NEW EVIDENCE FOR THE NATURE OF THE ATTIC BLACK GLOSS

New evidence is reported here using transmission electron microscopy, scanning electron microscopy, and laser reflectance for the nature of the black glossy decoration layer present on the Attic black or red figure vases of the sixth to fourth century BC. The black layer, of total thickness about 20 μm, consists mainly of poly crystalline magnetite (Fe₃O₄) particles of dimensions from 0.2 μm down to extremely fine sizes embodied in an amorphous vitreous matrix. On the outer surface of the black paint we discovered for the first time a thin clear glassy film of approximate thickness 0.1 μm which is rich in Al and Fe and poor in Si. This film must be responsible for the characteristic sheen of the surface. This is verified with the reflection of laser light mostly in specular direction, a unique property compared with black paints of other areas and other periods.     

Microstructural and Componential Characterization of the Plating Technology on Chinese Han Dynasty Bronze Fragments

The bronze wares of the Han Dynasty excavated in Chongqing are decorated with plating patterns, maintaining an exquisite lustre right up to modern times after the covering patina is cleared away. In this paper, a plated fragment of the Han Dynasty from the Wushan County Museum was characterized by combining optical microscopy (OM), scanning electron microscopy with X‐ray energy‐dispersive spectrometry (SEM–EDS), X‐ray fluorescence analysis (XRF), X‐ray diffraction (XRD) and X‐ray photoelectron spectroscopy (XPS). The results showed that the bronze fragment was gilded with a ~ 3 μm thick gilded layer and a ~ 20 μm thick silvered layer. The high concentration of Hg and Hg‐rich intermetallic compounds confirmed the existence of mercury gilding/silvering technology, for example, Au₉Hg in the gilded layer and Ag₁₃Hg₇ in the silvered layer. An ordered stripe structure was observed in the gilded surface, corresponding to the formation of rod‐like, intermetallic Au–Hg compounds. Specifically, a high concentration of Au was detected in the silvered layer. The exploration of gilded/silvered bronze casts light on this ancient technology and the benefit of identifying, protecting and reproducing it.     

Evaluation of Quantitative XRF Analysis Applied to Determine Cobalt Sources in Chinese Blue‐and‐White Porcelain

A method using the ratios between MnO, Fe₂O₃ and CoO to differentiate the cobalt sources for Chinese blue‐and‐white porcelain was developed in Oxford in the 1950s using X‐ray fluorescence (XRF) analysis directly on the glaze. In this paper, six blue‐and‐white porcelain sherds from the Luomaqiao kiln were analysed by XRF on the glaze and by scanning electron microscopy with energy‐dispersive spectrometry (SEM‐EDS) in cross‐section. The ratios between MnO, Fe₂O₃ and CoO calculated by quantitative XRF and EDS analyses are different. The analysis depths for MnO, Fe₂O₃ and CoO are < 60 μm by XRF analysis. However, the average glaze thickness of samples is > 400 μm, and the MnO, Fe₂O₃ and CoO mainly remain in the lower layer of the glaze, which is beyond the analysis depths of XRF analysis. The limitations of major and minor quantitative analyses for differentiating cobalt sources are discussed.     

Characterization of prehispanic cosmetics found in a burial of the ancient city of Teotihuacan (Mexico)

The present paper reports the chemical data obtained on samples of pigmenting materials contained in 31 miniature vessels found in a burial found in Teopancazco, a multiethnic neighborhood center located in the southeastern sector of the archaeological site of Teotihuacan (Central Mexico) and the analytical protocol established for the complete characterization of these archaeological materials. For this purpose a multi-technique approach based on the combination of several non destructive and micro-destructive instrumental techniques, namely, light microscopy (LM), scanning electron microscopy-X-ray microanalysis (SEM-EDX), transmission electron microscopy (TEM), voltammetry of microparticles (VMP), X-ray microdiffraction (μXRD), X-ray diffraction (XRD), UV-Vis spectrophotometry, FTIR spectroscopy and gas chromatography-mass spectrometry (GC-MS) has been developed in an attempt to completely characterize these materials. These instrumental techniques provide reliable and complementary data including elemental and mineralogical composition, identification of functional groups as well as speciation studies of electroactive species. Among the most relevant findings, volcanic pyroclastic rocks and clayey soils, most probably, from the Teotihuacan valley as well as galena, jarosite and mica from other provenances in Mesoamerica, have been identified. Charcoal and Ocote resin have also been identified. The chemical composition of the samples is discussed with a view to the possible function as cosmetic materials and their use in funerary rites. The results have been critically compared with those others obtained in other ancient civilizations. The study carried out on the materials found in the burial 105 is especially relevant insofar it represents the first evidence, scientifically characterized, of the use of cosmetics in Mesoamerica at this early period (AD 200-550).     

Historical Mortars from the Fortified Upper Town of Eivissa (Balearic Islands,Spain)

Samples of mortars and stone of Portal de ses Taules from the Renaissance city walls of Eivissa (16th century) were characterized using thermal analysis— thermogravimetry and derivative thermogravimetry (DTG)—x-ray diffractometry, and scanning electron microscopy. The granulometric fraction of particle size <63 μm was selected as representative of the binder, while the fraction 0.5–1 mm was taken as representative of the aggregate in order to characterize mortar samples. The results show that local materials were used. Lime was the main component of most of the samples tested. Thermal analysis revealed the hydraulic nature of the lime mortars. High amounts of sodium chloride were found in the samples analysed.     

Clarifying prehistoric parasitism from a complementary morphological and molecular approach

This paper reports an approach to the identification of prehistoric parasitic infection, which integrates traditional morphological methods with molecular methods. The approach includes the strengths of each method while mitigating the limitations. Demonstrating the efficacy of this approach, we provide a case study from a 1400 year old desiccated fecal sample from La Cueva de los Muertos Chiquitos, archaeological site, near Rio Zape, Durango, Mexico. Traditionally prepared microscope slides were processed via microscopy and tentative ascarids were identified. Information regarding the parasites' developmental stage was recorded. DNA was then extracted directly from the slide material. From this DNA extract, a small segment of the 18S ribosomal RNA gene variant that is specific to Ascaris, and its phylogenetically close relatives, was targeted for PCR amplification and sequencing. Phylogenetic analysis of the DNA sequence best matched a member of physalopterids, rather than ascarids, with a single exception of a match to Contracaecum spiculigerum. Subsequent extractions, amplifications and sequencing of the original rehydrated coprolite material confirmed these results. The C. spiculigerum sequence represented a phylogenetic anomaly and subsequent analysis determined the sequence was an error in the BLAST database, likely attributable to misidentification of juvenile specimens prior to sequencing and submission. Physaloptera are a difficult genus to identify morphologically and can carry major health burdens. They may be underreported in humans, in part, because of morphological similarities to the more common human parasites belonging to ascarids. We conclude that integrating traditional morphological methods with molecular methods can help resolve this issue, in both contemporary and prehistoric populations.     

Chemical analysis of 17th century Millefiori glasses excavated in the Monastery of Sta. Clara-a-Velha,Portugal: comparison with Venetian and façon-de-Venise production

A set of ten Millefiori glass fragments dating from the 17th century, originated from archaeological excavations carried out at the Monastery of Sta. Clara-a-Velha (Coimbra, Portugal), were characterized by X-ray electron probe microanalysis (EPMA), Raman microscopy and UV–Visible absorption spectroscopy. All glasses are of soda-lime-silica type. The use of coastal plant ash is suggested by the relatively high content of MgO, K₂O and P₂O₅, as well as by the presence of chlorine. Tin oxide or calcium antimonate were the opacifiers used in the opaque glasses, cobalt in the blue glasses, copper in the turquoise glasses, iron in the yellow and greenish glasses, and iron and copper were found in the opaque red and aventurine glasses. Based on the concentrations of alumina and silica four different sources of silica were identified, allowing the classification of the glasses into the following compositional groups: low alumina (<2 wt%), which includes a sub-group of cristallo samples with SiO₂ > 70 wt%, medium alumina (2–3 wt%), high alumina (3–6 wt%) and very high alumina (>6 wt%). Comparison with genuine Venetian and façon-de-Venise compositions showed that two fragments are of Venetian production, one of Venetian or Spanish production and the remaining are of unknown provenance. In two fragments the glass of the decoration is probably Venetian or Spanish but the glass used in the body is also of unknown provenance.     

Reflections into Ptolemaic glass: Colorless,white, blue,and green inlays from the workshop of Tebtynis

Inlays range among the most aesthetically pleasing and technically challenging glasses produced in the Ptolemaic period. Despite the central role of this phase in the history of glass technology, little is known about the recipes and the technological knowledge of the Egyptian artisans. This paper will thus focus on the study of the materials from the secondary workshop of Tebtynis (Fayum oasis, Egypt). We report the first multi-methodological study comprising textural, chemical, and mineralogical analyses (optical microscopy, scanning electron microscopy coupled with energy-dispersive system, electron probe microanalysis, and μ-Raman spectroscopy) on a set of 81 colorless, white, blue, and green samples carefully selected among the 800+ glasses from the craft area now stored at the Museo Egizio, Turin (Italy). Our study offers the biggest compositional database of well-dated Ptolemaic glasses currently available in the literature, highlighting some interesting novelties regarding the silica and alkali sources, and the coloring and opacifying techniques employed. The results suggest a specialized craft of traditional origin, but open to innovation and experimentation, as expected from transitional phases.     

A multi-analytical approach to characterize an Early Bronze Age cosmetic material from Müslümantepe,Southeastern Anatolia

The present paper reports the chemical and mineralogical composition of a black pigment material contained in a Syrian Bottle-shaped vessel excavated on an Early Bronze Age grave in Müslümantepe, a site located at the right bank of the Tigris River in Southeastern Anatolia. A combination of different analytical tools like state-of-the-art non-destructive μ-XRD², μ-XRF and μ-Raman spectroscopy compared to classical powder XRD was used to characterize the content of the bottle. The results attest the presence of a manganese mineral (pyrolusite) most probably used for cosmetic purposes. This is the first evidence, which is scientifically tested, of the earliest use of cosmetics in the Upper Tigris of Southeastern Anatolia during the Early Bronze Age period, c. 2700–2550 bc.     

Stable isotope analysis of dog,fox, and human diets at a Late Holocene Chumash village (CA-SRI-2) on Santa Rosa Island,California

Stable carbon (δ¹³C) and nitrogen (δ¹⁵N) isotope analyses of dog (Canis familiaris), island fox (Urocyon littoralis), and human bone collagen from CA-SRI-2 (AD 130–1830) on Santa Rosa Island, California provide a proxy of diet and the relationships between humans and these animals. Carbon isotopic signatures indicate that Native Americans and their dogs at CA-SRI-2 subsisted almost exclusively on marine resources, while the island fox ate primarily terrestrial foods. Nitrogen isotopes and archaeofaunal remains indicate that humans and dogs also ate higher trophic level foods, including finfishes, marine mammals, and seabirds with smaller amounts of shellfish. The CA-SRI-2 island foxes appear to have eaten higher amounts of terrestrial foods, similar to the diets observed in modern fox populations. These data generally confirm the commensal relationship assumed to exist between domesticated dogs and people, but the carbon isotopic composition of dogs is enriched ∼2‰ compared to humans. We hypothesize that the difference in carbon isotopes between dogs and humans may have resulted from a higher consumption of C3 plants with lower δ¹³C values by humans, or less likely from the ingestion by dogs of significant amounts of bone collagen, which is enriched by ∼4‰ over associated muscle.     

A longitudinal study of tooth growth in a single individual based on long- and short-period incremental markings in dentine and enamel

Ground sections of teeth from a single individual revealed approximately 30 fluorescent lines in the dentine resulting from successive courses of tetracycline antibiotics given over a period of approximately 12 years. In addition, many teeth showed long-period incremental markings in the dentine. Short-period daily cross-striations in the enamel were used to calculate the periodicity of the long-period incremental lines in both enamel and dentine. The incremental markings in the dentine were then used to calibrate the time of administration of each of the courses of tetracycline antibiotics. Enlarged micrographs of the teeth, constructed using fluorescence microscopy, were used to measure the increase in height of different teeth throughout the growth period on each occasion the tetracycline antibiotics were given. The times of initial mineralization of the teeth and the duration of crown formation were also determined for each tooth section. Line plots of tooth height against age were computed and used to calculate the rate of increase in tooth height during crown and root formation for one example of each tooth type. Initial rates of increase in height during enamel apposition and coronal dentine formation were fast, between 10 μm and 14 μm per day. During the latter phase of crown formation and during early root formation, tooth height increased at a slower rate of between 4 μm and 6 μm per day. Rates of increase in tooth height then rose to between 13 μm and 26 μm per day during the second half of root formation before falling off to a rate of approximately 4 μm per day during root completion (as the root apex formed). The times of initial crown mineralization and the total crown formation times estimated in this individual were all within the range known for modern humans but there was comparatively early mineralization of the third permanent molar. These findings are discussed in the context of other studies on human dental development.     

Plant microfossil analysis reveals disturbed forest and a mixed-crop,dryland production system at Te Niu,Easter Island

Plant microfossil analysis was carried out on 12 soil samples from a variety of landscape features at three locations (100–250 m a.s.l.) along a 950 m transect at Te Niu, Easter Island. Pollen and phytolith assemblages were dominated by palms and ground ferns, and suggested disturbed forest. We identified pollen of bottle gourd (Lagenaria siceraria) and starch grains of the common yam (Dioscorea alata), sweet potato (Ipomoea batatas) and taro (Colocasia esculenta). The data suggest a mixed-crop, dryland production system at Te Niu dominated by yam and sweet potato, and supplemented by taro and bottle gourd. The data provide direct evidence of crop type and range, supporting the indirect evidence (topographic and landscape features, field and historical research, comparisons with elsewhere in the Pacific) that much of the rock covered landscape of Easter Island was used for intensive horticulture.     

The Firing Temperature of Pottery from Ancient Mesopotamia,Turkey, Using Luminescence Methods: A Case Study for Different Grain‐Size Fractions

The assessment of the firing temperature of a prehistoric pottery sample collected from ancient Mesopotamia, Turkey was studied using luminescence techniques. The methods for this estimation involved the observation of the thermal and pre‐dose sensitization with various re‐firing temperatures for both TL and the OSL signals. In the former case, the 110°C TL peak and the rest of the glow curve were used as proxies in this study. In the framework of a first attempt to investigate the impact of grain‐size dependence on the sensitization of the luminescence signals, the aforementioned study was performed with four different pottery grain‐size fractions: (i) less than 60 μm, (ii) 60–90 μm, (iii) 90–180 μm and (iv) 180–250 μm. The results clearly demonstrated the firing temperature mark of ～500°C in for the grain size of 90–180 μm, while—as in the case of the lower grain‐size fraction—a third proxy, the ratio of the pre‐dosed to the thermal sensitization, was seen to indicate the firing temperature. The remaining two grain‐size fractions failed to provide any meaningful results with regard to the firing temperature estimation. The dependence of the TL characteristics on the grain size was explained in the framework of the mixed mineralogy.     

An Archaeomagnetic Study of a Roman Bath in Southern France

Absolute Thellier–Thellier archaeointensity determinations were conducted on 137 tiles and sedimentary blocks from five different structures from the ‘Site de la Molère’, southern France, to constrain the archaeological interpretation of a relative age difference between structures and add new data to the French secular variation database. We present 89 new archaeointensity and 20 new directional results, with averages of 57 (±8) μT in the second century ad and 68 (±7) μT in the third century ad . The overall data trend is consistent with the limited available data, indicating rapidly increasing field intensity from the second to the third century ad .     

Morphological,chemical and physical changes during charcoalification of wood and its relevance to archaeological contexts

Wood exposed to a heat source can be transformed into charcoal if subject to conditions of carbonisation (in the absence of air) or charring (in restricted air). Charcoal recovered from archaeological sites can yield fundamental information to our understanding of human economic and cultural development over time and (ecological) setting. This work describes the morphological (anatomy, degree of shrinkage), physical (reflectance) and chemical (elemental, molecular composition) properties of charcoal in relation to heat source and wood variables. In this study charcoal and charcoal fuel were experimentally produced whereby temperature (160–1200 °C), time of exposure (2–1440 min), heating rate (high and low) and wood type (angiosperm and conifer) were varied. The results show that charcoal, often described as an inert, black material, has different chemical and physical properties in relation to the investigated variables. By using these different properties it is possible to distinguish between the different types of fires (domestic and industrial) exploited by humans in the past. Morphological analyses and reflectance measurements are effective tools for this purpose and can be used in wood exposed to temperatures of 300 °C and above—temperatures which are relevant to archaeological research. Angiosperm and conifer wood react in different ways when exposed to heat and thus the taxonomic identity of archaeological material needs to be known. Chemical analyses can be used for wood exposed to temperatures below 400 °C whereas elemental analyses of the carbon content can be used for wood exposed to temperatures up to a maximum of 650 °C.     

Starch grain characterization of Prosopis chilensis (Mol.) Stuntz and P. flexuosa DC,and the analysis of their archaeological remains in Andean South America

The fruit (pods) of Prosopis (Fabaceae) are frequently recovered from pre-Hispanic Argentinian archaeological sites, suggesting that this genus was of importance in ancient economies in this region. Yet it is only recently that archaeobotanists have begun to carry out systematic research into this genus. Therefore many questions remain to be addressed concerning the food value of Prosopis fruit, and its potential contribution. This paper examines starch from the pods of two species, Prosopis flexuosa and Prosopis chilensis, for the purposes of describing and classifying their morphological features and biometrical parameters. Pods of both species were gathered from two extremes (northern and southern) of the Hualfín Valley, Catamarca, Argentina. Starch abundance is estimated and compared with that of Zea mays, an economically important plant with high concentrations of starch. This paper reveals that Prosopis pods contain very low amounts of starch compared to starch-rich edible species. Despite this, the recovery of Prosopis starch grains can be successfully used to assess archaeological tool uses. Prosopis starch grains were found to be highly variable in shape. Grain size ranged between 10 and 20 μm. Granule irregularity and the high birefringence under polarized light are two of the most important diagnostic features. No significant statistical differences were found in the structure (morphology, size and hilum) of the starch of the same species from both localities. Finally, the implications for the role of this plant in past societies are discussed.     

Provenance of marble sculptures and artifacts from the so-called Canopus and other buildings of “Villa Adriana” (Hadrian's villa – Tivoli,Italy)

The results of a minero-petrographic and isotopic study carried out on the marbles of statues and architectural elements belonging to several buildings on the “Hadrian's Villa” site (the so-called Canopus, the Peschiera, the Sala dei Pilastri Dorici and the Serapeum) are presented here as part of an ongoing archaeometric project which considers the determination of the provenance of all the marble decorations of the Villa complex. Analytical data indicate the prevailing presence of marmor lunense and the use of Pentelic and Thasian marbles for architectural elements in a few parts of the Sala dei Pilastri Dorici, the Peschiera and the Serapeum; no significant use is made of Proconnesian marble, probably the most inexpensive of the time. Analysis of sculptures from the Canopus showed that those of the Tiber and Nile gods were made of Parian marble, the Caryatids and Telamons of Pentelic marble and the Amazons of the precious white Dokymaean marble.     

Locally diagnostic phytoliths of wild rice (Zizania palustris L.) from Minnesota,USA: comparison to other wetland grasses and usefulness for archaeobotany and paleoecological reconstructions

Wild rice (Zizania spp.) is an important native grain of north-central North America, with spiritual and subsistence significance to many native peoples. Due to lack of suitable proxies, its past distribution and pattern of use are poorly known. This study demonstrates the diagnostic value of silica phytoliths from Z. palustris as a proxy tool to detect its past occurrence in a variety of paleoenvironmental and archaeological contexts. Our main findings are: 1) Dominant wetland grass species in Minnesota produce phytoliths distinct from Zizania phytoliths; 2) Closely related Leersia oryzoides produces a few Zizania-like phytolith morphotypes; however, these potential confusers can be identified based on 2-D and 3-D morphologies; 3) Z. palustris produces a wide variety of phytolith morphotypes, many of which are only found in certain parts of the plant (e.g., Inflorescence Type 1 from the spikelet); 4) Z. palustris produces 23 locally diagnostic phytolith morphotypes that can be used to determine the presence and abundance of wild rice in modern and paleo lake sediments; and 5) Wild rice phytolith Inflorescence Type 1 is the morphotype most likely to be observed in archaeological contexts, and may be unequivocally diagnostic for the genera Zizania.     

Chemical characterisation of anthro-technosols from Bronze to Middle Age in Bologna (Italy)

The aim of this research was the understanding of a peculiarly expanded soil sequence in Bologna (i.e., Roman Bononia, Etruscan Felsina), one of the most important archaeological poles for Etruscan colonisation and settlement in northern Italy. The uppermost part of the chronological sequence dating from the Bronze Age up to medieval and modern times was analysed for the first time from geochemical and pedological viewpoints. The integration of archaeological, stratigraphical and pedological data supported by soil chemical analysis, a fundamental key for reconstructing a correct evolutionary sequence, made it possible to recognise seventeen buried Soil Units (ancient Technosols, Anthrosols and Cambisols) characterised by different kinds and degrees of intensity of anthropogenic influence. In some cases, the results show a relatively severe element concentration (Cu, Sn) mainly characterising the Iron Age (Etruscan and Villanovan) stratigraphic units, representing an ancient industrial pollution linked to local dispersal of melting activity dump products generated in near-site surrounding areas. Therefore, a comparison was possible between natural blank and anthropogenically polluted geochemical values for some local soils.     

Savoury Recipes and the Colour of the Tlatelcomila Human Bones

Bones from Tlatelcomila (Tetelpan, México D.F.) were characterized by several complementary physical and chemical techniques, such as X‐ray diffraction, scanning electron microscopy, transmission electron microscopy, atomic force microscopy, energy‐dispersive spectroscopy and ultraviolet spectroscopy, to determine whether they were boiled or grilled. The usual correlation between thermal treatment and colour is revisited in terms of microscopic structure, morphology and texture. At temperatures less than 100°C, it is shown that colour depends not only on temperature or diagenesis but also on the cooking procedure; that is, on the presence of spice dyestuffs such as axiote (Bixa orellana) or chilli (Capsicum).