PROVENANCE OF OBSIDIAN EXCAVATED FROM LATE CHALCOLITHIC LEVELS AT THE SITES OF TELL HAMOUKAR AND TELL BRAK,SYRIA*

X‐ray fluorescence and laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS) analyses conducted on 40 obsidian samples from the Late Chalcolithic 2 levels at Tell Hamoukar and Tell Brak in north‐east Syria have shown trends towards the exploitation of obsidian sources in the eastern Taurus. While the Bingöl region appears to provide the majority of obsidian to both sites, there is also evidence of more minor exploitation of a source in the Lake Van area and an altogether unknown source (X). This paper presents the data acquired from the analyses of the archaeological obsidian and situates these results within their chronological and regional contexts.     

MICROANALYTICAL METAL TECHNOLOGY STUDY OF ANCIENT NEAR EASTERN BRONZES FROM TELL BEYDAR*

Forty‐six bronze objects have been investigated to assess their composition and microstructure, using SEM–EDX and optical microscopy. The bronzes originate from Tell Beydar, a site in the northeastern part of Syria that was mainly occupied during the third millennium bc . The compositional results of the metals show a clear chronological sequence in the use of the alloying elements arsenic and tin. In addition, the microstructure indicates advancement in the metalworking techniques that were used.     

INSIGHTS INTO NORTH MESOPOTAMIAN ‘METALLIC WARE’*

With the aim of shedding new light on the still poorly understood North Mesopotamian metallic ware, ceramic and soil samples from Tell Beydar (northeastern Syria, third millennium bc ) were investigated using a range of analytical techniques, including optical microscopy, SR–XRD and SEM–EDX. The objective of this work was to differentiate calcareous metallic ware from non‐calcareous ware without the aid of chemical analyses and to find further validation of the existing hypothesis that the former group is an imitation of the latter. A third group of metallic wares from Tell Beydar is believed to be of non‐local, still regional origin.     

REPRODUCIBILITY OF ELEMENTAL ANALYSES OF BASALTIC STONE ARTEFACTS BY QUADRUPLE ICP–MS USING DIFFERENT SAMPLE SIZES AND DIGESTION METHODS,WITH IMPLICATIONS FOR ARCHAEOLOGICAL RESEARCH

Using high‐precision inductively coupled plasma mass spectrometry (ICP–MS), we measured >40 elements in basalts sampled by diamond micro‐drills to evaluate the effectiveness of different digestion methods and the reproducibility of elemental analysis for different sample sizes from 5 mg to 100 mg. The results indicate that those elements that are most suitable for geochemical characterization, such as rare earth elements (REE), high‐field strength elements (HFSE) and certain mobile elements (Rb, Sr, Th, U), show excellent reproducibility with an average relative standard deviation (RSD) of 3% between open‐beaker and pressured ‘bomb’ digestion methods. This observation rules out the presence of refractory phases such as zircon, which can only dissolve in pressured ‘bombs’, and suggests that the results from open‐beaker digestion are reliable. The ICP–MS data for powders of different weights ranging from 10 to 100 mg collected from two fine‐grained basalt artefacts display excellent reproducibility, with a RSD of <5% for the most important elements. The reproducibility is reduced when including the 5 mg weight fraction (RSD of ～2–9%), which is still sufficient for archaeological applications. Our results demonstrate the usefulness of 10 mg samples for elemental measurement, which is valuable for geochemical characterization and sourcing of fine‐grained basalt artefacts from museum collections that require minimal destructive sampling.     

First Geochemical ‘Fingerprinting’ of Balkan and Prut Flint from Palaeolithic Romania: Potentials,Limitations and Future Directions

Long‐distance raw material transfers across Romania prior to the Last Glacial Maximum have previously been inferred from either visual and/or petrographic observations of East Carpathian sites. We investigated the potential to ‘fingerprint’ flint from archaeological sites at Mitoc‐Malu Galben and Bistricioara–Lut?rie III in Eastern Romania, using in situ high‐precision analyses of 28 major, minor and trace elements determined by laser ablation – inductively coupled plasma – mass spectrometry (LA–ICP–MS) in combination with multivariate statistical analysis. Our results suggest that geochemical analyses have the ability to distinguish between different geographical sources but are unable to positively associate flint artefacts from archaeological contexts to these geochemical groups. The mismatches of signatures between artefacts and geological materials, however, raise new questions and open unforeseen perspectives.     

THE USE OF TRACE ELEMENT ANALYSIS OF ENTRAPPED SLAG INCLUSIONS TO ESTABLISH ORE – BAR IRON LINKS: EXAMPLES FROM TWO GALLO‐ROMAN IRON‐MAKING SITES IN FRANCE (LES MARTYS,MONTAGNE NOIRE,AND LES FERRYS,LOIRET)*

Knowledge of the iron trade in ancient times rests on determining the source of the objects recovered during archaeological excavations. Unfortunately, attributing the origin is not always possible using archaeological tools alone. Trace element data of the ore and the archaeological material (reduction and reheating slags, entrapped slag inclusions from the bloom, bar iron and iron blades) from two Gallo‐Roman iron‐making centres, Les Martys (Montagne Noire) and Les Ferrys (Loiret), were determined using ICP–AES/MS and LA–ICP–MS. The results highlight a continuity of composition that makes it possible to establish a link between the initial ore and the semi‐finished iron products.     

Bitumen in Early Ceramic Art: Bitumen‐Painted Ceramics From Late Neolithic Tell Sabi Abyad (Syria)*

The paper presents the results of a chemical analysis of black pigment used to decorate pottery from Late Neolithic Tell Sabi Abyad, northern Syria (c. 6100 cal bc ). The pigment appears to be bitumen. A comparison with known reference samples from modern locations of bituminous sources in the Near East suggests that the bitumen used to paint ceramics at Tell Sabi Abyad came from at least two different source areas in northern Iraq. The bitumen‐painted ceramics at Tell Sabi Abyad represent the earliest evidence attested so far of bitumen used as a pigment for pottery decoration.     

Archaeobotanical inference of Bronze Age land use and land cover in the eastern Mediterranean

Charcoal and charred seeds at five Bronze Age archaeological sites discern ancient land use in the eastern Mediterranean. Seed frequencies of orchard crops, annual cereals and pulses, and wild or weedy plants are used to characterize plant utilization at different archaeological sites on the island of Cyprus, in the Rift Valley of Jordan, and in the Jabbul Plain and along the upper Euphrates River valley in Syria. Seed to charcoal ratios provide proxies to determine the relative usage of dung versus wood for fuel across the ancient Mediterranean landscape. Greater charcoal and lower charred seed values are interpreted to represent a wooded environment, while higher amounts of charred seeds and minimal wood charcoal suggest a much great use of dung as a fuel source. Interestingly, Politiko-Troullia (Cyprus, Cypriot archaeological sites are, by convention, named for the nearest modern village (Politiko), followed by an italicized toponym (Troullia) referring to the plot of land that incorporates the site) has the lowest seed to charcoal ratio, suggesting its residents primarily burned wood and that the landscape surrounding Troullia remained relatively wooded during the Bronze Age. In contrast, villagers at Tell el-Hayyat (Jordan) utilized a mixture of wood and dung, in contrast to Tell Abu en-Ni’aj (Jordan), and especially Umm el-Marra and Tell es-Sweyhat (Syria), where inhabitants relied solely on dung fuel. Comparative analysis and interpretation of seed and charcoal evidence thus illustrates the variety of fuel use strategies necessitated by the dynamic and diverse Bronze Age landscapes of the Eastern Mediterranean.     

Geochemical and Petrographic Analysis of Late Bronze Age Cypriot Ceramics (White Slip I and II and Monochrome) from Tell Atchana/Alalakh (Hatay) in the Amuq Valley

White Slip ware, both White Slip I and II, and Monochrome ware are Middle to Late Bronze Age Cypriot pottery types found across a large area of the Eastern Mediterranean region. A vast quantity of these wares has also been uncovered in Tell Atchana/ancient Alalakh in Hatay in southern Anatolia. We analysed a total of 56 White Slip (n = 36) and Monochrome potsherds (n = 20) from Tell Atchana using XRF, ICP–MS and petrographic thin‐section methods. The main aim of the study was to explore the compositional characteristics of the wares and to determine whether they are local imitations of the Cypriot White Slip and Monochrome wares or represent Cypriot exports to this region. The analytical results proved that White Slip I and II were produced from raw clay of mafic and ultramafic source rocks exposed in the Troodos Massif, available in the Limassol area of southern Cyprus and traded to Tell Atchana. Examples of Monochrome ware excavated in Tell Atchana were also imported to the region, most probably from east/north‐east Cyprus. These results demonstrate a close trading connection between Tell Atchana/Alalakh and southern Cyprus during the Middle to Late Bronze Age.     

A Diachronic Study of Networks of Ceramic Assemblage Similarity in Neolithic Western Anatolia,the Aegean and the Balkans (c.6600–5500 bc)

This study compares the results of Jaccard and Kulczynski‐2 similarity measures on a sample of ceramic assemblages to reveal spatio‐temporal patterns in the relationship between Neolithic sites in western Anatolia and south‐eastern Europe (c.6600–5500 bc ). The results show that the relationship between spatial distance and ceramic assemblage similarity has increased through time, which supports previous interpretations of leapfrog migrations and subsequent regionalization in ceramic assemblages during the Neolithic. A diachronic network analysis demonstrates the continuation of Aegean networking after the spread of farming.     

THE TRADING OF ANCIENT GLASS BEADS: NEW ANALYTICAL DATA FROM SOUTH ASIAN AND EAST AFRICAN SODA–ALUMINA GLASS BEADS*

The occurrence of similar glass beads at archaeological sites in Africa and Asia bears witness to the trade relationship between the two continents. This paper reports elemental analysis results from a recent in‐depth laser ablation – inductively coupled plasma – mass spectrometry (LA–ICP–MS) study of a group of archaeological glass beads with a specific alumina‐rich composition from East Africa, India and Sri Lanka. Based on the concentrations of the trace elements, two different subgroups were identified. One subgroup occurs at early periods (fourth century bce to fifth century ace ) in South India and Sri Lanka. The second subgroup appears at later dates in Africa and was identified at different Kenyan sites dated from the ninth to the 19th century ace , and at the contemporaneous site of Chaul in western India.     

Cultural interactions during the Ubaid and Halaf periods: Tell Kurdu (Amuq Valley,Turkey) obsidian sourcing

In order to decipher cultural influences, the inter-regional contacts of the Tell Kurdu settlement have been investigated through obsidian sourcing for the Halaf and Ubaid phases (c. 5700–4300 cal. BC). The chemical composition of nine artifacts from three archaeological levels of the site have been determined and compared to source data obtained in our laboratory or available in the literature. Trace and major element analyses were performed respectively by inductively coupled plasma - mass spectrometry (ICP-MS) and atomic emission spectrometry (ICP-AES). The results assignments point out five distinct sources which highlight northwestward and eastward connections. Besides the “traditional” procurement areas (Göllü Dag and Nemrut Dag massifs; Bingöl region), the development of new exploitation centers (northeast Anatolia and northeast Van lake) is noteworthy. These results of obsidian provenances are compared to those of other raw materials and production originating from distant areas, in order to outline Tell Kurdu trade networks during the Halaf and Ubaid periods.     

FINGERPRINTING ANCIENT EGYPTIAN QUARRIES: PRELIMINARY RESULTS USING LASER ABLATION MICROPROBE-INDUCTIVELY COUPLED PLASMA-MASS SPECTROMETRY*

Microchemical analysis of minerals present in pottery and stone artefacts may help determine their provenance. Electron microprobe major element analyses of augite suggest that minor elements (Ti0₂,MnO, Aa₂O) are important in fingerprinting basalts. This points to the potential usefulness of trace elements. Augite present in six basalt samples (representing all known/suspected Pharaonic basalt quarries in northern and middle Egypt) and basaltic temper fragments in two New Kingdom pottery sherds was analysed for 28 trace elements (Sr, Ba, Th, U, Zr, Hf, Nb, Ta, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu. Sc, V, Cr, Ni, Ga) by laser ablation microprobe-inductively coupled plasma-mass spectrometry (LAM-ICP-MS, laserprobe). Cluster and discriminant analysis indicate that (1) laserprobe trace element data are more effective at fingerprinting basalts than conventional electron-microprobe data and (2) basaltic temper in the two sherds does not match any of the quarries. Microbeam techniques providing trace element data may represent the future for mineral-based provenance studies.     

NO STONE UNBURNED: A COMPOSITIONAL ANALYSIS OF OBSIDIAN MICRODEBITAGE BY LASER ABLATION TOF–ICP–MS

Obsidian is an effective material for the study of prehistoric raw material use and exchange, due to the high degree of homogeneity and redundancy of obsidian materials and manufactured objects in the archaeological record. The destructive nature of many analytical techniques often impedes compositional research because of the damage that may occur to priceless archaeological artefacts. The combination of time‐of‐flight (TOF) ICP–MS with a laser ablation sample introduction system provides a highly efficient means of chemically characterizing obsidian. This study shows that sample size limit capabilities of TOF–ICP–MS analysis of obsidian can reach less than 100 μm. Sampling and analysis of microartefacts enables researchers to overcome problems of sampling bias with very little damage to the valuable existing materials within the archaeological record and expands the potential for chemical compositional analyses in archaeology.     

Kites — new discoveries and a new type

The stone structures known as kites and found widely in ‘Arabia’, are one of the more intriguing archaeological traces in what are often arid and bleak landscapes. They were first reported from the air in 1927, and by 1995 — largely through interpretation of old aerial photographs — c.500 had been identified. Now (2012), remote‐sensing techniques of various kinds have produced a huge increase, to over 3000. Recent work has also extended the geographical spread of kites in ‘Arabia’, from south‐eastern Turkey and north‐western Iraq to central Yemen. Much detailed work will be required to develop and refine a typology for kites as a whole and to digest and present data from remote sensing on which specialists may build interpretations and explanations. Current tabulation and mapping, however, already reveal patterns, and the discovery of an unusual form in the desert between Damascus and Palmyra in Syria deserves special attention.     

FINGERPRINTING OF ROMAN MINTS USING LASER‐ABLATION MC–ICP–MS LEAD ISOTOPE ANALYSIS*

In this paper we present data to demonstrate the applicability of laser‐ablation MC–ICP–MS isotope analysis to archaeological artefacts, in this case Roman silver coins. The technique requires no chemical preparation, does minimal damage to the sample and yields external reproducibility that is better than conventional TIMS analysis; ²⁰⁷Pb/²⁰⁶Pb =±0.015% 2σ in comparison with ²⁰⁷Pb/²⁰⁶Pb =±0.04% 2σ, respectively. We show that Pb isotope compositions give isotope fingerprints to mints despite the likely reworking of the metal during coin production.     

THE SEARCH FOR THE ORIGIN OF BITUMEN EXCAVATED FROM ARCHAEOLOGICAL SITES IN THE NORTHERNMOST ISLAND IN JAPAN BY MEANS OF STATISTICAL ANALYSIS OF FI–MS DATA*

The origin of bitumen excavated from archaeological sites in Hokkaido, the northernmost island in Japan, was sought by means of field‐ionization mass spectrometry (FI–MS) and gas chromatography – mass spectrometry (GC–MS) of the hydrocarbon components. The field‐ionization mass spectra were decomposed by Z‐numbers into several components, where the Z‐number refers to z in the formula C _n H _2n+z . This is equivalent to the deficit number of H atoms, when compared to the corresponding saturated hydrocarbon, which is related to the number of saturated hydrocarbon rings in alkanes. By use of the spectral intensities of the seven alkane components in each sample, multiple discriminant analysis was employed for the data of raw bitumen samples and excavated samples from archaeological sites. Based on this method and the gas chromatogram type, the following bitumen trade in the prehistoric age of Japan was elucidated: bitumen from Niigata, one of the main sources on the main island of Japan, spread to the north in 2000 bc , probably via the coastal zone, and reached a small island near the north end of Hokkaido. Bitumen from Sakhalin reached the central lowland in Hokkaido, but it went no further. Bitumen from Akita, another main source on the main island, spread over northern Honshu much earlier and reached the Oshima peninsula, the southwestern part of Hokkaido. The Akita bitumen scattered into the central lowland after the Niigata and Sakhalin bitumen. This area is believed to be the place where people from the south and the north met in those periods.     

IN‐SITU ELEMENTAL AND Sr ISOTOPE INVESTIGATION OF HUMAN TOOTH ENAMEL BY LASER ABLATION‐(MC)‐ICP‐MS: SUCCESSES AND PITFALLS*

Trace element and Sr isotope data were obtained by laser ablation‐ and solution mode‐(MC)‐ICP‐MS analysis for tooth enamel from remains excavated at the New Kingdom period Egyptian colonial and Nubian cemetery site of Tombos (Sudan). Elemental abundances determined by both methods of ICP‐MS analysis yielded comparable values; however, ⁸⁷Sr/⁸⁶Sr values obtained by laser ablation were higher compared to their solution mode counterparts. This discrepancy is related to the production of a molecular interference—Ca + P + O (overlaps ⁸⁷Sr); hence the higher ⁸⁷Sr/⁸⁶Sr values recorded during ablation analyses. Laser ablation studies of enamel may provide relatively precise ⁸⁷Sr/⁸⁶Sr values rather quickly but cannot be used for accurately deciphering historical population migrations.     

RADIOCARBON DATING ARCHAEOLOGICAL SAMPLES IN THE EASTERN MEDITERRANEAN, 1730 TO 1480 BC: FURTHER EXPLORING THE ATMOSPHERIC RADIOCARBON CALIBRATION RECORD AND THE ARCHAEOLOGICAL IMPLICATIONS*

The East Mediterranean Radiocarbon (Inter‐)Comparison Project (EMRCP) has measured time series of radiocarbon ages for known age samples of German oak (GeO) and for samples from the near‐absolutely placed Gordion juniper dendrochronology from central Anatolia. In this paper, we review the data for the calendar years from 1730 to 1480 bc , relevant in particular to controversy and debate concerning the absolute date of the Minoan eruption of the Santorini (Thera) volcano. We consider the issue of the radiocarbon (¹⁴C) dating of the Santorini eruption, and the problem of how this relates to the archaeological record and historical chronology of Egypt in light of the ¹⁴C data. We find that these ¹⁴C data, and other recent radiocarbon work, provide good grounds to be confident in the possibility of a robust radiocarbon‐based chronology for the eastern Mediterranean. In contrast, as the radiocarbon case becomes stronger, questions must be asked about some archaeological dating: in particular, at the site of Tell el‐Dab‘a in the Nile Delta of Egypt.     

DEEPLY COLOURED AND BLACK GLASS IN THE NORTHERN PROVINCES OF THE ROMAN EMPIRE: DIFFERENCES AND SIMILARITIES IN CHEMICAL COMPOSITION BEFORE AND AFTER ad 150*

In this work we attempt to elucidate the chronological and geographical origin of deeply coloured and black glass dating between 100 bc and ad 300 on the basis of their major and trace element compositions. Samples from the western and eastern parts of the Roman Empire were analysed. Analytical data were obtained by means of a scanning electron microscope – energy‐dispersive system (SEM–EDS, 63 samples analysed) and laser ablation – inductively coupled plasma – mass spectrometry (LA–ICP–MS, 41 samples analysed). Among the glass fragments analysed, dark brown, dark purple and dark green hues could be distinguished. Only among the dark green fragments could a clear compositional distinction be observed between fragments dated to the periods before and after ad 150. In the early samples (first century bc to first century ad ), iron, responsible for the green hue, was introduced by using impure sand containing relatively high amounts of Ti. In contrast, a Ti‐poor source of iron was employed, containing Sb, Co and Pb in trace quantities, in order to obtain the dark green colour in the later glass samples. The analytical results obtained by combining SEM–EDS and LA–ICP–MS are therefore consistent with a differentiation of glassmaking recipes, detectable in glass composition, occurring in the period around ad 150.