Artists before Columbus: A multi-method characterization of the materials and practices of Caribbean cave art


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Title:
Artists before Columbus: A multi-method characterization of the materials and practices of Caribbean cave art
Series Title:
Journal of archaeological science
Creator:
Samson, Alice V.M.
Wrapson, Lucy J.
Cartwright, Caroline R.
Sahy, Diana
Stacey, Rebecca J.
Cooper, Jago
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Elsevier
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Cave paintings ( lcsh )
Indian art ( lcsh )
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serial ( sobekcm )
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North and Central America -- Puerto Rico -- Mayaguez -- Mona, Isla

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This study represents the first positive identification of plant gum binding media in pre-Columbian art, and the first dates from indigenous cave art in the Caribbean. Mona Island reveals an extensive and well-preserved pre-Columbian and early colonial subterranean cultural landscape with dense concentrations of newly-discovered cave art in up to 30 caves. A multi-method approach to the research of pigments and binding media, charcoal, and cave sediments was used to elucidate the technologies, chronologies and processes of indigenous art and artists. Analyses included on-site use of a portable X-ray fluorescence (P-XRF) device to inform sample selection, scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX) on paint and charcoal samples, polarized light microscopy (PLM) for material characterizations, and gas chromatography - mass spectrometry (GC-MS) and X-ray diffraction (XRD) for detailed chemical analysis of paint structures and composition. In addition direct dates of cave art using radiocarbon (C14) and Uranium-thorium (U-Th) dating methods are discussed. Results demonstrate multiple centuries of cave use during indigenous occupation and multiple phases and techniques of mark-making in dark zone locations within extensive cave systems. Visitors set out on pre-meditated journeys underground, making rock art using pigments from the cave floors, which they mixed into complex paints with the addition of plant gums from outside. This study is the first of its kind in the Caribbean providing insight into native paint recipes, material choices, and mark-making techniques. The methods have scope for widespread application and advance the integration of cave art research in archaeology.
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Volume 88

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University of South Florida
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University of South Florida
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K26-05447 ( USFLDC DOI )
k26.5447 ( USFLDC Handle )

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ArtistsbeforeColumbus:Amulti-methodcharacterizationofthe materialsandpracticesofCaribbeancaveartAliceV.M.Samsona,LucyJ.Wrapsonb,CarolineR.Cartwrightc,DianaSahyd, RebeccaJ.Staceyc,JagoCoopere,*aCentreforHistoricalArchaeology,SchoolofArchaeologyandAncientHistory,UniversityofLeicester,LeicesterLE17RH,UnitedKingdombHamiltonKerrInstitute,MillLane,WhittlesfordCB224NE,UnitedKingdomcDepartmentofScienti cResearch,BritishMuseum,GreatRussellSt,LondonWC1B3DG,UnitedKingdomdNERCIsotopeGeosciencesLaboratory,BritishGeologicalSurvey,NottinghamNG125GG,UnitedKingdomeAmericasSection,DepartmentofAfrica,OceaniaandAmericas,BritishMuseum,GreatRussellSt,London,WC1B3DG,UnitedKingdomarticleinfoArticlehistory: Received8February2017 Receivedinrevisedform 11September2017 Accepted16September2017 Availableonline29October2017 Keywords: Cavesandrockart Organicandnon-organicpaintrecipes Plantgumbindingmedia ComparativeC14/U-Thdating CombinedP-XRF SEM/EDX GC-MSandXRDanalyses IndigenousCaribbeanabstractThisstudyrepresentsthe rstpositiveidenti cationofplantgumbindingmediainpre-Columbianart, andthe rstdatesfromindigenouscaveartintheCaribbean.MonaIslandrevealsanextensiveandwellpreservedpre-Columbianandearlycolonialsubterraneanculturallandscapewithdenseconcentrations ofnewly-discoveredcaveartinupto30caves.Amulti-methodapproachtotheresearchofpigmentsand bindingmedia,charcoal,andcavesedimentswasusedtoelucidatethetechnologies,chronologiesand processesofindigenousartandartists.Analysesincludedon-siteuseofaportableX-ray uorescence(PXRF)devicetoinformsampleselection,scanningelectronmicroscopywithenergydispersiveX-ray spectroscopy(SEM/EDX)onpaintandcharcoalsamples,polarizedlightmicroscopy(PLM)formaterial characterizations,andgaschromatography-massspectrometry(GC-MS)andX-raydiffraction(XRD)for detailedchemicalanalysisofpaintstructuresandcomposition.Inadditiondirectdatesofcaveartusing radiocarbon(C14)andUranium-thorium(U-Th)datingmethodsarediscussed.Resultsdemonstrate multiplecenturiesofcaveuseduringindigenousoccupationandmultiplephasesandtechniquesof mark-makingindarkzonelocationswithinextensivecavesystems.Visitorssetoutonpre-meditated journeysunderground,makingrockartusingpigmentsfromthecave oors,whichtheymixedinto complexpaintswiththeadditionofplantgumsfromoutside.Thisstudyisthe rstofitskindinthe Caribbeanprovidinginsightintonativepaintrecipes,materialchoices,andmark-makingtechniques.The methodshavescopeforwidespreadapplicationandadvancetheintegrationofcaveartresearchin archaeology. © 2017TheAuthors.PublishedbyElsevierLtd.ThisisanopenaccessarticleundertheCCBYlicense ( http://creativecommons.org/licenses/by/4.0/ ).1.Introduction:integratingcaveartandarchaeology Rockart,orthe insitu andmotivatedmarkingofnaturalplaces oftenoutsidedomesticsettings,presentschallengesintermsof basicarchaeologicalcharacterization( Bahn,2010;Chippindaleand Taçon,1998;Whitley,2001 ).Therearetworeasonsforthis.Firstly challengesinconnectingrockarttomainstreamareasofsociallife, especiallychronologically,andsecondlyintermsofthe hermeneuticalchallenge,ormeaning.Inthispaperweapproach caveartasaformofplace-basedcommunicationtechnologyand focusonthecontextofindigenousartpracticesasa rststepin addressinghowsuchpracticesfunctionedwithinindigenoussocieties( Gell,1998;Houston,2004;Robb,2015 ). 1.1.Caribbeancaveart InatreatiseonindigenousreligionwrittenatthetimeofColumbus ’ rstvoyagestotheAmericas,FriarRam onPan enamed speci ccavesinHispaniolafromwhereindigenouspeoples believedthe rsthumansemerged,andwherethesunandthe moonoriginated.Pan ealsomakesthe rstreferencetorockartin theNewWorld,describingapaintedcave( “ todapintadaasu * Correspondingauthor. E-mailaddresses: avms1@le.ac.uk (A.V.M.Samson), ljw31@cam.ac.uk (L.J.Wrapson), CCartwright@britishmuseum.org (C.R.Cartwright), dihy@bgs.ac.uk (D.Sahy), RStacey@britishmuseum.org (R.J.Stacey), JCooper@britishmuseum.org (J.Cooper). Contentslistsavailableat ScienceDirectJournalofArchaeologicalSciencejournalhomepage: http://www.elsevier .com/locate/jas https://doi.org/10.1016/j.jas.2017.09.012 0305-4403/ © 2017TheAuthors.PublishedbyElsevierLtd.ThisisanopenaccessarticleundertheCCBYlicense( http://creativecommons.org/licenses/by/4.0/ ). JournalofArchaeologicalScience88(2017)24 e 36

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modo ” ),muchrevered,called Iguaboina ,whereobjectswith ancestralagency( zemies )resided( Pan e,1999 ). Acrosstheislands,Caribbeancaveartischaracterizedbya diverseyetwidely-sharedcorpusoficonographicthemes ( Dubelaar,1986 ),whichalsoappearonothermedia.Iconographyis rarelyrepresentational(anexceptionisthe “ Borb onschool ” inthe DominicanRepublic, Atiles,2009 ),anddepictsschematized human-animal-plant gures,prominentfacialimagery,often sproutingappendages,andarangeofiteratedformswithinternal patterning.ScholarlyinterpretationeitherreliesonPan e ’ saccount asacribsheettotranslatemotifs( Abreuetal.,2011 ),ordismisses thesameasaEurocentricperspectiveatbestrelevanttonorthern Hispaniolaattheendofthe15thcentury. Aroundthecircum-Caribbean,rockart,mortuaryrituals,artefactdeposition,andoralhistoriesunderlinetheimportanceand sharedconceptualisationsofsubterraneanworldsacrossMesoamerica,thesoutheasternUnitedStates,andtheCaribbeanislands ( BradyandPrufer,2005;MoralesandQuesenberry,2005 ).Despite alonghistoryofCaribbeanrockartresearch( Dubelaar,1986; Haywardetal.,2009;Pag anPerdomo,1978 ),interpretiveprogressischallengedbyalackofsecurechronologicaldata,andscienti canalysisofproductiontechniques,processes,andmaterials. Caveartanditsattendantactivities oatdisconnectedlyalongside otheraspectsofdailylife,asisthecaseinmanyworldregions ( Bahn,2010;ChippindaleandTaçon,1998 ).Inthispaperweuse multi-methodanalysesofmaterialsandtechniquestoconsider howandwhenNativeAmericansonMonaIslandcreatedcaveart duringthec.7000yearssincethehumancolonizationofthe Caribbean.Thisisa rststageinbuildingbetterinterpretivehypothesesaboutwhatcaveart does asaformoflandscape communicationtechnology( Houston,2004 ). 1.2.CavescapesofMonaIsland e apreservedsubterranean landscape Monaisalimestoneisland,sevenby vemiles,juttingoutofthe seahalfwaybetweenPuertoRicoandtheDominicanRepublic ( Fig.1 ).Theislandhasover200cavesmostofwhichtrendaround theperimeteroftheislandatthegeologicalcontactbetweenthe lowerMonaDolomiteandupperLirioLimestone( Franketal.,1998; Mylroie,2012;Kambesis,2011 ).Theinter-islandregionofthe northernCaribbean,whichincludesMonaanditslargerneighbours,wasacentreofpre-Columbianculturalcomplexity( Rouse, 1992;VelozMaggioloetal.,1991 ). The ElCoraz ondelCariberesearchcollaboration1isdevelopinga heritagemanagementplanforMonaIslandbuildingonhistorical, speleological,andarchaeologicalresearch( D avila,2003;Samson etal.,2015;Vietenetal.,2016 ).Aprimaryfocusoftheprojectis toexplore,recordandinterprettheculturallandscapewithinless visitedandun-surveyedcavesystems.Sincethestartoftheproject, 70cavesystemshavebeensurveyed,30ofwhichcontainevidence forindigenousexploration,resourceextraction,andmark-making. 1.3.CaveartonMona Mona'scaveartismadeusingbothadditiveandextractive techniques( Fig.2 ).Theapplicationofpigmentsthroughpainting anddrawingwithtoolsorhands(additive)hasbeenfoundin5 caves( Fig.2 AandC).Thisincludescharcoaldrawings,aswellasthe useofwetpaints.However,themajorityofcaveartonMonaIsland ismadebytheremovalofthesoft,moonmilk-likesurfaceofthe cavewalls(extractive).Extractivemark-makingoccursin22caves bydragging ngers( ngeruting)and nger-sizedtoolsthrough thesoftcorrosiondepositsoncavesurfacesleavingincisionsbetween1and10mmdeep( Fig.2 BandD).Thereissomecross-media similarityiniconography,execution,andlocationbetweenadditive andextractivetechniques.Designsincludeclustersof gurativegeometricmotifs,facialiconography,andanimal/humanbodies, similartothosefoundincavesoneithersideoftheMonaPassage ( L opezBelando,2003;Roe,2009 ).Caveartisusuallylocatedin areasdevoidofnaturallight(darkzones),andcloselyrelatedto watersources,whetherseasonaldrippools,orunderwaterlakes ( Lace,2012;Samsonetal.,2015 ).Akeydifferenceisthatextractive designsaremorediverseandextensive,withindividualmotifs rangingfromafewcentimetrestolargespacellingmeandersand schemesoccupyingentiresurfacescoveringtensofsquaremetres. Inthesamechambersthesystematicremovalofthecavewallcrust byhorizontalandverticalscrapingincontinuouspatcheswiththe ngers/ nger-sizedtools( Fig.2 B)isinterspersedwithandsometimesinseparablefrom gurativeandmotifmakingextraction.The ubiquityofthispractice,asaformofindigenousminingtoextract calciumcarbonateaswellasthecreationofcomplexiconography, bringsintoquestiontheontologicalstatusofrockartandblurs functional/ritualboundaries. Mona'sindigenouscaveart,especiallythepictography,hasbeen recognisedinpreviousstudies( D avila,2003;Santana,1973 ), howeverthemajority,chie yextractiveactivity,hasremained hiddeninplainsightduetoitslackofprecedentinCaribbean archaeology,itsdarkzonelocation,anditsoftenapparent “ fresh ” appearancecastingdoubtonitsauthenticityasanindigenous practice. 2.Materialsandmethods 2.1.Samplingstrategy Fiveseasonsofarchaeological eldworkwereconductedto addresswhere,when,how,andwhynativepeoplemaderockart andtointegratecaveactivitieswithinthewiderculturallandscapes oftheCaribbean.Archaeologicalsurveyswereconductedtoidentifyarepresentativerangeofcaveartfromdifferentlocations aroundtheisland.Visualinspectionofmark-makingandoverlappingsequences,combinedwithpre-samplingscreeningwitha P-XRF,assistedbasiccharacterizationandsampleselection.Systematicanddetailedphotographicandlaserscanningrecordingofmodi edcavechamberslocatedonhigh-resolutionspeleological mapsprovidedspatialcontextsforthesampling.Samplesofcharcoalwerecollectedfrompaintedmotifsforspeciesidenti cations andradiocarbondating;paintsfromcavearttounderstand pigmentcompositionandpreparationtechniques;sedimentsfrom cavesandthesurfaceoftheislandforgeochemicalcharacterization andcomparisontocaveartpaints;and owstonesamplesfromon topofcaveartforU-Thdating( Table1 ). 2.2.P-XRFdataforpigmentanalysis ABrukerTracerIIIportableX-RayFluorescenceSpectrometer wasusedinthe eldbyWrapsontoprovide insitu informationand abasiccharacterizationoftheelementalcompositionofsediments, pigments,andcavefeatures.TheXRFanalysiswaspartofapresamplingstrategytominimisedestructivecollectionandto informsampleretrievalformoredetailed,quantitativeanalysis (Section 2.2.2 ).Sixtyassaysweremadeoverallincludingfrom surfacelocationswithpotentialsourcesofpigments,suchas 1BetweentheDepartmentofNaturalandEnvironmentalResourcesofPuerto Rico,theInstituteofPuertoRicanCulture,theCentreforAdvancedStudiesof PuertoRicoandtheCaribbean,theUniversityofPuertoRico,TheBritishMuseum, andtheCentreforHistoricalArchaeologyattheUniversityofLeicester.A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 25

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sedimenttrapsinkarsticdepressions( bajuras ),andfrom oorsand pictographsfromsevencaves(see Table1 ).Testsweretypically undertakenat25kV/35mAwithouttheuseofa ltertofacilitate broad-brushcharacterisationsoffairlylowmolecularweightmaterials.Assayswereinitially1mininlength,butthiswasreducedto 45swhenthespectrawereobservedtochangelittleovertime. 2.2.1.Microscopicanalysisofpaintcomponentsandcross-sections Twentyninesamples( Table1 )werepreparedandthenexaminedintheHamiltonKerrInstitutebyWrapsonusingpolarized lightmicroscopy(PLM)toexaminepaintproperties.Seventeenof thesesampleswerenaturallyoccurringsediments,elevenwere takenfrompictographs,andonefrom19thcenturyhistoricalpaint layers.Samplesizeswerekepttoaminimumandweretypicallyno morethan2mm3unlessalsoscheduledforC14analysis.Alllayers weresampled,groundinmethylethylketone,thenmountedona slidebeneathacoverslipandsetinMeltmount ™ resin.Theslides werethenexaminedusingaLeitzOrtholuxIIpolarizingmicroscope at200Xmagni cation,andwherepossiblethecomponents identi ed. Thematerialusedforpaintcross-sectionswastakenfromthe samesamplefragmentsasthosemountedasdispersions.Eleven Fig.1. MapofMonaisland.Samplelocationnumbersreferto Table1 .TheCavelocationsprovidedareonlyaccuratetowithin1kminaccordancewiththeMonaheritage managementplan. A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 26

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cross-sectionsamplestakenfrompictographsweresetinpolyester resincubesandre ectedlightmicroscopywascarriedoutona ZeissAxioskop ™ microscope.Observationsaboutlayerstructure andmaterialcontentweremadeat200and500Xmagni cationin normallightandbright eld,andUV uorescencewasobserved andphotographicallyrecorded.Themainadditionalbene tof stereomicroscopyoncross-sectionswastheexaminationofstratigraphyonthesesamples,allowingtheassessmentofpaint layeringand/ormulti-phasepainting. 2.2.2.SEM/EDX SEM/EDXanalysiswasundertakenbyWrapsontoprovide comparativequantitativedataontheelementalcompositionof cave oorsediments,sedimentsfromoutsidethecaves,andcave wallpaintstocomplementanalysisfromtheP-XRFdataand microscopicinspection.SEM/EDXanalysiswasundertakenusingan OxfordInstrumentsSiliconLithiumEDXspectrometerwithINCA software.Fourteensampleswereexamined( Table1 ).Sixofthese werereferencesamplesfromcave oors,walls,andredandyellow ochre-richsoilsfromthetopoftheisland.Eightwerefrom pictographs. 2.3.Charcoalidenti cation Charcoalfromthreepainteddesignsintwocaves( Table1 )was analysedbyCartwrightinthelaboratoriesoftheBritishMuseum, DepartmentofScienti cResearchtoexaminespeciesselectionand tosupportdatingassays.ThiswasdoneusinganHitachiS-3700N variablepressurescanningelectronmicroscope(VPSEM).Because ofthethree-dimensionalnatureofwoodanatomy,eachpieceof charcoal,irrespectiveofsize,wasfracturedmanuallytoshowa transversesection(TS),radiallongitudinalsection(RLS)and tangentiallongitudinalsection(TLS)forexamination(see Cartwright,2013,2015 ).EachTS,RLSandTLScharcoalsamplewas thenmountedonanaluminiumSEMstubandexamineduncoated intheVPSEM.Thebackscatterdetectorwasusedat20or15kV, withanaverageworkingdistanceof25mm,atmagni cations rangingfrom 10to 600andwithapartiallyevacuated(40Pa) chamber.Charcoalfragmentsthatwereparticularlysmallorinpoor conditionweremountedusingLeit-CPlastcarboncement(whichis aproprietarybrandofconductivematerialwithlowoutgassing properties).Usingtheobservedcellularfeatures,comparisonswere madewithin-housereferencecollectionspecimensofwoodand charcoalaswellascomputerisedanatomicalfeaturedatabasesand checklists. 2.4.Bindingmediumanalysis BindingmediumanalysiswasconductedbyStaceyinthelaboratoriesoftheBritishMuseum,DepartmentofScienti cResearch todeterminewhethertherawcolorantsweremixedwithother ingredientstoincreasepaintworkabilityanditsabilitytostickto surfaces.Sixpaintswereanalysedfrom4caves( Table1 )includinga historicpaintsample,and vesamplesfrompaintedmotifs selectedonthebasisofvarietyinpaintcolourandconsistency.The smallsizeofthepaintsamplesmeantthatonlyafewcouldbe subjecttomultipleanalyticalmethodstargetingdifferenttypesof organicbinder.Analysiswastargetedtowardsthedetectionand identi cationofcarbohydrates(gumbinders),aminoacids(proteinaceousglues)andlipid/resinbinders(detailedin Table1 ). 2.4.1.Sugars(monosaccharides) Sampleswerehydrolysedbyadding100mlof0.5Mmethanolic HClandheatingat80Cfor18h.Theyweredriedundernitrogen andderivatisedusing100mlofSigma-SilA(1:3:9ratiooftrimethylchlorosilane(TMCS),hexamethyldisilazane(HMDS)andpyridine)andheatingat80Cfor1h.Thisprocedureisbasedonthe methoddescribedby Bletonetal.(1996) foranalysisofplantgums. 2.4.2.Protein(aminoacids) Sampleswerehydrolysedwith100mlof6NHCl,heatedovernightat105Candthendriedundernitrogen.Thesampleswere Fig.2. AdditiveandextractivedesignsfromthedarkzonesofthreecavesonMona.A)charcoaldrawnmotifs;B) ngerutedmotifsandareaofsystematicextraction(righthand side);C)charcoaldrawnface;D) ngerutedfacewithlimbsandappendages. A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 27

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driedagainafteragitationwith100mlofdeionisedwaterand100ml ofdenaturedethanol.Priortoanalysis,thesampleswerederivatisedwith N -(tert-butyldimethylsilyl)N -methyl-triuoroacetamide(MTBSTFA) þ 1%tert-butyldimethylsilylchloride (TBDMCS). 2.4.3.Lipids(waxes/fats/resins) Sampleswereextractedwith100mlofdichloromethane,assistedbygentleheating(45C)andultra-sonication.Afterevaporationofthesolventunderastreamofnitrogen,sampleswere derivatisedwith50mlbis(trimethylsilyl)tri uoroacetamide (BSTFA) þ 1%(trimethylchlorosilane)TMCS. 2.4.4.GC-MSanalysis Samples(1ml)wereanalysedusinganAgilent6890NGC tted withanAgilentHP5-MS,30m 0.25mm,0.25mm lmthickness columnwith1m 0.53mmretentiongapandcoupledtoan Agilent5973NMSD(sugarsandaminoacids)oranAgilent6890N GC ttedwithaSGEHT-512m 0.1mm,0.1mm lmthickness with1m 0.53mmretentiongapandwithanAgilent5975CMS detector(lipids).Thecarriergaswasheliumwithaconstant owof 1.5ml/minandsampleswereinjectedinsplitlessmode(purgetime 0.8min)at10psiand250C(sugars)or300C(aminoacids).Lipid sampleswereinjectedon-columnat50C.Oventemperatures wereprogrammedasfollows:sugars-40Cto130Cat9C/min, thento290Cat2C/min naltemperaturehold10min;amino acids-300Cat20C/min,aftera1minisothermalholdat80C withthe naltemperatureheldfor3min;lipids-aftera1min isothermalholdat35Cto340Cat10C/min.Withthe nal temperatureheldfor20min.TheMSinterfacewasheldat280C (sugars)and300C(aminoacidsandlipids).Inallcasesthesource temperaturewas230Cwithacquisitioninscanmode(29 e 650 amu/sec)afterasolventdelayof5min.Massspectraldatawere interpretedmanuallywiththeaidoftheNIST/EPA/NIHMass SpectralLibraryversion2.0andbycomparisonwithpublisheddata andreferencestandards. 2.5.Dating 2.5.1.Radiocarbon Inordertodirectlydatethepresumedindigenouscaveart,two charcoalsampleswerecollectedfromcaveartpigmentsfromcaves onoppositesidesoftheisland.Onlytwosamplesweretakenin ordertotesttheef cacyofdatingverysmallcharcoalpiecesfrom rockart.Thesewerecharcoal ecksembeddedwithinthepaint matrixtakenfromareasofexistingmotifdeterioration( Fig.3 A). Thesamesamplesweresubmittedforspeciesidenti cation, bindingmediumanalysis,andcompositionalandpaintstructure analysis( Table1 ). 2.5.2.Uranium-thorium Extractivecaveart,whichaccountsforc.95%ofcaveartonMona cannotbedatedusingradiocarbon.However,calciteaccretions,or owstones,whichformoverthetopofcaveartareamenabletoUThdating,atechniquethatisincreasinglyusedinrockartresearch ( Pikeetal.,2016 ).U-Thdatingprovidesa terminusanteque ,or minimumagefortheunderlyingcaveart.Samplesofwhitecalcite accreteddirectlyover ngerutingweretakenfromfourlocations inthreecaves( Fig.3 D, Table1 ).Foreachsamplinglocationtwo adjacentsamplesofcalciteweretaken,weighingbetween0.3and 1.9g.Foreachsamplethewholecrosssectionwastaken,including thecontactlayerwiththeunderlyingarchaeology. ThecalcitesampleswereanalysedbySahyattheNatural EnvironmentResearchCouncilIsotopeGeosciencesLaboratory (NIGL),BritishGeologicalSurvey,followingtheU-Thdatingprotocoloutlinedin Cr emi ereetal.(2016) .SubsamplesforU-Thdating consistedofcalciteadjacenttothecontactbetweentheaccretions andtheunderlyingcaveart( Fig.4 ).Samplesweremechanically cleanedtoavoidcontaminationwitholdercarbonatefromthecave wallsandwerespikedwithanin-house229Th e236Uisotopic tracer.Isotoperatiomeasurementsonchemicallypuri ed ( Edwardsetal.,1987 )UandThfractionswerecarriedoutusinga ThermoNeptunePlusmulti-collectorinductivelycoupledplasma massspectrometer(ICP-MS). Fig.3. SamplingA)charcoalfromcavepaints;B)indigenouspaintsamples(notethe ngermarksinthispaint “ palette ” ,sample130);C)surfacesediments,redochrefromthe VeredadelCentro,samplelocation998;D)calciteaccretionsontopofcaveart.Notethesampledareawhichisawhiterpatchca.3mabovetheendofthe1 0cmscale.(For interpretationofthereferencestocolourinthis gurelegend,thereaderisreferredtothewebversionofthisarticle.) A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 28

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3.Results 3.1.InsituP-XRF,visualandmicroscopicobservationofcaveart Caveswithgreatercolourcontrastbetweenthesurfacecorrosionandthelayerunderneathattractedsomeofthelargerand moreelaboratedesigns(Caves7,13).Thesecontrastswere demonstratedchemicallybyP-XRFanalysisin3caves(Caves3,8, 13)wherethebrownerwallcrustscontainedadditionalironand manganeseincomparisontothelightercolourofthepurecalcium carbonateoftheextractivedesigns. P-XRFcombinedwithvisualexaminationindicatedtherepeated useofcave oordepositsinadditivecaveart.Thedominantconstituentof oordepositsappearedtobephosphorite,derivedfrom mineralizedbatorbirdguano( Briggs,1974;KayeandAltschuler, 1959 ),latercon rmedthroughSEM/EDX(Section 3.2 ).Floordepositstypicallycontainediron,andpigmentsincludingreddish ochres,yellowearths,andsomemanganese-containingbrown earthpigmentsasminorcomponentsinadmixtures. AtCave14,charcoalwasobservedbothonthe oorofthecave andmixedintothepaintings.Themixingofcharcoalandpigment isnotthoroughandappearsincidentalinsomecases,whereasin othersitformsaclearanddeliberatepaint lm.Charcoaldrawings andpaintswere,attimes,appliedinsequentialepisodes.Paints wereobservedinadeliberatelayerstructureinCave14( Fig.5 Dand E)andinoneexampleinCave6.InsomedesignsinCave6the charcoalwasapplied rst,beforeaphosphorite-basedlayer,ina processeitherindicativeofdeliberateunderdrawingorthe Fig.4. SamplesselectedforU-Thdating.Reddashedlinesshowthecontactbetweencavewalls/moonmilk(abovetheline)andcalciteaccretions(belowtheli ne).PlotshowsU-Th evolutiondiagramwherebluehorizontallinestracethesample's[234U/238U]activityratioovertime,andgreyobliquelinesaretheoreticalisoch ronslabelledinkyr.Uncertainty ellipsesareplottedatthe2slevel.Notethatsamples148and149,whichwerecollectedfromthesamecave,havesimilarinitial[234U/238U]values.(Forinterpretationofthe referencestocolourinthis gurelegend,thereaderisreferredtothewebversionofthisarticle.) A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 29

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retouchingofapre-existingimageusingadifferentcolour.Crosssectionsofpaintsamplesalsoclearlydemonstratethesoftnessof cavewalls,forexampleinCave14whereitissmearedandblended inwiththecharcoalblack( Fig.5 F).Thiscontrastswiththeharder, drierwallsofCave6,andmayaccountfortheuseofotherpaint ingredientsinthisinstance(Section 3.3.2 ). Fig.5. Paintsamplecross-sections, 200magni cation.A)Sample130,Cave6.Paintfrom “ palette ” ,lemonyyellowguanoandcalcite/dolomite(see Fig.3 B);B)Sample126,Cave8. Sampletakenfrompictograph,guanosomeplant-derivedcharblack(identi edas Burserasimaruba ,Section 3.3 ),somecalcite/dolomite;C)Sample128,Cave8.Sampletakenfrom pictograph,aplant-derivedcharblack(identi edas Burserasimaruba ,Section 3.3 )andcalcite/dolomite;D)Sample137A,Cave14.Frompictograph.Notelayerstructure:bottom calcite/dolomite,middleyellowishguano,topplant-basedcharblack;E)Sample137B,Cave14.Separateportionofsamepaintsample,alsonotethec learlayerstructure;F)Sample 138,Cave14.Sampletakenfrompictograph,thelayersaresoftandhavebecomemixed,slightlybrownguano,withoccasionalochreparticle,pluscalc ite/dolomiteandplant-based charblack.(Forinterpretationofthereferencestocolourinthis gurelegend,thereaderisreferredtothewebversionofthisarticle.) Fig.6. A)SEMimageofatransversesectionof Burserasimaruba charcoalfromMona;B)SEMimageofatangentiallongitudinalsectionof Burserasimaruba charcoalfromMona. Images:CarolineCartwright©TheTrusteesofTheBritishMuseum. A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 30

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Fig.7. Partial(17 e 35min)totalionchromatogramsshowingmonosaccharidecompoundsdetectedinsamples130A(palette)and131A(pictograph).Peaklabels: C -arabinose;-rhamnose;:-galactose; -mannose;;-xylose;s e unidenti edsugarcompounds.Tableindicatestherelativeabundanceofmonosaccharidecompoundsidenti edinthepaint samples. -moreabundant; -lessabundant;tr e trace. A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 31

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Alsopresentinallpaintsampleswereparticlesfromthecave walls.Typicallythiswasaverypurewhitecalciumcarbonatewith evidentmarineorigin.ThiscontrastedwithsamplesfromCaves6 and14whichhadadifferentcavewalltypeindicativeofdolomite. Thisdistinctionmaybesigni cantintermsofarttechniqueselection,andchoiceofingredients,aswellpotentiallyaccountfor differentialpreservationofcaveart. 3.2.Inorganicpaintconstituents:SEM/EDX SEM/EDXcon rmedwhatwassuspectedfromXRFanalysis; thatphosphoritedepositsfromthecave oorsarethekeyinorganic constituentofpictographpaints.MoreoverSEM/EDXcon rmed compositionalsimilaritybetweenthematerialsfoundoncave oorsandinpictographsonthecavewalls.Forexample,samples frompaintingsandthecave oorinCave14werepredominantly calciumandphosphorouscontaining,butalsocontained uorine, probablyintheformofcollophane,cryptocrystallineapatite,as wellastracesofiron.Samplesfromthe oorandwallsofCave8 werecompositionallysimilar,butadditionallycontainedsodium.In Cave6,samplesfrompaintingscontainedsigni cantlymorechlorine(betweentwoandtwentytimesasmuch)thanwasfoundin othersamples,thoughagain,calciumandphosphorousdominate. Aredochresoilsamplefromthetopoftheislandwascomposed elementallyofalumina,silica,ironmagnesiumandtitanium,containingcomparativelylittlephosphorousincontrastwithallpaint sampleswhichcontainedthirtytimesthequantityofphosphorous. Thisisaquantitativedemonstrationthatcave oorsaremadeup largelyofphosphoritewithsomeochres,andthatsotooarethe paintings,somewithadditionalcharcoal. 3.3.Paintadditives 3.3.1.Charcoalidenti cationincavepaints Inallthreecasesthecharcoalfromcavepaintswasidenti edas Burserasimaruba ,alm acigorojo/indiodesnudo( Fig.6 ).Thisisan indicatorspeciesfordrytropicalforestandnativetotheregion ( Newsom,2010 ). Bursera hasbeenidenti edatarchaeologicalsites inPuertoRico( Newsom,2014 ).Itmakesagoodtorchwoodasitis ne-texturedandresinous.Itislikelythatthecharcoalinthepaints wasderivedfromburnttorchesusedtoilluminatethecave,asa secondary,ratherthanaprimaryingredient. 3.3.2.Organicbindingmedia Nocompoundsabovenormalbackgroundcontaminationlevels couldbedetectedbytheaminoacidandlipidanalyses.Thisimplies thatanimal-derivedbinderssuchasegg,andblood,orplantderivedoilsandresinswerenotusedinthepaintssampledhere, orthatthesamplesizeswerenotconducivetotheirdetectionby theanalyticalmethodsused. Sugarswereobservedinallofthepaintsamples,butinmost casestherangeofmonosaccharidecompoundsdetectedwas limitedand/orpresentatlowortracelevelswhichmaybebackgroundlevels( Fig.7 ).Anexceptionissample130,ayellowpaint fromapictographinCave6,wherethelargersamplesizeallowed detectionofarangeofsugarsincludinggalactose,arabinoseand mannoseinanabundancedistributionconsistentwithaplant gumorigin(see Figs.7,3Band5 A).Importantlyandnotwithstandingthesamplesize,sample131,abrownpaintfromanother pictographfromanadjacentchamber,exhibitsasimilarcomposition( Fig.7 ). Qualitativeanalysisofsugars(anduronicacids)bythemethod usedherecantosomeextentdistinguishbetweendifferentplant gumsonthebasisofoccurrenceand/orrelativeabundanceofindividualsugarcomponents(Bletonetal.,1996 ).Nevertheless, cautionisvitalwheninterpretingarchaeologicalmaterialasaged gumscandisplayconsiderablevariationandthereisevidenceto suggestthattheinorganicpigmentspresentin uencethesurvival ofparticularsugarspeciesbothduringageing( Danielsetal.,2004 ) andanalysis( Lluveras-Tenorioetal.,2012 ).Futureworkwill comparearchaeologicalmaterialtoreferencespeciesfromMona. However,thepresenceofplantgumsinmorethanonepaint sampleisademonstrationthatbindingagentsweredeliberately combinedwithinorganicingredientstoformcomplexpaints. 3.4.Dating 3.4.1.Radiocarbon Twodirectdateswereobtainedfromcharcoalembeddedinthe paintmatrixofpictographs.Thesedatessupporticonographicand archaeologicalevidencethatcave-paintingoccurredwithinthe timeframeofnativeoccupationoftheisland.Sample128/OxA31348(Cave8)datestocal1302CE e 1413(2s),paintedinthelate pre-Columbianperiod,andsample134/OxA-31199(Cave6)tocal 1478CE e 1637(2s),paintedpriortoEuropeanarrivalorduringthe rstcenturyofSpanishcolonization( Cooperetal.,2016 )( Fig.8 ).In bothcasesthecharcoalinthepaintisfrom Burserasimaruba (Section 3.3.1 ),fromyoung,twiggypieceslessthan10yearsold, representingtheageofthebranchesattimeofcutting. 3.4.2.Uranium-Thorium U-Thassaysperformedoncalciteaccretionsoverthetopof extractivedesigns,notdateablethroughconventionalC14 methods,providea terminusantequem ,oryoungestpossibledate fortheunderlyingactivities.TwodatesfromCave2arefromthe samepanel,howeveritistheearlierwhichisclosesttotheproductionoftheunderlyingcaveart.DatesfromCaves2and18are cal1244CE ± 8,andcal1088CE ± 18respectively(2s).Thismeans thecaveartfrombothcaveswasmadeinlatepre-Columbian times.U-ThdatesareconsistentwiththeC14datesforpainted caveart.Afourthdateofcal1703CE ± 4fromCave3indicatesthe caveartwasatleastmadeinorbeforethe18thcentury.Itshould benotedthatanalyticalU-Thageuncertainties( ± 4 e 18years,see Fig.8. ProbabilityplotforC14datingresultsfromcharcoalfragmentsembeddedin paintmatrixfrompictographs,Caves8and6. A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 32

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Table2 )arelikelytounderestimatethetrueageuncertaintygiven thevolumeofcalciteanalysed.Amorerealisticageuncertainty estimatewouldbeintheorderof ± 50 e 100years,equivalenttoa growthrateof0.05 e 0.025mm/yearfora5mmthickcalcite sample. 4.Discussion Datesobtainedfromcaveartdemonstrateindigenousauthorshipandsupportahorizonofcaveuseinthelatepre-Columbian period.Bothradiocarbonanduranium-thoriumdatesareconsistentwitheachotherandwithdatesfromthe13thto15thcenturies obtainedfromotherarchaeologicalmaterialsfromcavesallaround theisland( Samsonetal.,2015 ;inprep.).Datesfromcavesoverlap withthosefromtheindigenousvillagesiteatSardinera( D avila, 2003 )suggestingitsuseasabaseforcaveexploration.This periodofintensi cationofcaveactivityinthe13thto15thcenturiesisconsistentwiththewiderLateCeramicAgeTainocultural developmentinPuertoRicoandHispaniolaoneithersideofthe MonaPassageatthistime.Theseactivitiesinthecavesdidnotstop withthearrivalofEuropeans,rathercavevisitationcontinuedinto the16thcentury( Cooperetal.,2016;Samsonetal.,2015 ).Future workwillbuildontheopportunitiestointegratemultiplechronometricmethodsforre ningrockartchronologies. Historicdocuments,ethnographicanalogy,andvisualappearancehavesuggestedavarietyofanimal,vegetableandmineral basedcolorantsandbindersforCaribbeanpictography( Greer, 2001;Haywardetal.,2009 :119; Haviser,2009 :163; Vega, 1976 :200).Therehasbeenverylittlescienti canalysisconducted onthepigmentsusedinrockartintheCaribbeanorsurrounding mainlandregions( Lietal.,2012 : Rooseveltetal.,1996;Sepúlveda etal.,2012;Simeketal.,2010 ).Inarchaeologicalcontexts,ground redhematiteanddropsoftreeresinwerefoundattheSavonetsite inCuracao( Haviser,2009 ),andVelozMaggiolo,anecdotallyasthe analysisofthis ndingisunpublished,reportedtheuseofiron oxideandgypsumfrompictographsinCuevadelasMaravillas,in theDominicanRepublic. OurresearchshowsthatindigenouspopulationsonMonawere makingpaintsfromphosphorites,charcoal,andochresfromcave oorstoapplytothecavewalls,sometimesmixingthemwithplant gumswhichtheybroughtintothecaves.Inadditioncharcoalwas broughtintothecavesastorchwoodandbothincidentallyand deliberatelymixedwithpaints.Multiplephasesofpainting, whetherstepsinarelatedsequence,orretouching,indicatespeci c chamberswererevisited.Theelaboratephasingofpictographyhas beennotedelsewhereintheCaribbean( Haviser,2007;Roe,2009 : 222). ParticulartoMonaisextractiononsoftsurfaceswhichisvery differentfromconventionalpeckingandgrindingofhardrock surfaces.Isolatedexploitationofasoftsubstratehasbeenreported inCuba,theDominicanRepublic,andthesoutheastUnitedStates ( DuVall,2010;Guti errezClavacheetal.,2013;SimekandCressler, 2005 ),butitsabundanceonMonaisunprecedentedandsuggests extractionwasbothaformofcommunicationtechnologyanda formofpre-Columbiancalciumcarbonatemining( Fig.2 B). Despitetheavailabilityofhighquality,strongly-colouredred ochres( Fig.3 C),neitherintensitynorvarietyofcolourappearstobethedriverforchoosingpigments.Theinorganicstuffofpainting, essentiallyphosphorite,camefromwithinthecaves.Addedtothis wereplant-derivedcharcoalblacks,polysaccharidegums,andared plantdyestuff,seeninseveraldesignsinCave6andasyetunidenti ed.Theincorporationof Burserasimaruba intomixedpaints onMonamayberelatedtoitsuseasatorchwood,orforother purposes.SeveralspeciesintheBurseraceaefamilyareutilizedfor copal,anaromaticresinwhichhasuseasglueandincense( Stacey etal.,2006 ).Charcoalparticlesidenti edfromcavepaintingsin Nicaragua( BakerandArmitage,2013;Cartwright,2013;Lietal., 2012 )alsocomefromtreespeciesthatwereasourceofresin,for example Hymenaeacourbaril, guapinolorjatob atree(Fabaceae family)and Pinus sp.,pine(Pinaceaefamily). The ndingofagumbindingmediumisparticularlyimportant fortheinterpretationofthepaintsbecause,unlikethepigments opportunisticallysourcedfromwithinthecaves,thegumbinder wasbroughtinbythepainters.Todate,mostoftheresearchon characterizationofgumbindingmediahasfocussedonWesternart materialsandOldWorldgumsources( Chiantoreetal.,2009;Mills andWhite,1994;Vallanceetal.,1998 ).ThecomparativecompositionsofexudatesfromnativeCaribbeansourceshavenotreceived thesameattentionalthoughdatacanbefoundforsomerelevant genera(e.g. Prosopis sp., Anacardium sp.( Lluveras-Tenorioetal., 2012 ); Anadenanthera sp.( Delgoboetal.,1998 ); Opuntia sp. ( Ribeiroetal.,2010 ).). 5.Conclusions Animportantstepinunderstandingrockartanywhereinthe worldisthereconstructionofthesocialandculturalcontextofits productionanduse.TothisendtheexcellentpreservationonMona hasshedlightonawidespreadpracticeallowingforthe rsttimeto dateCaribbeancaveartandreconstructnativepaintrecipesand techniques.Aprogressionofmutuallyinformedanalyticalsteps from eldobservation,sampleselection,throughtoanalyses involvingtheapplicationofmultiplemethodstoindividualsamplesisaparsimoniousandconservation-mindedapproachwhich canbeappliedtorockartallovertheworld. IndigenousartistsonMonacombinedexpedientandpremeditatedpracticesinvisitstothedarkzonesofcaves,makingdesigns byapplyingpreparedmixtures,orscrapingsurfacesofftoexploit colourcontrastandharvestwallmaterial.Inextractivecaveartthe visualcontrastbetweenadarkerbackgroundagainstlighterdesignsisre ectedchemicallyinP-XRFsignatures.Foradditivecave art,asequenceofvisualinspection,P-XRF,andSEM/EDXanalyses demonstratedthatphosphorite(derivedfrommineralizedguano), naturallyoccurringochresfromcave oors,andcharcoalarethe keyconstituentsofpaints.Thispreferenceforusingmaterials foundundergrounddespitethepresenceofmorevibrantcolorants outside,indicatesthatengagingwithspeleo-substances,through scrapingandpainting,wasbothameansandanend.2Elaborating onthis,weshouldnotmistakethecave-centredpracticesforexpediencyasGC-MSandXRDrevealedthedeliberateadditionof plantgumsasbindingmediatomakecomplexpaints.Thisisevidencefortheassemblageofapre-preparedart-kit,andalsothe rst evidenceforpre-ColumbianpaintmediafromtheCaribbean.The retouchingandoverpaintingofsomemotifs, rstacharcoallayer andsecondapaintlayerindicatesthatcaveartpracticeswere temporallylayered,whetherinstagesorepisodes.Thegatheringof rockartinpredominantlydarkzonelocationsandtheclusteringof differentmediaandiconographiesreferencescommunitiesof practiceformedthroughmotivatedvisitstoparticularplaces. Thediversityandubiquityofcaveartinwell-preservedenvironmentslikeMonaisaphysicalmanifestationofthecultural importanceofsubterraneanplacesforCaribbeansocietiespre-and post-Columbus.Indigenousartistsusedtheirknowledgeofthe affordancesofover200chemicallyandmorphologicallydistinct 2Asacounterparttothis,cavematerialssuchasspeleothemsandsodastraws haveturnedupinarchaeologicaldepositsinterrestrialcontextssuchasSardinera, showingthatpeoplealsobroughtcavespeleothemsbackfromtheirunderground visits.A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 33

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Table1 Overviewofsamplesperanalyticaltechnique.Samplelocationnumberscorrespondtomapin Fig.1 . Samplelocation(see map) Location type Sample_IDpXRFPLMRe ectedlightmicroscopy (X-section) SEM/ EDX Bindingmedium analysis Wood species C14UTh Description sugarsamino acids lipids Archaeologicalsamples 1Cave123XXXXXC19thhistoricpaintsample 8Cave126XXXXXXXPictograph,paintand charcoal 8Cave128XXXXXXXXPictograph,paintand charcoal 6Cave130XXXXXXXYellowpaintfrom " palette " 6Cave131XXXXXXBrownpaintfrom pictograph 6Cave132XXX Brownpaintfrom pictograph 6Cave134XXXXPictograph,paintand charcoal 14Cave137XXXXBrownpaintfrom pictograph 14Cave138XXXXXXXBlackpaintfrompictograph 6Cave167XXXPictograph,paintand charcoal 6Cave168XXXPictograph,paintand charcoal 6Cave170XXXPictograph,paintand charcoal 3Cave145 XCalciteontopof ngeruting 2Cave148 XCalciteontopof ngeruting 2Cave149 XCalciteontopof ngeruting 18Cave160 XCalciteontopof ngeruting Non-archaeologicalsamples 3Cave103XXXWallsurface(moonmilk) 4Cave107XXXDepositsfromminingcut, brown 4Cave108XX Depositsfromminingcut, calcite 4Cave109XX Depositsfromminingcut,d. brown 4Cave110XX Depositsfromminingcut, orange 4Cave111XX Sedimentsfromwall depression 2Cave116XXX Depositsfromminingpit, clay 2Cave118XX Claydeposit 3Cave119XX Surface oorsediments 13Cave120XX Surface oorsediments 999Baj.Cerezos 121XXX Brownochresamplefrom surface 999Baj. Cerezos 122XXXXRedochresamplefrom surface 998VER. CENTRO 124XX Ochresamplefromsurface 8Cave127XXXXCave oor 9Cave129XX Cave oor 14Cave139XXXClayfromcave oor 3Cave152XX Roofdepositunder extraction Table2 U-Thdatingresults.Datesandactivityratioscalculatedusingthedecayconstantsof Chengetal.(2013) .1 e measuredactivityratio;2-activityratiocorrectedusingthedetritus U-Thcompositionof Kaufmanetal.(1998) :[232Th/238U] ¼ 0.5407 ± 50%,[230Th/238U] ¼ 0.9732 ± 50%,[234U/238U] ¼ 1 ± 50%;3 e modelledinitialUactivityratio. SampleIDSite/cave238U(ppm)232Th(ppb)[230Th/232Th](1)[230Th/238U] ± 2s(%)(2)[234U/238U] ± 2s(%)(2)Age(AD ± 2sabs)[234U/238U]i± 2s(abs)(3) 14530.060.004121.50.00309 ± 1.271.0778 ± 0.111703 ± 41.0779 ± 0.001 14820.200.008222.20.00277 ± 0.901.0401 ± 0.111725 ± 31.0402 ± 0.001 14920.200.0041257.80.00733 ± 0.481.0390 ± 0.111244 ± 81.0391 ± 0.001 160180.140.04074.10.00684 ± 0.780.8080 ± 0.121088 ± 180.8075 ± 0.001A.V.M.Samsonetal./JournalofArchaeologicalScience88(2017)24 e 36 34

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cavesacrosstheisland,selectivelyexploitedspeleo-substances,and enhancedmaterialsinorderto(re-)enactchthonicinterventions overcenturies. Theresultsofthisresearchprovideafoundationinbuilding betterinterpretivehypothesesabouthumancaveuseinthe Caribbean,andalsoinintegratingrockartasadatasetwhichcan contributetowiderquestionsinarchaeology. Acknowledgements ThisworkwassupportedbytheNationalEnvironmentResearch Council[grantnumbersIP-1595-1115;1873.0914;IP-1467-1114]at theOxfordRadiocarbonAcceleratorUnitNERCRadiocarbonFacility andtheBritishGeologicalSurvey,andalsobyNationalGeographic Society(grantnumbersHJ-048R-17 & W437-16),theBritishCave ResearchAssociationCaveScienceandTechnologyResearch Initiative,theBritishMuseum,theUniversityofLeicester,The HamiltonKerrInstitute,theDepartmentofNaturalandEnvironmentalResourcesofPuertoRico,theInstituteofCultureofPuerto Rico,andtheCentreforAdvancedStudiesofPuertoRicoandthe Caribbean. 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