An Iron Age ceramic sequence from the Bayt Bin Ati,al‐Ain,UAE

Rescue excavations associated with the adaptive reuse of a historic building in the Qattara Oasis revealed a 5 m stratigraphic sequence spanning the past 3000 years. The main period of occupation—roughly half the sequence—belongs to the Iron Age II and III periods (c.1100–300 BC). Evidence of agriculture and industry was found which complements our understanding of the well‐known Iron Age settlements of al‐Ain. The present paper sets out the stratigraphic sequence and presents the phased ceramic assemblage, before considering the broader implications for the archaeology of Iron Age south‐east Arabia.     

UNIQUE PRE‐ROMANESQUE MURALS IN KOSTOĽANY POD TRÍBEČOM,SLOVAKIA: THE PAINTING TECHNIQUE AND CAUSES OF DAMAGE

Pre‐Romanesque murals at Kosto?any pod Tríbe?om, 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.     

SCIENTIFIC ANALYSIS OF SEVENTH‐CENTURY GLASS FRAGMENTS FROM THE CRYPTA BALBI IN ROME*

Inductively coupled plasma emission spectroscopy, reflectance spectroscopy and X‐ray diffraction were used to study seventh‐century AD glass fragments from the Crypta Balbi in Rome. All the samples were found to be silica‐soda‐lime glasses. Iron determines the colour of blue‐green, green and yellow‐green transparent glasses; chemical composition suggests deliberate addition of iron and/or manganese in about half the samples. Copper was found as the main colourant in red, pale blue and blue‐green opaque fragments; elemental copper acts as an opacifier in red glass, and calcium antimonate in white, pale blue and blue‐green glasses. Detection of antimony in transparent fragments suggests recycling of opaque mosaic tesserae.     

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).     

A CASE STUDY OF ARTHROPODS PRESERVED ON ARCHAEOLOGICAL BRONZES—MICRO‐ARCHAEOLOGICAL INVESTIGATION HELPS RECONSTRUCTING PAST ENVIRONMENTS

This paper offers new perspectives for improving our knowledge of arthropods in wet and aerobic archaeological contexts. The very‐near environment of uncleaned buried bronze artefacts, two ronde‐bosse ornaments of a Celtic grave from the Iron Age (275 to 250 bc , La Fosse‐Cotheret, Roissy‐en‐France), was studied by means of optical and scanning electron microscopies. Taking into account recent knowledge on bronze corrosion (decuprification), this micro‐investigation (micro‐archaeology) allowed identification of two fossilized arthropods—Cryptophagus sp. (Insecta, Coleoptera, Cryptophagidae) and Coccotydaeolus sp. (Acari, Tydaeoidea, Iolinidae)—which sheds some light upon the complex taphonomic process that occurred after the burial of a Celtic chariot. These first results support the idea that the local corroded metal/soil system has to be investigated for a better understanding of archaeological microenvironments. Efficient minute investigation of soiled bronzes could be performed prior to systematic cleaning of artefacts.     

CLIMATE FORCINGS AND THEIR INFLUENCE ON ALPINE HISTORY AS RECONSTRUCTED THROUGH THE APPLICATION OF SYNCHROTRON‐BASED X‐RAY MICROFLUORESCENCE ON LAYERED STALAGMITES*

Solar variability and volcanic activity strongly interact with climate and the environment. Synchrotron radiation X‐ray microfluorescence (micro‐XRF) to an annually laminated Alpine stalagmite confirmed that annual laminae result from hydrological variability and changes in the duration of soil microbial degradation. The latter is modulated by solar variability. At the centennial timescale, growth rate and solar activity appear to be correlated with temperature change, with low temperatures at solar minima. By combining micro‐XRF and absorption spectroscopy techniques (XANES), we also found that speleothems are a new archive of aerosol sulphate related to volcanic activity. Peaks in S‐concentration from c. 5.2 to 5.0 ka bp in an Alpine stalagmite suggest that multiple volcanic sulphate aerosol emissions enhanced Mid‐Holocene summer cooling, thus favouring the preservation of the Alpine Iceman mummy in a persistent ice casket.     

REGIONAL VARIATIONS IN BLOOMERY SMELTING SLAG OF THE IRON AGE AND ROMANO‐BRITISH PERIODS*

This study highlights regional variation in the composition of iron‐smelting slag produced in England prior to the medieval period and attempts to link slag composition to the type of ore smelted. For many sites, the slag compositions were consistent with the use of limonite ore, but there is evidence that siderite ore was smelted at sites in Sussex in the late Iron Age/Romano‐British periods. A compositional comparison of smelting slags and slag inclusions in Iron Age currency bars, using data from Hedges and Salter (1979 ), illustrates the potential of smelting slag compositional data in provenance studies of early iron objects.     

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 CHEMICAL COMPOSITION OF SOME ARCHAEOLOGICALLY SIGNIFICANT FLINT FROM DENMARK AND SWEDEN

Flint was one of the most widely employed raw materials for artefact manufacture in Denmark and Sweden during the Stone Age, and it continued to be used during subsequent periods. Prehistoric flint mining and lithic manufacturing studies in these countries have attracted considerable attention, but there have been no recent attempts to chemically characterize the geological source materials. This paper builds on a pilot study ( Hughes et al. 2010 ) and uses energy‐dispersive X‐ray fluorescence (EDXRF) analysis to determine quantitative composition estimates for nine major, minor and certain trace elements in seven archaeologically significant flint sources in Denmark and Sweden, along with new data on a number of other sources of prehistoric significance. These data provide a geochemical foundation for ongoing research devoted to determining contrasts and continuities in the time and space utilization of flint sources in Scandinavian prehistory.     

Coloured Prints of the 16th Century: Non‐Destructive Analyses on Coloured Engravings from Albrecht DÜrer and Contemporary Artists

Qualitative investigations of pigments and dyes using micro X‐ray fluorescence spectrometry (micro‐XRF) and visible spectrophotometry (VIS) are suitable non‐destructive methods for the characterization of different colorants in art objects. In this study, several rare coloured engravings from the work of Albrecht Dürer—and, in addition, from the work of Cornelis Cort, Servatius Raeven and Johannes Sadeler—were investigated. The analyses result in specific palettes of colours that were used by different artists or in different workshops for the coloration of engraved images. Starting from these different palettes, it is possible to distinguish coeval colorations that were added in the 16th century from those that were carried out at a later date (e.g., the 19th century).     

THE FIRST ARCHAEOMETRIC CHARACTERIZATION OF ROMAN MILLSTONES FOUND IN THE AQUILEIA ARCHAEOLOGICAL SITE (UDINE,ITALY)*

An archaeometric study of all the Roman millstones preserved today in the National Archaeological Museum of Aquileia, the ancient capital of the X Regio Augustea –‘Venetia et Histria’ located on the Friuli plain (northeastern Italy), has been recently envisaged to define their geological–geographical provenance. We present here the results of the first step of the research, which is aimed at characterizing all of the definitely allochthonous lithologies. In order to carry out petrography on thin‐section and geochemical analyses, 10 small samples were picked out directly from Pompeian‐style millstones (catilli and/or metae) and rotary querns. Five different lithologies originating in various Italian regions were recognized: eight samples consist of pale‐ and dark‐grey lavas from the Venetian Volcanic Province, Vulsini Volcanic District (Latium), Etna Volcano and Pantelleria island (Sicily), whereas two samples were shown to be made of green garnet‐bearing schists (pietra ollare) from the Western Italian Alps. The presence of Alpine pietra ollare in northeastern Italy, used to produce pots and food containers, was established for numerous classical findings at Roman and Middle Age sites, but the analysed items represent the first evidence for the utilization of this kind of stone to produce mills during the Roman epoch.     

NATURE AND MICROSTRUCTURE OF GALLIC IMITATIONS OF SIGILLATA SLIPS FROM THE LA GRAUFESENQUE WORKSHOP*

The red glaze (slip) that characterizes the Terra Sigillata potteries greatly contributed to their success during the Roman period. The colour of the slip can in fact be partially explained by the microstructure (crystalline phases, grain sizes) and the physico‐chemistry (composition) of the ceramics. However, the precise process and the diffusion of this technique are still not fully known. In particular, we do not know yet how the production of sigillata took place in the south of Gaul, and the role that was played by the production under Italian influence (pre‐sigillata) preceding the first local sigillata. In this work, a combination of transmission electron microscopy (TEM) and X‐ray synchrotron diffraction techniques was used to study the microstructure of pre‐sigillata slips from the main southern Gaul workshop (La Graufesenque), in order to compare their characteristics with those of high‐quality sigillata. These first results seem to indicate that the antique potters chose clays adapted to their firing conditions and to the type of coating that they wanted to make. These productions cannot be described as an initial phase for the later sigillata production and, rather, seem to correspond to the intention of developing a specific type of pottery only inspired by the famous Italian sigillata forms.     

THE HALLATON INGOT: SILVER IN IRON AGE BRITAIN

This article is a case study of the detailed contextual and scientific analysis of a single object, moving beyond a conventional object biography to consider flows of materials and shifts in meaning and value. The object is a simple triangular silver ingot from the Late Iron Age shrine site at Hallaton, Leicestershire, UK. Scientific analysis is used to uncover the biography of the ingot, and the raw materials from which it was created. The results suggest that the metal which eventually formed the ingot circulated through both Iron Age and Roman social networks, being reworked and transformed several times before it was deposited. Silver emerges as a material which mediated between the Mediterranean world and Iron Age communities in Britain, allowing translation and transmutation between different systems of value in conquest‐period Britain.     

ANALCIME CRYSTALLIZATION AND COMPOSITIONAL PROFILES—COMPARING APPROACHES TO DETECT POST‐DEPOSITIONAL ALTERATIONS IN ARCHAEOLOGICAL POTTERY*

The approaches of comparative studies and profile measurements, often used in order to detect post‐depositional alterations of ceramics, have been applied simultaneously to two sets of Roman pottery, both of which include altered individuals. As analytical techniques, Neutron Activation Analysis and X‐Ray Diffraction have been used. Both approaches lead to substantially different results. This shows that they detect different levels of alteration and should complement each other rather than being used exclusively. For the special process of a glassy phase decomposition followed by a crystallization of the Na‐zeolite analcime, the results suggest that it changes high‐fired calcareous pottery rapidly, and so fundamentally that the results of various archaeometric techniques can be severely disturbed.     

ANALYSING ARCHAEOLOGICAL BASALT USING NON‐DESTRUCTIVE ENERGY‐DISPERSIVE X‐RAY FLUORESCENCE (EDXRF): EFFECTS OF POST‐DEPOSITIONAL CHEMICAL WEATHERING AND SAMPLE SIZE ON ANALYTICAL PRECISION*

Energy‐dispersive X‐ray fluorescence (EDXRF) has been commonly used to determine geological sources of volcanic glass artefacts, but its ability to discriminate between basaltic sources is less developed. We examine the precision and accuracy of non‐destructive EDXRF for basalt artefacts by analysing varying size and weathering characteristics. The experiments identified no appreciable effect in reproducibility or measured composition due to thickness (down to 1 mm) or natural weathering of pre‐contact flake scars for the 17 elements measured in this study. Samples with surface area less than 100 mm², however, show significant variability in measured composition and reproducibility.     

A MULTI‐ANALYTICAL APPROACH FOR THE CHARACTERIZATION OF COMMODITIES IN A CERAMIC JAR FROM ANTINOE (EGYPT)*

This paper describes a multi‐analytical chemical study performed on the original, almost totally conserved, content of a small ceramic jar from the Antinoe archaeological site (fifth to seventh centuries ad, Roman Egypt) and now belonging to the archaeological collection of the Istituto Papirologico ‘Girolamo Vitelli’ (Florence, Italy). Scanning electron microscopy with an energy‐dispersive X‐ray spectrometer (SEM–EDX), Fourier transformed infrared spectroscopy (FTIR) and X‐ray diffraction (XRD) were all used to characterize the inorganic components of the archaeological material. The organic substances were analysed using FTIR, direct exposure mass spectrometry (DE–MS) and gas chromatography – mass spectrometry (GC–MS). The inorganic component essentially consisted of halite (NaCl). Among the NaCl crystals, lamellar elements were identified. They were chemically characterized by carbonato‐apatite and showed a concentric morphology typical of the scales of small fish. The most prevalent organic constituents of the sample were monocarboxylic acids, α,ω‐dicarboxylic acids, and cholesterol and its oxidation products. The organic material composition was consistent with the occurrence of lipids of animal origin. In addition, diterpenes related to pine pitch were also identified. The overall results suggest that the material recovered in the small ceramic jar found in Antinoe is a residue of fish‐based pickles such as garum, muria, allex and liquamen, which were commonly used in Roman times.     

DISCOVERY,PRODUCTION AND USE OF TIN‐BASED OPACIFIERS IN GLASSES,ENAMELS AND GLAZES FROM THE LATE IRON AGE ONWARDS: A REASSESSMENT*

Tin‐based opacifiers (lead stannate yellow and tin oxide white) were first used in glass production for a short period in Europe from the second to the first centuries bc , and then again throughout the Roman and Byzantine Empires from the fourth century ad onwards. Tin oxide was also used in the production of Islamic opaque glazes from the ninth century ad , and subsequently in enamels applied to Islamic and Venetian glasses from the 12th century ad onwards. A selection of published analytical data for the tin‐opacified glasses, enamels and glazes is summarized, and the methods used in their production are reassessed. The phase transformations occurring when mixtures of lead oxide, tin oxide and silica are fired are investigated with high temperature X‐ray diffraction (XRD) using a synchrotron radiation source, and these results are used to explain the observed differences in the glass, enamel and glaze compositions. Possible reasons for the use of tin‐based opacifiers in the second to first centuries bc , and for the switch from antimony‐ to tin‐based opacifiers in the fourth century ad are suggested, and the possible contexts in which tin‐based opacifiers might have been discovered are considered. The introduction of tin‐opacified glazes by Islamic potters in the ninth century ad is discussed in terms of technological transfer or independent invention.     

THE APPLICATION OF A PORTABLE X‐RAY FLUORESCENCE SPECTROMETER TO THE ON‐SITE ANALYSIS OF GLASS VESSEL FRAGMENTS FROM SOUTHERN THAILAND*

Ancient glass vessel fragments belonging to the seventh to ninth centuries ad , from the Ko Kho Khao, Laem Pho and Khuan Lukpad sites in southern Thailand, were studied. The glass vessel fragment samples are a collection belonging to the Department of Archaeology, the 15th Regional Office of Fine Arts of Thailand. The chemical compositions of the glasses were analysed using a modified portable energy‐dispersive X‐ray fluorescence spectrometer (OURSTEX 100FA‐II) by the introduction of a MOXTEK^® AP3.3 polymer window (5 mm²?) to the KETEK silicon drift detector for the measurement of light elements. The non‐destructive analysis was performed at the National Museum, Phuket, in Thailand. It is shown that the glass chemical compositions belong to mineral and plant‐ash based soda–lime–silicate glass. The origins of the glass artefacts are discussed in terms of raw materials and glass decoration, and compared with previously reported similar typological glasses from sites in the port city of Rāya and the Monastery of Wadi al‐Tur in Egypt.     

Roman traces in Germania magna: New thermoluminescence and pIRIR290 data from a lime kiln at Bergisch Gladbach,Germany

The applicability of a post‐infrared infrared stimulated luminescence (pIRIR₂₉₀) protocol and two different thermoluminescence (TL) protocols—a single aliquot regeneration (SAR) and a multiple aliquot additive dose (MAAD)—was tested on six polymineral fine‐grain (4–11 μm) samples extracted from the wall remains of a Roman lime kiln and a Roman roof tile. These remains had been excavated close to Bergisch Gladbach, which was at that time part of Germania magna. For the pIRIR₂₉₀ measurements, no dependence of D_e on first‐stimulation temperature was detectable, and the standard first stimulation temperature at 50°C was adopted. Fading tests and dose‐recovery tests were made for all samples. Background subtracted glow curves were recorded up to 480°C for TL after a preheat of 220°C for 120 s. A‐values were determined for all TL and pIRIR measurements. The results for all three protocols were fairly consistent, and TL and pIRIR₂₉₀ protocols are shown to be suitable to estimate reliable equivalent doses for the fired kiln walls. The resulting ages are in agreement with the expected time range—Roman Iron Age—and with independent age control provided by radiocarbon ages of animal bones and charcoal from the firing chamber.     

X‐RAY SUB‐MICRON TOMOGRAPHY AS A TOOL FOR THE STUDY OF ARCHAEOLOGICAL WOOD PRESERVED THROUGH THE CORROSION OF METAL OBJECTS

Wood preserved in the corrosion layer of two early medieval iron objects was examined using X‐ray tomography. A state‐of‐the art multi‐resolution X‐ray tomography set‐up ( http://www.ugct.ugent.be ) provided virtual cross‐sections of the archaeological wood samples at sub‐micron resolution. These were compared with scans of samples of similar modern wood. These scans demonstrate the power of sub‐micron X‐ray tomography for wood identification, although the process of mineralization pushes this technique to its limits. Furthermore, this technique facilitated appraisal of the mineral content of the archaeological wood, which is useful in selecting the most appropriate strategy for the (preventative) conservation of the archaeological object.