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- 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.
- Fire use and waste management in an Iberian iron age village: geoarchaeological insights into midden formation processesPublication . Tomé, Laura; Iriarte, Eneko; Blanco-González, Antonio; Fernández-Palacios, Enrique; Martín-Seijo, María; Carrancho, Ángel; Herrera-Herrera, Antonio V.; Mallol, CarolinaMiddens, commonly found in archaeological sites across different chronologies, serve as rich sedimentary archives of daily life by capturing the refuse and discarded artifacts of past human groups. This study focuses on the midden deposits of the Early Iron Age settlement site of Cerro de San Vicente (Central Iberia). We applied a high- resolution, microcontextual geoarchaeological approach, integrating soil micromorphology -including phytolith and charcoal analyses on thin sections-, sedimentary lipid biomarker analysis, X-Ray fluorescence (XRF), XRay diffraction (XRD) and magnetic properties analysis to investigate the formation processes and past functionality of the site's midden deposits. Our findings reveal that the targeted sequences are primarily composed of wood ash and charred plant refuse, as well as trampled and disintegrated earth-based construction materials. These deposits are interpreted as the result of multiple hearth rake-out events, maintenance and construction activities, and possible spatially-related communal storage practices within the village. Stratigraphic connections between deposits from inside and outside the dwellings are proposed, linking the middens to an intermediate phase (ca. 600 BCE) of the village's history. These results offer relevant insights into the spatial and temporal dynamics of refuse disposal, maintenance practices and space use at Cerro de San Vicente, highlighting the value of microcontextual geoarchaeological methods in unveiling domestic practices. This study contributes to enhancing our understanding of Early Iron Age socio-cultural and daily life practices in Central Iberia.