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- Hydroclimate reconstruction through MIS 3 in the Middle Paleolithic site of Crvena Stijena (Montenegro) based on hydrogen-isotopic composition of sedimentary n-alkanesPublication . Jambrina-Enríquez, Margarita; Mallol, Carolina; Tostevin, Gilbert; Monnier, Gilliane; Pajović, Goran; Borovinić, Nikola; Baković, MileThis study presents a hydroclimatic reconstruction from Crvena Stijena (Montenegro, Balkan Peninsula), a rock shelter that has yielded evidence for Middle Paleolithic human occupation. The integration of lipid biomarkers, hydrogen (dD) isotopic compositions of n-alkanes, and organic elemental geochemistry in the 7-m deep vertical sedimentary sequence enables reconstruction of the main hydrological and environmental changes during the MIS 3 and their correlation with the presence at the site. We apply agglomerative hierarchical clustering and principal component analysis to the geochemical, molecular, and stable isotopic data to obtain a robust hydrological record. We find evidence of three aridity trends from the studied period, one of them correlated with the Heinrich Event 5, and humid and cold -temperate conditions in archaeology-rich layers. Our dataset also contributes to the knowledge of past hydrological variability in the Balkan Peninsula, a sensitive area to short-lived climatic shifts, and overall, in the Mediterranean region during the last glacial/interglacial cycle.(c) 2022 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
- Reconstructing formation processes at the Canary Islands indigenous site of Belmaco Cave (La Palma, Spain) through a multiproxy geoarchaeological approachPublication . Fernández‐Palacios, Enrique; Jambrina‐Enríquez, Margarita; Mentzer, Susan M.; Rodríguez de Vera, Caterina; Dinckal, Ada; Égüez, Natalia; Herrera‐Herrera, Antonio V.; Navarro Mederos, Juan Francisco; Marrero Salas, Efraín; Miller, Christopher E.; Mallol, CarolinaThe indigenous populations of La Palma (Canary Islands), who arrived on the island from Northwest Africa ca. 2000 years B.P., were predominantly pastoralists. Yet, many aspects of their subsistence economy such as the procurement, management, and use of wild plant resources remain largely unknown. To explore this, we studied the 600-1100-year-old archaeological site of Belmaco Cave, which comprises a stratified sedimentary deposit representative of a fumier. Here, we present a highresolution, multiproxy geoarchaeological study combining soil micromorphology, lipid biomarker analysis, X-ray diffraction, mu-X-ray diffraction, mu-X-ray fluorescence, Fourier transform infrared spectroscopy, and mu-Fourier transform infrared spectroscopy, to characterize formation processes and explore plant sources. Recurrent goat/sheep habitation and maintenance activities are represented by interstratified layers of unburned dung, charcoal-rich sediment, and dung ash. Lipid biomarker data show a herd diet mainly composed of herbaceous plants, which is key to understanding the mobility of indigenous shepherds. Our results also revealed an unusual suite of authigenic minerals including hazenite, aragonite, and sylvite, possibly formed through diagenetic processes involving interaction between ash, dung, urine, volcanogenic components, and bacterial activity, coupled with arid and alkaline conditions. Our study shows the potential of a multiproxy approach to a fumier deposit in a volcanogenic sedimentary context.
- Investigating hydrogen isotope variation during heating of n-Alkanes under limited oxygen conditions: implications for palaeoclimate reconstruction in archaeological settingsPublication . Connolly, Rory; Jambrina-Enríquez, Margarita; Herrera-Herrera, Antonio V.; Mallol, CarolinaThis paper reports on a series of heating experiments that focus on n-alkanes extracted from leaf, bark, and xylem tissues of the Celtis australis plant. These lipid biomarkers were analysed for their compound-specific hydrogen isotopic composition (δ2Hwax) under limited oxygen conditions at 150, 250, 350, and 450 °C. Our results reveal isotopic variations in wax lipids of different plant organs during short-term low-temperature combustion. We conclude that, in the absence of a detailed characterisation of the depositional environment in advance of sampling, δ2Hwax values in archaeological or otherwise highly anthropogenic environments should be interpreted cautiously. In addition, we observed that variation in δ2Hwax of leaves is minimal at temperatures ≤ 350 °C, highlighting the potential for δ2Hwax in thermally altered combustion substrates to yield palaeoclimate information, which could allow researchers to investigate links between archaeological and climatic records at a high spatial and temporal resolution.
- Searching for traces of human activity in earthen floor sequences: high-resolution geoarchaeological analyses at an Early Iron Age village in Central IberiaPublication . Tomé, Laura; Iriarte, Eneko; Blanco-González, Antonio; Jambrina-Enríquez, Margarita; Égüez, Natalia; Herrera-Herrera, Antonio V.; Mallol, CarolinaThe Northern Iberian Plateau during the Early Iron Age witnessed the proliferation of villages, showcasing wellpreserved earthen architectural remains that offer valuable insights into past daily life practices. However, the application of high-resolution geoarchaeological approaches to these contexts has been largely overlooked, despite their significance in assessing complex sedimentary sequences predominantly composed of earth-based construction materials. This paper presents the outcomes of a microcontextual geoarchaeological study conducted on earthen dwellings from the Early Iron Age village of Cerro de San Vicente (Salamanca, Northern Iberia). Our study employed soil micromorphology, lipid biomarker analysis, XRD, and XRF analyses to investigate site formation processes, characterize construction materials and techniques, and explore aspects of daily life practices, functionality, and dwelling life histories. Our results have enabled the identification of three distinct construction layers within the dwellings, shedding light on recurrent events of floor use, maintenance, and repaving. Additionally, we have detected periods of abandonment and decay of the earth-based construction material that inform on the dynamics of abandonment and reuse within the village. Furthermore, our analysis has revealed the presence of well-preserved lipid biomarkers throughout the sequences, possibly associated with the past functionality of the dwellings. Ongoing and future analyses will further contribute to our understanding of ancient construction practices and the utilization of domestic spaces at Cerro de San Vicente. This study significantly enhances the limited availability of high-resolution, microcontextual data sets concerning Iron Age contexts in Iberia, underscoring the potential of our approach for future consolidation and advancement. By combining different geoarchaeological methodologies, we demonstrate the importance of integrating diverse analytical techniques to gain comprehensive insights into the socio-cultural dynamics of the Early Iron Age settlements.
- Compound-specific carbon isotope analysis of short-chain fatty acids from pine tissues: characterizing paleo-fire residues and plant exudatesPublication . Jambrina-Enríquez, Margarita; de Vera, Caterina Rodríguez; Davara, Javier; Herrera-Herrera, Antonio V.; Mallol, CarolinaDifferent types of plant tissues and resin can account for the wax lipids found in sedimentary contexts and archaeological samples. Consequently, there is increasing research to characterize the fatty acid carbon isotope ratios of different plant anatomical parts and their plant exudates (resin). With the aim to explore isotopic differences between plant tissues, state of the fine organic matter, effect of thermal degradation, and to identify plant residues we measured the δ13C values of short-chain fatty acids (δ13C16:0 and δ13C18:0) in: i) dead and fresh (collected and immediately dried) pine needles and branches (Pinus canariensis) and pine resin from laboratory-controlled heating experiments and ii) sediment and charred pine tissue samples from a wild pine forest fire. Our results are compared to previously published experimental open-air fire experiments and pine-fuelled archaeological combustion features. We found that for both fatty acid types, there are differences in δ13C signatures among anatomical parts and initial moisture content. These data allow us to characterize the isotopic signature of pine tissue and the effect of degradation on isotopic biomarkers, as well as to estimate combustion temperatures in pine-fuelled anthropogenic fires.
- Fuel sources, natural vegetation and subsistence at a high-altitude aboriginal settlement in Tenerife, Canary Islands: Microcontextual geoarchaeological data from Roques de García RockshelterPublication . Tomé, Laura; Jambrina-Enríquez, Margarita; Égüez, Natalia; Herrera-Herrera, Antonio V.; Davara, Javier; Marrero Salas, Efraín; Arnay de la Rosa, Matilde; Mallol, CarolinaHigh-altitude island environments, with their characteristic strong seasonal contrast and limited resources, are challenging contexts for human subsistence. However, although archaeological contexts in this kind of setting hold great potential to explore the diversity of human biological and cultural adaptations, such sites are rare. In this paper, we present the results of a microcontextual geoarchaeological study carried out at Rogues de Garcia Rockshelter, the highest altitude cave archaeological site in the Canary Islands (Spain). The site was inhabited by the aboriginal population of the island and has yielded a rich archaeological context derived from combustion activity. We carried out soil micromorphology to characterize site function and lipid biomarker analysis to investigate the natural and anthropogenic organic record. Our data indicate that the aboriginal groups that occupied the site kept goats with them (in the rockshelter) and probably used Juniperus turbinata (sabina) wood, a current distant fuel source. These results suggest that the aboriginal societies of Tenerife occupied the highlands regularly, taking their herds and firewood with them. Further research is necessary to explore the use and exploitation of fuel sources, the seasonality of these occupations and their differences with lowland sites.
- Pyrotechnology and lipid biomarker variability in pine tar productionPublication . Davara, Javier; Jambrina-Enríquez, Margarita; Rodríguez de Vera, Caterina; Herrera-Herrera, Antonio V.; Mallol, CarolinaTar or pitch produced from pine resin and wood played an important role in the past as an adhesive, waterproofing and medicinal product. However, the formation and biomolecular composition of pine tar produced only from resin under different combustion conditions (i.e., temperature and oxygen availability during heating) has not been as widely investigated as pine tar produced by dry distillation of wood or birch bark tar, for which an extensive literature is available. This lack of information hampers technological interpretations of biomolecular data obtained from organic residue analyses of archaeological pine tar products. In this study, we performed controlled laboratory heating sequences with pine resin (Pinus canariensis) at 150, 250, 350 and 450 oC under both oxygenated and oxygen-limited conditions, and analyzed the products using gas chromatography-mass spectrometry (GC-MS). A control unheated resin sample was also analysed. We found that the formation of pine tar from resin occurs around 250-350 oC under both oxygenated and oxygen-limited atmospheres. We also present and discuss the lipid biomarkers of pine resin and its combustion products according to changes in temperature and oxygen availability. Our reference data provide new information for the biomolecular identification of archaeological pine tar products and show potential for shedding light on the conditions in which tar was manufactured by ancient populations in different contexts.
- Soil micromorphological image classification using deep learning: the porosity parameterPublication . Arnay, Rafael; Hernandez-Aceituno, Javier; Mallol, CarolinaIdentifying components and microstructures in soil and sediment thin sections is one of the many subjects of analysis in archeological research, as these features can provide information regarding the deposit from which they were extracted, such as its origin and nature, clues about their associated human contexts or alteration processes they might have undergone over time. This article presents a Deep Learning system based on Convolutional Neural Networks (CNN) to classify different porosity types of structures in photomicrographs from archeological soils and sediment thin sections, as a first step to build and expand a database that will boost research in this field of archeological research. The results obtained are encouraging and show that the presented models can be successfully applied to this classification task. The trained models have been used to estimate the quantity of the different microstructures in test images, obtaining a median error of around 2%. (C) 2021 Elsevier B.V. All rights reserved.
- Modern human incursion into Neanderthal territories 54,000 years ago at Mandrin, FrancePublication . Slimak, Ludovic; Zanolli, Clément; Higham, Tom; Frouin, Marine; Schwenninger, Jean-Luc; Arnold, Lee J.; Demuro, Martina; Douka, Katerina; Mercier, Norbert; Guérin, Gilles; Valladas, Hélène; Yvorra, Pascale; Giraud, Yves; Seguin-Orlando, Andaine; Orlando, Ludovic; Lewis, Jason E.; Muth, Xavier; Camus, Hubert; Vandevelde, Ségolène; Buckley, Mike; Mallol, Carolina; Stringer, Chris; Metz, LaureDetermining the extent of overlap between modern humans and other hominins in Eurasia, such as Neanderthals and Denisovans, is fundamental to understanding the nature of their interactions and what led to the disappearance of archaic hominins. Apart from a possible sporadic pulse recorded in Greece during the Middle Pleistocene, the first settlements of modern humans in Europe have been constrained to similar to 45,000 to 43,000 years ago. Here, we report hominin fossils from Grotte Mandrin in France that reveal the earliest known presence of modern humans in Europe between 56,800 and 51,700 years ago. This early modern human incursion in the Rhone Valley is associated with technologies unknown in any industry of that age outside Africa or the Levant. Mandrin documents the first alternating occupation of Neanderthals and modern humans, with a modern human fossil and associated Neronian lithic industry found stratigraphically between layers containing Neanderthal remains associated with Mousterian industries.