RESEARCHARTICLE The glass walls of Samarra (Iraq): Ninth- century Abbasid glass production and imports NadineSchibille1*,AndrewMeek2,MarkT.Wypyski3,JensKro¨ger4,MariamRosser- Owen5,RosalindWadeHaddon6 1 IRAMAT-CEB,UMR5060,CNRS/Universite´d’Orle´ans,Orle´ans,France,2 DepartmentofScientific Research,TheBritishMuseum,London,UnitedKingdom,3 DepartmentofScientificResearch,The MetropolitanMuseumofArt,NewYork,NY,UnitedStatesofAmerica,4 Museumfu¨rIslamischeKunst, StaatlicheMuseenzuBerlin,Berlin,Germany,5 MiddleEasternSection,VictoriaandAlbertMuseum, London,UnitedKingdom,6 IndependentScholar,London,UnitedKingdom a1111111111 a1111111111 *[email protected] a1111111111 a1111111111 a1111111111 Abstract CapitaloftheAbbasidCaliphatebetween836and892CE,thepalace-cityofSamarraoffers aprecisewindowintoearlyIslamicartandarchitecture.Excavationsconductedmorethan 100yearsagoareseenasthebeginningsofscientificIslamicarchaeology,andhaveyielded OPENACCESS anexceptionalarrayoffindsincludingawealthofglassartefacts.Thechemicalcomposition Citation:SchibilleN,MeekA,WypyskiMT,Kro¨ger ofglassreflectsthenatureoftherawmaterialsandtheirgeologicalprovenanceandcan J,Rosser-OwenM,WadeHaddonR(2018)The glasswallsofSamarra(Iraq):Ninth-century thereforerevealpasttechnologiesandeconomicandculturalinteractions.Throughhigh-res- Abbasidglassproductionandimports.PLoSONE olutionanalysisofacomprehensiveglassassemblagefromSamarrawehavenewevidence 13(8):e0201749.https://doi.org/10.1371/journal. thatpointstotheexistenceofanadvancedAbbasidglassindustry,aswellastheimportof pone.0201749 specificglassobjectsforthethrivingnewcapitalcity.Quantitativeanalyticaldataof58ele- Editor:DongHoonShin,SeoulNationalUniversity mentsbylaserablationinductivelycoupledplasmamassspectrometry(LA-ICP-MS)showa CollegeofMedicine,REPUBLICOFKOREA strikingcorrelationbetweenobjecttypesandglasscompositions.Thecompositionalprofiles Received:February2,2018 oftworelatedplantashgroupsofarchitecturalglasspointtoalocalproduction,destinedfor Accepted:July20,2018 thedecorationofthefamedglasswallsofAbbasidpalaces.Theselectiveuseofobjects, Published:August22,2018 materialsandcolourstocreatereflectiveandluminousglasswallsareindicativeofthegreat culturalandeconomicvalueofglassduringtheAbbasidperiod.Ourfindingsthusconfirmthe Copyright:©2018Schibilleetal.Thisisanopen accessarticledistributedunderthetermsofthe veracityofwrittensourcesthatstipulatetheproductionofglassinthevicinityofSamarra,as CreativeCommonsAttributionLicense,which wellastheimportofselectedartefactssuchasByzantinemosaictesserae. permitsunrestricteduse,distribution,and reproductioninanymedium,providedtheoriginal authorandsourcearecredited. DataAvailabilityStatement:Allrelevantdataare withinthepaperanditsSupportingInformation Introduction files(S1andS2Tables). Funding:PreliminaryEPMAanalyseswere TheArabconquestofEgyptandSyria-PalestineinthetwodecadesfollowingMuhammad’s supportedbyaBritishAcademySmallResearch deathin632CEdoesnotappeartohavehadanimmediateimpactontheprimaryproduction Grant(grantno.SG090427toNS).Thisprojecthas ofglassinthatregion.Traditionallarge-scaleRoman-typemineralsodabasedglassmaking furthermorereceivedfundingfromtheEuropean continuedwellintotheearlyIslamicperiod[1–4].Newrawglasscompositionsreflectingthe ResearchCouncil(ERC)undertheEuropean useofsoda-richplantashinsteadofmineralsoda(natron)emergedonlytowardstheendof Union’sHorizon2020researchandinnovation theeighthandearlyninthcenturybothinEgyptandtheLevant[2,5–7].Thereasonsunderly- programme(grantagreementno.647315toNS). Thefundingorganizationshadnoinfluenceinthe ingthesechangesremainunknown.However,theycoincidedwithanincreasingcultural PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 1/15 Ninth-centuryAbbasidglassproduction studydesign,datacollectionandanalysis,decision eastwardshiftthatbeganduringthelaterUmayyadperiodandacceleratedwiththeriseofthe topublish,orpreparationofthemanuscript. AbbasidsandthefoundationofBaghdadasthenewcapitalin762CE[4,8].Whilenothing Competinginterests:Theauthorshavedeclared remainsoftheroundcityofBaghdad,thecityofSamarrasome125kilometresnorthofBagh- thatnocompetinginterestsexist. dadpreservestheartandarchaeologyoftheearlyAbbasidperiod[9].Samarrawasfoundedin 836CEbytheeighthAbbasidcaliphal-Mu‘tasim(r.833–842)ontheeasternbankoftheTigris asavastpalatialcomplexknownasDāral-Khilāfa[10].Thecityunderwentfurtherdevelop- mentandexpansionunderhissuccessors,mostnotablyhisnephewal-Mutawakkil(r.847– 861),whocommissionedtheGreatMosqueofSamarraandadditionalpalacessuchasal- MutawakkiliyyaandBalkuwārā[11].Samarraservedastheadministrativecentreofthe AbbasidEmpireuntil892CE,whentheAbbasidcourtreturnedtoBaghdad,markingtheend ofSamarra’scaliphalperiod[9]. ArchaeologicalexcavationsconductedatSamarrabyaGermanexpeditionunderErnst Herzfeldin1911and1912–13revealedextensivearchitecturalornamentationsofthepalaces, includinglargenumbersofglassartefacts[12].Circumstantialevidencesuggeststhatglass mighthavebeenworkedorevenmadeinSamarra.Al-Ya’qubireportsinhisKitabal-Buldan, theprincipalcontemporarydescriptionofthefoundationofSamarra,thatthecaliphal-Mu‘ta- sim‘broughtfromal-Basrapeoplewhomakeglass’[9],whilenearbyal-Qadisiyyawasknown inthethirteenth-centuryastheglassworks(ma‘malal-zujaj)andas‘thelargevillage...where glassismade’[9].Sitesurveysoftheareahaveyieldedsubstantialdebrisofapossibleglass industry,andceramicfindstestifytoacontinuousoccupationofal-QadisiyyafromtheSasa- nianperiodthroughtothethirteenthorfourteenthcentury[9].Anotherpieceofevidence comesfromtheglassassemblageitself.GlasswasputtoinnovativeusesatSamarrainawide rangeofarchitecturalornamentationsuchasmosaics,hollowdiamondshaped,triangular, roundorovalinlaysofcolourlesstransparentglassandshinypurpleormillefioritiles.The throneroomofal-Mu‘tasim’sDāral-Khilāfaranksamongtheearliestandmostimportant examplesofarchitecturalglassdecorations(836–842CE)[13],andwrittensourcesindicate thatthelavishglasswallsweresymbolicallycharged[9,14].Theproliferationofdecorative architecturalglassisoneofthemostdistinguishingfeaturesinthearchaeologicalrecordof Samarraandthistypeofglassisoftensupposedtohavebeenmadelocally[12,13]. Toreconstructthenetworksofsupplyandexchange,weconductedhigh-resolutionanaly- sisofmajor,minorandtraceelementcompositionsofastatisticallysignificantnumberof well-datedglasssamplesfromSamarrabyLA-ICP-MS.Thesenewcompositionaldataaredis- cussedinrelationtopublishedearlyIslamicglassassemblages,andidentifiedboththeselective importofspecificobjecttypesaswellastheregionalproductionofglassatSamarra.Ourfind- ingsbringaboutaradicalreinterpretationofthescaleandsophisticationofproductionand interregionaltradeofglassduringtheninthcentury.Theevidenceisfurthermoreconcurrent withearlyIslamictextualsources.Thisisproofoftheaccuracyoftheseaccountsthatexpressa culturalidentityandtheimportanceofglassinearlyIslamicsocieties.Thepresentworkthere- foreconsiderablyexpandsearlieranalyticalstudiesofIslamicglassassemblages[15–18]by relatingthecompositionaldatatoartefacttypeandopticalpropertiestoassesstheculturaland economicvalueofvitreousmaterialsduringtheearlyIslamicperiod. Materialsandmethods Glasssamples TheglassfindsfromSamarrahavebeenpublishedaspartoftheexcavationreportsin1928by CarlJohanLamm[12],representingthefirstextensivepublicationonIslamicglassandIslamic archaeologymoregenerally[19].Amongalmost400cataloguedglassfindsnowhousedinvari- ousmuseumacrosstheworldarealargenumberofrelativelysimpleblownandundecorated PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 2/15 Ninth-centuryAbbasidglassproduction vessels,includingbowls/plates,bottles,jugsandlamps,andmouldblownvesselsmostlyof weaklycolouredorcobaltblueglass,aswellasmoresophisticatedvesselswithpinched, stamped,engravedorlinearwheel-cutdecorationsandafewexampleswithappliedandpainted surfacedecorations[12].Numerousarchitecturalglassesmakeupalargepartoftheassemblage, andincludewindows,monochromeormillefioritiles,mosaictesserae,drawntesseraeaswellas hollowinlaysofcolourlesstransparentglassthatarediamondshaped,triangular,roundoroval. Forthepresentstudy,265oftheSamarraglassfindsfromthepubliccollectionsoftheMuseum fu¨rislamischeKunstinBerlin(Germany),theDepartmentoftheMiddleEastintheBritish MuseumandtheMiddleEasternSectionintheVictoriaandAlbertMuseuminLondon(UK) wereselectedforanalysis.Nopermitswererequiredforthedescribedstudy,whichcomplied withallrelevantregulations.Thesampleswerechosensoastoincludeallvesseltypes(bottles, bowls,plates),opticalproperties(transparent,opaque,differentcolours)anddecorativetech- niques(reliefcut,engraved,painted,mouldblown),andincludeallthearchitecturalglasses(Fig 1andS1Table).Mostoftheglassesforwhichthearchaeologicalcontextisknownwereeither foundinoneofthepalaces(Dāral-Khilāfa,Balkuwara)orintheGreatMosque,andtheoriginal cataloguenumbersfromLammarecross-referencedwherepossible(S1Table). Fig1.GlassartefactsfromSamarrarepresentingthedifferentcompositionalgroups.(A)Regularlyshapedmosaictesseraeofnatron typebaseglass(V&AA.58-1922);(B)glassinlaysofplantashgroup1(Sam806.2,I.9325.1,I.9325.2,I.9325.4;photosC.Krug,Museum fu¨rislamischeKunst/StaatlicheMuseenzuBerlin);(C)fragmentofmillefioriglasstileofplantashgroup2(V&AC.743-1922);(D) cobaltblueflaskneck(V&AC.750-1922);(E)rimfragmentofpaintedglassbowlbelongingtothemiscellaneoussamples(SamKat273; photoM.Wypyski,Museumfu¨rislamischeKunst/StaatlicheMuseenzuBerlin).ImagesA,CandDfromtheVictoriaandAlbert Museum,London[http://collections.vam.ac.uk];imagesBandEfromtheMuseumfu¨rislamischeKunst/StaatlicheMuseenzuBerlin [www.smb-digital.de/eMuseumPlus]. https://doi.org/10.1371/journal.pone.0201749.g001 PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 3/15 Ninth-centuryAbbasidglassproduction Analyticalmethods Smallfragmentsofglasswereremovedfromtheselectedartefacts,setinepoxyresinandpol- ishedtoremoveanysurfacecontamination.Laserablationinductivelycoupledplasmamass spectrometry(LA-ICP-MS)analyseswereperformedonthepolishedsamplesatIRAMAT-CEB inOrle´ans(France),usingaThermofisherElementXRmassspectrometerandaResoneticUV lasermicroprobeequippedwitha193nmExcimerlaser[20–22].Thelaserwassetata100μm spotsizethatwasoccasionallyreducedwhenmanganesesaturationoccurredandanalyseswere carriedoutat5mJwithafrequencyof10Hz,apre-ablationtimeof20secondsfollowedby30 secondsanalyticaltime.Quantitativewt%andppmconcentrationsofthefifty-eightelements measuredwerecalculated,using28Siasinternalstandardandarangeofwell-characterisedglass referencematerials(NistSRM610,CorningB,CandD,APL1).Toestablishprecisionandaccu- racy,glassstandardsNISTSRM612andCorningAwererunatregularintervals(S2Table).The detectionlimitsvarybetween0.1and0.01%formajorelementsandbetween20and500ppb fortraceelements. Results Glassgroupprovenance ThechemicalfingerprintsobtainedbyLA-ICP-MSclassifyallsamplesfromSamarraassoda- lime-silicaglassestypicaloflateByzantineandearlyIslamicassemblagesfromtheeastern MediterraneanandMesopotamia(S1Table).Themajorityofthesampleshaverelativelyhigh levelsofpotash(K O>1.5%)andmagnesia(MgO>2%),indicatingthatasoda-richplant- 2 ashservedasthesourceofthealkali[23].Asmallgroupofsampleshaslowpotassiumand magnesiumconcentrations(<1.5%)characteristicofglassmadewithsodaderivedfroma mineralsource.Theyarenatron-typeglassescharacteristicofglassproducedpriortotheninth centuryCE.Theemeraldgreendecorationofonevesselfragment(BerlinSam014)with approximately70%leadoxidecorrespondstoahighleadsilicaglass(S1Table).Similarcom- positionshavebeenidentifiedamongearlyIslamicglasses,forexample,fromtheSerc¸iLimani shipwreck[24]aswellasNishapur[25].Thissamplewillnotbediscussedfurther. Theanalysesidentifiedthreedifferentsourcesofsupply:thereuseofoldernatron-type glass,importsofcontemporaryplantashglassfromtheLevantand/orEgypt,andMesopota- mianglassproduction(Table1andFig2).Remarkably,theanalyticalresultsshowaclosecor- respondencebetweenthecompositionalgroupsandobjecttypes.Almostalltraditional Table1. Meansandrelativestandarderrorofthemean(RSEM)ofthefiveglassgroupsidentifiedatSamarra. Data[wt%]werereducedtotheshownmajor,minor andtraceelementoxidesandnormalisedto100%. NaO MgO AlO SiO PO Cl K O CaO TiO MnO FeO Sr Zr 2 2 3 2 2 5 2 2 2 3 [ppm] [ppm] Natronglass tesserae(n=33) 16.9 0.72 2.72 69.1 0.15 1.02 0.65 7.00 0.14 0.57 1.04 411 72.9 RSEM[%] 2.10 6.20 3.47 0.59 11.7 3.98 6.67 6.35 8.55 22.7 16.8 7.35 8.90 Mesopotamian group1(n=72) 13.2 5.09 0.81 70.0 0.12 0.64 3.22 6.39 0.03 0.29 0.23 398 31.0 RSEM[%] 0.58 0.93 2.10 0.17 1.91 1.48 1.76 0.83 3.48 3.78 4.03 0.93 3.58 group2(n=136) 15.2 5.55 1.37 67.0 0.12 0.61 2.71 5.43 0.08 1.28 0.65 438 106 RSEM[%] 0.73 0.85 1.08 0.25 1.75 0.78 0.87 0.94 1.37 4.13 4.63 0.86 1.87 Imports Coflasks(n=23) 14.3 2.83 2.10 67.6 0.19 0.71 2.26 6.66 0.13 0.59 2.56 332 95.7 RSEM[%] 0.81 2.83 2.63 0.40 3.59 2.98 2.42 2.28 2.46 10.4 4.25 1.55 4.56 misc(n=15) 14.4 3.25 2.60 65.9 0.31 0.61 3.07 7.13 0.15 1.48 1.06 453 93.5 RSEM[%] 3.25 3.17 13.7 1.48 4.49 5.34 3.38 5.88 11.3 21.1 13.1 7.92 10.9 https://doi.org/10.1371/journal.pone.0201749.t001 PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 4/15 Ninth-centuryAbbasidglassproduction Fig2.DifferentfluxingagentsoftheSamarraglasses.KOversusMgOconcentrationsidentifydifferencesbetween 2 natron-typeglasses,plantashglassesfromtheSyro-PalestinianIslamictraditionandplantashglassesof Mesopotamianprovenance(sub-divisionsareindicatedbydashedlines). https://doi.org/10.1371/journal.pone.0201749.g002 regularlyshapedtesserae(Fig1A)andonecolourlessbeakerwithlinearwheelcutdecorations (BerlinSam038MW)wereproducedfromnatron-typeglassessourcedfromtheLevantine coastorEgypt.TheplantashglassescanbefurthersubdividedintoMediterraneanandMeso- potamianglassgroups(Fig2)thatcorrespondroughlywithartefacttypesand/orcoloursand byextensionthequalityoftheglass.Thecolourlessdiamondshapedandroundwallinlaysas wellassomedelicatelydecoratedvesselsaremadeofaparticularlyhighqualityglassofMeso- potamianorigin,whilethestronglycolouredarchitecturalglassesandthemajorityofaquacol- ouredvesselsderivedfromasilicasourceofMesopotamianprovenancethatwasofalower purity.Athirdplant-ashgroup(henceforthreferredtoasmiscellaneous)isrelativelyheteroge- neousbothintermsofitscompositionaltraitsaswellasthetypologyanddecorativetech- niquesemployed,suggestingtheimportofindividualobjectstoSamarra(S1Table).Finally,a chemicallyrelativelytightclusterofcobaltblueflasksexhibitsclearMediterraneancharacteris- tics.Witheachcompositionalgroupbeingrepresentedbyatleast15samples(>5%ofthe assemblage),therelativestandarderrorsofthemean(RSEM)aregenerally(cid:20)5%forallbase glasselements(Table1).Thisshowsthatourgroupassignmentisrobust,whichallowsusto drawstatisticallyandarchaeologicallysignificantconclusionsfromourdata. ReusedtesseraeofLevantineandEgyptianorigins Uponcloserinspection,thenatron-typemosaictesseraedonotformahomogeneousgroup butshowsignificantvariationsintheiraluminium,calciumandheavyelementconcentrations reflectingdifferentsilicasourcesratherthansecondaryadditivesandthusdifferentorigins (Fig3).Aboutonethirdofthetesseraearecharacterisedbymoderatesodalevels,aluminacon- tentsofabout3%,limebetween8%and10.5%andlowheavymineralimpuritiesconsistent withLevantineIglass(Fig3A).Thistypeofglasshasbeenidentifiedamongfourth-toeighth- centuryglassassemblagesinIsrael(Apollonia,BetShean,DorandJalame)[2,26,27].Asec- ondgroupexhibitssignsofrecycling.Itresemblesso-calledFoy-2[28]onaccountofelevated heavyelements,relativelyhighsodalevelsandhigherstrontiumtocalciumratios(S1Table). Foy-2iswidespreadamongsixth-andseventh-centuryCEglassassemblagesfromdiverse MediterraneanandEuropeansites[22,29–31].Theremainingsampleshavesubstantially lowercalciumlevels,hightitanium,zirconiumandhafnium,andvaryingtitaniumtoalumin- iumratios(Fig3A).ThesefeaturespointtoanEgyptianorigin.Thesub-groupwiththelowest limeandhighestaluminaconcentrationsresemblethecharacteristicsofEgyptI,aprimary PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 5/15 Ninth-centuryAbbasidglassproduction Fig3.Analysisofthesilicasourcesofthenatron-typeglassesfromSamarra.(A)CaOversustheratioofTiO / 2 AlO;(B)CeO/ZrO versusYO/ZrO;(C)TiO/AlO versusAlO/SiO. 2 3 2 2 2 3 2 2 2 3 2 3 2 https://doi.org/10.1371/journal.pone.0201749.g003 productiongroupdatingtotheeighthcenturyCEbasedonastudyofIslamicglassweights [32].Asinglevesselfragmentwithlowaluminium,titaniumandrelativelyhighcalciumoxide concentrationsandnotabletracesofmanganeseandantimonycorrespondstorecycled Romanglass[33]. Correlationsbetweenthegeographicaloriginofnatron-typeglassesandtheratiosof yttriumtozirconiumversusceriumtozirconium,andtitaniumtoaluminiumversusalumin- iumtosilicahavebeenobservedelsewhere[6,31].GlassesfromEgypthavetypicallylower Y O /ZrO andCeO /ZrO ratios(<0.08and<0.18,respectively)comparedtoglassesfrom 2 3 2 2 2 theLevant(>0.1and>0.24).Duetothehigheraluminalevelsrelativetothesilicaandtita- niumcontents,LevantineIhassimultaneouslyhigherAl O /SiO (>0.04)andlowerTiO / 2 3 2 2 Al O ratios(<0.04)thanEgyptianglassgroups.Usingthesemodels,theinitialassignments 2 3 regardingtheprovenanceoftheSamarratesseraearereinforced(Fig3Band3C).Thetesserae thathadbeenattributedtotheLevantineItypehavehighY O /ZrO andCeO /ZrO ratios 2 3 2 2 2 aswellashighaluminarelativetosilicaandlowtitaniumtoaluminaratios(Fig3Band3C). TheEgyptiangroupshaveinversecharacteristics.TheprovenanceofFoy-2islessclear,asthe samplesoccupyanintermediatepositionasregardstheirY O /ZrO andCeO /ZrO ratios 2 3 2 2 2 thatsuggestssomedegreeofmixingand/orrecycling[6].Recyclingisconfirmedbytheele- vatedphosphorusandantimonycontentsofthesesamples(S1Table). ThecollectionofmosaictesseraeretrievedfromSamarraisevidentlyaneclecticmixtureof differentnatron-typebaseglasses,allofwhichpre-datethefoundationofSamarraintheninth century.Thetesseraewereclearlynotproducedtoasinglerecipeorasinglecommission. Theymightinsteadhavebeenscavengedfrombuildingsnolongerinuseandimportedto SamarrafromthewesternregionsoftheAbbasidCaliphate,fromSyria-Palestineand/or Egypt.Whatallthetesseraehaveincommonthoughisthefactthattheyarecompositionally distinctfromtheoutputoftheglassmakingindustrythatsuppliedSamarrawiththebulkof soda-richplantashglasses. Regionalproductionofplantashglassesandimports EarlierstudieshaveshownthatIslamicsoda-richplantashglassesfromtheLevantandEgypt canbedistinguishedfromMesopotamianplantashglassesbasedonthepotashandmagnesia concentrations[34].Applyingathresholdof6.5%forthesumofmagnesiumpluspotassium oxide,theassemblagefromSamarracomprisespredominantlyMesopotamianplantash glasses,whereasthecobaltblueflasksappeartorepresentaSyro-PalestinianorEgyptianpro- duction(Fig2).Themiscellaneousplantashgrouphasdiversefeaturesandconsistsofamix ofMediterraneanandMesopotamiansamples.TheglassesofMesopotamiangroup1and2 PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 6/15 Ninth-centuryAbbasidglassproduction arefurthermorecharacterisedbyhighermagnesiumtocalciumratiosandexceptionallylow phosphoruscontents(P O <0.15%)comparedtotheotherplantashtypes(Fig4A).Thelith- 2 5 iumandboronlevelsrelativetothesodaconcentrationsseparatetheplantashgroupseven moreclearly(Fig4B).Thecobaltblueflasksformaneatclusterwithhigherboronlevelsthan anyoftheotherplantashgroups,whilethemiscellaneousplantashgrouphasthelowestlith- iumvaluesrelativetosoda,whichmayberelatedtoitsoveralllowermagnesiumcontents(Fig 2).Groups1and2resembleeachothercloselyintermsofmostash-relatedelementssuchas potassium,magnesium,lithiumandboronbutdifferintheirabsolutecalciumcontents. Group1hasonaveragehighercalciumoxidelevels((cid:25)6.4%)comparedtogroup2((cid:25)5.4%) andaccordinglysomewhatlowermagnesiatolimeratios(Table1andFig4A).Thesecomposi- tionalfeaturesindicatedifferencesintheplantsthatwereusedand/orinthepreparationofthe ash.Soda-richplantashwascombinedeitherwithquartz-richsandorwithcrushedquartz pebbles,providingadditionalelementstoseparatethegroupsandtracetheirlikelyorigins. Highqualityarchitecturalglass—theuseofquartzpebbles(group1). Plant-ashgroup 1comprisesalmostallcolourlessglasses,particularlyallthediamondshapedandroundwall inlays(Fig1B)andseveralfinelydecoratedvesselssuchasacold-painted,gildedandengraved roundbottle(BerlinSam042)andareliefcutbowldecoratedwithpalmetteandanimalmotifs thatissaidtorepresentthehigheststandardsofearlyIslamicglass(BerlinSam018)[35].The samplesofgroup1containonaverageonly0.3%manganeseoxide,toolowtoactefficientlyas adecolourant.Allsampleshavelowsilica-relatedimpuritiessuchasverylowtitaniumandzir- coniumlevels(Fig5A),anaveragealuminacontentofonly0.8%(Fig5BandTable1)and overallverylowtraceelements(Fig5C).Thesecompositionalcharacteristicsaretheresultof theuseofaverycleansilicasource(seediscussion). Aneconomicalvariant—theuseofquartz-richsand(group2). Group2representsthe bulkoftheSamarraglassassemblageandincludesafewcolourlessandaquacolouredvessels, allofthescratch-engravedsamples(e.g.BMSamarra146–153),lampsandwindows,aswellas allofthecolouredarchitecturalglassessuchasdarkpurpleandgreendrawntesserae,chunky goldleaftesseraeandmillefioritiles(Fig1CandS1Table).Thealumina,iron,titaniumand zirconiumcontentsaswellasallothertraceandrareearthelementsareonaveragehigher thaningroup1(Fig5).Thisprovidesevidencethatthesilicasourceunderlyinggroup2was notaspureastheoneusedforgroup1. Thepurityoftherawmaterialswasapparentlynotasdecisiveinthecaseofgroup2given thefactthatcolouringorde-colouringagentswereaddedtotherawmaterial.Allthegoldleaf tesserae,forexample,aremadefromtransparentglasswithagreenishtingeandcontainsignif- icantamountsofmanganeseoxide(1%-2%)asadecolourant.Thedrawntesseraeareeither Fig4.Variationsintheplantashcomponentofthefourplantashgroups.(A)phosphoruscomparedto magnesiumtocalciumoxideratiosconfirmdifferentgeographicalorigins;(B)boronandlithiumconcentrations(both normalisedtothesodaconcentrations)identifydifferentplantashcomponentsandadditives. https://doi.org/10.1371/journal.pone.0201749.g004 PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 7/15 Ninth-centuryAbbasidglassproduction Fig5.AnalysisofthesilicasourcesoftheplantashgroupsfromSamarra.(A)differentialzirconiumandtitanium correlationsclearlydistinguishthecobaltblueflasksfromtheotherplantashgroups;(B)aluminiumandiron concentrationsindicatedifferentdegreesofsilicarelatedimpurities;(C)selectedtraceelements,normalisedtothe uppercontinentalcrustcompositions[36],highlightingtheverylowcontaminantsinplantashgroup1. https://doi.org/10.1371/journal.pone.0201749.g005 darkgreen,colouredbyacombinationofcopperandlead,ordarkpurpleduetomanganese. Themillefioritilescomprisemanganeseblack,cobaltblue,copper-ironred,lead-tinyellow andtinwhitesegments(S1Table).Giventhatthebaseglassofgroup2waseithercoloured and/ordestinedforobjectsoflowerprestigesuchassmallinkbottles(BerlinSam024MW),a moreeconomicalglassmakingrecipeandtechnologywereevidentlychosen.Thefactthat groups1and2arecompositionallycloselyrelatedandofacommonMesopotamianorigin demonstratesthediversityoftheAbbasidglassindustryandtheexistenceofdeliberatepro- ductionstrategies. Commoditybranding—thecobaltblueflasks. The23cobaltblueflasksformaverydis- tinctivegroup(Fig1D).Theplantashcomponentresemblesthatofplantashglassproduced inSyria-PalestineorEgyptwithmoderatepotassiumandmagnesiumlevels(Fig2).Thebase glassofthesebottlesisderivedfromasilicasourcedefinedbyhighertitaniumtozirconium ratiosaswellashigheralumina,traceandrareearthelementsthanplantashgroups1and2 (Fig5).Thecobaltblueflasksexhibitalsoadistinctboronsignature(Fig4B).Judgingfromlit- erarytreatisesthatdescribetheprocessingofthecobaltbluepigmentforglazedtiles[37],the elevatedboronmightinfactbetheresultoftheadditionofboraxduringthepre-treatmentof thecobaltore.Cobaltisstronglycorrelatedwithironandcopper,andzinclevelsarelikewise increased.Zinc-richcobaltisconsidereddiagnosticofearlyIslamicglassmaking[38–41]and wasidentifiedprimarilyamongassemblagesofsupposedlyMesopotamianoriginfromCtesi- phonandal-Raqqa[15],Nishapur[25,42]aswellasIslamicglassbeadsfromninth-ortenth- centurytombsinAlbania[43].However,therelativezinclevelsinthecobaltblueflasksfrom SamarraaremarkedlylowerthanthoseoftheMesopotamiancobalt-zincglasseswherezinc contentstypicallyequalorexceedthecobaltconcentrations.Incontrast,acobalttozincratio similartothatoftheSamarraflasks(*1.5x)wasrecentlyfoundinasetofalmostidentical PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 8/15 Ninth-centuryAbbasidglassproduction cobaltbluebottlesfromRamladatingfromtheninthtotheeleventhcentury[18]aswellasin twofragmentsassociatedwiththetenth-centurytankfurnace2intheglassmakingcomplexof Tyre[44].Consequently,thecobaltcolorantemployedfortheblueflasksfromSamarrais morecloselyassociatedwitheasternMediterraneanglassmaking,andtheglassesaretherefore not,ashasbeenpreviouslyproposed,ofMesopotamianprovenance[18].Theoriginofthe cobaltmineralitselfremainselusive.ThecobaltmineofQamsar,Kāshān(Iran)thathasoften beencitedasthesourceoftheIslamiccobaltpigmentdoesnotappeartocontainsufficient zinctobeasuitablecobaltore[45]. AccordingtoLamm[12],theHerzfeldexcavationsyieldedfragmentsofabout170ofthese elongatedtubularflaskswithshortnarrownecksandoftenroundedbases,madeofwafer-thin cobaltblueglass(Fig1D).Thebottlesthemselvesbearsignsofmassproductionasthenecks werecrudelysawnoff.Someofthenecksarestillclosedbyeithercottonwoolorpapyrus. Thesetypesofelongatedcobaltbluebottlesappeartohavebeenverywidespreadduringthe ninthtoeleventhcenturyCE.ThousandsoffragmentshavebeenfoundalloverNishapur[19] andfurtherexamplesareknownfromEgyptatFaiyum,FustatandRaya,fromPalestineat Tiberias,RamlaandCaesarea,fromTunisiaatSabraal-Mansuriya,aswellasfromtheArabian Peninsula,ChinaandKenya[18,46].Thepeculiarshapeoftheseflasksisveryconspicuous, whichmighthaveservedthepurposeofcommoditybrandingtofacilitateproductrecognition ofapresumablyvaluableandlight-sensitivecontent[46].Theirsupplytothepalacesof Samarra,wherelargenumberswerediscoveredintheso-called‘harim’southofthethrone roomoftheDāral-Khilāfa[12],suggeststhattheyservedsomesortofcosmeticpurpose. Miscellaneousvesselsandimports. Themiscellaneousgroupisastypologicallydiverse asitiscompositionallyvaried.Itencompassesvesselsrepresentingdifferentdecorativestyles suchasareliefcutvesselwithanimaldecoration(BerlinSam052MW),mouldblownbowls withverticalribs(BerlinSam033MW),vesselswithappliedtrails(BerlinSam054MW), paintedvesselfragments(Fig1E),asmallinkbottle(BerlinSam068MW)andtwomarvered bowls(BerlinSam060&062MW),adecorativetechniquethatiscommonlyattributedtoan EgyptianorSyrianprovenance[47]. Compositionally,thesamplesofthisgroupspanawiderangeofimpuritiesintroducedwith thesilicasource.Thealuminalevels,forexample,varyfromabout0.7%toover6%(Fig5B), whiletheheavyandrareearthelementsareonaveragehighercomparedtotheotherplantash groupsfromSamarrawithapositiveeuropiumanomaly,probablyduetothefeldspathicfrac- tionwithinthesilicasource(Fig5C).Ithastobestressed,however,thattheindividualsamples ofthisgrouparehighlyvariable(Fig5Aand5B).Thehighimpuritiesandvarianceareindica- tiveoftheuseofdifferentsandsasthestartingmaterial.Forinstance,thesampleswiththe highestaluminacontentsandlowmagnesiumtocalciumratios(Fig6)bearallthecomposi- tionalattributesofcolouredglassesfromNishapur,suggestingacentralAsianglassproduction [18].Giventhattheglassesofthisgroupareneithercompositionallynortypologicallyuni- form,itislikelythatfinishedglassobjectsarrivedindividuallyatSamarrasuchas,forexample, asmallinkbottle(BerlinSam068MW)thatmayhavebeenthepersonalpossessionofoneof themanypoetsthatwereactiveduringSamarra’scaliphalperiod.Thisisincontrasttothe blueflasksthatappeartohavebeenimportedinlargenumbers,implyingamorecentrally organisedtradeofthesespecialisedobjects. Discussion Thetraceelementanalysisincombinationwiththetypologicalaffiliationssupportsamodel wherebyglasswasproducedatandselectivelyimportedtoSamarra.Allthenatron-typetes- seraepredatethefoundationofSamarraandwereimportsfromSyria-Palestineand/orEgypt. PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 9/15 Ninth-centuryAbbasidglassproduction Fig6.TheSamarraplantashgroupscomparedtocontemporaryglassassemblages.Aluminaversusmagnesiato limeratiosofpublisheddataofglassesfromRamla[18],Tyre[44],Nishapur(Wypyski,inpreparation)andVeh Ardasir[48,49],indicatingtheproposedseparationlinesbetweenearlyIslamicglassesfromtheeasternMediterranean withlowmagnesiatolimeratios,theSamarraglasswithhighmagnesiatolimeratiosandlowaluminalevels,and MesopotamianglasseswithhigheraluminaconcentrationstypicalofcentralAsianproductions(lay-outofgraph adaptedfrom[18]). https://doi.org/10.1371/journal.pone.0201749.g006 Thecompositionalfeaturesofthecobaltblueflasksandsomemiscellaneoussamplespoint likewisetoaneasternMediterraneanprovenance.Plantashgroups1and2ontheotherhand areundoubtedlytheoutputofMesopotamianglassmakingeventhoughtheyrepresentdiffer- entproductionstrategiesandrawingredients.Theanalyticaldataprovedthatthesilicasource underlyingplantashgroup1wasexceptionallypure,implyingtheuseofquartzpebblesora verycleanquartz-richsand.Theheavyelementlevels(Zr,Hf,Th)ofSamarragroup1only slightlyexceedthoseofsomeIronAgeplantashglassesthatarebelievedtohavebeenmade fromquartzpebbles[50].Nonetheless,itisnearimpossibletodistinguishbetweentheuseof quartzpebblesandquartzrichsandsatthisstage.Whatiscertain,isthattheglassmakersdelib- eratelychoseapuresilicasourcethatallowedthemtocloselycontroltheingredientsandthe productionprocesses.Byexploitingrawmaterialsofhighpurity,theglassworkerswereableto obtaintrulycolourlessglasswithnodiscernibletingeoraquacolourthatisusuallyimparted toglassbytheironimpuritiesinsand.Theeffortandspecialcarethatwastakentoproduce thesecolourlessglassesareindicativeoftheirculturalvalueandhighprestige.Thesilicasource ofplantashgroup2wasricherinimpuritiesandpossiblyprovidedacheaperand/orless work-intensivealternativetothehigh-qualitygroup1glasses. CompositionalfeaturescomparabletothoseofSamarragroups1and2havepreviously beenattributedtoMesopotamianglassmakingassimilarglasseshavebeenfoundatninth-to tenth-centuryNishapur,earlyIslamicRamlaandRaqqa,aswellasamongthefourth-tofifth- centurySasanianglassesfromVehArdaˇsīrsouthofBaghdad(Fig6)[2,7,15,25,48,49].Our analyticalresultsprovidethefirstindicationoftheprimaryproductionofglassatSamarra itself.ThemanufactureofglassinthevicinityofSamarraseemshighlylikelygiventherelative homogeneityofthebulkoftheanalysedassemblage(groups1and2)compared,forinstance, totheglassfindsfromNishapurorVehArdaˇsīr(Fig6).InviewofthevariabilityoftheseMes- opotamianglasses,thetightclusteringofSamarragroup1,themajorityofwhichpertainstoa specialtypeofarchitecturalglass,anditscompositionalresemblancetogroup2pointto closelyrelatedprimaryproductions.Aregionalproductionofglasswouldhaveascertainedthe readysupplyofvitreousmaterialsfortheornamentationofthenewlybuiltpalace-cityof Samarra.ApossiblecandidateofanearlyIslamicglassproductionsiteisal-Qadisiyyaabout25 kmsouthofSamarra,knownfromhistoricalsourcesasthesitewhereglasswasproduced PLOSONE|https://doi.org/10.1371/journal.pone.0201749 August22,2018 10/15
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