectroscopyandSEMon fiveleafsbelongingto surfaceandoldexcavationsof fiveofthetombs:Alcalar(Hartmann, 1982),Matarrubilla(Hartmann,1982;Pereaetal.,2003,2010),La Pastora(Pereaetal.,2010),CañadaHonda(Hartmann,1982)and CañadaCarrascal(Hartmann,1982).
Withthisinformation,thepresenceofgoldproductsinthe societiesoftheSouthwestoftheIberianPeninsulainthe3rdMillenniumBChavebeeninterpretedasitemsofornamentations(of clothing,artefactsorofindividualsthemselves)associatedwitha purelysymbolicor ‘prestige’ valueinthefunerarypracticesof simplegroup-orientedorcollaborativechiefdoms(Chapman, 2008).Asregardstheirproduction,asimplemanufacturingtechnologybasedonamechanicalprocessinvolvingcoldhammering and,atalaterdate,lowtemperatureannealing(Hernando,1983;
Pereaetal.,2003,2010;Soaresetal.,2004)goldnuggets,ofuncertainand/orcontroversialorigin.Whilefor Hartmann(1982) the presence/absenceofSnwouldidentifygoldofalluvialorigin(Type S:CañadaHondayCañadaCarrascal)vs.frommines(TypeB: AlcalaryMatarrubilla)andalocaloriginfortheformerandasource intheEasternMediterraneanforthelatter;for Pereaetal.(2003, 2010),sincethepresenceofAu/Agalloysiscommonandin variousproportioninprimarymineralizationandplacers(Hough etal.,2009),thescarcepresenceofAg(<2%)atMatarrubillaand LaPastora(TypeBforHartmann)suggestedanalluvialoriginof unknownprovenance.
Withthisarchaeologicalbackground,thisinterpretationturns outtobeinsufficient.Itdependsnotonlyonthenumberofsamples analysedbutalsoontherepresentativenatureofthesame(asthey belongtoallthesurfaceandfunerarycontextswithanimprecise chronology).Italsodependstothelackofprecisionofoptical emissionspectroscopyandSEMforestablishingtheoriginofaraw materialorthetechnologicalprocessofmanufacturing.Itdepends tootothelackofcorrelativeinformationoftheregionaloredeposit andtotheneedtoexplainhowtheproductionofgoldartefactswas conductedusingsuchasimpletechnology,whenthesesocieties appliedsuchcomplexmetallurgicalproductiontechniques(mineralreduction,smeltingandmouldcasting,thermalandmechanicaltreatmentprocessesforcopper)andsufficientfortheir handling.
Inordertobeabletodevelopamoreefficientinterpretation, newsamplesofgoldareneededtobeabletoestablishaprecise chronology,givemeaningtosocialcontexts,onthesettlements, alternativestothefunerarydepositions,correlateinformationon theproductiontechnologyofcopperandgoldartefacts,compare informationonthepotentialminingterritoriesandonthemost efficientanalyticalmethodologiesinordertodeterminesourceand technology.Toachievethis,wehavesixarchaeologicalgold findsin theregion,inthecontextsoftwosettlementsdatingfromthe3rd millenniumBC(Fig.1):CabezoJuré(Huelva,Spain),asettlement specializedincopperproduction,locatedclosetoaminingarea fromtheSPZwithoxidizedfacies(gossan)ofmassivesulphides thathavebeenexploitedfortheirgolduptorecenttimes(minesat Tharsis,LaLapilla,FilónSur,Almagrera)andValencinadelaConcepción,thehugesettlementinthehierarchicalframeworksettlementintheagrarianterritoryoftheLowerGuadalquivirBasin(Seville,Spain)andtowhichthetombswiththegreatest presenceofgoldproductsareascribedinthesouthoftheIberian Peninsula(LaPastora,Matarrubilla,LasCabezas,LosVeinte,Señorío deGuzmánandMontelirio(seesupra)).
Thesesixarchaeologicalgold findshaveanenormousvaluefor theexplorationoftheeconomicandpoliticalcontextofgold productswithinthe firsthierarchizedsocietyintheSouthwestof theIberianPeninsuladuringthe3rdMillenniumBC.Firstly,they are,atpresent,theonlycontextualizedsamplesabletoprovide directchronology.Secondly,theyaretheonlyonesthat,bybeing relatedtospecialnon-funerarycontextsandinsettlementareas wherecopperproductionispresentathighlyspecializedlevels (Bayona,2008;Nocete,2004,2006;Noceteetal.,2008,2011a,b; Sáezetal.,2003),makeitpossibletocorrelatetheresultsoftheir analysiswiththoseofcoppermetallurgyandtoevaluatethesimilitudes,differencesandpossibletransfersinthemanufacturing technology.Thirdly,becausesincetheybelongtosettlements locatedbothinsidethegoldminingregion(CabezoJuré)andinat somedistancefromit(ValencinadelaConcepción)intheLower GuadalquivirBasin,theymakeitpossibletoevaluatethepresence oftechnologicaldifferencesinproductionandthesourceandcirculationoftheoresand/orproducts.Fourthlyandlastly,becauseas theyentailtwodifferentiatedmodelsofsettlementintheintersettlementhierarchicalsystemoftheSouthwestoftheIberian
Peninsulaofthe3rdMillenniumBC,theymakeitpossibleto exploringtheeconomicandpoliticalimplicationsthattheproduction,useandcirculationofgoldproductscouldhaveinvolved.
3.Material
Forthepurposesofourstudy,weselectedatotalofsix contextualizedsamplesofgoldfromthesettlementsofCabezoJuré andValencinadelaConcepción.
AtCabezoJuré,andfollowingtheexcavationofover50%of thissettlement(c.2ha),fourgoldleafshavebeendocumented which,inviewoftheirmorphologiesandsizes(Table1 and Fig.2:MIDAS378,434,435y506),couldberelatedtovarious ornamentationsofclothing,artefactsoroftheindividuals themselves(bracelets,singlehairring,singlehairribbon).All thesewererecordedinsideafortifiedenclosure(Fig.3)locatedin theupperpartofthesettlement,wherethearchaeologicalcontextssuggestthepresenceofaresidentialareabelongingtoa socialgroupwhich,withoutparticipatingdirectlyinmetallurgicalproduction,headedsaidproductionfromtheaccumulation ofproductsandthroughthecontrolandexclusiveownershipof theideographicrepresentations(terracotta figurines),themeans ofdestruction(weapons,fortification)andstorage(cisternand largepotterycontainer)ofwaterandfoodstuffs,andenjoyed exclusiveaccesstofoods(marinemolluscs)andproducts(oolitic limestoneblades,pottery,marblecupandvariscite)fromoutside (Nocete,2001,2004,2006;Noceteetal.,1995,2011a).
AttheValencinadelaConcepciónsettlement(ca.300ha),and followingresearchintoseveralhundredstructures,onlytwo archaeologicalgold findshavebeendocumented.The firstwasa leafsimilartothoseidentifiedatCabezoJuré(Table1 and Fig.4: MIDAS487)associatedwiththreelargecopperaxes(weighingover 4kg)inaresidentialarealocatedinthecentreofthesettlement (LópezandPajuelo,2013),withnolinktoproductionactivities whatsoever,exceptforthehandlingoffoodstuffs.Initssurroundingsaregroupedspacesdevotedtostoringlarge(c80cm)tuffite nodules-platformforprismaticbadecores(Noceteetal.,2005)and
Fig.1. LocationofthesettlementsatCabezoJuré,ValencinadelaConcepciónandthemineatLaSultanaongeologicalcartography. Table1tohousingideographic figurines(traditionallyknowas “idols”) madeinlimesrocks(Fig.5).Thesecond,acastingspill(regulus) (Table1 and Fig.4:MIDAS505)associatedwithacontextof metallurgicalactivityinvolvingcopperproduction,withthepresenceofcopperslagandcrucibles,locatedonthenorthborder (Lópezetal.,2001)ofsectorVinitsmetallurgicalarea(Noceteetal., 2008,2011b).
Finally,wehaveincludedinthisstudyaseventhsample(Figs.1 and 6:MIDAS343).Thisisprimarygold,associatedwithquartz, collectedinaminelocatedbetweenbothsettlementsandinthe contextsofOMZ:LaSultana(Cala,Huelva: Fig.1).Thisinclusionin theanalysisisaimedathavinginformationavailableonprimary mineralizationwiththickgrainsizedgold,locatedinthestudied area,inordertocontrastpotentialcatchmentareas.
4.Method
Inordertohavepreciseinformationavailableonchronology,on thesourceofthe “fingerprint” andonthemanufacturingtechnologyinvolvedinthesegoldproducts,wehaveselectedfourmethods ofanalysis:1)directchronologybyC14 AMS;2)opticaland metallographiccharacterization;3)geo-chemicalcharacterization byLA-ICP-MSand4)isotopiccharacterization(Pb)byMC-ICP-MS.
4.1.DirectchronologybyC14 AMS
Inordertoevaluatethedirectchronology,weselectedseven samplesoforganicmatterfromthedepositionalcontextsofthe goldproductsatCabezoJuréandValencinadelaConcepciónfor
Fig.2. GoldleafsfromCabezoJuré.datingwithC14 AMS.Thesampleswereextractedfrombranches withadiameteroflessthan1cmofasinglevegetablespecies (QuercusIlex)associatedwithdomesticcontextswherefoodwas produced.Allsampleshavebeenpreparedandmeasuredinthe AngströmLaboratory(Uppsala,Sweden)usingtheprocedures outlinedin BronkRamseyetal.(2004a,b,2009).Inaccordancewith internationalradiocarbonconvention,alldatesareexpressedin radiocarbonyearsbefore1950A.D.(yearsBP)usingthehalf-lifeof 5570years.Errorsarequotedastwostandarddeviations(1s and 2s)andarebasedonanassessmentofallcontributionstoerrorsin thelaboratoryisotoperatiomeasurement.Naturalfractionationof carbonisotopesisaccountedforbymeasuringthe d13Cvaluesto PDB.Allcalendardatesquotedhavebeencalibratedusingthe
OxCal4.0computerprogrammeby BronkRamsey(2006) andCalPal2007(-www.calpal-online.de-B.Weninger,O.Jörisch&U. Danzeglocke),usingatmosphericdatafrom ‘INTCAL09’ (Reimer etal.,2009),andarequotedto95.4%probability(Table2).Finally, theresultswerecorrelatedwiththeonlyC14 AMSchronometric databaseavailableonarchaeo-metallurgicalcontextsfromthe SouthwestoftheIberianPeninsulaandtheGuadalquivirBasin (Noceteetal.,2011b).
4.2.Opticalandmetallographiccharacterization
Thesurfaceofallthearchaeologicalgold finds(Table1)was observedbyStereozoomMicroscopeNIKONSMZ-10A.Inthecase
Fig.4. Goldleafandcastingspill(regulus)fromValencinadelaConcepción.ofthesampleMIDAS505(castingspill),andinordertoexplore itstexture,thewholesamplewasmountedonadoublefaced carbonadhesiveconductingbase,andwascharacterizedbyimagesofsecondaryelectronsinconditionsof20kV/20nAsensor currentinanElectronProbeMicroAnalysis(EPMA)JEOLJXA8200 SuperProbe.Forthestudyoftheinternalmetalstructure oftheproducts,itwasdecidedtoapplyamicro-structural analysisusingmetallographicmicroscopy,ontwoleafsfrom thesettlementsofCabezoJuré(MIDAS434y435)andonefrom ValencinadelaConcepción(MIDAS487).Thesampleswere mountedwithresininmouldsof300mmdiameterandwere ground(abrasivegrainsizeof#600 4000)andpolished(diamondpasteof3 mm/solidsolutionofMgO).Forthemicrostructuralobservationofthemetalbymeansofametallographic microscope,thesampleswereattackedwithetchingsolutionsof ammoniumpersulfate((NH4)2S2O8)andpotassiumcyanide (KCN)inaqueoussolution.Metallographicobservationwas conductedusinganinvertedmetallographicopticalmicroscope NIKONEPIPHOT(100 1000 )(see Bayona,2008;Calvo,1972; Noceteetal.,2008;Scott,1991 fordetails).
4.3.Geo-chemicalcharacterizationbyLA-ICP-MS
Elementalanalysesofarchaeologicalgoldsampleswereconductedbylaserablationinductivelycoupledplasmamassspectrometry(LA-ICP-MS)attheGeochronologyandIsotope Geochemistry-SGIkerfacilityoftheUniversityoftheBasque
Country(Spain).Goldsampleswerecleanedwithultrapurewater andsetona25mmdiameterresinmountwithdoublesidedadhesivetape.Theanalysesinvolvedtheablationofthegoldwitha UP213Nd:YAGlaserablationsystem(NewWave)coupledtoa ThermoFisherScientificXSeries2quadrupoleICP-MSinstrument withenhancedsensitivitythroughadualpumpingsystem.Instrumentandoperatingparametersusedaregivenin Table3.Spot diametersofca.100 mm(nominalsize, Fig.7)associatedwith repetitionratesof10Hzandlaser fluenceatthetargetofca.5J/cm2 wereusedforthegoldanalysis.Apre-ablationwasconductedto removesurfacecontamination,followedbyablationduring60s. Theablatedmaterialwascarriedintoheliumandthenmixedwith argon.Theprocedureappliedwasbasedonthatdescribedby Kovacsetal.(2009),i.e.,usingtheso-called ‘wetablation’ which,in thiscase,involvedtheuseofaPeltierrefrigeratedspraychamber andaPFAmicronebulizertointroducecalibrationsolutionsof knownconcentrationforthequantificationoftheelementsofinterest(see Kovacsetal.,2009 fordetails).TuningandmasscalibrationwereperformedusingtheNISTSRM612referenceglass,by inspectingthesignalof 238Utoobtainca.1,400,000cps/mgg 1 and byminimizingtheThOþ/Thþ ratiotoca.1.5%.
Oneofthemainproblemsintheelementalanalysisofgold-rich archaeologicalsamplesbyLA-ICP-MSmethodsistheabsenceof certifiedstandardssimilarinnaturetothoseinvestigated.To guaranteethereliabilityoftheresultsobtainedinourstudywe haveemployedavarietyofapproaches.Firstly,afterapropertuning andmasscalibrationoftheinstrument,wehaveverifiedthatthe amountsofAuandAg,thatis,thepotentialmaincomponentsof thearchaeologicalunknownswerecorrectlymeasured.Thiswas achievedbytherepeatedanalysisoftheNISTSRM481standard whichconsistsofsixgold-silveralloyswithdifferentamountsof thetwometals.Usingtheconditionsdescribedabove,theanalysis oftheNISTsilver-goldwiressatisfactorilyreproducedthecertified valuestolessthan1%SE.Asforthetraceelementcontents,weused adoublestrategy.Ononehand,bymeansofthesilicateNISTglasses forwhichthereisabundantinformationofmajorandtraceelement composition.ThisisastandardprocedureinmanyLA-ICP-MS studieswhennostandardsareavailableofmatrixcomposition similartothatoftheunknowns.Inthepresentcase,themethod employedprovidedtraceelementresultswithinlessthan20% deviationfromthereportedvalues(Jochumetal.,2011)whichis normallyregardedasacceptableinthistypeofanalysis.Atthe sametime,weusedasecondarystandardconsistingofa commerciallyavailablegoldfoil(AlfaAesar14721-FF)whose compositionwascarefullyestablished(<10%errorforalltheelementsdetermined)bysolutionICP-MSusingthemethodofstandardaddition.Oncewehadverifiedthevalidityandrepetitivityof themethod,wehaveselectedanumberofelementsfortheir quantificationonthebasisofpreviousstudiesonAuprovenancein archaeologicalremains(e.g. Ehseretal.,2011a;Kovacsetal.,2009; Schlosseretal.,2009,amongothers).Thecalculationofthe
Fig.6. NativegoldfromLaSultanamine. Table2Table3
OperatingconditionsoflaserablationICP-MS.
ScanningmodePeakhopping,1pointperpeak AcquisitionmodeTRA(TimeResolvedAnalysis) Analysisduration90s(30sbackground,60ssignal)
concentrationswasdoneassumingthattheanalysisincludedall theelementspresentinthesample.Aminimumof3 6spotswere analysedoneachgoldsample.Spotsusingdiameterslessthan 100 mm(Fig.7)yieldedsignificantlyincreasederrorsandhavenot beentakenintoaccount.Theresultsaregivenin Table4.
4.4.Isotopiccharacterization(Pb)byMC-ICP-MS
LeadisotopeanalyseswereperformedattheGeochronologyand Geochemistry-SGIkerfacilityoftheUniversidadofthePaísVasco UPV/EHU(Spain).Thegoldsampleswerecleanedovernightinhot, nitricacidconcentrate,rinsedwithultrapurewaterand finallydissolvedin aquaregia.LeadwasextractedbyconventionalionexchangechromatographyinHBr HClmedia;allemployedreagentsweretriple-distilledatsub-boilingtemperaturebeforeuse. PbisotoperatioshavebeenobtainedusingaNeptuneMC-ICP-MS instrumentwiththethalliumcorrectiontechnique(Walderetal., 1993),followingproceduressimilarto Chernyshevetal.(2007) DuetothelowPbcontents,sampleswereintroducedintothe plasmathroughanApexIRinletsystem(ElementalScientific,USA). TheaccuracyofthemethodwasconfirmedbyanalysisoftheNBS 981leadisotopecertifiedreferencematerialatsimilarconcentrationstotheunknownsamples.Theresultsaregivenin Table5
5.Resultsanddiscussion
5.1.DirectchronologybyC14 AMS
ThestudyusingC14 AMS(Table2)providesthe firstpreciseand directchronologicalinformationonthepresenceofgoldproducts
intheterritoryoftheIberianPeninsula,withthegreatestconcentrationofthesame(theSouthwest):thethirdquarterofthe3rd MillenniumBC(c.2500 2350cal.BC).Althoughtheabsenceof othercontextsdateddoesnotmakeitpossibletodiscardthe presenceoftheseproductsinpreviousphases,weshouldpointout thatthischronologycoincideswiththemaximumexpressionof inter-settlementhierarchizationinthissociety,withtheconstructionofitsmostmonumentaltombs,withthedevelopmentof itsmostintensivecopperproductionactivityaswellaswiththe stagetheprecededitspoliticalcollapsebyc.2400BC(Noceteetal., 2010,2011b).Asregardsthislatterstage,wepointoutthatin CabezoJuréandValencinadelaConcepción,thepresenceofthese goldproductsisassociatedwithcontextsofsuddenabandonment thatmarkedtheinterruptionoftheoccupationalsequence;contextsthatweretogiverisetonewmodelsofspatialorganization involvingadrasticreductionoftheirrespectivehabitatandadeep economicandsocialchange.Butontheotherhand,thischronologicalidentitybetweenbothsettlementshasanaddedvalueasit makesitpossibletodrawplausibleconclusionsfromacomparative studyofthesame.
5.2.Opticalandmetallographiccharacterization
TraceologicalanalysisofthegoldleafsfromCabezoJuréand ValencinadelaConcepciónsuggestsahighdegreeofuniformity, sinceinallcases,wecantalkofproductsmadeoncarefullyworked, highlyhomogeneouslaminatewithnoevidentmanufacturing faults.Polishingbyabrasiononbothsidesandhammeringinorder toregularizetheedgeswerethemain finishingmethodsused.On theendsoftwosamplesareperforationsmadewithcircularsection(Fig.2:MIDAS378)punchingandcutting(Fig.2:MIDAS506) tools.Thetechniquesusedandthesmallthicknessesachieved, especiallythoseintheMIDAS506sample(Fig.2),defineacomplex manufacturingprocesswheretheedgesshowaparallellineof cuttingpre-tracingandstraight,clearlyvisiblemarksonthesame. Microstructuralanalysisusingametallographicmicroscopealso suggestsaconsiderableuniformityinthemanufacturingprocess, aswellasitscorrespondencewiththoseusedintheproductionof copperproducts.ThesampleMIDAS434presentsatypicalmetal andFCCalloystexture(FaceCentredCubic)subjectedtosequences ofmechanicaldeformingandthermalprocesses.Herethesmall sizeofthecrystals,theirirregularappearance,theirchaotic arrangementanddisplayoftwincrystals,strainlinesandcurvilineargrainedgessuggesttheforceandreiterationofforgingworks (Fig.8A).ThesampleMIDAS435alsoshowsthealternation
betweenthermalandmechanicaltreatments.Thephotomicrographsobtainedshowarecrystallizationstructurewithaprofusion ofintragranulartwinnedcrystals.Here,thesizeofgrainthedeficientdefinitionofsomeedgesofcrystalsandthescarcedeforming oftwinnedgrainssuggestaninsufficientannealingoperationtobe abletofullyhomogenizethestructureofthisleaf,followedbya slight finaldeformation(Fig.8B).Finally,thesampleMIDAS487 allowsustonoteamonophasicstructureoflargesizedequi-axial crystals.Herethedislocationofthecrystallinenetworkandthe moderatedeformationofthetwinnedcrystalstowardstheedgeof theleafmakeitpossibletointerpretamechanicaltreatmentsubsequenttotherecrystallizingofthemetalstructure(Fig.8C).
TechnologicalanalysisofthecastingspillfromValencinadela Concepción(Fig.4:MIDAS505)bymeansofElectronMicroprobe (EPMA),showacolumnardendriticstructureaswellastheformationofaprimarycrystallinetextureoftriplepointcasting (Fig.9).Itsuggeststheformationofacastingprimarycrystalline structureoftriplepoints,indicatingconditionsofsolidification subsequenttothecastingprocessaffectedbyaheterogeneous coolingspeedofthismetalmass(dendritesvs.crystals).Thismay indicateasub-productfromametallurgicalprocessformedafter thecastingofthemetalmassofoneorseveralgoldnuggetsina crucible,similartothoseidentified,fromalaterdate,incontextsof the2ndy1stmillenniumBC(Bozonietal.,2003;Gebhard,1995; Pereaetal.,2010).
Onthisbasis,wecaninferthat,despitetheductilityand malleabilityofgold,ofitslowhardnessandthelowtemperatureof recrystallization,qualitiesunalteredbecauseoftheirAgalloycontentintheproportionsrecorded(Houghetal.,2009;Pingel,1995), thehighreductionsofthicknessnotedinthesamplesanalysed builtuptensionsandbehavioursinthemetalstructurethatrequire therotationofthermalandmechanicaltreatments(Chastainetal., 2011)tothoseidentified,bothatCabezoJuréandatValencinadela Concepción(Bayona,2008;Noceteetal.,2008)forthemanufacture ofcopperproductsfromthedawnofthe3rdmillenniumBC (Noceteetal.,2011b).
5.3.Geo-chemicalcharacterizationbyLA-ICP-MS
ThevaluesofAu(>85%),Ag(<15%),Cu(<1750 mgg 1)orPb (<21 mgg 1)forallthegoldproductsanalysedatCabezoJuréand ValencinadelaConcepción,aswellastheircorrelationwiththe primarygoldfromtheLaSultanamine(Table4),suggestanative gold(Chapmanetal.,2006;GuerraandCalligaro,2004).Nevertheless,thedifferencesinMg,Ni,Sb,Pb,Pd,PtandBi,butparticularlyinTiandSn,suggestsupplysystemsdifferentiatedbetween CabezoJuréandValencinadelaConcepción(Table4).
Thepresenceoftin,testedasthemainindicatorofthealluvial originofthegoldbytheincorporationofcassiteritein fluvial placers(Costantinescuetal.,2012;Esheretal.,2011a;Guerraand Calligaro,2003;Hartmann,1970,1982;Houghetal.,2009),inall thesamplesatCabezoJuré(Table4:Sn198 3896 mgg 1),suggests analluvialoriginofthegoldusedinmanufacturingproductsthere. ThenotablepresenceofTiinoneofthesamplesfromthissite (Table4:MIDAS506Ti1069 6505 mgg 1)mayalsobeconsidered asanotherexampleofalluvialoriginbytheinclusionofTi-oxides (Esheretal.,2011b).AlthoughthereductionofTi-oxidestype RutileandIlmeniteonmetalTiisnotpossibleattemperaturesthat canbereachedwithcoal,thismarkedpresenceshouldbe explained.Twopossibilitiesareopen:1)thattheyaresmallinclusionsofTi-oxides,althoughthiscouldberejectedduetothe homogeneityoftheanalyticaldatafromthesample;2)thatalluvial incorporateisnotintheformofoxideswithhighcrystallinity (Rutile Ilmenite),butratherintheformofproductsalteredonthe surface(Leucoxene),presentinglowerfusionpoints.
Table5
ResultsoftheleadisotopesanalysisinthegoldsamplesfromCabezoJuré,ValencinadelaConcepciónandLaSultana.
CabezoJuréSettlementGoldLeafMIDAS37818.1860.00215.6230.00238.1860.0042.09970.00010.85910.0001 CabezoJuréSettlementGoldLeafMIDAS43518.1890.00315.6280.00338.1940.0072.09910.00010.85920.0001 CabezoJuréSettlementGoldLeafMIDAS43418.3570.00315.6530.00238.5610.0062.10010.00010.85260.0001 CabezoJuréSettlementGoldleafMIDAS50618.5500.00515.6810.00538.7030.0142.08630.00010.84530.0001
ValencinadelaConcepciónSettlementGoldLeafMIDAS48718.3540.01615.6600.01338.5060.0342.09790.00030.85320.0001
ValencinadelaConcepciónSettlementCastingspillMIDAS50518.4530.01915.6630.01738.5850.0422.09090.00040.84810.0001 LaSultanaMineGoldOreMIDAS43618.5190.00115.6500.00138.5010.0032.07890.00010.84510.0001
Buthowever,andalthoughthedifferencesinMg,Ti,V,Mn,Co, Ni,Cu,Zn,As,Se,Ag,Cd,Sb,Te,PtoBi(Table4:MIDAS378,435,434 vs 506)atleastsuggestdifferentalluvialprovenancesatCabezo Juré,thevaluesofoneofthePlatinumGroupElement(PGE) associatedwithgold,suchasPd(<1.2 mgg 1),mayalsopointtoa possiblerelationshipwiththemassivesulphidedepositfromthe IberianPyriteBelt(IPB)intheSPZ,wherethePdcontentsarebelow 5 mgg 1 (Pasavaetal.,2007).Inthisregard,thelocationand exploitation(forcopperproduction)ofCabezoJuréononeofthe mainsourcesofthealluvialgold(Esheretal.,2011a),suchasthe auriferousgossansfromLaLapilla-Tharsis,aswellasthepresence ofcassiteriteinthem(Capitán,2006;Capitánetal.,2003),could pointtothepossibilityofadirectsupply,atlocalscale,forthis settlement.
Incontrast,thevaluesofSn,TiandthePGEintheValencinadela Concepciónsamples(Table4)suggestdifferentsupplysystemsand environments.Ontheonehand,thecontentsinPd(>27 mgg 1)in oneleaffromValencinadelaConcepción(Table4:MIDAS487) couldindicateasupplyarealocatedoutsidetheSPZ(Pasavaetal., 2007)andmayberelatedtotheOMZwheremines,suchasthat ofLaSultana,presentvaluesofPd > a5 mgg 1 (Table4:MIDAS 436).Ontheotherhand,theabsenceortestimonialpresenceof titaniumandtininthesamplesfromValencinadelaConcepción (Table5:MIDAS487and505),eventhoughthisdoesnotallowus todiscardanalluvialoriginin fluvialcourseswithnocassiteriteor Rutile Ilmenite Vs Leucoxene(see supra),suggestsapossible supplyofprimarygoldfrommine.Inthisregard,thesimilitudeof productsfromValencinadelaConcepciónandLaSultanamine (Table4)inthevaluesofrelatedelementsastracersofprimary minegold,suchasSb(Constantinescuetal.,2012)oBi(Chapman etal.,2006;Houghetal.,2009),andidentifiedintheOMZ (Garcíaetal.,2005),alsosuggestapossiblerelationshipbetween bothsamples.Ifthisrelationshipisconfirmed,thedistantlocation ofValencinadelaConcepciónintermsofthesepotentialsourcesof goldsupplycouldidentifyaregionallevelofcatchmentwhich, dependingontheirdifferencesinFe,Ni,Cu,Zn,As,Pd,Ag,Te,oBi (Table4:MIDAS487vs505),wouldhaveseveralsources,oneof whichpossiblybeingLaSultanamine.
Thedatacontributedbythisstudyaffordanadditionalreading thatconcernstheproductionprocessoftheleafsfromValencinade laConcepciónandCabezoJuré,suggestingtheirpossiblerelationshipwiththemetallurgicalcoppertechnologyinbothsettlements.
InCabezoJuré,therelativelyhighSnconcentrationinthreeof itsproducts(Table4:MIDAS378,435and434:Sn > 3000 mgg 1) suggeststhatthegoldleafsmayhavebeenproducedfromalluvial goldbysinteringormeltingunderreducingconditions(Chapman etal.,2006;Dube,2006;Esheretal.,2011a)andmaybe explainedbytheincorporationofalluvialcassiteriteintothe smeltingcharge(Hartmann,1970,1982).Alongsidethis,therelativelyhighTiconcentrationinthefourth(Table4:MIDAS506:Ti 1069 6505 mgg 1)maysuggestasimilarprocessiftheinclusions notedwereoftheLeucoxenetype(see supra).Inaddition,the identityinalloftheelementalvaluesintwodifferent(in
morphology,width,thicknessandsurfacetreatment: Table1, Fig.2: MIDAS378and435)leafsfromCabezoJuré(Tables4 and 5:MIDAS 378and435)suggeststwodifferentproductsfromthesame metallurgicalcasting.Howeverwecannotruleoutthefactthatit maybeamatteroftwofragmentsfromasingleproduct.Although, thisproductionprocessmayhavebeenperformedintheCabezo Jurésettlementitself,bothbecauseofthecoincidenceinthesupply sourcesofgoldandcopper,aswellasbecauseoftheexistenceofan earliermetallurgicaltechnologyofcopperproduction,ableto withstandthetemperaturesrequiredforfoundinggold(Bayona, 2008;Inácioetal.,2011;Nocete,2004;Sáezetal.,2003),the absenceofanyotherindicatordoesnotmakeitpossibletodiscard theirorigininanyoftheothermetallurgicalsettlementsidentified intheSPZ(Nocete,2001,2004,2008).
AtValencinadelaConcepción,inviewoftheabsenceofTiand thelowpresenceofSn,otherindicatorsofmetallurgicalactivity, suchasthevaluesofCu(Esheretal.,2011;Hartmann,1970,1982)o Sb(Constantinescuetal.,2012)arenotconclusiveastheyarefound closetothoseoftheprimarygoldintheLaSultanamine(Table4: MIDAS497and505vs436).Buthowever,alongwithanearlier metallurgicaltechnologyofcoppersimilartotheoneevidencedat CabezoJuré,withthecapacitytowithstandthetemperatures (Bayona,2008;Inácioetal.,2011;Noceteetal.,2008)requiredfor castinggold,wehaveanindicatorofthemetallurgicalprocessthat suggestthatthisactivityexistedandthatitwasappliedinthe settlementitself:thecastingspillatMIDAS505(Fig.4).Inaddition, thiscastingspillmayhavebeenrelatedtothegoldleafsfromthe tombsatMatarrubilla(Hartmann,1982)andLaPastora(Pereaetal., 2003,2010)wheretinisnotpresentandthevaluesofsilverare similar(approximately1.8%).
ThefactthatproductionprocessessimilartothoseatCabezo Juré,onthebasisofalluvialgold,canbefoundincontextsofthe 3rdmillenniumBCintheGuadalquivirValley,suchasCañada Carrascal(Sevilla,Spain)orMontilla(Córdoba,Spain)andinthe SouthwestandWestoftheIberianPeninsula,suchasExtremadura(Badajoz,Spain)oratGrutas1y2dePalmelaandZambujal,inPortugal,where Hartmann(1982) characterizedgold productswithSncontents,from0.18%to0.38%,and Esheretal. (2011b) placerswithcassiterite;andwithproductionprocesses similartothoseatValencinadelaConcepción,onthebaseof minegoldorotheralluvialgoldwithnoSnoTi,maybefoundin othercontextsoftheSouthwest,suchasAlcalar(Hartmann, 1982),suggeststheexistenceofasimilarmetallurgicaltechnologyofgold,generalizedintheSouthwestoftheIberianPeninsula duringthe3rdmillenniumBC,whosedifferences(CabezoJurévs. ValencinadelaConcepciónmodels)maybefoundinnature (alluvialormine)oftherawmaterial.Alongsidethis,thefactthat thetemperaturerangesrequired(1200 C)forthisgoldmetallurgyweredevelopedandbecamewidespread,over500years previously,inthecoppermetallurgyofCabezoJuréandValencinadelaConcepción,asindicatedbytheirslag(Noceteetal., 2008;Sáezetal.,2003),crucibles(Inácioetal.,2011)andcopperproducts(Bayona,2008),mayalsoindicatethepresenceofa
technologicaltransferbetweencopperandgoldbase productions.
5.4.Isotopiccharacterization(Pb)byMC-ICP-MS
Theleadisotopesanalysisofthesamplesprovidesanadditional levelofstudysince,despitethelowcontentsinPbofthesamples (Table4),theprecisionoftheanalysishasmadeitpossibleto identifythevaluesoftheirdiverserelationships(Table5),to
overcometheconfidencelevelsofthePb204 thatusedtocause uncertaintyintheiruseonsamplesofgold(Bendalletal.,2009; GuerraandCalligaro,2004)and,totestboththedifferencesbetweenCabezoJuréandValencinadelaConcepción,suchasthe diversityoftheirsourcesandsupplysystems.
Inviewofthelackofaregionaldatabaseofleadisotopesingold oredeposits,thehomogeneityoftheCuandAumetallogenetic systems,intermsoffractionationofPb,bothintheIPBandinOMZ (TornosandChiaradia,2004;Pomièsetal.,1997)leadsustouseour leadisotopesdatabaseoncopperoredepositslocatedthroughout theGuadalquivirDepressionandtheSouthwest(Sáezetal.,2013)
Fig.8. Imagesbymetallographicmicroscopyofgoldleafs.A)CabezoJuré,sample MIDAS434.B)CabezoJuré,sampleMIDAS-435.C)ValencinadelaConcepción,sample MIDAS487.Fig.10. Mirrorplotsofleadisotoperatiosmeasuredfromthegold findscompared withthecopperoresrangefromthemineralizationslocatedthroughouttheGuadalquivirDepressionandtheSouthwest(Sáezetal.,2013).G1(group1:Andújar, BañosdelaEncina),G2(group2:Hornachuelos,BañosdelaEncina,Montoro, SouthernOMZ),G3(group3:Hornachuelos,SPZVariscanHidrotermalVeins,LinaresLaCarolina,Cardeña,Montoro,CerroMuriano,NorthernSevilleRange,NewRed Sandstone,LosPedrochesBatolith,IPBMassiveSulphidesandGossan)andG4(group 4:Peñaflor).
asasuggestivelevelofanalysisinordertoidentifytheirsupply areas.Thus,thecorrelationofisotopicsignaturesofthegoldsamplesstudiedwiththatoftherangesofthebroadseriesofcopper orespresentthroughouttheGuadalquivirDepressionandthe SouthwestnotonlysuggestsaregionaloriginforthegoldinCabezo JuréandValencinadelaConcepción(Fig.10),butitalsoappearsto confirmthedifferenceinspatialzones(SPZvs.OMZ)oftheirpotentialcatchmentterritoriesnotedbyelementalanalysis,and makesitpossibletomakeamorepreciseidentificationoftheir supplyareas(Fig.11).
InthecaseofValencinadelaConcepción,weshouldpointout that,despitethemarginsoferrordeterminedbythelowpresence ofPb(Table5),thevaluesoftheirtwosamplesliewithintherange ofcoppermineralizationsinthecentralareaoftheOMZ,locatedto thenorthofthesettlement,suchasthemineralizationsatCala, Hornachuelos,Cuoresassociatedwithvariscangranitesrelated withtheLosPedrochesBatolith(Sáezetal.,2013).Nonetheless, theirdifferences(Table5 MIDAS487vs505),sincetheycoincide withdifferentelementalcharacterizations(Table4 MIDAS487vs 505),onceagainpointtotheexistenceoftwopossiblesources,one ofwhichcouldbenearLaSultana(Table5 and Fig.11:MIDAS505 and436).
InthecaseofCabezoJuré,theirisotopicdifferences,sincethey coincidewiththoseidentifiedintheirrespectiveelementalcharacterizations(Table4 MIDAS378-435vs434vs506),makeit possibletosuggestthreepossible,anddifferent,sourceareasinthe
Fig.11. Enlargedareaof Fig.8 showingindetailthegroupG3.A)LosPedroches Batolith,Cardeña(OMZ);B)VariscanHidrotermalVeins(SPZ)andLosPedroches Batolith,VariscangraniterelatedVeins,CerroMuriano(OMZ);C)MassiveSulphides andGossan(IPB).
alluvialsupply.Ontheonehand,thelessradiogenicvaluesofthe MIDAS378and435samples(Table5 and Fig.11:MIDAS378and 435),sincetheycoincidewiththevaluesofthemassivesulphides andgossansoftheIPB(Sáezetal.,2013:Pb206/204 < 18.20),they couldberelatedtothedrainagebasinsofthegossanswhitgoldand cassiterite(LaLapilla,Tharsis)locatedinthevicinity(<2km)ofthe settlement(Capitán,2006;Capitánetal.,2003;Velascoetal.,2013) ortothe fluvialcoursestotheeast,wherethepresenceofcassiteritehasbeendocumented(TintoandCorumbelrivers).Onthe otherhand,thevaluesoftheMIDAS343(Table5 and Fig.11:MIDAS 434Pb206/204 18.35,Pb207/204 15.65,Pb208/204 38.56,Pb207/206 0.85, Fig.10)mayberelatedtothedrainagebasinsintheVariscanHydrothermalVeinsoftheSPZ(Sáezetal.,2013:Pb206/204 18.30 18.40)locatedaroundthemassivesulphidesoftheIPB.Finally,the mostradiogenicvaluesoftheMIDAS506(Table5 and Fig.11: MIDAS506Pb206/204 18.55,Pb207/204 15.65,Pb208/204 38.70,Pb207/ 206 0.84),whichcoincidewiththegreaterelementaldifferencesof thesample(Table4),especiallyinthemarkedpresenceofTi, identifiesthesourceofsupplyasbeingfurtherawayfromthe settlement.Withthelackofisotopicinformationontheoredepositslocatedtothenorthwest,intheEvoraDomainfromtheOMZ (Fig.1),wheregoldleafswithamarkedpresenceofTihavebeen identifiedneartheGuadianaRiver,suchasTresMoinhos(Alves, 1994)orPortoTorrao(Soaresetal.,2004),themineralizations withthenearestsimilarisotopicsignaturesarefoundtothewest (>30km)intheSPZ,againneartheGuadianaRiver(Espingardinhas,CerrodaCruzorMontenovo: Bayonaetal.,2013;Sáezetal., 2013)andtotheeast(>100km)inLosPedrochesBatolithand Cardeña(Sáezetal.,2013).Onepossiblerelationshipwiththe
Guadianaroutecouldarisefromthefactthatasettlementlocated betweenCabezoJuréandtheGuadianaRiver,suchasLaJuntadelos Ríos(Huelva),theproductsofcopperpresentbothisotopicsignaturesintheIPBandinsimilarvaluesofthegoldsampleMIDAS506 (Nocete,2008).However,thepresenceofsameisotopesignatures inthecopperoresfromthemetallurgicalcontextfromValencinade laConcepción,donotmakeitpossibletodiscardtheValencina provenance.
Thecorrelationofisotopicsignaturesofthegoldsamples studiedwiththatoftherangesofthebroadseriesofcopperores presentinthecontextsofmetallurgicalproductionatCabezoJuré (Nocete,2004;Noceteetal.,2011a)andValencinadelaConcepción (Noceteetal.,2008)givesusafurtherreading(Fig.12).Whilein ValencinadelaConcepciónallthegoldsamplesfullycorrespondto therangeofcopperorespresentintheirmetallurgicalcontexts,at CabezoJuré,onlythreeofthese(Table5:MIDAS378,435and434) correspondwiththerangeofcopperoresintheirmetallurgical contexts.Althoughthisdoesnotmeandiscardingthepossibility thatthepresenceofsomegoldproducts,suchastheMIDAS506 samplefromCabezoJuré,maybetheresultofaregionalcirculation systemofrawmaterialsand/orproducts,inwhichothersettlementsmaybeinvolvedthatareclosertothepotentialsourcesof supply,italsoopensupthepossibilityofsuggestingthatthesupply ofgoldmayhavebeenrelatedtothesupplysystemsandterritories
thatbothsettlementsusedforthesupplyofcopperores,andthat bothmaybe,directlyalthoughindependently,involvedinthe productionofgoldartefacts.Thus,aninitiallinkbetweenthe productionofcopperandgold.
6.Conclusions
IntheSouthwestoftheIberianPeninsula,oneofthemaingold miningregionsinWesternEurope,anewsystematicresearch programme,basedonthedocumentation,radiocarbondatingand analysisofgoldproductsinthecontextsofasettlementspecialised incopperproductionsuchasCabezoJuré,intheminingregionof SPZandinthoseofahugecentralsiteatadistancefromit,located inthemainagrarianareaoftheLowerGuadalquivirBasin,suchas ValencinadelaConcepción,haschangedthetraditionalinterpretationofthepresenceofgoldproductsduringthe3rdmillennium BC.Theresultssuggesttheirlinkwithallthe fieldsofexpressionof the firstsocialinequalities,theirrelationshipwithaproduction systemlinkedtocoppermetallurgyinsettlementswherethesame achievedahighdegreeofspecializationandapoliticalnature (attachedorretainedproduction)similartothatinvolvedinthe productionofivoryartefactsatValencinadelaConcepción(Nocete etal.,2013).
GeochemicalcharacterizationbyLA-ICP-MS,leadisotopecharacterizationbyMC-ICP-MSandmetallographiccharacterizationof goldarchaeological findssuggesttwo(CabezoJurévs.Valencinade laConcepción)differentiates,independentandsystematicsupply rawmaterialsystemsin fluvialplacersandminesatlocaland regionalscales,withatleastfoursourceareas,thecirculationof goldrawmaterialorproductsandamanufacturingofgoldartefacts usingametallurgicaltechnologylinkedwiththoseoftheir respectivecopperproductions.Alongsidethis,thecontextsoftheir presence,overtime(thirdquarterofthe3rdmillenniumBC)and space(fromproductiontoconsumption),alsosuggestaneconomic processofapoliticalnature,wheresmallgroupsofthepopulation, withoutparticipatingdirectlyinanyoftheassetproductionsectors (includingthatofgolditself)andbymeansofitscontroloverfood storagesystems(CabezoJuré),rawmaterialsandmanufactures (ValencinadelaConcepciónandCabezoJuré)oroverthemeansof destruction(CabezoJuré)andovertheideologicalapparatus (ValencinadelaConcepciónandCabezoJuré),fosteredthedevelopmentofaproductionsector,suchasthatofgold,thatexclusively suppliedthemwithornamentalproducts,whichtheyaccumulated anddisplayed,distinguishingthembothinlifeandindeath,ina clearexerciseinproductionandreproductionofpowerandclass, coincidingwithaperiodinwhichinter-settlementhierarchization ofthissocietyreacheditspeakdevelopmentandcollapse.
Acknowledgements
ThisworkistheresultofthePIGMALIOMProject(HAR-201016210).WewouldliketothanktheAtlanticCopperFoundationof Huelvaforfundingthemetallographicstudiesincludedinthis work.ThanksalsotoProfessorBeatrizArandaLouvier,atthe DepartmentofMaterialsChemistryandScienceatthe Universityof Huelva,inaspectsrelatedtopreparingsamplesandmetallographic analyses.AlsotoFranciscoNocetePeramoforthephotographsand figures,andtoIanEmmettfortranslatingandproofreadingthis paper.
Alves,L.C.,1994.Determinaçãodacomposiçãoelementardeumfragmentodeplaca deouroencontradonopovoadodosTrêsMoinhos.In:Campos,J.M.,Pérez,J.A., Gómez,F.(Eds.),ArqueologíaenelentornodelBajoGuadiana.Universidadde Huelva,pp.199 200
Arteaga,O.,Cruz-Auñón,R.,1999.Lasnuevassepulturas(tholoi)ylosenterramientosbajotúmulos(Tartesios)deCastillejadeGuzmán(Sevilla).Excavacióndeurgenciade1995.In:AnuarioArqueológicodeAndalucía1995(III), pp.640 651
Baron,S.,Tomas,C.G.,Cauvet,B.,Munoz,M.,2011.LeadisotopeanalysesofgoldsilveroresfromRosiaMontana(Romania):a firststepofmetalprovenance studyofRomanminingactivityinAlburnusMaior(RomanDacia).
J.ArchaeologicalSci.38,1090 1100
Bayona,M.R.,2008.LainvestigacióndelaactividadmetalúrgicaduranteelIII MilenioA.N.E.enelsuroestedelaPenínsulaIbérica.LaArqueometalurgiayla aplicacióndeanálisismetalográficosycomposicionalesenelestudiodela produccióndeobjetosdemetal.In:BARInternationalSeries1769.Oxford Bayona,M.R.,Inácio,N.,Nocete,F.,Sáez,R.,Perámo,A.,2013.ActividadminerometalúrgicadelIIIMilenioA.N.E.enelsurdePortugal:ProspecciónGeoarqueológica.Fase1deInvestigación:resultadospreliminares.Informesy Trabajos(SerieDigitalIPCE).MinisteriodeEducación,CulturayDeporteInstitutodelPatrimonioCulturaldeEspaña(inpress)
Bendall,C.,Wigg-Wolf,D.,Lahaye,Y.,vonKaenel,H.M.,Brey,G.P.,2009.Detecting changesofcelticgoldsourcesthroughtheapplicationoftraceelementsandPb isotopelaserablationanalysisofcelticgoldcoins.Archaeometry51(4),598
625
Berdichewsky,B.,1964.LosEnterramientosenCuevasArtificialesdelBronceI Hispánico.In:BibliothecaPraehistoricaHispanaVI.Madrid
Bozzini,B.,Giovannelli,G.,Pagliara,C.,Guglielmino,R.,Maggiulli,G.,2003.CeremonialgoldartefactsoftheLateBronzeagefromthedepositionsiteofRoca:a metallurgicalinvestigation.In:ProceedingsInternationalConferenceArchaeometallurgyinEurope,vol.I.AIM,Milan,pp.267 276
BronkRamsey,C.,2006.Newapproachestoconstructingagemodels:OxCal4.
PAGESNews14(3),14 15
BronkRamsey,C.,Higham,T.F.G.,Leach,P.,2004a.Towardshigh-precisionAMS: progressandlimitations.Radiocarbon46(1),17 24
BronkRamsey,C.,Higham,T.F.G.,Bowles,A.,Hedges,R.,2004b.Improvementsto thepre-treatmentofboneatOxford.Radiocarbon46(1),155 163
BronkRamsey,C.,Higham,T.F.G.,Brock,F.,Baker,D.,Ditchfield,P.,2009.RadiocarbondatesfromtheOxfordAMSsystem:ArchaeometryDatelist33. Archaeometry51(2),323 349
Calvo,F.A.,1972.MetalografíaPráctica.EditorialAlambra,Madrid Capitán,M.A.,2006.Mineralogíaygeoquímicadelaalteraciónsuperficialde depósitosdesulfurosmasivosenlaFajaPiríticaIbérica.PhDthesis.Universidad deHuelva,Spain.
Capitán,M.A.,Nieto,J.M.,Sáez,R.,Almodóvar,G.R.,2003.Caracterizacióntexturaly mineralógicadelGossandeFilónSur(Tharsis,Huelva).BoletíndelaSociedad EspañoladeMineralogía26,45 58 Chapman,R.W.,1990.EmergingComplexity.Cambridge Chapman,R.W.,2008.Producinginequalities:regionalsequenceinlaterprehistoric SouthernSpain.J.WorldPrehistory21(3 4),195 260
Chapman,R.J.,Leake,R.C.,Earner,R.A.,Cahill,M.C.,Moles,N.R.,Shell,C.A.,Taylor,J.J., 2006.Microchemicalcharacterizationofnaturalgoldandartefact:acasestudy inIreland.Appl.Geochem.21,904 918
Chastain,M.L.,Deymier-Black,A.C.,Kelly,J.E.,Brown,J.A.,Dunand,D.C.,2011. MetallurgicalanalysisofcopperartifactsfromCahokia.J.ArchaeologicalSci.38, 1727 1736
Chernyshev,I.V.,Chugaev,A.V.,Shatagin,K.N.,2007.High-precisionPbisotope analysisbymulticollector-ICP-mass-spectrometryusing205Tl/203Tlnormalization:optimizationandcalibrationofthemethodforthestudiesofPbisotope variations.Geochem.Int.45,1065 1076
Clark,G.,1986.SymbolsofExcellence:PreciousMaterialsasExpressionsofStatus. CambridgeUniversityPress Collantes,F.,1969.EldolmendeMatarrubilla.In:ActasdelVSimposiumInternacionaldePrehistoriaPeninsular.Tartessosysusproblemas.Barcelona, pp.47 61
Constantinescu,B.,Cristea-Stan,D.,Vasilescu,A.,Simon,R.,Ceccato,D.,2012. ArchaeometallurgicalcharacterizationofancientgoldartifactsfromRomanian MuseumsusingXRF,MICRO-PIXEandMICRO-SR-XRFmethods.Proceeding Rom.Acad.Ser.A13(1),19 26
Domergue,C.,1970.LesexploitationsauriferesduNord-OuestdelaPeninsule Iberiquesousl’occupationromaine.In:LaMineríaHispanaeIberoamericanaI, pp.151 193.León
Dube,R.K.,2006.InterrelationbetweenGoldandTin:ahistoricalperspective.Gold Bull.39(3),103 113
Ehser,A.,Borg,G.,Pernicka,E.,2011a.ProvenanceofthegoldoftheEarlyBronze AgeNebraSkyDisk,centralGermany:geochemicalcharacterizationofnatural goldfromCornwall.Eur.J.Mineralogy23(6),895 910
Ehser,A.,Borg,G.,Oliveira,D.P.S.,Rosa,D.R.N.,Salgueiro,R.,2011b.Characterization ofplacergolddepositsfromcentralPortugal:preliminaryresults.In:Barra,F., Reich,M.,Campos,E.,Tornos,F.(Eds.),Let’sTalkOreDeposits,Proceedingsof theEleventhBiennialSGAMeeting.Antofagasta,Chile,pp.814 816
Eluere,C.,1995.GoldandsocietyinPrehistoricEurope.In:Morteani,G., Northover,J.P.(Eds.),PrehistoricGoldinEurope.Mines,Metallurgyand Manufacture,NATOASISeries,Netherlands,pp.29 31 Emmons,W.H.,1974.GoldDepositsoftheWorld.ArnoPress,NewYork
Fernández,F.,1984.Lasedadesdelmetal.In:Flores,A.M.(Ed.),SevillaysuProvincia,TomoII.Géver,Sevilla,pp.45 46 Fernández,F.,Ruiz,D.,1978.ElTholosdelCerrodelaCabezaenValencinadela Concepción(Sevilla).TrabajosdePrehistoria35,193 221 Flores,A.,Aycart,V.,2013.Montelirio.Unsepulcroclaveparalacomprensióndel registrodelosgrandesmonumentosmegalíticosdeValencinadelaConcepción-CastillejadeGuzmán(Sevilla).In:García,L.,Vargas,J.M.,Hurtado,V., Ruiz,T.,Cruz-Auñon,R.(Eds.),ElasentamientoprehistóricodeValencinadela Concepción(Sevilla):InvestigaciónyTutelaenel150aniversariodeldescubrimientodeLaPastora.UniversidaddeSevilla,pp.233 259 García,J.,Correcher,V.,Rojas,R.M.,Fierro,J.L.G.,Fernández,C.,López,P.,Rovira,S., 2005.Chemicaltracersinarchaeologicalandnaturalgold:AlisedaTartessos treasureandnewdiscoverednuggets(SWSpain).GoldBull.38(1),23 28 Gebhard,R.,1995.IndustryinCelticOppida aspectsofhightemperatureprocesses.In:Morteani,G.,Northover,J.P.(Eds.),PrehistoricGoldinEurope.Mines, MetallurgyandManufacture,NATOASISeries,Netherlands,pp.261 272 Guerra,M.F.,Calligaro,T.,2003.Goldculturalheritageobjects:areviewofstudiesof provenanceandmanufacturingtechnologies.Meas.Sci.Technol.14(9),1527 1537.
Guerra,M.F.,Calligaro,T.,2004.Goldtracestotradegold.J.ArchaeologicalSci.31, 1199 1208
Guerra,M.F.,Sarthre,C.O.,Gondonneau,A.,Barrandon,J.N.,1999.Preciousmetals andprovenanceenquiriesusingLA-ICP-MS.J.ArchaeologicalSci.26,1101 1110 Harrison,R.,1977.TheBellBeakersculturesofSpainandPortugal.In:American SchoolofPrehistoricResearch35
Hartmann,A.,1970.PrähistorischeGoldfundeausEuropa.In:Studienzuden AufängenderMetallurgie.3:1.Mann,Berlin
Hartmann,A.,1982.PrähistorischeGoldfundeausEuropa.In:Studienzuden AnfängenderMetallurgie.3:2.Mann,Berlin
Hernando,A.,1983.LaorfebreríaduranteelCalcolíticoyelBronceAntiguoenla PenínsulaIbérica.TrabajosdePrehistoria40,85 138
Hough,R.M.,Butt,C.R.M.,Fischer-Bühner,J.,2009.Thecrystallography,metallographyandcompositionofgold.Elements5,297 302
Hurtado,V.,Amores,F.,1984.ElTholosdeLasCanterasylosenterramientosdel BronceenlanecrópolisdeElGandul(AlcaládeGuadaira,Sevilla).Cuadernosde PrehistoriadelaUniversidaddeGranada9,147 175
Inácio,N.,Nocete,F.,Nieto,J.M.,Sáez,R.,Bayona,M.R.,Abril,D.,2011.Fromraw materialtoutilisation.Ceramicsassociatedwiththemetallurgicalactivityat ValencinadelaConcepción(Seville,Spain):Technologicalchoicesandsocial implications.In:Scarcella,S.(Ed.),ArchaeologicalCeramics:aReviewofCurrent Research,BarInternationalSeries2193,pp.73 79.Oxford
Jochum,K.P.,Weis,U.,Stoll,B.,Kuzmin,D.,Yang,Q.,Raczek,I.,Jabob,D.E., Stracke,A.,Birbaum,K.,Frick,D.A.,Günther,D.,Enzweiler,J.,2011.DeterminationofreferencevaluesforNISTSRM610 617glassesfollowingISOguidelines.GeostandardsGeoanalyticalRes.35,397 429
Kovacs,K.,Schlosser,S.,Staub,S.P.,Schmiderer,A.,Pernicka,E.,Günther,D.,2009. Characterizationofcalibrationmaterialsfortraceelementanalysisand fingerprintstudiesofgoldusingLA-ICP-MS.J.Anal.At.Spectrom.24,476 483 Lacalle,R.,Guijo,J.M.,Cruz-Auñón,R.,2000.Estudioantropológicodecinco sepulturasprehistóricasdeCastillejadeGuzmán(Sevilla).In:Jorge,V.O.(Ed.), Actasdo3 CongressodeArqueologiaPeninsular,vol.IX.ADECAP,Oporto, pp.343 359
Lehrberger,G.,1995.ThegolddepositsofEurope:anoverviewofthepossiblemetal sourcesforprehistoricgoldobjects.In:Morteani,G.,Northover,J.P.(Eds.), PrehistoricGoldinEurope.Mines,MetallurgyandManufacture,NATOASISeries,Netherlands,pp.115 144
Leisner,G.,Leiner,V.,1943.DieMegalithgräberderIberischenAlbinsel.DerSüden. DeGruyter,Berlín
Leisner,G.,Leiner,V.,1959.DieMegalithgräberderIberischenAlbinsel.DerWesten 2.DeGruyter,Berlín
López,P.,Pajuelo,A.,2013.LasecuenciaocupacionalduranteelIIImilenioANEenC/ Trabajadores14 18(ValencinadelaConcepción,Sevilla).In:García,L., Vargas,J.M.,Hurtado,V.,Ruiz,T.,Cruz-Auñon,R.(Eds.),ElasentamientoprehistóricodeValencinadelaConcepción(Sevilla):InvestigaciónyTutelaenel 150aniversariodeldescubrimientodeLaPastora.UniversidaddeSevilla, pp.115 127
López,P.,Sánchez,O.,Pajuelo,A.,Ruiz,S.,Vera,A.,García,I.,Velasco,M.,2001. ExcavacióndeurgenciadeunaestructuradehabitaciónenValencinadela Concepción(Sevilla).In:AnuarioArqueológicodeAndalucía1997,pp.623 634 Morteani,G.,Northover,J.P.(Eds.),1995.PrehistoricGoldinEurope.MInes,MetallurgyandManufacture.NATOASISeries,Netherlands
Nocete,F.,2001.TercerMilenioantesdenuestraera.Relacionesycontradicciones centro/periferiaenelValledelGuadalquivir.Bellaterra,Barcelona Nocete,F.(Coord.),2004.Odiel.Proyectodeinvestigaciónarqueológicaparael análisisdelorigendeladesigualdadsocialenelSuroestedelaPenínsula Ibérica.MonografíasdeArqueología19.ConsejeríadeCultura,JuntadeAndalucía,Sevilla.
Nocete,F.,2006.The firstspecialisedcopperindustryintheIberianPeninsula: CabezoJuré(2900 2200BC).Antiquity80,646 654 Nocete,F.(Coord.),2008.ElyacimientodeLaJuntadelosRíos.Monografíasde Arqueología29.ConsejeríadeCultura,JuntadeAndalucía,Sevilla.
Nocete,F.,Orihuela,A.,Peramo,A.,1995.CabezoJuré2500a.C.Huelva.Serviciode PublicacionesdelaDiputacióndeHuelva,Huelva
Nocete,F.,Sáez,R.,Nieto,J.M.,Cruz-Auñón,R.,Cabrero,R.,Álex,E.,Bayona,M.R., 2005.CirculationofsilicifiedooliticlimestonebladesinSouth-Iberia(Spainand
Portugal)duringthethirdmillenniumBC:anexpressionofacore/periphery framework.J.AnthropologicalArchaeology24,62 81
Nocete,F.,Queipo,G.,Sáez,R.,Nieto,J.M.,Inácio,N.,Bayona,M.R.,Peramo,A., Vargas,J.M.,Cruz-Auñon,R.,Gil-Ibarguchi,J.I.,Santos,J.F.,2008.Thesmelting quarterofValencinadelaConcepción(Seville,Spain):thespecialisedcopper industryinapoliticalcentreoftheGuadalquivirValleyduringtheThirdmillenniumBC(2750 2500BC).J.ArchaeologicalSci.35,717 732
Nocete,F.,Lizcano,R.,Peramo,A.,Gómez,E.,2010.Emergence,collapseandcontinuityofthe firstpoliticalsystemintheGuadalquivirBasinfromthefourthto thesecondmillenniumBC:thelong-termsequenceofÚbeda(Spain).
J.AnthropologicalArchaeology29,219 237
Nocete,F.,Lizcano,R.,Abril,D.,Bayona,M.R.,Inácio,N.,Peramo,A.,2011a.CabezoJuré (3000 2200ANE):Informedeinvestigación2008 2010.Consulcom,Huelva Nocete,F.,Sáez,R.,Bayona,M.R.,Peramo,A.,Inácio,N.,Abril,D.,2011b.Direct chronometry(14CAMS)oftheearliestcoppermetallurgyintheGuadalquivir Basin(Spain)duringthethirdmillenniumBC: firstregionaldatabase.
J.ArchaeologicalSci.38,3272 3295
Nocete,F.,Vargas,J.M.,Schumacher,T.,Benerjee,A.,Dindorf,W.,2013.Theivory workshopofValencinadelaConcepción(Seville,Spain)andtheidentification ofivoryfromAsianelephantontheIberianPeninsulainthe firsthalfofthe3rd millenniumBC.J.ArchaeologicalSci.40,1579 1592
Pasava,J.,Vymazalová,A.,Tornos,F.,2007.PGEdistributioninmassivesulfidedepositsoftheIberianPyriteBelt.MineraliumDeposita42(3),309 314
Peña,D.J.,1917.Informeemitidoconmotivodelavisitadeinspeccióngiradaalos distritosminerosquecomprendenla8aRegión.BoletínOficialdeMinasy
Metalurgia3,1 14
Perea,A.,Alguacil,F.J.,Adeva,P.,García,O.,2003.Contaminaciónyconservaciónde orfebreríaprehistórica. ¿Eselorounmetalsintiempo?RevistadeMetalurgia
39,3 8
Perea,A.,García-Vuelta,O.,Fernández,C.,2010.ElProyectoAu.EstudioarqueométricodelaproduccióndeoroenlaPenínsulaibérica.In:BibliothecaPraeshistoricaHispanaXXVII.CSIC,Madrid
Pingel,V.,1992.DievorgeschichtlichenGolfundederIberischenHalbinsel.In: MadriderForschungen17.W.deGruyter,Berlin
Pingel,V.,1995.Technicalaspectsofprehistoricgoldobjectsonthebasisofmaterial analyses.In:Morteani,G.,Northover,J.P.(Eds.),PrehistoricGoldinEurope.Mines, MetallurgyandManufacture,NATOASISeries,Netherlands,pp.385 398 Pomiès,C.,Cocherie,A.,Guerrot,C.,Marcoux,E.,Lancelot,J.,1997.Pb/Pbisotopicratio intercalibrationwithaccurateU/Pbmeasurement.Chem.Geol.144,137 149 Porter,D.,Paniagua,A.,Sáez,J.,1989.GoldmineralizationofNWSpain.In:SymposiumGold ’89inEurope.GuideBooks,Ex:3,Toulouse,33
Possac,C.,1975.LosAlgarves(Tarifa).UnanecrópolisdelaEdaddelBronce.NoticiarioArqueológicoHispánico4,85 120
Reimer,P.J.,Baillie,M.G.L.,Bard,E.,Bayliss,A.,Beck,J.W.,Blackwell,P.G.,Bronk Ramsey,C.,Buck,C.E.,Burr,G.S.,Edwards,R.L.,Friedrich,M.,Grootes,P.M., Guilderson,T.P.,Hajdas,I.,Heaton,T.J.,Hogg,A.G.,Hughen,K.A.,Kaiser,K.F., Kromer,B.,McCormac,F.G.,Manning,S.W.,Reimer,R.W.,Richards,D.A., Southon,J.R.,Talamo,S.,Turney,C.S.M.,vanderPlicht,J.,Weyhenmeyer,C.E., 2009.IntCal09andMarine09radiocarbonagecalibrationcurves,0 50,000 yearscalBP.Radiocarbon51(4), 1111 1150
Renfrew,C.,1978.Varnaandthesocialcontextofearlymetallurgy.Antiquity52, 197 203 Sáez,R.,Nocete,F.,Nieto,J.M.,Capitán,M.A.,Rovira,S.,2003.TheextractivemetallurgyofcopperfromCabezoJuré,Huelva,Spain:chemicalandmineralogical studyofslagsdatedtotheThirdMillenniumB.C.Can.Mineral.41,627 638 Sáez,R.,Nocete,F.,Gil-Ibarguchi,I.,Bayona,M.R.,Nieto,J.M.,Inácio,N.,Quispe,D., Rodríguez,J.,Santos,J.F.,2013.AleadisotopedatabaseforcoppermineralizationalongtheGuadalquivirrivervalleyandsurroundingareas.Archaeometry (inprep.)
Scott,D.A.,1991.MetallographyandMicrostructureofAncientandHistoricMetals. TheJ.PaulGettyTrust,Singapore.
Shlosser,S.,Kovacs,R.,Pernicka,E.,Günter,D.,Tellenbach,M.,2009.Fingerprintsin gold.In:Reindel,M.,Wagner,G.A.(Eds.),NewTechnologiesforArchaeology, NaturalScienceinArchaeology24.Springer-Verlag,pp.409 436 Soares,A.M.M.,Araújo,M.F.,Alves,L.C.,2004.Análisequímicanão-destrutivade artefactosemouropréeproto-históricos:algunsexemplos.RevistaPortuguesa deArqueologia7,125 138
Tornos,F.,Chiaradia,M.,2004.PlumbotectonicevolutionoftheOssaMorenaZone, IberianPeninsula:tracingtheinfluenceofMantle-Crustinteractionsinoreformingprocesses.Econ.Geol.99,965 985
Tylecote,R.F.,1987.TheEarlyHistoryofMetallurgyinEurope.Longman,London Veiga,S.P.M.EstácioDa,1886.AntiguidadesMonumentaisdoAlgarve,I.Imprensa Nacional,Lisboa
Veiga,S.P.M.EstácioDa,1889.AntiguidadesMonumentaisdoAlgarve,III.Imprensa Nacional,Lisboa
Velasco,F.,Herrero,J.M.,Suarez,S.,Yusta,I.,Alvaro,A.,Tornos,F.,2013.Supergene featuresandevolutionofgossanscappingmassivesulphidedepositsinthe IberianPyriteBelt.OreGeol.Rev.53,181 203
Walder,A.J.,Platzner,I.,Freedman,P.A.,1993.Isotoperatiomeasurementoflead, neodymiumandneodymium samariummixtures,hafniumandhafnium lutetiummixtureswithadoublefocusingmultiplecollectorinductively coupledplasmamassspectrometer.J.Anal.At.Spectrom.8,19 23