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Preview: Archaeometry


Wiley Online Library : Archaeometry

Published: 2018-02-01T00:00:00-05:00


The Life History of an Enslaved African: Multiple Isotope Evidence for Forced Childhood Migration from Africa to the Caribbean and Associated Dietary Change


Archaeological excavations of an enslaved African domestic area at the Spring Bay Flat plantation on the island of Saba, Dutch Caribbean, uncovered a small concentration of artefacts (shell, metal nails, animal bones and five human teeth) overlaid with a lock hinge, interpreted as a lockbox and its contents. Dental anthropological and multi-isotope (strontium, oxygen, carbon and nitrogen) analyses of the teeth revealed that they belonged to a single individual who originated from Africa and survived a period of pronounced nutritional stress as a juvenile. The results provide rare insights into the life history of an individual who probably experienced enslavement, (forced) migration from Africa and adaptation to plantation life in the colonial-era Caribbean.

Neutron Activation Analysis of Late Sixth Century bce Pottery from the Pointe Lequin 1A Shipwreck and Massalia, and Comparison with the Cala Sant Vicenç Shipwreck and Emporion


This paper presents the results of neutron activation analyses of pottery samples from four late sixth century bce sites in the Western Mediterranean: the Pointe Lequin 1A shipwreck, the Bourse site in Marseilles, the Greek colony of Emporion and the Cala Sant Vicenç shipwreck, with the goal of locating the production of a commonly found cup type, the so-called ‘Ionian’ cup, type B2. The NAA results show three distinct compositional groups, although the location of production could not be determined with certainty. The results also show that submarine diagenesis of pottery samples does not necessarily render them incomparable with samples from terrestrial sites.

First Insights into the Technique Used for Heat Treatment of Chert at the Solutrean Site of Laugerie-Haute, France


The earliest evidence of flint and chert heat treatment was found in the ~21.5–17 ka old European Solutrean culture. The appearance of pyrotechnology as part of the production of stone tools has important implications for our understanding of Upper Palaeolithic technological evolution and the specific adaptations during the last glacial maximum in Europe. However, the techniques and procedures used to heat-treat rocks during the Solutrean remain poorly understood. No direct archaeological evidence has so far been found and the most promising approach is to understand these techniques by determining the parameters with which flint and chert were heated at that time. In this study, we investigate the heating temperature of 44 heat-treated laurel-leaf points from Laugerie-Haute, using a non-destructive technique based on infrared spectroscopy. Our results document that most of the artefacts were heated to a narrow interval of temperatures between 250 °C and 300 °C. This indicates a standardized technique that allowed to created similar conditions during successive heating cycles. The implications of these results for our understanding of the technical complexity during the Solutrean must be discussed in the light of different heating techniques used at different places and periods.

Tesserae Recycling in the Production of Medieval Blue Window Glass


The purpose of this paper is to develop a means of quantifying glass recycling and to discuss the ‘anachronistic’ chemical composition of medieval blue window glass. This method relies on a new numerical method using kernel density estimates and is based on a database of published glass chemical compositions. It seeks to reveal when, to what extent and why blue tesserae were recycled for the production of French and English blue glass. First, it is suggested that blue glass had an ‘anachronistic’ chemical composition only before the 13th century. Second, the ‘anachronistic’ chemical composition of 12th-century blue glass comes from the recycling of both blue tesserae and non-coloured glass. Finally, this recycling was motivated by the scarcity of cobalt sources until mines were found in the 13th century.

Determining the Provenance of Cayo Pottery from Grenada, Lesser Antilles, Using Portable X-Ray Fluorescence Spectrometry


Portable XRF was used to analyse the chemical composition of 52 indigenous Cayo ceramics from excavations and from private collections on Grenada, Lesser Antilles. Initially, a comparative baseline of data representing three different islands (Grenada, St Vincent and Trinidad) was created by analysing with pXRF ceramic material that had previously been analysed both chemically and petrographically. The field data, when compared to the laboratory baseline data, indicated that the majority of the ceramics were made with clay local to Grenada. Four samples were potentially made with clay from another, as yet unidentified, source.

Fingerprinting Glues Using HS-SPME GC×GC–HRTOFMS: a New Powerful Method Allows Tracking Glues Back in Time


The use of glues for stone tool hafting is an important innovation in human evolution. Compared to other organic remains, glues are preserved more frequently, though mainly in small spots. Reliable identification requires chemical molecular characterization, which is traditionally performed by gas chromatography  –  mass spectrometry (GC–MS). Current methods of extraction and derivatization prior to GC–MS are destructive and require relatively large samples, which is problematic for prehistoric glue residues. In this paper, we discuss the results of an experimental study using a new method (HS-SPME GC×GC–HRTOFMS) that proves effective for identifying small quantities of compound glues. The method is non-destructive with an improved sensitivity in comparison to traditional GC–MS, and it has a high potential for prehistoric samples.

Lead Isotope Analysis of Tooth Enamel from a Viking Age Mass Grave in Southern Britain and the Constraints it Places on the Origin of the Individuals


Lead analysis of tooth enamel from individuals recovered from a Viking Age burial pit in southern England provides further evidence for their childhood origins outside Britain. All except one of the men have very low Pb concentrations that exclude anthropogenic Pb exposure. Strontium and oxygen isotope compositions identify a core group of men who have Pb isotope compositions of 208Pb/206Pb = 2.065 ± 0.021 (n = 20, 2SD) that, when compared with data from European soils, appear to exclude a childhood in the Scandinavian countries of Norway, Sweden and Finland, whereas areas of Northern continental Europe cannot be excluded.

New applications of LA–ICP–MS for sourcing archaeological ceramics: microanalysis of inclusions as fingerprints of their origin


This paper presents the latest methodological advances using the LA-ICP–MS technique for differentiating the origin of petrographically and chemically similar ceramic raw materials. Based on several examples form the Armorican Massif (France), from a chronological period extending from the Neolithic to the Second Iron Age, we will show that the comparison of the chemical signatures of minerals included in fired clay with those from clay and source rocks enables us to distinguish productions and to accurately trace the sources of the raw materials used by potters.

Portuguese Blue-on-Blue 16th–17th Century Pottery


Blue-on-blue (‘berettino’) sherds have appeared in numerous production and consumption archaeological excavations in Lisbon and other archaeological sites in Portugal (dated from the mid-16th century to the beginning of the 17th century). The abundance of this interesting faience led us to compare it with similar pottery from other well-known production centres in Italy, namely Liguria (Savona and Albisola), Spain (the Triana kilns) and the Low Countries. Differences in the diffraction patterns of the sherds' pastes from the four countries were observed. In most samples, cobalt blue silicate (cobalt olivine) was identified in the dark blue or light blue glazes through the use of micro-Raman spectroscopy and diffuse reflectance spectra. A remarkable difference in the calcite contents of the Lisbon and Seville pottery sherds was observed, in accordance with previous observations of high calcite contents of Seville ceramics. A comparison was also made for all of the blue-on-blue sherds studied here with many other 16th–17th century sherds from Lisbon using bivariate plots of K/Si versus Ca/Si. Lisbon and Seville pottery behave very differently, whereas sherds from Italy and the Low Countries occupy intermediate positions.

Stable Isotope Sourcing of Wool from Textiles at Pacatnamú


Stable carbon and nitrogen isotopic compositions were determined for wool textiles from the Lambayeque (c. ad 1100–1320) occupation at Pacatnamú in the Jequetepeque Valley, northern Peru. The isotopic data demonstrate that the wool was not obtained via long-distance exchange with the highlands and was most probably derived from locally raised camelids. In light of other lines of evidence (diversity of dyes used to produce the same colours in textiles and the low quality of the weaving), textiles at Pacatnamú appear not to have been as effective a marker of political power and prestige for local elites as they were elsewhere in the Andean region.

Ophiolites Associated with Pottery Production in Bronze Age Crete


This study investigates diversity among ophiolite-bearing sediments that were exploited for pottery production in Bronze Age Crete (c.3000–1200 bc). The focus is on loose and consolidated formations of Upper Tertiary to Quaternary ages that contain some detrital products of Mesozoic ophiolitic source rocks. A literature review, geological fieldwork, sediment sampling and petrographic analysis are combined to identify the origin, the geographical distribution and the stratigraphic position of these ophiolitic sediments, and to assess regional diversity in their mineralogy and texture. The results provide insights into current archaeological problems regarding the provenance and production of ophiolite-bearing pottery in Bronze Age Crete.

A Roman Egyptian Painting Workshop: Technical Investigation of the Portraits from Tebtunis, Egypt


Roman-period mummy portraits are considered to be ancient antecedents of modern portraiture. However, the techniques and materials used in their manufacture are not thoroughly understood. Analytical study of the pigments as well as the binding materials helps to address questions on what aspects of the painting practices originate from Pharaonic and/or Graeco-Roman traditions, and can aid in determining the provenance of the raw materials from potential locations across the ancient Mediterranean and European worlds. Here, one of the largest assemblages of mummy portraits to remain intact since their excavation from the site of Tebtunis in Egypt was examined using multiple analytical techniques to address how they were made. The archaeological evidence suggests that these portraits were products of a single workshop and, correspondingly, they are found to be made using similar techniques and materials: wax-based and lead white–rich paint combined with a variety of iron-based pigments (including hematite, goethite and jarosite), as well as Egyptian blue, minium, indigo and madder lake to create subtle variations and tones.

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.

Characterization of Materials and Artistic Techniques on Two 17th-Century Neapolitan Wood Sculptures


Two sculptures of Gaetano Patalano, one of the most important Italian sculptors of the late 17th century, were analysed to study the stratigraphy, the organic and inorganic materials, and to distinguish the original layers from the repaintings. Samples taken from the Immacolata Concezione and from San Gaetano da Thiene (Santa Chiara church, Lecce, Italy) were studied by optical microscopy, μ-Raman spectroscopy and Py-GC–MS. Different binders and pigments were used for the preparatory layers on the different parts of the statues: the results demonstrate that Patalano mastered the various materials and techniques, and that his choices have allowed his carving ability to be emphasized.

Improvements in Archaeomagnetic Dating in Western Europe from the Late Bronze to the Late Iron Ages: An Alternative to the Problem of the Hallstattian Radiocarbon Plateau


We present a new curve of the directional secular variation of the geomagnetic field in Western Europe between 1500 bce and 200 ce. Its computation relies on a Bayesian framework. The fast secular variation during the Late Bronze and Early Iron Ages makes archaeomagnetic dating efficient with a respective precision of 150–200 and 60–100 years during these periods. The Bayesian method also provides posterior date distributions that refine the dating of reference data, especially during the period of the Hallstattian radiocarbon plateau. Archaeomagnetism becomes a valuable alternative to radiocarbon and will help to improve the archaeological chronologies.

Testing Area-Scale Fractal Complexity (Asfc) and Laser Scanning Confocal Microscopy (LSCM) to Document and Discriminate Microwear on Experimental Quartzite Scrapers


Few microwear studies have been conducted on tools made from quartzite. Most rely on visual observation of microwear features using optical light microscopes and scanning electron microscopes. Quantification of microwear on quartzite tools is extremely rare, even though numerous methods to mathematically document surface roughness have been applied to other silicate tools. In this paper, laser scanning confocal microscopy (LSCM) was used to document surface roughness on four experimental scrapers made from two different subtypes of Mistassini quartzite that were used on either fresh or dry deer hide. Surface roughness data were analysed using area-scale fractal complexity (Asfc). The results of this test case indicate that Asfc can effectively discriminate between the unused and used regions on the quartzite tools based on surface roughness, and that it can also discriminate between surface roughness produced by working dry versus fresh hides. Differences in the subtypes of Mistassini quartzite did affect surface roughness, but not significantly enough to prevent discrimination of the dry and fresh hide-working tools. Although the use of the Asfc parameter for lithic microwear analysis requires further testing, these first results suggest it could be a reliable technique to mathematically document and discriminate wear patterns on archaeological quartzite tools.

The Analysis of Late Bronze Age Glass from Nuzi and the Question of the Origin of Glass-Making


This paper re-analyses a considerable corpus of glass from the Late Bronze Age site of Nuzi, found near Kirkuk in Iraq. SEM–WDS and Sr and Nd isotopic analysis were applied, in addition to cataloguing the glass. The work showed that the glass technology at Nuzi was subtly different from contemporary Egyptian sites, using different ways of opacifying and working glass. At least two, perhaps three, Near Eastern production sites are postulated. The range of glass colours and the skill of their application at Nuzi was perhaps not on a par with the Egyptian sites. This led to a reconsideration and review of the accepted wisdom that the Near East is the source of the innovation that is glass-making. This opinion is based on limited textual and iconographic sources and is dominated by an erroneous early date for a very developed Nuzi glass industry along with a few finds of glass vessels in early contexts. Some of this evidence has now been at least questioned, suggesting that glass-making in Egypt, at least as early as the middle of the 15th century bc, and probably earlier, is no later than that in the Near East. It is argued that it is far from clear that the Near East was the source of the innovation and that a more cautious approach would better fit the evidence.

A Study of Biodeterioration and Chromatic Alterations of Painted and Gilded Mummy Cartonnage at the Saqqara Museum Storeroom, Egypt


Microbial biofilms have developed on the surfaces and within the painted and gilded layers of mummy cartonnage at the Saqqara museum storeroom in Giza, Egypt. SEM–EDX, XRD and FT–IR–ATR techniques were applied to analyse the coloured and gilded materials, ground layer, textile support and binder used for the cartonnage. Aspergillus niger (24.8%), Penicillium chrysogenum (21.5%) and a novel cartonnage-biodegrading bacterium, Bacillus sonorensis (23.7%), were the most abundant microbes growing over the cartonnage surface. In addition, Aspergillus tamari (15.4%), A. fumigates (8.1%) and Fusarium solani (6.5%) were identified. The pigments comprised Egyptian blue (cuprorivaite), cinnabar (red), orpiment (yellow) and green pigment made from a mixture of cuprorivaite and orpiment. Gold leaf was used for the gilded layer, calcium carbonate and gypsum comprised the ground layer, gum arabic was the binding medium and the fibre base was a fine linen textile. Microbial colonization tests were performed on aged cartonnage replica samples made from linen and pigments of similar composition to ancient pigments found in the cartonnage. Each sample was inoculated separately with A. niger, P. chrysogenum and B. sonorensis. Yellow orpiment samples were the exception, as no colour change was detected after colonization by the examined micro-organisms.

Geochemical Variability in the Paredón Obsidian Source, Puebla and Hidalgo, Mexico: A Preliminary Assessment and Inter-Laboratory Comparison


Chemical characterization reveals intra-source variation in obsidian from the Paredón source area in Puebla and Hidalgo, Mexico. Two chemical sub-sources of obsidian from Paredón are spatially discrete and cannot be distinguished by visual characteristics. To facilitate future investigations of the prehistoric exploitation of these sub-sources, an inter-laboratory comparison of elemental concentrations is presented based on neutron activation analysis and several XRF instruments.

Breaking Traditions: An Isotopic Study on the Changing Funerary Practices in the Dutch Iron Age (800–12 bc)


Urnfields in the Dutch river area were replaced by cemeteries with a mixture of cremation and inhumation graves around the sixth century bc. This study provides the first biogeochemical evidence that the Iron Age communities were heterogeneous in terms of geological origins. The high percentage of non-locally born individuals (~48%) supports the hypothesis that the change in burial practice was the result of the influx of foreign people, who were being allowed to keep their own burial customs, whereas some of the local inhabitants adapted the burial rites of foreign cultures, leading to a heterogeneous burial rite for some centuries.

A Comparison Study of Middle Bronze Age II Daggers and Their Rivets as a Tool for a Better Understanding of Their Production


The Middle Bronze Age II is a period during which there exists a contemporaneous usage of arsenic copper and tin bronze for metal weaponry production. In order to learn more about the alloys used in this period, the blades and rivets from 65 daggers of two significantly different types, which were discovered at the Rishon LeZion (RL) cemetery, Israel, were tested by the non-destructive method of X-ray fluorescence (XRF). The results reveal new knowledge of the alloys selected for dagger and rivet production, both of which represent fine examples of the Middle Bronze Age II Southern Levant in metal industry.

Prehistoric Settlement, Mobility and Societal Structure in the Peak District National Park: New Evidence from Ceramic Compositional Analysis


Detailed compositional and technological analysis of a large assemblage of prehistoric ceramics from numerous sites situated within the Peak District National Park has been used to explore the settlement patterns, societal structure, mobility and interaction of the populations that inhabited this area during the Early Bronze Age to Early Iron Age. A surprising pattern emerges of the widespread dominance of a single, geographically restricted temper type, which appears to have been transported and mixed with locally procured clay and used to produce pottery at numerous different sites. The distribution of this and several other compositional groups are defined via thin-section petrography and compared to raw material field samples. The resulting patterns are used to assess the validity of previous theories about prehistoric life in this region during the third to first millennia bc.

Flint and Quartzite: Distinguishing Raw Material Through Bone Cut Marks


Since the 1980s, several experimental analyses have been able to differentiate some lithic tool types and some of their raw materials according to the morphology of cut marks imprinted by such tools when used for butchering activities. Thus, metal tool use has been differentiated in contexts with an abundance of lithic tools, or even the use of hand axes has been documented in carcass processing, in contrast with simple unretouched or retouched flakes. As important as this information is, there are still other important aspects to be analysed. Can cut marks produced with different lithic raw material types be differentiated? Can cut marks made with different types of the same raw material type be characterized and differentiated? The objective of this study is to evaluate if cut marks resulting from the use of different flints and different quartzites are distinguishable from each other. In the present work, an experimental analysis of hundreds of cut marks produced by five types of flint and five varieties of quartzite was carried out. Microphotogrammetry and geometric–morphometric techniques were applied to analyse these cut marks. The results show that flint cut marks and quartzite cut marks can be characterized at the assemblage level. Different types of flint produced cut marks that were not significantly different from each other. Cut marks made with Olduvai Gorge quartzite were significantly different from those produced with a set comprising several other types of quartzites. Crystal size, which is larger in Olduvai Gorge quartzites (0.5 mm) than Spanish quartzites (177–250 μm), is discussed as being the main reason for these statistically significant differences. This documented intra-sample and inter-sample variance does not hinder the resolution of the approach to differentiate between these two generic raw material types and opens the door for the application of this method in archaeological contexts.

Quantifying 3D Micro-Surface Changes on Experimental Stones Used to Break Bones and Their Implications for the Analysis of Early Stone Age Pounding Tools


We present a new method to assess use-wear formation processes of pounding tools used to break bones based on a combination of conventional microscopy, optical 3D surface measurements obtained with a confocal microscope and GIS analysis. The method involves 3D alignment and 3D surface change inspection techniques along with a surface morphometric characterization and 2D spatial pattern analysis, to measure the spatital distribution of significant changes in surface topography of pounding tools. Our results show that microscopic changes can be detected in the surfaces of hammers and anvils after bone breakage activities are performed. Use-wear on the active elements (hammers made on basalt and quartzite) occurred over a larger area than was observed on the passive element (quartzite anvil), but the latter often exhibited deeper modifications. Tool surfaces generally developed smoother topography with increased use, but grain microfracture also appeared with greater frequency over time. This methodology offers highly accurate and statistically robust analyses of microscopic use-wear traces that can be applied to the analysis of archaeological pounding tools.

Lisht as a New Kingdom Glass-Making Site with Its Own Chemical Signature


Lisht is one of a few New Kingdom sites with known glass-working debris. Here, we present evidence for the primary production of glass at Lisht, including crucible fragments and semi-finished glass. We also provide 12 new chemical analyses of glass from Lisht, including trace elements. We argue that the glass made at Lisht has a specific chemical signature within the broader range of Late Bronze Age glass compositions from Egypt, further underlining the former existence of primary glass production there and offering the possibility of identifying Lisht-made glass elsewhere in Egypt and beyond.

Archaeomagnetic Dating of Pyrotechnological Contexts: a Case Study for Copper Smelting Sites in the Central Timna Valley, Israel


This study is focused on establishing age constraints for several copper slag deposits at the centre of the Timna Valley (Israel) via reconstruction of their ancient geomagnetic intensities as recorded by the individual slag samples at the time of their formation. The results show a correlation between the location of the slag deposits (labelled as individual ‘mounds’ in our survey) and their inferred ages, reflecting varying socio-economic and political dynamics in the region. While the slag mounds found at the unprotected foothills represent a variety of dates (mostly Early Islamic), the slag mounds on the hilltops are chronologically constrained to the early Iron Age (late 11th to 10th centuries bce), supporting the idea for a need for protection during this period. Furthermore, in comparing the new data with previous archaeomagnetic studies from Timna, we can assert the existence of simultaneous copper production at the archaeological Sites 30, 30a and 34. This gives further support to the claim of intense smelting in the central Timna Valley during the early Iron Age. Finally, this project demonstrates the potential of archaeomagnetic experiments to provide chronological insights, and their particular advantage in addressing pyrotechnology-related cases.

High-boron and High-alumina Middle Byzantine (10th–12th Century ce) Glass Bracelets: A Western Anatolian Glass Industry


The trace element boron is present in most ancient glasses as an impurity, and high boron (≥ 300 ppm) marks raw material sources that are geologically specific and relatively uncommon. Recent analyses of Byzantine glass with high boron contents suggest that glass-making was not limited to the traditional regions of the Levant and Egypt, and a production origin in or near western Anatolia is proposed. Glass bracelets from Ḥiṣn al-Tīnāt in southern Turkey give fresh evidence for the production and circulation of high-boron glasses that closely correlates with object typology. The patterning of findspots suggests that high-boron glass was closely connected to the Byzantine world.

The Social and Economic Complexity of Ancient Jerusalem as Seen Through Choices in Lighting Oils


This paper presents and discusses the results of residue analysis conducted on 78 ceramic lamps found in archaeological excavations in ancient Jerusalem, in an attempt to identify the types of oils used and the reasons for their preferential choice. The oil lamps chosen for the study were taken from a variety of contexts, which represent the different periods during which Jerusalem was settled and the different sectors of the city. The results of the study show that even the most mundane activity of lighting using oil held within it social and economic choices, as mirrored in the different excavation areas.

The Potential of EBSD and EDS for Ceramics Investigations—Case Studies on Sherds of Pre-Columbian Pottery


The work focuses on the potential of structural and chemical examinations by scanning electron microscopy based methods for archaeometric studies on ceramics. Achieved by a single preparation technique (polished block sections), the feasibility and benefits of electron backscatter diffraction are demonstrated as case studies using polychrome examples of pre-Columbian pottery (Wari, Moche and Cajamarca). Elemental and phase maps allow for separate consideration of clay and temper. Identification of mineral phases and intergrowths of temper particles provide information for clarifying clay procurement and firing techniques with respect to local versus non-local pottery to enlighten trade relations, technological transfer and shared heritage of pre-Columbian cultures.

Tracing the Distribution of Late 16th and Early 17th Century European Copper Artefacts in Southern Québec and Ontario, Canada


To understand the nature of trade/exchange of ‘Basque’ copper kettles and their fragments among Indigenous communities from Québec to Ontario, Canada, we examined 948 copper samples from 75 archaeological sites. We found that 936 samples were sortable into 11 coarse chemical groups: seven biased towards Ontario, three favouring Québec and only one balanced between the two provinces. This pattern may represent kettles and pieces ‘mostly traded’ or ‘mostly kept’ by Indigenous groups within Québec. Chemical group distribution within individual provinces is complex. A tentative chronology of copper chemical groups provides additional insight into the complex trading/exchange patterns among the Indigenous groups of southern Ontario.

The So-called Venetian Enamelled Copper Artworks of the Italian Renaissance: the Technology and Provenance of the Enamels—an Analytical Approach


The so-called Venetian enamelled coppers are a group of objects produced in Italy during the 15th century. Up to now, about 300 objects have been recognized in private collections and in European and US museums. At the end of 19th century, a Venetian origin was suggested, but their provenance is still debated. In this study, the enamel compositions from 22 enamelled copper products from Italian and French collections have been analysed by invasive and non-invasive techniques. A comparison of the results with Tuscan and Venetian glass databases reinforces the suggestion of a Tuscan (most probably Florentine) origin for these works of art.

Characterizing the Alabastro listato or fiorito of Hierapolis in Phrygia: A Simple Method to Identify its Provenance using Carbon Stable Isotopes


Alabastro listato or fiorito of Hierapolis in Phrygia was a prestigious coloured marble widely used in Roman architecture and decoration. This stone is generally identified in artefacts on autoptic examination, but it may sometimes be confused with alabasters of different provenances. This study describes a simple, but effective, scientific method to contribute to the determination of Hierapolis alabaster. Due to its unique genetic context, it is characterized by a distinctive carbon isotope signature. A comparison between the stable carbon isotope data from this paper and from the literature confirms the uniqueness of the isotopic character of Hierapolis alabaster. Carbon isotopes can ensure a reliably provenance attribution of the alabaster artefacts along with visual recognition by an expert eye.

Determination of the Fineness of Medieval Coins—Evaluation of Methods in a Case Study of a Medieval Pfennig


The original fineness of coins is very important information that can help us to understand the commercial situation in a wide historical context. This paper deals with a comparison of analytical methods suitable for the evaluation of the actual and original fineness of coins based on a detailed case study of a medieval coin sample. Both non-destructive (i.e., scanning electron microscopy/energy-dispersive X-ray spectroscopy, X-ray fluorescence, atomic force microscopy and hydrostatic weighing) and destructive (i.e., inductively coupled plasma – mass spectrometry and the Volhard titration method) techniques were used. The original fineness can be also deduced from knowledge of the internal structure of the coin (limited miscibility of copper and silver). A new analytical method based on a combination of a micrograph of the metallographic cross-section with consequent image analysis was developed for determination of the original fineness. The proposed approach is relatively simple and provides reliable values. Sample heterogeneity and its impact on the determination of fineness are also discussed.

Towards a Chronology of the Jerzmanowician—a New Series of Radiocarbon Dates from Nietoperzowa Cave (Poland)


The period around 50 000–35 000 years ago constitutes one of the most debated research issues in European archaeology of the Palaeolithic. In this time period, the transition from the Middle to the Upper Palaeolithic took place. Locally, in different areas of Europe, this shift is recorded in so-called transitional assemblages. The eastern fringe of these transitional assemblages is represented by the Jerzmanowician, the unit described on the basis of a lithic assemblage from Nietoperzowa Cave (Poland). The unit is a part of a European transitional complex called the Lincombian–Ranisian–Jerzmanowician. Up to now, the radiocarbon dates presented in the literature have only allowed us to set the age of the Jerzmanowician at c.40 000–45 000 ka cal bp. In this study, we present 42 new radiocarbon dates. We attempt to set the archaeological record of the Jerzmanowician from Nietoperzowa Cave in an accurate chronological framework, based on Bayesian statistical processing of radiocarbon dates. We conclude that the lower boundary of layer 6 in Nietoperzowa Cave can be statistically located in the range 44 000–42 000 cal bp and the upper limit for the Jerzmanowician is estimated to c.31 000 cal bp. New data raises a question on the correlation with upper layer 4. In the light of the new chronology, the attribution of the archaeological inventory from layer 4 to the Jerzmanowician seems questionable.

‘Guard the Good Deposit’: Technology, Provenance and Dating of Bipyramidal Iron Semi-Products of the Durrenentzen Deposit (Haut-Rhin, France)


In the early days of iron metallurgy in Western Europe, the most widespread type of ‘trade iron’ (semi-product) was bipyramidal in shape. Although they are frequently found, little is known about how they were manufactured and circulated, or even about their age. An interdisciplinary approach was applied to the Durrenentzen deposit (Haut-Rhin, France), the third-largest in Europe in terms of artefact quantities, in an attempt to reconstruct the technological, social and economic context that caused them to be abandoned. A morphometric study of the 51 iron bars revealed a high degree of homogeneity, despite variations in detail. Four objects were selected for archaeometric studies. Metallographic analyses show internal differences (quality of the material, nature of the alloys and manufacturing techniques). Chemical analyses also showed different provenances. Finally, radiocarbon analyses of the carbon in steel (iron/carbon alloy) linked this deposit to the early Iron Age. This study provided the first benchmark for more general research, significantly changing perceptions of the economics of iron at the beginning of the Iron Age.

Early Imports in the Late Bronze Age of South-Western Iberia: The Bronze Ornaments of the Hypogea at Monte da Ramada 1 (Southern Portugal)


The composition and manufacture of Late Bronze Age metallic artefacts from funerary and domestic contexts of southern inland Portugal was studied. The prevailing trend comprises binary bronzes (10.3 ± 2.1 wt% Sn) showing deformed equiaxial grains, annealing twins and slip bands. The alloy composition is somewhat independent of artefact type, while the manufacture seems to rely on artefact function and the skilfulness of the metallurgist. The technological characteristics were linked with archaeological and chronological features, disclosing some artefacts of uncommon composition, such as low-tin bronze bracelets (4.3–7.1 wt% Sn) associated with ornaments of exotic materials (glass and Egyptian faience beads, and also ostrich egg shell beads). The assemblage testifies to an archaic trade with the Mediterranean region before the establishment of the first Phoenician colonies on the southern Iberian coast.

The Evolution of the Vitruvian Recipes over 500 Years of Floor-Making Techniques: The Case Studies of the Domus delle Bestie Ferite and the Domus di Tito Macro (Aquileia, Italy)


The paper reports the results of a research project aimed at the characterization of the floor bedding mortars of two Roman houses in Aquileia (north-eastern Italy), the Domus delle Bestie Ferite and the Domus di Tito Macro. Seventy floor bedding mortars of the two domus were selected and almost half were fully minero-petrographically characterized by means of optical microscopy operated in transmitted light (OM-TL), X-ray powder diffraction analyses coupled with quantitative phase analysis by means of the Rietveld method (XRPD-QPA) and scanning electron microscopy with EDS microanalysis (SEM–EDS). The results indicate an evolution of the mortar preparation techniques over time in the mosaic of both houses. The materials are compared to the traditional Roman recipes for specific construction techniques.

The Contribution of Transmission Electron Microscopy (TEM) to Understanding Pre-Columbian Goldwork Technology


This paper highlights the contribution of transmission electron microscopy (TEM) when combined with scanning electron microscopy and energy-dispersive X-ray microanalysis (SEM/XEDS) to characterize objects in archaeology. The application of TEM in archaeology is not yet a common tool, but it may provide data that are significant to understanding pre-Columbian gold metallurgy, specifically the gilding and silvering methods. Two gilded rods were studied using a combination of TEM and SEM/XEDS techniques. The objects were found at the Atacames archaeological site, in the Esmeraldas region, Ecuador, which was occupied between ad 750 and 1526 by the Atacames culture. The microchemical and structural results of the inner and the external gilded part of the artefacts support the hypothesis of a gold diffusion to the surface enhanced by chemical treatment with chloride-rich solutions, heating and successive annealing processes. The present study reveals that microstructural investigation by TEM provides useful information with which to investigate the techniques used to modify the chemical surface composition of pre-Columbian artefacts.

Electrochemical Characterization and Dating of Archaeological Leaded Bronze Objects Using the Voltammetry of Immobilized Particles


The application of solid state electrochemistry techniques for the characterization and dating of leaded bronze objects is described. Characteristic voltammetric signatures of copper and lead corrosion products were used as markers of more or less prolonged corrosion periods. The proposed methodology was applied to samples from the Roman archaeological sites of Valeria (Spain) and Gadara (Jordan), Roman and medieval sites in Xàtiva (Spain), and modern statuary exhibited outdoors, on the campus of the Universitat Politècnica of Valencia, Spain, covering a time interval between the fourth to second century bc and the 20th century ad. For such samples, the ratio between the signals for copper and lead corrosion products decreased monotonically with the corrosion time. This variation was modelled on the basis of thermochemical and kinetic considerations, the experimental data being consistent with a potential rate law for the corrosion process.

Stable Isotope and Radiocarbon Dating of the Remains of the Medieval Royal House of Aragon (Spain) Shed Light on Their Diets, Life Histories and Identities


The remains of 20 individuals buried in three different pantheons, putatively pertaining to the medieval Royal House of Aragon, were analysed for their isotope (14C, 13C and 15N) measurements. The radiocarbon dates and stable isotope data contributed to identifying individual members and, combined with additional osteological and taphonomic information, as well as documentary evidence, provided a fuller picture of the diets and life histories of particular people. This group comprised the first members of a royal dynasty that ruled the Kingdom of Aragon before the Spanish Crown was established, and that played a significant role in the reconquest of the Iberian Peninsula from Muslim control, this being of paramount importance in the Spanish and European history.

On the Metal-Leaf Decorations of Post-Byzantine Greek Icons


Metal leaves were widely used as decorative materials in post-Byzantine ritual painting. Fifty-two icons (mid-15th to mid-19th centuries) were studied by means of analytical techniques in order to reveal the materials and techniques encountered in their metal-leaf decorations. High-purity gold leaf was used throughout the studied period. Silver was employed rarely and mostly during the latter part of the period in consideration, while metal powders were mostly used from the mid-18th century onwards. The identification of a gold–silver powder mixture and an ‘electrum’-type alloy are among the reported findings, which are novel for post-Byzantine icons. Three micromorphologically distinct highlighting techniques were also documented.

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Multi-analytical Studies of Archaeological Chinese Earthen Plasters: The Inner Wall of the Longhu Hall (Yuzhen Palace, Ancient Building Complex, Wudang Mountains, China)


The Yuzhen Palace is one of the nine palaces in the Ancient Building Complex built by order of the Yongle Emperor during the Ming dynasty. The buildings were built with dressed black bricks. As a result of the planned national South–North Water Diversion project, the water level in the Danjiangkou Reservoir that surrounds the Yuzhen Palace was expected to rise by approximately 15 m. To avoid submersion of the site, three gates were elevated by 15 m in 2013 and other buildings dismantled, for later reconstruction. The characterization of the construction materials has therefore become of primary importance. Here, we present results on the plasters of the Longhu Hall. The analysis of materials involved a multi-analytical approach combining optical and electron microscopy with X-ray and vibrational spectromicroscopies and thermogravimetry. The results indicated the use of two earthen plaster layers and a whitewash finish coating applied over a thin preparatory intermediate layer to improve the adherence of the finish coating to the earthen plaster. Ramie and straw fibres identified in the earthen plasters were added to reduce shrinkage and cracking during drying. The raw materials used and the application technique pointed to a well-established construction industry using traditional earthen building materials together with lime technology.

The Chemical Composition and Production Area of Early Western Zhou Proto-Porcelain Unearthed from Yejiashan Cemetery, Suizhou, China


The bodies and glazes of 27 early Western Zhou proto-porcelain samples from Yejiashan cemetery, Hubei Province, were analysed using LA-ICP–AES, SEM, XRD, a thermal expansion instrument and other analytical methods. The results indicated that the bodies of all samples were characterized by high silicon and low aluminium, and were made with porcelain stone raw materials found in the south of China. The glazes are typical of high-temperature calcium glazes of the CaO (MgO) – K2O (Na2O) – Al2O3 – SiO2 series, with relatively high Mn and P content, which was probably caused by the addition of plant ashes. The physical properties and phase compositions of Yejiashan proto-porcelain show that firing processes were still in the early stages of development in ancient China. Multivariate statistical analyses indicated that Yejiashan proto-porcelain might have come from the Deqing area, in Zhejiang Province. These results provide new archaeological evidence for research on issues related to material flow in the Western Zhou dynasty.

A Study on the Elemental Composition of Chinese Mise Type Wares from Different Periods and Kilns


A large number of porcelain shards were unearthed at the Hehuaxin and Silongkou kilns around the Shanglin Lake, Ningbo, China, some of which had clear stratification to enable the determination of the date of firing. With the purpose of studying the elemental composition in different cultural periods and between kilns, the chemical compositions of 43 typical shards from these two kilns were determined by energy-dispersive X-ray fluorescence (EDXRF). The results show that the mean contents of K2O, CaO and MnO in the glaze fluctuate in different cultural periods at the Hehuaxin kiln, but not systematically. Principal component analysis (PCA) indicates that samples from the Five Dynasties and the Northern Song dynasty are similar to each other. This shows continuity in the raw materials and firing technology between the two dynasties. Comparing the mise type wares from the Hehuaxin and Silongkou kilns in the Northern Song dynasty, we found that MnO and ZrO2 in the glaze can be used as fingerprinting elements to distinguish between samples from these two sites. In spite of this, their chemical compositions are broadly similar. Thus, perhaps, their chemical compositions can be taken as typical for those of the mise type wares produced around the Shanglin Lake.

Study on the Material and Manufacturing Technology of Different Types of Longquan Ware Imitations from Dapu Kiln of Guangdong Province in the Ming Dynasty of China (ad 1368–1644)


Research on ancient Longquan wares and their imitations has attracted considerable attention. Using a series of experimental methods, including micro X-ray fluorescence spectroscopy (μ-XRF), X-ray diffractometry (XRD), optical microscopy (OM), polarizing microscopy (PLM), dilatometry (DIL) and spectrophotometery, different samples of Longquan imitations from Dapu in Guangdong Province were collected and analysed. The study of different types of celadon from the Dapu kiln factories shows that the pale yellow body had a higher TFe2O3 content, and the body material must therefore have been treated differently or have come from a different source. The SiO2 and Al2O3 contents in the body can be used as auxiliary parameters to identify Longquan wares and its imitations. The study also found that both kinds of glaze recipe—including calcium–alkali glaze and alkali–calcium glaze—existed in the Dapu products, which suggested that while imitating Longquan ware, the potters in Dapu also showed innovation in the recipe for the glaze material. Moreover, there were some differences in the TFe2O3 content, as well as the size, number and distribution of bubbles in the different types of glaze. Finally, the study revealed that the material of both the saggars and separators were composed of another porcelain clay, different from that of the celadon body. In addition, the white and compact body of the celadon had a higher firing temperature, of 1140–1187 °C, compared with other types of wares, which had a lower firing temperature of 1050–1080 °C.

A Study on Black-Body Celadon Excavated in The Altar Guan and Literature Ge (Longquan Ge) Kilns by EDXRF


Samples of celadon were collected from the Altar Guan Kiln in Hangzhou, and from the Xiaomeizhen and Xikou Kilns, two subordinate kilns of the Longquan Kiln producing black-body celadon called Literature Ge. Both the elemental contents in the sample bodies and the glaze were measured. The results reveal that the sample bodies contain fingerprint information for provenance, while this was lost in the glaze during the production process. The TiO2, MnO and Rb2O contained in the bodies are fingerprints to distinguish between celadons from the Xiaomeizhen and Xikou Kilns. In the Altar Guan Kiln, some low-TiO2 samples were found and their body colour is much lighter than some others, but they do not differ with regard to iron content. This indicates that both titanium and iron are indispensable for the blackness of the bodies: they may react to form some black minerals during the firing process. Ultimately, samples from the Literature Ge and Altar Guan Kilns differ in their body constituents. Principal component analysis reveals that the samples can be divided into two groups, corresponding to the two different areas.

A Comparative Study of the Early High-Fired Ceramic Shards from Dongtiaoxi, Zhejiang (China)


There is a generally accepted view that there is an obvious distinction between proto-porcelain and stamped stoneware. However, some early shards unearthed from the Dongtiaoxi region (northern Zhejiang) inspire people to rediscuss the relationship between them, because it is difficult to identify them as proto-porcelain or stamped stoneware. In this work, we have collected samples from three of the earliest kiln sites (Piaoshan, Beijiashan and Nanshan) in the Dongtiaoxi region. We have analysed the chemical composition, firing temperature and phase composition of the samples. Comparing samples from the three kiln sites, we find that, from Piaoshan and Beijiashan to Nanshan, there has been progression in the manufacturing technology. The Shang proto-porcelain and the stamped stoneware from Nanshan have similar raw materials, firing temperatures and body phase compositions—and they have obviously different decorative appearances, such as glazing or stamping. For ceramics from Piaoshan and Beijiashan, there is no clear distinction between glazed and unglazed samples. We believe that in the Dongtiaoxi region, the difference in the decoration between proto-porcelain and stoneware became obvious up to the time of the Nanshan production but that, subsequently, two different paths for the development of high-fired ceramics began to diverge.

The Archaeometry and Archaeology of Ancient Chinese Glass: a Review


This paper provides a new review of archaeometric research carried out on glass found in China, set in an archaeological context, from its earliest occurrence to the Song dynasty. It is set within a broad geographical context taking the terrestrial and maritime Silk Road contacts into account. We discuss chemical and isotopic compositional contrasts in glasses from different periods found in different parts of China, the glasses that were almost certainly made in China and those that were imported. A theme that runs through the paper is the problem of provenancing glass found in China, along with a lack of evidence for primary glass-making sites and minimal evidence for secondary glass production. We discuss the glass artefacts that are of typical Chinese types and contrast these with imports; the structure reflects this contrast. We discuss potential new scientific and archaeological approaches to Chinese glass.

Did China Import Metals from Africa in the Bronze Age?


The origins of the copper, tin and lead for China's rich Bronze Age cultures are a major topic in archaeological research, with significant contributions being made by archaeological fieldwork, archaeometallurgical investigations and geochemical considerations. Here, we investigate a recent claim that the greater part of the Shang-period metalwork was made using metals from Africa, imported together with the necessary know-how to produce tin bronze. A brief review of the current status of lead isotopic study on Shang-period bronze artefacts is provided first, clarifying a few key issues involved in this discussion. It is then shown that there is no archaeological or isotopic basis for bulk metal transfer between Africa and China during the Shang period, and that the copper and lead in Shang bronze with a strongly radiogenic signature is not likely to be from Africa. We call for collaborative interdisciplinary research to address the vexing question of the Shang period's metal sources, focusing on smelting sites in geologically defined potential source regions and casting workshops identified at a number of Shang settlements.

Some Recently Rediscovered Analyses of Chinese Bronzes from Oxford


We report here the rediscovery of the chemical analyses of approximately 540 Chinese bronze objects, carried out in RLAHA in the late 1950s by optical emission spectrometry. Although largely of historical interest, they do in fact even now approximately double the number analyses of Chinese bronze objects that contain data on both major and minor elements. In fact, the other major equivalent data sets, from the Freer Gallery and the Sackler Collection, are of approximately the same vintage. We attempt to evaluate the quality of the data, and address a controversy that appeared in the literature during the 1960s and 1970s about the value of arsenic measurements in Chinese bronzes as an indicator of authenticity.

Application of Kernel Density Estimates to Lead Isotope Compositions of Bronzes from Ningxia, North-West China


The aim of this paper is to apply kernel density estimates (KDEs) to the visualization and interpretation of lead isotope data from bronze assemblages found along the northern border of central China, here designated as the Arc. New lead isotope analyses of 30 leaded tin–bronze artefacts from the Wangdahu cemetery (c.500–300 bc) in the Ningxia Hui Autonomous Region, north-west China, provide the basis for the discussion. By using multivariate KDEs and the calculated likelihood of the overlap, the present work shows that the Wangdahu objects feature a unique linear array of isotope ratios, representing an important element of overall bronzes from the Arc in the first millennium bc. This characteristic isotope signature is fundamentally different from that of Dajing ores in north-east China, as well from that of early Qin bronzes in Shaanxi and Gansu provinces. This suggests that a variety of metal resources were utilized by peoples living in the Arc. The KDE approach thus proves effective at presenting and comparing lead isotope data.

Thirty-Four Years of Stable Isotopic Analyses of Ancient Skeletons in China: an Overview, Progress and Prospects


Stable isotope analysis of ancient skeletons has become a routine method and widely used to answer diverse archaeological questions related to the human (animal) diets since the initial study in 1977. However, this study in china is underestimated and much less unknown to international circles considering the infrequent publications in English journals. In this review paper, the research history in China was overviewed shortly and then, the research progresses concerning different research themes, such as the chronological trajectory of human diets, the development and spread of agriculture, the mechanism of animal domestication, human social hierarchy, and so on, were introduced in detail, trying to draw a rough framework of human dietary evolution given the unique Chinese geography and cultures. At last, the potential research directions were also suggested for the future studies.

Investigating Human Migration and Horse-Trading in Yelang (夜郎) Through Strontium Isotope Analysis of Skeletons from Zhougshui Sites, South-West China (1300 bc – ad 25)


Yelang (夜郎), a mysterious state located in the south-western area of early China and dating from the Bronze Age to the Early Iron Age (1300 bc – ad 25), is a cultural interactive junction between the Yunnan–Guizhou Plateau and the Yangtze River Basin. The Zhongshui Basin in Weining County, Guizhou Province, was one of the important distribution areas of the Yelang civilization. This area, which includes sites at Jigongshan (鸡公山; 1300 – 800 bc), Hongyingpan (红营盘; 700 – 400 bc) and Yinzitan (银子坛; 400 bc – ad 25), has provided a very integrated chronology, spanning from the Bronze Age to the Early Iron Age in the eastern Yunnan – western Guizhou area. To investigate human migration and horse-trading at these Yelang sites, we conducted a strontium isotopic analysis on the teeth enamel of humans and horses unearthed from these three sites. The results indicated the following: (1) people at the earlier sites (Jigongshan and Hongyingpan) were all indigenous, whereas in the Yinzitan cemetery, there was a more immigrant population, and all the people who were buried in an upper limb flexed supine position were non-local; and (2) most of the horses found at the Jigongshan and Yinzitan sites show different provenances, probably related to the famous Dian (滇) and Zuo (筰) horses recorded in historical documents, providing more clues for further study on horse-trading in South-West China during the Bronze Age and the Early Iron Age.

An Approach to the Diagnosis of Craniofacial Fibrous Dysplasia from the 2500-Year-Old Remains of a Skull from Ancient China


A human skull, buried about 2500 years ago in a Bronze Age cemetery at Jinggouzi, a site of an important ethnic group in ancient China, appeared to have characteristics of fibrous dysplasia. The CT images indicated a reduction in bone density and relatively homogeneous lesions. More features were revealed using CT reconstruction techniques. Lesions seen in low-magnification images using a 3D deep-field microscope had an irregular honeycomb-like structure. At higher magnification, the trabeculae morphology and the gaps between the trabeculae were irregular and varied in size and shape. Paraffin-embedded specimens stained with HE showed trabeculae with tortuous irregular arrangements varying in shape and width. The irregular trabeculae of woven bone has been described as having fibrous dysplasia. Molecular analysis of the GNAS gene indicated no mutation. This provides a non-invasive approach for us to make more comprehensive diagnoses and to assist research into ancient human diseases.

Erratum to Sukenik et al. (2017)