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Characterizing organic matter preserved in archaeological sediment is crucial to behavioral and paleoenvironmental investigations. This task becomes particularly challenging when considering microstratigraphic complexity. Most of the current analytical methods rely on loose sediment samples lacking spatial and temporal resolution at a microstratigraphic scale, adding uncertainty to the results. Here, we explore the potential of targeted molecular and isotopic biomarker analysis on polyester resin-impregnated sediment slabs from archaeological micromorphology, a technique that provides microstratigraphic control. We performed gas chromatography–mass spectrometry (GC–MS) and gas chromatography–isotope ratio mass spectromety (GC–IRMS) analyses on a set of samples including drill dust from resin-impregnated experimental and archaeological samples, loose samples from the same locations and resin control samples to assess the degree of interference of polyester resin in the GC–MS and Carbon-IRMS signals of different lipid fractions (n-alkanes, aromatics, n-ketones, alcohols, fatty acids and other high polarity lipids). The results show that biomarkers within the n-alkane, aromatic, n-ketone, and alcohol fractions can be identified. Further work is needed to expand the range of identifiable lipid biomarkers. This study represents the first micro-contextual approach to archaeological lipid biomarkers and contributes to the advance of archaeological science by adding a new method to obtain behavioral or paleoenvironmental proxies.

 

Abstract Burned or charred organic matter in anthropogenic combustion features may provide important clues about past human activities related to fire. To interpret archaeological hearths, a correct identification of the organic source material is key. In the present work, Raman spectroscopy is applied to characterise the structural properties of char produced in laboratory heating- and open-fire experiments. This reference data set is compared to analyses of three different archaeological sites with Middle Palaeolithic combustion contexts. The results show that it is possible to determine whether a charred fragment is the product of burning animal-derived matter (e.g. meat) or plant-derived matter (e.g. wood) by plotting a few Raman spectral parameters (i.e. position of G and D bands, and intensity ratios H D / H G and H V / H G ) against one another. The most effective parameters for discriminating animal- from plant-derived matter are the position of the G band and the H V / H G intensity ratio. This method can be applied on raw sample material and on uncovered micromorphological thin sections. The latter greatly compliments micromorphology by providing information about char fragments without any clear morphological characteristics. This study is the first of its kind and may provide archaeologists with a robust new method to distinguish animal- from plant-derived char in thin sections. 

SUMMARY An archaeomagnetic, rock magnetic and magnetic fabric study has been carried out on seven anthropogenic ash horizons in the Middle Palaeolithic sedimentary level XXIV at the rock shelter of Crvena Stijena (‘Red Rock’), Montenegro. The study has multiple goals, including the identification of iron bearing minerals formed during combustion, assessment of the suitability of these combustion features for recording the Earth´s magnetic field direction, revelation of the magnetic fabric and its significance in the characterization of cave (rock shelter) burnt facies, and identification of post-burning alteration processes. Magnetite has been identified as the main ferromagnetic component of the ash. The ash layers exhibit a high thermomagnetic reversibility in contrast to the irreversible behaviour of their subjacent burnt black layers which is related to the different temperatures attained. Seven mean archaeomagnetic directions were obtained with acceptable statistical values indicating that these features recorded the field direction at the time of burning. However, some of them are out of the expected range of secular variation for mid-latitude regions suggesting post-burning alterations. The magnetic fabric of the ash was characterized by anisotropy of low field magnetic susceptibility measurements. Statistical analysis (box and whisker plot) of the basic anisotropy parameters, such as foliation, lineation, degree of anisotropy and the shape parameter, along with the alignment of the principal susceptibilities on stereoplots, revealed variation among the ash units. The diverse, oblate to prolate, lineated or strongly foliated, quasi-horizontally and vertically oriented fabrics of the units may indicate different slope processes, such as orientation by gravity, solifluction, run-off water, quasi-vertical migration of groundwater and post-burning/post-depositional alteration of the fabric by rockfall impact. In sum, the magnetic characterization of the ash layers has shown the occurrence of different post-burning alteration processes previously not identified at the site. Alteration processes in prehistoric combustion features are often identified from macroscopic observations but our study demonstrates that multiple processes can affect them and are usually unnoted because they take place on a microscopic scale. Their identification is critical for a correct chronological and cultural interpretation of a site (e.g. collection of samples for dating, stratigraphic displacement of remains), especially if significant alterations are involved. Magnetic methods are therefore a powerful but underutilized tool in palaeolithic research for the identification and evaluation of taphonomic processes affecting prehistoric fires. 

The rockshelter of Crvena Stijena (Nikšić municipality, Montenegro) is one of the most important Paleolithic sites in southeastern Europe. Its 20-meter deep sequence of archaeological deposits spans the Middle Paleolithic through the Bronze Age. The Middle Paleolithic deposits themselves, which cover an astonishing 12 meters in depth, contain one of the longest records of Neanderthal occupation in the region. Since its discovery in 1954, the site has been the subject of two major research projects; the data they have produced have helped make it a critical type-site for the Paleolithic in the Balkans. In this paper, our goal is to introduce the aims and methodologies of the new research collaboration at Crvena Stijena that we established in 2016. We first present the site within the context of the Middle Paleolithic of the western Balkans. We then describe the history of research at Crvena Stijena, and summarize the results of the last project, which were recently published. Finally, we describe the research questions that are guiding our new investigations, and the methods we are applying in order to answer these questions while preserving as much of the site as possible for future generations of archaeologists.