Characterization of Late Prehistoric Plasters and Mortars from Erimi – Laonin tou Porakou (Limassol,Cyprus)

Several plasters and mortars from the Middle Bronze Age site of Erimi – Laonin tou Porakou (Cyprus) were analysed in order to perform a technological characterization. Morphological (SEM), elemental (EDX), mineralogical (XRPD), petrographic (polarized OM, SEM–EDX), thermal (TGA) and spectroscopic (FT–IR) techniques were applied. Plasters and mortars were identified as pyrotechnological lime products, obtained using local raw materials and containing a moderate amount of spathic calcite fragments. The use of organic fibres was ascertained and a seminal use of a crumbled ceramic as additive was evidenced.     

Ceramic findings from the archaeological site at Aiano-Torraccia di Chiusi (Siena,Italy): a multi-analytical approach

In 2005, the remains of a Roman villa, dating from the early fourth to the sixth centuries ad, were discovered at the archaeological site of Aiano-Torraccia di Chiusi (Siena, Italy). After being abandoned in the sixth century ad, the complex was occupied by a group of Ostrogothic or Lombardic artisans in the period between the sixth and the seventh centuries ad. Many ceramic remains (coarse pottery and red slip ceramics) from the first to the seventh centuries ad have been discovered on this archaeological site. These findings have been analysed using different analytical techniques (optical microscopy (OM), X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscope-energy dispersive spectroscopy (SEM-EDS), attenuated total reflection Fourier transform infrared (ATR-FTIR), and micro-Raman in order to characterize the ceramic body, the coating, the temper, and to investigate the compositional relationship between the different kinds of ceramics. The use of different techniques on the same samples yielded information at different scales. OM and SEM-EDS yielded interesting information on the coarse pottery: the analyses performed on some minerals and rock fragments suggest that stone tesserae from the Roman villa (in the form of numerous marble fragments) were used in the production of this pottery. Bulk analyses (XRD and XRF) and subsequent micro-analyses (SEM-EDS, ATR-FTIR, and micro-Raman) of the red slip pottery revealed clear chemical, mineralogical and textural differences: some ceramics (the TCC sample group) typically have a Fe-enriched coating while others (the INGR sample group) present a clear difference in grain size but no chemical or mineralogical differences between the ceramic body and the coating.     

Archaeometric analysis of ceramic production in Tiwanaku state (c.500–1000 ce): An exploratory study

The chemical and mineralogical characterization of seven ceramic fragments produced within Tiwanaku state (c.500–1000 ce ) is reported. The instrumental techniques used included X‐ray elemental and mineralogical chemical analysis, Raman spectroscopy, and scanning and light microscopy. The results indicate there are several clay types, although they show similarities, such as the use of a plant‐based temper. The red colour of the decoration is hematite, and manganese oxides such as jacobsite are present in the black. The white colour is a mixture of gypsum and clay, and the orange is a mixture of hematite and clay. The use of colours, the quality of the clays and the temperatures reached during pottery firing point to expertise in ceramic production and to complex decision‐making processes. The multi‐elemental archaeometric approach documented here could become an important tool to shed a light on ancient ceramic technology and the internal variance of Tiwanaku pottery.     

STEEL FILES AS CHRONOLOGICAL MARKERS IN NORTH AMERICAN FUR TRADE SITES*

A selection of fragments of steel files excavated from dated western Canadian fur trade sites has been examined metallographically to assess their value as chronological indicators. It was possible in some, but not all, cases to identify the steelmaking process, distinguishing between cementation steel and crucible steel. In other file fragments manganese was detected in the steel both as manganese sulphide inclusions and in solution in the steel matrix. The identification of crucible steel provides a terminus post quem of 1740 for the fragment, and the presence of manganese a terminus post quem of about 1840. The site occupation dates were consistent with the dates deduced from the steelmaking technologies.     

LUSTRE-DECORATED CERAMICS FROM A 15TH TO 16TH CENTURY PRODUCTION IN SEVILLE*

A set of 17 fragments of ceramics have been uncovered on the occasion of excavations of a workshop in Triana near Seville. These ceramics are typical of objects that are not commonly encountered in present collections in spite of intensive production during the 15th–16th centuries. Chemical and mineralogical analyses have been performed using various techniques (X-ray fluorescence and diffraction, SEM, ion beam analyses). The majority of the ceramic sherds represent the diversity of the Seville production; three fragments recovered in the same archaeological context were not locally produced and belong to the production of eastern Spain (Valence area). The ceramic bodies of the Seville sherds are compatible with the use of clays from the Guadalquivir valley. The glaze and the lustre decoration are comparable to those produced in eastern Spain. These conclusions are based on data that represent the production of a single workshop in Seville; the scatter of the data is due to variations in the processing and/or to alterations during the five centuries of burial of the ceramic fragments.     

A STUDY ON LATE MEDIEVAL TRANSPARENT‐GLAZED POTTERY AND ARCHAIC MAJOLICA FROM ORVIETO (CENTRAL ITALY)*

Nineteen samples of medieval transparent‐glazed pottery and archaic majolica from Orvieto (central Italy) were studied. They were classified by archaeological criterion as follows: five transparent‐glazed fragments with green and brown decorations (first half of the 13th century), eight green transparent‐glazed fragments (13th century) and six tin‐glazed fragments with green and brown decorations (second half of the 13th century). SEM–EDX, XRD (the Rietveld method) and XRF were used to characterize the chemical and mineralogical compositions both of the bodies and the coatings. In all of the samples, the paste is Ca‐rich with CaO contents as high as 13–20 wt%. The mineralogical composition is compatible with a firing temperature of about 950°C, which is the typical temperature reached in a wood kiln. No difference was observed between the bodies of transparent‐ and tin‐glazed pottery. In the case of transparent glazes, the burial conditions lead to heavy weathering of the samples. However, on the basis of the analyses carried out in non‐weathered areas, the typical composition is PbO 55–65 wt%, SiO₂31–35 wt%. In tin glazes, the tin is scattered on the mass of the glaze as SnO₂crystals with a concentration of 7–14 wt%. Concerning the decorations, it is established that the green colour is due to the presence of copper, while manganese is responsible for the brown colour. These pigments, which represent the typical colours of ‘archaic majolica’, are spread through the glaze homogeneously, apart from one case in which there is clear evidence of manganese oxide crystals.     

The Archaeometric Characterization of Majolica Ceramics from Talavera de la Reina and El Puente del Arzobispo (Toledo,Spain)

In this study, an archaeometric characterization of 32 ceramic fragments from Talavera de la Reina and El Puente del Arzobispo, dated between the 16th and 18th centuries, has been carried out. Together with three fragments of biscuit, they have been analysed through X‐ray diffraction (XRD), X‐ray fluorescence (XRF), differential scanning calorimetry and thermogravimetric analysis (DSC–TGA). From these chemical results, a statistical study using exclusively majolica ceramics has been carried out. This work has allowed us to find certain differences between the manufactures of the two production centres on the basis of their chemical composition. The mineralogical study has allowed us to determine the estimated firing temperatures of each sample, using the estimated firing temperature (EFT) as an argument for their classification into three fabrics.     

THERMOLUMINESCENCE DATING OF A CRUCIBLE FRAGMENT FROM AN EARLY TIN PROCESSING SITE IN TURKEY

Archaeological exploration in the Taurus mountains at Göltepe in south-central Turkey has uncovered a site indicating the presence of extensive tin ore mining and smelling operations The most recent find of smelting crucible fragments allowed for a thermoluminescence-hased age determination spanning a late fifth to early third millennium BC date. This result is consistent with a number of radiocarbon dates derived for charcoal also found at the site. The importance of this site relates to the possible tin production and subsequent trade with southwestern Asia which would have provided this otherwise scarce ingredient to bronze technology in that area. This date is directly for crucible material and thus confirms the antiquity of tin smelting at Göltepe.     

Disclosing mineralogical phases in medioeval iron nails by non-destructive neutron techniques

There is not only one methodology for the study of mineralogical phases in archaeological samples. In this paper, we discuss a strategy applied to ancient iron nail samples completely based on non-destructive analyses. The archaeological samples come from the archaeological site of Valle delle Forme (province of Brescia–Italy) and date back to the 1300–1400 ad. Neutron-based techniques, like time-of-flight neutron diffraction and neutron tomography, have been used to determine the mineralogical composition and the structure of nails. An independent check for the assessment of the presence of different mineralogical phases was given by Raman spectroscopy. The combination of different non-destructive techniques has provided very useful information on their chemical composition, nature of the patina and corrosion features of the nails (also in the bulk of the samples).     

A characterisation study of Ubaid period ceramics from As-Sabbiya,Kuwait, using a non-destructive portable X-Ray fluorescence (pXRF) spectrometer and petrographic analyses

The Ubaid cultural phenomena (6500–4200 BC) of southern Mesopotamia has been used to characterise other archaeological sites in the Arabian Gulf region. The aim of this inquiry is to explore the nature of the interaction between the homeland of the Ubaid and the wider Gulf region. Through the use of a non-destructive portable X-ray fluorescence (pXRF) spectrometer, this study seeks to characterise and identify the chemical and mineralogical compositions of the ceramic assemblage from the Bahra 1 site of the As-Sabbiya region, Kuwait. The chemical results demonstrated that a combination of six trace elements [rubidium (Rb), strontium (Sr), yttrium (Y), zirconium (Zr), niobium (Nb) and barium (Ba)] occur significantly enough to delineate clay-based artifact groups—local red coarse from Ubaid, while the mineralogical analysis confirms the pXRF result and identifies the source of the raw materials and temper as well. Also, the comparison between the Ubaid and Bronze Age assemblage results suggests that potters used different clay resources within their own regions and/or production techniques.     

Geochemical signatures of Roman amphorae produced in the Sado River estuary,Lusitania (Western Portugal)

Several archaeological sites located in the Sado estuary, Lusitania province (Western Portugal), show evidence of an important amphorae production, mainly related to the Roman Tróia industrial centre of fish preserves. The chemical analysis of amphorae sherds found in Barrosinha, Bugio, Zambujalinho, Xarrouqueira and Vale da Cepa (Lower Sado) was performed by instrumental neutron activation analysis, and the mineralogical composition obtained by X-ray diffraction. The chemical results were compared with amphorae from the Herdade do Pinheiro production centre, also located in the Sado estuary. Application of several exploratory and discriminant techniques of multivariate statistical analysis using chemical data of Lower Sado amphorae allowed the characterization and differentiation of two reference groups, named Sado 1 and Sado 2. The geochemical patterns and the mineralogical composition of these groups indicate the use of two different raw materials, the selection of which appears to have been based on the proximity factor of the kilns. The amphorae produced in the Sado basin were differentiated from amphorae from the Gualdalquivir estuary (Villa Nueva, Cádiz, Spain) in Baetica province.     

The Production of Lead–Tin Yellow at Merovingian Schleitheim (Switzerland)*

A Merovingian crucible fragment, with internally adhering yellow glass, and yellow glass beads of the same region and period were investigated by non‐destructive XRF, optical microscopy and SEM‐EDS. Although the microstructure and chemical composition of the yellow pigment (lead–tin yellow type II, ‘PbSnO₃’) are almost identical in both the beads and the crucible, in the latter the pigment occurs in a much higher concentration. However, the glass base in the beads and the crucible is very different, indicating that the beads were not manufactured directly from the crucible. Instead, the crucible most likely served to produce lead–tin yellow, which was subsequently mixed elsewhere with a colourless soda–lime glass to produce yellow glass beads.     

IBERIAN CERAMIC PRODUCTION FROM BASTI (BAZA,SPAIN): FIRST GEOCHEMICAL,MINERALOGICAL AND TEXTURAL CHARACTERIZATION

Ceramic fragments from the archaeological excavation of the Iberian–Roman city of Basti (Spain) were studied from a geochemical point of view and by applying a statistical tool to X‐ray fluorescence data to discover similarities between ceramic materials. The analysis of these samples was completed by performing a mineralogical analysis, textural observation, and by characterizing the porous system and the colour of the pieces. Our results enabled us to identify the source area of the clayey raw material in the surroundings of Basti and to estimate the firing temperature of the ceramics. Differences in the chemistry were confirmed by characteristics of the pastes and the mineralogical composition of the pieces. Some samples show black cores, which would suggest the presence of organic matter in the raw material and fast firing of the ceramics. The main types of temper were quartz grains and gneiss fragments, although carbonate grains were also identified. Our evidence suggests that most of the samples were well fired. New silicate phases were found to be present in several samples. The mercury intrusion porosimetry verified and confirmed the firing temperature of non‐carbonated samples. Colorimetry showed that the colour of the ceramics varied according to the amount of CaO that they contained.     

Another (mud)brick in the wall: scientific analysis of Bronze Age earthen construction materials from East Crete

Mudbricks appear to have been one of the most common building materials used in domestic architecture in Bronze Age Crete. Well-preserved earthen construction materials from the sites of Vasiliki, Makrygialos and Mochlos in East Crete have been examined with regard to their macromorphological characteristics and their mineralogical and chemical composition in order to investigate the nature of the raw materials used, the technology of manufacture and the potential use of specific recipes. The methods applied include a combination of mineralogical and chemical analytical techniques, namely petrography, neutron activation (NAA), X-ray fluorescence (XRF), and X-ray diffraction (XRD) analysis. Finally, a range of raw materials from the immediate vicinity of each site were sampled and analyzed in order to compare with the archaeological data and identify potential sources. The analyses suggested that there is a degree of standardization in the recipes and the manufacturing process and that the selection of the raw materials depends on availability.     

STONES FROM MEDIEVAL GLASSMAKING: A SUITABLE WASTE PRODUCT FOR RECONSTRUCTING AN EARLY STAGE OF THE MELTING PROCESS IN THE MT LECCO GLASS FACTORY*

The Mt Lecco glass factory was one of the most important production centres in Liguria (Italy) during the 14th and 15th centuries. Archaeological evidence indicates that the whole production cycle took place here. During the glassworking process, production defects such as ‘stones’ were identified and discarded. Stones are partially melted, glass‐coated relics of raw materials or fragments of crucible. The study of the microtexture of stones together with microprobe analyses of phases provides a key for understanding the glassmaking procedure carried out in the Mt Lecco glass factory. The melting rate can be inferred from the compositional variability of glass, which suggests fractional melting of the batch. Glass composition indicates that the Mt Lecco production was a mixed‐alkali one, probably made of quartz‐bearing material as vitrifying agents, plant ashes as fluxing agents and dolomitic limestones as stabilizing agents.     

Chemical tracers of Lusitanian amphorae kilns from the Tagus estuary (Portugal)

In this paper, the characterization of Roman amphorae from the Porto dos Cacos (PC) and Quinta do Rouxinol (QR) workshops, in the Tagus estuary, dating to a period between the 1st and 5th century AD was carried out on the basis of instrumental neutron activation analysis data on 260 amphorae fragments, together with mineralogical compositional studies obtained by X-ray diffraction.     

MINERALOGICAL INVESTIGATIONS OF MEDIEVAL BRICK SAMPLES FROM BÉKÉS COUNTY (SE HUNGARY)

Brick samples from nine archaeological sites representing seven contemporary medieval settlements in Békés County (SE Hungary) were analysed by quantitative X‐ray powder diffraction, optical microscopic, scanning electron microscopic and coupled thermal analytical – evolved gas analytical methods. The aims of this study were to give a mineralogical–petrographical characterization of the brick samples, to gain possible information on the raw clay and the admixed materials, and to determine the firing techniques applied in medieval southeastern Hungary. The mineralogical composition of the samples suggests that the locally extracted clay was mixed with fluvial sand and wheat (Triticum monococcum L.) chaff. The moulded bricks were fired in clamps. The different degrees of calcite consumption suggest that the firing temperature ranged from ～750°C to ～950°C. Moreover, the well‐developed reaction coronas on calcite grains indicate long firing times, lasting perhaps several days.     

Mineralogical analysis and provenancing of ancient ceramics using automated SEM-EDS analysis (QEMSCAN®): a pilot study on LB I pottery from Akrotiri,Thera

A wide range of existing mineralogical and geochemical methodologies such as optical microscopy, X-ray diffraction, manual scanning electron microscopy, ICP-MS and INAA have been utilised in the analysis of ancient ceramics, in attempts to elucidate patterns of regional trade and interaction. However, advances in automated scanning electron microscopy with linked energy dispersive spectrometers (SEM-EDS) have created the potential to offer a seamless combination of textural and mineralogical data based on the acquisition of energy dispersive spectra that has so far been unattainable with existing techniques. In this pilot study on pottery from the Cycladic Bronze Age site of Akrotiri (Thera), we have quantified the mineralogy of the ceramics based on automated SEM-EDS using QEMSCAN^® technology and imaged the textures of the ceramics through compositional mapping. Thirteen samples were analysed and, based upon the automated analysis, four groups of ceramic compositions are defined. These data are consistent with, but also refine, previous traditional petrographic examination of the ceramic samples, and enable the likely provenance of the raw materials used in the ceramic manufacture to be identified. This technique allows the acquisition of fully quantitative data, not only for the larger inclusions within the ceramics but also for the typically finer-grained groundmass/matrix, whilst also providing the overall texture of the ceramic.     

Long-term clay raw material selection and use in the region of Classical/Hellenistic to Early Byzantine Sagalassos (SW Turkey)

A provenance study was carried out on coarse ceramics from the Classical/Hellenistic to Mid-Byzantine city of Sagalassos, SW Turkey. The ceramics were sampled from the excavations of the city, and clay raw materials were sampled throughout its ancient territory. Used techniques were optical microscopy and electron microprobe analysis on thin sections, geochemical analysis (fusion ICP/MS and mineralogical analysis (X-ray diffraction). The geochemical/mineralogical diversity in the ceramics is not as wide as for the clay raw materials. It seems that even at the restricted scale of this study, the resources were limited to the area around the ancient site. The differences between the ceramics are likely due to the use of different ophiolitic clay bodies being exploited for their production.