Speleothems (stalagmites, stalactites, flowstones, …) are currently one of the best datable terrestrial archives valuably recording past environmental and climatic variability. Their geochemical composition reflects complex interactions between host rock, rainwater infiltration and soil processes dependent on climate (Fairchild & Baker, 2012). In particular, Mg, Sr and Ba are commonly linked to prior calcite precipitation related to water availability and therefore indirectly to rainwater amount (Fairchild et al., 2000), while other elements such as P or S, may reflect organic matter cycling or anthropogenic and marine aerosol inputs (Borsato et al., 2007). Despite their importance, high-resolution spatial profiling of trace elements in speleothems remain analytically demanding, often requiring destructive sample preparation and time-consuming laboratory workflows.Within the framework of the LEAP project (Learning from the Past - https://www.leap-belgium.be/) funded by BELSPO, we developed and implemented a Laser-Induced Breakdown Spectroscopy (LIBS) hyperspectral imaging methodology to obtain rapid, minimally destructive trace-element profiles along speleothem growth axes. The approach combines automated raster scanning with synchronized multi-spectrometer acquisition, producing two-dimensional LIBS spectral images over scan widths of 15–20 mm at 100 µm spatial resolution. Elemental ratio maps (Mg/Ca, Sr/Ca, Ba/Ca) are generated from the hyperspectral data cube and converted into one-dimensional profiles by buffered averaging along growth-parallel transects. A robust filtering and masking strategy based on Ca signal thresholds and calculated plasma parameters allows efficient exclusion of spectra affected by surface defects, detrital inclusions or existing sampling holes.The method was first validated through comparison with LA-ICP-MS elemental mapping on a reference speleothem section, showing consistent relative variations and stratigraphic coherence in Mg/Ca, Sr/Ca and Ba/Ca profiles. Following validation, multiple trace-element profiles were extracted from speleothems from Hotton, Père Noël and Remouchamps caves (Belgium). In the Père Noël cave for example, the approach enabled the extraction of a continuous >1 m long profile at 0.1 mm spatial resolution, demonstrating the capability of LIBS hyperspectral imaging to generate high-resolution geochemical records over large stratigraphic distances.Applied to a flood-impacted speleothem (calcite floor) from the Hotton Cave, the LIBS-derived profiles also revealed distinct elemental profiles associated with thin detrital layers incorporated within the calcite. This allows a more precise and objective assessment of past extreme flooding events at that location that can be compared to population migration information and changes in funerary practices. This contributes to the investigation of the link between climatic and environmental changes and human behaviour in the LEAP project. References:Borsato, A., Frisia, S., Fairchild, I.J.,, Somogyi, A.,, and Susini,J. 2007. Trace Element Distribution in Annual Stalagmite Laminae Mapped by Micrometer-Resolution X-Ray Fluorescence: Implications for Incorporation of Environmentally Significant Species. Geochimica et Cosmochimica Acta 71 (6): 1494–1512.Fairchild, I. J., & Baker, A. (2012). Speleothem science: From process to past environments. Wiley-Blackwell.Fairchild, I. J., Borsato, A., Tooth, A. F., Frisia, S., Hawkesworth, C. J., Huang, Y., McDermott, F., & Spiro, B. (2000). Controls on trace element (Sr–Mg) compositions of carbonate cave waters: Implications for speleothem climatic records. Chemical Geology, 166(3–4), 255–269.
Our study reveals multiple signals of Palaeolithic occupation in the Flemish Valley, a large depression in coastal northwestern Europe with an extremely sparse Pleistocene archaeological record until now. We show that mechanical coring can reveal archaeological evidence of hominin presence from deep palaeolandscapes that are inaccessible for standard survey techniques. At nine out of 41 coring sites, we encountered a total number of 56 lithic artefacts at depths up to 8 m below the surface. We conclude that this unexpected success rate indicates a widespread archaeological record. We believe that this survey method has the potential to increase the number of Palaeolithic sites in northwestern Europe by an order of magnitude, leading to a very different image of Pleistocene hominin settlement in this vast European lowland.
A truncated conical-shaped building constructed using the cyclopean technique, called Talayot 1 or East Talayot, is conserved in the Talayotic settlement of Sant Agust & iacute; Vell. The monument has an internal chamber with two polylithic columns and a pilaster that helps holding up a roof made of large stone slabs, below which three well-conserved wooden beams can be seen, as well as the remains of two other beams, only one end of each is conserved. The study of a sample of each of these beams extracted from the outer rings of the trunks enable us to determine that all the beams come from the Olea europea L. (olive tree) species. The radiocarbon dating of the samples suggest that the trees from which the trunks come were felled between 1259-1123 cal BC. It was the first time that construction elements of a Menorcan talayot could be dated.
Inaccurate lake chronologies are often an outcome of unresolved radiocarbon (14C) reservoir effects. These phenomena may impose considerable challenges to the 14C dating of lacustrine samples, limiting the accuracy of environmental and archaeological research. In South America, the importance of such studies around the Lake Titicaca basin, which presents a vast biodiversity and a rich archaeological heritage, cannot be overstated. However, the lack of preserved terrestrial organic macrofossils in the region hinders the derivation of age offsets for the lake. Despite a previous attempt to quantify the 14C reservoir effect associated with Lake Titicaca, the phenomenon requires further investigation. Here, we used a combination of new and published 14C dates to recalculate the offset using Bayesian approaches, obtaining a value of R = 163 f 83 14C yr for the period between 4000 and 3000 cal BP. Moreover, in the present study we employed a novel approach using mercury peaks as a chrono-tracer across different cores to construct a Bayesian chronological model. This allowed us to derive an R value of 315 f 33 14C yr for the southern basin of the lake at 1590 CE, indicating temporal variation in the radiocarbon reservoir effect. The same approach allowed us to calculate offsets of 166 f 53 14C yr and 335 f 29 14C yr for the shallow and deep parts of the basin, respectively, showing evidence of depth-dependent variation. The methods are thoroughly described and the potential explanations for these values are discussed.
Understanding the spatial distribution of strontium isotopes in plants or other archives within a region is crucial for various fields, including archaeology, environmental studies, food sciences and forensic science. This study aims to create a detailed dynamic strontium isoscape for Belgium through high-density plant sampling, presented in a web application (IsoBel) that serves the mentioned research fields. A total of 540 plant samples (199 locations), representing various species of grass, shrubs, and trees across Belgium were collected and were analysed for their strontium isotope ratios (Sr-87/Sr-86) to create a first biologically available strontium map. Sampling sites were selected to cover diverse lithological formations and soil types, ensuring representative coverage of the region's geological heterogeneity, by using a novel high density grid mapping method. Sixty-four previously published plants from 21 locations are also included in this study, bringing the total amount of plant samples used to 604 from 220 locations. The results reveal significant variations in Sr-87/Sr-86 across Belgium (ranging from 0.7054 to 0.7259), which reflect the underlying lithology and geological processes (tectonics, weathering,& mldr;) which shaped the landscape. Although overlapping Sr-87/Sr-86 is seen across the majority of lithologies, there is a statistically significant difference between the distribution of Sr-87/Sr-86 values across all different lithological units in Belgium (Kruskal-Wallis test; p < 0.0001). Distinct regional patterns were observed, with higher Sr-87/Sr-86 in the older geological south-eastern part of Belgium, compared to the younger north-western parts. The high-density plant sampling approach employed in this study allowed for enhanced spatial resolution and improved accuracy in the predictive surfaces for bioavailable Sr-87/Sr-86 created by Empirical Bayesian Kriging (EBK). These findings provide valuable insights into the geographic distribution of strontium isotopes within Belgium and offer a foundation for future studies in archaeology, ecology, environmental studies, food sciences and forensics. Furthermore, the extensive coverage of various plant species provided a robust representation of the local ecosystems and their strontium sources. Overall, this study contributes to the growing body of knowledge on regional strontium isoscapes, enhancing our understanding of the complex interplay between litho- and biosphere in shaping the strontium isotope compositions of ecosystems.
This study assesses cremation conditions in the Roman period using a multi-proxy analysis (FTIR-ATR and carbon and oxygen isotope analysis) on 332 burned bones from five Belgian Gallo-Roman cemeteries. The results suggest similar pyre structure, size, temperature, and body positioning across Gallo-Roman cremations. However, high variability in delta C-13 and delta O-18 values indicates differences in fuel selection and environmental factors. The wide delta C-13 range likely reflects the use of multiple wood types (e.g., Quercus sp./oak, F. sylvatica/beech) and different tree parts (e.g., trunk, branch, stump) in pyre construction. In contrast, delta O-18 variation may relate to quenching methods and/or seasonal and weather conditions during combustion. Differences were also observed in cremation conditions between the Metal Ages and the Gallo-Roman cremations from Belgium, with Roman cremations presenting better oxygen availability during combustion. Finally, the Gallo-Roman cemetery of Fouches is particularly interesting, as it dates to the Early Roman period and presents similarities in ventilation conditions with the cemeteries from the Metal Ages instead of the other Gallo-Roman cemeteries. The evidence from Fouches suggests a gradual transition from the Metal Ages to Roman cremation practices. The dating of Fouches to the Early Roman period could potentially explain that Roman cremation expertise was not immediately widespread but rather transferred gradually to the edges of the Roman Empire.
Several collagen extraction protocols are described in the literature, but most lack detailed descriptions of the laboratory manipulations and the specific material used. This collagen extraction protocol described here largely follows Longin's (1971) with a few changes. Shortly; The full bone is demineralised using diluted HCl (0.2 to 0.5M). This is followed by removing humic acids using a short NaOH rinse, and by solubilisation and filtration of the collagen. This protocol aims to provide collagen of appropriate quality for both stable isotope analysis and 14C dating, at a low cost and with a decent duration. This protocol was found to also be suitable, with minor adaptations, to badly preserved samples.
Cremation graves appear in different forms and shapes, from urns to simple pits and from single to plural graves. The challenging nature of highly fragmented cremated human remains renders the identification of multiple individuals within the same cremation grave rather complex. Osteological analyses alone are often insufficient to detect the presence of bone fragments from different individuals as they are small and diagnostic elements are often missing, although, detection of nonadult bone fragments within adult bone assemblages (or the other way around) points to the presence of at least two individuals-one adult and one nonadult-within the same grave. The combination of osteological analyses, radiocarbon dating, and strontium isotope ratios has proven to be particularly powerful. At different Belgian Metal Age sites, this novel multi-disciplinary approach enabled to identify the presence of bone fragments belonging to up to three different individuals within the same cremation grave who were cremated up to several centuries apart. Whether the presence of these two or three individuals in the same grave is intentional (e.g. curation) or not requires more in-depth analyses. This study shows the high level of complexity of cremation burial (intentionally or not) and shows the necessity to carry out all analytical measurements (i.e. radiocarbon dating, infrared, elemental and isotope analyses) on the same bone fragment to ensure the results are related to the same individual.
ABSTRACT Since the first developments of anthropogenic lime materials radiocarbon ( 14 C) dating in the 1960s, numerous studies have been undertaken and developed to investigate the topic further. Historic mortars are complex composite and open system materials that can incorporate a large range of components. Due to the complexity of the historic lime mortars composition, they are not part of a routine protocol in most radiocarbon laboratories and reliable dating is not always achieved. A thorough characterization needs to be performed and different preparation methods can be considered as a function of their compositions. A vast range of terms are employed to qualify the lime mortars components and alterations that can possibly have an influence on the dating result. Here, a detailed description of these components and the various terms used is listed. To illustrate this, images obtained by thin-section petrography and cathodoluminescence are presented in addition to radiocarbon results using stepwise acid hydrolysis on Belgian mortars having different provenance, state, age and composition. Depending on the type of aggregate used, the type of binder and its conservation state, the eventual presence of weathering carbonates and the assumed speed of the carbonation process, the reliability of radiocarbon measurements using the stepwise acid hydrolysis technique is discussed and confronted with presumed historical constraints.
The work shows the history (1992–2022) of chronological studies of the key archaeological site of the Lower Amur region - the multi-layer settlement of Khummi. The main attention is paid to dating the lower cultural layer containing materials from the Osipovskaya culture of the initial Neolithic. The work proposes the analysis of the sampling process, their study, obtaining radiocarbon dates; The issues of correlation of the obtained datings with the content of the cultural layer are discussed. A new page in the research of the Hummi settlement was the first four radiocarbon dates of the upper layer containing the remains of the Voznesenovskaya culture of the late Neolithic. Various carbon-containing materials (coal, organics in ceramics and carbon deposits on the surface of ceramics) were used as materials to determine the age of the layers. The results of the thirty years research were the determination of the time of the settlement and habitation of two groups of carriers of the Osipovskaya culture of the initial Neolithic: XIV–XIII thousand years ago (15,900–12,800 calendar years ago or 14,000–10,800 BC) and XI thousand years ago (12,400–12,200 calendar years ago or 10,500–10,200 BC). The appearance of these groups was established with a gap of approximately 1000 years. Dating of the upper cultural layer indicated the time of existence of the Voznesenovsky group of inhabitants: V–IV thousand years ago. (about 4,900–4,100 cal BP or 3,000–2,200 BC). The data obtained made it possible, to a certain extent, to reconstruct the events associated with the settlement of the bank of the channel in the early Holocene; the initial development of the fishing grounds of the Lake Hummi region, which gave rise to a new type of management and culture of sedentary fishermen. Dating of the upper cultural layer made it possible to clarify the time of stay of the Voznesenovtsy group, carriers of an established and developed culture of sedentary fishermen, on the bank of the channel.
Currently in NW Europe little is known about the human response to the extensive cold reversal at the end of the Pleistocene, the Younger Dryas (ca. 12,850 till ca. 11,650 cal BP), mainly due to the poor chronological resolution of the archaeological sites belonging to the Ahrensburgian Culture. Here we present a series of 33 radiocarbon dates performed on the seminal cave site of Remouchamps, situated in the Belgian Meuse basin. Combined with a revision of the available radiocarbon evidence along the southern North Sea basin (Belgium, southern Netherlands, western Germany), it is suggested that the first half of the Younger Dryas, characterized as extremely cold and wet, faced a significant population reduction. Repopulation started around the middle of the Younger Dryas, from ca. 12,200 cal BP onward, probably in response to a slight climatic improvement leading to somewhat warmer summers. This might be considered a prelude to the subsequent population boost of the Early Holocene (Mesolithic).
This study represents the first extensive residue analysis of prehistoric pottery from northern Belgium. It examines pottery use and culinary practices across the Mesolithic-Neolithic transition, from the late 6th to the early 4th millennium cal BC. Residue analyses were performed on more than 200 samples from nine archaeological sites, representing different cultural groups from this transitional phase. This includes the analysis of charred food residues encrusted on the vessel surfaces by elemental analysis-isotope ratio mass spectrometry (EA-IRMS), gas chromatography-mass spectrometry (GC-MS), stereomicroscopic analysis and Scanning Electron Microscopy (SEM), as well as the analysis of absorbed lipids by gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS). This study provides the first evidence of ruminant dairy fats in Early Neolithic Limburg pottery, supporting the hypothesis that this pottery was produced and used by LBK farmers rather than hunter-gatherer populations. The first indigenous pottery of the Swifterbant culture was frequently used to process freshwater fish (often together with plant foods) and ruminant meat, although several of the studied vessels likely contained mixtures of resources which could also include porcine products. Ruminant dairy is nearly absent from this pottery. Similar results were obtained for pottery of the subsequent Michelsberg culture/Group of Spiere of the late 5th and early 4th millennium cal BC. The limited presence of ruminant dairy fats in this pottery contrasts with the findings for Middle Neolithic pottery from neighbouring regions, providing further evidence for the existence of regional variations in pottery use or culinary practices throughout prehistoric NW Europe. However, our current view of pottery use during the Mesolithic-Neolithic transition in northern Belgium might be biased by the difficulties in distinguishing between wild and domesticated ruminant adipose fats as well as in detecting plant foods through lipid residue analysis.
ABSTRACTThe Final Neolithic and the Bronze Age (3000–800 BC) are periods of great transformations in the communities inhabiting the area of modern-day Belgium, as testified by archaeological evidence showing an increasing complexity in social structure, technological transformations, and large-scale contacts. By combining 599 available radiocarbon dates with 88 new 14C dates from 23 from funerary sites, this paper uses kernel density estimates to model the temporality in the use of inhumation vs. cremation burials, cremation deposits in barrows vs. flat graves, and cremation grave types. Additionally, by including 78 dates from settlements, changes in population dynamics were reconstructed. The results suggest a phase of demographic contraction around ca. 2200–1800 BC highlighted by a lack of dates from both settlements and funerary contexts, followed by an increase in the Middle Bronze Age, with the coexistence of cremation deposits in barrows and, in a lower number, in flat graves. At the end of the 14th–13th century BC, an episode of cultural change with the almost generalized use of flat graves over barrows is observed. Regional differentiations in the funerary practices and the simultaneous use of different grave types characterize the Late Bronze Age.
Archaeological textiles are suitable material for radiocarbon dating as they are mainly made of organic matter, such as plant and/or animal fibres. Radiocarbon dating provides objective age estimates of archaeological finds, based on measurements of the carbon-14 isotope present in the organic matter against an internationally used reference standard. However, the quantity and quality of carbon present in the organic matter of archaeological textiles can be affected either by the conditions under which the find was preserved (such as carbonisation, chemical change of organic matter to carbon, and mineralisation, which is the gradual replacement of organic matter by metal degradation products), or by the application of certain interventive methods of conservation (such as, consolidation and the application of organic adhesives that add foreign organic matter/carbon to the textile). Six case studies of archaeological textiles dated using the carbon-14 method are presented here. Two carbonised textile finds, two which were mineralised (one treated with adhesives in the past), and a final two which come from inhumation burials (similar to the textile previously treated with adhesives). This paper includes a discussion and review of the dating method, focusing on sample selection, sample preparation, and by evaluating the efficiency of the technique on textile finds at various states of preservation. This study shows that efficiency of the technique is highly dependable on the amount of carbon present in the finds, which does not seem to be affected by carbonisation, but is greatly affected by mineralisation and the incorporation of foreign organic matter, like synthetic consolidants.
Urnfields were the common type of cemetery in the Late Bronze Age (LBA) and Early Iron Age (EIA) in much of Northwest Europe. Rarely are there clear social or chronological differences between burials apart from changing pottery types. The cemetery of Destelbergen stands out because of the relatively high prevalence of monumental ditches surrounding a selection of graves, indicating a certain status difference between the deceased. Strontium concentrations ([Sr]) combined with radiocarbon (14C) dates and spatial analysis bring to light clear differences between LBA and EIA traditions. The end of the LBA went hand in hand with the abandonment of the oldest part of the cemetery, which new 14C dates demonstrate was strict. Additionally, [Sr] reveal changing diets in individuals buried centrally within monumental ditches. In the EIA these individuals present significantly lower [Sr] than the surrounding burials, potentially the result of a diet richer in animal protein at the expense of plant-based food, a distinction not seen in LBA burials. Even though continuity and equality are reflected in the uniform burial tradition seen within urnfields, this paper’s analyses unlock subtle changes in social attitudes between the LBA and EIA and suggest increasing (dietary) social differentiation in the EIA.
The high temperatures reached during cremation lead to the destruction of organic matter preventing the use of traditional isotopic methods for dietary reconstructions. Still, strontium isotope ( 87 Sr/ 86 Sr) and concentration ([Sr]) analyses of cremated human remains offer a novel way to assess changing consumption patterns in past populations that practiced cremation, as evidenced by a large amount of new data obtained from Metal Ages and Gallo-Roman human remains from Destelbergen, Belgium. The Gallo-Roman results show significantly higher [Sr] and a narrower interquartile range in 87 Sr/ 86 Sr (0.7093–0.7095), close to the value of modern-day seawater (0.7092). This contrasts with the Metal Ages results, which display lower concentrations and a wider range in 87 Sr/ 86 Sr (0.7094–0.7098). This typical Sr signature is also reflected in other sites and is most likely related to an introduction of marine Sr in the form of salt as a food preservative (e.g. salt-rich preserved meat, fish and fish sauce). Paradoxically, this study highlights caution is needed when using 87 Sr/ 86 Sr for palaeomobility studies in populations with high salt consumption.