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Over 120 prehistoric pottery sherds from mainland Finland and the Åland Islands in the north Baltic region were studied for their organic residue content. Preserved fat residues found in these vessels indicated that the food procurement pattern was broad during the Neolithic and Early Metal periods. Based on previous research and these results, it appears that animal husbandry came to Finland with the Corded Ware culture. Groups using the succeeding Late Neolithic Kiukainen Ware did not, however, practice animal husbandry to any great extent, as there is an indication of dairy fats in only a single sherd. In general, even after dairy farming arrived in the area, prehistoric groups in southern and south-western Finland continued or returned to a hunter-gatherer lifestyle. During the Early Metal period, animal husbandry increased in importance among the groups living in the area, and the level of dairying then intensified.
The Bristol Radiocarbon Accelerator Mass Spectrometry (BRAMS) Facility was established at the University of Bristol after the commissioning of our dedicated sample preparation laboratories and the installation and acceptance of the BrisMICADAS AMS in 2016. Routine measurements commenced in mid-2016, once validation was completed for each sample type. Herein, we give an overview of the standard pretreatment methods currently employed in the Facility and the results of radiocarbon (14C) determinations on a wide range of standards, blank materials, and intercomparison samples which have been measured during our extensive pretreatment method validation program and during our routine 14C analyses.
The preservation of compounds of biological origin (nucleic acids, proteins, carbohydrates, lipids, and resistant biopolymers) in terrigenous fossils and the chemical and structural changes that they undergo during fossilization are discussed over three critical stratigraphic levels or “time slices.” The youngest of these is the archeological record (e.g., <10 k.y. B.P.), when organic matter from living organisms undergoes the preliminary stages of fossilization (certain classes of biomolecule are selectively preserved while others undergo rapid degradation). The second time slice is the Tertiary. Well-preserved fossils of this age retain diagenetically modified biomarkers and biopolymers for which a product-precursor relationship with the original biological materials can still be identified. The final time slice is the Carboniferous. Organic material of this age has generally undergone such extensive diagenetic degradation that only the most resistant biopolymers remain and these have undergone substantial modification. Trends through time in the taphonomy and utility of ancient biomolecules in terrigenous fossils affect their potential for studies that involve chemosystematic and environmental data.
We have developed and demonstrated a practical methodology for dating specific compounds (and octade-canoic or stearic acid—C18:0—in particular) from the lipid material surviving in archaeological cooking pots. Such compounds may be extracted from about 10 g of cooking potsherd, and, after derivatization, can be purified by gas chromatography. To obtain sufficient material for precise dating repetitive, accumulating, GC separation is necessary. Throughout the 6000-year period studied, and over a variety of site environments within England, dates on C18:0 show no apparent systematic error, but do have a greater variability than can be explained by the errors due to the separation chemistry and measurement process alone. This variability is as yet unexplained. Dates on C16:0 show greater variability and a systematic error of approximately 100-150 years too young, and it is possible that this is due to contamination from the burial environment. Further work should clarify this.
Cutan, a resistant non-hydrolyzable aliphatic biopolymer, was first reported in the cuticle of Agave americana and has generally been considered ubiquitous in leaf cuticles along with the structural biopolyester cutin. Because leaves and cuticles in the fossil record almost always have an aliphatic composition, it was argued that selective preservation of cutan played an important role in leaf preservation. However, the analysis of leaves using chemical degradation techniques involving hydrolysis to test for the presence of cutan reveals that it is absent in 16 of 19 taxa (angiosperm and gymnosperm), including many previously reported to contain cutan on the basis of pyrolysis data. Cutan is clearly much less widespread in leaves than previously thought, and its presence or absence does not exert any major bias on the preservation of leaves in the fossil record. In the absence of cutan, other constituents—cutin, plant waxes, and internal plant lipids—are incorporated into the geomacromolecule and contribute to the formation of a resistant aliphatic polymer by in situ polymerization during diagenesis.
The Jomon culture is an ancient Japanese society that existed during approximately 14,000 to 400 BC and which is characterized by Jomon (cord pattern) pottery. To investigate the paleodiet of the people of northeastern Tohoku in Japan during the Final Jomon period (about 1000–400 BC), we studied three sites in Aomori Prefecture, the center of the Kamegaoka culture. The Fubinashi site is on the coast and was supported by a rich fishing culture. Imazu was a coastal salt-making site. Sugisawa is a mountainous inland site on the banks of a river. We determined the 14C ages of the interior and exterior surfaces of carbonized material on potsherds and compared the data with pottery typology and age to study the marine reservoir effect. We also analyzed the bulk carbon and nitrogen stable isotopes and C:N ratios to determine the presence of aquatic foodstuffs. The organic residues from pottery typology corresponding to the described analyses provided a general perspective of differences in the ancient diets at each site. When we recovered sufficient lipids, we analyzed compound-specific stable isotopes of fatty acids to obtain a multilateral view of those diets. Our findings indicate that the diets of inhabitants of both Fubinashi and Imazu consisted primarily of marine products and some terrestrial foodstuffs, whereas people from Sugisawa processed mainly C3 plants and some terrestrial animals and aquatic commodities.
In 1990 a stone covered pit containing a Trevisker Ware vessel was found eroding from the cliffs at Harlyn Bay and excavated. The vessel contained cremated bone from several individuals with some animal bone, quartz pebbles, and a small bronze pendant. A radiocarbon date on the cremated bone fell in the range 2120–1880 cal bc and is a valuable addition to the small number of securely-dated Early Bronze Age burials in Cornwall with metalwork associations. This early date also makes a major contribution to the debate on the sequence of Trevisker Ware as the vessel, of gabbroic clay, has a band of incised chevron decoration. Lipid residue analysis showed traces of ruminant dairy fat. This paper examines the significance of unmounded burial sites in Cornwall and also assesses the importance of Early Bronze Age burials around Harlyn Bay which have produced an unusually wide range of artefacts.
The Romans brought the mortarium to Britain in the first century AD, and there has long been speculation on its actual purpose. Using analysis of the residues trapped in the walls of these ‘kitchen blenders’ and comparing them with Iron Age and Roman cooking pots, the authors show that it wasn't the diet that changed — just the method of preparing certain products: plants were being ground in the mortarium as well as cooked in the pot. As well as plants, the mortars contained animal fats, including dairy products. The question that remains, however, is why these natural products were being mixed together in mortaria. Were they for food, pharmaceuticals or face creams?
During the past four and a half years this group has been involved in a programme of development and testing of methods for the study of organic residues in archaeological ceramics. The analytical approach used is based on solvent extraction of powdered potsherds to release lipids absorbed in the ceramic fabric, with gas chromatography (GC) and combined gas chromatography/mass spectrometry (GC/MS) being used to characterise andquantify the individual components of the residues. Our most recent work has focused on an assemblage of more than sixty reconstructed vessels of Late Saxon/early medievaldate for which full or partial profiles were available. Analysis of potsherds sampled from different parts of these vessels, e.g. rim, body and base, have shown that different concentrations of lipid can exist in different parts of a vessel. This observation has important consequences for the sampling of potsherds for organic residue analysis. More significantly, these results indicate that the variation in the concentration of lipid in different parts of a vessel may reflect the way in which the vessel was used in antiquity. This paper discusses the results obtained from preliminary laboratory simulation experiments which have been carried out using replica vessels to provide supporting evidence for this potentially new approach to interpreting vessel use. Consideration will also be given to the possibility of using potsherds from these replica vessels in laboratory experiments aimed at simulating the decay of absorbed lipids during burial.
The authors examine the role of horses as expressed in assemblages from settlement sites and cemeteries between the Eneolithic and the Bronze Age in Kazakhstan. In this land, known for its rich association with horses, the skeletal evidence appears to indicate a fading of ritual interest. But that's not the whole story, and once again micro-archaeology reveals the true balance. The horses are present at the funeral, but now as meat for the pot, detected in bone fragments and lipids in the pot walls.
During the ongoing excavations in the palace of the famous Qatna complex, the excavators noted patches of brown staining on the floor of a high status tomb. Chemical extraction revealed the presence of brominated derivatives of indigo and indirubin, and more detailed characterisation showed that it likely came from Hexaplex trunculus. In short, this was none other than the renowned Tyrian or Royal Purple mentioned by Pliny, which was to have such an influential career colouring the clothing of the powerful. Furthermore, it was associated in the tomb with ghosts of high quality textiles preserved in gypsum.
Part of a large male woolly mammoth (Mammuthus primigenius) was preserved in permafrost in northern Yakutia. It was radiocarbon dated to ca. 18,50014C yr BP (ca. 22,500 cal yr BP). Dung from the lower intestine was subjected to a multiproxy array of microscopic, chemical, and molecular techniques to reconstruct the diet, the season of death, and the paleoenvironment. Pollen and plant macro-remains showed that grasses and sedges were the main food, with considerable amounts of dwarf willow twigs and a variety of herbs and mosses. Analyses of 110-bp fragments of the plastid rbcL gene amplified from DNA and of organic compounds supplemented the microscopic identifications. Fruit-bodies of dung-inhabiting Ascomycete fungi which develop after at least one week of exposure to air were found inside the intestine. Therefore the mammoth had eaten dung. It was probably mammoth dung as no bile acids were detected among the fecal biomarkers analysed. The plant assemblage and the presence of the first spring vessels of terminal tree-rings of dwarf willows indicated that the animal died in early spring. The mammoth lived in extensive cold treeless grassland vegetation interspersed with wetter, more productive meadows. The study demonstrated the paleoecological potential of several biochemical analytical techniques.
Using pyrolysis-gas chromatography/mass spectrometry and Fourier transform infrared spectroscopy, the authors show that amber was imported into Late Bronze Age Syria and used for making the prestige artefacts found in a Royal tomb of c. 1340 BC. The objects included beads and a unique vessel in the form of a lion, likely fashioned in Syria from raw amber imported from the Baltic via the Aegean.
We report here on the results of AMS dating and isotopic analysis of the frozen human remains named Kwaday Dän Ts'inchí and associated materials recovered from a glacier located in Northwest British Columbia, Canada in 1999. The isotopic analysis of bone collagen (bulk and single amino acids) from the individual indicates a strongly marine diet, which was unexpected given the location of this find, more than 100 km inland eroding out of a high elevation glacier; however, bulk hair and bone cholesterol isotopic values indicate a shift in diet to include more terrestrial foods in the year before death. The radiocarbon dating is not straightforward, as there are difficulties in determining the appropriate marine correction for the human remains, and the spread of dates on the associated artifacts clearly indicates that this was not a single use site. By combining the most recent date on a robe worn by Kwaday Dän Ts'inchi with direct bone collagen dates we conclude that the individual likely dates to between cal A.D. 1670 to 1850, which is in the pre-(or early) European contact period for this region.
By extracting lipids from potsherds and determining the δ13C of the most abundant fatty acids, degraded fats from ruminant animals, such as cattle, and non-ruminant animals, such as pigs, can be distinguished. The authors use this phenomenon to investigate Late Neolithic pig exploitation and find that the pig ‘signature’ was more frequently found among residues from Grooved Ware than other prehistoric pottery types.
The diets of laboratory rats were isotopically and nutritionally manipulated using purifiedC3 and/or C4 macronutrients to investigate the routing of dietary carbonto bone collagen biosynthesis. Diets were formulated with purified proteins, carbohydrates andlipids of defined composition and natural abundance stable isotope ratios. Bulk protein and constituent amino acid δ13C values determined for whole diet and bone collagen provided the basis for assessing isotopic fractionation and estimating the degree of routing versus synthesis de novo of essential, non-essential and conditionally indispensable amino acids. Essential and conditionally indispensable amino acids were shown to be routed from diet to collagen with little isotopic fractionation whereas non-essential amino acids differed by up to 20‰. Mathematical modelling of the relationships between macronutrient and tissue δ13C values provided qualitative and quantitative insights into the metabolic and energetic controls on bone collagen biosynthesis. Essential amino acids comprise 21·7% of the carbon in collagen, defining the minimum amount of dietary carbon routing. Estimates of 42 and 28% routing were shown for the non-essential amino acids, glycine and aspartate, respectively. In total, the routing of non-essential and conditionally indispensable amino acids was estimated to equal 29·6% of the carbon in collagen. When the contribution of carbon from the essential amino acids is also considered, we arrive at an overall minimum estimate of 51·3% routing of dietary amino acid carbon into bone collagen.
Discovering what was cooked in a pot by identifying lipids trapped in the potsherds has been a highly successful method developed in recent years. Here the authors identify a compound which shows the pots had been used to process maize – probably the most important foodstuff in later prehistoric North America. The uptake of maize is confirmed as coincident with the Mississippian fluorescence.
While palaeobotanical remains provide clear evidence for the exploitation of the date at various locations in Egypt and Nubia, it is the detection amongst lipid residues in closed form vessels of fatty acid distributions dominated by diagnostic short-chain fatty acids, i.e. C12:0 and C14:0′ that provides the first direct evidence for the processing of palm fruit in pottery vessels.