The distinction between freshwater- and terrestrial-based diets: methodological concerns and archaeological applications of sulphur stable isotope analysis

Sulphur isotopes in archaeological bone collagen are not routinely analysed in palaeodietary studies. Here we investigate the potential contribution that sulphur isotope analysis can provide toward the study of ancient human diet and economy, with particular emphasis on the distinction between freshwater and terrestrial consumers. For material from the Late Bronze Age site of Chicha in the south-western Eurasian forest-steppe, sulphur isotopes effectively separate freshwater and terrestrial animal food resources. The sulphur isotope data coupled with nitrogen isotope values from Chicha reflect a dietary reliance upon freshwater animal protein (fish) for the Late Bronze Age inhabitants. In contrast, sulphur isotope values for freshwater and terrestrial potential food species from the Eneolithic site of Bil'shivtsi in western Ukraine were indistinguishable, demonstrating that δ³⁴S values cannot always be relied upon to identify freshwater and terrestrial consumers. The data from this study support the adoption of δ³⁴S analysis as a standard component of palaeodietary studies; apart from its potential to distinguish freshwater from terrestrial consumers, it can provide supplementary dietary information not evident from the carbon and nitrogen isotope data. In addition, certain indices are considered that may be used to assess the validity of sulphur isotope data, as currently exist for carbon and nitrogen. According to the analysis of modern collagen samples, N:S appears to be a broad indicator of collagen sulphur isotope quality. However, more work needs to be done to establish an effective means by which highly-altered sulphur isotope values can be identified and thereby removed from consideration.     

Stable carbon and nitrogen isotope analysis on human remains from the Early Mesolithic site of La Vergne (Charente-Maritime,France)

We report here the results of stable carbon and nitrogen isotope analysis of human and faunal remains from La Vergne (Charente-Maritime, western France), a rare Early Mesolithic burial site (ca. 8500–8000 cal BC). The results for nine humans (average δ¹³C = −19.3‰; δ¹⁵N = 9.4‰) indicate a strongly terrestrial diet, dominated by animal protein, with the possibility of, at best, a slight contribution of marine-derived protein. Given lower sea-levels in the early Holocene, the site would have been some 60–80 km from the sea at the time of its use; nevertheless, contacts with the coast are shown by the presence of numerous marine shell beads in the graves. In the light of the stable isotope results, it is suggested here that such contacts most likely took the form of exchange with coastal communities whose remains now lie underwater.     

Contrasting paleofluid systems in the continental basement: a fluid inclusion and stable isotope study of hydrothermal vein mineralization,Schwarzwald district,Germany

An integrated fluid inclusion and stable isotope study was carried out on hydrothermal veins (Sb‐bearing quartz veins, metal‐bearing fluorite–barite–quartz veins) from the Schwarzwald district, Germany. A total number of 106 Variscan (quartz veins related to Variscan orogenic processes) and post‐Variscan deposits were studied by microthermometry, Raman spectroscopy, and stable isotope analysis. The fluid inclusions in Variscan quartz veins are of the H₂O–NaCl–(KCl) type, have low salinities (0–10 wt.% eqv. NaCl) and high T_h values (150–350°C). Oxygen isotope data for quartz range from +2.8‰ to +12.2‰ and calculated δ¹⁸O_H2O values of the fluid are between ?12.5‰ and +4.4‰. The δD values of water extracted from fluid inclusions vary between ?49‰ and +4‰. The geological framework, fluid inclusion and stable isotope characteristics of the Variscan veins suggest an origin from regional metamorphic devolatilization processes. By contrast, the fluid inclusions in post‐Variscan fluorite, calcite, barite, quartz, and sphalerite belong to the H₂O–NaCl–CaCl₂ type, have high salinities (22–25 wt.% eqv. NaCl) and lower T_h values of 90–200°C. A low‐salinity fluid (0–15 wt.% eqv. NaCl) was observed in late‐stage fluorite, calcite, and quartz, which was trapped at similar temperatures. The δ¹⁸O values of quartz range between +11.1‰ and +20.9‰, which translates into calculated δ¹⁸O_H2O values between ?11.0‰ and +4.4‰. This range is consistent with δ¹⁸O_H2O values of fluid inclusion water extracted from fluorite (?11.6‰ to +1.1‰). The δD values of directly measured fluid inclusion water range between ?29‰ and ?1‰, ?26‰ and ?15‰, and ?63‰ and +9‰ for fluorite, quartz, and calcite, respectively. Calculations using the fluid inclusion and isotope data point to formation of the fluorite–barite–quartz veins under near‐hydrostatic conditions. The δ¹⁸O_H2O and δD data, particularly the observed wide range in δD, indicate that the mineralization formed through large‐scale mixing of a basement‐derived saline NaCl–CaCl₂ brine with meteoric water. Our comprehensive study provides evidence for two fundamentally different fluid systems in the crystalline basement. The Variscan fluid regime is dominated by fluids generated through metamorphic devolatilization and fluid expulsion driven by compressional nappe tectonics. The onset of post‐Variscan extensional tectonics resulted in replacement of the orogenic fluid regime by fluids which have distinct compositional characteristics and are related to a change in the principal fluid sources and the general fluid flow patterns. This younger system shows remarkably persistent geochemical and isotopic features over a prolonged period of more than 100 Ma.     

Nitrogen isotopes and the trophic level of humans in archaeology

Human and domesticate animal bone collagen δ¹⁵N values in prehistory differ generally by 3‰ or more from Neolithic to post- Roman times in Northwest Europe, leading to an assumed dietary animal protein fraction of 60–80% using a standard interpretation of δ¹⁵N values. We examine the assumptions on which this model rests and the limitations of our knowledge in the analysis of δ¹⁵N values in archaeology. We have developed a set of models which, with small changes made in assumptions (on the order of 1‰), can produce substantially lower estimates of the dietary animal protein fraction for given δ¹⁵N values. We consider the implications of various dietary animal protein fractions on agricultural carrying capacities and human population densities in prehistory.     

Stable isotopic analysis of human and faunal remains from the Incipient Chulmun (Neolithic) shell midden site of Ando Island,Korea

We analyzed stable carbon and nitrogen isotope ratios of human and animal remains from the Ando shell midden, South Korea. The Ando site is a rare Incipient Chulmun (Neolithic) site (ca. 6000–5000 BC), which contains well-preserved human and animal bones in shell mounds. The stable isotope results for humans (average δ¹³C = −13.5 ± 0.5‰ and δ¹⁵N = 15.2 ± 0.5‰) indicate that Ando people in the Incipient Chulmun period strongly depended on marine resources. There were no isotopic differences between humans of different sex and age at this site. We compared our data with other previous published isotopic data from the Chulmun sites and found that the Ando people had similar isotope values to the southern Chulmun people (Tongsamdong and Daepo), but different isotopic ratios than the western Chulmun people (Daejukri and Konamri). These results indicate that marine foods were the main food resources in the southern coastal regions, but not in the western coastal regions in Chulmun Korea.     

Seasonality and season of birth in early Eneolithic sheep from Cheia (Romania): methodological advances and implications for animal economy

Cheia (early 5th millennium cal BC) is a prehistoric village in the Dobrodgea province in Romania. Its occupation is attributed to the Early Eneolithic period or Hamangia III phase. The exploitation of animal resources is heavily dominated by husbandry. Although cattle are dominant, they were complemented by caprines, mainly sheep, exploited for tender meat (as highlighted by a 6–12 months age class peak in the mortality profile). Sheep reproduction patterns were investigated through stable isotope analyses in order to characterize the annual rhythms of slaughtering for tender meat acquisition while informing a more general picture on sheep demographical management and animal husbandry at the settlement. Results from δ¹⁸O analysis on second and third molar enamel were modeled and compared with modern reference populations. Sheep births took place over less than four months, from late winter to early summer. From this it could be concluded that tender meat could be provided most of the year, excepted over short period in early summer. Finally, comparison of datasets obtained on the M2 and M3 suggests that the M2 presents a more accurate representation of birth seasonality due to lower inter-individual variability in the chronology of tooth growth.     

Beyond the grave: variability in Neolithic diets in Southern Germany?

Carbon and nitrogen stable isotope analyses were undertaken on human and faunal remains from two Neolithic sites in Southern Germany; the LBK settlement at Herxheim and the middle Neolithic cemetery at Trebur. Stable isotope data were used to reconstruct the diets of individuals buried at these sites and to look at dietary variation between groups classified by their sex, age, grave goods and cultural affiliation. Overall there was surprisingly little variation in the diet between the groups, as described by the stable isotope analysis, despite significant differences in the composition of grave goods. Also surprising, considering the archaeological evidence for extensive grain cultivation in this region during the Neolithic, was that the majority of individuals had δ¹⁵N values consistent with the consumption of significant amounts of animal protein.     

Manuring and stable nitrogen isotope ratios in cereals and pulses: towards a new archaeobotanical approach to the inference of land use and dietary practices

This paper explores the impact of animal manure application on the δ¹⁵N values of a broad range of crops (cereals and pulses), under a range of manuring levels/regimes and at a series of locations extending from northwest Europe to the eastern Mediterranean. We included both agricultural field experiments and areas where ‘traditional’ farming is practised. Our aim is to ground-truth interpretation of δ¹⁵N values in archaeobotanical crop remains as evidence of past growing conditions and husbandry practices. The results confirm the potentially radical impact of manuring on δ¹⁵N values in cereals, depending on manuring level, but indicate only a slight effect on pulses, which can fix atmospheric nitrogen. The expected geographical trend towards greater δ¹⁵N with increasing climatic aridity is not apparent, probably because the growing conditions for crops are ‘buffered’ through crop management. Each of these observations has fundamental implications for archaeobotanical interpretation of δ¹⁵N values as evidence of land use practices and (together with analysis of bone collagen/tooth enamel in potential consumers) palaeodiet.     

Anthropogenic saltpetre: dual (oxygen and nitrogen) isotopic constraints to the biogeochemical processes

Saltpetre constitutes one of the major ingredients of gunpowder, which was a driving force during the political changes in late medieval to early modern times in Japan. Two types of model saltpetre mineralization are studied. One represents efflorescent saltpetre formed as the byproduct of indigo dye manufacture, whereas the second is anthropogenic, derived from relict nitre‐beds. Here, oxygen and nitrogen isotopic analysis, as expressed by δ¹⁸O and δ¹⁵N notations, is applied. The calculated δ¹⁸O values for ambient water, responsible for the microbial‐mediated oxidation of ammonium into oxygen in nitrates, tended to have higher ranges than average local meteoric waters of the relevant regions. An overall trend could be seen, showing the apparent positive nitrogen isotopic fractionation during the microbial transformation from initial organic nitrogen into nitrate product. Dual isotopic analysis for industrial nitrates provides a useful tool for investigation of the provenance of historic gunpowder. Present anthropogenic saltpetre involves positive control over temperature–moisture regimes and oxygen fugacity during formation, the process being distinctive from those prevailed in British India and other European countries.     

Stable isotopic evidence for diet in a Roman and Late Roman population from Leptiminus,Tunisia

This study investigates the diet of the Roman and Late Roman population of Leptiminus on the Mediterranean coast of Tunisia. Stable carbon and nitrogen isotope analysis of human bone collagen and carbonate samples obtained from individuals buried in four cemeteries at Leptiminus was conducted in order to reconstruct the diet of the population, investigate the relative importance of marine vs. terrestrial resources, explore sex-, age-, and status-based variations in diet, examine temporal changes in the types of foods consumed, and compare the diet at Leptiminus with that of other Roman populations. The results of this study indicate that the residents of Leptiminus consumed a diet that was heavily reliant on terrestrial plant resources with the addition of a significant amount of marine resources. There were no significant sex differences in isotope values. In contrast, distinct dietary differences were seen between the adults and children. Nitrogen isotope values suggest that weaning began before the age of two and was completed by about 3 years of age, a finding consistent with previous isotopic studies of Roman samples. A temporal shift in diet is suggested by the nitrogen isotope values measured in samples from the most recent cemetery. A comparison of the data from Leptiminus with that derived from other Roman sites indicates that regional variability in diet existed within the Empire.     

Stable Isotope Analysis Reveals Variations in Human Diet at the Poundbury Camp Cemetery Site

Stable isotope analysis was undertaken on 48 individuals from Iron Age, Roman and Post-Roman periods of the Poundbury Camp Cemetery, Dorchester, England. Variations in diet, reflected by the stable isotope values, were observed between individuals from the different time periods. Differences in diet within the Late Roman period were particularly interesting, as we found that the isotope values could be related to burial type. We also found evidence of possible immigrants at Poundbury; individuals that may have come to the site from a warmer climate.     

Bone stable isotope studies in archaeology

Stable isotope ratios of carbon and nitrogen in bone have become increasingly frequent inclusions in archaeological reports over the past few decades. The majority of such studies has been done in North America, where the use of marine foods and the introduction of maize have been monitored. Similar questions have been addressed in Mesoamerica and South America. In Europe, stable isotope ratios have documented the shift from marine fishing and gathering to agriculture in coastal areas and the introduction of millet in parts of eastern and southern Europe. Much work remains to be done in Asia, where millet replaced early C3 plant foods and, in turn, was replaced by rice. In Africa marine adaptations, freshwater fishing, agriculture, and pastoralism all yield diagnostic isotopic signatures. We review these studies, discuss areas requiring further study, and close with discussions of areas promising interesting future developments.     

Stable carbon and nitrogen isotope variations in tooth dentine serial sections from Wharram Percy

Here we report δ¹³C and δ¹⁵N measurements of serial sections of human deciduous and permanent tooth dentine from archaeological samples taken from the medieval village site of Wharram Percy, Yorkshire, UK. We found a pattern of enrichment, for both δ¹³C and δ¹⁵N, where the tooth crown was greater than the cervical part of the root, which in turn was greater than the apical portion of the root and the associated rib collagen values. This pattern reflects a decrease in the consumption of isotopically enriched breast milk and the introduction of less enriched weaning foods in the diet. The (mean±SD) difference between the deciduous second molar crowns and corresponding rib samples from the same individuals after 2 years of age was 1.2±0.4‰ for δ¹³C and 3.2±0.8‰ for δ¹⁵N. The δ¹⁵N values are as predicted, but as there were no C₄plants at Wharram Percy, this 1.2‰ enrichment in δ¹³C represents clear evidence of a carbon trophic level effect in collagen from breastfeeding infants. Carbon and nitrogen results also show that the infant diet among those who died in infancy did not differ from those who survived into childhood. This study demonstrates the promise of using dentine serial sections to study the temporal relationships of breastfeeding, weaning, and dietary patterns of single individuals.     

Discovery of colon contents in a skeletonized burial: Soil sampling for dietary remains

Recovering dietary and parasitological data from skeletonized burials is often overlooked or attempted without sufficient consideration of preservation possibilities, quality sampling areas or the confounding influences of post-interment processes. A case study of a skeletonized Anasazi burial is presented to demonstrate three important points. First, that macrobotanical remains can be preserved in addition to the more durable pollen and parasite eggs. Second, that the sacrum can act as a structural container for the contents of the lower digestive tract upon decomposition of the body, thereby providing a productive sampling area. Finally, that reliable interpretation of any biological remains from skeletonized burials depends upon the analysis of several control samples. Since awareness of probable data sources plays a central role in what is actually collected and analysed, it is important to alert archaeologists to the possibilities of colon content analysis from skeletonized burials.     

The effect of parity status on δN: looking for the “pregnancy effect” in 18th and 19th century London

This study examined the effect of parity status on δ¹⁵N using the well-characterised 18th and 19th century skeletal collection from the crypt of Christ Church, Spitalfields, London. We tested whether the cumulative effect of multiple pregnancies and breastfeeding could significantly reduce female δ¹⁵N values compared to males. The results from stable isotope analysis of 92 adult ribs show that the population of Spitalfields had relatively little variation in diet, compared to contemporary urban populations, and had abundant animal and marine protein. We were able to rule out any effect attributable to socio-economic status, date or age at death on the stable isotope ratios. There were no significant differences in δ¹⁵N due to parity status, nor were there any differences between males and females. Models of collagen turnover rates in ribs suggest that the effect of δ¹⁵N depletion due to pregnancy would be undetectable except in ideal circumstances, where bone of the optimal turnover period was sampled, and in cases where multi-parous individuals died shortly after parturition.     

Stable hydrogen isotopes of bone collagen in palaeodietary and palaeoenvironmental reconstruction

The stable hydrogen isotope ratios (δD) of bone collagen in archaeological human and animal samples demonstrate a trophic level effect, with increasing δD from herbivores to omnivores to humans, in steps of 10–30‰. In addition the archaeological sites studied (Yarnton, Eton Rowing Lake, Danebury Environs–Suddern Farm, and Windmill Hill in the UK, Balatonszárszó in Hungary, and Huari in Peru) demonstrate geographical variation in δD. The detection of manuring in prehistory by comparison of δ¹⁵N to δD values in humans and a local herbivore (cattle) is also considered. This work is the first to measure δD in a large number and range of archaeological samples, with several animal species and humans. It demonstrates unequivocally that δD is different between species in ancient material, increasing from herbivores to omnivores to carnivores.