LEAD ISOTOPIC ANALYSIS FOR THE IDENTIFICATION OF LATE BRONZE AGE POTTERY FROM HALA SULTAN TEKKE (CYPRUS)

Lead isotopic compositions were measured for 65 sherds from five pottery wares (Plain White, Coarse, Canaanite, White Slip and Base‐ring) excavated from the Late Bronze Age site of Hala Sultan Tekke (Cyprus). The elemental composition and isotopic signature of the sherds were compared with those of 65 clay samples collected in south‐east Cyprus, mainly in the surroundings (<20 km) of Hala Sultan Tekke. This work shows the effectiveness of using lead isotopic analysis in provenance studies, along with other analytical techniques, such as X‐ray diffraction (XRD) and a scanning electron microscope (SEM) equipped with an energy dispersive X‐ray detection (EDX) facility, to identify the composition of pottery wares and the clay sources used for pottery ware production.     

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.     

MODELLING CHANGES IN MOLLUSC SHELL INTERNAL MICROSTRUCTURE DURING FIRING: IMPLICATIONS FOR TEMPERATURE ESTIMATION IN SHELL‐BEARING POTTERY*

Firing experiments have been carried out on a clay containing naturally occurring fragments of mollusc shell. The transformation and/or decomposition of mineral phases with temperature was monitored by thermal analysis on the starting material and compared with X‐ray diffraction data on the fired specimens. Scanning electron microscopy revealed systematic changes in the internal microstructure of the shell fragments. Micrometer‐sized intra‐ and inter‐layer pores formed in the shells before the complete decomposition of calcite. The shape, dimension and location of the pores within the shell microstructure were found to be directly related to the firing temperature. The analysis of these microstructural features in archaeometric studies offers a good constraint on the estimation of the firing temperature in shell‐bearing pottery.     

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.     

Preliminary Characterization of Pottery by Cathodoluminescence and SEM–EDX Analyses: An Example from the Yeha Region (Ethiopia)

Yeha was a political and cultural centre of the Ethio‐Sabaean culture (D’MT) in northern Ethiopia and southern Eritrea. Part of the archaeological research deals with pottery of local, regional and imported origin. The research—investigations and examinations—tries to classify local pottery in two ways: first, by analysing the mineralogy of the temper using light microscopy and cathodoluminescence; and, second, by analysing the main element composition of the clay matrix using a scanning electron microscope with energy‐dispersive X‐ray detection (SEM–EDX). The cathodoluminescence shows that the temper material has differences in the colours of feldspars with a similar mineralogical composition. The results demonstrate that the pottery was produced by using local material that originates from various sources in the Yeha region and that the same raw materials were used in different types of pottery.     

Mycenaean pottery from the Argolid and Achaia—a mineralogical approach where chemistry leaves unanswered questions

The chemical classification of Mycenaean pottery from the Northern Peloponnese by neutron activation analysis (NAA) resulted in two groups with very similar chemical compositions assigned to production centres in the Argolid and in Achaia, respectively. The statistical separation of these two groups on the basis only of their chemical composition was difficult, and not clear‐cut for all of the examined samples. A complementary mineralogical examination by X‐ray diffraction (XRD) of some selected samples indicated differences in the mineralogical composition, which confirmed the determined chemical differences. Furthermore, a clay sample was examined, which showed a composition similar to that of the pottery.     

MINERO‐PETROGRAPHIC STUDY OF COOKING WARE AND POMPEIAN RED WARE (ROSSO POMPEIANO) FROM CUMA (SOUTHERN ITALY)

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.     

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.     

ARCHAEOMETRIC ANALYSES ON ‘CORINTHIAN B’ TRANSPORT AMPHORAE FOUND AT GELA (SICILY,ITALY)*

The aim of this work is to throw light on the archaic production of ‘Corinthian B’ amphorae, which are widely diffused in the Western Mediterranean basin and are also present in Greece, but whose geographical provenance is still under discussion. We analysed a group of 37 samples belonging to different ceramic classes dated to the sixth and fifth centuries bc . In particular, there were 19 sherds of trade amphorae of the so‐called archaic ‘Corinthian B’ type, from archaeological excavations in Gela (Sicily, Italy). As a comparison, we also investigated 18 samples of tiles and local coarse pottery from Sibari (Calabria, Italy). The samples were analysed using different techniques, such as optical analysis with a polarized‐light microscope (OM), X‐ray diffraction (XRD), Fourier transform–infrared absorption (FT–IR) and inductively coupled plasma–optical emission spectroscopy (ICP–OES). The combination of these complementary analytical methods allowed us to characterize the samples, determine their firing temperatures and identify the probable provenance. The study of thin sections of sherds by OM allowed us to divide the investigated amphorae into two main groups: the first was characterized by a composition that suggested a Western provenance, in particular from the Calabrian–Peloritan region; the second one was very similar to the ‘Corinthian B’ amphorae that come from Corinth and have been classified as ‘fabric class 1’ by Whitbread (1995 ). The XRD and FT–IR results permitted us to determine the mineral composition of the findings and to estimate their firing temperature. The ICP–OES technique was particularly useful in identifying the production centres. In fact, in the studied pottery, this analysis revealed Ni and Cr values that were noticeably different between Greek and southern Italian production.     

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.     

Lipid Residues from Low‐Fired Pottery

This paper assesses the fate of lipids associated with low‐temperature and pit‐fired pottery to determine to what degree organic compounds persist or are removed during short‐firing episodes below 800 °C. Three different types of clay were fired using contrasting techniques including at 400 °C for 4 h in a muffle furnace, and pit‐firing in which pottery was fired to higher temperatures but for shorter periods of time. Total lipid extracts obtained by solvent extraction of test sherds were screened using gas chromatography‐flame ionization detection (GC‐FID) to determine the lipid concentrations and gas chromatography–mass spectrometry (GC–MS) to identify the organic compounds present. The results showed that firing of clay removes all naturally occurring alkyl lipids; however, during pit‐firing, diterpenoid lipids were introduced into the clay as a condensate from pine ( Pinus spp.) wood used as fuel. These results confirm that alkyl lipids, e.g., fatty acids, can be reliably associated with the use of vessels, although caution is required when interpreting the origins of lipids that might derive from fuel used in firing.     

THE DETERMINATION OF BRICK PROVENANCE AND TECHNOLOGY USING ANALYTICAL TECHNIQUES FROM THE PHYSICAL SCIENCES*†

This work applies established analytical techniques from the physical sciences to Irish brick, in order to gather evidence of ceramic technologies, provenance and sources of raw materials. Petrographic microscopy, X‐ray diffractometry and scanning electron microscopy with an energy‐dispersive X‐ray diffraction attachment were used to study the brick of Rathfarham Castle, Dublin, built c. 1618, where clay brick was introduced in 1771. Local clay was fired in the laboratory and analysed in a similar manner. The petrography of the pointing mortar was studied in order to gather evidence of ceramic provenance. This paper concludes that the brick was hand‐ moulded with a silica‐based, predominantly non‐calcareous clay of glacial origin, gathered locally, including fluxes and a high percentage of non‐plastic material. The mineralogy and petrography of the brick, together with the presence of pebbles and a coarse matrix, suggest that the raw clay was probably gathered from a glacial deposit. The presence of abundant pebbles and colour inhomogeneities suggests a lack of processing of the raw clay. The brick was probably fired in clamps at top firing temperatures ranging from 750°C to above 900°C. Transformation of limestone temper involving the breakdown of calcite and the generation of calcium silicates, and the new formation of plagioclase, high‐temperature quartz, hematite and spinel were revealed. The presence of spinel in ‘hot spots’ indicates that fuel was added to the raw clay in order to assist firing.     

Transmission electron microscopy (TEM) applied to ancient pottery

A comparative study of ancient pottery has been carried out, which utilized X‐ray diffraction, optics and scanning and transmission electron microscopy (SEM and TEM). Samples came from three prehistoric sites in northern Spain (La Rioja). Transmission electron microscope techniques, which use intact ion‐milled samples, allow minerals and glass to be imaged in situ, providing data on textures, crystal structures and composition. TEM provided detailed characterization of both source‐characteristic raw materials and products of the firing process, and revealed the range of intermediate phases, most of which had sizes beyond that of resolution by SEM. More importantly, TEM provided definition of the reaction processes, from starting materials through glass and new crystalline phases, providing data on both temperature and duration of firing.     

Firing Techniques of the Impasti from the Protohistoric Site of Concordia Sagittaria (Venice)

⁵⁷Fe Mössbauer spectroscopy provided relevant information on the firing techniques employed in manufacturing concotto and coarse pottery, two types of fired clay mixtures (impasti) of the protohistoric settlement site of Concordia Sagittaria. The firing techniques of Concordia were reconstructed by comparing the Mössbauer patterns of the artefacts with those of the local raw clays fired in the laboratory. The concotto was produced in kilns by firing clay mixtures under oxidizing conditions at 700–1000°C, or at lower temperatures in the open air. The firing of these clay mixtures containing mainly ground pieces of waste pottery, resulted in hard and variously coloured construction materials, particularly suitable for humid environments. In turn, the coarse pottery was produced by firing clay mixtures more homogeneous than those used for the artefacts of concotto. The firing of coarse pottery was performed under reducing conditions at about 900°C with a final exposure to air by opening the hot kiln. Light and agreeable coarse pottery, with a red surface on the grey-black core, was obtained when the effective temperature of air was higher than 500°C.     

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 PRODUCTION OF SASANIAN GLAZED POTTERY FROM VEH ARDAŠ?R (CENTRAL IRAQ)

Scanning electron microscopy coupled with an energy dispersive X‐ray detector (SEM‐EDS) has been used to study samples of Sasanian glazed pottery. Analysis of ceramic bodies revealed a general homogeneity in composition among the studied samples and the use of calcareous clay for their manufacture. Glazes are typically alkaline in composition, with sodium and potassium oxide contents between 8 and 13%, and between 3 and 5%, respectively; calcium and magnesium oxide contents are between 7 and 10%, and between 3 and 5%, respectively. These data suggest the use of plant ash together with a silica source for glaze production. Coating thickness is highly variable among different samples, from some 400 up to 1200 µm, but it is generally uniform when a single sample is concerned. Glazes are mostly coloured blue or blue‐green; copper and iron are the colouring agents detected; abundance of bubbles, silicate crystals and relics of unmelted material are responsible for their generally opaque appearance, together with the presence of weathering products. The characteristics of the body to glaze contact zone, together with the widespread presence of bubbles, would not rule out production by a single firing process. A few samples feature a peculiar gritty coating on one side of their surface; SEM images show that they are actually partially vitrified, and EDS data denote a rather heterogeneous composition. It seems possible that they result from mixing clay together with the frit used for glaze development.     

CYPRIOT BYZANTINE GLAZED POTTERY: A STUDY OF THE PAPHOS WORKSHOPS

Twenty‐five samples of Byzantine glazed pottery from two archaeological sites between Limassol and Paphos region (Cyprus), dated between the 12th and 15th century ad were studied using micro X‐ray fluorescence spectroscopy, scanning electron microscopy and X‐ray diffraction analysis. It was found that all the glazes contain lead, following the main manufacturing process of medieval pottery in the Mediterranean territory, while some of them contain tin, possibly for better opacity. Furthermore, it is shown that copper, iron and cobalt with nickel are responsible for the decoration colours. Finally, the application of principal component analysis revealed significant differentiation for some of the samples.     

Ancient Egyptian Pottery from the Subsurface Floodplain of the Saqqara–Memphis Area: Its Mineralogical and Geochemical Implications*

Potsherds recovered from the Saqqara–Memphis floodplain in Egypt, dated according to their typology and radiocarbon dating of the included sediments, are analysed geochemically and mineralogically to identify source materials and fabrication characteristics. Pottery layers were identified and potsherds were recovered from several settlement levels. Sherd typology was used to identify sherds from four periods (the Old and New Kingdoms, and from the Late Period to the Ptolemaic). The Pharaonic pieces were found at depths of between 8 and 12 m and the later material was between 6 and 3 m. Chemical analyses of the potsherds revealed three main source materials: local Nile silt, marl clay and mixed Nile silt–marl. Two marl clay types were recognized: marl clay from Upper Cretaceous marine sediment and another one from Late Pliocene deltaic sediments. The mineralogical composition of the pottery samples shows that the estimated firing temperature was about 850–900°C. No consistent differences in sherd mineralogy and geochemistry were found according to pottery types, so that the ancient Egyptian potters used essentially the same materials throughout the Pharaonic period. However, this initial study has revealed the existence of extensive pottery‐rich occupation sites buried within the Nile floodplain deposits between Memphis and Saqqara.     

Archaeometric study of medieval pottery excavated at Stari (Old) Ras,Serbia

A combined study of a series of polychromatic and monochromatic glazed medieval pottery shards excavated from the archaeological area of Stari (Old) Ras in southern Serbia, including petrographic and chemical analysis, powder X-ray diffraction (PXRD) and Fourier transform infrared (FTIR) spectroscopy, allowed us to clearly distinguish between two groups of ceramics. Ras pottery, made of fine-grained well-cleaned clay and characterised by a rich mineral assemblage, was produced by firing in a temperature range between 800 and 900 °C. Reljina Gradina ceramics were produced at similar temperatures from materials which, with regard to mineralogical and chemical composition, show clear similarity with local clay, suggesting that these samples are of local origin and production. This work is the first systematic archaeometric study of medieval pottery excavated on the territory of Serbia.     

Determining the Firing Temperature of Low‐Fired Ancient Pottery: An Example from the Donghulin Site,Beijing, China

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.