The origin of black pigmentation in a sample of Mexican prehispanic human bones

The study of black patches and spots in prehispanic bones of Tlatelolco and Tlapacoya is presented. The chosen characterization techniques, X-ray Fluorescence, X-ray Diffraction, Scanning Electron Microscopy, Energy Dispersive X-ray Spectroscopy, Infrared Spectroscopy and Gas Chromatography are complementary and they all conclude that the bone black pigment is constituted, mainly, by amorphous carbon and some mineral inclusions. Gas Chromatography and Infrared Spectroscopy show that the pigment is constituted by organic compounds as aromatic hydrocarbons, mainly bitumen. An explanation on how the spots were formed is proposed.     

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.     

Building an Experimental Comparative Reference Collection for Lithic Micro-Residue Analysis Based on a Multi-Analytical Approach

Residue analysis applied to stone tools is a useful aid for better understanding their past function and, by extension, reconstructing early human behaviour. However, if the nature of residues found on the lithic tools is misinterpreted, so will be our understanding of their archaeological context. As a consequence, correctly identifying residues in the domain of lithic studies is of paramount importance. With this main goal in mind, we analysed different experimental materials likely to have been involved in daily tasks in the prehistoric context (e.g. bone, wood, meat). Microscopic analyses were then carried out using two (comparable) techniques: Optical Light Microscopy and Scanning Electron Microscopy. Also, energy dispersive X-rays spectroscopy (EDX or EDS) was applied to the experimental samples to determine their elemental composition. Advantages and disadvantages of both microscopic methods and their implications for correct residue identification are discussed. The distribution of residues on lithic surfaces is also considered. This study resulted in the construction of a data-set including both photographic material and EDX spectra for each residue analysed. The main result is that, compared to OLM scanning, SEM analyses highly improves the accuracy of residue identification.     

Identification of materials in post-Byzantine textiles from Mount Athos

Numerous textiles of inestimable historical significance have been preserved in the monasteries of Mount Athos for several centuries. However, our knowledge regarding the materials used in these objects is very limited. In the present study, microsamples extracted from ecclesiastical textiles (16th – 19th c.) of the monastery of Xeropotamou (Mount Athos) are investigated using Optical Microscopy (OM), Fourier Transform Infrared Spectroscopy (FTIR), High Performance Liquid Chromatography coupled to a Photodiode Array Detector (HPLC-PDA) and Scanning Electron Microscopy equipped with an Energy Dispersive X-ray spectrometer (SEM-EDX). The first goal of the study is to identify the colouring materials of the historical samples, which were of silk nature (OM). The presence of Prussian blue is revealed using FTIR and organic colourants such as cochineal, dyer’s broom (Genista tinctoria L.), fuchsin, indigo carmine, old fustic (Chlorophora tinctoria L.), soluble redwood (Caesalpinia trees), weld (Reseda luteola L.), young fustic (Cotinus coggygria Scop.) and indigoid dyestuff source(s) are identified using HPLC-PDA. Dyestuff extraction from silk substrates is achieved using the TFA method, which preserves the contained glycosides. Thus, the report provides further evidence to support the efficacy of the TFA method to extract various organic colourants from historical silk samples (second goal). Finally, metal threads included in some historical samples are studied using OM and SEM-EDX. The latter is employed to analyse the composition of the metal surfaces. Silver (Ag) and gold (Au) are detected on the surfaces of the majority of the samples. Two samples were manufactured only with Ag.     

北周武帝孝陵出土铜器的焊接模拟实验研究

为研究出土铜器的焊接技术,但文献中仅有少量关于铜焊的记载,而且模拟实验研究少有进行,因此,进行了实验室焊接工艺的模拟研究。以北周武帝孝陵出土铜器中检测发现的焊料为依据,进行了相关的焊接模拟实验研究,并利用金相显微镜、扫描电子显微镜及X射线能谱分析仪分别对铜锡合金、纯锡焊接红铜样品进行了检测分析,结合结果的分析与讨论,排除了焊料为纯锡的可能性,进一步证实了孝陵发现的焊料为铜锡合金焊料。本研究开展的铜焊模拟实验为日后系统研究铜焊技术具有一定的参考与借鉴意义。     

钴蓝颜料（Smalt）在故宫建福宫彩画中的发现

钴蓝颜料（Smalt）是一种产自欧洲的进口蓝色颜料,是一种经过研磨的钴玻璃粉末,从十五世纪中叶开始广泛用于欧洲油画与壁画中。在故宫的建福宫中发现有这种钴蓝颜料（Smalt）。但在明清文献中,钴蓝颜料（Smalt）尚无明确记载。本文主要对始建于乾隆七年（公元1742年）的建福宫内檐脊枋彩画进行了调查和采样,采用显微镜分析和显微激光拉曼光谱分析蓝色颜料的种类和彩画结构,特别是钴蓝颜料（Smalt）使用的时代和分布进行了认真的研究。分析结果表明：建福宫建造时,靛蓝是一种经常使用的蓝色颜料,故宫建福宫钴蓝（Smalt）颜料的使用时代晚于建筑的建成年代（公元1742年）,而且一般与颗粒大小接近的石青混用。     

Pigments from the Middle Palaeolithic levels of Es-Skhul (Mount Carmel,Israel)

Discovery of pigments at Middle Palaeolithic sites is of interest in the context of the ongoing debate about the tempo and mode of the emergence of modern human behaviour. Here we analyse four previously undescribed fragments of pigmental material from Es-Skhul shelter, layer B, Israel, McCown excavations, identified at the Department of Palaeontology, Natural History Museum, London. One of them is still partially embedded in the hard breccia characteristic of this layer. Inspection of breccia fragments from layer B has led to the identification of small pieces of red and orange pigmental material still enclosed in large clasts, further corroborating the attribution of the larger pieces analysed in this study to layer B. The four objects are studied using optical microscopy, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Energy Dispersive X-ray (EDX), X-ray micro-diffraction (μ-XRD), Particle-Induced X-Ray Emission Spectrometry (PIXE), and Proton-Induced Gamma-ray Emission (PIGE). The specimens display various hues of yellow, orange, red, and one of them presents a gradual variation of shade from yellow to dark orange. SEM/EDX analysis identifies two specimens (Skhul 1 and 2) as being composed of iron-rich calcium phosphate, the third (Skhul 3) of potassium-rich clay with titanium-rich iron oxide inclusions, and the fourth (Skhul 4) of pure iron oxide crystals. TEM/EDX and μ-XRD analysis demonstrate that three pieces (Skhul 1, 2 and 4) were heated to at least 300 °C, a process that has partially or completely dehydrated goethite into haematite and changed their pristine yellow colour into orange or red. Skhul 3 shows no sign of heating, suggesting that its haematite content has a geological origin. The different mineral composition of the pieces suggests that they must come from a variety of sources. This implies that the associated collection strategies included the selection of materials that differed not only with respect to colour but also with respect to other physical and chemical properties. Although no formal proof exists that these lumps of pigmental material were deliberately heated, results obtained are consistent with this explanation.     

Analytical characterization of lacquer objects excavated from a Chu tomb in China

This work presents the results of an investigation of the lacquer objects excavated from a Chu tomb in China (Warring States, 481–221 BC). This study is engaged in the examination of the methods and the materials used for the urushi coating on the objects. X-Ray fluorescence and Scanning Electron Microscopy/Energy Dispersive Using X-Ray (SEM/EDX) analyses were applied for the pigment identification. The results show that vermilion was for the red colour, while carbon black was for the black colour. Pyrolysis gas chromatography and mass spectrometry (Py-GC/MS) was applied for the characterization of the lacquer resulting that it is based on urushi. The possibility to classify the drying oil (tung or linseed oil) present in the lacquer is highlighted and discussed in this paper. Py-GC/MS with in-situ hydrolysis and methylation reagent tetramethylammonium hydroxide (TMAH) were performed on reference materials of linseed oil and tung oil as well as on the lacquer object samples. The results show that it is possible to unambiguously identify the drying oil, in our case, linseed oil was identified to retard the rate of hardening.     

A hoard of Nilotic nacreous shells from Egypt to Jericho (Early Bronze II, 3000–2800 BCE): Their finding,content and historical archaeological implications

ABSTRACT

The Tell es-Sultan, ancient Jericho, is amongst the earliest “cities” that rose in the Southern Levant between the end of 4th and the beginning of the 3rd millennium BCE. The site is being excavated, studied and rehabilitated for tourism by Sapienza University of Rome and the Palestinian Ministry of Tourism and Antiquities since 1997. In 2017, during the 13th season of excavation, an unexpected discovery occurred: five Chambardia rubens shells have been found piled up in a dwelling unit dating back to the Early Bronze Age IB-II. The discovery is a tangible evidence of trade and cultural interconnections between the Southern Levant and Egypt, as these shells belong to a species that is only been found to live in the Nile. Moreover, chemical analysis, and thorough Scanning Electron Microscopy examination revealed that the shells contained Manganese Dioxide, an inorganic compound used as make-up ingredient in ancient Egypt, and available in the ores of the Sinai. These findings strongly support the existence of a link between the urban rise in EB IB-II through international trade of luxury goods, and are suggestive of the emergence at Jericho of a ruling elite that was influenced by Egypt.     

Microwear study of quartzite artefacts: preliminary results from the Middle Pleistocene site of Payre (South-eastern France)

Preliminary functional results obtained from the quartzite assemblage of the Early Middle Palaeolithic site of Payre (South-eastern France) are presented. In an area rich in flint, hominins at Payre also collected quartzite in their local environment, specifically along the Rhône River banks. Although the Payre lithic assemblage is largely composed of flint, quartzite was introduced in the site mainly as large cutting tools knapped outside. This fact pointed out an apparently highly differential treatment of the raw material types available in the region. A major concern is to understand the reason why. Is there any functional reason for the introduction of those artefacts, perhaps to perform specific activities related to the toughness of quartzite? Or is there any functional differentiation among the various raw materials? Use-wear analysis is a useful tool for better understanding human technological choices and strategies of lithic raw material management. Before attempting to extensively apply use-wear analysis on the quartzite assemblage, we analysed a limited sample to evaluate the general surface preservation. A specific experimental programme with the same local quartzite was carried out in order to provide a reliable comparative reference for interpreting use-wear evidence on archaeological implements. Methodological difficulties related to use-wear analysis applied to quartzite artefacts are also discussed. Both Optical light microscopy (OLM) and Scanning Electron Microscopy (SEM) were employed in this study; however, interpretations were elaborated considering principally SEM micro-graphs.The analysis of the archaeological material showed a good state of preservation of the surfaces with a low incidence of post-depositional alterations. The documented use-wear allowed us to identify the active edges, the kinematics and, more rarely, the worked material. Chopping activities were documented on two large artefacts suggesting a specific utility of those tools.     

Dendrochemical analysis of a tree-ring growth anomaly associated with the Late Bronze Age eruption of Thera

The most marked tree-ring growth anomaly in the Aegean dendrochronological record over the last 9000 years occurs in the mid 17th century BC, and has been speculatively correlated with the impact of the Late Bronze Age eruption of Thera (Santorini). If such a connection could be proved it would be of major interdisciplinary significance. It would open up the possibility of a precise date for a key archaeological, geological and environmental marker horizon, and offer a direct tie between tree-ring and ice-core records some 3600 years ago. A volcanic explanation for the anomaly is highly plausible, yet, in the absence of a scientifically proven causal connection, the value of the proposed correlation is limited. In order to test the hypothesis, dendrochemical analysis via Synchrotron Radiation Scanning X-ray Fluorescence Microscopy (SXFM), Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) was carried out on growth-ring series from four trees displaying the anomaly. Increases of sulfur, calcium, and rare earth elements following the onset of altered growth, plus concentration spikes of zinc and hafnium in the first affected growth-ring provide promising new evidence in support of a volcanic causal factor. Although a volcanic association is implied, the new data are not sufficient to prove a link to the exact eruption source.     

Egyptian faience glazing by the cementation method part 1: an investigation of the glazing powder composition and glazing mechanism

In cementation glazing, for various reasons, there are significant differences between the composition of the glass phases present in the faience microstructure and the glazing powder composition. Furthermore, in this glazing method, the glazing powder should perform more functions, which are: producing a shiny and smooth glaze coating, producing a firm capsule surrounding objects entirely (to prevent adhesion between sintered glazing mixture and the melting glaze coating), and, finally, producing a porous and friable sintered glazing mixture for safe and easy removal of buried objects. It is obvious that these functions also have significant effects on the glazing powder composition and constitution. Therefore, analytical data on faience glass phases are very unlikely to reflect the strict composition and constitution of the original glazing powder properly. Accordingly, the composition and constitution of cementation glazing powder have remained obscure for a long time. These data are particularly crucial factors for cementation replication experiments and, consequently, for our awareness of the ancient faience production. In this paper, a series of cementation replication experiments have been conducted in an attempt to provide further clarification of these issues. In addition, as a comparative indicator for alkali and copper vaporisation, a small piece of rock quartz was placed separately above the glazing powder. After firing, the appearance of the faience objects and quartz pieces and the microstructures and chemical compositions of a select group of samples, obtained using Scanning Electron Microscopy – Energy Dispersive Spectroscopy (SEM-EDS), were investigated. The discussion has focused mainly on issues such as the raw materials and their contribution in the glazing process, the criteria for determining the faience glazing methods, the necessary quantity of alkalis for a successful cementation glazing, and, particularly, the glazing mechanism.     

The Influence of Soil Moisture,Temperature and Oxygen on the Oxic Decay of Organic Archaeological Deposits

The sensitivity of organic‐rich archaeological layers at Bryggen in Bergen, Norway, to changes in soil temperatures, water contents and oxygen concentrations is investigated. This is done by linking measurements of oxic decay at varying temperatures and water contents with on‐site monitoring data using a one‐pool decomposition model. The results show that the model can be used to elucidate the current in situ decay and to evaluate where and when the decay takes place. Future investigations need to include long‐term incubation experiments and decay studies at zero or very low oxygen contents in order to improve the robustness of predictions.     

Remains of the day-preservation of organic micro-residues on stone tools

Here I report on the decay processes of microscopic organic residues left on stone tool surfaces after their use. Residue analysis on ancient stone tools facilitates reconstruction of past activities. This study enables predictions about the circumstances under which ancient residues preserve. Experimental tool sets with modern residues were buried for a year in separate deposits at Sterkfontein, Sibudu (South Africa) and Zelhem (the Netherlands) whose pH and geomorphology varied, they were then analysed using light microscopy. Biological weathering mainly causes residue decay. In unstable environments rich in microbes and micro-organisms, residues decay quickly. From an archaeological perspective this means that sites that are stable, desiccated, waterlogged, extremely acidic or alkaline and extremely cold or hot sites. Different residue types have different preservation optima and this may lead to a preservation and perhaps interpretation bias. The preliminary predictive models presented in this paper could aid in the considered selection of sites and samples.     

Geochemical and mineralogical analysis of stone anchors from west coast of India: provenance study using thin sections,XRF and SEM-EDS

Stone anchors have been recovered along the Indian coast as a part of the maritime archaeological studies at the National Institute of Oceanography (NIO), Goa. Study of stone anchors provides clues to understand the ancient maritime trade contacts of India with other countries. These anchors resemble those found in the Mediterranean Sea, Persian Gulf and Red Sea Coast. Underwater explorations at Bet Dwarka, Dwarka, Goa, Visawada and Somnath have yielded stone anchors of widely varying shapes, sizes and weights ranging between 16 and 410 kg. Sixteen (10 Indo-Arabian, 4 Ringstone and 2 Single hole type) of the total of 269 stone anchors have been studied to determine provenance of rock through petrographic analysis using thin section studies, X-ray Fluorescence (XRF), and Scanning Electron Microscope – Energy Dispersive Spectrometer (SEM-EDS).     

A new approach to recording and monitoring wet-preserved archaeological wood using three-dimensional laser scanning

The analysis and preservation of organic materials preserved within wetland environments represents one of the most costly parts of any post-excavation strategy. This paper outlines the application of high-resolution terrestrial laser scanning to one class of preserved material, worked archaeological wood. Scanning allowed the recording of the artefacts in three dimensions and the identification of features such as toolmarks. Features can be measured and volumetrically modelled within the digital environment, which may not always be possible for these often fragile materials using conventional techniques. Repeat scanning of the artefacts provided an opportunity to use comparative analysis software to investigate changes in the morphology of artefacts under contrasting conditions of short-term storage. The results suggest that immersion in water results in the least deterioration, whereas both freezing and air-drying caused distortion and degradation. This paper demonstrates that laser scanning provides a viable alternative post-excavation method for the recording, analysis and long-term ‘virtual archiving’ of organic archaeological materials, which may be more cost-effective in some instances than other methods of preservation.     

Efficient but destructive: a test of the dental wash technique using secondary electron microscopy

The Boyadjian et al dental wash technique provides, in certain contexts, the only chance to analyze and quantify the use of plants by past populations and is therefore an important milestone for the reconstruction of paleodiet. With this paper we present recent investigations and results upon the influence of this method on teeth. A series of six teeth from a three thousand years old Brazilian shellmound (Jabuticabeira II) was examined before and after dental wash. The main focus was documenting the alteration of the surfaces and microstructures. The status of all teeth were documented using macrophotography, optical light microscopy, and atmospheric Secondary Electron Microscopy (aSEM) prior and after applying the dental wash technique. The comparison of pictures taken before and after dental wash showed the different degrees of variation and damage done to the teeth but, also, provided additional information about microstructures, which have not been visible before. Consequently we suggest that dental wash should only be carried out, if absolutely necessary, after dental pathology, dental morphology and microwear studies have been accomplished.     

Salt Effects in Plastered and Unplastered Outdoors Brick Masonry: Quantitative Laser Monitoring of Surface Decay Evolution

In masonry materials, the superficial decay is a widespread problem. Aggressive environmental agents such as moisture and salts trigger the damage by propagating through the material capillary pores. Although several studies have been carried out on salt crystallization and their damaging effects, additional research effort is required to better investigate this phenomenon on real cases and real weathering conditions. To this purpose, testing and monitoring tools capable of following degradation process since the early beginning are necessary. Repeated visual inspections are commonly used to monitor the superficial decay, but this technique is subjective and thus not capable of providing any quantitative information. In this work, an experimental campaign, carried out in Bologna, Italy, is presented. A two-header brick wall, one main face unplastered and one plastered, was stored outdoors and exposed to weathering over two summers. Before the start of the second aging season, moisture and salt capillary rise was simulated by low-concentrated sodium chloride solution (0.1% -wt). The aim was to favor solution evaporation and salt crystallization and to provoke material damage. The degradation process was monitored based on a contactless, rapid and accurate image diagnostic technique. In particular, high-resolution laser scanning by triangulation technique was adopted. Three-dimensional data acquisition was repeated at the end of both seasons. The proposed procedure successfully extracted quantitative information approximately areas of material spalling and detachment even in the initial phases of decay.     

Relax,Don’t Do It: A Future for Archaeological Monitoring

Preservation in situ and the monitoring of archaeological sites have become important themes since the acceptance and implementation of the Valletta Treaty. In the last few decades, our knowledge of degradation processes has increased manyfold, and a range of techniques have been tested and applied for use in both assessment and monitoring. Despite these successes, all is not well. First, we have little notion of the speed of the decay processes involved. This makes it difficult to distinguish between acute and protracted degradation. Apart from that, many assessments and subsequent monitoring projects rely (too?) heavily on complex and costly specialist technology. For any future preservation — in situ — projects low-tech observations together with best estimates of decay rates and archaeological site information should be combined to make an accurate assessment of the effects of decay on the archaeological record. Monitoring for preservation purposes is only appropriate if (1) decay processes occur within a relevant and measurable time scale, and (2) if mitigating actions can be taken or preservation ex situ can be performed (i.e. a rescue excavation) if significant degradation takes place.     

石质文物病害机理研究

导致石质文物产生病害的因素很多,其中近年来日益加剧的环境污染带来的病害加速问题引起文物保护工作者的广泛关注。精确的病害诊断是文物保护的先决条件,因此,多学科综合研究和新技术不断引进到病害机理研究方面。对各种可能的病害原因从最初的定性分析逐渐转变到定量模拟分析方面。目前,石质文物病害研究从地质勘察、室内试验、现场试验等各个方面展开,但是由于各个试验条件不同,会出现不一致,甚至相悖的结论。在对石质文物病害的研究现状进行了总结后,认为试验体系标准的制定可以使得文物保护工作者的研究具有可比性,从而可以得出较具一般性的结论,这也是进行病害机理研究的基础。由于文物完整性保护的特殊要求,无损检测技术的发展及检测结果的判定是整个的试验体系中一个重要方面。同时,由于室内实验存在时间及尺寸等比例效应问题,室外长期观测试验应是今后的研究方向。最终将病害严重程度及发展趋势的判定和有效预防发展成为一个科学体系。