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- 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.
- 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.
- 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.