Organic residue analysis of Iron Age ceramics from the archaeological site of Kani-zirin,western Iran

Organic residue analysis of potshards excavated from the Iron Age archaeological site of Kani-zirin, western Iran, was achieved with acidified methanol extraction and gas chromatography-mass spectrometry (GC-MS). The GC-MS data showed plant and animal commodities incorporated in the shards. Also, the investigations confirmed the presence of plant resin together with a tartrate ion within a group of the shards, suggesting a probable use of grape-related products. Evidence of resins from the Pinaceae family, as an exotic species in Iran, was evinced in several of the shards.     

The technology and production of glazed ceramics from Middle Islamic Jerash,Jordan

Jerash in northern Jordan was, despite a focus on its classical heritage, also active in the Middle Islamic period, but little is known about actual developments during this period. This study represents the first study on the Middle Islamic glazed pottery from the site using scanning electron microscopy energy‐dispersive spectrometry (SEM‐EDS) and thin‐section petrography. The results show that two production traditions existed, each with different provenances. The local production is characterized by a non‐calcareous ceramic body and the use of a high‐lead glaze coloured with iron and copper oxides, whereas the turquoise‐glazed samples, likely imported from Mesopotamia, have a calcareous ceramic body and alkali or alkali‐lead glaze.     

RELATIONSHIP BETWEEN THE COLORATION AND THE FIRING TECHNOLOGY USED TO PRODUCE SUSA GLAZED CERAMICS OF THE END OF THE NEOLITHIC PERIOD*

Ancient decorated potteries from Susa (Mesopotamia) dating from 4200 to 3700 bc , were studied in order to determine the origin and the nature of the raw materials used, and to identify the technological processes applied to make the ceramic bodies and their decorations. Bulk compositions were determined by particle induced X‐ray emission (PIXE), while the microstructure and the mineralogical phases were studied using scanning electron microscopy (SEM), energy dispersive X‐ray analyses (EDX) and X‐ray powder diffraction (XRD). The results showed that the raw materials used to elaborate these potteries were similar for all the ceramic bodies (carbonates and iron and magnesium‐rich clays containing sand), and for all the decorations (iron oxides, silica, potassic and alumina sources). The variations of coloration of the ceramics and of their decorations were due to different firing temperatures. The ranges of firing temperatures used by potters were evaluated on the basis of mineral stability domains.     

A SPECTROSCOPIC INVESTIGATION OF PIGMENT AND CERAMIC SAMPLES FROM COPÁN,HONDURAS*

A combination of micro‐Raman spectroscopy, micro‐infrared spectroscopy and SEM–EDX was employed to characterize decorative pigments on Classic Maya ceramics from Copán, Honduras. Variation in red paint mixtures was correlated with changing ceramic types and improvements in process and firing techniques. We have confirmed the use of specular hematite on Coner ceramics by the difference in intensities of Raman bands. Different compositions of brown paint were correlated with imported and local wares. The carbon‐iron composition of the ceramic type, Surlo Brown, was confirmed. By combining micro‐Raman analysis with micro‐ATR infrared and SEM–EDX, we have achieved a more comprehensive characterization of the paint mixtures. These spectroscopic techniques can be used non‐destructively on raw samples as a rapid confirmation of ceramic type.     

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.     

Non-destructive chemical characterization of ceramic sherds from Shipwreck 31CR314 and Brunswick Town, North Carolina

The purpose of this study was to chemically and texturally characterize ceramic oil jar sherds from North Carolina Shipwreck 31CR314 and to explore the utility of environmental scanning electron microscopy/X-ray energy dispersive spectrometry (SEM/EDS) for that purpose. The oil jar sherds, widely dispersed about Shipwreck 31CR314, are morphologically similar to each other, which suggests they could be from a single jar, but with so few joins this could not be concluded with certainty. Therefore, an aim of this study was to investigate whether chemical or textural characterization of the sherds might reveal unique attributes that could distinguish individual jars; results of characterization perhaps could give information on their origin and possibly site formation processes, such as whether environmental forces could have scattered sherds of a single jar during and after sinking of the ship. Previous studies have indicated this shipwreck is likely the remnants of the Queen Anne's Revenge, flagship of the pirate Blackbeard. Sherds from this shipwreck were compared with similar oil jar sherds excavated from a land site, Brunswick Town, North Carolina, to explore the use of composition and texture as hallmarks. The chemical components of the artifacts were determined by SEM/EDS. This method of analysis is valuable for archaeological research because it is rapid and non-destructive to the ceramic artifacts. Both groups of lead-glazed coarse red earthenware sherds were texturally similar except for the glazed sides of all 31CR314 sherds that exhibited small tracks of unique crescent-shaped marks. These marks may be due to manufacturing effects and immersion in seawater, and the marks may serve as hallmarks for individual jars or potentially individual manufacturers. The sherds were generally similar in composition, but the two groups exhibited distinct differences. Brunswick Town sherds consistently contained more phosphate on unglazed sides, an average 1.46 wt.% P₂O₅, and also contained trace elements not detected in the Shipwreck 31CR314 sherds. These distinct differences could be due to different manufacturing origins for Shipwreck 31CR314 and Brunswick Town ceramics but also could reflect their subjection to different environments during use and loss prior to archaeological recovery.     

A Quasi Non‐destructive Microsampling Technique for the Analysis of Intact Glass Objects By Sem/edxa

A novel sampling technique for the analysis of glass is described, which involves the removal of minute particles from an object with a diamond‐coated file, followed by energy‐dispersive X‐ray analysis in the scanning electron microscope (SEM/EDXA). The particles are fixed to adhesive carbon discs and carbon coated without grinding or polishing. Mean compositions are determined for 10 arbitrarily selected particles above a minimum grain size of 150 mm and normalized to totals of 100%. Tests were carried out on two standard soda–lime–silica glasses of well‐characterized composition, using two files of different grade. The analyses showed good agreement with the accepted values of all elements. Although the precision is somewhat reduced, this highly portable and quasi non‐destructive microsampling procedure provides almost the same information as that gained from samples embedded and polished in the normal way. Its application is thought to be especially useful for the investigation of intact glass objects and ceramic glazes.     

SIENESE ‘ARCHAIC’ MAJOLICA: A TECHNOLOGICAL STUDY OF CERAMIC BODIES AND COATINGS*

The aim of the present study is to reconstruct the production technology of Sienese ‘archaic’ majolica in the early decades of the 14th century ad . The integration of archaeological data with archived data revealed the presence of numerous workshops, suggesting that the Sienese tradition of majolica production was well developed up until the end of the 16th century. Sixty‐seven uncoated and coated waste products were analysed. The ceramic bodies were examined by OM, XRDp, SEM–EDS, XRF, ICP–OES, ICP–MS and INAA. The coatings (enamels and glazes) were analysed by SEM–EDS and Raman microspectroscopy. The results showed that ceramics were rejected due to poor control of the firing temperature (technological wastes), faulty production technology (wastes of uncertain classification) and accidents (post‐firing wastes). Finally, the analyses revealed extreme homogeneity of the ceramic bodies, indicating the continued use of the same raw material over the whole period studied.     

AN INVESTIGATION INTO THE RELATIONSHIP BETWEEN THE RAW MATERIALS USED IN THE PRODUCTION OF CHINESE PORCELAIN AND STONEWARE BODIES AND THE RESULTING MICROSTRUCTURES*

The microstructures of porcelain and stoneware bodies from north and south China, spanning the period from the Tang to the Ming dynasty (7th–17th centuries ad ), were examined in polished sections in a scanning electron microscope (SEM) after etching the sections with hydrofluoric acid (HF). Mullite, present as fine, mainly elongated crystals, is the dominant crystalline phase observed. The bulk chemical compositions of the bodies are determined by energy‐dispersive spectrometry in the SEM, and the relative amounts of mullite and quartz present in the different ceramics are estimated from X‐ray diffraction measurements. Mullite formed from areas of kaolinitic clay, mica particles and feldspar particles is distinguished through a combination of the arrangement of the mullite crystals, and the associated SiO₂/Al₂O₃ wt% concentration ratios. It is shown that very different microstructures are observed in ceramic bodies produced using kaolinitic clay from north China (Ding porcelain and Jun stoneware), porcelain stone from south China (qingbai and underglaze blue porcelain and Longquan stoneware), and stoneware clays from south China (Yue and Guan stonewares). Therefore, SEM examination of HF‐etched, polished sections of the bodies of high‐refractory ceramics has considerable potential for investigating the raw materials used in their production.     

云南剑川海门口遗址饱水古木降解的微观构造分析

文中采用扫描电镜(SEM)和透射电镜(TEM)对海门口遗址饱水古木进行降解机理分析。结果表明:古木细胞次生壁收缩严重并与胞间层分离;胞间层保存较完好,呈连续网状。说明古木纤维素和半纤维素降解相对严重,木质素降解相对较轻。古木主要是受细菌降解,通过SEM和TEM均可见明显的细菌腐朽特征。细菌首先侵入细胞腔,再通过S3层侵入细胞壁内部。细胞壁内由于降解而产生的空隙在几十到几百纳米之间。饱水古木也受到了一定程度的真菌降解,但这类真菌主要降解古木内淀粉等物质,对细胞壁物质降解能力差,主要是使古木变色。     

CHEMICAL AND MINERALOGICAL APPROACHES TO THE ORGANIZATION OF LATE BRONZE AGE NUZI WARE PRODUCTION

In order to investigate the nature and organization of high‐status ceramic production in the Late Bronze Age, samples of Nuzi Ware from four different sites were analysed using scanning electron microscopy (SEM–EDS) and inductively coupled plasma atomic emission spectroscopy (ICP–AES). Chemical and mineralogical evidence suggests that Nuzi Ware was produced in at least two distinct regions, one probably in the Adhaim Basin in northern Iraq and another possibly in the Orontes catchment in southeastern Turkey. The existence of individual production units probably developed in response to the local elites' desire to imitate the tastes of the Mitanni aristocracy, resulting in a mapping of political relationships on to material culture.     

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.     

THE EVOLUTION OF LUSTRE CERAMICS FROM MANISES (VALENCIA,SPAIN) BETWEEN THE 14TH AND 18TH CENTURIES

A set of 33 fragments of lustre‐decorated ceramics uncovered during an archaeological excavation in Manises (Valencia, Spain) have been studied. These ceramics were produced in Manises from the 14th to the 18th century. This well‐dated set of ceramic shards represents the diversity of Manises lustre production and is a complete time sequence of reference for the technological analysis. Texture analysis of the glazes has been carried out by SEM–EDAX, the inner and outer surfaces of the lustre decorations being analysed with non‐destructive ion beams by PIXE and RBS, and also by high‐resolution electron microscopy. The results are compared with other lustre productions and the time trend of the microstructures, glaze and lustre composition is analysed. It is concluded that Sn was used to opacify glazes until the beginning of the 17th century and that changes in the lustre microstructure occurred around ad 1500.     

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.     

The Tomb of the Three Brothers in Palmyra: The Use of Mimetite,A Rare Yellow Pigment,in A Rich Decoration

The wall paintings of the Tomb of the Three Brothers in Palmyra display a very rich Greco‐Roman iconography. The study of the painting reveals the use of a great variety of pigments, including Egyptian blue and an extremely rare bright yellow pigment, mimetite, of which no other traces are known for this period. This pigment was identified through the combined use of two methods of analysis, scanning electron microscopy associated with X‐ray microanalysis (SEM–EDS) and X‐ray micro‐diffraction (XRD). The varied chromatic palette used underlines the refinement and the particular care given to these decorations. Notable differences have been found between the pigments of the decorations of the arch and those used for the rest of the chamber.     

ANALYSIS OF THE NOTCHES OF ANCIENT SERRATED DENARS*

A number of serrated silver denars of the Roman Republic and a Greek bronze coin were investigated, paying special attention to the notches, in order to reveal their production technique. Particular interest was devoted to three contemporary forgeries of serrated denars, because the official pure silver issues were also available for inspection. Several microbeam analytical techniques were applied, such as scanning electron microscopy (SEM), electron probe micro‐analysis (EPMA) and secondary ion mass spectrometry (SIMS). The surfaces of the notches, which show traces of the tools used, were investigated by SEM. In the case of the forged coins, the thickness of the silver layer (inside the notches as well as on the surface of the coin) was determined by SEM and SIMS. The main components of the surfaces were similar in both cases as measured by EPMA. Combining the results, it is possible to reconstruct the steps in the production of the serrated denars. The investigations also permit a review of different opinions about the purpose of the notches.     

TECHNOLOGY OF PRODUCTION OF GHAZNAVID GLAZED POTTERY FROM BUST AND LASHKAR‐I BAZAR (AFGHANISTAN)

Fifteen fragments of glazed pottery were studied by scanning electron microscopy coupled with energy‐dispersive X‐ray analysis (SEM–EDS). The fragments, dated from between the 11th and the 12th centuries, are part of a group excavated at ancient Bust and Lashkar‐i Bazar (southern Afghanistan) and belonging to the International Museum of Ceramics in Faenza. All the samples are characterized by highly calcareous bodies, and all of them but one is coated with a transparent lead glaze; the last fragment is, instead, coated with a turquoise opaque lead–alkali glaze. With three exceptions, the studied fragments show underglaze decorations featuring white, red, green or black motifs applied on to a white, red or black engobe; one of the remaining glazes is applied on to a monochrome white slip and the other two directly on to the ceramic body. Optical microscopy and SEM images show that engobes and decorations were obtained by deposition of differently coloured clayey slips, the composition of which was characterized by EDS analyses. In particular, black engobes and decorative motifs were obtained by recourse to manganese and iron compounds or to chromium, magnesium and iron compounds; it appears that both possibilities could be exploited for obtaining different decorative motifs on the same object.     

Raspadita: a new lithic tool from the Isthmus of Rivas,Nicaragua

A new lithic tool type was discovered at the Pacific Nicaraguan archaeological site of Santa Isabel (AD 800–1350) and named raspadita (small scraper). Thousands of these small tools (1–2 cm in length) were found. They have a rounded proximal edge and a pointed distal end. In this study, the raspaditas are proved to be a coherent tool class with minimal variation in size, shape, material type and usewear. They were manufactured from white chert bladelet cores using soft hammer percussion and pressure flaking unifacial retouch. Usewear points to a composite tool form and a scraping function for the raspaditas. Scanning electron microscopy determined a ventral leading, dorsal following, unidirectional scraping motion for the raspadita proximal end. The material that was scraped has still to be definitely determined but phytoliths visible in the SEM images suggest that the composite tool was used for plant processing.     

Pottery technology in the Tang dynasty (ninth century ad): archaeometric analyses of a Gongyi sherd found at Siraf,Iran

In 1969–70, a single Tang dynasty blue‐spotted Gongyi sherd was found at Siraf, Iran, the main trading port on the Persian Gulf in the early Islamic period. This is the only known example of Chinese blue‐and‐white ware, whether low‐ or high‐fired, found in the Middle East from such an early date. The sherd provides direct archaeological evidence for the Indian Ocean trade between China and the Middle East in the ninth century ad . The body paste, clear glaze and blue glaze or pigment were analysed by thin‐section petrography, scanning electron microscopy with energy‐dispersive X‐ray spectrometry (SEM‐EDX) and X‐ray fluorescence (XRF). The technological analysis reveals the different steps of the chaîne opératoire: clay mixing, slip and glaze application, and decoration with the cobalt blue glaze before high‐temperature firing. These steps are characteristic of Tang stoneware production at Gongyi in Henan province, China. The use of cobalt blue pigment as part of a simple spotted decoration scheme on the Gongyi sherd, and its find context within the Middle East, provides evidence for the complex interplay and influence occurring between Chinese and Middle East ceramic industries at this time. Closely comparable examples of contemporary low‐fired earthenware ceramics with cobalt blue decoration on a white tin glaze manufactured within the Middle East also occur within the same assemblage from Siraf.     

A Late Roman ceramic production from Pompeii

The Via Lepanto site is one of the best examples showing how the Vesuvian region was partially reconstructed and earlier re-occupied after Vesuvius's eruption in the year 79 AD. The large amount of ceramic finds illustrates the typology in use in this area during the IV and V century AD. Analyses were focused on table and cooking ware productions. Archaeometric data were obtained using chemical and minero-petrographical methods (OM, XRD, XRF and SEM). Grain size measurements using Image Analyses on thin sections and a geochemical comparison with clayey deposits outcropping in the Campania region permitted the identification of the raw materials used for these pottery productions. XRD and SEM completed the data set, establishing the protocols used for pottery production in the Pompeii area during Late Roman period. The Via Lepanto site was part of an exchange network of markets with a periodic frequency, where locally produced and imported pottery was sold, indicating a flourishing network of exchanges spanning short, medium and long distances.