A SCIENTIFIC INVESTIGATION ON THE PROVENANCE AND TECHNOLOGY OF A BLACK‐FIGURE AMPHORA ATTRIBUTED TO THE PRIAM GROUP*

The restoration of a Greek black‐figure amphora provided an opportunity to study the provenance and production technology of the vase. The composition of the ceramic body, determined by inductively coupled plasma optical emission spectroscopy (ICP–OES), matches that of Attic products. Investigation by X‐ray diffraction and reflectance spectroscopy suggests a maximum firing temperature around 900°C and a body re‐oxidation temperature around 800°C, respectively. The morphology and composition of black, red and dark red surface areas were studied by scanning electron microscopy and X‐ray energy‐dispersive analysis; the black areas show the features of a typical well‐vitrified black gloss, while the red areas were most probably obtained by simple burnishing of the body; the dark red additions, on the other hand, are the likely result of a partial re‐oxidation of a clay–ochre mixture.     

The Study of Attic Black Gloss Sherds using Synchrotron X-ray Diffraction

We have studied the mineral composition of the gloss and the ceramic body of three pieces of Attic Greek pottery by applying the technique of high-resolution powder diffraction using synchroton X-rays. The measurements were performed on Stations 2·3 and 9·1 at the Synchrotron Radiation Source, Daresbury Laboratory. High quality powder patterns from the bulk of the ceramics and from the gloss surfaces have been obtained. The diffraction results show interesting variations of mineral composition between the gloss of the different sherds as well as variations between the bulk and the gloss. This makes phase identification and comparison between different fabrics less ambiguous. Spinel minerals are present in the gloss which are absent in the main body of the ceramics. Diffraction lines from one surface match the patterns of hematite, magnetite/maghemite and hercynite, while solid solutions of spinel structures appear to be present in the gloss layer of another sample. Crystallite particle sizes and lattice parameters of the minerals in the gloss layer have been accurately determined. Supplementary scanning electron microscopy (SEM) reveals the gloss thickness to be approximately 20 μm but with variations down to 5 μm. Analysis of the diffraction profile for the hematite component reveals a particle size in the order of 0·027 μm.     

Black Gloss Pottery: Production Sites and Technology in Northern Etruria,Part I: Provenance Studies

The object of the present study is an assemblage of 149 black gloss pottery samples found in northern Etruria (Tuscany, Italy), at Arezzo, Volterra, Chiusi and Populonia. Complete chemical analyses have been performed for the whole set of samples, whereas mineralogical characterization has been provided for most of the Volterra, Chiusi and Populonia samples. The Chiusi‐Marcianella production site has been the further object of a detailed study aimed at the creation of a complete reference group. Moreover, several trade routes have been reconstructed, shedding light on the import and export of these ceramics from inland Etruria to the coast and vice versa.     

The Belgammel Ram,a Hellenistic‐Roman Bronze Proembolion Found off the Coast of Libya: test analysis of function,date and metallurgy,with a digital reference archive

The Belgammel Ram was found off the coast of Libya in 1964, and examined during 2008–9. The following techniques were used: surface non‐contact digitizing using a laser scanner, reflectance transformation imaging using polynomial texture mapping and hemi‐spherical harmonics, digital photogrammetry with dense surface modelling, structured light optical scanning, and X‐ray fluorescence analysis. For internal structure the ram was examined by X‐radiography and 3‐D X‐ray tomography. Metallurgical composition was studied by micro‐drilling and subjecting the samples to scanning electron microscope X‐ray micro‐analysis, micro X‐ray fluorescence and X‐ray backscatter. The lead isotope composition was analysed. The alloy has average percentage composition Cu = 86.9, Sn = 6.3, Pb = 6.6, and Zn = < 0.10. The Belgammel Ram is probably a Hellenistic‐Roman proembolion from a small military vessel or tesseraria. The archived data are at the Faculty of Engineering and Environment, Engineering Sciences, Material Data Centre, University of Southampton ( muvis@soton.ac.uk ).     

COLOURED OPAQUE GLASS BEADS OF THE MEROVINGIANS*

Monochrome coloured opaque glass beads of the Merovingians have been examined by different analytical methods. A large number of mostly unprepared beads have been measured by X‐ray fluorescence analysis. X‐ray diffraction was used for the identification of the crystalline colouring and opacifying pigments, and electron probe micro‐analysis as well as scanning electron microscopy were applied to study the composition and the microstructure of a white, brown, green, orange and yellow glass bead. After subtracting the content of colouring oxides of the glass beads and normalizing the residual values to 100% an identical soda‐lime‐glass matrix was obtained. The origin of the colouring metal oxides is discussed.     

The production and technology of glazed ceramics from the middle ages,found in the saepinum territory (Italy): a multimethodic approach*

A collection of ceramics from the Middle Ages found in Altilia and Terravecchia (the Saepinum area, Campobasso, Italy) were characterized by using different mineralogical analyses to investigate their provenance and production techniques. The body ceramic was investigated using Rietveld phase analysis of X‐ray powder diffraction patterns, X‐ray fluorescence spectrometry and scanning electron microscopy. The chemical compositions of the coatings were measured by scanning electron microscopy and their mineralogical compositions were determined using a particular technique of X‐ray small‐angle scattering (SAS) optimized for studies of thin films. Moreover, the material used for decoration was studied using micro‐Raman spectroscopy. The archaeometric results confirmed the distinction into two different ceramic classes, already individuated from archaeological analysis: the Altilia objects belong to the protomajolica class, whereas the objects from Terravecchia are RMR (ramina‐manganese‐red) ceramics. A comparison between the chemical and mineralogical compositions of good‐quality ceramic objects and those of waste products indicated local production of the ceramics. A sharp distinction was found in the chemical composition of the coatings: the Altilia products have tin‐opacified lead glazes, while the Terravecchia ones have transparent high‐lead glazes. Among the Altilia products, the unsuccessful process that produced a large quantity of discarded materials was attributed to the high lead content of the glazes. In fact, the principal advantage of the high lead content was to make the preparation and application of the glaze suspension easier, but the risk of reduction of lead oxide to metallic lead was greatly increased. Using micro‐Raman spectroscopy, the following minerals were identified as pigments: pyrolusite for the dark colour, malachite for green, lepidocrocite for yellow and hematite for red.     

DISCOVERY AND CHARACTERIZATION OF AN UNKNOWN BLUE‐GREEN MAYA PIGMENT: VESZELYITE*

Blue‐green mosaic and polychrome masks and funerary offerings from the royal tombs of Calakmul, Mexico, were analysed by scanning electron microscope equipped with energy dispersive X‐ray spectroscopy (SEM‐EDS), X‐ray diffraction (XRD), and particle induced X‐ray emission (PIXE). This led to the first identification of the use of veszelyite, a rare hydrated copper‐zinc phosphate, as green pigment. Analyses of a geological sample of this mineral have been done to confirm the characterization of this Mayan pigment, which might help determine pre‐Columbian trade routes of precious and luxury objects in the ancient Maya Classic period (ad 250–800).     

Studying the process of enamel powder preparation for émail champlevé by colour measurements and μ‐X‐ray mappings

Colour measurements and non‐destructive μ‐X‐ray mappings have been used for the first time in a comprehensive study of medieval émail champlevé works from different production areas in France and Germany. This approach has given a new insight into the enamel powder preparation process of the glass material used for enamelling. Colour measurements demonstrated that all production centres used glass of very similar hues, but with large differences in colour saturation. The μ‐X‐ray mapping results of blue enamels are described by a semi‐qualitative approach. Significant variations in oxide contents of lead, cobalt, manganese and antimony oxides were found. The variations suggest that more than one glass material was used to prepare the powder for enamelling. The variations in antimony and cobalt show that glass had different degrees of opacity and colour depth. The manganese and lead contents, which do not correlate with the cobalt or antimony contents, indicate that probably glass of different base compositions was used to prepare the enamel powder for one champlevé field.     

CHARACTERIZATION OF ARCHAEOLOGICAL AND IN SITU SCOTTISH WINDOW GLASS

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.     

NORTH APULIAN COARSE WARES AND FINE PAINTED WARES: A REAPPRAISAL ACCORDING TO NEW DATA FROM HERDONIA AND CANUSIUM

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.     

COOKING AND PAINTED WARE FROM SAN GIUSTO (LUCERA,FOGGIA): THE PRODUCTION CYCLE,FROM THE SUPPLY OF RAW MATERIALS TO THE COMMERCIALIZATION OF PRODUCTS*

Archaeological excavation at the San Giusto site (Lucera, Italy) has unearthed a Late Antique kiln that was most certainly dedicated to the production of cooking ware. An archaeometric study of numerous specimens of cooking and painted ware found at this site was carried out using optical microscopy, scanning electron microscopy, micro‐Raman spectroscopy, X‐ray diffraction, X‐ray fluorescence, inductively coupled plasma mass and optical emission spectrometry and instrumental neutron activation analysis. The integration of historical–archaeological data with archaeometric data has revealed that these specimens can be attributed to the San Giusto site. Furthermore, the production cycle of this ware can thus be reconstructed: from the diversified supply of raw materials (fluvial and marine sediments), to the relatively complex preparation of the paste, to firing at variable temperatures (600–750°C for cooking ware; 850–1050°C for painted ware).     

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.     

PAUL‐LOUIS CYFFLÉ'S (1724–1806) TERRE DE LORRAINE: A TECHNOLOGICAL STUDY

Fragments of four Terre de Lorraine biscuit figurines were subjected to porosity analysis, X‐ray fluorescence analysis, X‐ray diffraction analysis, backscattered‐electron image analysis—coupled with energy dispersive spectrometry—and electron backscatter diffraction analysis to determine the porosity, bulk, major, minor and trace element compositions, and the composition and the proportion of their constituent phases. Cyfflé's Terre de Lorraine wares embrace two distinct types of paste, a calcareous and an aluminous–siliceous one. Both are porous (9–25% water adsorption). The former consists of a mixture of different proportions of ground quartz or calcined flint, ground Pb‐bearing glass and calcium carbonate with a refractory clay. The firing temperature was between 950 and 1050°C. For the latter, Cyfflé mixed ground pure amorphous SiO₂, ground quartz or calcined flint, ground porcelain, ground Na–Ca‐glass and coarse‐grained kaolinite with a fine‐grained kaolinitic clay. The figurines were fired below 1000°C. The result was a porous, hard paste porcelain‐like material. Cyfflé's recipes for both pastes can be calculated from the chemical and the modal analyses.     

THE TECHNOLOGY OF ‘GLAZED’ RESERVED SLIP WARE—A FINE CERAMIC OF THE HARAPPAN PERIOD*

‘Glazed’ Reserved Slip Ware (RSW) is a high‐quality glossy bichrome pottery of the Indus Valley civilization, and dates to the mature Harappan period (c. 2600–1900 bc ). Scanning electron microscopy with energy‐dispersive X‐ray analysis indicates that the surface coat on RSW is composed of a pale grey vitrified clay slip, which overlies a black slip with significantly higher iron oxide. Hence the term ‘sintered’ Reserved Slip Ware is to be preferred. X‐ray diffraction analysis indicates that both the pale and black slips contain hercynite, mullite and quartz, but observation by scanning electron microscopy shows that the black slips contain higher amounts of coarser‐grained hercynite. The elemental data suggest that different clays were used to make the bodies and the slips. However, key element ratios are very close in associated black and pale slips. The grey slip may have been produced by elutriation of the fine, iron oxide‐rich clay that was used to prepare the black slip. The pale grey slip was laid over the black and removed by combing to produce a bichrome effect, which evoked semi‐precious materials such as agate. RSW was a specialist product that required significantly higher input skill and resources than the majority of Harappan clay‐based ceramics. It is a further example of the range of sophisticated Harappan ceramic wares, which included faience, fired steatite and stoneware.     

PETROGRAPHIC AND CHEMICAL CHARACTERIZATION OF POTTERY PRODUCTION OF THE LATE MINOAN I KILN AT HAGHIA TRIADA,CRETE*

Pottery from the Late Minoan I kiln at Haghia Triada in the Mesara Plain, southern Crete, was analysed by a range of techniques, comprising thin‐section petrography, scanning electron microscopy, X‐ray diffraction, X‐ray fluorescence and neutron activation analysis. The project characterizes the ceramic fabrics and probable raw materials, correlates paste recipes with shape, reconstructs the firing conditions of the kiln and establishes a chemical reference group, taking into account post‐burial alteration and contamination. Comparison of the reference group formed with that from the neighbouring, broadly contemporary, kiln at Kommos shows an unexpected differentiation of the two kilns.     

WASTE GLASS,VESSELS AND WINDOW‐PANES FROM THAMUSIDA (MOROCCO): GROUPING NATRON‐BASED BLUE–GREEN AND COLOURLESS ROMAN GLASSES

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 (R oman B lue–G reen and Y ellow 1) and RBGY 2 (R oman B lue–G reen and Y ellow 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 (R oman‐C olourless) 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.     

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.