- Proteomics, Archaeology, Collagen, LCMSMS, TOF-SIMS, MALDI-TOF, and 19 moreBones, Mummy Studies, ATR-FTIR, SEM-EDX, IRMS, Stable Isotope Analysis, Powder X-Ray Diffraction, Pair Distribution Function, FTIR SPECTROSCOPY CULTURAL HERITAGE, Raman Spectroscopy, Ancient Cosmetics, Py GC/MS, Radiocarbon Dating (Archaeology), Rock painting, Science for Conservation and Restoration of Cultural Heritage, Ancient Biological Tissue, Bioarchaeology, Mortuary archaeology, and AMS 14C datingedit
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Collagen glue has been used for nearly two centuries to consolidate bone material, although its prevalence in museum collections is only now becoming visible. Identifying and removing collagen glue is crucial before the execution of any... more
Collagen glue has been used for nearly two centuries to consolidate bone material, although its
prevalence in museum collections is only now becoming visible. Identifying and removing collagen
glue is crucial before the execution of any geochemical or molecular analyses. Palaeolithic bone
objects from old excavations intended for radiocarbon dating were frst analysed using ZooMS
(Zooarchaeology by Mass Spectrometry) to identify the animal species, however peaks characteristic
of both cattle and whale were discovered. Two extraction methods for ZooMS were tested to identify
the authentic animal species of these objects, which revealed that these were originally whale bone
objects that had been consolidated with cattle collagen glue. This is the frst time animal collagen glue
has been identifed in archaeological remains with ZooMS, illustrating again the incredible versatility
of this technique. Another technique, Fourier Transform Infrared Spectroscopy in Attenuated Total
Refectance mode (FTIR-ATR), was also tested if it could rapidly identify the presence of collagen
glue in archaeological bone material, which was not the case. Two other cleaning methods were
tested to remove bone glue contamination prior to radiocarbon dating, along with two modifed
collagen extraction methods for ZooMS. These methods were applied to bone blank samples
(FmC= 0.0031 ± 0.0002, (n= 219), 47 336 ± 277 yr BP) that were experimentally consolidated with
collagen glue and to the Palaeolithic bone material (ca. 15 000 and 12 000 yr BP). The experimental
bone blanks produced excellent 14C ages, suggesting the cleaning methods were successful, however
the 14C ages for some of the Palaeolithic material remained too young considering their contextual
age, suggesting that the collagen glue contamination had most likely cross-linked to the authentic
collagen molecule. More research is needed in order to gain a deeper understanding of the occurrence
and elimination of cross-linked collagen-based glues in material from museum collections.
prevalence in museum collections is only now becoming visible. Identifying and removing collagen
glue is crucial before the execution of any geochemical or molecular analyses. Palaeolithic bone
objects from old excavations intended for radiocarbon dating were frst analysed using ZooMS
(Zooarchaeology by Mass Spectrometry) to identify the animal species, however peaks characteristic
of both cattle and whale were discovered. Two extraction methods for ZooMS were tested to identify
the authentic animal species of these objects, which revealed that these were originally whale bone
objects that had been consolidated with cattle collagen glue. This is the frst time animal collagen glue
has been identifed in archaeological remains with ZooMS, illustrating again the incredible versatility
of this technique. Another technique, Fourier Transform Infrared Spectroscopy in Attenuated Total
Refectance mode (FTIR-ATR), was also tested if it could rapidly identify the presence of collagen
glue in archaeological bone material, which was not the case. Two other cleaning methods were
tested to remove bone glue contamination prior to radiocarbon dating, along with two modifed
collagen extraction methods for ZooMS. These methods were applied to bone blank samples
(FmC= 0.0031 ± 0.0002, (n= 219), 47 336 ± 277 yr BP) that were experimentally consolidated with
collagen glue and to the Palaeolithic bone material (ca. 15 000 and 12 000 yr BP). The experimental
bone blanks produced excellent 14C ages, suggesting the cleaning methods were successful, however
the 14C ages for some of the Palaeolithic material remained too young considering their contextual
age, suggesting that the collagen glue contamination had most likely cross-linked to the authentic
collagen molecule. More research is needed in order to gain a deeper understanding of the occurrence
and elimination of cross-linked collagen-based glues in material from museum collections.
International audienc
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This paper presents new results of on-wall and excavated pigments from two major rock art sites in northern Australia: the ‘Genyornis’ site, and Nawarla Gabarnmang. The former site has been argued in the archaeological literature to... more
This paper presents new results of on-wall and excavated pigments from two major rock art sites in northern Australia: the ‘Genyornis’ site, and Nawarla Gabarnmang. The former site has been argued in the archaeological literature to feature a painting of Genyornis newtoni, thought to have become extinct across Australia 40-45,000 years ago. The second site, Nawarla Gabarnmang, has extensive paintings on its ceiling and pillar walls as well as numerous coloured rocks (some of which are demonstrably ochre crayons) recovered by excavation. To determine the constituents and modes of preparation, pigment sources, and the potential antiquity of on-wall paintings at the ‘Genyornis’ site, tiny pieces of both pigmented and unpigmented rock were sampled from the‘Genyornis’ panel. X-ray fluorescence, SEM-EDX, PIXE, Raman and infrared spectroscopies, and XRD analyses were undertaken to determine the natural or cultural status of the excavated coloured rocks (potential ochre pieces)from Nawarla ...
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The house mouse (Mus musculus) is one of the most invasive mammals and an evolutionary model. However, the timing and components of its origin and dispersal remain poorly documented. To track its synanthropisation and subsequent... more
The house mouse (Mus musculus) is one of the most invasive mammals and an evolutionary model. However, the timing and components of its origin and dispersal remain poorly documented. To track its synanthropisation and subsequent biological invasion during the develoment of complex human societies, we analyzed 829 Mus specimens from 43 archaeological contexts in Southwestern Asia and Southeastern Europe, dating between 40,000 and 3,000 cal. BP, combining geometric morphometris numerical taxonomy with ancient mitochondrial DNA and direct radiocarbon dating. We found that large early hunter-gatherer sedentary settlements in the Levant, c. 14,500 cal BP, drove the commensal pathway of Mus musculus, but it was the emergence of agriculture 12,000 years ago that fostered its biological invasion throughout the Near East, with its earliest stowaway transport identified in Cyprus as early as 10,800 years ago. However, the Neolithic spread of domestic animals and plants across Europe did not f...
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Abstract Phenotypic variation was characterized in 187 modern and archaeological specimens of the lesser white-toothed shrew (Crocidura suaveolens), obtained from both insular and continental European locations. Geometric morphometric... more
Abstract Phenotypic variation was characterized in 187 modern and archaeological specimens of the lesser white-toothed shrew (Crocidura suaveolens), obtained from both insular and continental European locations. Geometric morphometric methods were used to quantify variation in size and shape of the mandible. The phenotypic distance between populations, and the influence of several eco-geographical factors on the size and shape of the mandible in island populations, were assessed. Based on mandible shape divergence, the populations of C. suaveolens were clustered into continental, insular Atlantic and insular Mediterranean groups. Archaeological specimens from Molene Island, more than 3400 years old, display a mandible shape signal closer to that of the continental population than those of modern island populations. Conversely, the continental shape signals of the modern populations from Hoedic and Sark suggest that these are relatively recent anthropogenic introductions. The populations of C. suaveolens from both the Atlantic and Mediterranean islands (except for Rouzic and Cyprus) show a significant increase in mandible size, compared to those from continental Europe. Significant phenotypic differences support the indigenous condition of C. suaveolens on most of the Atlantic islands, suggesting that the species arrived there before the separation of the Scilly Isles and Ushant from the continent due to the post-glacial rise in sea level. This provides an ante quem for its colonization of the north-western fringe of continental Europe, notwithstanding its absence from the region in the present day.
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Research Interests:
Bone remains of small vertebrate fossils provide valuable information for paleoenvironmental and paleoclimatic reconstructions. However, direct radiocarbon dating of small vertebrates remains challenging as the extraction of sufficient... more
Bone remains of small vertebrate fossils provide valuable information for paleoenvironmental and paleoclimatic reconstructions. However, direct radiocarbon dating of small vertebrates remains challenging as the extraction of sufficient good quality collagen is required. The efficiency of eight collagen extraction protocols was tested on seven samples, representative of different ages and burial environments, including both macro and small vertebrate taxa. First, the samples were prescreened using attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR) to quantify collagen content in archaeological bones, revealing that one should be discarded for 14C dating. Then, the quantity of protein extracted (yield) and collagen integrity were checked using conventional elemental analysis. The results show that one protocol was not able to accurately extract collagen from the samples. A soft HCl-based protocol seems more appropriate for the pretreatment of archaeologica...
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This article demonstrates the possibility to perform X-ray diffraction/scattering computed tomography experiments with a laboratory diffraction setup. This technique is useful to characterize samples with inhomogeneities on a length scale... more
This article demonstrates the possibility to perform X-ray diffraction/scattering computed tomography experiments with a laboratory diffraction setup. This technique is useful to characterize samples with inhomogeneities on a length scale of a couple of hundred micrometres. Furthermore, the method can be applied to preliminary phase-selective imaging prior to higher-resolution characterization using synchrotron radiation. This article presents the results of test experiments carried out on a rhombohedral C60sample previously studied at the ESRF.
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Conservation of the preserving medium is an essential element for the proper preservation of specimens in fluid collections. However, the preservatives can become chemically altered over time or be lost by processes such as evaporation.... more
Conservation of the preserving medium is an essential element for the proper preservation of specimens in fluid collections. However, the preservatives can become chemically altered over time or be lost by processes such as evaporation. To combat such changes and properly care for and maintain immersed specimens, it is therefore necessary to know what preservative fluid was initially chosen and how its chemistry may have evolved with time. The present work explores the possibilities offered by Raman spectrometry for a rapid, nondestructive, noninvasive alternative to commonly employed chemical identification tests, which are often limited to the identification of simple fluids. In a first step, fluids were reconstituted and analyzed in small standard glass containers to evaluate the potential of the technique. Then we successfully applied the procedure to real cases and considered its possible use to estimate the concentration of ethanol and to detect small quantities of formaldehyd...
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Parmi les materiaux archeologiques, les restes humains, comme la peau de momie,constituent un heritage precieux et particulier des pratiques funeraires et des modes de vieanciens. Ils donnent egalement acces a des informations sur la... more
Parmi les materiaux archeologiques, les restes humains, comme la peau de momie,constituent un heritage precieux et particulier des pratiques funeraires et des modes de vieanciens. Ils donnent egalement acces a des informations sur la degradation des tissusbiologiques sur des echelles de temps particulierement longues. L’imagerie chimique, notamment par spectrometrie de masse TOF-SIMS a ete appliquee a l’analyse de ces materiaux hybrides, particulierement complexes. Completee par d’autresmethodes d’analyse (MEB-EDX, FT-IR, DRX), cette etude a permis de preciser la structure etla composition de micro-echantillons de peau de momies naturelles ou artificielles. Pour cela,l’etape cruciale de preparation des echantillons a ete optimisee. Afin de comprendre les processus de degradations, proteiques en particulier, des tissus biologiques, anciens et modernes, de composition proches ont egalement ete analyses (os,cornes, laine, soie, cheveux et poils animaux). Notre etude a ainsi pu mettre e...
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Cet article presente les derniers resultats issus respectivement de l’etude de pigments preleves sur un panneau rupestre et de pigments excaves de deux sites majeurs d’art rupestre dans le nord de l’Australie : le site de ‘Genyornis’, et... more
Cet article presente les derniers resultats issus respectivement de l’etude de pigments preleves sur un panneau rupestre et de pigments excaves de deux sites majeurs d’art rupestre dans le nord de l’Australie : le site de ‘Genyornis’, et Nawarla Gabarnmang. Il a ete avance dans la litterature archeologique que le premier site abriterait la peinture de Genyornis newtoni, dont l’extinction est estimee a 40-45000 ans sur le continent australien. Le second site, Nawarla Gabarnmang, se caracterise quant a lui par un vaste ensemble archeologique dont les plafonds et les piliers sont recouverts de plusieurs generations de peintures ; les fouilles archeologiques ont permis de mettre au jour une importante collection de blocs colores (dont certains ont ete identifies comme etant des crayons d’ocre). Afin de determiner pour le site de ‘Genyornis’, les constituants des pigments utilises, leur mode de preparation, leur origine geographique et la chronologie des peintures, des micro-echantillons...
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Research Interests:
Conservation of the preserving medium is an essential element for the proper preservation of specimens in fluid collections. However, the preservatives can become chemically altered over time or be lost by processes such as evaporation.... more
Conservation of the preserving medium is an essential element for the proper preservation of specimens in fluid collections. However, the preservatives can become chemically altered over time or be lost by processes such as evaporation. To combat such changes and properly care for and maintain immersed specimens, it is therefore necessary to know what preservative fluid was initially chosen and how its chemistry may have evolved with time. The present work explores the possibilities offered by Raman spectrometry for a rapid, nondestructive, noninvasive alternative to commonly employed chemical identification tests, which are often limited to the identification of simple fluids. In a first step, fluids were reconstituted and analyzed in small standard glass containers to evaluate the potential of the technique. Then we successfully applied the procedure to real cases and considered its possible use to estimate the concentration of ethanol and to detect small quantities of formaldehyde (down to 1%). The results demonstrate the power of this technique, which opens up new possibilities for the management of fluid collections.
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Research Interests: Zoology, Archaeology, Near Eastern Archaeology, Zooarchaeology, Geometric Morphometrics, and 15 morePalaeolithic Archaeology, Biology, Ecology, Neolithic Archaeology, Bronze Age Europe (Archaeology), Biological invasions, Biogeography, Ancient Near East, Ancient DNA (Archaeology), Pleistocene Vertebrate, Neolithic Europe, Late Pleistocene to Early Holocene, Mouse, Mouse genetics, and Human Animal Studies
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Carbon black materials have been frequently used from prehistory as pigments for drawings and paintings and also as dyes, inks and cosmetics, since they are easy to make by burning organic matter. However, the carbonaceous phases they... more
Carbon black materials have been frequently used from prehistory as pigments for drawings and paintings and also as dyes, inks and cosmetics, since they are easy to make by burning organic matter. However, the carbonaceous phases they form are often ill-ordered and not easy to characterize. Five carbon black Roman micro samples found in vessels in houses in Pompeii were studied. These precious powders correspond to mixed phase samples that contain both crystalline and ill-ordered components. Here, a methodological approach that accomplishes the identification, quantification and mapping of the different phases in these heterogeneous samples using synchrotron-based techniques is proposed. The results were compared with those from scanning electron microscopy. Information about the nature of the mixtures and the origin of carbon black pigments is obtained. The use of charred vegetable materials is concluded, independently of the shape and the nature of the container.
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Carbon black materials have been frequently used from prehistory as pigments for drawings and paintings and also as dyes, inks and cosmetics. If these material are easy to make by burning organic matter from animal or vegetal origin (e.g.... more
Carbon black materials have been frequently used from prehistory as pigments for drawings and paintings and also as dyes, inks and cosmetics. If these material are easy to make by burning organic matter from animal or vegetal origin (e.g. peach black), they form carbonaceous phases, often ill-ordered, that can hardly be characterized [1]. This project is part of studies on archaeological cosmetics, shedding light on ancient manufacturing in physical-chemistry. Six black Roman micro samples found in vessels in Pompeii Houses were studied. To understand the composition of these complex, heterogeneous (mixture of organic/mineral, crystallized/amorphous phases) and precious black powders, a new methodology had to be developed. X-ray powder diffraction tomography enabled to locate the various phases (either crystallized or not) in virtual slices among which ill-ordered materials were analyzed using the Pair Distribution Function (PDF) [2]. X-ray diffraction data were recorded on D2AM bea...
Research Interests: Microscopy, Mass Spectrometry, Calcium, Chile, Imaging Mass Spectrometry, and 15 moreMummy Studies, Lipids, Humans, Collagen, High Resolution Transmission Electron Microscopy, Mummies, Skin, Epidermis, CHEMICAL SCIENCES, Mass Spectrometry Imaging, High Resolution, Mummy Skin, Delayed Ion Extraction, Dermis, and Keratins
Research Interests: Microscopy, Mass Spectrometry, Calcium, Chile, Imaging Mass Spectrometry, and 15 moreMummy Studies, Lipids, Humans, Collagen, High Resolution Transmission Electron Microscopy, Mummies, Skin, Epidermis, CHEMICAL SCIENCES, Mass Spectrometry Imaging, High Resolution, Mummy Skin, Delayed Ion Extraction, Dermis, and Keratins
Phenotypic variation was characterized in 187 modern and archaeological specimens of the lesser white-toothed shrew (Crocidura suaveolens), obtained from both insular and continental European locations. Geometric morphometric methods were... more
Phenotypic variation was characterized in 187 modern and archaeological specimens of the lesser white-toothed shrew (Crocidura suaveolens), obtained from both insular and continental European locations. Geometric morphometric methods were used to quantify variation in size and shape of the mandible. The phenotypic distance between populations, and the influence of several eco-geographical factors on the size and shape of the mandible in island populations, were assessed. Based on mandible shape divergence, the populations of C. suaveolens were clustered into continental, insular Atlantic and insular Mediterranean groups. Archaeological specimens from Mol ene Island, more than 3400 years old, display a mandible shape signal closer to that of the continental population than those of modern island populations. Conversely, the continental shape signals of the modern populations from H€ oedic and Sark suggest that these are relatively recent anthropogenic introductions. The populations of C. suaveolens from both the Atlantic and Mediterranean islands (except for Rouzic and Cyprus) show a significant increase in mandible size, compared to those from continental Europe. Significant phenotypic differences support the indigenous condition of C. suaveolens on most of the Atlantic islands, suggesting that the species arrived there before the separation of the Scilly Isles and Ushant from the continent due to the post-glacial rise in sea level. This provides an ante quem for its colonization of the northwestern fringe of continental Europe, notwithstanding its absence from the region in the present day.
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Because hard tissues can be radiocarbon dated, they are key to establishing the archaeological chronologies, palaeoenvironmental reconstructions and historical-biogeographical processes of the last 50,000 years. The advent of accelerator... more
Because hard tissues can be radiocarbon dated, they are key to establishing the archaeological chronologies, palaeoenvironmental reconstructions and historical-biogeographical processes of the last 50,000 years. The advent of accelerator mass spectrometers (AMS) has revolutionized the field of archaeology but routine AMS dating still requires 60–200 mg of bone, which far exceeds that of small vertebrates or remains which hold a patrimonial value (e.g. hominid remains or worked bone artefacts). Here, we present the first radiocarbon dates obtained from minute amounts of bone (3–60 mg) using a MIni CArbon DAting System (MICADAS). An optimized protocol allowed us to extract enough material to produce between 0.2 and 1.0 mg of carbon for graphite targets. Our approach was tested on known-age samples dating back to 40,000 BP, and served as proof of concept. The method was then applied to two archaeological sites where reliable dates were obtained from the single bones of small mammals. These results open the way for the routine dating of small or key bone samples. Hard tissues (i.e. bones, teeth, antler and ivory) found in the fossil record have a tremendous informative potential relevant to the fields of archaeology, palaeoecology and the history of art and technology. Because they can be identified to the species level and radiocarbon dated, these fossil remains are key to establishing the archaeological chronologies, palaeoenvironmental reconstructions and historical-biogeographical processes (i.e. post-glacial recolonization events) of the last 50,000 years. In effect, they provide us with windows to past societies, and contribute to our knowledge of ancient human evolution and cultural development 1 , palaeoclimates 2 , paleoenvi-ronments 3 and past trade networks 4. Hard tissues contain an organic phase (mainly the protein collagen type I) embedded in a mineral phase (made of a non-stoichiometric biogenic apatite). While the exchange of inorganic carbon occurs much more readily 5, 6 , the relative chemical inertness of biopolymers makes them ideal for dating; therefore, the majority of bone radiocarbon dates are obtained from the collagen phase. The chemical integrity of this biomolecule can be assessed using simple biochemical criteria such as %C, %N and C/N ratio 7–9. The amount of collagen in fresh bone is approximately 20–25% 9, 10. As the diagenetic alteration proceeds, the quantity and quality of the collagen decreases; consequently, the sample size must increase in order to compensate for protein loss. Radiocarbon dating ancient bones can therefore prove challenging. The advent of accelerator mass spectrometers (AMS) in the eighties revolutionized the field of archaeology by allowing smaller samples to be measured. While it decreases the amount of carbon required for a radiocarbon measurement by several orders of magnitude, the AMS dating of bone collagen still requires at least 60–200 mg of bone 11–13 , depending on the protein preservation and the extraction protocol. However, this is still excessive for two classes of bone remains: (1) individual bones of small vertebrates which often weigh less than 60 mg; and (2) unique remains such as hominid bones or worked bone artefacts for which curators do not permit invasive sampling 14. The specification of sample weights used for dating is not considered necessary by the scientific community 15 and is seldom reported in publications, even when supplementary information is available (see for example refs 16–19). However, careful examination of the literature suggests that attempts at dating samples smaller than 60 mg are rare. Regarding small vertebrates, only two case studies were found: the Late Prehistoric dispersal of
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Research Interests:
Bone remains of small vertebrate fossils provide valuable information for paleoenvironmental and paleoclimatic reconstructions. However, direct radiocarbon dating of small vertebrates remains challenging as the extraction of sufficient... more
Bone remains of small vertebrate fossils provide valuable information for paleoenvironmental and paleoclimatic reconstructions. However, direct radiocarbon dating of small vertebrates remains challenging as the extraction of sufficient good quality collagen is required. The efficiency of eight collagen extraction protocols was tested on seven samples, representative of different ages and burial environments, including both macro and small vertebrate taxa. First, the samples were prescreened using attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR) to quantify collagen content in archaeological bones, revealing that one should be discarded for 14 C dating. Then, the quantity of protein extracted (yield) and collagen integrity were checked using conventional elemental analysis. The results show that one protocol was not able to accurately extract collagen from the samples. A soft HCl-based protocol seems more appropriate for the pretreatment of archaeological small mammal bones, whereas a harsher protocol might be more efficient to extract a higher amount of collagen from large mammals as well as amphibian bones. The influence of the tested protocols on carbon and nitrogen isotope values was also investigated. The results showed that isotopic variability, when existing, is related to the interindividual differences rather than the different protocols.
Bone remains of small vertebrate fossils provide valuable information for paleoenvironmental and paleoclimatic reconstructions. However, direct radiocarbon dating of small vertebrates remains challenging as the extraction of sufficient... more
Bone remains of small vertebrate fossils provide valuable information for paleoenvironmental and paleoclimatic reconstructions. However, direct radiocarbon dating of small vertebrates remains challenging as the extraction of sufficient good quality collagen is required. The efficiency of eight collagen extraction protocols was tested on seven samples, representative of different ages and burial environments, including both macro and small vertebrate taxa. First, the samples were prescreened using attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR) to quantify collagen content in archaeological bones, revealing that one should be discarded for 14 C dating. Then, the quantity of protein extracted (yield) and collagen integrity were checked using conventional elemental analysis. The results show that one protocol was not able to accurately extract collagen from the samples. A soft HCl-based protocol seems more appropriate for the pretreatment of archaeological small mammal bones, whereas a harsher protocol might be more efficient to extract a higher amount of collagen from large mammals as well as amphibian bones. The influence of the tested protocols on carbon and nitrogen isotope values was also investigated. The results showed that isotopic variability, when existing, is related to the interindividual differences rather than the different protocols.
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Cersoy, S., Martinetto, P., Bordet, P., Hodeau, J.-L., Van Elslande, E., Walter, P. Five black carbon-based archaeological powders from Pompeii are fully characterized by using a combination of non-destructive techniques. Characterizing... more
Cersoy, S., Martinetto, P., Bordet, P., Hodeau, J.-L., Van Elslande, E., Walter, P.
Five black carbon-based archaeological powders from Pompeii are fully characterized by using a combination of non-destructive techniques. Characterizing these heterogeneous samples in this way provides a practical demonstration of a methodology available to be used for the identification, quantification and mapping of the crystalline and amorphous phases coexisting in a single sample.
Five black carbon-based archaeological powders from Pompeii are fully characterized by using a combination of non-destructive techniques. Characterizing these heterogeneous samples in this way provides a practical demonstration of a methodology available to be used for the identification, quantification and mapping of the crystalline and amorphous phases coexisting in a single sample.
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Ouvrage collectif
Musée de Saint-Antoine-l'Abbaye
6 juillet - 5 octobre 2014
AICr 2014
Cartels scientifiques
Musée de Saint-Antoine-l'Abbaye
6 juillet - 5 octobre 2014
AICr 2014
Cartels scientifiques
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A skin sample from a south Andean mummy dating back from the XIth century was analyzed using Time-of-flight Secondary Ion Mass Spectrometry imaging using cluster primary ion beams (cluster-TOF-SIMS). For the first time on a mummy, skin... more
A skin sample from a south Andean mummy dating back from the XIth century was analyzed using Time-of-flight Secondary Ion Mass Spectrometry imaging using cluster primary ion beams (cluster-TOF-SIMS). For the first time on a mummy, skin dermis and epidermis could be chemically differentiated using mass spectrometry imaging. Difference in amino-acid composition between keratin and collagen, the two major proteins of skin tissue, could indeed be exploited. A surprising lipid composition of hypodermis was also revealed and seems to result from fatty acids damage by bacteria. Using cluster-TOF-SIMS imaging skills, traces of bio-mineralization could be identified at the micrometer scale, especially formation of calcium phosphate at the skin surface. Mineral deposits at the surface were both characterized using scanning electron microscopy in combination with energy-dispersive X-ray spectroscopy (SEM-EDX) and mass spectrometry imaging. The stratigraphy of such a sample could be for the first time revealed using this technique. More precise molecular maps were also recorded at higher spatial resolution, below 1 µm. This was achieved using a non-bunched mode of the primary ion source, while keeping intact the mass resolution thanks to a delayed extraction of the secondary ions. Details from biological structure as can be seen on SEM images are observable on chemical maps at this sub micrometer scale. Thus, this work illustrates the interesting possibilities of chemical imaging by cluster-TOF-SIMS concerning ancient biological tissues.
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The painting materials of the Portrait of Nicolaes van Bambeeck (Royal Museums of Fine Arts of Belgium, Brussels, inv. 155) painted by Rembrandt van Rijn in 1641 has been studied using high resolution cluster-TOF-SIMS imaging. In a first... more
The painting materials of the Portrait of Nicolaes van Bambeeck (Royal Museums of Fine Arts of Belgium, Brussels, inv. 155) painted by Rembrandt van Rijn in 1641 has been studied using high resolution cluster-TOF-SIMS imaging. In a first step, a moderate spatial resolution (2 µm) was used to characterize the layer structure and the chemical composition of each layer thanks to a high mass resolution. Then, in a second step, and despite a low mass resolution, the cluster primary ion beam was focused well below 1 µm in order to reveal smaller structures in the painting sample. The study confirmed the presence of starch in the second ground layer, which is quite surprising and, at least for Rembrandt paintings, has never been reported before. TOF-SIMS also pointed out indication for the presence of proteins, which, added to the size and shape of lake particles, suggests that it was manufactured from shearings (waste of textile manufacturing) of dyed wool, used as source of the dyestuff. The analyses have also shown various lead carboxylates, being the product of the interaction between lead white and the oil of the binding medium. These findings considerably contribute to the understanding of Rembrandt’s studio practice and thus demonstrate the importance and potential of cluster-TOF-SIMS imaging in the characterization at a sub-micrometer scale of artist painting materials.igh resolution; painting cross-section.
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We report on measurements of the cavitation pressure in several liquids subjected to tension in an acoustic wave and compare the results to classical nucleation theory (CNT). This study is motivated by the sizable discrepancy between the... more
We report on measurements of the cavitation pressure in several liquids subjected to tension in an acoustic wave and compare the results to classical nucleation theory (CNT). This study is motivated by the sizable discrepancy between the acoustic cavitation threshold measured in water and the value predicted by CNT. We find that the same discrepancy is present for heavy g water, whereas the agreement is better for ethanol and heptane and intermediate in the case of dimethyl sulfoxide. It is well-known that water is an anomalous liquid, a consequence of its hydrogen-bonded network. The other liquids studied represent very different molecular interactions. Our results indicate that the cavitation threshold approaches the prediction of CNT as the surface Conversely, this raises the question of the validity of a simple theory such as CNT to account for high surface tension liquids and suggests that an appropriate microscopic model of such liquids may be necessary to correctly predict the cavitation threshold.
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Les microvertébrés sont d'excellents marqueurs environnementaux et climatiques. Par ailleurs, leur histoire phylogéographique récente n'est pas toujours bien cernée. La datation directe de leurs restes retrouvés en contexte archéologique... more
Les microvertébrés sont d'excellents marqueurs environnementaux et climatiques. Par ailleurs, leur histoire phylogéographique récente n'est pas toujours bien cernée. La datation directe de leurs restes retrouvés en contexte archéologique permettrait d'inscrire les reconstructions associées à leur découverte dans une chronologie absolue. La datation 14 C de microéchantillons osseux représente aujourd'hui un défi car cela nécessite de pouvoir extraire suffisamment de collagène purifié de toute contamination. Les os de ces taxons pèsent typiquement 20 mg alors qu'un échantillon osseux datable aujourd'hui pèse au moins 150 mg. Ils ne contiennent donc, au mieux, que quelques milligrammes de collagène pour un os frais. En conséquence, la quantité de carbone que l'on peut extraire de tels os pour la datation rend la mesure délicate sur un AMS conventionnel. Le cas des os archéologiques, pour lesquels le collagène est souvent dégradé est encore plus problématique. Pour cette raison, il était nécessaire d'une part d'optimiser la quantité de collagène extrait et d'autre part d'optimiser la mesure du 14 C restant dans les échantillons. Dans un premier temps, huit protocoles d'extractions différents, décrits dans la littérature ont été testés sur onze échantillons représentatifs. Les résultats de l'optimisation des protocoles d'extraction en termes de rendement et de qualité du collagène extrait seront rapidement évoqués. Nous nous attarderons ici sur la deuxième étape du projet c'est-à-dire l'optimisation de la dernière étape de préparation et de la datation sur le nouveau spectromètre de masse par accélérateur ECHoMICADAS. Les difficultés liées à la manipulation de microquantités de collagène, les risques de contamination ainsi que la graphitisation pour la mesure en mode « solide » seront exposés. Les résultats des tests effectués sur des os de macromammifères d'âges consensus (VIRI) seront ensuite présentés. Enfin, l'application au cas d'échantillons réels de musaraignes
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Intervention en Masters (M1 et M2) "Evolution Patrimoine Naturel et Sociétés" (EPNS), Spécialité "Quaternaire et Préhistoire", Module "Biologie pour l'Archéologie" (QP 41): Cours et démonstration (MALDI-MS et LC-MS/MS)
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(Conférence à deux voix avec Hervé Legal, ancien directeur de la société RSA le Rubis à Jarrie) Dans le cadre de l’exposition « Le cristal, un bijou pour la chimie », émerveillez-vous en voyageant au cœur de la structure des rubis et... more
(Conférence à deux voix avec Hervé Legal, ancien directeur de la société RSA le Rubis à Jarrie)
Dans le cadre de l’exposition « Le cristal, un bijou pour la chimie », émerveillez-vous
en voyageant au cœur de la structure des rubis et saphirs et découvrez comment il est aujourd’hui possible d’optimiser la croissance des cristaux de synthèse pour
des applications à la pointe de l’innovation !
Dans le cadre de l’exposition « Le cristal, un bijou pour la chimie », émerveillez-vous
en voyageant au cœur de la structure des rubis et saphirs et découvrez comment il est aujourd’hui possible d’optimiser la croissance des cristaux de synthèse pour
des applications à la pointe de l’innovation !
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Les gemmes, qu’elles soient des cristaux ou des matériaux d’origine organique, ont fasciné les hommes. Cet émerveillement tient en particulier à leurs qualités esthétiques : couleurs, formes, éclat…Certaines gemmes sont tout... more
Les gemmes, qu’elles soient des cristaux ou des matériaux d’origine organique, ont fasciné les hommes. Cet émerveillement tient en particulier à leurs qualités esthétiques : couleurs, formes, éclat…Certaines gemmes sont tout particulièrement mises en valeur par le processus de la taille.
Quels sont les mystères des pierres fines et précieuses ? Quelle est la structure de ces cristaux ? Comment expliquer les différences de propriétés optiques du rubis et du saphir ? Comment la connaissance de la cristallographie permet de connaitre leur nature ? Comment optimiser la taille accomplie par l’orfèvre ?
Grâce à des analyses physico-chimiques et cristallographiques, nous présenterons comment déterminer la nature puis l’origine géographique d’une gemme. Des exemples d’études de gemmes, comme les diamants « qui s’évaporent » ou les yeux de rubis d’une statuette de la déesse Ishtar, retrouvée dans les ruines de Babylone, seront développés.
Quels sont les mystères des pierres fines et précieuses ? Quelle est la structure de ces cristaux ? Comment expliquer les différences de propriétés optiques du rubis et du saphir ? Comment la connaissance de la cristallographie permet de connaitre leur nature ? Comment optimiser la taille accomplie par l’orfèvre ?
Grâce à des analyses physico-chimiques et cristallographiques, nous présenterons comment déterminer la nature puis l’origine géographique d’une gemme. Des exemples d’études de gemmes, comme les diamants « qui s’évaporent » ou les yeux de rubis d’une statuette de la déesse Ishtar, retrouvée dans les ruines de Babylone, seront développés.
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Pour la ligne BM02 / D2AM
Research Interests: X-Ray Absorption Spectroscopy (in Materials Characterisation/X Ray Analysis), Synchrotron Radiation, Tomography, Materials Characterization, X-ray diffraction and Rietveld Method applied areas of physics, chemistry, geology, medical and engineering and materials science., and Pair Distribution Function
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"Parmi les matériaux archéologiques, les restes humains, comme la peau de momie, constituent un héritage précieux et particulier des pratiques funéraires et des modes de vie anciens. Ils donnent également accès à des informations sur la... more
"Parmi les matériaux archéologiques, les restes humains, comme la peau de momie, constituent un héritage précieux et particulier des pratiques funéraires et des modes de vie anciens. Ils donnent également accès à des informations sur la dégradation des tissus biologiques sur des échelles de temps particulièrement longues.
L’imagerie chimique, notamment par spectrométrie de masse TOF-SIMS a été appliquée à l’analyse de ces matériaux hybrides, particulièrement complexes. Complétée par d’autres méthodes d’analyse (MEB-EDX, FT-IR, DRX), cette étude a permis de préciser la structure et la composition de micro-échantillons de peau de momies naturelles ou artificielles. Pour cela, l’étape cruciale de préparation des échantillons a été optimisée.
Afin de comprendre les processus de dégradations, protéiques en particulier, des tissus biologiques, anciens et modernes, de composition proches ont également été analysés (os, cornes, laine, soie, cheveux et poils animaux).
Notre étude a ainsi pu mettre en évidence l’apport de l’imagerie TOF-SIMS pour comprendre les processus de préparation des corps et de dégradation des tissus au cours des siècles.
"
L’imagerie chimique, notamment par spectrométrie de masse TOF-SIMS a été appliquée à l’analyse de ces matériaux hybrides, particulièrement complexes. Complétée par d’autres méthodes d’analyse (MEB-EDX, FT-IR, DRX), cette étude a permis de préciser la structure et la composition de micro-échantillons de peau de momies naturelles ou artificielles. Pour cela, l’étape cruciale de préparation des échantillons a été optimisée.
Afin de comprendre les processus de dégradations, protéiques en particulier, des tissus biologiques, anciens et modernes, de composition proches ont également été analysés (os, cornes, laine, soie, cheveux et poils animaux).
Notre étude a ainsi pu mettre en évidence l’apport de l’imagerie TOF-SIMS pour comprendre les processus de préparation des corps et de dégradation des tissus au cours des siècles.
"
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Parmi les matériaux archéologiques, les restes humains, comme la peau de momie, constituent un héritage précieux et particulier des pratiques funéraires et des modes de vie anciens. Ils donnent également accès à des informations sur la... more
Parmi les matériaux archéologiques, les restes humains, comme la peau de momie, constituent un héritage précieux et particulier des pratiques funéraires et des modes de vie anciens. Ils donnent également accès à des informations sur la dégradation des tissus biologiques sur des échelles de temps particulièrement longues.
L’imagerie chimique, notamment par spectrométrie de masse TOF-SIMS a été appliquée à l’analyse de ces matériaux hybrides, particulièrement complexes. Complétée par d’autres méthodes d’analyse (MEB-EDX, FT-IR, DRX), cette étude a permis de préciser la structure et la composition de micro-échantillons de peau de momies naturelles ou artificielles. Pour cela, l’étape cruciale de préparation des échantillons a été optimisée.
Afin de comprendre les processus de dégradations, protéiques en particulier, des tissus biologiques, anciens et modernes, de composition proches ont également été analysés (os, cornes, laine, soie, cheveux et poils animaux).
Notre étude a ainsi pu mettre en évidence l’apport de l’imagerie TOF-SIMS pour comprendre les processus de préparation des corps et de dégradation des tissus au cours des siècles.
L’imagerie chimique, notamment par spectrométrie de masse TOF-SIMS a été appliquée à l’analyse de ces matériaux hybrides, particulièrement complexes. Complétée par d’autres méthodes d’analyse (MEB-EDX, FT-IR, DRX), cette étude a permis de préciser la structure et la composition de micro-échantillons de peau de momies naturelles ou artificielles. Pour cela, l’étape cruciale de préparation des échantillons a été optimisée.
Afin de comprendre les processus de dégradations, protéiques en particulier, des tissus biologiques, anciens et modernes, de composition proches ont également été analysés (os, cornes, laine, soie, cheveux et poils animaux).
Notre étude a ainsi pu mettre en évidence l’apport de l’imagerie TOF-SIMS pour comprendre les processus de préparation des corps et de dégradation des tissus au cours des siècles.
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Research Interests:
Wet collections are rich in information to study the evolution of species or ancient pathologies. However, they are sometimes neglected, poorly documented and difficult to preserve. To keep these archives for future generations, we have... more
Wet collections are rich in information to study the evolution of species or ancient pathologies. However, they are sometimes neglected, poorly documented and difficult to preserve. To keep these archives for future generations, we have inventoried in detail the degradations observed in the collections and undertaken research on the hermeticity of the jars. To top up the jars appropriately, the fluids is first identified without opening the jar and the impact of a change of fluid from the macroscopic to the microscopic scale was studied. The results of this research are shared through publications and exchanges with collection managers.