Combining SR-FTIR, SR-LEXRF and PIXE microscopies for residue analysis on Palaeolithic stone artefacts

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DOMINICI C.,  STANI C.,  BONANNI V.,  ROSSINI M.,  BOŽIČEVIĆ MIHALIĆ I.,  PROVATAS G.,  FAZINIĆ S.,  BOSCHIN F.,  GIANONCELLI A.,  VACCARI L., 2023 – Combining SR-FTIR, SR-LEXRF and PIXE microscopies for residue analysis on Palaeolithic stone artefacts, The European Physical Journal Plus, 138, 742.

https://link.springer.com/article/10.1140/epjp/s13360-023-04320-7

Abstract

Residue analysis in the field of Palaeolithic studies represents a powerful source of information, as well as a challenging operation of deduction, based on the interpretation of what remains of organic and inorganic compounds that testify to the ancient use of lithic artefacts. The disposal of reliable methods for residue characterisation is thus essential in the approach to this discipline, along with the collection of comprehensive, high-quality data. In this paper, the development of a new analytical protocol is presented through the chemical characterisation of red residues coming from three lithic artefacts retrieved from the Upper Palaeolithic stratigraphic sequence of Grotta Paglicci (Apulia, Italy). The morphological description of each residue was followed by the application of an advanced set of complementary techniques (namely Synchrotron Radiation Fourier-Transform InfraRed microscopy, Synchrotron Radiation Low-Energy X-ray Fluorescence and Particle Induced X-ray Emission) to obtain the molecular and elemental composition. The results provided by this pilot study allowed the identification of various organic and inorganic fractions within the samples, proving the reliability and high sensitivity of our newly designed protocol in dealing with ancient residues.

 

Application of 2D shape analysis to study Epigravettian lithic assemblages: assessing its analytical potential

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ROSSINI M., FALCUCCI A., DOMINICI C., RONCHITELLI A., TOMASSO A., BOSCHIN F., 2023 – Application of 2D shape analysis to study Epigravettian lithic assemblages: assessing its analytical potential, Acta IMEKO 12 (4), 1-8.

https://acta.imeko.org/index.php/acta-imeko/article/view/1539

Abstract

In this paper, we apply a two-dimensional (2D) Geometric morphometric analysis to a sample of Epigravettian lithic artefacts with the aim of assessing the potential of such an approach to study Epigravettian lithic assemblages. The lithic sample comes from layer 9c2 (Evolved Epigravettian, Upper Palaeolithic, about 18,000-19,000 years ago) of Grotta Paglicci (Apulia, southern Italy). After extracting the outline coordinates from high-resolution images using the software DiaOutline, we conduct Elliptic Fourier Analysis, Principal Component Analysis, and Linear Discriminant Analysis in  the R package Momocs to investigate the internal variability of the sample. Shape analysis confirms that 1) the production of microbladelets was not linked to a dedicated reduction sequence and 2) the modification of blanks into backed points followed a rather standardised stone tool design. The result opens interesting perspectives for the routine implementation of 2D shape analyses complementary to the classical technological ones.

Palaeogenomics of Upper Palaeolithic to Neolithic European hunter-gatherers

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POSTH C., YU H., GHALICHI A., ROUGIER H., CREVECOEUR I., HUANG Y., RINGBAUER H., ROHRLACH A.B., NÄGELE K., VILLALBA-MOUCO V., RADZEVICIUTE R., FERRAZ T., STOESSEL A., TUKHBATOVA R., DRUCKER D.G., LARI M., MODI A., VAI S., SAUPE T., L. SCHEIB C., CATALANO G., PAGANI L., TALAMO S., FEWLASS H., KLARIC L., MORALA A., RUÉ M., MADELAINE S., CRÉPIN L., CAVERNE J-B., BOCAEGE E., RICCI S., BOSCHIN F., BAYLE P., MAUREILLE B., FONI LE BRUN-RICALENS F., BORDES J-G., OXILIA G, BORTOLINI E., BIGNON-LAU O., DEBOUT G., ORLIAC M., ZAZZO A., SPARACELLO V., STARNINI E., LUCA SINEO L., VAN DER PLICHT J., PECQUEUR L., MERCERON G., GARCIA G., LEUVREY J-M., BAY GARCIA C., GÓMEZ-OLIVENCIA A., POŁTOWICZ-BOBAK M., BOBAK D., LE LUYER M., STORM P., HOFFMANN C., KABACIŃSKI J., FILIMONOVA T., SHNAIDER S., BEREZINA N., GONZÁLEZ-RABANAL B., GONZÁLEZ MORALES M.R., MARÍN-ARROYO A.B., LÓPEZ B., ALONSO-LLAMAZARES C., RONCHITELLI A., POLET C., JADIN I., CAUWE N., SOLER J., COROMINA N., RUFÍ I., COTTIAUX R., CLARK G., STRAUS L.G., JULIEN M-A., RENHART S., TALAA D., BENAZZI S., ROMANDINI M., AMKREUTZ L., HERVÉ BOCHERENS H., WIßING C., VILLOTTE S., FERNÁNDEZ-LÓPEZ DE PABLO J., GÓMEZ-PUCHE M., ESQUEMBRE-BEBIA M.A., BODU P., SMITS L., SOUFFI B., JANKAUSKAS R., KOZAKAITĖ J., CUPILLARD C., BENTHIEN H., WEHRBERGER K., SCHMITZ R.W., FEINE S.C., SCHÜLER T., THEVENET C., GRIGORESCU D., LÜTH F., KOTULA A., PIEZONKA H., SCHOPPER F., SVOBODA J., SÁZELOVÁ S., CHIZHEVSKY A., KHOKHLOV A., CONARD N.J., VALENTIN F., HARVATI K., SEMAL P., JUNGKLAUS B., SUVOROV A., SCHULTING R., MOISEYEV V., MANNERMAA K., BUZHILOVA A., TERBERGER T., CARAMELLI D., ALTENA E., WOLFGANG HAAK W. & KRAUSE J., 2023 – Palaeogenomics of Upper Palaeolithic to Neolithic European hunter-gatherers, Nature, 615, 117-126.

https://www.nature.com/articles/s41586-023-05726-0

Abstract

Modern humans have populated Europe for more than 45,000 years. Our knowledge of the genetic relatedness and structure of ancient hunter-gatherers is however limited, owing to the scarceness and poor molecular preservation of human remains from that period. Here we analyse 356 ancient hunter-gatherer genomes, including new genomic data for 116 individuals from 14 countries in western and central Eurasia, spanning between 35,000 and 5,000 years ago. We identify a genetic ancestry profile in individuals associated with Upper Palaeolithic Gravettian assemblages from western Europe that is distinct from contemporaneous groups related to thisarchaeological culture in central and southern Europe, but resembles that of preceding individuals associated with the Aurignacian culture. This ancestry profile survived during the Last Glacial Maximum (25,000 to 19,000 years ago) in human populations from southwestern Europe associated with the Solutrean culture, and with the following Magdalenian culture that re-expanded northeastward after the Last Glacial Maximum. Conversely, we reveal a genetic turnover in southern Europe suggesting a local replacement of human groups around the time of the Last Glacial Maximum, accompanied by a north-to-south dispersal of populations associated with the Epigravettian culture. From at least 14,000 years ago, an ancestry related to this culture spread from the south across the rest of Europe, largely replacing the Magdalenian-associated gene pool. After a period of limited admixture that spanned the beginning of the Mesolithic, we find genetic interactions between western and eastern European hunter-gatherers, who were also characterized by marked differences in phenotypically relevant variants.

A 23,000-year-old southern Iberian individual links human groups that lived in Western Europe before and after the Last Glacial Maximum

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VILLALBA-MOUCO V., VAN DE LOOSDRECHT M.S., ROHRLACH A.B., FEWLASS H., TALAMO S., YU H., ARON F., LALUEZA-FOX C., CABELLO L., CANTALEJO DUARTE P., RAMOS-MUÑOZ J., POSTH C., KRAUSE J., WENIGER G-C. & HAAK W., 2023 – A 23,000-year-old southern Iberian individual links human groups that lived in Western Europe before and after the Last Glacial Maximum, Nature Ecology & Evolution, 7 (4), 597-609.

https://www.nature.com/articles/s41559-023-01987-0.pdf

Abstract

Human populations underwent range contractions during the Last Glacial Maximum (LGM) which had lasting and dramatic effects on their genetic variation. The genetic ancestry of individuals associated with the post-LGM Magdalenian technocomplex has been interpreted as being derived from groups associated with the pre-LGM Aurignacian. However, both these ancestries differ from that of central European individuals associated with the chronologically intermediate Gravettian. Thus, the genomic transition from pre- to post-LGM remains unclear also in western Europe, where we lack genomic data associated with the intermediate Solutrean, which spans the height of the LGM. Here we present genome-wide data from sites in Andalusia in southern Spain, including from a Solutrean-associated individual from Cueva del Malalmuerzo, directly dated to ~23,000 cal yr bp. The Malalmuerzo individual carried genetic ancestry that directly connects earlier Aurignacian-associated individuals with post-LGM Magdalenian-associated ancestry in western Europe. This scenario differs from Italy, where individuals associated with the transition from preand post-LGM carry different genetic ancestries. This suggests different dynamics in the proposed southern refugia of Ice Age Europe and posits Iberia as a potential refugium for western European pre-LGM ancestry. More, individuals from Cueva Ardales, which were thought to be of Palaeolithic origin, date younger than expected and, together with individuals from the Andalusian sites Caserones and Aguilillas, fall within the genetic variation of the Neolithic, Chalcolithic and Bronze Age individuals from southern Iberia.

A 23,000-year-old southern Iberian individual links human

Ancient oral microbiomes support gradual Neolithic dietary shifts towards agriculture

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QUAGLIARIELLO A., MODI A., INNOCENTI G., ZARO V., CONATI BARBARO C., RONCHITELLI A., BOSCHIN F., CAVAZZUTI C., DELLÙ E., RADINA F., SPERDUTI A., BONDIOLI L., RICCI S., LOGNOLI M., BELCASTRO M.G., MARIOTTI V., CARAMELLI D., MARIOTTI LIPPI M., CRISTIANI E., MARTINO M. E., MUNTONI I. M. & LARI M.(2022) – Ancient oral microbiomes support gradual Neolithic dietary shifts towards agriculture, Nature Communications, 13, 1-14.

https://www.nature.com/articles/s41467-022-34416-0

Abstract

The human microbiome has recently become a valuable source of information about host life and health. To date little is known about how it may have evolved during key phases along our history, such as the Neolithic transition towards agriculture. Here, we shed light on the evolution experienced by the oral microbiome during this transition, comparing Palaeolithic hunter-gatherers with Neolithic and Copper Age farmers that populated a same restricted area in Italy. We integrate the analysis of 76 dental calculus oral microbiomes with the dietary information derived from the identification of embedded plant remains. We detect a stronger deviation from the hunter-gatherer microbiome composition in the last part of the Neolithic, while to a lesser extent in the early phases of the transition. Our findings demonstrate that the introduction of agriculture affected host microbiome, supporting the hypothesis of a gradual transition within the investigated populations.

Analytical potential of 2D shape analysis to study Epigravettian lithic assemblages

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ROSSINI M., FALCUCCI A., DOMINICI C., RONCHITELLI A., TOMASSO A., BOSCHIN F., 2022 – Analytical potential of 2D shape analysis to study Epigravettian lithic assemblages, IMEKO TC-4 International Conference on Metrology for Archaeology and Cultural Heritage, MetroArchaeo 2022, 52-56.

https://www.imeko.org/publications/tc4-Archaeo-2022/IMEKO-TC4-MetroArchaeo2022-011.pdf

Abstract

In this paper we apply for the first time a 2D shape analysis to a sample of Epigravettian lithic artefacts with the aim of evaluating the potential of such approach. The lithic sample comes from layer 9c2 (Evolved Epigravettian, Upper Palaeolithic) of Grotta Paglicci (Apulia, southern Italy).

After extracting the outline coordinates from high-resolution images using the software DiaOutline, we conduct Elliptic Fourier Analysis, Principal Component Analysis, and Linear Discriminant Analysis in the R package Momocs to investigate the internal variability of the sample. The results of the analysis are extremely promising and highlight significant separation between common tools, laminar blanks, and backed tools. Furthermore, this analysis can be useful to evaluate the technical investment in the retouching of the blanks to manufacture backed points.

Analytical potential of 2D

 

SR-FTIR microscopy for the study of residues on Palaeolithicstone tools: looking for a methodological protocol

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DOMINICI C.,  STANI C.,  ROSSINI M.,  VACCARI L., 2022 – SR-FTIR microscopy for the study of residues on Palaeolithicstone tools: looking for a methodological protocol, Journal of Physics: Conference Series, 2204(1) IOP Publishing, 012050.

https://iopscience.iop.org/article/10.1088/1742-6596/2204/1/012050

https://iopscience.iop.org/article/10.1088/1742-6596/2204/1/012050/pdf

Abstract

In this paper, we use SR-FTIR microscopy to analyse residues identified on seven lithic artefacts from the Evolved Epigravettian layer 9c2 of the cave site of Grotta Paglicci (Apulia, southern Italy). Synchrotron radiation, thanks to its properties that particularly increase the sensitivity of FTIR microscopy, allows the analysis of samples of microscopic size and the characterisation of even highly degraded compounds, such as the residues of materials worked by Palaeolithic stone tools or complex compounds used for hafting. This pilot study has been carried out in the framework of a project concerning the reconstruction of hunting technologies between the Middle and Upper Palaeolithic. The preliminary results allowed us to focus on the issues of our methodological approach and to show the potential of the SR-FTIR microscopy for the analysis of residues on lithic implements.

SR-FTIR microscopy for the study of residues on Palaeolithicstone tools

Le più antiche evidenze di elaborazione di alimenti vegetali nel Paleolitico, in “Preistoria del cibo. L’alimentazione nella preistoria e nella protostoria”

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REVEDIN A., ARANGUREN B., MARCONI E., MARIOTTI LIPPI M., RONCHITELLI A., 2021 – Le più antiche evidenze di elaborazione di alimenti vegetali nel Paleolitico, in “Preistoria del cibo. L’alimentazione nella preistoria e nella protostoria” (a cura di I. Damiani, A. Cazzella, V. Copat), Studi di Preistoria e Protostoria – 6, Firenze, 353-364.

https://www.researchgate.net/publication/355700489

Riassunto

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Gli studi recenti mettono in evidenza l’importanza della componente vegetale nella dieta umana del Paleolitico, grazie soprattutto alle evidenze costituite dalle analisi isotopiche, dai residui vegetali rinvenuti nei siti, dai granuli di amido nel tartaro dei denti e sugli strumenti per la macinazione, i quali costituiscono il principale oggetto di ricerca del progetto IPP sulle “Risorse vegetali nel Paleolitico”.

Il progetto IIPP ha come obiettivo sia ottenere informazioni sulla dieta, sia ricostruire le complesse tecniche per la preparazione di cibi di origine vegetale e quindi le strategie di sussistenza che costituivano una parte importante del bagaglio culturale delle popolazioni paleolitiche. I ritrovamenti dimostrano che questa tecnologia era sviluppata fin dagli inizi del Gravettiano ed estesa su una vasta area dell’Europa, dall’Italia meridionale alla pianura del Don in Russia, in tipi di insediamenti molto diversi fra loro.

Lo studio si è rivolto: 1 – all’individuazione dei manufatti attraverso l’analisi degli elementi morfotecnici ricorrenti e le tracce d’uso; 2 – all’individuazione dei vegetali utilizzati, attraverso il campionamento dei residui sulle macine, l’analisi dei granuli di amido, l’individuazione delle specie di provenienza; 3 – alla comprensione dei procedimenti tecnici impiegati per la produzione di farine, tramite la sperimentazione; 4 – alla caratterizzazione chimico-nutrizionale delle porzioni vegetali macinate, per valutare l’apporto quantitativo-qualitativo di proteine, carboidrati complessi e acidi grassi.

Tutti i manufatti sono stati usati per trattare differenti specie vegetali che chiaramente variavano a seconda di quello che offriva l’ambiente circostante. La varietà dei manufatti e delle tecniche utilizzate appare come il risultato dell’adattamento a contesti economici e ambientali diversi di conoscenze che dovevano essere comuni e diffuse. Si tratta di un’attività economica complessa che necessita di un notevole investimento di risorse da parte della comunità: questo dimostra che l’introduzione delle farine nelle strategie di sussistenza dei gruppi umani del Paleolitico superiore doveva rivestire un ruolo non secondario. L’importanza della farina consiste infatti nell’alto contenuto energetico concentrato in un prodotto poco voluminoso e poco pesante, facilmente trasportabile e conservabile.

Abstract

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Recent studies have cast light on the importance of the vegetal component in the Palaeolithic. This finding is based largely on the evidence of isotopic analyses, on the vegetal residue found in the sites and the starch grains found in tooth tartar and on tools used for grinding. These tools are the main subjects of research in the IIPP project Vegetal Resources in the Palaeolithic.

The aim of the IIPP project is both to obtain information about the diet and to reconstruct the complex techniques used in the preparation of foods of vegetal origin and, consequently, the subsistence strategies that were a significant component of the cultural baggage of the Palaeolithic populations. Discoveries demonstrate that this technology was developed starting in the early Gravettian in extremely varied types of settlement ranging over a vast area of Europe, from southern Italy to the plain of the river Don in Russia.

The aims of the study are: 1- to identify the artefacts by analysing the recurrent morphotechnical elements and the use-wear traces; 2 – to identify the plants used by sampling the residue on the grindstones and analysing the starch grains to identify the species of origin; 3 – to perform experiments to understand the technical procedures used in the production of flour; 4 – to perform chemical and nutritional characterisation of the vegetal portions that were ground in order to assess the quantitative and qualitative content of proteins, complex carbohydrates and fatty acids.

The artefacts were used to process different vegetal species, which naturally varied depending on the resources offered by the local environment. The variety of the artefacts and of the techniques used appears to be the result of adaptation of widespread and common knowledge to different economic and environmental contexts. This was a complex economic activity that required a significant investment of resources on the part of the community, demonstrating that the introduction of flour must have played a major role in the subsistence strategies of the human groups of the Upper Palaeolithic. The importance of flour is in fact related to the high energy content concentrated in a product of reduced bulk and weight that could be stored and transported.

More data on ancient human mitogenome variability in Italy: new mitochondrial genome sequences from three Upper Palaeolithic burials

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MODI A., VAI S., POSTH C., VERGATA C., ZARO V., DIROMA M.A., BOSCHIN F., CAPECCHI G., RICCI S., RONCHITELLI A., CATALANO G., LAURIA G., D’AMORE G., SINEO L., CARAMELLI D. & LARI M., 2021 – More data on ancient human mitogenome variability in Italy: new mitochondrial genome sequences from three Upper Palaeolithic burials, Annals of Human Biology, 48 (3), 213-222.

https://doi.org/10.1080/03014460.2021.1942549

https://www.tandfonline.com/doi/full/10.1080/03014460.2021.1942549

Abstract

Background: Recently, the study of mitochondrial variability in ancient humans has allowed the definition of population dynamics that characterised Europe in the Late Pleistocene and Early Holocene. Despite the abundance of sites and skeletal remains few data are available for Italy.

Aim: We reconstructed the mitochondrial genomes of three Upper Palaeolithic individuals for some of the most important Italian archaeological contexts: Paglicci (South-Eastern Italy), San Teodoro (South-Western Italy) and Arene Candide (North-Western Italy) caves.

Subjects and methods: We explored the phylogenetic relationships of the three mitogenomes in the context of Western Eurasian ancient and modern variability.

Results: Paglicci 12 belongs to sub-haplogroup U8c, described in only two other Gravettian individuals; San Teodoro 2 harbours a U2’3’4’7’8’9 sequence, the only lineage found in Sicily during the Late Pleistocene and Early Holocene; Arene Candide 16 displays an ancestral U5b1 haplotype already detected in other Late Pleistocene hunter-gatherers from Central Europe.

Conclusion: Regional genetic continuity is highlighted in the Gravettian groups that succeeded in Paglicci. Data from one of the oldest human remains from Sicily reinforce the hypothesis that Epigravettian groups carrying U2’3’4’7’8’9 could be the first inhabitants of the island. The first pre- Neolithic mitogenome from North-Western Italy, sequenced here, shows more affinity with continentalEurope than with the Italian peninsula.

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