Anthropological and physicochemical investigation of the burnt remains of Tomb IX in the ‘Sa Figu’ hypogeal necropolis (Sassari,Italy) – Early Bronze Age

Excavations carried out in Tomb IX of the hypogeic necropolis of ‘Sa Figu’, near the village of Ittiri (Sassari, Italy), supplied burnt human bone remains and pottery unambiguously referred to the Early Bronze Age (characterised by the local culture of ‘Bonnannaro’). Besides the anthropological study, we have investigated and evaluated the possibility of a funerary cremation practice in Sardinian pre‐history, a subject that has previously not been considered from a scientific point of view. Making use of a calibration procedure based on X‐ray diffraction (XRD) line‐broadening analysis, related to the microstructural properties, it was possible to estimate the combustion temperature to which the fragmented bones were subjected. It was found that the studied bones reached temperatures varying from 400°C up to a maximum of 850°C. This spread of values suggested inhomogeneous combustion of the bones, which seems compatible with funerary cremation practices. Copyright © 2007 John Wiley & Sons, Ltd.     

Is X-ray diffraction able to distinguish between animal and human bones?

The possibility of determining the human or animal origin of bones from the lattice parameters of their inorganic bioapatite phase, when subjected to a high temperature treatment using the powder X-ray diffraction (XRD) technique, has been explored on a wide number of specimens. Forty-two animal bones were treated in a furnace at 1100 °C for 36 min and compared to 53 cremated human bones from a range of ancient necropolises. The X-ray diffraction patterns of bioapatite were simulated using both monoclinic P21/b and hexagonal P63/m structures to verify any occurrence of phase transformation and any difference in the lattice parameters due to the model. It was determined that the differences between the a-axis and c-axis of the monoclinic and hexagonal lattice were unimportant. Some outlying values were revealed to be caused by the presence of chlorine ions diffused into the apatite structure increasing its average unit cell values. Nevertheless, our results clearly show that in terms of lattice parameters the variability of human specimens are completely overlapped by the non-human variability making the use of XRD in order to distinguish animal from human bones questionable.     

A study by thermal treatment and X-ray powder diffraction on burnt fragmented bones from tombs II,IV and IX belonging to the hypogeic necropolis of “Sa Figu” near Ittiri,Sassari (Sardinia,Italy)

In the course of an anthropological investigation of three tombs of the hypogeic necropolis of “Sa Figu” (near the village of Ittiri in North Sardinia, Italy), numerous burnt bone fragments were collected. In particular, from the whole necropolis we selected a tenth of long bones from tomb IV, a small fragment of femur from tomb II and four fragments belonging to tomb IX. The aim of this work is to determine a temperature range to which the bone fragments were heated, in order to assess a funerary cremation which was presumably used at that time to quickly and hygienically eliminate the flashy parts of deceased people rather than a purification rite with fires inside the sepulchres. We attempted to evaluate the range of temperature to which the bones were likely subjected, making a joint use of thermal treatment and powder X-ray diffraction investigations. From our X-ray line broadening results carried out with a modern approach (Rietveld method), it emerged that a group of five fragmented burnt bones (one specimen belonging to tomb IV, the other four from tomb IX) were subjected to a heat treatment in a temperature range from 600 and 750 °C. Conversely another group of bones (belonging to tombs II and IV) turned out to be subjected to temperatures not higher than 250 °C.     

Black Cyclope neritea Marine Shell Ornaments in the Upper Palaeolithic and Mesolithic of Franchthi Cave,Greece: Arguments for Intentional Heat Treatment

Abstract

The prehistoric site of Franchthi Cave yielded an exceptionally rich collection of personal ornaments. A reassessment of the Palaeolithic and Mesolithic ornaments from the site led to the hypothesis that a variable fraction of at least one type of personal ornaments, i.e. marine shell beads belonging to the species Cyclope neritea, may have been intentionally heated to change their natural whitish color to black. The limited conditions in which blackening can occur through heating, as well as comparison with the percentage of burnt land snails, animal bones, fish bones, and marine molluscan food remains in the Upper Palaeolithic and Mesolithic sequence, supports a special heat treatment for Cyclope neritea shells at Franchthi Cave.     

周原甲骨灼烧状况与风化原因研究

为了研究周原出土甲骨的灼烧状况与风化原因,用测色色差、X射线衍射、热重、扫描电镜和显微红外等多种分析手段对九种周原无字甲骨样进行了分析。结果表明,被分析样品都曾经受不同温度的灼烧,造成有机质丢失与骨头结构的破坏,这是导致甲骨风化的主要原因。出土后用酸浸泡清洗水垢,可能是导致甲骨风化的另一原因。在用于研究甲骨灼烧状况的诸多方法中,X射线衍射与扫描电镜分析两的作用突出。     

Assessing the reliability of criteria used to identify mandibles and mandibular teeth in sheep, Ovis, and goats, Capra

Criteria developed to distinguish between the mandibles and mandibular teeth of sheep and goats are evaluated using modern specimens from the collections of the National Museum of Natural History and the Field Museum of Natural History. Certain teeth prove to be quite reliable in this regard (dP3, P3, P4). Other dental elements, however, are not reliable and should not be used in dental based identifications of these closely related species (dP4, M1, and mandibular bones). Overall, the identification of sheep dentition using these criteria is more reliable than it is for goats. However, the generally greater likelihood of incorrect identification of goat teeth and mandibles means that specimens identified as sheep are likely to contain high proportion of misidentified goats. Both the proportion of remains that can only be classified as ‘Ovis-Capra’ and the proportion of incorrectly identified teeth and mandibular bones varies with age, with identifications of younger and older animals less reliable than those of animals in the 1.5–6 year age range. Reliability of identifications increases when more criteria and more elements are used. Identifications based on whole mandibles with complete tooth rows are quite reliable. However, the proportion of specimens likely to be classified as ‘Ovis-Capra’ also increases in whole mandible identifications, especially in goats. Systematic differences in the proportions of indeterminate and incorrect identifications have a significant impact on species-level dentition-based harvest profiles. Recommendations are made for the use of dentition and long bone based harvest profiles in the study of sheep and goat exploitation strategies.     

A new calibration of the XRD technique for the study of archaeological burned human remains

A new calibration of human bones as a function of programmed temperature (200–1000 °C) and time (0, 18 and 60 min) is presented and discussed in order to investigate the issues related to the study of cremated bone remains by using the powder X-ray diffraction approach. The experimental results confirm the growth of hydroxylapatite crystallites as a function of the applied temperature, with a sigmoid behaviour that has been parameterized to the experimental data points. Particularly, it was observed that the thermal treatments for 60 min anticipate of about 100 °C the effects that are otherwise observed after the treatments for 0 min. The developed procedure was subsequently applied to cremated remains of various archaeological sites of Spain and supplied precise information not only about the temperature reached during the funerary rites, but also on the presumed duration for the cremation.     

THERMAL ALTERATIONS IN ARCHAEOLOGICAL BONES*

Archaeological bones, found close to Mexico City (Tlatelcomila), with alterations due to probable thermal exposure attributed to a possible case of cannibalism, have been characterized by XRD, SAXS and SEM. It is shown how these non‐destructive techniques, which are not conventionally used in archaeological research, may provide useful information. The deterioration degree of the bone structure is quantified through parameters such as gyration radius or fractal dimension. As some of the reported modifications could be attributed to diagenesis, a discussion is presented in terms of bone crystallinity and ionic exchange. Furthermore, the hydroxyapatite crystallite size increased depending on colour: this feature is not explained by diagenesis—it can only be attributed to temperature. We conclude that the samples were thermally treated. Indeed, thermal treatment alters the structure and morphology of bone at a very fine level (microscopic and nanometric), while morphology follows the structural modifications. It is determined that the studied human bones were treated at three different temperatures close to 100, 250 and 600°C. Therefore, they were either boiled (barbacoa) or grilled.     

Early hominid hunting,butchering, and carcass-processing behaviors: Approaches to the fossil record

A major aim of paleoanthropology is to learn what ancient behaviors were related to the acquisition, processing, and consumption of meat and when these behaviors arose. For this reason, studies focusing on purported early hominid hunting and butchery sites are important if rigorous criteria for recognizing such sites are used. Different criteria currently used as evidence of hominid involvement with ancient bones are reviewed and it is concluded that the presence of cutmarks, verified by scanning electron microscope (SEM) inspection, is the most reliable. Successful application of this criterion depends upon a thorough knowledge of the normal variations in microscopic morphology of different types of marks that are found on bones. Therefore, variations in microscopic and gross morphology within and among a large sample of known stone tool cutmarks, carnivore tooth scratches, and rodent gnawing marks are documented. The effects of sedimentary abrasion, as caused by fluvial transport of bones, are also presented. Guidelines are presented for using microscopic criteria to identify unknown marks on fossils and possible applications of this approach are discussed. Further, it is suggested that evidence of hominid carcass-processing activities can be placed into one of three ranked categories of certainty according to the type of data used. Explicitly stating the category and type of evidence used to deduce hominid activities, and by extension to define site types (i.e., butchery, kill, base camp), may improve the clarity of hypotheses about and interpretations of early hominid behaviors.     

Bone Degradation and Environment: Understanding,Assessing and Conducting Archaeological Experiments Using Modern Animal Bones

Archaeological experiments that use modern bones to replicate past animal bone assemblages have often failed to consider the effects of environment, storage and preparation on modern bones. Often, these experiments make little mention of the conditions to which bones were subject during their storage and preparation for use in experiments. In other instances, these variables are reported but not considered as factors that contribute to the nature of the results obtained. This study considers previously reported data concerning the degradation of frozen bones (−20°C), and bones exposed to hot, dry conditions (40°C), and presents new data for bones exposed to room temperature environments (22°C) and refrigerated environments (2°C), and bones that are frozen (−20°C) and then thawed (22°C). These conditions are all relevant to understanding the nature of bone degradation and the use of bones in modern archaeological experimentation. This article also surveys a range of previously reported experiments that utilise modern bones to create analogies to the past and considers different methodological approaches and their relationship to the condition of bones at the time of their fracture and fragmentation. The longitudinal data presented in this study demonstrate differential rates of bone degradation over time in various environmental conditions. This degradation results in dramatic changes in bone fracture morphology, bone strength and utility for bone tool production. These observations have significant implications for experiments that utilise modern bones, especially when experimental data are used to create analogies to the archaeological past. Copyright © 2012 John Wiley & Sons, Ltd.     

Taphonomy of Burnt Burials: Spatial Analysis of Bone Fragments in Their Secondary Deposition

Examining recently excavated burnt burials, we explore the potential of spatial analysis to contribute to the understanding of changes that human body goes through during burning and relocation to the place of secondary deposition. Artificial heat decomposition of a body is a complex process that consists of several stages of intentional manipulation with the body. Each stage can be biased by several accidental factors which then significantly change the final archaeological record. We focussed on the post‐burning stage, especially the pathways of bone fragments to secondary deposition. We investigated spatial distribution and weight of bones in urns and pits and asked whether it is possible to observe their intentional arrangement. The trend of bone arrangement could be distinguished in most cases. Bones of peripheral parts of body were typically situated at the bottom; skull bones were usually concentrated in the upper part. However, the weight underrepresentation of all investigated burials was apparent. Deposition of selected burnt bones suggests their careful collection from the pyre and complex post‐mortem manipulation. Our detailed analysis aims to reconstruct particular steps executed during funeral rites of past populations. Copyright © 2016 John Wiley & Sons, Ltd.     

An Investigation of Possible Fluorosis in Human Dentition Using Synchrotron Radiation

Macroscopic analysis of collections of archaeological human dentition from sites in the United Arab Emirates varying in chronological age and geographical location revealed the presence of enamel defects on the buccal, lingual and occlusal surfaces of some of the teeth. The morphology of these enamel defects suggested a possible diagnoses of fluorosis. Because not all teeth in the samples studied exhibited the defect, a conclusive diagnosis could not, however, be offered. Given that fluoride can enter the crystal lattice of hydroxyapatite (the major mineral component of calcified tissue including bones and teeth), and that the uptake of higher than optimal levels of fluoride can alter the molecular structure of dentition, it was thought that the application of X-ray diffraction to this problem may aid a more conclusive diagnoses. This paper details the application of synchrotron radiation to this problem. Initially, details of the archaeological problem are outlined. This is followed by a discussion of synchrotron radiation and the advantages it has over conventional X-rays. The materials and methods used in the analysis are provided, followed by a discussion of the results. While further work is required to fully attribute the enamel defects to the effects of fluoride, this paper illustrates that synchrotron radiation, in particular X-ray diffraction, can be applied to archaeological materials as a means of quickly and effectively obtaining a structural analysis.     

苏家村遗址烧土样品的过火温度研究

烧土制品作为最早的人工建筑材料,使人类的居住环境得到了根本性的改善。然而,学界关于烧土建筑的成因存在人为烘烤处理、缘自火焚、废弃习俗等多种观点。通过科技手段研究烧土制品的过火温度,有助于科学分析烧土建筑的成因,探讨与之相关的建筑工艺,丰富史前建筑史研究。磁学研究表明,考古遗址中的土壤及其他沉积物在受热后新生成了磁铁矿、磁赤铁矿等强磁性矿物导致磁性显著增强,且矿物成分和磁性几乎不会再发生变化;但当重烧的温度接近或大于原始烧成温度时,样品中原始矿物的破坏或新矿物的生成,会引起矿物磁性的改变。基于这一原理,实验室内分析受热黏土的磁化率随再加热温度的变化特征,可反映烧土制品的过火温度。苏家村遗址是大汶口文化晚期至龙山文化中期早段一处重要的聚落遗址,遗址中第5层为厚约20～40 cm的红烧土层且覆盖整个遗址,推测为房屋倒塌造成的建筑垃圾堆积层或人为堆积层,出土大量烧土块。本研究利用X射线衍射分析法、X射线荧光光谱分析法和磁化率法等对苏家村遗址出土的烧土样品开展了组成及构造特征和样品的过火温度的综合分析。结果表明,苏家村遗址烧土样品中的白灰层中人为地添加了白色陶土原料,土层中有意地添加了植物残骸作...     

Biochemical and physical correlates of DNA contamination in archaeological human bones and teeth excavated at Matera,Italy

The majority of ancient DNA studies on human specimens have utilised teeth and bone as a source of genetic material. In this study the levels of endogenous contamination (i.e. present within the sample prior to sampling for the DNA analysis) are assessed within human bone and teeth specimens sampled from the cemetery of Santa Lucia alle Malve, Matera, Italy. This site is of exceptional interest, because the samples have been assayed for 18 measures of biochemical and physical preservation, and it is the only one identified in a study of more than 107 animal and 154 human bones from 43 sites across Europe, where a significant number of human bones was well preserved. The findings demonstrate several important issues: (a) although teeth are more resilient to contamination than bone, both are readily contaminated (presumably through handling or washing), and (b) once contaminated in this way, both are difficult (if not impossible) to decontaminate. Furthermore, although assessed on bone samples, several of the specific biochemical and physical characteristics that describe overall sample preservation, levels of microbial attack and related increases in sample porosity directly correlate with the presence of observable contamination in both bone and teeth samples from individual samples. While we can only speculate on the cause of this relationship, we posit that they provide useful guides for the assessment of whether samples are likely to be contaminated or not.     

Cooked Bones? Method and Practice for Identifying Bones Treated at Low Temperature

Is it possible to determine low‐temperature cooking in archaeological bones? The indirect exposure of bones to fire at low temperature (≤ 100 °C), linked to cooking, produces macroscopic modifications on these bones. These modifications have not been clearly or systematically described previously. Instead, physicochemical changes at nanometric level are only now beginning to be understood. In this paper, our principle aim is to explore new methods and techniques that correlate macroscopic features such as smoothness or light transparency with physicochemical characterization results that could aid towards detecting cooked bones in the archaeological record. This study then selected 11 archaeological samples, both human and non‐human. Bones were considered to be thermally treated or not, on the basis of macroscopic criteria. Complementary characterization techniques were used to study morphology (scanning electron microscopy and small angle X‐ray scattering), structure (X‐ray diffraction and transmission electron microscopy), local composition (energy‐dispersive X‐ray spectroscopy) and texture (gas adsorption). Indeed, fractal dimension, particle size, crystalline percentage or specific surface area may well explain some of the macroscopically observed modifications on these samples. The possibility that such apparent modifications may also be due to diagenesis is also considered. From an archaeological point of view, the results are promising. Our characterization of human and non‐human bones demonstrates that physicochemical techniques are complementary and provide good criteria against which to distinguish boiled from un‐boiled archaeological samples. Copyright © 2013 John Wiley & Sons, Ltd.     

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.     

Well preserved non‐collagenous extracellular matrix proteins in ancient human bone and teeth

Ancient bones in a good preservation state, ascertained by microscopic techniques, conserve extracellular matrix proteins over thousands of years. With new techniques, intact extracellular matrix proteins from ancient bones and teeth are extracted and separated by one‐dimensional and two‐dimensional electrophoresis. Proteins were identified in Western blots by special antibodies against different human extracellular matrix (ECM) molecules of bone. We have confirmed different types of ECM human bone molecules such as osteonectin, osteopontin, and alkaline phosphatase with specific antibodies in human bone samples from different age groups. Additionally, we selected bone samples from different cultural time periods, such as the Middle Ages, the Bronze Age and the Late Pre‐Pottery Neolithic Phase (PPNB), and teeth from individuals from the Early Middle Ages and from the Late PPNB. The survival of intact extracellular matrix proteins in ancient bones and teeth dating from recent times to the Late PPNB, and reliable techniques to identify these proteins, present a great challenge to further research. A Match Set with PD‐Quest 7.2 shows that only 16% of protein spots in the teeth are also found in the bone of the same individual. In combination with the results of macro‐ and microscopic investigation, biochemical techniques will help us in obtaining a better understanding of bone and teeth in health and disease. Copyright © 2006 John Wiley & Sons, Ltd.     

Pottery firing temperatures: a new method for determining the firing temperature of ceramics and burnt clay

A new method for determining the maximum firing temperature of ceramics and burnt clay is presented. The technique relies on measuring the magnetic susceptibility on a step-wise re-fired sample. The validity of the method has been tested by determining firing temperatures of two sets of clay samples fired at temperatures ranging from 400 to 1000 °C. Aliquots of the same samples have been studied petrographically by optical microscopy on thin sections and analyzed by powder X-ray diffraction in order to monitor structural and mineralogical changes as a function of temperature. The method is demonstrated on samples from four geographically widely different sites and it is applied to a larger set of ceramics of Late (ca. AD 900–AD 1450) and Inca (ca. AD 1480–AD 1532) periods from the Northwestern Argentine region, dating to a limited period of time prior to the fall of the Inca Empire. The method is shown to be a powerful tool in revealing archaeological information about the change in firing technologies in the pre-Hispanic societies in the Andean area through time.     

Stable carbon- and nitrogen-isotope ratios and electron spin resonance (ESR) g-values of charred bones: changes with heating and a critical evaluation of the utility of g-values for reconstructing thermal history and original isotope ratios

Changes in the stable carbon and nitrogen isotope ratios of modern bone samples heated to a variety of times and temperatures were used to determine the effect of heating on isotope ratios and the retention of organic matter in charred bones. For organic extracts produced by slow demineralization in weak acid, δ¹³C values were unchanged, while δ¹⁵N values increased by up to 5‰ and were primarily determined by heating temperature. Changes in the electron spin resonance (ESR) g-value of whole bone and organic extracts were also measured. For organic extracts from charred bones, the g-value was well-correlated with δ¹⁵N and temperature, suggesting that g-values could be used to estimate the charring temperature and original δ¹⁵N values of charred bones. Thus, g-values from demineralized extracts could be very useful in forensic investigations where it would important to reconstruct the thermal history of burned bones. Isotope ratios and g-values of demineralized extracts from four prehistoric components at three sites that produced cremated human bone were used to test whether the same approach can be applied to archaeological materials. While carbon isotope ratios of the prehistoric samples were similar to those of uncharred specimens, nitrogen isotope ratios were increased and the g-value corrections for nitrogen isotope ratios were not effective.     

Charcoal scarcity in Epigravettian settlements with mammoth bone dwellings: the taphonomic evidence from Mezhyrich (Ukraine)

Fuel management during the Paleolithic periods is an important issue to understand past human subsistence. Numerous Palaeolithic sites relate an abundance of burnt bones in hearths and an absence or scarcity of wood charcoals, which leads studies to focus on burnt bone remains and the use of bones in hearths. Few works take into account the micro-residues of wood charcoals which can still be present in hearth areas and excavated sediments. We studied the Epigravettian site with mammoth bone dwellings of Mezhyrich (Ukraine) previously characterized by its high content of burnt bones and an “absence” of wood charcoal during the so-called mammoth steppe. The presence or absence and proportions of both wood charcoals and burnt bones were quantified in macro-, meso- and microscale sediment size fractions by an image analysis method. Our results show that excavations during field-works at Mezhyrich give only a partial image of the original anthracological record and that most charcoal materials are lost with standard archaeological and anthracological approaches. The scarcity of charcoals in this site was possibly due to an important mass reduction accentuated by the addition of bones in hearths. By applying our protocol we recovered a significant amount of wood charcoals which provides the first ¹⁴C dates from charcoals at Mezhyrich. Numerous charcoals are identified contributing subsequent information about vegetation, environment and burning practices. They indicate, by comparison with pollen data already collected, the presence of forest patches in a mammoth steppe landscape, which might have influenced the collecting behavior of Epigravettian populations.