Institut de Recherche sur les ArchéoMATériaux

In the field of luminescence and electron spin resonance dating, dose rate conversion factors are widely used to convert concentrations of radioactive isotopes to dose rate values. These factors are derived from data provided by the National Nuclear Data Center of the Brookhaven National Laboratory, which are compiled in Evaluated Nuclear Structure Data Files (ENSDF) and Nuclear Wallet Cards. The recalculated dose rate conversion factors are a few percent higher than those previously published, except for beta and gamma emissions of the isotopes of the U-series decay chains.

Two sites of the Neandertal-associated Middle Paleolithic of Iberia, dated to as early as approximately 50,000 years ago, yielded perforated and pigment-stained marine shells. At Cueva de los Aviones, three umbo-perforated valves of Acanthocardia and Glycymeris were found alongside lumps of yellow and red colorants, and residues preserved inside a Spondylus shell consist of a red lepidocrocite base mixed with ground, dark red-to-black fragments of hematite and pyrite. A perforated Pecten shell, painted on its external, white side with an orange mix of goethite and hematite, was abandoned after breakage at Cueva Antón, 60 km inland. Comparable early modern human-associated material from Africa and the Near East is widely accepted as evidence for body ornamentation, implying behavioral modernity. The Iberian finds show that European Neandertals were no different from coeval Africans in this regard, countering genetic/cognitive explanations for the emergence of symbolism and strengthening demographic/social ones.

The controlled use of fire was a breakthrough adaptation in human evolution. It first provided heat and light and later allowed the physical properties of materials to be manipulated for the production of ceramics and metals. The analysis of tools at multiple sites shows that the source stone materials were systematically manipulated with fire to improve their flaking properties. Heat treatment predominates among silcrete tools at approximately 72 thousand years ago (ka) and appears as early as 164 ka at Pinnacle Point, on the south coast of South Africa. Heat treatment demands a sophisticated knowledge of fire and an elevated cognitive ability and appears at roughly the same time as widespread evidence for symbolic behavior.

Earliest modern humans out of Africa Recent paleoanthropological studies have suggested that modern humans migrated from Africa as early as the beginning of the Late Pleistocene, 120,000 years ago. Hershkovitz et al. now suggest that early modern humans were already present outside of Africa more than 55,000 years earlier (see the Perspective by Stringer and Galway-Witham). During excavations of sediments at Mount Carmel, Israel, they found a fossil of a mouth part, a left hemimaxilla, with almost complete dentition. The sediments contain a series of well-defined hearths and a rich stone-based industry, as well as abundant animal remains. Analysis of the human remains, and dating of the site and the fossil itself, indicate a likely age of at least 177,000 years for the fossil—making it the oldest member of the Homo sapiens clade found outside Africa. Science , this issue p. 456 ; see also p. 389

Ongoing debates about the emergence of modern human behavior, however defined, regularly incorporate observations from the later part of the southern African Middle Stone Age and emphasize the early appearance of artifacts thought to reflect symbolic practice. Here we report a large sample of 270 fragments of intentionally marked ostrich eggshell from the Howiesons Poort at Diepkloof Rock Shelter, Western Cape, South Africa. Dating from approximately 60,000 years ago, these pieces attest to an engraving tradition that is the earliest reliable evidence of what is a widespread modern practice. These abstract linear depictions were made on functional items (eggshell containers), which were curated and involved in daily hunter-gatherer life. The standardized production of repetitive patterns, including a hatched band motif, suggests a system of symbolic representation in which collective identities and individual expressions are clearly communicated, suggesting social, cultural, and cognitive underpinnings that overlap with those of modern people.

Abstract Iron archaeological artefacts were studied to understand long‐term corrosion by the atmosphere. Indeed, these samples collected on the construction elements of ancient monuments present ancient rust layers formed during their exposure over centuries to the indoor atmosphere. Thanks to Raman spectroscopy and the acquisition of hyperspectral images of the corrosion scales, several zones of the samples observed on cross sections could be characterised. It has been shown on six dated samples that the main phase is goethite (α‐FeOOH). Lepidocrocite and akaganeite (γ‐FeOOH and β‐FeOOH) occur locally in the corroded products, often correlated with cracks. A less crystallised phase, a hydrated oxy‐hydroxide, has been identified abundantly in more or less extended zones inside the layer. This phase could play an important role in atmospheric corrosion mechanisms. Copyright © 2006 John Wiley & Sons, Ltd.

Determining the extent of overlap between modern humans and other hominins in Eurasia, such as Neanderthals and Denisovans, is fundamental to understanding the nature of their interactions and what led to the disappearance of archaic hominins. Apart from a possible sporadic pulse recorded in Greece during the Middle Pleistocene, the first settlements of modern humans in Europe have been constrained to ~45,000 to 43,000 years ago. Here, we report hominin fossils from Grotte Mandrin in France that reveal the earliest known presence of modern humans in Europe between 56,800 and 51,700 years ago. This early modern human incursion in the Rhône Valley is associated with technologies unknown in any industry of that age outside Africa or the Levant. Mandrin documents the first alternating occupation of Neanderthals and modern humans, with a modern human fossil and associated Neronian lithic industry found stratigraphically between layers containing Neanderthal remains associated with Mousterian industries.

Abstract The description and identification of corrosion products formed on archaeological iron artefacts need various approaches at different observation scales. For this study, samples from five sites were prepared using two techniques. The first consists in cutting cross‐sections perpendicular to corrosion layers. This allows local observations and analysis of the corrosion layer stratigraphy at different levels. The second consists in performing manual grinding or abrading of the corrosion layers starting from the current surface of the excavated artefact to the metal core. It allows the description of the successive layers and is well adapted for the analysis on a larger scale. In addition to these two observation scales, the identification of the iron oxides formed needs the coupling of several complementary techniques. Elementary compositions were determined by scanning electron microscopy–energy‐dispersive x‐ray (SEM–EDX) analysis and electron probe microanalysis (EPMA). Structural identification was performed by x‐ray micro‐diffraction under synchrotron radiation (µXRD) and micro‐Raman spectroscopy. These analyses were performed on the same samples with both x‐ray diffraction and Raman spectroscopy in order to ensure a reliable characterization. In some cases there are some ambiguities or overlapping between signatures of different phases by µXRD (such as maghaemite–magnetite) or Raman spectroscopy (such as goethite–magnetite) which can be overcome by the association of the two methods. The final aim is to set up an analytical methodology that will be optimal for the study of ancient iron corrosion products. It is the first step in the study of long‐term mechanisms of iron in soil. Copyright © 2004 John Wiley & Sons, Ltd.

Palestine and Egypt supplied the Mediterranean and Europe with virtually all of its glass for most of the first millennium CE. While the Muslim conquest in the 7th century saw major political and economic adjustment, immediate changes to material culture appear to have been minimal. This paper examines the impact of the Byzantine-Islamic transition on the natron glass industry of Palestine from the 7th to 12th century. A series of 133 well-contextualised glass vessels from selected excavations in modern day Israel have been analysed for major, minor and trace elements using LA-ICP-MS. These glasses are assigned to previously established primary production groups, allowing the elucidation of the chronology of key changes in glass production in the region. Results indicate a relatively abrupt compositional change in the late 7th - early 8th centuries, covering the reforming reigns of al-Malik and al-Walid, which marks the end of “Byzantine” glass production and the establishment of the furnaces at Bet Eli'ezer. At about this time there was an influx of glass of an Egyptian composition. Production of Bet Eli'ezer type glass appears to have been limited to a short time span, less than 50 years, after which natron glass production in Palestine ceased. Plant ash glass is first encountered in the late 8th-early 9th century, probably as a result of reduced local natron glass production creating the conditions in which plant ash glass technology was adopted. Egypt continued to produce natron glass for up to a century after its demise in Palestine. It is reasoned that the change and then collapse in natron glass production in Palestine may well have been as a consequence of a reduction in the quantities of available natron. This affected Palestine first, and Egypt up to 100 years later, which suggests that the factors causing the reduction in natron supply originated at the source and were long term and gradual, not short term events. • Dataset of LA-ICP-MS analyses of early Islamic Palestinian and Egyptian glass. • Trace element data for Apollonia and Bet Eli'ezer production sites. • New chronology for changes in glass production in the Palestinian glass industry. • First plant ash glass in Palestine recognised in the late 8th century. • Changes to production broadly coincident with political changes in the early and late 8th century.

The hunting methods of the Neanderthals are rarely evident in detail in the archaeological record. Here, the rare and important discovery of a fragment of broken Levallois point, embedded in the neck-bones of a wild ass, provokes plenty of discussion of the methods of hafting and killing game in the Middle Palaeolithic of Syria.

Dans un article antérieur, nous présentions un modèle d'approvisionnement en cobalt pour l'industrie verrière en France, pour la période s'étalant de l'Antiquité à nos jours. Nous avons récemment étendu cette étude aux glaçures de céramiques. Les premiers résultats que nous présentons ici concernent un échantillonnage très varié tant du point de vue géographique que chronologique. Ces résultats confirment et affinent ceux obtenus sur le verre pour la période postérieure au XIIIe siècle. Ils montrent, de plus, que les résultats obtenus sur les verres français peuvent être généralisés à la partie occidentale du Bassin Méditerranéen. Pour la partie orientale de ce bassin, ils ouvrent de nouvelles perspectives de recherche.

The description and identification of corrosion products formed on archaeological iron artefacts need various approaches at different observation scales. Among analytical techniques available to document phase structure at the microscopic range, Raman spectroscopy offers sensitivity and discrimination between iron corrosion products with an easy implementation. Results obtained for iron artefacts corrosion in soils and atmosphere are presented. Corrosion forms observed for anoxic and aerated soils on one hand and indoor atmosphere on the other are documented. Beyond the identification and organisation of corrosion products through hyperspectral imaging, Raman micro-spectroscopy could also provide quantitative phase proportions which will be needed in the proposition of reactivity diagnosis indicators.

The date of the first settlement of the Americas remains a contentious subject. Previous claims for very early occupation at Pedra Furada in Brazil were not universally accepted (see Meltzer et al. 1994). New work at the rockshelter of Boqueirão da Pedra Furada and at the nearby open-air site of Vale da Pedra Furada have however produced new evidence for human occupation extending back more than 20 000 years. The argument is supported by a series of 14 C and OSL dates, and by technical analysis of the stone tool assemblage. The authors conclude that the currently accepted narrative of human settlement in South America will have to be re-thought. The article is followed by a series of comments, rounded off by a reply from the authors.

The Arabian Peninsula is a key region for understanding climate change and human occupation history in a marginal environment. The Mundafan palaeolake is situated in southern Saudi Arabia, in the Rub' al-Khali (the 'Empty Quarter'), the world's largest sand desert. Here we report the first discoveries of Middle Palaeolithic and Neolithic archaeological sites in association with the palaeolake. We associate the human occupations with new geochronological data, and suggest the archaeological sites date to the wet periods of Marine Isotope Stage 5 and the Early Holocene. The archaeological sites indicate that humans repeatedly penetrated the ameliorated environments of the Rub' al-Khali. The sites probably represent short-term occupations, with the Neolithic sites focused on hunting, as indicated by points and weaponry. Middle Palaeolithic assemblages at Mundafan support a lacustrine adaptive focus in Arabia. Provenancing of obsidian artifacts indicates that Neolithic groups at Mundafan had a wide wandering range, with transport of artifacts from distant sources.

Le but de ce travail est l'étude de la provenance des colorants bleus au cobalt utilisés par les verriers, de l'Age du Bronze jusqu'au XVIIIe siècle. Les premiers résultats que nous présentons ici concernent essentiellement les verres médiévaux d'ateliers du sud et de l'est de la France. Ces résultats nous permettent à la fois de mettre en évidence l'existence de quatre principaux types de minerais de cobalt parmi les verres étudiés et de préciser les périodes d'utilisation et l'origine de certains d'entre eux.

Compositional data of archaeological glasses offer an opportunity to trace the movement of materials in the ancient and medieval world. The lack of a comprehensive record of well-dated samples from Egypt, one of the major producers of glass throughout the first millennium CE, has limited the systematic application of a chronological and geographical model. Here, we report LA-ICP-MS results of Islamic glass weights and stamps from Egypt that provide a precise record of high temporal resolution of glass compositions from Abd al-Malik's monetary reform in 697 CE to the year 1020 CE. This period covers several radical changes in Islamic glassmaking. After a significant hiatus in the production of glass weights between the last quarter of the ninth and the middle of the tenth century we see the advent of novel glassmaking recipes based on the use of soda-rich plant ash. Our study establishes a temporal model that serves as a tool for dating archaeological glass assemblages, as well as a geographical model that allows for a clear classification of Levantine and Egyptian plant ash glasses.

Abstract The authors identify natural bitumen on stone implements dating to 70 000 BP. It is proposed that this represents residue from hafting, taking the practice back a further 30 000 years from the date previously noted and published in Nature . The bitumen was tracked to a source 40km away, using gas chromatography-mass spectrometry and carbon isotopes.

In this work, we study borate glasses doped with a low concentration of iron oxide by X band (9.5 GHz) electron magnetic resonance. These glasses (composition: 0.63B2O3–0.37Li2O–0.75×10−3 Fe2O3 in mole %) were annealed at increasing temperatures Ta, starting at the glass transition temperature. A new composite resonance at gef≈2.0 arises in the spectra measured at room temperature (300 K). The narrow component of this resonance is predominant in glasses annealed at lower Ta while the broad component increases in intensity as Ta increases. This resonance is ascribed to an assembly of superparamagnetic nanoparticles of a crystalline iron-containing compound. Numerical simulations assuming a lognormal particle volume distribution show that the mean particle diameter increases from 5.3 to 8.5 nm as Ta increases from 748 to 823 K. The integrated spectra intensity shows that the total number of spins in the nanoparticles increases rapidly with Ta. At lower anneal temperatures Ta, a striking increase occurs in the particle diameters, while at higher Ta these diameters reach a limit value. When the measurement temperature is increased, the resonance spectra show a reversible narrowing and an increase in intensity. The temperature dependence of the individual linewidths is attributed to thermal fluctuations of the orientations of the magnetic moments with respect to the magnetic anisotropy axes.

Les nouvelles investigations menées sur les tufs du bassin de la Somme dans le cadre du programme SITEP (CNRS) ont permis de mettre en évidence une formation tufacée reposant sur une nappe alluviale en position de très basse terrasse à Caours (Scardon). La séquence de tufs est séparée de la nappe alluviale périglaciaire sous-jacente par des limons fluviatiles calcaires se terminant par un petit sol de marais coiffé par un liseré de tourbe compactée. La formation tufacée proprement dite comporte essentiellement des faciès palustres à nombreux restes végétaux encroûtés en place et des concrétions travertineuses de type stromatolithes. En direction de la vallée actuelle l’ensemble passe rapidement à des faciès nettement fluviatiles à oncolithes structurés en grandes lentilles à stratifications obliques. La séquence de tuf ainsi que les limons fluviatiles ont livré une abondante faune malacologique qui a permis de décrire une évolution climatique contemporaine des phases initiales d’un interglaciaire, suivi d’un optimum climatique, puis d’une phase de réouverture du milieu exprimant le déclin des conditions tempérées. La base du tuf comporte plusieurs horizons organiques qui ont livré des restes de grands mammifères et de rongeurs contemporains de l’optimum interglaciaire déterminé par les assemblages malacologiques. Dans ces horizons, plusieurs niveaux du Paléolithique moyen ont été découverts en place, en association avec des restes de grande faune interglaciaire fortement fracturés par l’action de l’homme et présentant des traces de découpe. Compte tenu de sa position dans le système de la Somme, des datations par U/Th obtenues sur le tuf (moyenne : ± 120 ka BP) et des conclusions des études bioclimatiques, la séquence de Caours représente le premier témoin de l’interglaciaire Eemien en contexte fluviatile dans le bassin de la Somme. Enfin, les niveaux archéologiques découverts à Caours constituent un exemple unique d’occupation humaine contemporaine du dernier interglaciaire dans la France septentrionale.

The calendering process aims at enhancing the electrode energy density, and improving the electronic conductivity, and determines the final porous electrode micro/mesostructure. In this sense, one of the main parameters of interest is its impact in the electrode porosity (ε) and the electrochemical performance. Here, we present a systematic study of the calendering conditions (applied calender pressure and roll temperature) effect on the final NMC-based electrodes ε in terms of the active material/carbon additive/binder composition and the amount of solvent used during the preparation of the slurries. The calendering processability was assessed through the cathodes compressibility resistance and minimal attainable ε, the electrode mechanical properties (hardness and elastic deformability), the pore size distribution, the electrode film mesostructure and the C-rate cathode electrochemical performance. Based on our results, it was found that the distribution and organization of the inactive carbon black (CB)/PVdF phase and the electrode mesostructure are the key parameters that control the cathode processability through calendering. Electrodes with high CB/PVdF content and prepared with higher amounts of solvent in the slurry ensure a good electronic conductivity and a film-like structure of the electronic conducting phase around the NMC particles which upon calendering outputs a better electrochemical performance.