MediterraneanArchaeologyandArchaeometry,Vol.10,No.2,pp.1523 Copyright2010MAA PrintedinGreece.Allrightsreserved.

WINEANDOLIVEOIL FROMANEARLYMINOANIHILLTOPFORT

Koh,A.J.andBetancourt,P.P.
TempleUniversity,1210W.BerksSt.,PhiladelphiaPA191226008,USA

Received:09/11/2009 Accepted:14/09/2010 Correspondingauthor:Ppbcourt1@aol.com

ABSTRACT
AphroditesKephaliisasmallhilltopsiteinEasternCrete.Itspotteryindicatesthatitwasinhab itedduringEarlyMinoanI(EMI),ca.32002700B.C.Thefortifiedsitehasaconsiderableamountof storage,includingninepithoi.Theanalysisbygaschromatographyofsherdsfromthesiteindicates thatvesselscontainedoliveoilandwine.Theseresultsaretheearliestdocumentedpresenceofboth ofthesecommoditiesinCrete.Theevidenceisimportantbecausethedomesticationoftheoliveand grapeatthisearlyperiodinCretehasbeenpreviouslyquestioned. KEYWORDS: Early Minoan I, EM I, olive oil, olives, grapes, wine, fortifications, Aphrodites Kephali,Isthmus of Ierapetra, pithos,pithoi,Hagios Onouphrios,Minoanpottery, gaschromatog raphy,ARCHEM

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INTRODUCTION
AphroditesKephaliisasmallhilltopsitein eastern Crete. It is located on the Isthmus of Ierapetra,7kmnorthofthesoutherncoastand 5 km south of the northern coast. The location was excavated in 1997 under the direction of TheodoreEliopoulos(Eliopoulos1998,312)and in 2003 under the direction of Stavroula Apos tolakou. Cleaning and conservation work was conductedonthehilltopin2006and2007under thedirectionofStavroulaApostolakouwiththe assistance of Philip Betancourt (Betancourt 2008a;2008b)1. Thesitecontainsasmallbuilding,fragments ofotherwallsthatseemtoformcasementsfora fortificationenclosingtheupperpartofthehill, asmallopencourtyardwithanareaburnedred from fires, and an entrance for a natural cave. The pottery, which is all from EM I (ca. 3200 2700 B.C.), includes vases in the Hagios Onouphrios Style, heavily burnished vessels made of calcitetempered fabric, and several otherclassesofpottery.Thepresenceofceram ics made in several different fabrics suggests that the vessels originate from various sources, all of them within Crete. Among the vases are many sherds from pithoi including enough fragmentstorestoreoneexample. Organic residues were extracted from sev eral fragments in order to provide information on the commodities contained by the clay ves sels. The program of extraction and analysis was accomplished by a collaboration between the following institutions: Archaeochemistry Research in the Eastern Mediterranean (AR CHEM);the24thEphorateofClassicalandPre historic Archaeology; the Foundation for Re search and TechnologyHellas (FORTH); the Department of Classics and Archaeology Pro gram at Tufts University, the INSTAP Study Center for East Crete (INSTAPSCEC) in Pacheia Ammos, Crete; the Museum of Cretan Ethnology Research Centre in Vori, Crete; and theDepartmentofArtHistory,TempleUniver sity, Philadelphia, Pennsylvania. This non destructive field technique can provide impor tantinformationtosupplementthedatarecov eredbyothermeans2.Paststudieshavehelped illuminate the function of both objects and the

spaceinwhichtheywerefoundandthenature of production and consumption (Koh 2008b; Brogan and Koh 2008); in the future, studies willhopefullyrevealintricaciesrelatedtoover archingissuessuchaseconomyandtrade.

METHODOLOGY
Sherdsofpotteryforanalysiswerecollected in 2006 under the supervision of Philip Betan court during the cleaning of the site under the directionofStavroulaApostolakou(Fig.1).

Figure1.ProfiledrawingsofpotteryfromAphrodites Kephalianalyzedfororganicresidues.Scaleas marked.

Sherds were lifted from the soil without be ing directly touched by anyone,and they were immediately wrapped in aluminum foil in the fieldandtransportedtotheINSTAPStudyCen ter for extraction of the sample. This swift and careful isolation of sherds likely contributed to the excellent results produced for this present study, which stands in contrast to poor results yieldedinthepastfrom objectsexcavateddec ades ago and provided by both active excava tion projects and museums. Residues for this studywereextractedandprocessedinthepro gram designed by Andrew Koh for ARCHEM (Koh2008a)onJune25,2006withtheassistance ofMiriamClintonoftheUniversityofPennsyl vania.Theresiduewasextractedbyheatingthe sherdintwodifferentsolvents.Theprocesswas

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performedintheconservationlaboratoryofthe INSTAP Study Center for East Crete, with two samples extracted from each sherd in succes sion, one using dichloromethane followed im mediately by one using ethanol3. This process produced twentyeight samples from fourteen objects.Theresultingsampleswereanalyzedat the Museum of Cretan Ethnology Research Centre in Vori using the Centres GCMS in strument (Gas Chromatography and Mass Spectrometry)4. This instrument couples the separation potential of gas chromatography with the characterization ability of mass spec trometry.Itshouldbenotedthatapreliminary interpretationofthechromatogramswasmade without the advance benefit of a formal study ofthesubsequentlycleanedandconservedves sels, minimizing unwarranted influences on interpretation. After a formal study of the ves sels by P. Betancourt, the preliminary interpre tation of the organic contents was further nu anced by A. Koh, but no significant changes needed to be made. Wepresent below the best interpretationswehavetodateforthefiveob jects that produced the clearest and strongest chromatograms and are of particular relevance tothestudyofthesite. As a control on the methodology, a sample of the soil that contained the sherds was col lected and processed for extraction of organic

compounds. The goal was to discover if any significant traces of organic compounds were included within the natural sediment on this siteasaresultofleachingfromdecayingplant matter or from other causes. The soil yielded two samples using dichloromethane and etha nol, and they were processed using the same methodology as that employed for the twenty eight samples extracted from sherds. The soil samplesproducedonlyminutetracesoforganic residues,indicatingtheprobabilitythatnocon taminationenteredthesherdsfromcasualcon tact with the soil at the site. In addition to the soil samples, blanks were inserted periodically ineachGCMSrunatVori.Eachoftheseblanks producednopeaksintheirchromatogramscon firmingforusthattherewerenoresidualcom pounds from preceding samples injected into theGCcolumn.

RESULTSOFTHEINVESTIGATION(TA BLE1)5
AK1(ARCHEM135[ethanol]andARCHEM 136[dichloromethane],Figs.1and2) Closed vessel, base sherd. D of base ca. 12 cm. A light red fabric (2.5YR 6/6 to 6/8) with angular red inclusions, with the surface miss ing.

Figure2.GCMSchromatogramforvesselAK1(no.136AK1D).

Comments: The fabric suggests this closed vessel, which is probably a jug or a small jar, originated in eastern Crete. Almost all of the EMIpotteryfromKephalaPetras,asettlement

eastofSiteia,ismadeofthisfabric(forthesite, seePapadatos2007). AnalysisResults:Thetwosamplesproduced nearly identical chromatograms with the strongest peaks suggesting the presence of or

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KOH,A.J.ANDBETANCOURT,P.P.

ganicacids.Mostnotablewerepeakselutingat 11.4min(tartaricacid),15.9min(syringicacid), 20.2min(stearicacid),20.8min(palmitate),24.2 min (stearate), 28.6 (oleanolic acid), and 32.3 (phthalate). Conclusions:Tartaricacidindicatesthepres enceofwine,whilesyringicacidspecifiesthatit isred.Oleanolicacidisacommonindicatorfor thepresenceofpistaciaresin.Thevesselproba bly stored resinated red wine (for shortterm usejudgingbyitssize). AK4(ARCHEM139[DCM]andARCHEM140 [E],Fig.1) Open vessel, rim sherd. D of rim ca. 12 cm. Anunevenlycolored,blacktoduskyred(2.5YR 3/2) calcitetempered fabric, burnished on inte riorandexterior.Straightrim. Comments: The fabric indicates the vessels productioncenterisdifferentfromthatofAK1. Thisfabriciscommononthenorthcoastinthe regionoftheGulfofMirabello. Analysis Results: The E chromatogram pro ducedresultsthatweresimilartothoseofAK1 butwiththeabsenceofoleanolicacid,suggest ing that the wine was not resinated. Perhaps this is due to the vessels closer point of origin and/oritsopenshape.TheDCMchromatogram hasstronganddistinctpalmiticandstearicacid peaks but little otherwise. Why this difference from AK 1? It is difficult to say with certainty, butitispossiblethatthesherdslocationonthe rim(versusthebaseforAK1)playedarolein howtheresidueswereabsorbedandpreserved onthedifferentvessels.

Conclusions: The vessel held red wine, whichwaslikelynotresinated.Thesherdwasa rim fragment, which often produces quantita tively weaker and qualitatively distinct results in comparison with samples from bases and bodysherds. AK6(ARCHEM143[DCM]andARCHEM144 [E],Fig.1) Jar, body sherd. Max dim 5.6 cm. An un evenly colored, mostly black fabric with a red dishyellow(5YR6/6)surface,withangularred inclusions,wipedonexteriorandroughonthe interior. Comments:Theroughinteriorindicatesthat thiswasaclosedvessel.Thefabricissimilarto thatofAK1. AnalysisResults:Thissamplehasachroma togram that is both qualitatively (multitude of fatty acid peaks) and quantitatively (limits of the yaxis for intensity had to be tripled to ac commodate unusually strong peaks) different from the previous samples.4 Most importantly, the peak for oleic acid at 24.2 min is especially strong, strongly supporting the presence of oliveoil. Conclusions: Vessel AK 6 was probably a storagejarforoliveoil. AK8(ARCHEM147[ethanol]andARCHEM 148[DMC],Figs.1and3) Closedvessel,bodysherd.Maxdim4.8cm. A reddish yellow fabric (5YR 7/8), with roundedtosubroundedinclusionsofmanydif ferent stones (South Coast Fabric), wiped on exterior.

Figure3.GCMSchromatogramforvesselAK8(no.148AK8D).

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Comments: This fabric is from a different source from the other vessels discussed in this study. The vessel had a closed shape (it was probablyajugorajar). Analysis Results: The two chromatograms arequitesimilartothoseofAK6,downtothe unusually strong peaks produced by the DCM extraction. Conclusions:Strongoleicacidpeakssuggest thestorageofoliveoil. AK9(ARCHEM149[DCM]and150[ethanol], Figs.1and4) Pithos,completeprofile.Ht74.6,htofcollar 14.5to15,dofrim42,dofbody65,dofbase42

cm,capacity150litersfilledtothebottomofthe collar, 165 liters filled to the rim. Fabric with angular red inclusions, mostly light red (2.5YR 6/8), wiped on exterior. Flat rim with short in cised lines, above a plain collar; body with roundedprofile,withfourverticalhandleswith thick oval sections; slightly rounded base. Decoratedwithraisedmoldings:bandwithver tical incisions at base of collar; large herring bone motifs, placed vertically, on shoulder, withsetsofthreeverticalbandsabovethehan dles; nine horizontal bands on body. Dark slip (varyingfromredtoblack)onexterior.

Figure4.GCMSchromatogramforvesselAK9(no.149AK9D).

Comments:Thefabricindicatesthattheves sel comes from East Crete (see AK 1). Sherds fromsimilarpithoicomefromseveralotherEM I contexts in Crete, including from Knossos (Wilson and Day 2000, 4850), Debla (Warren and Tzedhakis 1974,323), Kalo Chorio (Haggis 1996,674 and fig. 30, no. KT 87), and Kephala Petras(Papadatospersonalcommunication;for thesite,seePapadatos2007). Analysis Results: The results are somewhat similartothoseforAK4,butwithsomenotable differences.TheDCMchromatogramisdevoid of any of the organic acid peaks that typically occurearlyinthechromatogramupto15min. The ethanol chromatogram produced weak peaksforthepresenceofwinewithnoevidence forresination. Conclusions: This pithos shows weak evi denceforredwine,possiblynonresinated.The large vessel had a long enough life for it to crackandthenberepairedbydrillingtoallowa

cord to be laced across the crack.Because stor ageofliquidwouldhavebeenimpossibleafter the crack appeared, the wine must have been storedinthevesselatanearlyperiodinitshis toryofuse.Thisconclusionissupportedbythe relatively weak chromatographic evidence for wine noticed from the outset during the pre liminary interpretation before cleaning and conservation. Perhaps the pithos attractive ap pearance provided a second life for a vessel originallyusedtostorewine.

DISCUSSION
Authors studying early agriculture have re marked on the absence of data to support the production of wine and olive oil during the Early Minoan period (for olive oil, see Hansen 1988,4446,5152;forwine,seeHalstead1988, 529). The evidence from gas chromatography forthepresenceofbothcommoditiesisimpor tant for an understanding of the agricultural

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KOH,A.J.ANDBETANCOURT,P.P.

production of the early stages of Minoan cul ture. In fact, the evidence providesmuch more than the information that these two products were present. Sherds from the pithos no. AK 9 survivedinenoughfragmentstoallowitsresto ration(Fig.1),andtestswithfillingthelargejar demonstratedthatitwouldhold150kgiffilled to the bottom of the collar and ca. 165 kg if filledtonearthebrim.Thisrepresentsthestor ageofalargequantityofwine.Aminimumof nine pithoi could be recognized from the large numberofpithossherdsatthesite,whichindi cates that the site was engaged in bulk storage of commodities in large amounts. That dry products were stored as well is proved by the continueduseofthepithosafteritcrackedand was repaired. Wine from several different places was also present in smaller vessels, and olive oil was being stored at this site as well. Only red wine was recognized from these analyses, but some of it was resinated. The presenceofresinatedwineisnotasurprise,be cause this class of beverage has already been recognized by gas chromatography of Minoan vessels from the end of the Early Bronze Age (Beestonetal.2006,420423,426)andevenear lierbyliquidchromatographyinLevantineves sels found in the Protodynastic tomb of Scor pion I at Abydos, Egypt (McGovern 2003, 85 106). Thoughthesamplesetissmall,thepossibil ityexiststhatthereisacorrelationbetweenthe resination of wines and their point of origin, though this can be difficult to ascertain when there is a quantitative difference in extant or ganicsandadditionalvariablesinherenttoves sels from disparate origins. Besides the evi dence for pistacia resin, there were no obvious signs of flavors added to the wine at Aphro ditesKephali,thoughthepossibilityexiststhat theydidnotsurviveortheyarestillwaitingto bediscoveredinthehundredsofminutepeaks yet to be identified in each chromatogram. However,judgingbytheunclutteredsimplicity of the chromatograms (based on the relatively few,butstrongpeakspresent)andthenatureof thesiteitself,chancesarethatthevastmajority of commodities were used as basic sustenance in a setting surrounded by few luxurious adornments.

The remarkable preservation of wine and oliveoilatsuchanearlysiteinCretepresuma bly has much also to dowith the nature of the site and its associated vessels. As a relatively shortlived hilltop fort overlooking a strategic route across the Isthmus of Ierapetra, Aphro dites Kephali, in fact, provides an ideal situa tion for organic residue analysis. Its size and function predicates that the storage of basic commodities will likely be emphasized in its archaeological record with less likelihood for a preponderance of luxury or specialized vessels complicating the task of residue interpretation, arguablythemostdifficultpartoftheanalytical process since scientific instruments only iden tify compounds, not the original commodities fromwhichtheywerederived.Therefore,final interpretationsintheendmustrelyonaholistic knowledgeofasiteandthecharacteristicsofits naturallandscape,fromwhichthecommodities derive,inordertodeducethemostlikelyiden tificationofthecommoditiesinquestion.Natu rally, interpretations must periodically be reas sessed,furthernuanced,andevenalteredwhen new information arises. ARCHEM studies in thepasthaveshownthatsimplercontextssuch as the one at Aphrodites Kephali, or, con versely,extraordinarilyspecializedspaces,such as perfumed oil workshops, provideeasier tar gets for immediate interpretation than typical, daily, domestic spaces, where vessels were of tenreusedinantiquitytoholddifferentorgan ics, like todays kitchen (cf. Brogan and Koh 2008,128129). Finally, it should be noted that one methodological advantage of using a double solventextractiontechnique,asshownthrough this study, is the hint it provides as to the nature of commodities originally contained in thevessel.Thisresultsfromcomparingthetwo resultant chromatograms from the same object with each other and comparing these chromatograms, in turn, with those produced by other objects from the same context. In the caseofAphroditesKephali,thevesselsusedto hold olive oil, and its various fatty acids, were separated more discriminately by the two solvent process, especially when compared to vessels used to hold wine and its diagnostic organic acids. While this two step extraction

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process is not absolutely necessary and constraints related to resources and time often make it impractical, this study shows that doublesolventextractionscanbeaninvaluable

toolforthecharacterizationofancientresidues in the right situation and can be selectively utilized when certain compound are expected (e.g.fattyacids).

REFERENCES
Beeston,R.F.,Palatinus,J.,Beck,C.,andStout,E.C.(2006).AppendixM.OrganicResidueAnaly sis of Pottery Sherds from Chrysokamino, in The Chrysokamino Workshop and Its Territory (HesperiaSuppl.36),AmericanSchool,Princeton,413428. Betancourt,P.P.(2008a).AphroditesKephali,Kentro.TheNewsletteroftheINSTAPStudyCenterfor EastCretevol.11,1213. Betancourt,P.P.(2008b).TheBronzeAgeBegins:TheCeramicsRevolutionofEarlyMinoanIandtheNew FormsofWealthThatTransformedPrehistoricSociety,INSTAPAcademicPress,Philadelphia. Biers,W.R.,Gerhardt,K.O.,andBraniff,R.A.(1994).LostScents:InvestigationsofCorinthianPlas tic Vases by Gas ChromatographyMass Spectrometry. MASCA Research Papers in Science andArchaeologyvol.11,UniversityofPennsylvaniaMuseum,Philadelphia. Brogan,T.M.,andKoh,A.(2008).FeastingatMochlos?NewEvidenceforWineProduction,Stor age, and Consumption from a Bronze Age Harbor Town on Crete, in Dais: The Aegean Feast,editedbyL.HitchcockandR.Laffineur,125131.Aegaeum29,LigeandAustin. Eliopoulos,T.1998.APreliminaryReportontheDiscoveryofaTempleComplexoftheDarkAges atKephalaVasilikis,inEasternMediterranean:CyprusDodecaneseCrete16th6thcent.B.C. Proceedings of the International Symposium Held at Rethymnon, Crete in May 1997, V. Kara georghisandN.Chr.Stampolidis,eds.,MinistryofCulture,Athens,301313. Gerhardt, K. O., Searles,S., and Biers, W. R. (1990). Corinthian Figure Vases: Nondestructive Ex tractionandGasChromatographyMassSpectrometry,inOrganicContentsofAncientVes sels: Materials Analysis and Archaeological Investigation, W. R.Biers and P.McGovern, eds., MASCAResearchPapersinScienceandArchaeology,vol.7,UniversityofPennsylcvania Museum,Philadelphia,.4150. Haggis,D.C.(1996).ExcavationsatKaloKhorio,EastCrete,AmericanJournalofArchaeologyvol.100, 645681. Halstead,P.(1988).OnRedistributionandtheOriginofMinoanMycenaeanPalatialEconomies,in ProblemsinGreekPrehistory:PapersPresentedattheCentenaryConferenceoftheBritishSchool ofArchaeologyatAthens,Manchester,April1986,E.BFrenchandK.A.Wardle,eds.,Bristol ClassicalPress,Bristol,519529. Hansen,J.M.(1988).AgricultureinthePrehistoricAegean:DataversusSpeculation,AmericanJour nalofArchaeology,vol.92,3952. Koh,A.(2008a).TheARCHEMProjectTurnsFive,Kentro.TheNewsletteroftheINSTAPStudyCenter forEastCrete,vol.11,68. Koh, A. (2008b). Wreathed in a Fragrant Cloud: Reconstructing a Late Bronze Age Aegean Workshop of Aromata,VDMAktiengesellschaft,Saarbrucken. McGovern, P. (2003). Ancient Wine: The Search for the Origins of Viniculture, Princeton University Press,Princeton. Papadatos,Y.(2007).TheBeginningofMetallurgyinCrete:NewEvidencefromtheFNEMISet tlementatKephalaPetras,Siteia,inDay,P.M.,andDoonan,R.C.P.,eds.,Metallurgyinthe EarlyBronzeAgeAegean(SheffieldStudiesinAegeanArchaeology7),Oxbow,Oxford,154167. Warren,P.,andTzedhakis,J.(1974).Debla,anEarlyMinoanSettlementinWesternCrete,Annualof theBritishSchoolatAthens,vol.69,299342. Wilson,D.E.,andDay,P.M.(2000).EMIChronologyandSocialPractice:PotteryfromtheEarly PalaceTestsatKnossos,AnnualoftheBritishSchoolatAthens,vol.95,2163.

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Table1.ObjectsandContents

OBJECT AK1 AK4 AK6

SHAPE closedjugorjar openvessel closedjar

AK8

closedjugorjar

AK9

pithos

FABRIC light red with angu larredinclusions blacktoduskyred black with reddish yellow surface and angular red inclu sions reddish yellow with rounded/subrounded inclusions light red with angu larredinclusions

PLACEOFORIGIN EastCrete GulfofMirabello EastCrete

CONTENTS resinatedredwine redwine oliveoil

southcoast

oliveoil

EastCrete

originally red wine but later onlydrygoods

NOTES
1. Thanks are expressed to Stavroula Apostolakou and Theodore Eliopoulos for permission to publish this site. Research was supported by Temple University and the Institute for Aegean Prehistory. Koh would like to thank his coauthor for inviting him to Aphrodites Kephali and introducing him to Aegean Prehistory those many years ago. This study would not have been possible without the capable staff of the Institute for Aegean Prehistory in both Philadelphia and Pacheia Ammos. Christophe and Despina Vallianos opened up their office and home in Vori to support this research; the Museum of Cretan Ethnology Research Centre has been an invaluable resourceforthestudyofancientcommodities.Finally,itissafetosaythatbothmeasurable(Figs.2 4 layout) and immeasurable contributions by Laura Labriola Koh were vital to this studys completion. 2.Inadditiontotheinsightgainedintotheefficacyofthistechniquefromthispresentandpast studies,researchisnowbeingconductedatTelKabriwiththesupportofcodirectorsAssafYasur LandauandEricH.Clinetodirectlycomparethistechniquewithdestructivetechniquescommonly usedtoday(cf.Beestonetal.,pp.413414,foragooddescriptionofthisdestructiveextractiontech niqueandanexcellentoverviewoforganicresidueanalysisingeneral;cf.Gerhardtetal.,p.42,and Biersetal,p.19forstudiesshowingtheefficacyofnondestructiveextractiontechniques).AtTel Kabri,adjacentsherdsfromvesselswerecollectedbyARCHEMandKristineMerrimanofOxford University with the intent of comparing results in the near future. The ARCHEM sherds were processed using the nondestructive extraction technique outlined in this study while Merriman will use the destructive extraction technique favored by chemists. Combined with petrographic thinsectionanalysisbyDavidBenShlomooftheHebrewUniversity,ourultimategoal,however,is toilluminatepatternsinbothlocalconsumptionandtradenotpossiblewithoutthecontributionof theseanalyticaltechniques. 3.SherdswereplacedinaBuchiPolyevaporatorwith~200mlofsolventfor~20minat60Cun dervacuumandthengravityfilteredtoproduce20mlmastersamples. 4.ForGCMSanalysis,subsamplesweretakenfromthemastersamplesbymeasuring300lof solutionintoglassinsertsplacedinto2mlvials,whichwerethencentrifugallyevaporatedandre filledwithdichloromethaneforinjectionintoaShimadzu5050AGCMSattheMuseumofCretan EthnologyResearchCentre. ThesplitlessinjectorandinterfaceontheGCwerebothsetto250Cwitha1minuteinterface time.Thecarriergas(helium)hadacolumninletpressureof60kPawithalinearvelocityof53.8 cm/sec.Theinitialoventemperaturewassetto130Candheldfor2minutesbeforereaching250C atarateof5C/min,atwhichtimeitwasheldforanadditional19minutes,givingatotalprogram

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time of 45 min/sample. A fused silica SPB5 GC capillary column (30m x 0.32 mm, 0.50m) was usedintheGCanddirectlyinsertedintoamethanechemicalionizationsourcesetat0.85kVwitha 50450m/zscan. 5. The chromatogram produced from the nonpolar DCM solvent had significantly stronger peaks overall but certain compounds were especially pronounced compared to the E chroma togram.Thisnotonlypointstodifferencesinthevesselscontentswhencomparedtoothervessels atthesite,butalsopossiblyhintsatthenatureofthevesselsuseinantiquityanditsstateofpreser vationoverthemillenniasince.