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.     

A Better Shade of Black: Effects of Manufacturing Parameters on the Development of Ancient Black Bronzes*

Copper alloys with controlled contents of Sn, Ag and Au were treated with methods and solutions that mimic those used in ancient and traditional procedures for the production of black bronze. Examination of the resulting patinas with colorimetry, SEM–EDS, TEM, Raman spectroscopy and XRD revealed no systematic differences according to the fabrication method, whereas patina homogeneity and colour in those alloys that did not contain precious metal were affected by superficial work. Patina microstructure determines adherence and coverage, and depends upon the solution used irrespective of the alloy composition, but the colour of the patina is mainly related to the alloy composition. Gold promotes the development of cuprite, slowing the oxidation to tenorite in the corrosion process. Gold additions produce a more uniform patina as well as a desirable blue–black tone, which is likely to have been a factor in alloy selection.     

Starch granules,dental calculus and new perspectives on ancient diet

Recent work in various parts of the world has suggested the possibility of ancient starch granules surviving and adhering to archaeological artefacts. Often this information is used to infer aspects of diet. One additional source for recovery of archaeological starch granules is dental calculus. The presence of plant food debris in dental calculus is well known but has not been not widely investigated using archaeological material. The extraction of starch granules from dental calculus represents a direct link to the consumption of starchy food by humans or animals. Using dental calculus also sidesteps many other questions still inherent in using starch granules to reconstruct aspects of ancient diet, such as the effects of diagenesis on their morphology; as the starches are trapped inside a concreted matrix they are less likely to alter over time. We used amylase digestion by a starch-specific enzyme to confirm the material as starch.     

THE SECTILIA PANELS OF FARAGOLA (ASCOLI SATRIANO,SOUTHERN ITALY): A MULTI‐ANALYTICAL STUDY OF THE RED,ORANGE AND YELLOW GLASS SLABS*

SEM–EDS, EMPA, ICP–MS and ICP–OES were applied to the study of three sectilia panels made of red, orange and yellow glass slabs. In order to determine the chemical state of Cu, XAS was also performed. The results indicate that, with the exception of the red samples, all slabs were made by mixing a siliceous sand with natron. The red slabs show significant compositional differences with respect to K₂O and MgO contents, probably linked to the use of plant ashes as a source of alkali. The red, orange and yellow slabs are coloured by metallic copper, cuprite and Pb antimonates, respectively. The comparison between the chemical composition of the Faragola samples and several glass reference groups did not provide conclusive evidence of provenance.     

CHARACTERIZATION OF PLASTERS FROM PTOLEMAIC BATHS: NEW EXCAVATIONS NEAR THE KARNAK TEMPLE COMPLEX,UPPER EGYPT*

The aim of the present work is to characterize plasters from Ptolemaic baths recently discovered in front of the Karnak temple complex, by the excavations of an Egyptian–French team. The characterization was carried out by means of optical microscopy (OM), scanning electron microscopy (SEM) equipped with an energy‐dispersive X‐ray detector (EDS), X‐ray diffraction analysis (XRD) and Fourier transform infrared spectroscopy (FT–IR). The results allowed the identification of the chemical composition and structure of these plasters. In addition, samples of red, yellow, black and white pigments were examined and identified. The results helped in providing an image concerning some materials used during the Ptolemaic era in ancient Egypt.     

Integrated Analytical Techniques for the Study of Colouring Materials from Two Megalithic Barrows

We have determined the composition of rock art pigments from two megalithic barrows located in the north of Portugal. The use of XRD, SEM–EDS and FT–IR spectroscopy confirmed the presence of hematite and kaolinite in the red pigments from the Eireira barrow, and kaolinite in the white pigment from the Leira das Mamas barrow. The organic composition of the pigments was studied by GC–MS, suggesting that the red sinuous lines and dots from the Eireira barrow were prepared with cooked or heated algae and/or aquatic plants, with egg as binder, while the white pigment from the Leira das Mamas barrow revealed a mixture of vegetable oils for kaolinite moulding, which could be stabilized by temporary exposure to high temperatures. The multi‐analytical approach used on this study of megalithic pigments allowed the recovery of important data about north‐western prehistoric communities, namely the way in which they exploited existing resources and their ability to transform them.     

Visigothic Jewellery: A Technical Study of Glass Used as Gems in Belt Buckles from a Spanish Necropolis

In this work, we studied coloured and colourless glass used as gems in Visigothic buckles possibly originating from the necropolises of Torredonjimeno, Duraton or Castilltierra in Spain. Scanning electron microscopy (SEM) with energy‐dispersive analysis (EDS) and observations made with an optical microscope in reflected and transmission mode were performed in order to establish the composition, origin of the colour and decay process of these glass pieces. The chemical analysis of ancient glass can provide relevant information regarding the manufacturing approach used during a specific period. The results revealed the presence of various transition metal elements used as chromophore elements, as well as some metallic backing foils used to improve the colour of pieces of almost colourless glass.     

新疆山普拉墓地出土金线结构形貌与材质特征研究

山普拉墓地出土的珍贵纺织品与新疆其他古墓葬群出土的纺织品一样,是研究世界古代纺织史、丝绸之路物质文化交流的重要标本,承载着人类社会发展极其重要的历史、文化、科技价值。为研究古代纺织品的用金技术,以新疆和田洛浦县山普拉墓地出土金线为研究对象,借助光学显微镜和扫描电镜对金线的形貌进行显微观察,以揭示金线及其芯线的结构特征,获取了金线相关几何尺寸等信息。同时结合能谱仪分析,对金线的成分进行检测,获得了金线合金中各元素的比例。本研究结果可为中国古代纺织品的用金技术研究提供科学依据,并且期冀通过今后逐步积累的大量金线分析数据能够揭示出中国较早时期纺织品用金技术的起源及其发展脉络。     

Plant microfossils in human dental calculus from Nemrik 9, a Pre-Pottery Neolithic site in Northern Iraq

Samples of dental calculus were taken from 11 human individuals buried at Nemrik 9, a Pre-Pottery Neolithic site in Northern Iraq. All of them represented the time span of ca. 9100–8600 bp. In total, 95 microfossils were retrieved from these samples, including 70 phytoliths, 9 starch granules or clusters of starch, 3 pollens, and 1 xylem fragment. Most microfossils could be attributed to C₃ cool season cereals, most likely wheat and barley, which is consistent with previous knowledge about the composition of crops in early farming communities living in the Fertile Crescent. In addition, three phytoliths and one starch granule typical of C₄ warm season grasses were recovered including one subangular and faceted starch granule, which might derive from a native grass, but is not diagnostic of any genus. Prior to assigning diagnostic status to this starch, exhaustive reference work on native grass seeds is necessary. The presence of one Phragmites phytolith suggests non-alimentary processing of reeds using teeth or perhaps using the stem of this grass as a toothbrush or toothpick.     

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).     

First Evidence Of The Use Of Freshwater Pearls As A Cosmetic In Ancient China: Analysis Of White Makeup Powder From A Northern Song Dynasty Lv Tomb (Lantian,Shaanxi Province,China)

The Lv family tombs in Lantian, Shaanxi Province are one of the most important archaeological sites of China in recent years, providing numerous objects and a wealth of information for the study of the history of the Northern Song dynasty. There were a large number of exquisite cultural relics unearthed from the tombs, including one porcelain box containing white powder, which was identified as women's makeup. The phase composition, microstructure, thermal properties and characteristics of the trace elements in the unearthed white cosmetic powder were comprehensively analysed by X‐ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry – thermogravimetry (DSC–TG), Fourier transform infrared (FT–IR) microscopy and inductively coupled plasma atomic emission spectroscopy (ICP–AES). The white makeup powder was determined to be a product made from high‐quality freshwater pearls. These results, for the first time, showed evidence that freshwater pearl powder was used as a cosmetic in ancient China using archaeological objects, providing scientific evidence and new clues to enrich and expand research into the ancient Chinese cosmetic materials.     

PROVENANCE OF MEDIEVAL PIETRA OLLARE ARTEFACTS FOUND IN ARCHAEOLOGICAL SITES OF CENTRAL–EASTERN ITALY: INSIGHTS INTO THE ALPINE SOAPSTONE TRADE*

Medieval archaeological findings made of pietra ollare (basic and ultrabasic metamorphic rocks belonging to the greenschist facies) and coming from central–eastern Italy have been characterized through a petrological study (modal mineralogy, whole‐rock geochemistry, XRD and SEM–EDS analyses). The pietra ollare artefacts considered in this work consist of fine‐grained, grey to pale‐grey, magnesite‐bearing talc‐schists (i.e., soapstones). In order to determine their production centres, Alpine soapstones quarried in ancient times were selected on the basis of their mineralogical and textural compatibility with the archaeological findings. The mineralogy and chemistry (major and trace elements) contributed to establishing the ancient quarries of the Valchiavenna (central Alps) as the probable provenance area. This archaeometric investigation proves that Alpine artefacts made of pietra ollare spread to the south of the Po Plain during the Middle Ages. It can be inferred that the Alpine soapstone trade towards the Marche and Abruzzo regions was addressed through the main waterways: Lake Como, the Adda and Po Rivers and finally the Adriatic Sea.     

DEEPLY COLOURED AND BLACK GLASS IN THE NORTHERN PROVINCES OF THE ROMAN EMPIRE: DIFFERENCES AND SIMILARITIES IN CHEMICAL COMPOSITION BEFORE AND AFTER ad 150*

In this work we attempt to elucidate the chronological and geographical origin of deeply coloured and black glass dating between 100 bc and ad 300 on the basis of their major and trace element compositions. Samples from the western and eastern parts of the Roman Empire were analysed. Analytical data were obtained by means of a scanning electron microscope – energy‐dispersive system (SEM–EDS, 63 samples analysed) and laser ablation – inductively coupled plasma – mass spectrometry (LA–ICP–MS, 41 samples analysed). Among the glass fragments analysed, dark brown, dark purple and dark green hues could be distinguished. Only among the dark green fragments could a clear compositional distinction be observed between fragments dated to the periods before and after ad 150. In the early samples (first century bc to first century ad ), iron, responsible for the green hue, was introduced by using impure sand containing relatively high amounts of Ti. In contrast, a Ti‐poor source of iron was employed, containing Sb, Co and Pb in trace quantities, in order to obtain the dark green colour in the later glass samples. The analytical results obtained by combining SEM–EDS and LA–ICP–MS are therefore consistent with a differentiation of glassmaking recipes, detectable in glass composition, occurring in the period around ad 150.     

Comparative microstructural and elemental analysis of iron artefacts from Kaveri valley archaeological sites

Iron has been one of the most critical technotraditions that had lasting impact on social formation throughout the Iron Age and historical period. Iron was used in warfare and subsistence economy. Our knowledge on ancient iron smelting and working have generally been derived from ethnography and ethnohistory, which is by all means, time, region, and raw material specific. Scientific analyses of ancient iron have contributed in understanding this heritage to a respectable extent, yet a comprehensive knowledge about the evolution of iron making through time and space in India eludes us. In this work, a comparative study of iron artefacts from two Iron Age/Megalithic-Early Historic sites of Tamil Nadu, south India, that is, Mangadu (burial site) and Ambal (habitation-cum-burial site) is carried out to understand the iron thermal-processing capabilities. The retrieved artefacts were examined using X-ray fluorescence (XRF) for elemental composition. The imaging of the artefacts was done using Scanning Electron Microscopy (SEM), Electron Backscatter Diffraction (EBSD), and Optical Microscopy (OM). In addition, phase identification was performed using X-ray diffraction (XRD) and Energy Dispersive X-ray Spectroscopy (EDS). Combination of these analyses illustrates that inhabitants of Mangadu and Ambal were aware of the iron alloy manufacturing/processing techniques such as forging and hammering.     

Comparison of analytical techniques for analysis of archaeological bronze

While many analyses of archaeological bronzes have been reported in the literature, in practice it is very difficult to compare them. To assess the present status of the chemical analysis of bronze two ancient objects—a flat axe (arsenic bronze) and a sickle (tin bronze)—were cut into pieces weighing about 2 g each and were distributed to 11 laboratories. The participants used the following methods for analysis: INAA, ED–XRF, PIXE, TRXRF, FAAS, ICP–AES, ICP–MS, SEM–EDS, LA–ICP–MS and PGAA. The samples were analysed in at least quadruplicate. Dixon's and Iglewicz and Hoaglin's tests were used to detect outliers. The majority of methods provided comparable results, especially for macroelements, independent of the technique and standards used. The number of determined elements depended on the method and, naturally, on the concentration level. Therefore an important recommendation that can be made is to supply, with each archaeometric investigation, data from the analysis of appropriate Certified Reference Materials (CRMs) used in the study.     

Starch residues on museum artefacts: implications for determining tool use

A sample of 11 museum artefacts was examined to assess the preservation of any adhering organic residues, particularly starch granules, and to assess the potential for the identification of cooked starchy foods. The primary aim was to examine starchy deposits, extract starch granules and examine their physical condition to increase our understanding of the taphonomy of starch granules and associated organic residues in archived material and archaeological deposits. The study shows that organic plant residues could be recovered from archived artefacts and makes a significant contribution to understanding the function of this material. Recovered starch granules showed an interesting pattern of varying organic preservation on the surface of stone and wooden artefacts. Some starch granules were found to be well preserved while others in the same sample appeared to have been affected by enzyme degrading micro-organisms. Recovered residues included fully gelatinised starch.     

GLAZED CERAMIC MANUFACTURING IN SOUTHERN TUSCANY (ITALY): EVIDENCE OF TECHNOLOGICAL CONTINUITY THROUGHOUT THE MEDIEVAL PERIOD (10TH–14TH CENTURIES)*

Archaeometric investigation allowed the characterization of two important classes of ceramics: ‘vetrina sparsa’ and ‘invetriata grezza’. Their archaeological peculiarity makes them particularly suited for tracing the evolution of glaze manufacturing in southern Tuscany throughout the medieval period (10th–14th centuries). These ceramics were found in different sites of historical importance, and also from a mining perspective. Local copper, lead, zinc and iron mineralizations supported the growth of several settlements in the vicinity of the mines. The many castles and different archaeological finds (ceramics, glazed ceramic, slag etc.) attest to the intense mineral exploitation of the area from at least the first millennium bc up to the modern period. In light of these geological and archaeological characteristics, archaeometric investigation was intended to provide insight into ancient technical knowledge of ceramic glazing and to determine the source area for raw materials in the medieval period (10th–14th centuries). Ceramic bodies were analysed through OM, XRDp, SEM–EDS and XRF, while coatings were investigated through SEM–EDS. Mineralogical, petrographic and chemical analyses revealed slightly different preparation and firing processes for the two classes of ceramics. These data suggest the continuity through the centuries of the ‘vetrina sparsa’ and ‘invetriata grezza’ production technology. The mineralogical phases, such as monazite, xenotime, zircon, barite, Ti oxide, ilmenite, titanite, tourmaline and ilvaite, and the lithic (intrusive and volcanic) fragments detected within the ceramic bodies suggest a source area in the vicinity of the Campiglia mining district. Lastly, the presence of Cu–Zn–Pb (Ag) and Fe sulphide mineralizations (materials used to produce glaze) in the area supports the hypothesis of local manufacture.     

Middle Bronze Age Arsenical Copper Alloys in Southern Portugal

In the Iberian Peninsula, the copper metallurgy from the Chalcolithic to the Middle Bronze Age (MBA) was mostly characterized by low arsenic contents. A collection of 53 MBA artefacts from southern Portugal was analysed by micro‐EDXRF, optical microscopy, SEM–EDS and Vickers to investigate the metal composition and manufacture. No technological distinction was found between artefacts from domestic and funerary contexts, which were radiocarbon‐dated to 2000–1500 cal bc . The arsenic contents of almost 100 MBA artefacts from this region, including the above‐mentioned set, have a Gaussian distribution with a high average (3.9 wt% As). Possible explanations are discussed for this distinctive metallurgy at the south‐western end of the Iberian Peninsula.     

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.     

ANALYTICAL CHARACTERIZATION OF ROMAN PLASTERS OF THE ‘DOMUS FARINI’ IN MODENA*

The paper refers to the analytical characterization of Roman painted plasters dating back to the second century ad . The following techniques were used: optical microscopy (OM), scanning electron microscopy (SEM–EDS), micro‐Raman and Fourier transform infrared spectroscopies (µ‐Raman and FT–IR), X‐ray diffraction (XRPD), colorimetry and thermal analyses (TG/DTA). The investigation analysed the chemical composition and structure of the plasters, the chemical composition of the pigment layers, the use of binders and any chemical alteration of pigments as well as deterioration of the samples. Stratigraphic analysis of plasters allowed identification of their individual components, which proved helpful in finding out more about the mural painting technique employed.