Lead isotopes combined with trace element data represent a powerful tool for non-ferrous metal provenance studies. Nevertheless, unconsidered geological factors and archaeological data, as well as ignored analytical procedures, may substantially modify the interpretation of the isotopic and trace element signature obtained as a potential ore candidate. Three archaeological examples, accompanied by high-resolution lead isotopic measurements (MC–ICP–MS), are presented here to discuss the above-mentioned criticisms and to propose some solutions. The first example deals with prehistoric/historical gold/silver-mining activity from Romania (the Baia Borşa and Roşia Montană ore deposits). The second one regards the lead/silver metallurgical activity from the Mont-Lozère massif (France) during medieval times. The third example focuses on the comparison between two batches of lead isotope data gathered on Roman lead ingots from Saintes-Maries-de-la-Mer, using different SRM 981 Pb values.

Ceramics are usually the most common artefact found on any ancient archaeological site. Compositional analysis of this pottery, and characterization of the clay fabrics from which they are made, has the potential to pinpoint sources of manufacture as well as identify trade routes and consumption patterns in the ancient world. Currently, most analytical techniques require the partial or total destruction of the ceramic sample. This research investigates the use of dual energy computed tomography (DECT) to analyse Black Gloss and Vesuvian Sigillata from Pompeii. The results indicate that DECT may be a viable adjunct or alternative to conventional analytical techniques. Importantly, unlike traditional methods, DECT is totally non-destructive, a highly significant factor when analysing irreplaceable artefacts.

Stone knives were used widely in Neolithic East Asia, presumably in the harvesting of grain crops, but their function has not been clearly understood due to the lack of study of residues from these tools. To address this issue, starch grain analysis was employed to study the residues on the surface of ancient stone knives and large amounts of starches were recovered. The sources of these starches, however, were not well understood, because harvesting of crops involves the cutting of stems rather than direct contact with starchy seeds. To determine whether harvesting could deposit these types of residues, we designed a simulation experiment using stone flakes to harvest ears of wheat, rice and foxtail millet, then analysed the residues on both the flakes and in the plant tissues. A large number of starch grains were found in the stems, including both typical morphotypes from seeds and newly described types that occur only in stems, which can be used as indicators of harvesting. Our study demonstrates that starch grains from residues on the surfaces of archaeological stone knives can indicate not only that the tools were used to harvest ears, but also the type of crops harvested.

In ancient Goryeo celadon excavated from the kiln sites in the GangJin and Buan areas, the effect of the chemical composition and ionic state of Fe on the colour was evaluated by Mössbauer spectroscopy and chromaticity analysis. According to chromaticity analysis, the L* value (brightness) of the glaze was shown to be affected more by TiO₂ and MnO than by Fe₂O₃, and the body was affected more by Fe₂O₃ than by TiO₂. The a* value was found to be affected by Fe₂O₃ and TiO₂ in the glaze, whereas there was hardly any change in the body according to the composition. As for the b* value, changes due to the composition were shown to be smaller than those for the L* and a* values. According to the Mössbauer spectroscopy results, as the quantities of TiO₂ and Fe₂O₃ are increased, Fe²⁺/Fe³⁺ decreases; while the changes in Fe²⁺/Fe³⁺ with MnO and P₂O₅ are negligible. As the quantity of Fe²⁺/Fe³⁺ increases, the a* and b* values decrease, which results in the change of colour from red–yellow to blue–green. The characteristic green colour can be attributed to increased L* (brightness) and decreased a* and b* values (blue–green shift) due to the reduced Fe ion, which is mainly determined by the TiO₂ and Fe₂O₃ contents.

In order to identify the fibre material of the pall imprint excavated from the Peng-state cemetery in Shanxi, biomass spectrometry was applied to determine the amino acid sequences of the residual protein extracted from the soil underneath the imprint. The sequences were searched against a standard protein sequence database. A well-preserved silk pall sample from the Warring States Period was used as a comparative template. The protein extracted is identified as silk fibroin (Bombyx mori). This finding indicates that the extremely degraded pall was made of silk and that the deceased in the Peng-state cemetery enjoyed high social status. In this way, a novel methodology, which is very promising in uncovering the origin of silk, could be initiated.

Fired bricks are a hard and durable masonry material that has played a major role in the emergence of early human urban civilization. In China, fired clay bricks have been widely used as a building and flooring material since the Qin Dynasty (476−206 bc), although a few lines of evidence show that fired clay bricks might have been invented as early as 5500 years ago in eastern central China. However, these burnt clumps of clay appear not to be bricks in the strict sense, and our knowledge about the origin of fired clay bricks in China still remains fragmentary. Archaeological excavations at a Middle Neolithic cultural site in northwestern China reveal that the making of fired clay bricks began some 5000 years ago. Our findings also open a window into the process of prehistoric brickmaking in East Asia.

The traditional thermal expansion method using a dilatometer fails to accurately determine the original firing temperatures of low-fired ancient pottery. For this reason, we have developed an improved method of determining firing temperatures for low-fired pottery. This paper explains the theory of the improved method and presents the reasonably satisfactory results obtained on ancient pottery from the Donghulin site (c. 10 000 bp). The method and the results are very important for the study of ancient pottery culture and clay moulds used for bronze casting.

A total of 33 ancient glass beads unearthed from the Kizil reservoir cemetery and Wanquan cemetery in Xinjiang are studied using Raman spectroscopy, scanning electron microscopy with energy-dispersive spectrometry (SEM–EDS) and other methods. The detailed study of the glassy matrices, the crystalline inclusions and the microstructural heterogeneities for these glass beads has revealed some valuable information to help in the understanding of their possible manufacturing technology and provenance. At least two different types of glass were present in the two cemeteries. For the first time, antimony-based colourant/opacifier—for example, Pb₂Sb₂O₇ or CaSb₂O₆—was systematically identified in some beads of plant-ash type soda–lime glass dated to about 1000–500 bc. The limited number of potash glass beads from the Kizil reservoir cemetery, which were dated to about 500–300 bc, used tin oxide as an opacifier. The diverse resources of the soda–lime and potash glasses indicate the existence of a complex trade network between China and the West much earlier than the Western Han Dynasty.

This study investigated the technological features of the Neo-Elamite glazed bricks discovered at the Acropolis of Susa, south-western Iran, by conducting micro-Raman spectroscopy, differential thermal analysis/thermogravimetry (DTA/TG), X-ray diffraction (XRD) and scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM–EDS). The results showed that calcium antimonate white and lead antimonate yellow were used as opacifiers in the white, yellow and green glazes, and that green and turquoise glazes were achieved using copper. Coloured glazes were separated by a Si-rich brown glaze to prevent them from running together during firing. The glazed bricks most probably were not fired at temperatures higher than 900°C.

There is increasing evidence for complexity in mortuary practices in Britain during the Roman period. One class of burials demonstrates an association between inhumation in stone sarcophagi or lead-lined coffins, ‘plaster’ coatings, textile shrouds and natural resins. It has been suggested that this ‘package’ represents a deliberate attempt at body preservation. Fragments with a resinous appearance found in one such burial from Arrington, Cambridgeshire, UK were analysed using gas chromatography–mass spectrometry. The triterpenic compounds identified are biomarkers for the genus Pistacia and provide the first chemical evidence for an exotic resin in a mortuary context in Roman Britain.

The study of the health of a building connects humanistic and scientific research, and a complete characterization can be achieved by integrating all the available historical documentation, architectural and metrological studies, as well as laboratory and in situ analyses of the materials. A contactless, non-invasive surveying technique such as terrestrial laser scanning (TLS) allows the acquisition of dense and accurate geometric and radiometric (electromagnetic measurements such as signal intensity) information about the observed surface of the building, which can be easily integrated with data provided by high-resolution digital imaging. The early Christian Cantalovo church was surveyed for the first time in April 2011, by means of the ILRIS-3D ER very long range scanner. The second and last survey was performed in June 2012, after the main shocks of the Emilia earthquake seismic sequence. A very long range instrument is suitable for fast, simple and independent measurements, due to its technical characteristics and, for this reason, is easily usable for accurate surveying in emergency conditions. The main results are obtained by applying a data analysis strategy based on the creation of TLS-based morphological maps computed as point-to-primitive differences, which allow the creation of a deformation map and its evolution in time.

The laser ablation ICP–MS transect of a speleothem from GB Cave, close to Charterhouse, Mendip Hills, UK, records Pb variations over the past 5 ka. The speleothem record correlates well with the known historical record of lead mining in the district, the principal features of which include: the Roman lead mining peak; the Dark Ages cessation; gradual, episodic revival up to the late 16th century peak; the 17th century collapse and subsequent recovery; and the final short-lived burst at the end of the 19th century. This correlation supports the assumption that the pre-Roman lead record also derives from local mining. Thus, this record is the first example of quantifying ancient human mining activity through trace element signature of a speleothem. This record also provides the first solid evidence of significant pre-Roman mining activity in the Charterhouse region, and the first solid dating of that activity. This pre-Roman mining can be divided into three main peaks dated to 1800–1500 bc, 1100–800 bc and 350–0 bc.

This paper provides a contribution to FTIR analysis of calcium sulphate-based grounds of paintings when a mixture of compounds with different degrees of hydration is present. The study is based on the analysis with that technique, electron microscopy coupled with energy-dispersive X-ray spectrometry and X-ray diffraction of both the grounds of 16th-century Portuguese paintings and reference samples prepared with anhydrite and calcium sulphate dihydrate bound in an animal glue solution. It is shown that the interpretation of the degree of hydration of calcium sulphate ground samples using FTIR cannot be based solely on the study of the hydroxyl bands, as is usual in routine work, but that small deviations of the S–O vibration bands are an important indicator of the presence of anhydrite in the grounds.

The Roman town of Ammaia (in Marvão Region) is considered one of the most important recent findings of the Roman presence in Portuguese territory. It was settled in Republican times and abandoned in the seventh century. In this research, 17 masonry mortars and renders from the West Tower (South Gate), the residential area near the West Tower, the macellum, the peristylium, the public bath building, the podium of the temple and the portico of the forum were analysed. The methodology of chemical, mineralogical and microstructural characterization has involved several complementary techniques, including stereomicroscopy, X-ray diffraction, thermal analysis and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy. The results indicate that the mortars from the beginning of the town's edification were mainly composed of soil (clays). Later, during the main Roman building period, mortars were composed using a calcitic binder and the mortar composition varied according to their use and function. The samples from a period subsequent to the Roman occupation are based on a dolomitic binder. From the present study, relevant information has been acquired about the technological evolution of Roman construction in Ammaia, the historical context of the archaeological structures and guidelines for the conservation and restoration of mortars.

A multi-proxy study by palynological, geochemical, archaeological and dendrochronological analyses discloses the mining activities at the Mitterberg Main Lode. By these means, several mining phases with varying intensity are recorded during the Bronze and Early Iron Age, whereupon a west to east shift of the mining activity at the Mitterberg Main Lode can be observed. The initial mining phase (Phase II), from the 21st to the 15th centuries bc, is characterized by an opening up of the forest vegetation and, additionally, by slightly elevated heavy metal deposition. Phase III shows a first bloom phase of the chalcopyrite mining during the 14th and 13th centuries bc. Pollen analyses disclose extensive clearings used for pasture and settlement. The increased human impact and higher heavy metal pollution suggest intensive mining activity, which is corroborated by the dendrochronological and archaeological data. Phase IV is characterized by mining activities in progress during the 12th century bc. The pollen data reflect a stabilization of the vegetation and slightly elevated As/Cu/Sb to Sc ratios. During Phase V, in the 11th century bc, new clearings indicate a re-intensification of the mining activities at the Mitterberg Main Lode. Phase VI, from the ninth century bc onwards, describes a human impact with lower intensity at the mining site. This interdisciplinary study at the Mitterberg Main Lode contributes new environmental data for an important area of past metal mining and extends our understanding of the relationship between miners and their landscape.

Ten geological samples (five from each source—Romanian amber and Baltic amber) in duplicate for five different media (air, water, saline, acid and basic) were subjected to thermal alteration at 80 ± 2°C for 12 weeks, in the dark. The samples were analysed before and after the accelerated alteration experiment by Fourier transform infrared spectroscopy, both in transmittance and reflectance mode, and the acquired spectra were statistically processed by multivariate data analysis, mainly using principal component analysis. The results of the experiment are useful in giving a better picture of how to discriminate between archaeological amber artefacts.

In this work we report a pre-restoration spectroscopic study by a multi-technique approach on the green pigment and the binder used in illuminations in a codex of the late 15th century. Our analysis aimed to characterize the badly deteriorated parts of the codex, mainly the green parts, by electron paramagnetic resonance (EPR), X-ray diffraction (XRD), X-ray fluorescence (XRF) and infrared spectroscopy (ATR-IR). We will show that a combined study by EPR and IR spectroscopies on model systems allowed us to refine the general information obtained with the other techniques and to identify the binding media surrounding the chromophore Cu(II) ion.

The degradation of archaeological wood at freezing and thawing temperatures is studied at the site of Qajaa in West Greenland through a combination of environmental monitoring, measurement of oxygen consumption and microscopy of wood samples. Permanently frozen wood is still very well preserved after 2–4000 years, while wood samples that thaw every summer show attack by soft rot and an average density loss of 0.1 g cm^–3 (corresponding to 25% of the dry mass) over the past 27 years. Future increases in temperature may increase the decay rate significantly (Q₁₀ = 4.2 at 0–10°C) but the effects on site depend on local hydrology.

Mineralogical and geochemical results derived from analyses of the pottery ensemble documented in the Cave of Los Gitanos (Castro Urdiales, Spain) are presented in this paper. This site contains an archaeological deposit formed in the mid-fifth millennium cal bc, which has yielded one of the oldest pottery assemblages in northern Spain. The analysis of the pottery remains has focused on both petrographic (thin-section and XRD) and geochemical characterization (SEM–EDS) of samples selected after a macroscopic study. The mineralogical analysis has revealed procurement of raw materials from different sources, as well as different manufacturing processes. In addition, the petrographic analysis has shown different methods of manufacture, such as pottery tempered with calcite, limestone, ophite (ophitic dolerite) and grog, and fabrics with non-modified clays. Variations observed between the oldest assemblage (Sub-levels A4 and A3) and the most recent one (Sub-level A2) suggest a modification in pottery-making practices between the fifth and the third millennia cal bc.

At Santa Filitica, a Roman settlement in north-western Sardinia occupied until the ninth century ad, archaeological excavations have found the remnants of a furnace consisting of a semi-circular base made of stony slabs and tiles bound with clay. The furnace is attached to a wall of Roman age. Layers of the sixth century ad, bearing several variously oxidized slags, were found close to the furnace. These findings first testify to an ironworks in Sardinia, within a well-defined context. XRPD and SEM–EDS mineralogical and textural analyses suggest that the slags derive from a bloomery and smithing work that was the first evidence of this type documented in Sardinia during the Early Middle Ages. Chemical analyses (performed with ICP and INAA) of rare earth elements and trace elements in two slags and in two Sardinian iron deposits allow some conclusions to be drawn on the local provenance of the ore. Our comparison of the Sardinian findings and some slags representative of archaeological smelting sites at the front of Elba island—the largest and longest lived iron-working sites in the Mediterranean—also improves the methodology with which iron slags derived from different ores are compared.

Lead isotopes, thin- and sherd-section analyses are coupled on pottery-vessel fragments excavated from the Late Bronze Age site of Hala Sultan Tekke (south-east Cyprus) and representing fabrics used for the production of storage and trade containers. The fabrics of the sherds are first described according to general macroscopic observations. Based on the different fabrics identified, a petrographic analysis is carried out on thin sections and compared to lead isotope results on the same samples. This study shows that a specific fabric corresponds to a specific lead isotopic composition and proposes different sources for the various groups of associated sherds/fabrics. It also demonstrates the compatibility and complementarity of petrography and lead isotopes within pottery provenance study.

In the framework of the EU–UNDP project ‘Rehabilitation of Old Nicosia’ (Cyprus, 2004–9), a high-resolution geoelectrical survey has been performed inside the partially ruined monumental complex of St Nicholas of the English, now called the Bedestan, which was designed to become a venue space for cultural activities. The aim was to detect buried traces of a Byzantine basilica of the sixth century, on the ruins of which, according to tradition, the construction of St Nicholas was begun in the 12th century. The survey has been conducted on the floor of the monument, using a dipole–dipole electrode array along two perpendicular sets of profiles. In order to model the resistivity distribution, the probability-based electrical resistivity tomography inversion (PERTI) method has been applied. Sets of aligned blocks with resistivity in the range 100–400 ohm·m, bounding a three-room rectangular space, and traces of a rounded structure with mean resistivity about 150 ohm·m, appearing at one extremity of the central room, are the main resistive features recognized down to 4 m depth, within a conductive background with resistivity in the range 20–40 ohm·m. Altogether, these resistive features, showing in plan the shape of a church characterized by a central nave with an apse and two side aisles, have been interpreted as an evidence of the existence of remains of the earlier Byzantine basilica. Moreover, small volumes with resistivity in the range 10–12.6 ohm·m have been found, scattered underneath the whole surveyed area. Taking into account the PERTI results, ground-truth has been performed in two sites, designed to become two permanent protected exposures of the archaeological findings beneath the floor of the newly restored Bedestan. At one site, excavations detected remains of masonry in correspondence of the alignment of resistive blocks at the left margin of the left side aisle of the churchlike structure. At the other site, graves, entirely filled with wet debris in an alluvial soil matrix, have, instead, been found in correspondence with the greatest conductive volume, detected outside the perimeter of the churchlike structure. Both findings have been dated back to the sixth century. Since the Bedestan case-history is one of the first applications of the PERTI algorithm to real field data sets, its performance has been tested using the well-known ERTLab^TM commercial software as benchmark. The comparison has shown a general consistency between the two inversions, and also confirmed the much higher computing speed, better filtering capacity and greater versatility of the PERTI algorithm, already outlined in a previous paper where only synthetic models were tested.

Within variation, three major iron smelting furnaces were used in the Iron Age of sub-Saharan Africa, ranging from the natural draught driven tall shaft to the forced draught powered low shaft and bowl furnaces. These furnace types are, however, mostly known from the ethnographic context. Often, archaeologists are confronted with remnants from the smelting process, forcing them to speculate on the anatomy of the extant furnaces. The presence of multiple fused tuyeres has been used to identify natural draught furnaces in the archaeological record. However, working back from smelting remains such as slag to the furnace type using physical and chemical evidence has generally proved to be ‘undoable’. Thus, when randomly selected, the chances are high that one cannot separate bowl furnace slags from those that formed in their tall or low shaft counterparts. This observation is hardly unexpected; analogous thermodynamics and thermo-chemical reactions governed bloomery smelting irrespective of furnace type. Rehren et al. () have labelled this phenomenon the ‘tyranny of system driven constraints’. In this study, we argue that the hierarchical use of statistical methods may add another layer of evidence which, when coupled to archaeological indicators, may be useful in correlating slag chemistry to furnace types used in antiquity.

The aim of this work is to examine whether it is possible to find chemical markers that allow a distinction to be made between the imported black glossed ‘Campanian A’ and the Sicilian imitation (end of fourth to first century bc) of these productions by carrying out quantitative chemical microanalysis of the slip using the SEM–EDS technique. The efficiency of the proposed analytical method has been tested on a set of ceramic samples corresponding to Sicilian black gloss imitations whose ceramic body has already been characterized petrographically by thin-section microscopy and chemically by XRF. The analytical data point to Na₂O as a suitable chemical marker to distinguish between original ‘Campanian A’ imported from the Gulf of Naples area and Sicilian imitations of the same forms of Hellenistic pottery. In order to verify the above result, the enrichment factors (EFs) between the raw clays, the corresponding ceramic body and black gloss slip were calculated. Some differences in the patterns of EFs between original ‘Campanian A’ and Sicilian imitations were recognized and explained. Therefore, the obtained results can help to accomplish a first distinction between imported and local material on a firm analytical basis, working on a statistically significant number of individuals.

An investigation was made of the fracture risk to buried ceramic pots and bones from the subsurface pressures generated by agricultural operations. A method for generating subsurface pressures at 0.25 m depth in a soil bin was developed and used to explore fracture failure of modern replicates of ceramic pots corresponding to different archaeological periods and aged medieval human bone. Application of conductive traces to the objects’ surfaces allowed detection of fracturing in real-time without excavation. Predictive models relating fracture of objects to subsurface pressure application were developed by relating the probability of fracture to observed survival statistics at increasing subsurface pressures. Subsurface pressures of above 100 kPa were sufficient to fracture the more fragile pots at a probability level of 90%. The lowest subsurface pressure causing bone fracture was 280 kPa; however, no relationship was observed between subsurface pressure and bone fracture, probably due to variation in bone material. The subsurface pressures generated and applied are within the range reported from field measurements during typical agricultural operations. They indicate that measures to control the generation of subsurface pressures would be necessary to mitigate risk of harm from agriculture to buried archaeology; for example, via low-pressure tyres, tracks and appropriate tillage.

Tempers added to pottery have the potential to obscure geographical variation in the chemistry of exploited clay resources when analysed using bulk methods. A pilot study was conducted to assess the possibility of using LA–ICP–MS to analyse clay matrix in pottery with extremely subtle partitions between INAA chemical groups. LA–ICP–MS was used to analyse the clay matrix of 32 pottery samples from seven Middle and Late Woodland period (c. ad 200–800) sites in north-east Florida and results were compared to data from INAA of the same samples. The results reveal many of the challenges in analysing highly heterogeneous materials with LA–ICP–MS. However, the study also generated data that are potentially useful in the determination of pottery provenance. In some respects, LA–ICP–MS of clay matrix replicated the chemical variation recorded by INAA, and in other respects the results are divergent. The similarities and differences between these results are explained by specific differences between the methods and the materials analysed (matrix versus bulk analysis). Suggestions for improving the method are discussed.

In this paper, the construction period of the cruciform terraces with columns and the elevated causeways in the Angkor monuments of Cambodia is reconsidered, based on the results of our investigation of magnetic susceptibility and other characteristics of sandstone blocks. From an art-historical point of view, they are generally considered as modifications in the post-Bayon style period—the period during the reign of Jayavarman VIII (1243–95 ce) or later. However, from a lithological point of view, the average magnetic susceptibilities of the sandstone blocks in the cruciform terraces with columns and the elevated causeways are consistent with the rest of the monument. In addition, the characteristics of the sandstone blocks in the cruciform terraces, such as their shape, the orientation of the bedding plane and the stacking method, suggest that they were constructed in the same period as the rest of the monument.

The main objective of this study is to recover the initial geometry of earthen walls from the shape of wall remains. The original parameters of the walls have been estimated by fitting the field-measured profiles with the theoretical shape predicted by the model. We estimate: (i) the initial wall height (between 2 and 3 m); (ii) their shape (vertical or nearly vertical); and (iii) the time for complete degradation (between 250 and 400 years, depending on wall orientation). We show that this approach yields the best results when the main degradation factor is the temperature gradient, as it is for south-oriented wall faces.

The calcium isotope ratios (δ^44/42Ca) in milk-consuming infants and juveniles are compared to adults at two archaeological sites to test whether milk consumption is detectable in the skeleton using calcium isotopes. At Aşıklı Höyük, δ^44/42Ca is correlated with δ¹⁵N and differs significantly between juveniles and adults, suggesting that δ^44/42Ca is responding to dietary milk input. However, at Christ Church, Spitalfields, no correlation between δ^44/42Ca and δ¹⁵N or age is noted. At this site, δ^44/42Ca of adult females is not related to the minimum number of births, and we conclude that the maternal skeleton is not sufficiently isotopically perturbed for this signal to remain throughout her lifetime. Growth may result in an increase in very young infants' δ^44/42Ca, in contrast to an expected decrease due to milk consumption, complicating the interpretation of the data. We conclude that milk consumption does not always result in a change in skeletal δ^44/42Ca, or is masked by other effects.

Excavations carried out in Cuma by the Centre Jean Bérard archaeologists have uncovered a large quantity of pottery. This study is focused on cooking ware and on internal red-slip cookware, also known as Pompeian Red Ware (Rosso Pompeiano), dated from the first century bc to the first century ad. A comparison with the minero-petrographic composition of beach sands collected along the Bay of Naples coastline highlights the provenance of the temper from the Somma-Vesuvius area, marked by leucite-bearing scoriae and garnet. Petrochemical analyses allow us to distinguish two main groups of pottery characterized by different technological options based on the amount of temper and on the type of clay. X-ray diffraction and scanning electron microscope data demonstrate improved accuracy in the production of Rosso Pompeiano, especially with regard to firing control, which was in a prevailing oxidizing atmosphere and in a narrow thermal range, between about 800 and 900°C.

This paper focuses on plain, stylistically unvaried pottery from three Late Neolithic sites from the Mondego Plateau, Portugal, and investigates ceramic production and exchange among small-scale prehistoric societies by means of thin-section petrography and chemical analysis (INAA). The results show that the majority of the pottery was made with widely available, granite-derived sedimentary clays, but petrographic differences between fabrics indicate collection at multiple locations within these deposits. Variation in chemical composition is consistent with site-specific sourcing areas, while comparison with data from earlier sites in the Mondego and surrounding mountains suggests that such sources were geographically restricted within the plateau. In contrast, the small percentage of vessels produced with residual clays of metamorphic and intermediate igneous origin, which outcrop over 10 km and 30 km from the archaeological sites, demonstrates that plain pottery did circulate during the Neolithic beyond the funerary sphere. This is the product of the routines of mobility and social networks of Neolithic groups across the wider landscape, which involved the exchange of ‘mundane’ vessels. Finally, the study demonstrates that micro-regional provenance studies can provide significant insights into prehistoric social landscapes if the data are interrogated beyond simplistic classifications of local and non-local.

The prehistoric settlement on the Kiechlberg hilltop is located a few kilometres to the north-east of Innsbruck, in the Tyrolean Inn Valley. Despite its rather isolated location, a multiphase settlement between the fifth and the second millennium bc was confirmed by archaeological investigations in 2007 and 2008. Metallurgical artefacts, such as copper ore fragments, copper slag and raw copper, as well as finished copper and bronze artefacts, are concentrated mainly in Late Copper Age to Middle Bronze Age layers. The chemical compositions of the slag and raw metals confirm Fe—Zn tetrahedrite–tennantite (fahlore) smelting. The ore was most probably imported from the 30–50 km distant copper ore deposits (mainly fahlore) of Schwaz–Brixlegg, in the Lower Inn Valley. The small amount of slag and the presence of slagged and thermally altered ceramic fragments suggest copper production in small-scale workshops. Most probably, sulphide-rich ores were smelted in crucibles in a hearth fire. The process was relatively reducing below the 2Sb + 1.5O₂ → Sb₂O₃ reaction (−8.5 log fO₂ at 1100°C), producing Sb-rich (>10 wt% Sb in metal) raw copper. Inhomogeneous slag remains containing high amounts of sulphide and metal inclusions suggest a poor separation of the metal, matte (copper sulphide) and silicate/oxide melt during the smelting process.

Heat treatment of lithic raw material is known from the Middle Stone Age to the Neolithic. These findings require archaeometric techniques and methods for detecting the heat-induced effects within lithic artefacts. However, the existing methods are often cost-intensive and time-consuming, and most of them are destructive. Here, we present a new method using the infrared spectroscopic measurement of the strength of H-bonds formed between surface silanole groups (SiOH) and H₂O molecules held in open pores of the samples. The reduction of H-bond strength in chalcedony is shown to be strongly correlated with the loss of open pores induced by heat treatment. Hence, the method is based on measuring one of the transformations aimed for by the instigators of the heat treatment: the reduction of porosity that modifies the rock's mechanical properties. A first application to heat-treated material from the Neolithic Chassey culture (southern France) shows that flint was heated to temperatures between 200°C and 250°C in this period. This has important implications for the study of the procedures used and the heating environments. Our new method is non-destructive, rapid, cost-effective and allows for detection of the used annealing temperatures.

This paper thematically characterizes a large body of recent obsidian sourcing discourse as a means of highlighting the current place of obsidian provenance studies in larger archaeological discourse. It is shown that the field of obsidian sourcing is flourishing, with a clear upward trend in the number of published studies in the past decade. This paper further argues that sourcing is a means to an end, a way to determine where artefacts originate, and thus a means of addressing broader archaeological problems. Through this contextual framework, obsidian sourcing studies—and indeed all provenance studies—are seen as relevant because they transcend the increasingly specialized world of archaeological discourse.

We report a molecular methodology to obtain and analyse ancient bacterial DNA from archaeological dental calculus. Recent and archaeological DNA samples, as old as 4000 bp, were successfully extracted and amplified with species-specific PCR primers. We propose this approach in order to: detect the presence of specific bacterial species infecting past human populations; compare the composition of ancient oral microbiomes among human populations; and analyse the genetic variability and covariation of bacteria and human host populations. Genomic analysis of bacteria from dental calculus is a promising source of evidence for palaeopathological and micro-evolutionary studies, focused either on micro-organisms or their human hosts.

Fifteen fragments of glazed pottery were studied by scanning electron microscopy coupled with energy-dispersive X-ray analysis (SEM–EDS). The fragments, dated from between the 11th and the 12th centuries, are part of a group excavated at ancient Bust and Lashkar-i Bazar (southern Afghanistan) and belonging to the International Museum of Ceramics in Faenza. All the samples are characterized by highly calcareous bodies, and all of them but one is coated with a transparent lead glaze; the last fragment is, instead, coated with a turquoise opaque lead–alkali glaze. With three exceptions, the studied fragments show underglaze decorations featuring white, red, green or black motifs applied on to a white, red or black engobe; one of the remaining glazes is applied on to a monochrome white slip and the other two directly on to the ceramic body. Optical microscopy and SEM images show that engobes and decorations were obtained by deposition of differently coloured clayey slips, the composition of which was characterized by EDS analyses. In particular, black engobes and decorative motifs were obtained by recourse to manganese and iron compounds or to chromium, magnesium and iron compounds; it appears that both possibilities could be exploited for obtaining different decorative motifs on the same object.

Contamination of ceramic specimens resulting from sample-preparation techniques has the ability to confound efforts of chemical characterization. Primary contamination, identified by significant concentrations of one or more elements, is easily identified. Secondary contamination, resulting from undetected elements influencing detected elements, is more difficult to identify. Evaluation of six powder-extraction techniques identifies variable effects of contamination. Extraction by drilling carries the highest risk of contamination. The grinding of specimens with silicon-carbide wheels may artificially deplete abundances by introducing Si and C. Grinding specimens in an agate mortar and pestle is found to be the technique least likely to result in contamination effects.

Forty-seven decorated samples of Archaic pottery excavated at a Heracles sanctuary (Thebes, Boeotia) were studied through a combined surface and body approach, using non-destructive techniques. Most of the samples were archaeologically classified as Theban/Boeotian, others as Corinthian and a few as possibly Euboean. The techniques employed were optical microscopy and SEM–EDAX (micromorphology and compositional analysis of the surfaces) and XRF for the analysis of the ceramic body. The results provided information on the technological level of the collected pottery as well as on the relation of the chemistry and micromorphology of the pigments, aimed at assisting provenance studies.

Pre-Romanesque murals at Kostoľany pod Tríbečom, Slovakia, have been investigated by portable X-ray fluorescence and by microanalytical methods to identify painting materials (pigments and binders), and to explain the degradation of colours. Today, missing green and blue shades have been reconstructed according to residual concentrations of Cu, which correspond to copper chlorides—products of salt corrosion of the copper carbonates azurite and/or malachite, accelerated by micro-organisms. As confirmed by powder X-ray microdiffraction, original minium (Pb₃O₄) has been transformed to brown–black plattnerite (PbO₂). In increased humidity, even insoluble pigments are washing down from the walls and the intensity of colours further diminishes.

In Trommsdorfstraße, Erfurt, a glass-processing workshop has been excavated, which produced lead glass rings and beads in the 13th century. This workshop produced two different lead glasses. The first, a high-lead glass, could be found throughout Europe, from England to Russia. However, another newly defined type of glass could be identified (Central European lead–ash glass). This can be demonstrated by analysing the literature, and it has been found in eastern Germany, Poland, Slovakia and the Czech Republic. A Slavic lead–ash glass with the same ash content as the Central European lead–ash glass but lower amounts of lead was produced in Eastern Europe. In western Germany, another type of ash (beech ash) was used to produce a wood-ash lead glass. Lead-isotope analysis proved that the same source of lead was used for the wood-ash lead glass and the high-lead glass in western Germany and the two types of glass from Erfurt.

Tin bronze replaced arsenical copper as the preferred alloy in the Levant for reasons that have long been debated. Found almost exclusively in graves, these two types of copper alloys share nearly identical mechanical properties. The Bronze Age cemetery of ‘Enot Shuni has yielded the first metals ever analysed from an uninterrupted stratigraphic sequence in the Levant, spanning the earliest adoption of tin bronze from the Early Bronze Age (EB) IV through the Middle Bronze Age (MB) II (c. 2300–1530 bc). SEM–EDS analysis of these artefacts, combined with a compositional meta-database of all previously published EB IV – MB II alloys, reveals diachronic alloy progression as selected by populations of the Levant. It has long been qualitatively understood that bronze became the primary alloy by the MB II. These results verify this trend and quantify human demand, showing that tin importation increased by 103% and arsenic content decreased by 49% throughout these periods. This shift in technological choice is attributed to cultural reorientation from the Egyptian to Mesopotamian sphere of influence, as well as to tin's appreciable fuel efficiency over pure copper and arsenical copper in light of unprecedented timber shortages.

This study explores the potential of carbon and oxygen isotope data from human enamel carbonate (n = 50) to contribute to mobility studies in the Caribbean. Most oxygen and carbon isotope results display limited variation, with substantial overlap between islands. However, a few individuals from El Chorro de Maíta, Cuba possess relatively low δ¹⁸O and high δ¹³C. Two of these individuals were previously identified as possible non-Antillean immigrants on the basis of strontium isotopes, and bioarchaeological and mortuary evidence. The carbon and oxygen isotope results provide additional evidence supporting the proposed non-local origins of these individuals and contribute to explorations of their potential natal origins.

A collection of window-panes, vessels and alleged waste from Thamusida has been investigated by OM, SEM–EDS, ICP–MS, ICP–OES and XAS at the Fe–K and Mn–K edges. Glass samples have been characterized as natron-based soda–lime–silica glasses, with low magnesium and low potassium. The results have been compared with 43 reference groups available for ‘naturally coloured’ and colourless glasses of both Roman and later ages. Two main types were distinguished: RBGY 1 (Roman Blue–Green and Yellow 1) and RBGY 2 (Roman Blue–Green and Yellow 2). Given their compositional similarity to the Levantine I or, to a lesser extent, HIMT glasses, the Syrian–Palestinian coast for RBGY 2 and Egypt for the RBGY 1 have been suggested for their provenance. Most Thamusida samples have been assigned to the RBGY 2 type. A small group of Thamusida colourless vessels was included into the RC (Roman-Colourless) compositional field; the latter still being defined. The alleged waste pieces may define a local production that should have been of secondary type. The investigations performed on local raw materials seem to discount the possibility of a primary glass-making site. XAS measurements determined that Fe²⁺ contents ranging between 30 and 52% are able to assure an aqua blue colour; below 30%, the glasses turn light green or light yellow.

This study investigates the earliest surviving Tibetan paper, from the Dunhuang cave library, using paper fibre analysis combined with codicological, palaeographical and textual information. The hypotheses tested by this method concern the regional origins and production centres of early Tibetan paper and methods for dating this material. Using overlapping typologies, we classify a sample of manuscripts into coherent groups, relating them to particular ‘book cultures’. By linking three main manuscript groups to different geographical regions, we offer new insights into an important manuscript collection, and show that the method of overlapping typologies has the potential to yield further insights.

The geochemical compositions for obsidian from two of the most important sources on the Japanese island of Hokkaido, Shirataki and Oketo, are presented. This work represents the first systematic study of obsidian geochemistry on Hokkaido from the view of modern methodological standards. The study was performed with the help of neutron activation analysis to determine the concentrations for 28 elements. The results obtained allow us to subdivide both sources into two geochemical groups (Shirataki-A and -B; and Oketo-A and -B), with each representing an individual sub-source. Obsidian from both Shirataki and Oketo sources is identified at archaeological sites located on Hokkaido, on the neighbouring Sakhalin Island and Kurile Islands, and in the lower course of the Amur River basin. The distance of obsidian transport during the Upper Palaeolithic was up to ∼250 km, and in the following Neolithic and Palaeometal periods up to ∼1200 km. This testifies to the wide distribution of Hokkaido obsidian to archaeological complexes in North-East Asia and its active transport/exchange in prehistory. The data presented here should be used as a reference for the obsidian geochemistry of Shirataki and Oketo sources from now on.

A multimethod approach using petrography and strontium (Sr) isotopic analysis was applied to determine the geological source of 17 marble artefacts from the Roman town of Ammaia (Portugal). All samples are calcitic, with dolomite, quartz and muscovite as accessory minerals. The marbles are characteristically medium-grained with a maximum grain size (MGS) between 0.98 mm and 1.82 mm, have a heteroblastic texture, and have curved to embayed calcite grain boundaries. ⁸⁷Sr/⁸⁶Sr values of marble leachates range from 0.708488 to 0.708639. Comparison with Hispanic and Mediterranean marbles suggests the Estremoz Anticline as the most likely source for the Ammaia marble, especially for architectural marble. This hypothesis is supported by the geographical proximity of the Estremoz marble district and the long and expensive overland transport required for other marbles to reach Ammaia.

The Archaeological Museum of Jaén's sizeable collection of Iron Age sculptures, dating from the fifth century bce, were all found at Cerrillo Blanco de Porcuna, a site in the Spanish province of Jaén. The collection comprises over 40 statues and hundreds of fragments. Incisions recently identified on some of these sculptures have been interpreted as sculptors' marks. The present archaeometric study, conducted with a 3D roughness meter, showed that the marks on several of the sculptures analysed were made with the same type of tool and the same engraving technique. While the graphological differences denote different authorship, they would appear to have been made in the same workshop. The morphological differences observed in the lines analysed on other sculptures are interpreted to indicate the use of other types of tools and engraving techniques.

A combination of two autoradiography methods was applied to investigate the radionuclide distribution patterns in a range of different silices. We obtained greyscale images (β-radiation) and α-track patterns for qualitative assessment, and used a statistical approach to quantify the degree of uniformity of the radiation fields. It was found that almost all samples are poor in potassium, thorium and uranium, and that locally high concentrations are present only in dark-coloured veins and inclusions. Statistical analyses reveal evidence of radionuclide clustering in more than half of the 21 specimens. Concerning thermoluminescence dating of burnt lithics, such gradients should be taken into account to improve precision and accuracy in cases where the external radiation is not strongly dominating for the sample under consideration.

Late Antique coarse cooking wares and painted fine wares found at Herdonia (second half of the fourth century to mid-fifth century ad) and Canusium (late sixth century to early seventh century ad) have been chemically and mineralogically characterized. A total of 74 samples (40 of coarse ware and 34 of fine painted ware) was investigated through optical microscopy, scanning electron microscopy, X-ray powder diffraction, inductively coupled plasma optical emission spectrometry, inductively coupled plasma mass spectrometry, neutron activation analysis and X-ray fluorescence. A new statistical method, namely the classification tree methodology, was used for the treatment of geochemical data. The characterization of the Herdonia and Canusium assemblages was combined with a review of earlier results obtained for San Giusto and Posta Crusta, in order to get an insight on Late Antique ceramic trades in northern Apulia. It appears possible to reconstruct a production pattern organized at multiple production sites, both rural and urban, that exploited similar raw material deposits, specialized in certain productions, and commercialized products at different geographical scales. Imports from outside northern Apulia may be identified for coarse wares. A likely area of production is difficult to establish; however, the northern Adriatic coast and the area of Greece may be suggested.

In this study, we have evaluated the applicability of Nd isotopic analysis for the provenancing of Roman glass and we present a database of Nd isotopic compositions of possible sand raw materials from the western Mediterranean, as a means of comparison for the growing number of isotopic studies on ancient glass. The ¹⁴³Nd/¹⁴⁴Nd isotope ratio of sands is a good indicator for their geological (and sometimes geographical) provenance. The use of the isotopic signature of Nd as a proxy for the source of silica in glass is, however, not always straightforward because of the possible overlap of signatures from different suppliers.

Scottish window glass from both archaeological sites and historic buildings was examined using portable X-ray fluorescence (pXRF) and scanning electron microscopy – energy-dispersive X-ray micro-analysis (SEM–EDX). The elemental composition of the glass provides information regarding the materials used and, subsequently, an approximate range of dates of manufacture. pXRF is shown to be more vulnerable than SEM–EDX to the effects of surface corrosion and matrix effects in archaeological samples. The study showed that the production of window glass in Scotland from the 17th century onwards appears to closely parallel that in England. It also demonstrated the potential of pXRF for in situ studies of window glass in historic buildings. pXRF was used to assess two Scottish buildings; one in state care and one in private ownership. The building in state care, the Abbot's House at Arbroath Abbey, showed a uniform glass type, suggesting that the building was re-glazed completely at some point during the late 19th or early 20th century. The building in private ownership, Traquair House, had a range of glass types and ages, demonstrating a different maintenance and repair regime. This type of data can be useful in understanding historic buildings in the future, particularly if re-glazing is being considered.

The mineralogy, petrography and major- and trace-element composition of iron ores from Elba Island (Tuscany, Italy), one of the most important iron sources in the Mediterranean area since the first millennium bc, revealed that hematite-rich ores display prominent enrichments in W and Sn (up to 4950 μg g⁻¹ and 8400 μg g⁻¹, respectively). These two elements are hosted by tiny grains of W–Sn mineral phases (ferberite, scheelite and cassiterite) that are disseminated throughout the hematite matrix. A comparison with iron ores from many Italian and European localities (most of which were exploited in ancient times) suggests the uniqueness of the geochemical pattern of Elba Island hematite-rich ores (i.e., high W and Sn, low Mo and low Cu, Pb and Zn). We suggest that this geochemical signature may represent a new provenance marker not only for discarded ore at smelting/smithing sites, but, possibly, also for metallurgical slag and smelted metal produced in the chaîne opératoire of the iron process.

Archaeological bone undergoes alterations after burial (diagenesis) that constitute a problem for the survival of archaeological information. A common method to assess this alteration is Fourier transform infrared spectrometry (FTIR). However, the commonly applied method (FTIR–KBr) is destructive and sample preparation may influence the results. This paper tests the suitability of FTIR attenuated total reflection (FTIR–ATR), a method not commonly used to investigate bone diagenesis. FTIR–ATR requires less sample preparation and can be non-destructive, allowing analysis of bone cross-sections. Modern and archaeological bones were analysed using both methods and different sample preparation methods were tested. The results show that FTIR–ATR has advantages for the rapid assessment of bone diagenesis.

The discovery of wells of the linear pottery culture since 1990 has led to new insights on the ability and needs of humans at this time. The still small number of about 20 wells in Europe, compared to the much greater number of known settlements of this period, led to the assumption that they were built for special purposes, other than the water supply for the whole village. Investigations on the origin of archaeosediments of a more than 7000-year-old and 4.2 m deep well from the linear pottery culture in north-west Saxony, Germany were carried out by geochemical analysis to improve our knowledge of the building, the usage and the decay of this wooden construction. Special emphasis was put on the material around two 10-week-old piglets that were intentionally deposited in the construction pit. Three major units—the sediment in the well, the infilling of the construction pit and the surrounding gravels—influenced by lateral transport of fine clay could be identified and described.

This paper discusses the problems with sampling materials and sampled contexts in the framework of radiocarbon dating of Mesolithic sites situated in generally dry, acid and bioturbated coversand deposits within north-western Europe. The case studies presented all relate to the coversand regions of northern Belgium and the Netherlands, two areas for which very large sets of radiocarbon dates performed on different organic components are currently available. The study points out that charred hazelnut shells from surface hearths and charcoal from hearth pits guarantee the most secure dating results, while the dating of calcined bones and food crusts from Final Mesolithic pottery so far remains problematic.

The asphalt from the Dead Sea was an important item of trade in antiquity. Among its many uses, the most widespread was its export to Egypt for use in the mummification process, albeit at a relatively late date; that is, post 1000 bc. Its use became particularly important in the Ptolemaic–Roman period, as demonstrated by a war in the fourth century bc specifically to gain commercial control of this product. Although the reasons why the Egyptians wanted Dead Sea asphalt at this specific time are nowhere specified, the answer may lie in its increasing availability as a (partial) replacement for the plant resins used previously. A review of the historical literature shows that Dead Sea asphalt was used for at least two millennia as a biocidal agent in agricultural practices. It is proposed that the reasons for using Dead Sea asphalt in the mummification process are due to its dual role; first, as an external mechanical shield, when smeared on the exterior of mummy wrapping, to prevent ingress by insects, fungi, bacteria and moisture; and, second, as a biocidal agent (perhaps due to its high sulphur content), which prevented the flesh from decaying, the prime concern for the ancient Egyptians.