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Lead isotopic compositions were measured for 65 sherds from five pottery wares (Plain White, Coarse, Canaanite, White Slip and Base-ring) excavated from the Late Bronze Age site of Hala Sultan Tekke (Cyprus). The elemental composition and isotopic
  See discussions, stats, and author profiles for this publication at: Lead isotopic analysis for the identification of Late Bronze Age pottery from Hala SultanTekke (Cyprus)  Article   in  Archaeometry · April 2010 DOI: 10.1111/j.1475-4754.2010.00535.x CITATIONS 12 READS 75 7 authors , including: Some of the authors of this publication are also working on these related projects: NOCEM: Non-destructive Optical analysis of Cultural Heritage Materials   View projectThe valorization of a portable optical measurement system for the non-destructive, in situcharacterization of cultural heritage materials   View projectKarin NysVrije Universiteit Brussel 48   PUBLICATIONS   236   CITATIONS   SEE PROFILE Nadine MattielliUniversité Libre de Bruxelles 140   PUBLICATIONS   1,906   CITATIONS   SEE PROFILE Frank VanhaeckeGhent University 440   PUBLICATIONS   8,529   CITATIONS   SEE PROFILE Nathalie FagelUniversity of Liège 173   PUBLICATIONS   1,659   CITATIONS   SEE PROFILE All content following this page was uploaded by Nadine Mattielli on 10 February 2014. The user has requested enhancement of the downloaded file. All in-text references underlined in blue are added to the srcinal documentand are linked to publications on ResearchGate, letting you access and read them immediately.  LEAD ISOTOPIC ANALYSIS FOR THE IDENTIFICATIONOF LATE BRONZE AGE POTTERY FROM HALA SULTANTEKKE (CYPRUS)* V. RENSON, 1† J. COENAERTS, 2 K. NYS, 2 N. MATTIELLI, 3 F. VANHAECKE, 4 N. FAGEL 5 and PH. CLAEYS 1 1  Earth System Science, Geology Department, Vrije Universiteit Brussel, Pleinlaan 2, 1050 Brussels 2  Mediterranean Archaeological Research Institute, Vrije Universiteit Brussel, Pleinlaan 2, 1050 Brussels 3  Département des Sciences de la Terre et de l’Environnement, Université Libre de Bruxelles, Avenue F. D. Roosevelt 50, 1050 Brussels 4  Department of Analytical Chemistry, Ghent University, Krijgslaan 281 – S12, 9000 Ghent  5  Department of Geology, Université de Liège, Allée du 6–Août B18, 4000 Liège  Lead isotopic compositions were measured for 65 sherds from five pottery wares (Plain White,Coarse, Canaanite, White Slip and Base-ring) excavated from the Late BronzeAge site of HalaSultan Tekke (Cyprus). The elemental composition and isotopic signature of the sherds werecompared with those of 65 clay samples collected in south-east Cyprus, mainly in the sur-roundings ( < 20 km) of Hala Sultan Tekke. This work shows the effectiveness of using lead isotopic analysis in provenance studies, along with other analytical techniques, such as X-raydiffraction (XRD) and a scanning electron microscope (SEM) equipped with an energydispersive X-ray detection (EDX) facility, to identify the composition of pottery wares and theclay sources used for pottery ware production. KEYWORDS:  LEAD ISOTOPES, POTTERY, CYPRUS, PROVENANCE STUDY, LATE BRONZEAGE, HALA SULTAN TEKKEINTRODUCTION For decades, elemental analysis has been widely used in pottery provenance studies (e.g., Knappand Cherry 1994; Hein  et al . 2002; Mommsen  et al . 2002;Asaro andAdan-Bayewitz 2007;Yellin2007).This approach is often successfully combined with petrographical analysis (e.g., Day  et al .1999; Ben-Shlomo  et al . 2007) and other analytical techniques (e.g., Tchegg  et al . 2008, 2009). Because of the various processes that can be applied to clays before and during pottery produc-tion, as well as the large variety of clays that occur in the vicinity of a production site, mostpottery provenance studies compare pottery samples with a reference group or with pottery of known or assumed provenance. Rarely are pottery samples compared with potential clay sources.Nevertheless, several studies have successfully linked pottery to their raw material (e.g., Adan-Bayewitz and Perlman 1985; Gomez  et al . 2002; Hein  et al . 2004; Tchegg  et al . 2009).Lead isotopic analysis is commonly used to study processes and reveal provenance in geo-sciences (e.g.,Allègre 2005; Dickin 2005). In archaeometry, lead isotopic analysis is largely usedto trace sources of different artefacts, such as glasses (e.g., Shortland 2006), glazes (e.g., Wolf  et al . 2003) and metals from different periods and srcins (e.g., Stos-Gale  et al . 1997; Nieder-schlag  et al . 2003; Durali-Mueller  et al . 2006). So far, lead isotopes have hardly ever been *Received 9 November 2009; accepted 9 January 2010†Corresponding author: email  Archaeometry  53 , 1 (2011) 37–57 doi: 10.1111/j.1475-4754.2010.00535.x © University of Oxford, 2010  applied to characterize the source materials of ceramics (Knacke-Loy  et al . 1995; Renson  et al .2007). However, srcinal isotopic ratios are unlikely to be strongly affected by the pottery-making process, and consequently the isotopic signature of a pottery sherd should indeed reflectthe isotopic signature of the parent material used to manufacture it. Moreover, the recentimprovements in mass spectrometry techniques make it possible not only to determine Pbisotopic compositions with high precision but also to process large batches of samples efficiently.A better insight into the use of raw materials selected for pottery-making contributes to theunderstanding of the socio-economic and cultural relations within a given area and period. Thepresent study uses lead isotopic compositions to document the sources of different pottery wares,found at the Late Bronze Age site of Hala Sultan Tekke- Vyzakia , Cyprus. This harbour townrepresents an ideal case study: it was a major polity involved in diverse and international traderelations and its existence spanned from  c . 1600  bc  to the end of the 12th century  bc .The  207 Pb/  204 Pb and  206 Pb/  204 Pb ratios determined for 65 sherds from Hala SultanTekke- Vyzakia were compared with the values obtained for an extensive set of samples collected from surround-ing geological formations, lithologically well suited for Late Bronze Age ceramic production.This data set is complemented by elemental analysis of selected pottery sherds using a scanningelectron microscope (SEM) equipped with an energy dispersive X-ray detection (EDX) facilityand information on the mineralogy of the sediments using X-Ray diffraction (XRD). Thismulti-proxy study aims: (1) to identify the range of the lead isotopic signatures of the claysavailable in the surroundings of the site and more largely in south-east Cyprus; (2) to define thecharacteristic lead isotopic fingerprint of the pottery production at Hala Sultan Tekke- Vyzakia  bycomparing the signature of the sherds with that of the raw material; (3) to identify the leadisotopic composition of four categories of Late Bronze Age pottery found at Hala SultanTekke- Vyzakia  and compare it with clay sources; and (4) to show that lead isotopes can success-fully be applied in pottery provenance studies. SITE DESCRIPTION The Late Bronze Age settlement of Hala Sultan Tekke- Vyzakia  (hereafter HST) lies on the westshore of the Larnaca salt lake in south-east Cyprus (Fig. 1). The oldest indication of humanhabitation at the site dates from the very end of the Middle Cypriot III Period,  c . 1600  bc . Thematerial culture indicates that the town flourished from the second half of the 14th century  bc  tothe first half of the 12th century  bc . HST is undoubtedly one of the Cypriot urban polities thatactively participated in the Eastern Mediterranean exchange network, in particular during thetimespan of LC IIC–LC IIIA ( c . 1340 to 1110  bc ). By the end of the 12th century  bc  it had beenabandoned (Åström 1986). MATERIAL Pottery sherds Hala Sultan Tekke yielded a large variety of pottery fabrics ranging from the end of MiddleCypriot III until Late Cypriot IIIA2 ( c . 1600 to 1110  bc ).Arepresentative set ( n  =  65) of potterywares was selected covering a timespan from LC IIA to LC IIIA2 contexts ( c . 1410 to 1110  bc )(Renson  et al . 2007, 56–7). Fifty-four samples srcinated from Areas 8 and 22 in the settlement,while 11 more sherds were collected from the assemblage in Tomb 24 (Åström and Nys 2007).Two samples were taken from misfired PlainWhiteWheel-made sherds (HST1a and HST1b; see38  V. Renson  et al . © University of Oxford, 2010,  Archaeometry  53 , 1 (2011) 37–57  Table 2). Since it is unlikely that misfired pots would be imported to the site as such, these twosamples must be considered as purely local products. To define the local (HST) fingerprint, thesemisfired fragments were compared with seven other Plain White and two Coarse sherds. Threeother wares were selected to evaluate their relation to the HST composition: 30 White Slip II andfour Base-ring sherds were considered as representative examples of the two most characteristicLate Bronze Age wares in Cyprus, while 20 Canaanite sherds were chosen to test commonassumptions about the potential provenances of this ware within the Eastern Mediterranean. Sediment and rock samples A geologically and geographically comprehensive set ( n  =  65) of fine-grained or clay-rich sedi-ments was collected in south-east Cyprus (Fig. 1).Among these, 42 samples srcinated from thesurroundings of the site ( < 20 km). Sampling locations were selected based on geologicalmaps and ‘Memoirs’ published by the Geological Survey of Cyprus (Bagnall 1960; Gass 1960;Pantazis 1967; Gass  et al . 1994), to cover the following geological units judged appropriate forpottery production: (1) Holocene alluvium and colluvium (clays); (2) Pleistocene Marine Terracedeposits; (3) Plio-Pleistocene (Apalos-Athalassa Kakkarista formation); (4) Pliocene (Nicosiaformation); (5) Miocene (Pakhna formation); (6) Palaeogene (Lefkara formation) marls and Upper CretaceousVolcanic sequenceUpper CretaceousIntrusive sequencePalaeogeneLefkara formationPleistoceneMarine TerracePlioceneNicosia formationMiocene Pakhna formationUpper CretaceousMoni formationQuaternarysedimentsSouthern TroodosTransform Fault Zone5 kmN Figure 1  Location of samples and Hala Sultan Tekke, modified after the Geological Map of Cyprus (GSD, 1995). Somesamples have been collected from the same outcrop; because of the proximity of some outcrops, the circles represent thelocation of one or several samples. The star indicates the location of Hala Sultan Tekke- Vyzakia  settlement.  Lead isotopic analysis of Late Bronze Age pottery from Hala Sultan Tekke  39 © University of Oxford, 2010,  Archaeometry  53 , 1 (2011) 37–57  chalks; (7) Upper Cretaceous clays (Moni formation); (8) Upper Cretaceous umbers (Fe, Mn richclays) and shales (Perapedhi formation); (9) rocks and clays derived from the weathering of therocks from the volcanic sequence of the Troodos Ophiolite; and (10) a soil from the TroodosOphiolite area. METHODS  Lead isotopic analysis All the samples were dried at 40°C and crushed in an agate mortar under an extracting hood. Thesurface of the sherds was first cleaned using a diamond-bit micro-drill prior to crushing. Theresulting powders were calcined at 550°C for 4 h. Acid digestions were achieved in a laminar-flow clean-air cabinet. About 200 mg of powder was dissolved in closed Savillex ® beakers(125°C, 48 h) using 24M HF sub-boiled and 14M HNO 3  sub-boiled in a proportion of 4:1. Afterevaporation, 5 ml of 6.8M HCl sub-boiled was added (125°C, 48 h), and the solutions wereslowly evaporated at 90°C. The dry residues were finally dissolved in 2 ml 0.5M HBr. Leadisolation was accomplished via ion-exchange chromatography (IEC with DowexAG1–X8 anionexchange resin) and was achieved by successive HBr and HCl additions following the method-ology described in Weis  et al . (2006). The eluted pure Pb solution was evaporated and stored.Prior to isotopic analysis, this purified Pb fraction was re-dissolved in 100  m l of 14M HNO 3 sub-boiled, evaporated and finally dissolved in 1.5 ml of 0.05M HNO 3 .Lead isotope ratios were measured using two multicollector – inductively coupled plasma –mass spectrometers (MC–ICP–MS): a Nu Plasma (Nu Instruments) in operation at the Départe-ment des Sciences de la Terre et de l’Environnement of the Université Libre de Bruxelles,Belgium, and a Thermo Scientific Neptune (Thermo Scientific) in operation at the Department of Analytical Chemistry of Ghent University, Belgium. Thirteen pottery samples were previouslymeasured on the two MC–ICP–MS units to control the reproducibility of the measurements (seeTable 2).A Tl solution was added to each sample and standard to monitor and correct for instrumentalmass discrimination. Lead concentrations varied among the samples; consequently sample solu-tions were prepared to obtain a beam intensity in the axial collector ( 204 Pb) of a minimum of 100 mVand a Pb/Tl ratio of ~5, matching the Pb andTl concentration ratio of the NISTSRM 981‘Common lead’ isotopic standard (150 ng g - 1 in Pb, with 50 ng g - 1 in Tl). The NIST SRM 981standard was measured several times before each analytical session and between each setof two samples on both devices. In total, 219 analyses of the standard were carried out onthe Nu Plasma and yielded the following mean values:  208 Pb/  204 Pb  =  36.714  1  0.006 (2SD), 207 Pb/  204 Pb  =  15.497  1  0.002 (2SD),  206 Pb/  204 Pb  =  16.940  1  0.002 (2SD). Such values agree wellwith the long-term laboratory values [ n  =  1000,  208 Pb/  204 Pb  =  36.713  1  0.012 (2SD),  207 Pb/  204 Pb  =  15.495  1  0.004 (2SD),  206 Pb/  204 Pb  =  16.939  1  0.004 (2SD)] and the MC–ICP–MS valuesof Weis  et al . (2006). These values are also in agreement with thermal ionization mass spectrom-etry (TIMS) triple-spike values previously published by Galer and Abouchami (1998). Thestandard was measured 30 times on the Neptune and yielded the following mean values:  208 Pb/  204 Pb  =  36.669  1  0.003 (2SD),  207 Pb/  204 Pb  =  15.481  1  0.001 (2SD),  206 Pb/  204 Pb  =  16.927  1  0.001(2SD). Although the NIST SRM 981 standard results were within the error of the triple-spikevalues after on-line correction for instrumental mass bias using the bias observed for the addedTl, the sample results were further corrected using the sample-standard bracketing method (asdescribed by White  et al . 2000 and Weis  et al . 2006) to circumvent any instrumental drift during40  V. Renson  et al . © University of Oxford, 2010,  Archaeometry  53 , 1 (2011) 37–57
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