Characterisation and blind testing of radiocarbon dating of cremated bone

The success of radiocarbon dating of burned or cremated bones depends on the exposed temperature during burning and the degree of re-crystallisation of the inorganic bone matrix. We present a method for characterisation of likely cremated bones by employing visual inspection, infrared spectrometry and carbon stable isotope analysis on the bio-apatite fraction. The method of radiocarbon dating of cremated bones was tested by dating paired samples of bone and associated context materials such as pitch, charcoal and a dendrochronologically dated oak coffin. The dating of these paired test samples were largely performed as blind tests and showed excellent agreement between pitch and bone. The weighted mean age difference of all test samples is observed to −9 ± 60 ¹⁴C yr. To test the indicators and the effects of the degree of burning, a Late-Neolithic human individual has been studied, as this individual exhibits the full spectrum from low temperature burning (charred) to high temperature (“cremated”) from one end of a single bone to the other. This is reflected as a marked step in numerous parameters as well as in a significant difference in ¹⁴C age between the charred and the cremated bone samples.     

Crystallographic and structural transformations of sedimentary chalcedony in flint upon heat treatment

The early occurrence of intentional heat treatment of silica rocks has recently become a key element in the discussion about the cultural modernity of prehistoric populations. Lithic vestiges are the only sources that remain of this process and the understanding of the material’s properties and transformations are essential for reconstructing the conditions and parameters applied during heat treatment. Several models of the structural transformations upon heating have been proposed in the current literature. These models are often contradictory and do not account for the most recent structural and mineralogical data on chalcedony. In order to propose a new model, we elaborated an experimental procedure and applied different techniques involving infrared spectroscopy, solid state NMR, X-ray diffraction and electron microscopy. The results show that the major transformation to happen is the loss of silanole (SiOH) and the creation of new Si-O-Si bonds according to the reaction: Si?OH HO-Si → Si-O-Si + H₂O. This reaction starts between 200 °C and 300 °C and causes an increase in the hardness of the rocks. The maximal annealing temperature and the ramp rate are the functions of the ability of the structure to evacuate newly created H₂O and depend on the size of the specimen and the volume of its porosity. These results also show that the annealing duration at maximum temperature can be relatively short (<50 min) for a sufficiently large amount of transformation to be accomplished.     

Obsidian hydration dating by infrared spectroscopy: method and calibration

Low temperature (90–190 °C) hydrothermal experiments have been conducted on seven obsidians where composition of the glass varies significantly in the concentration of structural water within the unhydrated bulk material. Infrared transmission spectroscopy was used to track the diffusion of molecular water into the glass surface as a function of time and temperature. Long-term (60–360 days) hydration sequences at 90 °C show a t^0.6 time dependence for the mass uptake of molecular water that forms the hydration layer. The structural water concentration of the unhydrated bulk obsidian is highly correlated with the pre-exponential and activation energy and may be used to estimate the Arrhenius constants. In addition, secondary ion mass spectrometry (SIMS) hydrogen profiling of Napa Glass Mountain obsidian hydrated at 90 °C reveals that the early stages of diffusion exhibit a dynamic behavior that includes a fluctuating hydrogen concentration and a changing diffusion coefficient that slows with time.     

A comparative experiment in the consolidation of cremated bone

This experiment assessed whether consolidation of cremated remains facilitated cross‐sectioning and grinding, which often are required for microstructural analyses such as the histomorphometric estimation of age and the examination of pathological lesions. Green, bovine femoral diaphyses were cremated at three temperature ranges (346–357°C; 610–755°C; 684–838°C) in an electric furnace and then consolidated with Acryloid B‐72 or Butvar B‐98 using simple brushing and immersion techniques. After consolidation was complete, bone pieces were cross‐sectioned and ground to a thickness of 100–120 μm. Results indicate that specimens treated with Acryloid B‐72 are harder and stronger than Butvar treated and untreated control specimens. Acryloid B‐72 is, therefore, recommended for the consolidation of cremated remains in preparation for microstructural analysis. Copyright © 2004 John Wiley & Sons, Ltd.     

Morphological,chemical and physical changes during charcoalification of wood and its relevance to archaeological contexts

Wood exposed to a heat source can be transformed into charcoal if subject to conditions of carbonisation (in the absence of air) or charring (in restricted air). Charcoal recovered from archaeological sites can yield fundamental information to our understanding of human economic and cultural development over time and (ecological) setting. This work describes the morphological (anatomy, degree of shrinkage), physical (reflectance) and chemical (elemental, molecular composition) properties of charcoal in relation to heat source and wood variables. In this study charcoal and charcoal fuel were experimentally produced whereby temperature (160–1200 °C), time of exposure (2–1440 min), heating rate (high and low) and wood type (angiosperm and conifer) were varied. The results show that charcoal, often described as an inert, black material, has different chemical and physical properties in relation to the investigated variables. By using these different properties it is possible to distinguish between the different types of fires (domestic and industrial) exploited by humans in the past. Morphological analyses and reflectance measurements are effective tools for this purpose and can be used in wood exposed to temperatures of 300 °C and above—temperatures which are relevant to archaeological research. Angiosperm and conifer wood react in different ways when exposed to heat and thus the taxonomic identity of archaeological material needs to be known. Chemical analyses can be used for wood exposed to temperatures below 400 °C whereas elemental analyses of the carbon content can be used for wood exposed to temperatures up to a maximum of 650 °C.     

Is vitrification in charcoal a result of high temperature burning of wood?

The term ‘vitrified’ is used to describe the glassy appearance of some charcoals recovered in the archaeological record. It has been generally considered that this phenomenon is a result of wood being subjected to high temperatures similar to the role of temperature in the formation of glass and pottery. Charcoals displaying characteristics of vitrification from three distinct archaeological contexts were analysed using reflectance microscopy to determine their temperature of formation. Charcoal was also generated in laboratory charring experiments at temperatures of 900–1100 °C for durations of 1, 6, 12 and 24 h to determine if subjection to high temperature led to vitrification. None of the laboratory-produced charcoals displayed characteristics of vitrification. Mean random reflectance of the vitrified archaeological fragments indicated temperature of formation from 310 to 530 °C. A charring experiment was also conducted, at 500 °C for 6 h, using green wood with some bark attached, and added sugars, but no evidence of vitrification was seen. Therefore vitrified charcoals do not result from high temperature charring or primarily from the use of green wood.     

Going underground: experimental carbonization of fruiting structures under hearths

We show that carbonized fruits and seeds recovered from Middle Stone Age deposits in rock shelters are likely to have been carbonized as part of post-depositional processes. We buried indigenous South African fruits, nuts and seeds at pre-determined depths and distances from the centers of experimental fires. The cold ashes of the hearths and the sand surrounding them were subsequently excavated, using standard archaeological techniques and dry-screening. The fruiting structures from the oxidizing part of the fire were burnt to ashes, whereas those buried in sand under anoxic conditions survived in varying forms. Those buried 5 cm below the center of the fire were carbonized; those buried 10 cm below the center of the fire were dehydrated; and those 5 cm and 10 cm below the surface at the outer edge of the fire were unaffected. Size, moisture or oil content of the original fruit or seed did not appear to influence whether or not carbonization took place. Temperatures recorded 5 cm below the experimental fires suggest that the carbonization occurred at or before a maximum temperature of 328 °C, and also at lower maximum temperatures (152 °C) that were maintained for long periods. Even when the quantities of a particular wood are controlled, open fires may produce variable underground temperatures and the temperatures below ancient hearths would have been equally variable. We suggest that Cyperaceae (sedge) nutlets, the most numerous fruiting structures in the Sibudu Middle Stone Age archaeobotanical assemblage, occur in the shelter as a result of human activity, subsequent burial, and accidental carbonization when hearths were built directly above the buried nutlets.     

Estimation of temperatures beneath archaeological campfires using carbon stable isotope composition of soil organic matter

An Inceptisol and an Alfisol from Western Maryland were sampled by horizon and exposed to the elevated temperatures associated with heat transfer measured beneath campfires. Substantial loss in organic carbon and change in carbon stable isotope composition was observed, even after exposure to relatively low temperatures (200–400 °C). Analyses showed that a comparison of carbon isotope enrichment in organic matter beneath a suspected campfire site to that of unaltered soil would give quantitative information about the minimum effective campfire temperature. Application of these results may lead to particular insight for archaeological sites where soil surfaces have been eroded or otherwise truncated.     

‘Old wood’ effect in radiocarbon dating of prehistoric cremated bones?

Numerous reports of successful radiocarbon dating of cremated bones have emerged during the last decade. The success of radiocarbon dating cremated bones depends on the temperature during burning and the degree of recrystallisation of the inorganic bone matrix. During cremation bones undergo major morphological and mineralogical changes which have raised some interesting questions and discussion on the origin of the carbon source in archaeologically cremated bones. Recent laboratory experiments reveal that the properties of the combustion atmosphere play a significant role regarding the source carbon in cremated bones. Thus radiocarbon dating cremated bones is potentially dating the wood used for the cremation fire. Here we compare a high precision radiocarbon dated human bone with an associated dendrochronological age from an oak coffin. We find that the age discrepancy between the dendrochronological age and the cremated bone of 73 ± 26 ¹⁴C yr is best accounted for by the so called ‘old wood’ effect.     

Sorting the butchered from the boiled

Is it possible to identify cooked, rather than burnt, bone? Mild heating (≤100 °C,1 h) – typical of cooking – does not lead to detectable changes in any biochemical parameter of bone yet measured. If it is only possible to detect charred bone, how is it possible to detect cooking in the archaeological record? In a previous paper (Koon et al., 2003, J. Arch. Sci.), we used a Transmission Electron Microscopy (TEM) based approach to investigate changes in the organization of the bone protein, collagen, as it is heated, using bone from heating experiments and short term burials. The work revealed that mineralized collagen, despite requiring aggressive treatment to gelatinise the protein (e.g. 90 °C, 240+ h), readily accumulates minor damage. We believe that the presence of mineral matrix stabilises the collagen enabling the damage to accumulate, but preventing it from causing immediate gelatinisation. Once the mineral is removed, the damage can be observed using appropriate visualization methods.     

Reassessing the Age,Sex and Metric Variation of Commingled Human Remains from a 1911 Excavation of a Neolithic Passage Tomb Complex in North‐West Ireland

The Neolithic passage tomb complex at Carrowkeel, County Sligo, Ireland, is one of the best preserved and most significant megalithic funerary and ritual landscapes in Europe. The most substantial archaeological excavations at the complex were undertaken in 1911, from which a relatively large sample of commingled unburnt and cremated human remains from seven chambered passage tombs was recovered. Although the archaeological value of this material is reduced as its spatial and stratigraphic context is uncertain, the skeletal remains have the potential to provide insights into how these monuments were used. This study is a quantitative reassessment of that osteological material from the passage tombs excavated in 1911, with a focus on a contextual analysis of the remains. Overall, the age‐at‐death and sex ratios do not indicate any demographic differentiation between monuments in selecting locations for the deposition of bodies, and there is no clear evidence to suggest any selectiveness of certain skeletal elements took place. There may however have been a differentiating age and gender aspect in terms of the unburnt versus cremated bone surface depositions within the passage tombs, as a higher proportion of 5+ years non‐adults and adult females were present in the cremated material. By using the log‐ratio metric scaling technique on the cremated adult material, a statistically significant difference in skeletal dimensions is observed between individual passage tombs; however, it is unclear how significant this disparity is from a biocultural point of view. Despite apparent methodological difficulties in assessing an archaeological bone assemblage collected by early 20th‐century antiquarians, the material can still yield new knowledge about the rituals conducted at Carrowkeel. Copyright © 2016 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.     

Tracking changes in bone fracture morphology over time: environment, taphonomy, and the archaeological record

Zooarchaeologists have often employed studies of bone fracture morphology as a means of understanding past human cultural activity, and various methodological approaches have been developed for analyzing archaeological broken bone assemblages. It is widely understood that bones degrade over time, however, few studies have attempted to define and quantify the rate at which bones degrade and fracture morphologies change. This study examines degradation in frozen bones (−20 °C) and bones exposed to hot (40 °C) dry conditions. These two simulated environmental conditions represent extreme real-world climates, and allow for an actualistic understanding of the rates of degradation that bones experience in nature. When frozen, bones degrade slowly but significantly, and demonstrate measurable differences in samples frozen for 1, 10, 20, 40, and 60 weeks. In hot, dry conditions, bones degrade very quickly, and demonstrate measurable differences after 1, 3, 7, 14, and 21 days. These data allow for a more detailed understanding of the relationship between the cultural and natural processes that result in bone fracture, and the time period during which bones can be expected to maintain fresh fracture characteristics. This research also has implications for understanding human subsistence and survival strategies and for interpreting the archaeological record.     

A Unique Case of Prone Position in the Primary Cremation Tomb 252 of Monte Sirai Necropolis (Carbonia,Sardinia, Italy)

A series of graves belonging to the Phoenician period were investigated after the campaign excavation of 2007 in the Phoenician‐Punic necropolis of Monte Sirai (Carbonia, Sardinia, Italy). One tomb in particular (labelled 252) is presented here because of its uniqueness. Tomb 252 contained the cremated remains of an individual, probably male, and comparison of the excavation records alongside reconstruction of the bone material itself makes clear that the individual was cremated in a prone position. It represents the first case of prone cremation reported in the literature. To investigate whether the temperature of the cremation was homogenous across the entire body, we have conducted a combined physical–chemical analysis using X‐ray diffraction spectroscopy and Fourier transform infrared. Copyright © 2012 John Wiley & Sons, Ltd.     

Determination of the parameters of the Guildhall amphitheatre ellipse in London

The paper presents an algorithm for computing the parameters of an ellipse that fits, in a least-squares sense, the surveyed remains of Roman amphitheatre arena walls. The algorithm is validated using ideal data and the near complete remains of the amphitheatre at Sarmizegetusa in Romania. The technique is then applied to the partial remains of the amphitheatre at the Guildhall in the City of London, in the UK, which cover only the Eastern end of the monument. The underlying mathematical model and method of solution is presented. The method was developed with a view to determining firstly whether or not an ellipse is a feasible model for the actual constructed curve geometry, and secondly, where the Western end of the Guildhall amphitheatre might be located. One single ellipse was found to fit the Guildhall remains, with measurement residuals at the level of 30 mm in the eastings and 26 mm in the northings. The ellipse had a semi-major axis of 28.345 m and a semi-minor axis of 22.775 m. The issues of alternative geometries and the practicalities of their use in construction are considered.     

Distilling zinc for the Ming Dynasty: the technology of large scale zinc production in Fengdu, southwest China

Our understanding of zinc distillation technology in ancient China has traditionally been limited by a lack of studies of production remains. The discovery of nearly 20 zinc smelting sites dated to the Ming Dynasty (AD 1368-1644) along the Yangtze River in Fengdu, Chongqing, southwest China since 2002 is allowing a detailed technological reconstruction of zinc production. This paper presents the analytical study by OM, SEM-EDS and EPMA-WDS of the production remains from three of these sites, including zinc ore, zinc metal, retorts and slag. The analytical results reveal the use of large-scale installations for zinc distillation with retorts made of pots, condensers, pockets and lids, all well designed to meet specific performance characteristics. The retorts were charged with iron-rich oxidic zinc ores, coal and charcoal; a high temperature of around 1200 °C and highly reducing atmosphere were achieved to reduce the zinc ores; the zinc vapour formed within the pots was cooled and collected in the condensers. The mass production of zinc in Fengdu was probably set up to supply governmental mints.     

Improved methodology for extraction and amplification of DNA from single grains of charred wheat

Comparisons were made between two commonly used methods for the extraction of ancient DNA from charred plant remains. Using artificially charred wheat seeds, we show that silica-binding is the most efficient method for extraction of DNA. We describe a improved silica-binding procedure, including pre-incubation with N-phenacylthiazolium bromide and increased washing of bound DNA, which yields amplifiable DNA from seeds heated at 200 °C for up to 8 h, conditions which promote the formation of Maillard products which often copurify with aDNA and inhibit subsequent PCRs. We believe that this method will be effective in ancient DNA extraction with most types of charred archaeobotanical material. Both cold- and hot-start PCR procedures gave good amplicon yields with extracts prepared in this way, but cold-start PCRs also resulted in synthesis of short artefact products. Addition of bovine serum albumin to PCRs, an inert carrier substance thought to enhance amplification efficiency by binding contaminants, had no advantageous effect and in fact reduced amplicon synthesis.     

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.     

On the provenance and manufacture of red-slipped fine ware from ancient Cassope (NW Greece): evidence by X-ray analytical methods

Energy-dispersive X-ray fluorescence spectroscopy was used to characterize red-slipped pottery (2nd–1st century BC) from ancient Cassope, north-western Greece. The compositional data were statistically treated by principal component analysis and chemical groups were established, representing locally produced and imported items. Mineralogical investigation by X-ray diffraction indicated firing temperatures in the range from 850 to 1000 °C for most of the sherds, while one group consisted of over-fired items, possibly in excess of 1050 °C. The morphology and elemental composition of the ceramic bodies and surface slips were examined through scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy. The analyses revealed that different pottery groups exhibit surface slips of different nature, in terms of thickness, degree of vitrification and elemental composition. Overall, the diversity in technological characteristics of the examined sherds is indicative of the socio-economic conditions prevailing in Cassopaea during the late Hellenistic period.