A microscopic and biomolecular investigation of Middle Palaeolithic combustion features at Abric del Pastor (Alicante, Spain) (original) (raw)

Insights into the timing, intensity and natural setting of Neanderthal occupation from the geoarchaeological study of combustion structures: A micromorphological and biomarker investigation of El Salt, unit Xb, Alcoy, Spain

PLoS ONE, 2019

Middle Paleolithic lithic and faunal assemblages throughout Eurasia reflect short-term Neanderthal occupations, which suggest high group mobility. However, the timing of these short-term occupations, a key factor to assess group mobility and territorial range, remains unresolved. Anthropogenic combustion structures are prominent in the Middle Paleolithic record and conceal information on the timing and intensity and natural setting of their associated human occupations. This paper examines a concentration of eleven combustion structures from unit Xb of El Salt, a Middle Paleolithic site in Spain through a geoarchaeological approach, in search of temporal, human impact and paleoenvironmental indicators to assess the timing, intensity and natural setting of the associated human occupations. The study was conducted using micromorphology, lipid biomarker analysis and compound specific isotope analysis. Results show in situ hearths built on different diachronic topsoils rich in herbivore excrements and angiosperm plant residues with rare anthropogenic remains. These data are suggestive of low impact, short-term human occupations separated by relatively long periods of time, with possible indicators of seasonality. Results also show an absence of conifer biomarkers in the mentioned topsoils and presence of conifer charcoal among the fuel residues (ash), indicating that fire wood was brought to the site from elsewhere. A microscopic and molecular approach in the study of combustion structures allows us to narrow down the timescale of archaeological analysis and contributes valuable information towards an understanding of Neanderthal group mobility and settlement patterns.

Molecular features of organic matter in anthropogenic earthen mounds, canals and lagoons in the Pago Lindo archaeological complex (Tacuarembó, Uruguayan lowlands) are controlled by pedogenetic processes and fire practices

Journal of Archaeological Science: Reports, 2019

The Pago Lindo site in the River Plate basin (Uruguay) is an important pre-hispanic mound settlement (ca. 3000-600 B.P.), of which the technologically and socially advanced nature have only recently been revealed. Different angles of pedogenetic and palaeo-ecological science are rapidly improving our understanding of the history of the site and the relationships between human activity and habitat alteration. Here we add to this progress by molecular characterization of soil organic matter (SOM) in anthropogenic earthen mounds, canals and lagoons from Pago Lindo, by pyrolysis-GC-MS. The results showed that the SOM in the earthen mound and the archaeological lagoon are composed of microbial (partially chitin), aliphatic (partially root-derived) and pyrogenic (from fireplaces or wildfires) materials, whereas the canal and younger lagoon contained SOM with larger proportions of relatively intact plant remains (lignin and polysaccharides from herbaceous species). In most systems, a clear degradation trend can be observed with increasing depth-either from intact plant remains to microbial tissues (canal, young lagoon), or from microbial tissues to recalcitrant aliphatic and pyrogenic sources (earthen mound, ancient lagoon)-which is indicative of a strong control of decay intensity on SOM composition. Multivariate statistics confirmed that most variability in pyrolysis fingerprints can be attributed to degradation/preservation dynamics, which probably erased most of the molecular information on habitat development under the influence of past societies, including nearby maize cultivation.

Marine sedimentary lipidomics of the glacial-interglacial changes during the lower Pleistocene (SW Iberian Margin)

Environmental Science and Pollution Research, 2017

Analyses of trimethylsilyl-derivatized neutral lipids by gas chromatography coupled to mass spectrometry afford a wealth of information contained in the marine sediments. This information is useful for unraveling the processes associated with past climate changes such as those from glacial and interglacial periods. Studies of samples from the Iberian Margin deposited about 1,300,000-1,400,000 years ago afforded the qualitative identification and quantification of n-alkanes, n-alkan-1-ols, isoprenoids, triterpenoids, sterols, hopanols, alkenones, alkenols, and polycyclic aromatic hydrocarbons. Using this information, the lipidomic approach has allowed to identifying differences in sea surface temperatures, marine productivity, microbial degradation processes, and inputs from continental plants between these periods. Differences in predominant higher plant species related to climate changes have also been observed.

A multiproxy record of palaeoenvironmental conditions at the Middle Palaeolithic site of Abric del Pastor (Eastern Iberia)

Quaternary Science Reviews, 2019

This paper presents a multiproxy palaeoenvironmental study from Abric del Pastor (Alcoy, Spain), a rock shelter which has yielded evidence for Middle Palaeolithic human occupation. The sedimentary sequence has been analysed for lipid biomarker n-alkane abundances (ACL, CPI), compound specific leaf wax d 2 H and d 13 C, and bulk organic geochemistry (TOC, %N, %S), providing a record of past climate and local vegetation dynamics. Site formation processes have been reconstructed through the application of soil micromorphology. Analyses of anthracological, microvertebrate and macrofaunal assemblages from selected subunits are also presented here. Our data indicates that a variable climate marked by predominantly cold conditions persisted through most of the sequence and that Neanderthal occupations in stratigraphic unit IVd, assigned to MIS 4 or late MIS 5, occurred in a landscape setting characterised by a mosaic of biotopes. The presence of key resources inside the ravine where the site is located suggests that the occupation of the rock shelter may have been strategically motivated by a subsistence and mobility strategy which focused on zones of localised ecological resilience, such as intra-mountainous valleys or ravines, during periods of global or regional environmental downturn.

n-Alkyl nitriles and compound-specific carbon isotope analysis of lipid combustion residues from Neanderthal and experimental hearths: Identifying sources of organic compounds and combustion temperatures

Quaternary Science Reviews, 2019

Molecular and isotopic approaches offer the chance to identify combustion residues and substrate components of archaeological combustion features to infer past fire-related activities. Analysis of fatty acid methyl esters by gas chromatography-combustion-isotope ratio mass spectrometry have been successfully used to distinguish among different animal fat groups. However, plant oils from different tissues have not been widely investigated even though organic residues from leaf, root, and wood tissues are preserved in sediments from archaeological combustion structures. Our analyses of plant residues from controlled laboratory heating sequences and experimental hearths involving wood and animal residues, provide references to discern anatomical parts of fresh and charred plants and to differentiate contributions of terrestrial plants and animal sources in open air hearths. This information is compared with charred organic residues from combustion structures from three Middle Palaeolithic sites: El Salt (Spain), Abric del Pastor (Spain) and Crvena Stijena (Montenegro). The occurrence of n-alkyl nitriles in our samples corroborates their potential as combustion temperature biomarkers and the d 13 C 16:0 and d 13 C 18:0 values allow us differentiate between charred and fresh plant anatomical parts and between fresh plant oils and animal fats.

A geochemical multi-proxy approach for anthropogenic processes in a Middle–Upper Pleistocene endokarstic deposit

Quaternary International, 2016

Deciphering human activities in archaeological sites is a priority issue in archaeological studies, nevertheless its geochemical fingerprints on sediments are poorly known. In sites belonging to the recent prehistory these geochemical signals have been taken into account, but in oldest sites this subject has not been studied sufficiently. The aim of this paper consists on tracking geochemical proxies that can be attributed to anthropogenic processes in endokarstic Pleistocene deposits. Recognize these elements can be a key factor in order to explore the potential of non-excavated archeological levels and find out activities performed in those sediments more accurately. For that purpose a MiddleeUpper Pleistocene endokarstic deposit (Cueva del Angel) belonging to the Iberian Peninsula has been chosen. This site provides numerous evidences of human activities, as butchering and cooking of predated animals or the habitual use of fire throughout its main stratigraphic sequence. This geochemical/archaeological approach highlights that the upper units consist of anthropogenic influenced sediments, while the lower unit shows a greater percentage of geogenic inputs. Based on P and ZneCueSr, several levels with higher anthropogenic inputs have been identified. These two attributes can be suggested as proxies of human activities for this site. High values of P appear to be linked with "butchering highly occupied" levels, and high levels of ZneCueSr seem to be related with fires. This geochemical information has been compared and tested with previous archeological information.

Investigating Hydrogen Isotope Variation during Heating of n-Alkanes under Limited Oxygen Conditions: Implications for Palaeoclimate Reconstruction in Archaeological Settings

Molecules, 2021

This 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.

Organic geochemical evidence of human-controlled fires at Acheulean site of Valdocarros II (Spain, 245 kya)

Scientific Reports

Among the outstanding questions about the emergence of human-controlled fire is the systematic recurrence between the geochemical remains of fire and its preservation in the archaeological record, as the use of fire is considered a technological landmark, especially for its importance in food cooking, defensive strategies, and heating. Here we report fossil lipid biomarkers associated with incomplete combustion of organic matter at the Valdocarros II site, one of the largest European Acheulean sites in Spain dated to marine isotopic stage (MIS) 8/7 (~ 245 kya) allowing a multiproxy analysis of human-controlled fire use. Our results reveal isolated cases of highly concentrated and diverse polycyclic aromatic hydrocarbons (PAHs) and alkylated PAHs (APAHs), along with diagnostic conifer-derived triterpenoids in two hearth-like archaeological structures. The presence of combustion byproducts suggests the presence of anthropogenic (controlled) fires at Valdocarros—one of the oldest evide...

Pyrogenic organic matter from palaeo-fires during the Holocene: A case study in a sequence of buried soils at the Central Ebro Basin (NE Spain)

Journal of environmental management, 2018

We studied the fire record and its environmental consequences during the Holocene in the Central Ebro Basin. This region is very sensitive to environmental changes due to its semiarid conditions, lithological features and a continuous human presence during the past 6000 years. The study area is a 6 m buried sequence of polycyclic soils developed approximately 9500 years ago that is exceptionally well preserved and encompasses four sedimentary units. The content and size distribution of macroscopic charcoal fragments were determined throughout the soil sequence and the analysis of the composition of charcoal, litter and sediments via analytical pyrolysis (Py-GC/MS). The high amount of charcoal fragments recovered in most horizons highlights the fire frequencies since the beginning of the Neolithic, most of which were probably of anthropogenic origin. In some soil horizons where charcoal was not found, we detected a distribution pattern of lipid compounds that could be related to biom...