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M. Cotte. Why do the red walls of pompeii go black? ESRF newsletter, 44:4-5, December 2006.

Why have the characteristic red walls of Pompeii, revealed by excavations of the city buried by the eruption of Vesuvius, turned black over the last two decades? ESRF's synchrotron offers new insight into this process.

M. Cotte. X-rays help to unravel brush strokes. ESRF newsletter, 44:6-7, December 2006.

Scientists and conservators combine forces to apply imaging techniques to study a Manet picture in depth.

M. Cotte. Cosmetics and paints share the same recipes. ESRF newsletter, 44(9-10), December 2006.

Scientists have recreated lead salt mixtures of similar composition used in medical remedies, make-up and oilpaints to unearth some of the secrets of the past and help them to preserve artefacts well into the future.

M. Cotte. Aztec pigment proves to be ahead of its time. ESRF newsletter, 44:11-12, December 2006.

How did the Maya civilization create a beautiful, long-lasting turquoise-blue pigment when no-one else could?

M. Cotte. Different minerals dictate colour of glass. ESRF newsletter, 44:13, December 2006.

Scientists from Italy and the ESRF are studying how the elements in glass can determine its colour.

M. Cotte. Bliss group helps to crack da vinci's code. ESRF newsletter, 44:14-15, December 2006.

The ESRF mainly contributes to research via scientific results. However, tools such as precise software can become essential in the quest for the unknown. PyMCA is a programme for online and offline X-ray spectrum analysis that was developed by the ESRF for its beamlines, but it is also being used in art research.

M. Cotte, J. Susini, N. Metrich, A. Moscato, C. Gratziu, A. Bertagnini, et M. Pagano. Blackening of Pompeian cinnabar paintings: X-ray microspectroscopy analysis. Anal. Chem., 78(21):7484 -7492, November 2006. [ doi ]

Red Pompeian paintings, very famous for their deep intensity, are currently suffering from darkening. The origins of this darkening degradation are not clearly identified yet and remain a major issue for curators. In the specific case of cinnabar (HgS)-based red pigment, a photoinduced conversion into black metacinnabar is usually suspected. This work is focused on the blackening of red cinnabar paintings coated on a sparry calcite mortar. Different samples exhibiting different levels of degradation were selected upon visual observations and analyzed by synchrotron-based microanalytical techniques. Atomic and molecular compositions of the different debased regions revealed two possible degradation mechanisms. On one hand, micro X-ray fluorescence elemental maps show peculiar distributions of chlorine and sulfur. On the other hand, X-ray absorption spectroscopy performed at both Cl and S K-edges confirms the presence of characteristic degradation products: (i) Hg-Cl compounds (e.g., corderoite, calomel, and terlinguaite), which may result from the reaction with exogenous NaCl, in gray areas; (ii) gypsum, produced by the calcite sulfation, in black coatings. Metacinnabar is never detected. Finally, a cross section was analyzed to map the in-depth alteration gradient. Reduced and oxidized sulfur distributions reveal that the sulfated black coating consists of a  5-μm-thick layer covering intact cinnabar.

J. W. Hagadorn, S. Xiao, P. C. J. Donoghue, S. Bengtson, N. J. Gostling, M. Pawlowska, E. C. Raff, R. A. Raff, F. R. Turner, Y. Chongyu, C. Zhou, X. Yuan, M. B. McFeely, M. Stampanoni, et K. H. Nealson. Cellular and Subcellular Structure of Neoproterozoic Animal Embryos. Science, 314(5797):291 - 294, October 2006. [ doi ]

Stereoblastic embryos from the Doushantuo Formation of China exhibit occasional asynchronous cell division, with diminishing blastomere volume as cleavage proceeded. Asynchronous cell division is common in modern embryos, implying that sophisticated mechanisms for differential cell division timing and embryonic cell lineage differentiation evolved before 551 million years ago. Subcellular structures akin to organelles, coated yolk granules, or lipid vesicles occur in these embryos. Paired reniform structures within embryo cells may represent fossil evidence of cells about to undergo division. Embryos exhibit no evidence of epithelial organization, even in embryos composed of  1000 cells. Many of these features are compatible with metazoans, but the absence of epithelialization is consistent only with a stem-metazoan affinity for Doushantuo embryos.

L. Tian, N. Zhen-Wei, et W. Chang-Sui. Study on colored drawing technique of Qionglai kiln by SRXRF. Spectrosc. Spectr. Anal., 26(8):1560-1563, August 2006.

The colored drawing technique of Qionglai kiln is a debate problem in the archaeology and ancient ceramic research. In the present paper, SRXRF linescan technology was used to study the distribution mode of the colorific elements on the cross-sections of samples. The analytical result indicates that there existed two kinds of decoration techniques of colored drawing, i.e. the techniques of the underglaze color and oveglaze color coexisted in that time.

P. C. J. Donoghue, S. Bengtson, X. P. Dong, N. J. Gostling, T. Huldtgren, J. A. Cunningham, C. Yin, Z. Yue, F. Peng, et M. Stampanoni. Synchrotron X-ray tomographic microscopy of fossil embryos. Nature, 442(7103):680-683, August 2006. [ doi ]

Fossilized embryos from the late Neoproterozoic and earliest Phanerozoic have caused much excitement because they preserve the earliest stages of embryology of animals that represent the initial diversification of metazoans(1-4). However, the potential of this material has not been fully realized because of reliance on traditional, non- destructive methods that allow analysis of exposed surfaces only(1-4), and destructive methods that preserve only a single two- dimensional view of the interior of the specimen(5,6). Here, we have applied synchrotron- radiation X- ray tomographic microscopy ( SRXTM)(7), obtaining complete three-dimensional recordings at submicrometre resolution. The embryos are preserved by early diagenetic impregnation and encrustation with calcium phosphate, and differences in X- ray attenuation provide information about the distribution of these two diagenetic phases. Three- dimensional visualization of blastomere arrangement and diagenetic cement in cleavage embryos resolves outstanding questions about their nature, including the identity of the columnar blastomeres. The anterior and posterior anatomy of embryos of the bilaterian worm- like Markuelia confirms its position as a scalidophoran, providing new insights into body- plan assembly among constituent phyla. The structure of the developing germ band in another bilaterian, Pseudooides, indicates a unique mode of germ- band development. SRXTM provides a method of non- invasive analysis that rivals the resolution achieved even by destructive methods, probing the very limits of fossilization and providing insight into embryology during the emergence of metazoan phyla.

S. J. Veith. Unearthing the Neanderthal, digitally. Biophotonics Int., 13(8):84-85, August 2006.

L. Marivaux, Y. Chaimanee, P. Tafforeau, et J.-J. Jaeger. New Strepsirrhine primate from the late Eocene of peninsular Thailand (Krabi Basin). Am. J. Phys. Anthrop., 130(4):425-434, August 2006. [ doi ]

In this paper, we describe the newly discovered lower jaw of a primate from the late Eocene Krabi coal mine (Bang Mark pit) of Peninsular Thailand. We performed microtomographic examinations at the European Synchrotron Radiation Facility (ESRF, Grenoble, France) to analyze different morphological aspects of the jaw and teeth. Although partially preserved, this fossil mandible reveals a set of distinctive dental traits (e.g., double-rooted P2 and molarized P4) that allow us to describe a new stepsirrhine adapiform: Muangthanhinius siami, new genus and species. This taxon is somewhat atypical among Paleogene adapiforms, and more specialized than the sivaladapid adapiforms (hoanghoniines) that existed in Asia in the same epoch. In fact, Muangthanhinius shows a degree of dental specialization approximating that of some modern strepsirrhine lemuriforms, although it lacks the highly specialized anterior dentition characterizing this living primate group (canine + incisors forming a very procumbent tooth-comb). In contrast, Muangthanhinius exhibits a large canine deeply anchored within the dentary that probably protruded high above the toothrow. Finally, despite the development of a molarized P4 as in Miocene sivaladapid sivaladapines, Muangthanhinius differs in molar morphology from this group, and the position of this new taxon within the Adapiformes remains indeterminate. Clarification of its phylogenetic position will require more morphological evidence than is currently available.

L. Marivaux, L. Bocat, Y. Chaimanee, J. J. Jaeger, B. Marandat, P. Srisuk, P. Tafforeau, C. Yamee, et J. L. Welcomme. Cynocephalid dermopterans from the Palaeogene of South Asia (Thailand, Myanmar and Pakistan): systematic, evolutionary and palaeobiogeographic implications. Zoologica Scripta, 35(4):395-420, July 2006. [ doi ]

Cynocephalid dermopterans (flying lemurs) are represented by only two living genera (Cynocephalus and Galeopterus), which inhabit tropical rainforests of South-East Asia. Despite their very poor diversity and their limited distribution, dermopterans play a critical role in higher-level eutherian phylogeny inasmuch as they represent together with Scandentia (tree-shrew) the sister group of the Primates clade (Plesiadapiformes + Euprimates). However, unlike primates, for which the fossil record extends back to the early Palaeogene on all Holarctic continents and in Africa, the evolutionary history of the order Dermoptera sensu stricto (Cynocephalidae) has so far remained undocumented, with the exception of a badly preserved fragment of mandible from the late Eocene of Thailand (Dermotherium major). In this paper, we described newly discovered fossil dermopterans (essentially dental remains) from different regions of South Asia (Thailand, Myanmar, and Pakistan) ranging from the late middle Eocene to the late Oligocene. We performed microtomographic examinations at the European Synchrotron Radiation Facility (ESRF, Grenoble, France) to analyse different morphological aspects of the fossilized jaws. The abundant material from the late Oligocene of Thailand (Nong Ya Plong coal mine) allows us to emend the diagnosis of the genus Dermotherium and to describe a new species: Dermotherium chimaera sp. n. This species exhibits an interesting mosaic of plesiomorphic cynocephalid characters shared with Cynocephalus and Galeopterus, and as such, it probably documents a form close to the ancestral morphotype from which the two extant forms are derived (supported by cladistic assessment of the dental evidence). The discovery of Palaeogene cynocephalids is particularly significant since it attests to the great antiquity of the order Dermoptera in Asia, and besides, it provides the first spatio-temporal glimpse into the evolutionary history of that enigmatic mammal group. In that respect, these fossils testify to a long history of endemism in South Asia for dermopterans, and demonstrate that their modern geographic restriction in south-eastern Asia is clearly a relictual distribution. Cynocephalids had a more widespread distribution during the Palaeogene, which extended from the Indian subcontinent (the rafting Greater India) to South-East Asia. Their subsequent extinction on the Indian subcontinent was probably mediated by the major palaeogeographic and geomorphologic events related to the India-Eurasia collision (retreat of the Paratethys Sea, formation of orogenic highlands) that have strongly affected the climate of South Asia at the end of the Oligocene.

S. Padovani, D. Puzzovio, C. Sada, P. Mazzoldi, I. Borgia, A. Sgamellotti, B. G. Brunetti, L. Cartechini, F. d'Acapito, C. Maurizio, F. Shokoui, P. Oliaiy, J. Rahighi, M. Lamehi-Rachti, et E. Pantos. XAFS study of copper and silver nanoparticles in glazes of medieval middle-east lustreware (10th-13th century). Appl. Phys. A, 83(4):521-528, June 2006. [ doi ]

E. Welcomme, P. Walter, E. van Elslande, et G. Tsoucaris. Investigation of white pigments used as make-up during the Greco-Roman period. Appl. Phys. A, 83(4):551-556, June 2006. [ doi ]

M. O. Figueiredo, J. P. Veiga, et J. P. Mirao. Modelling the size of red-colouring copper nanoclusters in archaeological glass beads. Appl. Phys. A, 83(4):499-502, June 2006. [ doi ]

The origin of a red colour in ancient soda-lime glasses has been attributed either to the presence of both copper clusters and cuprous oxide or to copper alone. As a contribution to this question, a non-destructive X-ray absorption study at the [Cu]K-edge was undertaken on the red layer from a singular 'rosette'-type archaeological glass bead dated as pre-XVII century. On comparing with data collected from metallic copper and the mineral cuprite, cubic Cu2O, XANES spectra of the red glass are identical to the first. Theoretical modelling of Cu 1s XANES spectra was undertaken using the FEFF code based on a multiple scattering formalism. A hypothetical tetragonal structure was simulated for Cu2O in order to remove the constraints arising from linear O-Cu-O bonds, unstable within the silica glass matrix, and an ideal body-centred array was considered on the basis of real metallic Cu-Cu distances in the metal. Calculations were performed for atom clusters of variable size within real and hypothetical structures. A spherical cluster of about 5 angstrom radius, capped by 24 copper atoms already provides a calculated Cu 1s XANES spectrum that compares well with data collected from the red glass. Post-edge details are noted in relation to the oxide, considering ionic states and effective valences of copper. The possibility of estimating the size of copper clusters through simulated structures is discussed.

J. P. Veiga et M. O. Figueiredo. Copper blue in an ancient glass bead: a XANES study. Appl. Phys. A, 83(4):547-550, June 2006. [ doi ]

The blue colour in ancient soda-lime glasses has been attributed to the presence of copper and/or cobalt but the origin of different shades is not yet fully interpreted. As a contribution to this question, a non-destructive X-ray absorption study at [ (C)u]K-edge was undertaken on the blue (turquoise) layer from a 'Nueva Cadiz' type tubular glass bead dated pre-XVII century where copper is the unique colouring agent. Minerals configuring two distinct blue tonalities due to Cu (2+) in similar square coordination were selected as basic model compounds: azurite, which is a classical navy-blue pigment used in ancient wall paintings over plaster, and chalcanthite, displaying exactly the same turquoise-blue tonality of tubular glass beads manufactured since the Egyptian Antiquity. Theoretical modelling of the XAFS spectra was undertaken using the FEFF code. The IFEFFIT software package was used for fitting the calculated spectra to experimental data. EXAFS results are discussed in view of the crystal structures of copper minerals chosen to model the speciation state and structural situation of that element prevailing in the turquoise-blue archaeological glass. Special attention is focused on the difficulties in theoretical modelling [ (C)u]K-XANES spectra of ancient glasses with different colourings.

R. Pedrazzani, I. Alessandri, E. Bontempi, F. Cappitelli, M. Cianci, E. Pantos, L. Toniolo, et L. E. Depero. Study of sulphation of Candoglia marble by means of micro X-ray diffraction experiments. Appl. Phys. A, 83(4):689-694, June 2006. [ doi ]

This research is aimed at assessing the particular kind of damage caused by the interaction between atmospheric pollution and the marble surface of a magnificent late gothic church, Milan Cathedral, restored in the early 1970s. On the basis of visual inspections and diagnostic investigations the facade appears to be seriously damaged by surface erosion and thick black crusts; biological crusts, micro-fractures and detachments are widely present. This paper reports on SR-mu XRD data collected at the Synchrotron Radiation Source (SRS), Daresbury Laboratory, and at the European Synchrotron Radiation Source (ESRF) from selected samples, covered with black crusts, originating from the Milan Cathedral facade. Mineralogical maps of the deterioration layers have been recorded by two spatial resolutions (5-100 μm), from the bulk of the stone material to the outer layer of the black surface. These maps help in elucidating the mechanism of formation of the black crusts.

J. Roqué, N. R. J. Poolton, J. Molera, A. D. Smith, E. Pantos, et M. Vendrell-Saz. X-ray absorption and luminescence properties of metallic copper nanoparticles embedded in a glass matrix. Physica Status Solidi B, 243(6):1337-1346, May 2006. [ doi ]

A new method of ion-exchange between raw compounds containing copper oxide and alkali glasses has been used to grow copper nanoparticles within a glass matrix, forming a metal-glass nanocomposite that is the structure on which both ancient and modem lustre glazes are based. When excited by X-rays at 300 K, two dominant emission bands appear in the material in the visible region, peaking at 2.60 eV and 1.98 eV. Synchrotron radiation methods are deployed that enables the luminescence and structural properties of the nanocomposite to be interlinked. Standard Extended X-ray Absorption Fine Structure (EXAFS) shows that both metallic copper and copper oxide local sites structure are present in the glass matrix, and the detailed atomic arrangement of each are derived; however, the method provides no information as to whether either structures are actually involved in the luminescence processes. In order to provide this direct link, Optically Detected X-ray Absorption Spectroscopy (OD-XAS) has been deployed, and this provides strong evidence that copper metal natroparticles are responsible for the red emission. The method also shows that the X-ray absorption processes of the metal particles and silicate lattice (that result in the red and blue emissions respectively) are distinctly different. This is the first report of OD-XAS involving metallic nanoparticles, and opens the possibility of using the method more generally for metal nanoparticle research. (c) 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

M. G. Dowsett et A. Adriaens. Cell for simultaneous synchrotron radiation X-ray and electrochemical corrosion measurements on cultural heritage metals and other materials. Anal. Chem., 78(10):3360-3365, May 2006. [ doi ]

We describe the construction of an electrochemical cell of the Bragg type suitable for in situ synchrotron X-ray measurements on rough, heterogeneous metals such as cultural heritage alloys and simulants with corroding or passivated surfaces. The cell features a working electrode, which may be moved under remote control from a position close to an X-ray window to full immersion in the electrolyte. A pocket of electrolyte in contact with the bulk can be maintained on the working electrode surface at all times. Its thickness (typically 100-200 mu m) can be controlled by adjusting the working electrode position and, independently, altering the conformation of the X-ray window with hydrostatic pressure. Alternatively, the electrode may be lowered into the bulk of the electrolyte. Early results from the cell showing a time-resolved study of the reduction of nantokite to cuprite in sodium sesquicarbonate, accompanied by corrosion potential measurements obtained in parallel, are presented here.

T. Broekmans, A. Adriaens, et E. Pantos. Insights into North Mesopotamian 'metallic ware'. Archaeometry, 48(2):219-227, May 2006. [ doi ]

With the aim of shedding new light on the still poorly understood North Mesopotamian metallic ware, ceramic and soil samples from Tell Beydar (northeastern Syria, third millennium bc) were investigated using a range of analytical techniques, including optical microscopy, SR-XRD and SEM-EDX. The objective of this work was to differentiate calcareous metallic ware from non-calcareous ware without the aid of chemical analyses and to find further validation of the existing hypothesis that the former group is an imitation of the latter. A third group of metallic wares from Tell Beydar is believed to be of non-local, still regional origin.

M. Müller, B. Murphy, M. Burghammer, I. Snigireva, C. Riekel, J. Gunneweg, et E. Pantos. Identification of single archaeological textile fibres from the Cave of Letters using synchrotron radiation microbeam diffraction and microfluorescence. Appl. Phys. A, 83(2):183-188, May 2006. [ doi ]

Single 2000-year-old archaeological fibres from textile fragments excavated in the Cave of Letters in the Dead Sea region were investigated by a combined approach using microscopy (optical and SEM), X-ray microbeam diffraction and X-ray microbeam fluorescence. In comparison with modern reference samples, most of the fibres were identified as wool, some as plant bast fibres (flax). The molecular and supermolecular structure of both keratin (wool) and cellulose (flax) were found completely intact. In many fibres, mineral crystals were intimately connected with the fibres. The fluorescence analysis of the dyed wool textiles suggests the possible use of metal-containing mordants for the fixation of organic dyes.

E. Chalmin, C. Vignaud, H. Salomon, F. Farges, J. Susini, et M. Menu. Minerals discovered in paleolithic black pigments by transmission electron microscopy and micro-x-ray absorption near-edge structure. Appl. Phys. A, 83(2):213-218, May 2006. [ doi ]

Analysis of archeological materials aims to rediscover the know-how of prehistoric men by determining the nature of the painting matter, its preparation mode, and the geographic origin of its raw materials. The preparation mode of the painting matter of the paleolithic rock art apparently consisted of mixing, grinding, and also heat-treatment. In this study, we focus on black pigments and more particularly manganese oxides. Using the combined approach of transmission electron microscopy (TEM) and Mn K-edge X-ray absorption near-edge structure (XANES) spectroscopy, we analyzed a variety of archeological black painted samples. The studied pigments arise from the caves of Ekain (Basque country, Spain), Labastide and Gargas (Hautes-Pyrénées, France). In addition, a black 'crayon' (i.e., a 'pen') from the cave of Combe Saunière (Dordogne, France) was also investigated. From the analysis of these painting matters, several unusual minerals have been identified as black pigment, such as manganite, groutite, todorokite and birnessite. These conclusions enable us to estimate the technical level of paleolithic artists: they didn't use heat-treatment to prepare black painting matter. Consequently, the unusual mineralogy found in some of these pigments suggests that some of the manganese ores are coming from geological settings that are sometimes relatively far away from the Dordogne and Basque region such as in Ariège (central-oriental Pyrénées).

A. R. Woll, J. Mass, C. Bisulca, R. Huang, D. H. Bilderback, S. Gruner, et N. Gao. Development of confocal X-ray fluorescence (XRF) microscopy at the Cornell high energy synchrotron source. Appl. Phys. A, 83(2):235-238, May 2006. [ doi ]

A confocal X-ray fluorescence microscope was built at the Cornell High Energy Synchrotron Source (CHESS) to obtain compositional depth profiles of historic paintings. The microscope consists of a single-bounce, borosilicate monocapillary optic to focus the incident beam onto the painting and a commercial borosilicate polycapillary lens to collect the fluorescent X-rays. The resolution of the microscope was measured by scanning a variety of thin metal films through this confocal volume while monitoring the fluorescence signal. The capabilities of the technique were then probed using test paint microstructures with up to four distinct layers, each having a thickness in the range of 10-80 microns. Results from confocal XRF were compared with those from stand-alone XRF and visible light microscopy of the paint cross-sections. A large area, high-resolution scanner is currently being built to perform 3D scans on moderately sized paintings.

K. Krug, J. Dik, M. den Leeuw, A. Whitson, J. Tortora, P. Coan, C. Nemoz, et A. Bravin. Visualization of pigment distributions in paintings using synchrotron K-edge imaging. Appl. Phys. A, 83(2):247-251, May 2006. [ doi ]

X-ray radiography plays an important role in the study of artworks and archaeological artifacts. The internal structure of objects provides information on genesis, authenticity, painting technique, material condition and conservation history. Transmission radiography, however, does not provide information on the exact elemental composition of objects and heavy metal layers can shadow or obscure the ones including lighter elements. This paper presents the first application of synchrotron-based K-edge absorption imaging applied to paintings. Using highly monochromatic radiation, K-edge imaging is used to obtain elemental distribution images over large areas. Such elemental maps visualize the distribution of an individual pigment throughout the paint stratigraphy. This provides color information on hidden paint layers, which is of great relevance to art historians and painting conservators. The main advantage is the quick data acquisition time and the sensitivity to elements throughout the entire paint stratigraphy. The examination of a test painting is shown and further instrumental developments are discussed.

A. Huq, P. W. Stephens, N. Ayed, H. Binous, L. Burgio, R. J. H. Clark, et E. Pantos. Combined technique analysis of the composition of punic make-up materials. Appl. Phys. A, 83(2):253-256, May 2006. [ doi ]

Ten archaeological Punic make-up samples from Tunisia dating from the 4th to the 1st centuries BC were analysed by several techniques including Raman microscopy and synchrotron X-ray diffraction in order to determine their compositions. Eight samples were red and found to contain either quartz and cinnabar or quartz and haematite. The remaining two samples were pink, the main diffracting phase in them being quartz. Examination of these two samples by optical microscopy and by illumination under a UV lamp suggest that the pink dye is madder. These findings reveal the identities of the materials used by Carthaginians for cosmetic and/or ritual make-up purposes.

S. Reguer, P. Dillmann, F. Mirambet, J. Susini, et P. Lagarde. Investigation of Cl corrosion products of iron archaeological artefacts using micro-focused synchrotron X-ray absorption spectroscopy. Appl. Phys. A, 83(2):189-193, May 2006. [ doi ]

Synchrotron-based micro-X-ray absorption spectroscopy is used in the present study to obtain chemical information at the microscopic scale such as coordination and oxidation state of Fe atoms in phases constituting corrosion products within archaeological iron artefacts buried in soil. This technique is required in order to answer questions about the iron corrosion process related to the presence of chloride, particularly for restoration and conservation of metallic artefacts of the cultural heritage. The samples available for X-ray microprobe analyses are cross sections from corroded iron archaeological objects. Previously, complementary techniques have been used such as μXRD and μRaman. This specific study applies micro-X-ray absorption spectroscopy to determine the spatial variation of the predominant Fe oxidation state and to identify the corresponding crystallographic phase. The analyses performed at Fe and Cl K -edges (μXANES) reveal the correlation between the valence distribution in the corrosion products and the evolution of the chloride concentration. In addition to the presence of the well-known iron oxyhydroxide α-FeOOH: akaganeite, we highlight the presence of another important phase, the β-Fe2 (OH)3 Cl hydroxychloride. These important findings help to gain new insights concerning the influence of such phases in the iron corrosion mechanism within their precise characterization.

R. Arletti, M. C. Dalconi, S. Quartieri, M. Triscari, et G. Vezzalini. Roman coloured and opaque glass: a chemical and spectroscopic study. Appl. Phys. A, 83(2):239-245, May 2006. [ doi ]

This work reports the results of an archaeometrical investigation of opaque Roman glass and is mainly focussed on the role of configuration and oxidation state of copper on the colour and opacity of red and green opaque finds (mosaic tesserae, game counters, and glass artefacts) from Sicily and Pompeii excavations. The glass fragments were characterised by EMPA, SEM-EDS, TEM, and XRPD analyses and the copper local environment was investigated using X-ray absorption spectroscopy. The analyses of high-resolution Cu-K edge XANES and EXAFS spectra suggest that, in red samples, copper is present as monovalent cations coordinated to the oxygen atoms of the glass framework, accompanied by metallic clusters. In green samples all the copper cations are incorporated in the glass matrix.

A. Mazurier, V. Volpato, et R. Macchiarelli. Improved noninvasive microstructural analysis of fossil tissues by means of SR-microtomography. Appl. Phys. A, 83(2):229-233, May 2006. [ doi ]

Bone is a dynamic tissue which records and partially stores a relevant amount of biological and biomechanical information. In paleobiological investigation, a satisfactory access to this hidden archive is limited by the unavoidable need to assure integrity of the fossil record. According to our experience, based on a variety of advanced nondestructive approaches in imaging fossil tissues, synchrotron radiation microtomography (SR-?CT) assures the quasi-ideal physical conditions to explore and to finely characterise at a high spatial resolution the inner structural morphology of relatively large-sized and highly mineralised fossil specimens for 2D and 3D modelling and reliable quantitative analyses.

M. O. Figueiredo, T. P. Silva, et J. P. Veiga. A XANES study of the structural role of lead in glazes from decorated tiles, XVI to XVIII century manufacture. Appl. Phys. A, 83(2):209-211, May 2006. [ doi ]

Aged lead-rich, tin-opacified glazes from polychrome tiles manufactured in the 16th-18th century were studied to ascertain the structural role of lead. Glaze fragments with white, blue, yellow, brown and green colouring were analysed using non-destructive X-ray techniques, both laboratorial - X-ray diffraction to identify crystalline components - and synchrotron-based. Elemental analyses by synchrotron radiation X-ray fluorescence were performed at the former LURE photon microprobe (line D15A at DCI, in Orsay). The instrumental set-up of beamline BM29 at the ESRF, in Grenoble, was applied to collect X-ray absorption spectra at the Pb L3-edge. Natural minerals and synthetics with known crystal structure were used as model oxy-compounds to configure different formal valences and coordinations of lead ions by oxygen anions, and to interpret the effects upon details of X-ray absorption near-edge spectroscopy (XANES) spectra. Experimental evidence supports the general conclusion that lead is hosted by the glassy matrix, irrespective of the glaze colour. Furthermore, it was concluded that lead ions assume coordinations higher than usual for silica glasses, acting as network modifiers in the silica-lime-alkali glasses of ancient tile glazes.

I. Reiche, M. Radtke, A. Berger, W. Görner, S. Merchel, H. Riesemeier, et H. Bevers. Spatially resolved synchrotron radiation induced X-ray fluorescence analyses of rare Rembrandt silverpoint drawings. Appl. Phys. A, 83(2):169-173, May 2006. [ doi ]

New analyses of a series of very rare silverpoint drawings that were executed by Rembrandt Harmensz. van Rijn (1606-1669) which are kept today in the Kupferstichkabinett (Museum of Prints and Drawings) of the State Museums of Berlin are reported here. Analysis of these drawings requires particular attention because the study has to be fully non-destructive and extremely sensitive. The metal alloy on the paper does not exceed some hundreds of ?g/cm2. Therefore, synchrotron radiation induced X-ray fluorescence (SR-XRF) is - together with external micro-proton-induced X-ray emission - the only well-suited method for the analyses of metalpoint drawings. In some primary work, about 25 German and Flemish metalpoint drawings were investigated using spatially resolved SR-XRF analysis at the BAMline at BESSY. This study enlarges the existing French-German database of metalpoint drawings dating from the 15th and 16th centuries, as these Rembrandt drawings originate from the 17th century where this graphical technique was even rarer and already obsolete. It also illustrates how SR-XRF analysis can reinforce art historical assumptions on the dating of drawings and their connection.

M. L. Young, F. Casadio, S. Schnepp, J. Almer, D. R. Haeffner, et D. C. Dunand. Synchrotron X-ray diffraction and imaging of ancient Chinese bronzes. Appl. Phys. A, 83(2):163-168, May 2006. [ doi ]

High-energy synchrotron X-ray diffraction and imaging experiments were performed at the Advanced Photon Source on two ancient Chinese bronzes from the Art Institute of Chicago with the goal to nondestructively study their microstructure. The first object, a bronze fragment from an early Western Zhou dynasty vessel (Hu, 11th/10th century B.C.), was investigated with spatially-resolved diffraction to reveal the depth and composition of the surface corrosion layer as well as the composition and grain size of the underlying bronze core. The second object, a bronze dagger-axe (Ge, 3rd/2nd century B.C.) with a silver-inlaid sheath, was studied under both diffraction and imaging conditions. It was found to have been cast as a single object, answering longstanding scholars' questions on whether the ceremonial object concealed an interior blade.

P. Sciau, P. Goudeau, N. Tamura, et É. Dooryhée. Micro scanning X-ray diffraction study of Gallo-Roman Terra Sigillata ceramics. Appl. Phys. A, 83(2):219-224, May 2006. [ doi ]

The red glaze (slip) that characterizes the Terra Sigillata potteries, greatly contributed to their success during the Roman period. This feature can in fact be partially explained by the microstructure (crystalline phases and grain sizes) and the physico-chemistry (compositions) of the ceramics. In this paper, we describe how the technique of synchrotron micro scanning X-raydiffraction could contribute to the understanding of the elaboration process and origins of these ceramics. The small (micron) size of the X-raybeam coupled with the use of a sample scanning stage allows one to spatially resolve the distribution and other characteristics of the constitutive mineral phases.

T. Pradell, J. Molera, C. Bayés, et P. Roura. Luster decoration of ceramics: mechanisms of metallic luster formation. Appl. Phys. A, 83(2):203-208, May 2006. [ doi ]

Luster is a metallic decoration produced since early Islamic times (9th century AD in Iraq). Different studies have shown that medieval lusters are a metal-glass nanocomposite (metal nanoparticles embodied in a silica glassy matrix) obtained from the reaction of a copper and/or silver containing paint with a glaze. The mechanisms of formation of these metallic-like layers are investigated by laboratory reproductions of Medieval luster. Copper and silver lusters are obtained based on different thermal paths and atmospheres, and by using different glaze compositions. The ionic exchange between Cu+ and Ag+ ions from the luster paint with Na+ and K+ of the glaze, is demonstrated in either oxidizing or inert atmospheres and at firing temperatures between 500 ^oC and 600 ^oC. The reduction of copper and silver to their metallic state is obtained by introducing a reducing gas afterwards. The lusters are non-metallic red ruby copper or green with brown spots silver when developed over alkaline glazes, while they appear coppery and golden metallic when developed over mixed alkaline-lead glazes. SR-XRD, optical absorption and microprobe chemical analysis of the lusters indicate that the total amount of copper and silver, and the nature and size of the nanoparticles, are similar in both cases. Further work is needed to clarify the origin of these differences.

P. Tafforeau, R. Boistel, E. Boller, A. Bravin, M. Brunet, Y. Chaimanee, P. Cloetens, M. Feist, J. Hoszowska, J. J. Jaeger, R. F. Kay, V. Lazzari, L. Marivaux, A. Nel, C. Nemoz, X. Thibault, P. Vignaud, et S. Zabler. Applications of X-ray synchrotron microtomography for non-destructive 3D studies of paleontological specimens. Appl. Phys. A, 83(2):195-202, May 2006. [ doi ]

Paleontologists are quite recent newcomers among the users of X-ray synchrotron imaging techniques at the European Synchrotron Radiation Facility (ESRF). Studies of the external morphological characteristics of a fossil organism are not sufficient to extract all the information for a paleontological study. Nowadays observations of internal structures become increasingly important, but these observations should be non-destructive in order to preserve the important specimens. Conventional microtomography allows performing part of these investigations. Nevertheless, the best microtomographic images are obtained using third-generation synchrotrons producing hard X-rays, such as the ESRF. Firstly, monochromatisation avoids beam hardening that is frequently strong for paleontological samples. Secondly, the high beam intensity available at synchrotron radiation sources allows rapid data acquisition at very high spatial resolutions, resulting in precise mapping of the internal structures of the sample. Thirdly, high coherence leads to additional imaging possibilities: phase contrast radiography, phase contrast microtomography and holotomography. These methods greatly improve the image contrast and therefore allow studying fossils that cannot be investigated by conventional microtomography due to a high degree of mineralisation or low absorption contrast. Thanks to these different properties and imaging techniques, a synchrotron radiation source and the ESRF in particular appears as an almost ideal investigation tool for paleontology.

L. Bertrand, D. Vantelon, et E. Pantos. Novel interface for cultural heritage at SOLEIL. Appl. Phys. A, 83(2):225-228, May 2006. [ doi ]

The information that can be retrieved from the study of ancient materials and studies on their conservation strongly rely on the development and application of new techniques of physical analysis. This is particularly important at a time when global changes affecting our environment and way of life impose new stresses putting heritage preservation at risk. For this purpose, synchrotron techniques are particularly suited to the non- (or micro-) destructive characterisation of such heterogeneous materials, and a steep increase in number of publications has been noticed recently from cultural heritage works using synchrotron radiation. In 2004, an interface dedicated to archaeology and cultural heritage was launched at the SOLEIL synchrotron to allow researchers from the international scientific community to be granted specific expertise. This interface aims at easing the access of researchers to the synchrotron, facilitating contacts, providing technical support and informing the community. The very first applications of SOLEIL beamlines in the heritage field are illustrated through works recently carried out at the first beamline of SOLEIL, LUCIA, currently located at the SLS. The setup of the beamline is succinctly described.

T. Pradell, N. Salvado, G. D. Hatton, et M. S. Tite. Physical processes involved in production of the ancient pigment, Egyptian blue. J. Am. Ceram. Soc., 89(4):1426-1431, April 2006. [ doi ]

Egyptian blue, which was the first synthetic pigment to be used in antiquity, consists of crystals of calcium-copper tetrasilicate (i.e. cuprorivaite (CaCuSi4O10)). The physical processes associated with the formation of Egyptian blue were investigated by high-temperature X-ray diffraction measurements on synthetic mixtures of quartz, malachite, and calcium carbonate. The high-brilliance, high-energy radiation ID15B beamline at the European Synchrotron Radiation Facility was necessary to ensure good time/temperature resolution, penetration, and high-quality data. The results established that the Egyptian blue crystals are formed through nucleation and growth within a liquid or glass phase, even for mixtures with an alkali content as low as 0.3 wt% soda. Furthermore, the microstructures observed in a scanning electron microscope indicated the ancient Egyptian blue pigments were produced from mixtures containing several weight percent of alkali.

P. Sciau, S. Relaix, C. Roucau, Y. Kihn, et D. Chabanne. Microstructural and microchemical characterization of Roman period Terra sigillate slips from archaeological sites in Southern France. J. Am. Ceram. Soc., 89(3):1053, March 2006. [ doi ]

Terra Sigillata is a fine ware produced during the Roman period. Its great success was because of its remarkable gloss (or slip), which provides a bright deep red color. Transmission electron microscopy and X-ray powder diffraction techniques were used to characterize the microstructure and microcomposition of Roman period Terra Sigillata slip from two sites in southern France. Investigations on eight samples are presented. The slip coatings have similar structures and compositions, consisting of sub- micrometric hematite (<=[mu]m) and nanometric corundum (few tens nm) crystals in a glass matrix with inclusions of spinel and quartz crystals of varying size depending on the extent of preparation by eleutriation. The firing temperature, determined in previous studies, was in the range of 1020deg-1080^oC. The matrix does not contain iron or other metallic ions. Hematite and corundum crystals are homogeneously dispersed in the matrix and, together, confer the specific red-orange color to the sigillata.

S. Pages-Camagna, I. Reiche, C. Brouder, D. Cabaret, S. Rossano, B. Kanngiesser, et A. Erko. New insights into the colour origin of archaeological Egyptian blue and green by XAFS at the CuK-edge. X-ray Spectrom., 35(2):141-145, March-April 2006. [ doi ]

New results on the local chemical environment of Cu2+ in archaeological Egyptian blue and green and also modem Egyptian green were obtained by x-ray absorption fine structure (XAFS) analysis. The information is essential for the understanding of the colouring mechanisms in both pigments. In a previous study, a clear physico-chemical characterisation of Egyptian blue and green was achieved using a complementary analytical approach with ancient and modern synthesized pigments. Electron microscopy (SEM-EDX and TEM), x-ray diffraction and micro-Raman and UV-visible spectroscopy were used to gain information about the conditions of the ancient Egyptian fabrication processes and permitted the clear distinction of both pigments. However, the exact colouring mechanisms could not be elucidated by these methods. Different Cu-bearing amorphous and crystalline phases were found in both pigments. These phases should be at the origin of the blue and turquoise colours. Using XAFS data at the Cu K-edge, new insights into the origin of the colouring mechanisms of both pigments could be obtained from the precision of the Cu speciation. In Egyptian blue, Cu2+ is mainly allocated in a square-planar site in a crystalline cuprorivaite phase, whereas in Egyptian green, Cu2+ is basically situated in a distorted octahedral site in an amorphous phase. Copyright (c) 2006 John Wiley & Sons, Ltd.

A. C. Hermes, R. J. Davies, S. Greiff, H. Kutzke, S. Lahlil, P. Wyeth, et C. Riekel. Characterizing the decay of ancient Chinese silk fabrics by microbeam synchrotron radiation diffraction. Biomacromolecules, 7(3):777-783, March 2006. [ doi ]

Scanning synchrotron radiation microdiffraction with an approximately 1 X 1 μm(2) beam has been used as a novel method for characterizing the decay of several T'ang dynasty (618-907 AD) silk fabrics. The crystalline fraction could be visualized based on beta-sheet 210 reflection intensities, extracted by recursive peak fits from several thousand diffraction patterns recorded during mesh scans. The azimuthal width of the 210 reflection, which is related to the orientation distribution of the crystalline domains within nanofibrils and the macroscopic orientation of the fibers traversed by the beam, was found to be sensitive to the overall state of decay of the fabric. The fine structure of the histogram of azimuthal width was related to the fiber hierarchical microstructure and the fabric morphology. SAXS/WAXS analysis supports the assumption of an initial loss of the random chain network with decay. At a subsequent state of aging, decay proceeds into the nanofibrils and the silk fibers break up into even smaller fractions.

B. Constantinescu, R. Bugoi, R. Simon, et S. Staub. Some results on microanalysis of gold using micro-xrf at the anka-karlsruhe synchrotron radiation facility. Dans H. Wiedemann, éd., Advanced Radiation Sources and Applications. Proceedings of the NATO Advanced Research Workshop, held in Nor-Hamberd, Yerevan, Armenia, August 29 - September 2, 2004, vol. 199 de NATO Science Series II: Mathematics, Physics and Chemistry, p. 373-380. Springer Netherlands, 2006. [ doi ]

In the present paper, the possibility to use Synchrotron Radiation - based micro X-Ray Fluorescence (XRF) method to study the micro-inclusions of Platinum Group Elements (PGE) and other high temperature melting point metals in gold archaeological objects is demonstrated. The analyzed samples belonged to different pieces of the Pietroasa hoard. The presence of Ta inclusions was determined indicating the Ural Mountains as a source for the gold ore used to manufacture the objects. Conclusions on how to proceed for a complete examination of different groups of elements (Ir, Os, Ta - Nb, Rh, Ru, Pd - Sn, Sb, Te) are also presented.

A. D. Smith, T. Pradell, J. Roqué, J. Molera, M.Vendrell-Saz, A. J. Dent, et E.Pantos. Colour variations in 13th century hispanic lustre - an exafs study,. J. Non-Cryst. Solids, 352:5353-5361, 2006.

W. Gorner, M. Eichelbaum, R. Matschat, K. Rademann, M. Radtke, U. Reinholz, et H. Riesemeier. Non-destructive investigation of composition, chemical properties and structure of materials by synchrotron radiation. Insight, 48(9):540-544, Sep 2006.

A. Manescu, A. Giuliani, F. Fiori, et B. Baretzky. Residual stress analysis in reed pipe brass tongues of historic organs. Mater. Sci. Forum, 524-525:969-974, 2006.

True Baroque organ music can only come back to life in the 21(st) century by developing Cu-based alloys and implementing them in the organ reed pipes. Reed pipes contain a vibrating part, the brass tongue that crucially influences its sound. Energy dispersive synchrotron X-ray diffraction has been performed in order to investigate residual stresses in the tongues. The in depth analysis gives us an important indication on the processes the tongues were submitted to during their manufacturing: hammering, annealing, filing to the neat thickness, curving of the tongues. A biaxial stress state in the organ tongues was considered. The residual stress values and behaviour were correlated to the manufacturing processes.

R. Macchiarelli, L. Bondioli, A. Debénath, A. Mazurier, J.-F. Tournepiche, W. Birch, et M. C. Dean. How neanderthal molar teeth grew. Nature, in press, 2006. [ doi ]

Growth and development are both fundamental components of demographic structure and life history strategy. Together with information about developmental timing they ultimately contribute to a better understanding of Neanderthal extinction. Primate molar tooth development tracks the pace of life history evolution most closely[1,2], and tooth histology reveals a record of birth as well as the timing of crown and root growth. High-resolution micro-computed tomography now allows us to image complex structures and uncover subtle differences in adult tooth morphology that are determined early in embryonic development^3. Here we show that the timing of molar crown and root completion in Neanderthals matches those known for modern humans but that a more complex enamel-dentine junction morphology and a late peak in root extension rate sets them apart. Previous predictions about Neanderthal growth, based only on anterior tooth surfaces[4,5], were necessarily speculative. These data are the first on internal molar microstructure; they firmly place key Neanderthal life history variables within those known for modern humans.

P. J. Potts, A. T. Ellis, P. Kregsamer, C. Streli, C. Vanhoof, M. West, et P. Wobrauschek. Atomic spectrometry update - X-ray fluorescence spectrometry. J. Anal. At. Spectrom., 21(10):1076-1107, 2006. [ doi ]

This annual review of X-ray fluorescence covers developments over the period 2005-2006 in instrumentation and detectors, matrix correction and spectrum analysis procedures, X-ray optics and microfluorescence, synchrotron XRF, TXRF, portable XRF and on-line applications, as assessed from the published literature. The review also covers a survey of applications, including sample preparation, geological, environmental, archaeological, forensic, biological, clinical, thin films, chemical state and speciation studies. The trend set in previous years continues with large numbers of papers published in the areas of environmental, industrial and biological/clinical applications, followed this year by a significant contribution in the area of archaeological science and cultural heritage. Notable contributions this year are in areas of topical societal interest, including the rapid throughput screening for combatorial materials. Interest continues in nanotechnological applications as well as the related micro-analytical instrumentation that permits pro. ling and mapping of samples, which was previously undertaken by non-XRF techniques.

C. Streli. Recent advances in TXRF. Appl. Spectrosc. Rev., 41(5):473-489, 2006. [ doi ]

Total reflection X-ray fluorescence analysis (TXRF) is a special method of energy-dispersive X-ray fluorescence analysis extending EDXRF to the ultra trace element level. The achievable detection limits depend on the excitation source and are in the range of picograms to femtograms. Only small amounts of sample are required and the quantification by adding one element as an internal standard is easy as thin film approximation is valid. In this article, the recent advances in TXRF are reviewed with over 80 references. The principles, advantages, instrumentation, improvements with X-ray optics, synchrotron radiation as excitation sources as well as various fields of application, wafer surface analysis, depth profiling, absorption spectroscopy, medical samples, biological samples, environmental monitoring, archeological and polymer samples are described. Related techniques are also mentioned and discussed.

Z. Šmit, K. Janssens, et M. Kos. Non-destructive analysis and testing of museum objects, chap. Production of glass in the Venetian manner. Dans Denker et al. [ .ref ], 2006.

S. Gerlach, H. Römich, E. Lopéz, F. Zanini, L. Mancini, et L. Rigon. Non-destructive analysis and testing of museum objects, chap. Phase contrast microtomography for archaeological glasses, p. 147-151. Dans Denker et al. [ .ref ], 2006.

I. Reiche, A. Berger, A. Duval, W. Görner, H. Guicharnaud, S. Merchel, M. Radtke, J. Riederer, H. Riesemeier, et M. Roth. Non-destructive analysis and testing of museum objects, chap. Synchrotron radiation and protons on the trace of famous artists: Non-destructive analyses of silverpoint drawings by Albrecht Dürer, p. 91-101. Dans Denker et al. [ .ref ], 2006.

A. Adriaens et M. G. Dowsett. Non-destructive analysis and testing of museum objects, chap. Observing corrosion, passivation and cleaning as they happen - in-situ spectroelectrochemistry for the conservation of metals, p. 31-46. Dans Denker et al. [ .ref ], 2006.

E. Pantos, W. Kockelmann, L. C. Chapon, L. Lutteroti, S. L. Bennet, M. J. Tobin, J. F. W. Mosselmans, T. Pradell, N. Salvadó, S. Butí, R. Garner, et A. J. N. W. Prag. Non-destructive analysis and testing of museum objects, chap. Synchrotron radiation and neutron study of a 7th-century BC Corinthian-type bronze helmet at the Manchester Museum, p. 25-30. Dans Denker et al. [ .ref ], 2006.

E. Pantos, N. Salvadó, S. Butí, M. J. Tobin, et T. Pradell. Characterization of ancient painting pigments using synchrotron radiation. Dans Proc. COST G8 Workshop on Qumran, Jerusalem May 2005, vol. in press, 2006.

J. Roqué, J. Molera, P. Sciau, E. Pantos, et M. Vendrell-Saz. Copper and silver nanocrystals in lustre lead glazes: development and optical properties. J. Eur. Ceramic Society, 26(16):3813-3824, 2006. [ doi ]

In the early 9th century AD ancient potters of Iraq discovered that after firing some copper oxides and silver salts with clay, iron oxides and some sulphur compounds applied on a ceramic glaze produced a beautiful layer with a wide range of colours, from reddish to yellowish or even greenish, and some with a characteristic metallic copper or purplish shine. Modern studies of these layers showed that they are formed by nanocrystals of copper and silver embedded in a glass matrix. Some attempts have been performed to understand ancient lustre coloration and characteristic gloss but have failed to give a clear correlation between chemical composition and colour, and generally make some assumptions on the shape and the size of the nanoparticles and the lustre nanostructure. The aim of this paper is to establish a basis for understanding lustre nanostructure linked to its optical properties from a sequence of lustre reproductions on traditional lead glazed tiles. These modern lustre decorations have been studied by means of optical microscopy, transmission electron microscopy and electron energy loss spectroscopy, UV-vis spectroscopy, low irradiation angle X-ray diffraction, synchrotron radiation X-ray diffraction and electron microprobe analysis. These results show that changes in the lustre nanostructure affect the glaze colour and shine during the lustre formation process. Lustre nanostructure showed crystal size range as a function of depth, that subsequently disappeared followed by an increase of nanoparticles mean diameter and reduction of the interparticle distances. Consequently, the dipole plasmon coupling between copper nanoparticles appeared, and seems to be responsible for the metallic shine and copper metal like coloration of the copper lustre. However, colour from the glaze surface differs when calculated for diffuse or reflected light. Diffuse coloration appears strongly affected by the copper nanocrystals, while specular coloration is not only affected by copper but also by the presence of an inhomogeneous distribution of silver nanocrystals which gives the lustre a characteristic purplish shine.

L. Bertrand. Non-destructive analysis and testing of museum objects, chap. SOLEIL and COST organised the first training school on the synchrotron analysis of ancient materials, p. 212-215. Dans Denker et al. [ .ref ], 2006.

Y. Fors et M. Sandström. Sulfur and iron in shipwrecks cause conservation concerns. Chem. Soc. Rev., 35:399-415, 2006. [ doi ]

Synchrotron-based sulfur X-ray absorption spectroscopy reveals considerable accumulation of organosulfur (e.g. thiols), pyrite and iron(II) sulfides in marine-archaeological wood preserved in seawater, e.g. for historical shipwrecks such as the Vasa and Mary Rose. In the museum, oxidation of the sulfur compounds in the presence of iron ions may cause severe acidity in the moist wood. This tutorial review discusses developments of conservation methods to remove acid and iron, and how to analyse and stabilise sulfur compounds in the wood.

C. J. Kennedy et T. J. Wess. The use of X-ray scattering to analyse parchment structure and degradation, chap. 4. Vol. 1 de Bradley et Creagh [ .ref ], 2006.

J. C. Hiller et T. J. Wess. Investigation of Diagenetic and Postmortem Bone Mineral Change by Small-Angle X-Ray Scattering, chap. 3. Vol. 1 de Bradley et Creagh [ .ref ], 2006.

D. Bradley et D. Creagh, éds. Physical Techniques in the Study of Art, Archaeology and Cultural Heritage, vol. 1. Elsevier, 2006.

This volume is the first of a series on 'Physical Techniques in the Study of Art, Archaeology and Cultural Heritage'. It follows a successful earlier publication by Elsevier (Radiation in Art and Archaeometry). There has been an upsurge of interest world wide in cultural heritage issues, and in particular, large organizations such as UNESCO and the European Union are active in providing funding for a very diverse range of projects in cultural heritage preservation. It is perceived that it is essential to preserve the cultural heritage of societies, both to benefit the future generations of those societies, and to inform other cultures. A growing need exists for the education of conservators and restorers because it is these professionals who will make decisions on how best to preserve our cultural heritage. This book series therefore has as its primary aim, the dissemination of technical information on scientific conservation to scientific conservators, museum curators, conservation science students, and other interested people. Scientific conservation, as a discipline, is a comparatively modern concept. Interested scientists have for many years addressed scientific problems associated with cultural heritage artefacts. But their involvement has been sporadic and driven by the needs of individual museums, rather than a personal lifetime study of issues of conservation of for example, buildings, large functional objects, paintings, and so on. In this book series contributors will come from both 'interested scientists' and the 'museum-based scientists'. The authors have been selected with an eye to involving young, and well as established, scientists. Dr Jean Louis Boutaine, was Head of the Research Department of the Centre de Recherche et de Restauration des Musees de France at the Louvre. Dr Boutaine has had a most distinguished career within the conservation science community. He writes here on the concept of the 'Modern Museum'. Professor Casali is responsible for the teaching of 'Archaeometry' at the University of Bologna. He has developed advanced equipment for both micro-Computer Tomography and for large-object Computer Tomography. His chapter deals with X-ray, neutron, and digital radiography as applied to the study of objects of cultural heritage significance. Professor Tim Wess holds the Chair of Biomaterials in the Biophysics Division in the School of Optometry and Vision Science at Cardiff University. The systems in which he is interested contain collagen, fibrillin, and cellulose (which relate, in the cultural heritage discipline, to an interest in parchment and papers). A parallel interest is in the structure of bone and artificial composite materials (which relates to his interest in historical studies of bone materials). Chapter 3 will describe the techniques used to study alteration to structure of minerals in the bone. Preservation of intact bone mineral crystallites has been shown to relate to the endurance of amplifiable ancient DNA from archaeological and fossil bone. In collaboration with Drs K. Nielsen and Rene Larsen (School of Conservation, Copenhagen, Denmark) Tim Wess has analyzed the deterioration of historic parchments and also simulated ageing processes. Chapter 5 has been written by Dr Andrew Hardy who began studying Middle Eastern eye cosmetics ('kohls') in the early 1990's whilst working in Oman. He has continued this work at the Centre for Medical History, School of Historical, Political and Sociological Studies, Exeter University. The chapter summarizes and reviews the usage and composition of kohls in ancient (Pharaonic) Egypt. It also gives information, from later time periods, on kohl usage and its 'recipes', which have been studied using a wide range of experimental techniques.

A. Denker, A. Adriaens, M. Dowsett, et A. Giumlia-Mair, éds. Non-destructive analysis and testing of museum objects. Fraunhofer IRB Verlag, 2006.

D. C. Creagh. The characterization of artefacts of cultural heritage significance using physical techniques. Rad. Phys. Chem., 74(6):426-442, December 2005. [ doi ]

All societies attempt to preserve their cultural heritage because it is this that gives them their identity. How artefacts are identified as being of significance to society, and how to preserve these for posterity, depend on the sophistication of those societies, their wealth, and the determination of members of the societies to preserve their past. If conservation or restoration measures are being undertaken complex analytical experiments must be undertaken beforehand to ensure that the work is being undertaken in an appropriate manner. These investigations may employ electromagnetic (IR, VIS, UV, X-ray, gamma-ray) or particulate (electron, proton, neutron, and ion beams) radiation. The use of many of these techniques is described in this paper in experiments on Australian Aboriginal bark paintings, a suit of armour belonging to a famous Australian outlaw, and the degradation of colour motion picture film. (C) 2005 Elsevier Ltd. All rights reserved.

C. Ghioni, J. C. Hiller, C. J. Kennedy, A. E. Aliev, M. Odlyha, M. Boulton, et T. J. Wess. Evidence of a distinct lipid fraction in historical parchments: a potential role in degradation? J. Lipid Res., 46(12):2726-2734, December 2005. [ doi ]

Parchment, a biologically based material obtained from the processed hides of animals such as cattle and sheep, has been used for millennia as a writing medium. Although numerous studies have concentrated on the structure and degradation of collagen within parchment, little attention has been paid to noncollagenous components, such as lipids. In this study, we present the results of biochemical and structural analyses of historical and newly manufactured parchment to examine the potential role that lipid plays in parchment stability. The lipid fraction extracted from the parchments displayed different fatty acid compositions between historical and reference materials. Gas chromatography, small-angle X-ray scattering, and solid-state NMR were used to identify and investigate the lipid fraction from parchment samples and to study its contribution to collagen structure and degradation.

We hypothesize that the origin of this lipid fraction is either intrinsic, attributable to incomplete fat removal in the manufacturing process, or extrinsic, attributable to microbiological attack on the proteinaceous component of parchments. Furthermore, we consider that the possible formation of protein-lipid complexes in parchment over the course of oxidative degradation may be mediated by reactive oxygen species formed by lipid peroxidation.

K. Leyssens, A. Adriaens, M. G. Dowsett, B. Schotte, I. Oloff, E. Pantos, A. M. T. Bell, et S. P. Thompson. Simultaneous in situ time resolved SR-XRD and corrosion potential analyses to monitor the corrosion on copper. Electrochem. Comm., 7(12):1265-1270, December 2005. [ doi ]

The focus of this study consists of examining how simultaneous SR-XRD and electrochemical measurements can provide information on the effectiveness of stabilization and storage treatments of copper artefacts in aqueous solution. The electrochemical cell used here was designed for in situ, time resolved SR-XRD studies of corrosion and inhibition studies on cultural heritage materials. Key objectives of the new cell were to monitor corrosion layers on alloys with realistic metallographic structures and to obtain co-incident, time resolved, electrochemical data such as reduction measurements, oxidation measurements and corrosion potential (Ecorr) measurements. Here we present some early results from the cell. Firstly, a correlated SR-XRD and corrosion potential (Ecorr) study of the reduction of nantokite during storage in sodium sesquicarbonate, which shows that the surface chemistry continues to change after Ecorr has stabilized. Secondly, the use of X-ray data to identify specific changes occurring as a function of potential in the forced reduction of a more complex system.

M. Cotte, P. Dumas, G. Richard, R. Bréniaux, et P. Walter. New insight on ancient cosmetic preparation by synchrotron-based infrared microscopy. Anal. Chim. Acta, 553(1-2):105-110, November 2005. [ doi ]

Synchrotron IR micro-spectroscopy is appropriately suited to the analysis of small particles of archaeological cosmetics. The sample originates from a 33 centuries old Egyptian cosmetic remain. Thanks to the high spectral quality and high lateral resolution achieved by this synchrotron-based microspectroscopic tool, new insights into the composition and spatial location of both organic and mineral components of the sample were obtained. Five different particles were analyzed and delivered similar findings: the core is fat rich, and surrounded with a mineral phase. In two particles, lead palmitate was clearly identified as a major component. Phosgenite (Pb2CO3Cl2), a lead salt synthesized in aqueous solution, was also located in region near the surface of the particles. (c) 2005 Elsevier B.V. All rights reserved.

S. Quartieri, M. P. Riccardi, B. Messiga, et F. Boscherini. The ancient glass production of the Medieval Val Gargassa glasshouse: Fe and Mn XANES study. J. Non-Cryst. Solids, 351(37-39):3013-3022, October 2005. [ doi ]

Glass finds from the Medieval Val Gargassa glasshouse (Genova, Italy) were investigated by chemical and spectroscopic techniques (colorimetric analysis and X-ray absorption spectroscopy) with the aim to obtain information on the ancient glass production technique. Sampling covers all the typologies of archaeological findings unearthed by the digging, as well as fragments of finished glass-wares. The results indicated that the samples are soda-lime based glasses. The color variability was exerted by the glassmakers by both controlling the kiln atmosphere and/or adding MnO2 as decoloring agent. In both cases, the Fe2+/Fe3+ ratio was modified at a specific step of the production cycle. (c) 2005 Elsevier B.V. All rights reserved.

S. Reguer, P. Dillmann, F. Mirambet, et L. Bellot-Gurlet. Local and structural characterisation of chlorinated phases formed on ferrous archaeological artefacts by μXRD and μXANES. Nucl. Instrum. Methods B, 240(1-2):500-504, October 2005. [ doi ]

The deterioration after excavation of archaeological artefacts buried in soil is often associated with the presence of chlorine ions which play an important role in iron corrosion mechanisms. The understanding of these processes, related to the presence of chlorine, has to be made towards a precise study of the morphological and physicochemical properties of the iron corrosion products. A characterisation study on ferrous artefacts coming from four archaeological sites has been carried out; the rust layers have been studied using several techniques. The composition analyses were performed by energy dispersive spectroscopy coupled to scanning electron microscope. Structural information has been obtained by micro X-ray diffraction, micro Raman spectrometry and micro X-ray absorption experiments. The results obtained illustrate the necessity of the combination of these different techniques for the detailed study about corrosion typology.

M. F. Guerra, T. Calligaro, M. Radtke, I. Reiche, et H. Riesemeier. Fingerprinting ancient gold by measuring Pt with spatially resolved high energy Sy-XRF. Nucl. Instrum. Methods B, 240:505-511, October 2005. [ doi ]

Trace elements of ancient gold such as Pt, give fundamental information on the circulation of the metal in the past. In the case of objects from the cultural heritage, the determination of trace elements requires non-destructive point analysis in general. These conditions and the need of good detection limits restrain the number of applicable analytical techniques. After the development of a PIXE set-up with a selective Cu or Zn filter of 75 μm and of a PIXE-XRF set-up using a primary target of As, we tested the possibilities of spatially resolved Sy-XRF to determine Pt in gold alloys. With a Zn filter, PIXE showed a detection limit of 1000 ppm in gold while PIXE-XRF lowers this detection limit down to 80 ppm. This last value being constrained by the resonant Raman effect produced on gold. In order to improve the detection limit of Pt keeping the non-destructiveness and access to point analysis, we developed an analytical protocol for XRF with synchrotron radiation at BESSY II, using the BAMline set-up. The L-lines of Pt were excited by a beam of energy above and below 11.564 keV and measured using a Si(Li) detector with a 50 μm Cu filter. A p-beam of 100-250 μm2 was used according to the size of the sample. The determination of the Pt content in the samples was carried out by Monte-Carlo simulation and subtraction of An and Pt spectra obtained on pure standards. The limit of detection for Pt of 20 ppm was determined by using certified standards. The detection limits of a small set of other characteristic elements of gold were also measured using an incident energy of 33 keV. (c) 2005 Elsevier B.V. All rights reserved.

M. Sandström, F. Jalilehvand, E. Damian, Y. Fors, U. Gelius, M. Jones, et M. Salomé. Sulfur accumulation in the timbers of King Henry VIII's warship Mary Rose: A pathway in the sulfur cycle of conservation concern. PNAS, 102(40):14165-14170, October 2005. [ doi ]

In marine-archaeological oak timbers of the Mary Rose large amounts of reduced sulfur compounds abound in lignin-rich parts such as the middle lamella between the cell walls, mostly as thiols and disulfides, whereas iron sulfides and elemental sulfur occur in separate particles. Synchrotron-based x-ray microspectroscopy was used to reveal this environmentally significant accumulation of organosulfur compounds in waterlogged wood. The total concentration of sulfur in reduced forms is approx1 mass % throughout the timbers, whereas iron fluctuates up to several mass %. Conservation methods are being developed aiming to control acid-forming oxidation processes by removing the reactive iron sulfides and stabilizing the organosulfur compounds.

C. J. Kennedy, J. Hiller, C. A. Maxwell, et T. J. Wess. X-ray diffraction analysis of parchment: applications to manufacture, conservation and restoration. Dans Verger [ .ref ], p. 180-185.

É. Dooryhée, M. Anne, I. Bardiès, J.-L. Hodeau, P. Martinetto, S. Rondot, J. Salomon, G. B. M. Vaughan, et P. Walter. Non-destructive synchrotron X-ray diffraction mapping of a Roman painting. Appl. Phys. A, 81(4):663 -667, September 2005. [ doi ]

The history and the properties of materials are deduced not only from their elemental and molecular signatures, but also from their exact phase compositions, and from the structures and the defects of their constituents. Here we implement a non-destructive synchrotron X-ray based method, which combines both the quantitative structural content of diffraction and the imaging mode. As a demonstration case, the pigments of a Roman wall painting are examined. The joined elemental and mineral maps mimic the major features of the painting. Different structural phases made of common atomic elements are differentiated. Textures and graininess are measured and related to the artist's know-how.

I. Verger, éd. 14th Triennial Meeting, The Hague, 12-16 September 2005: Preprints, London, September 2005. ICOM Committee for Conservation, James & James/Earthscan.

F. Farges, S. Djanarthany, S. de Wispelaere, M. Munoz, B. Magassouba, A. Haddi, M. Wilke, C. Schmidt, M. Borchert, P. Trocellier, W. Crichton, A. Simionovici, P. E. Petit, M. Mezouar, M. P. Etcheverry, I. Pallot-Frossard, J. R. Bargar, G. E. Brown, D. Grolimund, et A. Scheidegger. Water in silicate glasses and melts of environmental interest: from volcanoes to cathedrals. Phys. Chem. Glasses, 46(4):350-353, August 2005. [ doi ]

In silicate glasses and melts, water acts according to two main processes. First, it can be dissolved in high temperature/high pressure melts. Second, it constitutes a weathering agent on the glass surface. A number of in-situ x-ray absorption fine structure (XAFS) studies for Fe, Ni, Zr, Th and U show that the more charged cations (Zr, Nb, Mo, Ta, Sn, Th and U) are little affected by the presence of dissolved water in the melt. In contrast, divalent iron and nickel are highly sensitive to the presence of water, which enhance nucleation processes, for example, of phyllosilicates at the angstrom-scale. Such information provides additional constraints on the role of water deep in the Earth, particularly in magmatology. By contrast, the weathering of glass surfaces by water can be studied from a durability perspective. Experimental weathering experiments Of nuclear waste glasses performed in the laboratory show a variety of surface enrichments (carbon, chlorine, alkalis, iron) after exposure to atmospheric fluids and moisture. Mn-, and Fe-surface enrichments of analogous glasses of the XIVth century are related to the formation of Mn and Fe oxy/hydroxides on the surface. The impact on the glass darkening is considered in terms of urban pollution and mass tourism.

M. O. Figueiredo, J. P. Veiga, T. P. Silva, J. P. Mirao, et S. Pascarelli. Chemistry versus phase constitution of yellow ancient tile glazes: A non-destructive insight through XAS. Nucl. Instrum. Meth. B., 238(1-4):134-137, August 2005. [ doi ]

Using synchrotron radiation-based analytical (SRXRF) and spectroscopic (XAS) non-destructive techniques, a study was carried out on lead-rich, tin-opacified yellow glazes (silica-lime-alkali type glasses) decorating ancient tiles (17-19th century). These glasses have a rather complex chemistry, being currently assumed that the yellow pigment used for centuries - a pyrochlore-type double oxide of lead and antimony - prevails within the glaze, despite Sb(3+) being recognized as a network-forming cation in glasses. Minerals and synthetics with known crystal structure were used as model compounds to interpret X-ray absorption spectroscopy data at Sb K-edge and Pb L-3-edge collected from ancient glazes. Theoretical modelling of Sb 1s XANES spectra was applied to demonstrate that antimony alone may be responsible for the yellow colour through a finely dispersed pyrochlore-type Sb-oxide, while lead remains hosted in the glassy matrix. (c) 2005 Elsevier B.V. All rights reserved.

M. Sánchez del Río, A. Sodo, S. G. Eeckhout, T. Neisius, P. Martinetto, E. Dooryhée, et C. Reyes-Valerio. Fe K-edge XANES of Maya blue pigment. Nucl. Instrum. Methods B, 238(1-4):50-54, August 2005. [ doi ]

The utilization of techniques used in Materials Science for the characterization of artefacts of interest for cultural heritage is getting more and more attention nowadays. One of the products of the ancient Maya chemistry is the “Maya blue” pigment, made with natural indigo and palygorskite. This pigment is different from any other pigment used in other parts of the world. It is durable and acid-resistant, and still keeps many secrets to scientists even though it has been studied for more than 50 years.

Although the pigment is basically made of palygorskite Si8(Mg2Al2)O20(OH)2(OH2)4.4H2O and an organic colourant (indigo: C16H10N2O2), a number of other compounds have been found in previous studies on archaeological samples, like other clays and minerals, iron nanoparticles, iron oxides, impurities of transition metals (Cr, Mn, Ti, V), etc. We measured at the ESRF ID26 beamline the Fe K-edge XANES spectra of the blue pigment in ancient samples. They are compared to XANES spectra of Maya blue samples synthesized under controlled conditions, and iron oxides usually employed as pigments (hematite and goethite). Our results show that the iron found in ancient Maya blue pigment is related to the Fe exchanged in the palygorskite clay. We did not find iron in metallic form or goethite in archaeological Maya blue.

D. Fan, S. Feng, et Q. Xu. X-rays for Archaeology, chap. Study of Chemical Composition in Ancient Celadon of Yue Kiln, p. 223-230. Dans Uda et al. [ .ref ], July 2005.

Y. Lei, S. L. Feng, J. Jiang, Z. X. Zhuo, S. L. Zhang, et Y. M. Liao. X-rays for Archaeology, chap. Study on the compositional differences among different kilns' Tang Sancai by SRXRF, p. 217-222. Dans Uda et al. [ .ref ], July 2005.

E. Pantos. X-rays for Archaeology, chap. Synchrotron Radiation in Archaeological and Cultural Heritage Science, p. 199-208. Dans Uda et al. [ .ref ], July 2005.

Y. Y. Huang, P. L. Leung, et W. He. X-rays for Archaeology, chap. Study of the elemental distribution in ancient Chinese porcelain using synchrotron radiation X-ray fluorescence, p. 209-216. Dans Uda et al. [ .ref ], July 2005.

I. Nakai. X-rays for Archaeology, chap. Synchrotron radiation X-ray fluorescence analysis of archaeological ceramics and glass, p. 183-198. Dans Uda et al. [ .ref ], July 2005.

M. Uda, G. Demortier, et I. Nakai, éds. X-rays for Archaeology. Springer, July 2005. [ doi ]

The application of X-rays to objects of archaeology and the attempt to gain insight into both construction and chemical composition in a non-destructive manner date back to the days of the discovery of radiation. Nowadays, X-ray techniques, such as X-ray fluorescence and diffraction are standard tools.

The book contains scientific data, i.e. in situ measurement data taken with portable XRF and XRD, and fine data taken with accelerating ion beams and synchrotron radiations, and with their explanation. Results obtained by traditional scientific methods are also reviewed. The book contains experimental data taken both from monuments in the field and exhibits in museums, i.e. ancient Egyptian wall painting pigments, ancient Egyptian wooden statues, ancient Egyptian mummies, ancient Greek funerary monuments, Cypriot ceramics, Medieval, Lyubliana and Venetian glass, Romanian ceramics, ancient Near East clay, old Japanese porcelain, pre-Hispanic items from ancient America, ancient Chinese underglaze-red, blue and white porcelain, Chinese celadon, Phoenician cosmetics, glazes, ancient gold and silver coins, gold jewelleries, gold alloys, corroded metals, gemstones (ruby, emerald and garnet), painting pigments, pottery, bronze, obsidian, stucco, turquoise, and so on. This discussion between natural scientists and archaeologists predicts the future direction of archaeology.

M. Cotte, P. Walter, G. Tsoucaris, et P. Dumas. Studying skin of an Egyptian mummy by infrared microscopy. Vibrational Spectrosc., 38(1-2):159-167, July 2005. [ doi ]

The state of conservation/degradation of mummy human remains, can be inferred from their biochemical composition, as well as the secondary structures of proteins. Infrared microscopy is a very appropriate technique for addressing such issues. In this study, skin leg of an Egyptian mummy, was collected and prepared by microtomy, and was analysed using an infrared imager (Spectrum Spotlight) and using synchrotron infrared microscopy. Complementary analyses at both large scale and size close to the diffraction limit help tremendously for understanding the state of degradation. The external layer of mummy skin appears to be more preserved as evidenced by the presence of characteristic biological vibrational features (in particular amide bands) in spectra collected within this region. Adipocere and calcium oxalate are the main degradation products identified in the mummy skin. The origin of the degradation process is not yet fully understood.

W. J. Chitty, P. Dillmann, V. L'Hostis, et C. Lombard. Long-term corrosion resistance of metallic reinforcements in concrete - a study of corrosion mechanisms based on archaeological artefacts. Corrosion Sci., 47(6):1555-1581, June 2005. [ doi ]

This paper presents an analytical study on ferrous reinforcements embedded in binders found in ancient buildings aged from the Gallo-Roman period to the beginning of the 20th c. AD. The study of this kind of archaeological analogues is necessary to improve knowledge on the long-term corrosion behaviour of low carbon steels that could be used in concrete to build the substructure of nuclear wastes storage or reversible disposal facilities. The corrosion system can be described as a multi-layer pattern made of metal, a dense corrosion product layer, a transformed medium and a binder. The morphological, and physico-chemical properties like composition, structure and porosities of each part were studied with different analytical methods like optical and electronical microscopies, Energy Dispersive Spectrometry coupled with Scanning Electron Microscopy, Electron Probe MicroAnalysis, Mercury porosimetry, micro-Raman spectroscopy and micro- Diffraction under Synchrotron Radiation. Moreover, average corrosion rates were evaluated. These rates are relatively low compared to the same parameters measured on low alloyed contemporary steels and are comparable with corrosion rates noted for passivated systems. (c) 2004 Elsevier Ltd. All rights reserved.

N. Salvadó, S. Butí, M. J. Tobin, E. Pantos, J. N. W. Prag, et T. Pradell. Advantages of the use of SR-FT-IR microspectroscopy: applications to cultural heritage. Anal. Chem., 77(11):3444-3451, June 2005. [ doi ]

Synchrotron radiation Fourier transform infrared (SR-FT-IR) microspectroscopy represents an advance over conventional FT-IR spectroscopy because it gives a higher signal/noise ratio at the highest spatial resolution due to the high brightness and collimation of synchrotron radiation. It has been successfully applied to the study of ancient paintings, alteration and corrosion layers which are heterogeneous microlayered materials made by complex mixtures of organic and inorganic compounds. Moreover, the high brightness attribute allows FT-IR spectra to be routinely obtained directly on the surfaces of the objects and opens the possibility for nondestructive testing of museum objects. We present in this paper a selection of applications of SR-FT-IR to the analysis of ancient paintings, alteration and corrosion layers where the technique has proven to be especially useful: first, the separation and identification of pigment microparticles from ancient Roman wall paintings; second, the determination of the binding media and the byproducts resulting from the interaction between binders and pigments from medieval altarpieces; and third, the study of the surface corrosion layers of a bronze helmet by means of direct analysis of the surface.

T. Pradell, J. Molera, J. Roque, M. Vendrell-Saz, A. D. Smith, E. Pantos, et D. Crespo. Ionic-exchange mechanism in the formation of medieval luster decorations. J. Am. Ceram. Soc., 88(5):1281-1289, May 2005. [ doi ]

Analysis of medieval luster ceramics seems to indicate that the formation of luster layers could involve an ion exchange between some alkali ions of the glaze (Na+ and K+), and copper and silver cations of the luster raw paint during firing. However, because of the weathering shown by the medieval luster decorations analyzed, conclusive proof is difficult to obtain. A realistic reproduction of the luster decorations has been fabricated in order to follow the process of formation of the luster layer. This has been studied by optical microscopy, transmission electron microscopy, electron probe microanalysis, extended X-ray absorption fine structure, X-ray absorption near-edge structure, and the results give direct evidence that ion exchange and diffusion are the physicalchemical mechanisms responsible for the introduction of copper and silver into the glaze.

M. Brunet, F. Guy, D. Pilbeam, D. E. Lieberman, A. Likius, H. T. Mackaye, M. S. Ponce de León, C. P. Zollikofer, et P. Vignaud. New material of the earliest hominid from the Upper Miocene of Chad. Nature, 434(7034):752-755, April 2005. [ doi ]

Discoveries in Chad by the Mission Paleoanthropologique Franco-Tchadienne have substantially changed our understanding of early human evolution in Africa. In particular, the TM 266 locality in the Toros-Menalla fossiliferous area yielded a nearly complete cranium (TM 266-01-60-1), a mandible, and several isolated teeth assigned to Sahelanthropus tchadensis and biochronologically dated to the late Miocene epoch (about 7 million years ago). Despite the relative completeness of the TM 266 cranium, there has been some controversy about its morphology and its status in the hominid clade. Here we describe new dental and mandibular specimens from three Toros-Menalla (Chad) fossiliferous localities (TM 247, TM 266 and TM 292) of the same age. This new material, including a lower canine consistent with a non-honing C/P3 complex, post-canine teeth with primitive root morphology and intermediate radial enamel thickness, is attributed to S. tchadensis. It expands the hypodigm of the species and provides additional anatomical characters that confirm the morphological differences between S. tchadensis and African apes. S. tchadensis presents several key derived features consistent with its position in the hominid clade close to the last common ancestor of chimpanzees and humans.

A. Somogyi, R. Tucoulou, G. Martinez-Criado, A. Homs, J. Cauzid, P. Bleuet, S. Bohic, et A. Simionovici. ID22: a multitechnique hard X-ray microprobe beamline at the European Synchrotron Radiation Facility. J. Synchrotron Radiat., 12(2):208-215, March 2005. [ doi ]

The ID22 beamline is dedicated to hard X-ray microanalysis allowing the combination of fluorescence, spectroscopy, diffraction and tomography techniques in a wide energy range from 6 to 70 keV The recent installation of an in-vacuum undulator, a new sample stage and the adaptation of various focusing optics has contributed to a great improvement in the capabilities of the beamline, which is now accessed by a wide user community issued from medical, earth and environmental science, archaeology and material science. Many applications requiring low detection limits for localization/speciation of trace elements together with structural analysis have been developed at the beamline on the (sub)micrometer scale. The possibility of combining simultaneously different analytical probes offers the opportunity of a thorough study of a given sample or scientific problem. This paper presents a review of the recent developments of the beamline and a detailed description of its capabilities through examples from different fields of applications.

R. R. Chianelli, M. Perez De la Rosa, G. Meitzner, M. Siadati, G. Berhault, A. Mehta, J. Pople, S. Fuentes, G. Alonzo-Nuñez, et L. A. Polette. Synchrotron and simulations techniques applied to problems in materials science: catalysts and Azul Maya pigments. J. Synchrotron Radiat., 12(2):129-134, March 2005. [ doi ]

Development of synchrotron techniques for the determination of the structure of disordered, amorphous and surface materials has exploded over the past 20 years owing to the increasing availability of high-flux synchrotron radiation and the continuing development of increasingly powerful synchrotron techniques. These techniques are available to materials scientists who are not necessarily synchrotron scientists through interaction with effective user communities that exist at synchrotrons such as the Stanford Synchrotron Radiation Laboratory. In this article the application of multiple synchrotron characterization techniques to two classes of materials defined as 'surface compounds' is reviewed. One class of surface compounds are materials like MoS2-xCx that are widely used petroleum catalysts, used to improve the environmental properties of transportation fuels. These compounds may be viewed as 'sulfide-supported carbides' in their catalytically active states. The second class of 'surface compounds' are the 'Maya blue' pigments that are based on technology created by the ancient Maya. These compounds are organic/inorganic 'surface complexes' consisting of the dye indigo and palygorskite, common clay. The identification of both surface compounds relies on the application of synchrotron techniques as described here.

D. Neff, P. Dillmann, L. Bellot-Gurlet, et G. Béranger. Corrosion of iron archaeological artefacts in soil: characterisation of the corrosion system. Corrosion Sci., 47(2):515-535, February 2005. [ doi ]

This paper presents a study made on 40 iron archaeological artefacts buried in soil during several centuries. Samples were taken with the adhering soil and cross-sections were made. The used characterisation techniques are optical and electronic microscopies, EDS coupled to SEM, EPMA, micro-XRD under synchrotron radiation, micro-Raman spectrometry. A specific vocabulary is proposed to describe the corrosion layout. The most identified corrosion layout is made of several ten micrometers zones of magnetite and/or maghemite embedded in a goethite matrix. A corrosion mechanism is proposed in order to explain this profile. When the soil water contains more chlorine or carbonates, some specific corrosion product appear as akaganeite, oxychlorides and siderite. (C) 2004 Elsevier Ltd. All rights reserved.

A. Denker, O. Hahn, S. Merchel, M. Radtke, B. Kanngiesser, W. Malzer, S. Röhrs, I. Reiche, et H. Stege. Röntgenanalytik für Kunstwerke und Kulturgüter. Nachrichten aus der Chemie, 2:118-123, February 2005. [ doi ]

Naturwissenschaftler arbeiten mit Archäologen, Kunsthistorikern und Restauratoren zusammen, um Materialinformationen über Kunstwerke mit den Erkenntnissen aus Altertumsforschung, Kunstgeschichte und Denkmalpflege zu verbinden. Röntgenfluoreszenz und Röntgenemission sind die Methoden der Wahl, wenn wertvolle und fragile Objekte zerstörungsfrei zu untersuchen sind.

A. Adriaens. Non-destructive analysis and testing of museum objects: An overview of 5 years of research. Spectrochim. Acta B, 60:1503 - 1516, 2005. [ doi ]

This paper gives an overview of research in or associated with the pan-European network COST Action G8, which aims at achieving a better preservation and conservation of our cultural heritage by increasing the knowledge of art and archaeological objects through advanced chemical and physical analyses. The paper is focussed on the use of various analytical techniques for the examination of cultural heritage materials and includes research examples on painted works of art, ceramics, glasses, glazes and metals. In addition attention is drawn to advances in analytical instrumentation, for example the development of portable techniques to perform analyses on site, and to the need for collaboration between people directly involved in the field of cultural heritage and analytical scientists.

C. J. Kennedy, K. von Lerber, et T. J. Wess. Measuring cristallinity of laser cleaned silk by X-ray diffraction. e-Preservation Sci., 2:31-37, 2005.

B. A. et al.. The Vikings in Berlin. SyXRF-analyses of the Hiddensee gold jewellery. Bessy highlights, 2004:32-33, 2005.

I. Ioannou, C. Hall, W. D. Hoff, V. A. Pugsley, et S. D. M. Jacques. Synchrotron radiation energy-dispersive x-ray diffraction analysis of salt distribution in lépine limestone. Analyst, 130:1006 - 1008, 2005. [ doi ]

We describe an analytical application of synchrotron radiation energy-dispersive diffraction tomography to map the distribution of crystalline sodium sulfate deposited by evaporation from solution within a building limestone.

L. Bertrand et P. Dillmann. Round table: Synchrotron and archaeometry. Revue d'archéométrie, 29:169-171, 2005.

M. Cotte, P. Dumas, et P. Walter. Synchrotron infrared microscopy of ancient biological and cosmetics material. Dans Picollo [ .ref ], p. 75-82.

M. Cotte, P. Dumas, et P. Walter. Analyses de savons de plomb présents dans des produits cosmétiques et pharmaceutiques antiques. Dans Verger [ .ref ].

D. H. Bilderback, J. Powers, N. Dimitrova, R. Huang, D.-M. Smilgies, K. Clinton, et R. E. Thorne. X-ray fluorescence recovers writing from ancient inscriptions. Z. Papyrol. Epigr., 152:221-227, 2005.

J. Powers, N. Dimitrova, R. Huang, D.-M. Smilgies, D. H. Bilderback, K. Clinton, et R. E. Thorne. Recovering ancient inscriptions by X-ray fluorescence. CHESS News Mag., p. 56-59, 2005.

A. Woll. Science meets art: Confocal X-ray Fluorescence Microscopy at CHESS. CHESS News Magazine, 2005.

R. Larsen, D. V. Poulsen, F. Juchauld, H. Jerosch, M. Odlyha, J. de Groot, Q. Wang, C. Theodorakopoulos, T. Wess, J. Hiller, C. Kennedy, G. Della Gatta, E. Badea, A. Masic, S. Boghosian, et D. Fessas. Damage assessment of parchment: complexity and relations at different structural levels. Dans Verger [ .ref ], p. 199-208.

F. Farges, E. Chalmin, C. Vignaud, I. Pallot-Frossard, J. Susini, J. Bargar, G. E. Brown, et M. Menu. Archeological Applications of XAFS: Prehistorical Paintings and Medieval Glasses. Physica Scripta Online, 115:885, 2005. [ doi ]

Highresolution manganese and iron Kedges XANES spectra were collected on several samples of archeological interest prehistorical paintings and medieval glasses. XANES spectra were collected at the ID21 facility ESRF, Grenoble, France using a microbeam device and at the 112 beamline SSRL, Stanford, USA using a submillimetric beam. The medieval glasses studied are from gothic glass windows from Normandy XIVth century. The aim of this study is to help understand the chemical durability of these materials, exposed to weathering since the XIVth century. They are used as analogues of weathered glasses used to dump metallic wastes. These glasses show surficial enrichment in manganese, due to its oxidation from II glass to IIIIV surface, which precipitates as amorphous oxyhydroxides. Similarly, iron is oxidized on the surface and forms ferrihydritetype aggregates. The prehistorical paintings are from Lascaux and Ekain Basque country. We choose in that study the black ones, rich in manganese to search for potential evidences of some savoirfaire that the Paleolithic men could have used to realize their paint in rock art, as shown earlier for Febearing pigments. A large number of highly valuable samples, micrometric scaled, were extracted from these frescoes and show large variation in the mineralogical nature of the black pigments used, from an amorphous psilomelanetype to a wellcrystallized pyrolusite. Correlation with the crystals morphology helps understanding the knowhow of these early artists.

M. Feist, J. Liu, et P. Tafforeau. New insights into Paleozoic charophyte morphology and phylogeny. Am. J. Bot., 92(7):1152-1160, 2005. [ doi ]

Examination of Paleozoic charophyte fructifications using microscopy and high-resolution x-ray synchrotron microtomography has revealed that most of them have a utricle that forms a supplementary calcified cover around the gyrogonite. All Paleozoic families with utricles have been assigned to the Sycidiales. We consider the Moellerinaceae to occupy a central position in the phylogeny of the Charophyta. From these, one group of descendants constitutes the gyrogonites inside the utricles of the Sycidiales; a second descendant goup is thought to be the utricle-free ancestors of the Charales prior to inversion of spiralization and reduction in cell number. The Sycidiales have a multilayered wall and an internal vesicle, but their families are distinguished by diversity in orientation of external cells, complexity of the utricle wall, and in presence or absence of antheridia. The solidly packed structure of the utricle is believed to be an organ protecting the zygote against dessication. We interpret the morphological similarities between Paleozoic Sycidiales and Mesozoic Clavatoraceae, both with a utricle, as homoplasous rather than expressing a true phylogenetic relationship. We confirm that some umbellids might correspond to utricles of charophytes.

S. Frisia, A. Borsato, J. Susini, et A. Somogyi. Climate forcings and their influence on Alpine history as reconstructed through the application of synchrotron-based X-Ray microfluorescence on layered stalagmites. Archaeometry, 47(2):209-219, 2005. [ doi ]

Solar variability and volcanic activity strongly interact with climate and the environment. Synchrotron radiation X-ray microfluorescence (micro-XRF) to an annually laminated Alpine stalagmite confirmed that annual laminae result from hydrological variability and changes in the duration of soil microbial degradation. The latter is modulated by solar variability. At the centennial timescale, growth rate and solar activity appear to be correlated with temperature change, with low temperatures at solar minima. By combining micro-XRF and absorption spectroscopy techniques (XANES), we also found that speleothems are a new archive of aerosol sulphate related to volcanic activity. Peaks in S-concentration from c. 5.2 to 5.0 ka bp in an Alpine stalagmite suggest that multiple volcanic sulphate aerosol emissions enhanced Mid-Holocene summer cooling, thus favouring the preservation of the Alpine Iceman mummy in a persistent ice casket.

Z. Šmit, K. Janssens, O. Schalm, et M. Kos. Analysis of façon-de-Venise glass originating from Central and Western Europe. Dans J. E. Fernandez, G. Maino, et A. Tartari, éds, Radiation physics for preservation of the cultural heritage, p. 165-176. Bologna, CLUEB, 2005.

B. Kanngiesser, W. Malzer, A. F. Rodriguez, et I. Reiche. Three-dimensional micro-XRF investigations of paint layers with a tabletop setup. Spectrochim. Acta B, 60:41-47, January 2005. [ doi ]

The non-destructive investigation of art and archaeological objects with depth sensitivity is now possible using 3D micro- XRF spectroscopy. More detailed answers for questions on painting techniques, on the pigment palette, on the production processes and indirectly on dating or provenancing of objects are accessible now. This was already illustrated by the investigation of Mughal miniatures with a confocal setup at the synchrotron source BESSY. In this paper we demonstrate the feasibility of 3D micro-XRF spectroscopy with a tabletop setup and discuss its sensitivity in comparison to the synchrotron- based setup. Investigated objects are glass standards and also prepared paint layers. Perspectives for other types of studies are proposed. (C) 2004 Elsevier B.V. All rights reserved.

N. Salvadó, S. Butí, M. Tobin, E. Pantos, et T. Pradell. The nature of medieval synthetic pigments: the capabilities of SR-Infrared spectroscopy. Dans Picollo [ .ref ], p. 296-301.

E. Pantos, W. Kockelmann, L. C. Chapon, L. Lutteroti, S. L. Bennet, M. J. Tobin, J. F. W. Mosselmans, T. Pradell, N. Salvadó, S. Butí, R. Garner, et A. J. N. Prag. Neutron and X-ray characterisation of the metallurgical properties of a 7th century BC Corinthian-type bronze helmet. Nucl. Instrum. Methods B, 239:16-26, 2005. [ doi ]

Neutron and synchrotron X-ray diffraction, X-ray fluorescence and FTIR were used to examine a Corinthian-type bronze helmet which is now on display at The Manchester Museum, UK. This type of helmet was manufactured out of a single piece of bronze, probably on a rod-anvil, and like all body-armour it was made to measure. Neutron diffraction sampling of the bronze volume in different areas was used to study the composition, microstructure and crystallographic texture of the alloy in order to draw conclusions about the manufacturing processes. The neutron data revealed the presence of microstrains and non-random distributions of bronze grains hinting at annealing-hammering working cycles in order to harden and shape the alloy. X-ray fluorescence showed that the main body of the helmet is a copper-tin alloy, while the noseguard contains zinc in high abundance. This key compositional difference confirms that the noseguard is not the original but is a modern substitute fabricated for restoration purposes. SR XRD and FTIR from several spots on the head and noseguard identified several surface corrosion products and showed a variation of the Cu-Sn or Cu-Zn percentage compositions, and of the mineral phases. Small samples of corrosion flakes extracted from the outside and inside of the helmet were used to obtain powder XRD patterns.

M. Picollo, éd. Proc. Vol. of the Sixth infrared and Raman users group conf. (IRUG 6) - Florence, Italy - March 29th - April 1st 2004. Il Prato, 2005.

R. Tabuce, M. Mahboubi, P. Tafforeau, et J. Sudre. Discovery of a highly-specialized plesiadapiform primate in the early-middle Eocene of northwestern Africa. J. Hum. Evol., 47(5):305-321, November 2004. [ doi ]

In this paper we report the first occurrence of an endemic African plesiadapiform primate from the early-middle Eocene locality of Glib Zegdou (Hammada du Dra, Algeria). Dralestes (new genus) is a very specialized taxon, and its closest known relative is the enigmatic and controversial genus Azibius from Gour Lazib (Hammada du Dra). We group both together as the Azibiidae (new rank). Dralestes provides the first evidence of the upper dentition in this group. Some critical dental characters, such as a postprotocingulum on upper teeth, consistently reveal a primate status for the azibiids. Dralestes exhibits, however, a very unusual configuration of the upper molars by the enlarged parastyle, the lack of a metaconule, and the ectoloph structure (preparacrista, centrocrista and postmetacrista are aligned in a high blade-like structure). The apparent dental specializations of both lower premolars and molars of azibiids (exaenodonty, large P(4) bearing sharp apical cusps, and M(1) having a highly elongated trigonid) point to potential relationships with Chronolestes and carpolestid plesiadapiforms. A phylogenetic analysis, performed on 55 dental characters scored for 19 primate genera, clarifies the euprimate status of Altiatlasius, and thus indicates that azibiids are the only known plesiadapiforms from Africa. Azibiids are the sister group of the clade carpolestids/Chronolestes in the superfamily Plesiadapoidea. However, the azibiids differ fundamentally from carpolestids by the combined lack of a centroconule and multiple buccal cusps on P(4). The exact position of both Chronolestes and azibiids in the plesiadapoids appears difficult to resolve. A basal position of Chronolestes in this superfamily cannot be ruled out because it exhibits a simple morphology of I(1) and no conule on P(3). Considering this ad hoc hypothesis, azibiids are found to lie outside a clade including carpolestids/plesiadapids/saxonellids, and they are the sister group to Chronolestes. The clade including the carpolestid, saxonellid, and plesiadapid families is characterized by the occurrence of a centroconule on P(3-4). The lack of this trait in Dralestes and Chronolestes could mean that azibiids are basal plesiadapoids that diverged before the evolution of the common ancestor of the three derived plesiadapoid families, i.e. at least around the Paleocene-Eocene boundary or more probably during the Paleocene. The report of the first offshoot in Africa of plesiadapoids enhances the role of Africa in the early primate radiation.

I. Reiche, A. Berger, W. Görner, S. Merchel, M. Radtke, J. Riederer, H. Riesemeier, et M. Roth. Following the traces of albrecht dürer: analysis of silverpoint drawings by spatially resolved synchrotron-induced x-ray fluorescence analysis. Nucl. Instrum. Methods B, 226(1-2):83-91, November 2004. [ doi ]

Spatially resolved X-ray fluorescence analysis using synchrotron radiation (SR-XRF) at the wavelength shifter beamline, BAMline, at BESSY was used to investigate Renaissance silverpoint drawings as it is extremely sensitive, non-destructive and can be carried out in air using an excitation spot in the hundred micrometer range.This paper deals with first results of the study of silverpoint drawings of Albrecht Dürer (1471-1528) belonging to the sketchbook that Albrecht Dürer used during a travel to the Netherlands in 1520/21. These results are compared to a PIXE study performed on drawings from the same sketchbook.The minor element composition of the silverpoint used for the drawings in the sketchbook was (10.6 3.5) wt.% of Cu and traces of Zn. Mercury was found in the marks but does not belong to the initial composition of the silverpoint as it is attributed to an alteration phenomenon. One drawing of the sketchbook represents an exception. It consists of silver marks containing an additional minor element, Zn, in the marks and was, therefore, created with another silverpoint, probably at a different time than the other drawings.

É. Dooryhée, P. Martinetto, P. Walter, et M. Anne. Synchrotron X-ray analyses in art and archaeology. Rad. Phys. Chem., 71(3-4):863-868, October-November 2004. [ doi ]

X-ray synchrotron techniques play an increasingly important part in the analysis strategy of archaeological materials, in order to determine the source materials, their provenance and the ancient techniques of preparation. In favourable cases, the microstructure (crystallite size and deformation) can be interpreted as a residual mark of the elaboration techniques and origin of ancient polycrystalline materials. Our study on cosmetic recipes and make-up manufacturing in Antiquity, illustrates some possible applications of non-destructive synchrotron techniques, complementing other standard analytical tools.

K. Janssens, K. Proost, et G. Falkenberg. Confocal microscopic X-ray fluorescence at the HASYLAB microfocus beamline: characteristics and possibilities. Spectrochim. Acta B, 59(10-11):1637-1645, October 2004. [ doi ]

The possibilities of performing non-destructive elemental analysis in three dimensions on a variety of heterogeneous materials by means of an innovative variation of the microscopic X-ray fluorescence analysis (μ-XRF) method are described. Next to employing focusing optics for concentration of the primary beam of X-rays, a second optical element between the sample and the energy-dispersive detector is used in confocal μ-XRF. Thus, only X-ray fluorescence signals from a cube-like volume (within certain limits imposed by the absorption of the radiation in the sample) can be arbitrarily positioned within the sample. The distribution of major, minor and trace elements (down to the sub-ppm concentration level in some matrices) along lines and planes within the sample can be visualized with a spatial resolution of the order of 15-40 μm. The lowest detectable amounts in confocal mode using pink-beam excitation are situated at the sub-femtogram level.

M. Müller, B. Murphy, M. Burghammer, C. Riekel, M. Roberts, M. Papiz, D. Clarke, J. Gunneweg, et E. Pantos. Identification of ancient textile fibres from Khirbet Qumran caves using synchrotron radiation microbeam diffraction. Spectrochim. Acta B, 59:1669-1674, October 2004. [ doi ]

Archaeological textiles fragments from the caves of Qumran in the Dead Sea region were investigated by means of X-ray microbeam diffraction on single fibres. This non-destructive technique made the identification of the used plant textile fibres possible. Apart from bast fibres (mainly flax), cotton was identified which was most unexpected in the archaeological context. (C) 2004 Elsevier B.V. All rights reserved.

J. Bartoll, S. Röhrs, A. Erko, A. Firsov, A. Bjeoumikhov, et N. Langhoff. Micro-X-ray absorption near edge structure spectroscopy investigations of baroque tin-amalgam mirrors at BESSY using a capillary focusing system. Spectrochim. Acta B, 59(10-11):1587-1592, October 2004. [ doi ]

An elliptically shaped glass monocapillary with a spatial resolution of 5 μm has been used for the fine focusing of the pre-focused X-ray beam produced by the graded-crystal monochromator beamline, KMC-2. The flux density gain of 50 was experimentally measured. The microprobe has been used in the energy range of 3.5-15 keV. Micro-X-ray fluorescence analysis (μXFA) and micro-X-ray absorption near edge structure spectroscopy (μXANES) measurements on test samples and investigations of baroque tin-amalgam mirrors were done.

M. S. del Río, P. Martinetto, A. Somogyi, C. Reyes-Valerio, É. Dooryhée, N. Peltier, L. Alianelli, B. Moignard, L. Pichon, T. Calligaro, et J.-C. Dran. Microanalysis study of archaeological mural samples containing Maya blue pigment. Spectrochim. Acta B, 59(10-11):1619-1625, October 2004. [ doi ]

Elemental analysis by X-ray fluorescence and particle induced X-ray emission is applied to the study of several Mesoamerican mural samples containing blue pigments. The most characteristic blue pigment is Maya blue, a very stable organo-clay complex original from Maya culture and widely used in murals, pottery and sculptures in a vast region of Mesoamerica during the pre-hispanic time (from VIII century) and during the colonization until 1580. The mural samples come from six different archaeological sites (four pre-hispanic and two from XVI century colonial convents). The correlation between the presence of some elements and the pigment colour is discussed. From the comparative study of the elemental concentration, some conclusions are drawn on the nature of the pigments and the technology used.

B. Kanngiesser, O. Hahn, M. Wilke, B. Nekat, W. Malzer, et A. Erko. Investigation of oxidation and migration processes of inorganic compounds in ink-corroded manuscripts. Spectrochim. Acta B, 59:1511-1516, October 2004. [ doi ]

We studied the oxidation and migration processes of inorganic compounds in iron gall inks with a combination of micro X-ray fluorescence analysis (micro-XRF) and micro X-ray absorption near edge structure spectroscopy (micro-XANES). With elemental mapping by micro-XRF, the correlation of the minor elements in the ink to the major element Fe was investigated. Along concentration profiles of Fe, micro-XANES measurements were carried out in order to determine the oxidation state and the local environment. With the help of model inks, we could show that Cu is a further important element in the paper degradation process due to iron gall ink corrosion. (C) 2004 Elsevier B.V. All rights reserved.

D. Grolimund, M. Senn, M. Trottmann, M. Janousch, I. Bonhoure, A. Scheidegger, et M. Marcus. Shedding new light on historical metal samples using micro-focused synchrotron X-ray fluorescence and spectroscopy. Spectrochim. Acta B, 59:1627-1635, October 2004. [ doi ]

Synchrotron-based micro-X-ray fluorescence (micro-XRF) and micro-X-ray absorption spectroscopy (micro-XAS) were used in the present study to obtain spatially resolved micro-scale information on elemental composition, trace element distribution, chemical speciation and oxidation state and/or mineral phase distribution within historical iron artefacts dating from the Iron Age to early Medieval Times. Large area two-dimensional trace element distribution maps and oxidation state maps with micrometer spatial resolution were required to answer open archaeological questions in the context of ancient metal processing. The first set of examples was focusing on historical weapons and included two ancient iron sword blades. The micro-XRF maps revealed a distinct, highly correlated distribution pattern of trace elements such as As, Ni, Cu and Zn. Accordingly, the number of used raw materials could be determined unambiguously and key information concerning the used ancient smithing technique were gained. Further, the ability to record-in a fast manner-large area maps with high spatial resolution ('elemental screening') led to the discovery of a hitherto unknown enhanced occurrence of selected trace elements (Cu, Zn, and An) at the blade surface. Complementary investigations by high resolution scanning electron microscopy were able to localize these trace metals within a carbon-rich matrix may be pointing towards an artifact induced during preservation. A second set of investigated artefacts is dealing with smithing waste products and related historical processing techniques and conditions. Synchrotron-based micro-XRF and micro-XAS were used to determine the structural composition as well as the spatial variation of the predominant Fe oxidation state and corresponding crystallographic phases. The study revealed the presence of distinct domains of Fe-0, (FeO)-O-II (wustite), and alpha-(FeOOH)-O-III (goethite), separated by sharp domain boundaries. These findings help to gain new insights concerning the nature and origin of used raw materials as well as regarding employed processing techniques during historic iron fabrication and weapon manufacturing. The study demonstrates the potential of oxidation state and mineral phase mapping based on energy selective micro-XRF maps and spectroscopic phase identification. Such a spatially resolved recording of the chemical speciation is based on X-ray absorption spectroscopy. This analytical technique is exclusive to synchrotron light sources. However, the steadily increasing number of available synchrotron-based X-ray microprobes allows nowadays for more routine utilization of such micro-XAS techniques. (C) 2004 Elsevier B.V. All rights reserved.

A. Cedola, S. Lagomarsino, V. Komlev, F. Rustichelli, M. Mastrogiacomo, R. Cancedda, S. Milita, et M. Burghammer. High spatial resolution X-ray microdiffraction applied to biomaterial studies and archeometry. Spectrochim. Acta B, 59:1557-1564, October 2004. [ doi ]

The high spatial resolution X-ray microdiffraction by using X- ray optics can provide unique information on regions with very high gradients in physical quantities, as in the case of interfaces. Among the several available X-ray optics for synchrotron radiation producing high intensity micron and sub- micron beams, the X-ray waveguide (WG) can provide the smallest X-ray beam in one direction. Moreover, its applicability has been widened by an improved set-up installed at ID13 beamline at ESRF, where a new undulator is combined with an horizontally focusing mirror. In this work, we show different applications of waveguide-based microdiffraction, the first two regard biological problems and in particular the structural analysis of newly formed bone in ceramic scaffolds. The second application regards archeometry and in particular the sulphatation process and the thin gypsum crust formation on the surface of carbonate rocks (travertine, marbles), due to the exposure of the monuments at aggressive atmospheres. In the three cases, the local structural information derived thanks to the high spatial resolution demonstrates the power of the microdiffraction technique based on WG, and the possibility to apply this new methododogy in different scientific fields. (C) 2004 Elsevier B.V. All rights reserved.

K. Leyssens, A. Adriaens, E. Pantos, et C. Degrigny. Study of corrosion potential measurements as a means to monitor the storage and stabilization processes of archaeological copper artefacts. Dans Proceedings of the International Conference on Metals Conservation, Canberra, October 4-8, 2004, vol. 332-343, Canberra, Australia, October 2004. Canberra National Museum of Australia.

Archaeological copper artefacts recovered from wet saline environments are often stored in tap water and stabilized in sodium sesquicarbonate solutions. Modification of the natural patina and development of active corrosion can occur during these processes. This implies that monitoring of storage/stabilisation processes is necessary. The focus of the study consists of examining how corrosion potential (Ecorr) measurements can contribute in providing information on the effectiveness of storage and stabilisation treatments. This paper reports on the Ecorr versus time plots of artificially prepared copper coupons (covered or not with corrosion layers) immersed in tap water and a sodium sesquicarbonate solution. Synchrotron radiation XRD was performed in parallel to understand the reactions that take place during the immersion processes.

W. P. Adderley, I. L. Alberts, I. A. Simpson, et T. J. Wess. Calcium-iron-phosphate features in archaeological sediments: characterization through microfocus synchrotron X-ray scattering analyses. J. Archaeol. Sci., 31(9):1215-1224, September 2004. [ doi ]

The occurrence of amorphous calcium (Ca)-iron (Fe)-phosphate infilling features in thin-section samples from archaeological stratigraphies is increasingly being reported and used in the cultural interpretations of sites. In some contexts, these materials are the product of dissolution and recrystallization of bone material within pores of the soil or sediment matrix. This study uses transmitted microfocus X-ray scattering to characterize and measure features of known cod fish bone (Gadus morhua) materials, and compare them to archaeological samples of amorphous Ca-Fe-phosphate infilling material found in thin section from early fishing community sites. The analyses characterize the structure of these features for the first tinge, and allow discussion of the diagenetic processes that lead to their formation. (C) 2004 Elsevier Ltd. All rights reserved.

D. Neff, S. Reguer, L. Bellot-Gurlet, P. Dillmann, et R. Bertholon. Structural characterization of corrosion products on archaeological iron: an integrated analytical approach to establish corrosion forms. J. Raman Spectro., 35(8-9):739-745, August 2004. [ doi ]

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 (muXRD) 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 muXRD (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 (C) 2004 John Wiley Sons, Ltd.

M. O. Figueiredo, T. P. Silva, J. P. Veiga, A. M. D. Diogo, et L. Trindade. Archaeology of Lisbon old city: ceramic crucibles from pre-XVIIIth century metallurgical foundries. Appl. Phys. A, 79(2):327-329, July 2004. [ doi ]

During an emergency archaeological intervention conducted in downtown Lisbon (the Old City), ceramic foundry crucibles were collected in a layer of embankment debris used after the earthquake that destroyed the city in 1755. A chemical and phase-constitution study was undertaken to complement the dating and to ascertain the kind of foundries (metallurgical or glass-working) concerning two intact cup-shaped crucibles and a fragment displaying glassy outflows. Non-destructive methodologies were used - namely, laboratory techniques (X-ray fluorescence spectrometry and X-ray diffraction) combined with synchrotron-radiation-induced micro-fluorescence (SRXRF). Analytical results are presented and discussed. SRXRF analysis of the glassy outflow on the larger crucible revealed the presence of mercury and traces of gold, along with copper, suggesting that it might have been used to manipulate gold amalgams. A possible Islamic origin was disclosed for the smaller crucible as only tin was detected in the external outflow and further confirmed by minute cassiterite (SnO2) grains.

P. Dillmann, F. Mazaudier, et S. Hoerlé. Advances in understanding atmospheric corrosion of iron. I. Rust characterisation of ancient ferrous artefacts exposed to indoor atmospheric corrosion. Corrosion Sci., 46(6):1401-1429, June 2004. [ doi ]

Metallic substrates and rust layers of several hundred year old (y.o.) ferrous artefacts were characterised. Composition, structure and porosity of the rust were analysed by different methods: OM, SEM, EDS, EPMA, XRD, [mu]XRD, SAXS, BET and mercury porosimetry.Several important parameters to describe an old rust layer were determined and measured. These parameters will be used for the modelling of long-term indoor atmospheric corrosion.

T. Pradell, J. Molera, M. Vendrell, J. Pérez-Arantegui, E. Pantos, M. Roberts, et M. DiMichiel. Role of cinnabar in luster production. J. Am. Ceram. Soc., 87(6):1018-1023, June 2004. [ doi ]

Ancient documentation referring to the use of cinnabar in the production of luster decorations has recently been corroborated by archaeological findings. However, luster decorations do not show any trace of the use of cinnabar in their composition because the temperatures involved in luster firing (500-600C) result in the complete decomposition and volatilization of cinnabar. An in situ x-ray diffraction experiment was designed to clarify the role of cinnabar in the production of luster decorations. The high-energy, high-flux radiation ID15B beamline at the European Synchrotron Radiation Facility was necessary to ensure good time/temperature resolution, penetration, and high-quality data. Results show that cinnabar acts as a reducing agent for copper because it provides the formation of copper (Cu+) and silver (Ag+) sulfur-containing phases, and it inhibits the crystallization of metallic silver in the temperature range of interest in luster production. The addition of elemental sulfur also produces these phases, but at temperatures <500C, which are not adequate for the production of copper-containing lusters.

Z. Šmit, K. Janssens, K. Proost, et I. Langus. Confocal μ-XRF depth analysis of paint layers. Nucl. Instrum. Methods B, 219-20:35-40, June 2004. [ doi ]

Focused narrow-band beam of the synchrotron radiation was used for in-depth analysis of historic and modern paint layers. The fluorescent radiation induced by 21 keV impact radiation was detected by a Si(Li) detector equipped with a polycapillary X-ray lens in con-focal geometry. Scanning of the sample was performed by a motorized x-y-z stage. Space resolution of 30 [mu]m was achieved. The procedure of evaluation of concentrations was based on the independent parameter method and included absorption of radiation in the outer layers and secondary fluorescence enhancement induced by hard X-rays of the same and neighboring layers.

E. Gliozzo, I. W. Kirkman, E. Pantos, et I. Memmi-Turbanti. Black gloss pottery: production sites and technology in Northern Etruria, part II: gloss technology. Archaeometry, 46(2):227-246, May 2004. [ doi ]

The present study aims to understand the reasons for the visual differences of black gloss pottery found in northern Etruria. The results obtained by conventional (scanning electron microscope, electron microprobe) and synchrotron (X-ray diffraction, X-ray absorption spectroscopy) techniques indicate that the thickness, porosity or chemical composition of the different types of gloss cannot be used as the principal distinguishing factor. The size of quartz or feldspar crystals may well be a critical factor responsible for the matt effect in some samples, while the range of mixtures of iron compounds indicated by XRD and XAS could be the reason for differences in colour and reflectivity. The Fe L-edge XAS results in particular show that a correlation does exist between the oxidation state characteristics and the visual appearance. The Si, Fe and Al contents seem to further discriminate the different types of gloss that have differing visual appearances.

C. J. Kennedy, J. C. Hiller, D. Lammie, M. Drakopoulos, M. Vest, M. Cooper, W. P. Adderley, et T. J. Wess. Microfocus X-ray diffraction of historical parchment reveals variations in structural features through parchment cross sections. Nano Lett., 4(8):1373-1380, April 2004. [ doi ]

We propose a new method of investigating variation of preservation within a parchment sample, which allows a more detailed analysis of alteration of the material structure. X-ray diffraction analysis of parchment typically involves the sample aligned with the plane of the parchment perpendicular to the direction of the X-ray beam, with a beam size of approximately 200 μm and an image consisting of the composite diffraction features from the entire thickness of the sample. Here we describe the use of microfocus X-ray beams, with a beam size of 1.5 μm vertically x 15 μm horizontally, to carry out surface-to-surface scans of thin sections of parchment. Up to 200 images can be taken in a single cross-sectional scan of a 300 μm thick parchment section. This allows for X-ray diffraction analysis of features present only in specific areas of the parchment, such as at the surface. The orientation of collagen fibrils in the plane of the parchment, the effects of laser cleaning (including possible laser induced damage), mineral phases and crystalline lipids present in samples, and parchment structure under an inked region are investigated. It is shown that the long collagen fibril axis lies parallel to the parchment surface throughout the sections. Laser cleaning appears not to damage the collagen in parchment, while laser-damaged samples display gelatinization of the collagen at the surface. Polymorphs of calcium carbonate were detected in several samples but in most cases were not confined to the surfaces, as would be expected if the chalk finishing process was the main source of mineral phases in parchment. Crystalline lipid is found in most samples and appears to exhibit a preferential alignment with the plane of the phospholipid bilayer arranged parallel to the long fibril axis of collagen. The d spacing of the lipid is variable throughout a parchment section, indicating fluctuations in the hydration state, phase, or biochemical composition of the lipid. Ink affects the parchment to a depth of approximately 90 μm, as measured by principal components analysis, disrupting the structure of the collagen to this depth. These features demonstrate the ability of this technique to examine diagenesis of individual components of parchment on a scale not previously studied.

M. Mantler et J. Klikovits. Analysis of art objects and other delicate samples: Is XRF really nondestructive? Powder Diff., 19(1):16-20, March 2004. [ doi ]

XRF is generally considered a nondestructive analytical method in the sense that a specimen is not altered by the analytical procedure. This study is related to paintings and illuminated manuscripts, where the analytes are often inorganic pigments embedded into organic matrices such as fabrics (canvases), paper or parchment, binders, and varnish. We found that a typical measurement cycle with conventional tubes and energy dispersive systems (e.g., 100 s, 100 W tube-power) causes no visible harm. However, 3 kW radiative power for several minutes and more (as often required for wide angle scans as well as for the analysis of light elements or traces in a wavelength dispersive spectrometer) can leave visible traces of permanent yellowing, brittleness, and even mechanical decomposition. In such cases scanning electron microscopy-images indicate permanent alteration of the cellulose fibers and, in paper, of the binder. Employment of modern X-ray optical devices which focus the photons of a wide beam onto a small spot may also leave visible (and invisible) traces of destruction.

B. Newbury, B. Stephenson, J. Almer, M. Notis, G. S. Cargill III, G. B. Stephenson, et D. Haeffner. Synchrotron applications in archaeometallurgy: analysis of high zinc brass astrolabes. Powder Diff., 19(1):12-15, March 2004. [ doi ]

Synchrotron X rays were used to perform nondestructive transmission diffraction and fluorescence experiments on a group of 24 European and Islamic astrolabes dated between 1350- 1720 A.D. in order to determine their compositions. A group of six astrolabes produced in Lahore between 1601-1662 A.D. were found to contain a mixed alpha+beta brass microstructure, proving that the brass was produced by a comelting technique rather than the traditional cementation process. The results also show evidence of dezincification, attributed to heavy annealing of the brass during astrolabe manufacture. This effect was so severe that an accurate analysis of the bulk Zn composition could not be determined from the fluorescence results alone; transmission X-ray diffraction gives a more accurate measurement of the bulk Zn composition. (C) 2004 International Centre for Diffraction.

M. Schreiner, B. Frühmann, D. Jembrih-Simbürger, et R. Linke. X-rays in art and archaeology: an overview. Powder Diff., 19(1):3-11, March 2004. [ doi ]

An overview of the techniques used in art and archaeology is presented and the applicability of X-ray radiography, X-ray fluorescence (XRF), and X-ray diffraction analysis (XRD) as a tool for nondestructive investigations of objects of art and archaeology is discussed. X-ray radiography, for example, is a standard technique widely used and accepted by art historians, archaeologists, curators, and conservators as this method enables information about the manufacturing process and the condition of an object without touching the artifact. XRF and XRD enable a nondestructive determination of the material composition of artifacts and the determination of the crystalline structure of the components too. Air path systems and instruments with the micro-beam of X-ray and synchrotron radiation were applied for the analysis of easel paintings, pigments in paint layers, glass artifacts, and coins.

M. Matsunaga et I. Nakai. A study of the firing technique of pottery from Kaman-Kalehöyük, Turkey, by synchrotron radiation-Induced Fluorescence X-Ray Absorption Near-Edge Structure (Xanes) Analysis of trace elements in human hair by PIXE elemental analysis of South American mummy hair. Archaeometry, 46:103-114, February 2004. [ doi ]

Fe K-XANES spectra of a series of pottery sherds excavated from the archaeological site of Kaman-Kalehöyük, Turkey, were measured to reveal the firing technique of the pottery. The analysis disclosed relationships among the chemical form of the iron, the firing conditions and the colour of the pottery. The pottery referred to as 'Grey Ware' found at this site was classified into two groups according to the chemical form of the iron. Also, it was revealed that the Iron Age pottery referred to as 'Cream Ware' was produced first under reducing conditions, and then fired under oxidizing conditions.

C. J. Kennedy, M. Vest, M. Cooper, et T. J. Wess. Laser cleaning of parchment: structural, thermal and biochemical studies into the effect of wavelength and fluence. Appl. Surf. Sci., 227(1-4):151-163, 2004. [ doi ]

Laser cleaning of parchment is a novel technique that has the potential to provide contactless, chemical-free cleaning of historically important documents. However, the effect of laser cleaning on the collagenous structure of parchment is still poorly understood, as is the effect of the wavelength or the energy density (fluence level) used to clean parchment. In this study, small angle X-ray scattering (SAXS), shrinkage temperature (Ts) measurements by the micro hot table technique and SDS-polyacrylamide gel electrophoresis (SDS-PAGE) of parchment samples after laser cleaning reveal the effect of cleaning to the structural, thermal and molecular characteristics of parchment, respectively. The effect of cleaning at infrared (1064 nm), green (532 nm) and ultraviolet (266 nm) wavelengths at a range of fluence levels is investigated. SAXS is used to investigate the removal of dirt from parchment. Laser cleaning at IR or green wavelengths appears not to alter the collagen diffraction pattern from SAXS, the shrinkage activity or shrinkage temperature from Ts measurements or the molecular integrity of parchment as shown by SDS-PAGE. However, parchments cleaned at the ultraviolet wavelength display structural damage and a reduction in hydrothermal stability and molecular integrity.

J. Rius, E. Elkaim, et X. Torrelles. Structure determination of the blue mineral pigment aerinite from synchrotron powder diffraction data: The solution of an old riddle. Eur. J. Mineral., 16(1):127-134, January 2004. [ doi ]

P. Fredrickx, I. D. Ryck, K. Janssens, D. Schryvers, J.-P. Petit, et H. Döcking. EPMA and μ-SRXRF analysis and TEM-based microstructure characterization of a set of Roman glass fragments. X-Ray Spectrom., 33:326-333, 2004. [ doi ]

A set of Roman glass fragments, excavated at Bliesbruck-Reinheim (French-German border), were analysed by electron probe microanalysis (EPMA) and micro-synchrotron radiation-induced x-ray fluorescence (μ-SRXRF) in order to determine the major, minor and trace chemical composition. Based on this analysis, five classes of mono-coloured glass could be discerned. However, one piece of this set was not mono-coloured, but consisted of a mixture of brown and white opaque glass. This fragment was investigated using EPMA and transmission electron microscopy (TEM) in order to gain a better insight into its microstructure. Both colours proved to contain small crystalline inhomogeneities. Structural information reveals the form in which the detected elements are present and helps to explain the appearance (e.g. colour) of the material. Copyright ? 2004 John Wiley & Sons, Ltd.

M. Brunet, F. Guy, J.-R. Boisserie, A. Ibaye, T. Lehmann, F. Lihoreau, A. Louchart, M. Schuster, P. Tafforeau, A. Likius, H. Mackaye, C. Blondel, H. Bocherens, L. De Bonis, Y. Coppens, C. Denis, P. Duringer, V. Eisenmann, A. Flisch, D. Geraads, N. Lopez-Martinez, O. Otero, P. Campomanes, D. Pilbeam, M. Ponce de Leon, P. Vignaud, L. Viriot, et C. Zollikofer. Touma{"\i}, Miocène supérieur du Tchad, le nouveau doyen du rameau humain. C. R. Palevol, 3(4):277-285, 2004. [ doi ]

`Toumaï', Late Miocene of Chad, the new earliest member of the human branch. The new Chadian hominid Sahelanthropus tchadensis Brunet et al., 2002, nicknamed `Toumaï', recovered by the MPFT (Mission paléoanthropologique franco-tchadienne, scientific collaboration between the University of Poitiers, University of N'Djamena and CNAR, National Center for the support of Science of N'Djamena) from the Late Miocene of Toros-Menalla (Djurab desert) is associated with a vertebrate fauna (more than 45 species) for which the mammalian component (at least 25 species) indicates a biochronological age close to 7 Ma. The fauna comprises vertebrates that are aquatic (fish, turtles, crocodiles) and amphibious (anthracotheriids, hippopotamids) but also species adapted to the gallery and islet forests (monkeys), wooded savanna (proboscideans, giraffids, suids, etc) and grassland (bovids, tridactyl equids). Sedimentological data (aeolian sandstones, perilacustrine sandstones, diatomites) agree with this mosaic of environments and indicate a vegetated perilacustrine belt between lake and desert. The new hominid is probably temporally close to the common ancestor of chimpanzees and humans but displays a unique combination of primitive and derived characters that clearly shows a close relationship with later hominids rather than with chimpanzees or gorilla. The geographic location of Toumaï, 2500 km west of the Rift Valley, along with its great antiquity, suggest an early widespread hominid distribution (Sahel and East Africa, at least by 6 Ma), and a somewhat earlier chimpanzee-human divergence (at least by 7 Ma ago) than previously indicated by many molecular studies.

I. Reiche. Synchrotron-induzierte Roentgenfluoreszenzanalyse - Untersuchungen an Renaissance-Zeichnungen und indischen Miniaturen. Restauro, 6:378-384, 2004. [ doi ]

When chemo-physical analysis of a work of art is required, it should be done in situ and in a nondestructive manner. In the last ten years, great strides have been made in the development of chemo-physical methods that do not call for sample-taking or otherwise damage the object, i.e. are non-destructive. Here X-ray methods play a special role. One of the newest developments is synchrotron-induced X-ray fluorescent analysis to determine characteristic trace elements, layers (paint layers) or two-dimensional or three-dimensional phase distribution. Today art objects can be examined directly on museum premises or on archaeological excavation sites with portable devices, such as mobile X-ray fluorescent analysis (RFA). Compared to portable laboratory devices, synchrotron radiation, however, offers more exact analysis. It was applied to examine Renaissance silver-point drawings from the Kupferstichkabinett Berlin as well as the paint layers of Indian miniatures from the Museum für Indische Kunst Berlin. In the case of Dürer's portrait of “Willibald Pirkheimer”, it could be proven that the same type silver point had been employed for both the inscription as well as the drawing itself and that the mysterious inscription must, therefore, have been added at least with his knowledge. In the case of the 17th century Indian miniatures, ia. the green pigment rosasite (Cu,Zn)2 CO3(OH)2 could be identified and thus the use of zinc white could be proven. Further tests will have to show whether these are natural ore admixtures or a synthetic zinc oxide.

L. Bertrand. First european training school on the synchrotron analysis of ancient materials. Soc. Archaeol. Sci. Bull., 27(4):8-9, 2004.

K. Proost, K. Janssens, B. Wagner, E. Bulska, et M. Schreiner. Determination of localized Fe2+ /Fe3+ ratios in inks of historic documents by means of μ-XANES. Nucl. Instrum. Methods B, 213:723-728, January 2004. [ doi ]

An important part of the European cultural heritage is composed of hand-written documents. Many of these documents were drawn up with iron-gall ink. This type of ink present a serious conservation problem, as it slowly oxidizes ('burns') the paper it is written on, thereby gradually disintegrating the historic document. Acid hydrolysis of the cellulose and/or the oxidation of organic compounds promoted by radical intermediates that are formed due to the presence of Fe2+ ions are considered to be the cause of the disintegration. μ-XANES measurements were performed with a lateral resolution of 30-50 mum in order to determine the local Fe2+/Fe3+ ratio in 19th C. documents from the Austrian National Archives and fragments of 16th C documents from the Polish National Library. In the 19th C documents, no significant amount of Fe2+ was detected. On the other hand, in the 16th C fragments, significant amounts of Fe2+ and appreciable differences in distribution of Fe2+ and Fe3+ within individual letters/ink stains were observed. (C) 2003 Elsevier B.V. All rights reserved.

M. Sandström, Y. Fors, F. Jalilehvand, E. Damian, et U. Gelius. Analyses of sulfur and iron in marine-archaeological wood. Dans P. Hoffmann, J. A. Spriggs, K. Strætkvern, et D. Gregory, éds, Proc. of the 9th ICOM group on Wet Organic Archaeological Materials conference, Copenhagen, June 6-11, 2004. Deutsches Schiffahrtsmuseum, Bremerhaven, Germany, 2004.

I. Reiche, A. Berger, A. Duval, W. Görner, S. Merchel, M. Radtke, J. Riederer, et H. Riesemeier. Metallstiftzeichnungen Albrecht Dürers - Zerstörungsfreie Spurenanalyse mit Synchrotron-induzierter Röntgenfluoreszenzanalyse. Dans PapierRestaurierung - Mitteilungen der IADA (Internationale Arbeitsgemeinschaft der Archiv-, Bibliotheks- und Graphikrestauratoren), vol. 5, p. 30-38, 2004.

Metallstiftzeichnungen gehören zu den wertvollsten Schätzen graphischer Sammlungen. Sie wurden vor allem in der Renaissance geschaffen und sind durch eine sehr feine und präzise Linienführung gekennzeichnet. Bisher ist nur wenig über die chemische Zusammensetzung der Zeichnungen bekannt, da zum Zeichnen nur hauchdünne Metallspuren auf speziell präpariertem Papier aufgebracht wurden und infolge der Empfindlichkeit der Zeichnungen, Analysen nur schwer schadensfrei durchführbar sind. Grundsätzlich kann die Bestimmung der chemischen Zusammensetzung eines Kunstwerks Informationen über Genese, Herkunft und 'Vita' des untersuchten Objekts liefern. Eine weit verbreitete Methode hierfür ist die Bestimmung des 'chemischen Fingerabdrucks', bei der die Verhältnisse bzw. Gehalte ausgewählter Elemente bestimmt werden. Der Fingerabdruck ist charakteristisch für den Ursprung der verwendeten Materialien, aber auch für die Verarbeitung und die Umstände der Nutzung und Lagerung. So führen chemische Analysen zu einem besseren Verständnis der vom Künstler verwendeten Materialien und deren Alterungserscheinungen. Dank der Definition eines charakteristischen Fingerabdrucks ist es auch möglich, Zeichnungen zu gruppieren bzw. innerhalb einer Werkstatt zu differenzieren und somit eventuell genauere Zuschreibungen zu ermöglichen. In unserer Arbeit wurde die ortsaufgelöste Synchrotron-induzierte Röntgenfluoreszenzanalyse (SY-RFA), die hochsensitiv und absolut schadensfrei ist, zur präzisen Charakterisierung und Gruppierung von Zeichnungen Albrecht Dürers (1471-1528) angewandt. Sie zeigt das Potential der Methode und neue Perspektiven in der Erforschung von historischen Handzeichnungen.

I. De Ryck, A. Adriaens, P. Storme, et F. Adams. The Tin Mercury Inlay of a Cabinet Manufactured by Hendrik Van Soest: A Case Study. e-Preservation Sci., 1:9-14, 2004. [ doi ]

The tin inlay of a piece of furniture designed by Hendrick Van Soest has been investigated for its composition, microstructure and corrosion. Small samples were removed and investigated with optical microscopy, micro X-ray fluorescence spectroscopy and, scanning electron microscopy with energy-dispersive X-ray detection and synchrotron radiation X-ray diffraction. The results show that the inlay is composed of a binary alloy consisting tin and mercury. The composition suggests the use of an amalgam to produce the metal inlay. However the microstructure of the inlayed fillets proves that tin sheet was used instead of a tin mercury amalgam.

Corrosion of the tin inlay is the most important sign of deterioration. Analyses show the presence of a thin layer of tin oxide chloride hydroxide in direct contact with the metal. This layer is covered by a layer of the more common tin corrosion compounds romarchite and cassiterite. The harmful effect of chloride containing compound is shown by the advanced corrosion. For future preservation of the tin inlay this compound must be either removed or immobilized.

A. N. Fitch. The high resolution powder diffraction beam line at ESRF. J. Res. Natl. Inst. Standards Technol., 109(1):133-142, January-February 2004. [ doi ]

The optical design and performance of the high-resolution powder diffraction beam line BM16 at ESRF are discussed and illustrated. Some recent studies carried out on BM16 are described, including crystal structure solution and refinement, anomalous scattering, in situ measurements, residual strain in engineering components, investigation of microstructure, and grazing-incidence diffraction from surface layers. The beam line is built on a bending magnet, and operates in the energy range from 5 keV to 40 keV. After the move to an undulator source in 2002, it will benefit from an extented energy range up to 60 keV and increased flux and resolution. It is anticipated that enhancements to the data quality will be achieved, leading to the solution of larger crystal structures, and improvements in the accuracy of refined structures. The systematic exploitation of anisotropic thermal expansion will help reduce the effects of peak overlap in the analysis of powder diffraction data.

J. Siurek, P. Chevallier, C.-U. Ro, H. Y. Chun, H. S. Youn, E. Zieba, et A. Kuczumow. Studies on the wood tissue substitution by silica and calcite during the preservation of fossil wood. J. Alloys Compounds, 362(1-2):107-115, 2004. [ doi ]

Three representative samples of petrified wood were investigated: wood from King George Island, Antarctica; wood from Bio-Bio province, middle Chile and wood from Lukow, Poland. Microdiffraction measurements of the Chilean and Lukow wood were made at LURE. Chilean and Antarctic samples were permineralised by silica material, but the share of undefined calcium silicates in construction of some intracellular locations in the latter sample was significant. In contrast, the wood from Lukow was replaced by calcite with a small presence of secondary silica. Linear scans were conducted using the X-ray microfluorescence beamlines in synchrotron devices in Orsay, France and Pohang, South Korea. The results were completed by the measurements of light elements with the use of electron microprobe. The list of major and minor constituents of all samples was established. The occurrence of such medium-Z elements as Fe, Zn, Cu and Ni was common in the samples. The samples of Chilean wood were more enriched in trace elements and minor amounts of As, La, Br and Cl were found in addition to the previously mentioned elements. Correlation of the trace element contents with the ring structure of the wood was detected. The annual ring, tissue and even cell details of the original wood were preserved by silica and calcite minerals and could be studied using the elemental mapping technique. Implications of the recent study for the material science are indicated. (C) 2003 Elsevier B.V. All rights reserved.

A. Kuczumow. Microprobe investigations of patterned natural and petrified biological objects. J. Alloys Compounds, 362(1-2):71-82, January 2004. [ doi ]

The possibilities of examining patterned natural and mineralised biological objects, using X-ray synchrotron facilities, complemented by electron microprobe and optical analysis are reviewed. The objects under investigation include: petrified wood, speleothems, corals, shells of molluscs and remains of belemnites. All those objects have important information embedded in their patterned structure. Using microprobe type devices, one can disentangle the internal structure of the objects and reveal the hidden information. This information can be of great significance to climatic, geological, chronological, and ecological studies and specific examples in each category are shown, taken from our work and compared with the results of other authors where necessary. The added value of the X-ray and electron microprobe measurements in relation to the mass-spectrometric methods is shown for the specific cases. In addition, the results concern materials where organic and even biological material is combined with inorganic matter, like calcite, silica varieties and metal oxides. The investigation of such patterned objects as goethitized wood, composed of goethite, calcite and organic matter should therefore be of interest to materials scientists, synthesizing composite materials.

Z. Šmit, K. Janssens, O. Schalm, et M. Kos. Spread of façon-de-Venise glassmaking through central and western Europe. Nucl. Instrum. Methods B, 213:717-722, 2004. [ doi ]

The major and trace composition of a series of 16th century glass fragments, originating from the ruins of different 15-17th century castle sites in the neighborhood of Ljubljana (Slovenia) was determined. The resulting compositions are compared to those obtained from archaeological glass finds originating from Ljubljana city center, Antwerp (Belgium) and Venice (Italy). In these urban centers, historic documents describe the existence of a flourishing glass making and working industry in the 16th century. Electron probe X-ray microanalysis (EPXMA) combined with microscopic synchrotron induced X-ray fluorescence (-SRXRF) was used to analyze the glasses from the Slovenian castles and from Antwerp while ion beam analysis (proton induced X-ray and -emission PIXE/PIGE) was used for the Ljubljana samples. A comparison of the major glass compositions of the latter glass samples obtained by means of EPMA and the ion beam methods revealed that the differences between the two sets of data are generally smaller than 10%, except in the case of concentrations smaller than 1% w/w where typical values of 20% of relative deviation are encountered. In contrast to Antwerp, where both local and Venetian glass compositions are encountered, the Ljubljana and Slovenian castle glasses feature a composition that closely resembles that of Venetian vitrum blanchum glass.

D. C. Creagh et V. Otieno-Alego. The use of radiation for the study of material of cultural heritage significance. Nucl. Instrum. Methods B, 213:670-676, January 2004. [ doi ]

For the indigenous people of Northern Australia the expression of their experience of life, their 'dreaming', is in the form of painting, usually on the bark stripped from trees growing in their tribal lands. These are often works of great beauty and the major collecting institutions in Australia and elsewhere have significant holdings of Aboriginal bark paintings. A wide range of analytical techniques (optical microscopy, FTIR microscopy, Raman microscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy, and synchrotron radiation X-ray diffraction) has been used in a project to determine how best to conserve Aboriginal bark paintings. (C) 2003 Elsevier B.V. All rights reserved.

T. Broekmans, A. Adriaens, et E. Pantos. Analytical Investigations of Cooking Pottery From Tell Beydar (NE-Syria). Nucl. Instrum. Methods B, 226:92-7, 2004. [ doi ]

Within the framework of a technological and socio-economical study of pottery production in Tell Beydar (NESyria) during the third millennium BC, the chemical composition and mineralogy of cooking pottery from that site has been studied using polarizing microscopy, scanning electron microscopy with energy dispersive X-ray detection (SEMEDX) and X-ray diffraction by means of synchrotron radiation (SR-XRD). The obtained data were used to make inferences concerning the pottery's technology, such as clay preparation and firing techniques.

M. L. Carvalho, J. P. Marques, A. F. Marques, et C. Casaca. Synchrotron microprobe determination of the elemental distribution in human teeth of the Neolithic period. X-ray Spectrom., 33(1):55-60, 2004. [ doi ]

The purpose of the present work was to investigate whether the distribution of trace elements in human teeth of the Neolithic period in Portugal can reflect environmental conditions, dietary habits and uptake of some elements from the surrounding soil. An X-ray fluorescence set-up with microprobe capabilities, installed at the LURE synchrotron (France), was used for elemental analysis of teeth. The resolution of the synchrotron microprobe was 100 mum and the energy of the incident beam was 18 keV. The synchrotron microprobe concentration profiles for V, Mn, Fe, Cu, Zn, Sr and Pb in different regions of the tooth are discussed and correlated with the results obtained by cranio-facial studies. The Mn and Fe concentrations were much higher in Neolithic teeth than in those of present humans. This may suggest uptake of both elements from the soil. Low concentration levels of Sr were found, which can be correlated with dietary habits. Moreover, the Pb concentration was very low in all the teeth analysed, in agreement with the low pollution levels of this element in this population. All samples were analysed without any chemical preparation. Copyright (C) 2004 John Wiley Sons, Ltd.

E. Pantos, A. D. Smith, I. W. Kirkman, T. Pradell, N. Salvadó, J. Molera, M. Vendrell, E. Gliozzo, I. Memmi-Turbanti, L. Burgio, G. Martin, W. Kockelmann, et A. J. N. W. Prag. Synchrotron radiation and neutrons in archaeological and cultural heritage science. Dans M. Martini, M. Milazzo, et M. Piacentini, éds, Physics methods in archaeometry, Proc. of the International School of Physics Enrico Fermi, Varenna, Italy, p. 299-308. Società Italiana di Fisica, 2004.

I. Reiche, M. Radtke, A. Berger, W. Görner, T. Ketelsen, S. Merchel, J. Riederer, H. Riesemeier, et M. Roth. Spatially resolved Synchrotron-induced X-ray fluorescence analyses of metal point drawings and their mysterious inscriptions. Spectrochim. Acta B, 59:1657-1662, 2004. [ doi ]

Synchrotron-induced X-ray fluorescence (Sy-XRF) analysis was used to study the chemical composition of precious Renaissance silverpoint drawings. Drawings by famous artists such as Albrecht Dürer (1471-1528) and Jan van Eyck (approximately 1395-1441) must be investigated non-destructively. Moreover, extremely sensitive synchrotron- or accelerator-based techniques are needed since only small quantities of silver are deposited on the paper. New criteria for attributing these works to a particular artist could be established based on the analysis of the chemical composition of the metal points used. We illustrate how analysis can give new art historical information by means of two case studies. Two particular drawings, one of Albrecht Dürer, showing a profile portrait of his closest friend, “Willibald Pirckheimer” (1503), and a second one attributed to Jan van Eyck, showing a “Portrait of an elderly man”, often named “Niccolò Albergati”, are the object of intense art historical controversy. Both drawings show inscriptions next to the figures. Analyses by Sy-XRF could reveal the same kind of silverpoint for the Pirckheimer portrait and its mysterious Greek inscription, contrary to the drawing by Van Eyck where at least three different metal points were applied. Two different types of silver marks were found in this portrait. Silver containing gold marks were detected in the inscriptions and over-subscriptions. This is the first evidence of the use of gold points for metal point drawings in the Middle Ages.

L. Cheng, S. L. Feng, Q. Xu, Y. Y. Huang, W. He, et Z. R. Lu. Colored glaze from Shanxi province sudied by SRXRF and multivariable statistical analysis. High Energy Phys. Nucl. Phys., 27:97-100, December 2003.

The major and trace elements in the bodies and glazes of ancient colored glazes were determined by Synchrotron Radiation X-ray Fluorescence (SRXRF). The ancient colored glazes were unearthed from the stratums of Song, Yuan, Ming, Early Qing and Late Qing dynasty in Shanxi province. Multivariable statistical analysis of the experimental data were carried out by SPSS software. The result indicate the chemical compositions in the bodies are stable in samples from Song to Early Qing dynasty, but have distinctly difference from that of Late Qing dynasty. Those results are consistent with the conclusion by INAA method. The primary colored elements are Fe, Cu and Co for these samples. The colors variety of glazes are due to the change of those three elements concentrations.

D. Y. Fan, S. L. Feng, Q. Xu, Y. Lei, X. Q. Feng, L. Cheng, Y. Y. Huang, W. He, K. S. Quan, et Y. M. Shen. Non-destructive analysis of glaze elemental constitute of Zhejiang Yue kiln celadon. High Energy Phys. Nucl. Phys., 27:101-104, December 2003.

The ancient celadon that made in the period front Late Tang Dynasty to Southern Song Dynasty (900-1200 A.D.) were excavated in Yue kiln, Zhejiang province of China. This paper studied elemental constitute of Yue kiln glaze by synchrotron radiation X-ray fluorescence (SRXRF) with non-destructive analysis. The feasibility of non-destructive analysis method was also discussed. We analyzed ancient celadon samples of 6 cultural periods that produced from Yue kiln of Si Long Kou, the celadon of He Hua Xin kiln where is about 5 km to Si Long Kou kiln were used to contrast the provenance performance. The statistical analysis of elemental abundances indicated that most of celadon samples belong to their corresponding production age, which evidently reflects the Yue kiln characteristics. There was age correlation among the ancient celadon of special cultural period.

K. Stahl, K. Nielsen, J. Jiang, B. Lebech, J. C. Hanson, P. Norby, et J. van Lanschot. On the akaganeite crystal structure, phase transformations and possible role in post-excavational corrosion of iron artifacts. Corrosion Sci., 45(11):2563-2575, November 2003. [ doi ]

The crystal structure of akaganéite and the akaganéite to hematite transition has been studied by means of conventional and synchrotron X-ray and neutron powder diffraction. The chemical formula of akaganéite can be written as FeO0.833(OH)1.167Cl0.167. The crystal structure does not contain free water. Heating below 200 degree C will not alter the akaganéite structure. Initial water loss can be attributed to a large amount of adsorbed water due to a very small particle size; 0.15 μm by 0.03 μm. Chloride is released from the structure only in connection with the transformation to hematite. Due to its stability, the presence of akaganéite does not in itself posses a threat to iron artifacts, but it is rather a symptom of the presence of high concentrations of chloride in an acidic environment.

B. Kanngiesser, W. Malzer, et I. Reiche. A new 3D micro X-ray fluorescence analysis set-up - First archaeometric applications. Nucl. Instrum. Methods B, 211:259-264, October 2003. [ doi ]

A new 3D micro X-ray fluorescence (micro-XRF) analysis method based on a confocal X-ray set-up is presented. The capabilities of this new method are evaluated and illustrated with depth sensitive investigations of paint layers in ancient Indian Mughal miniatures. Successive paint layers could be distinguished non-destructively with a depth resolution of about 10 mum. Major and minor elements are detectable and can be discriminated in different layers. New light could be shed on ancient painting techniques and materials with this new 3D micro-XRF set-up.

L. Bertrand, J. Doucet, P. Dumas, A. Simionovici, G. Tsoucaris, et P. Walter. Microbeam synchrotron imaging of hairs from Ancient Egyptian mummies. J. Synchrotron Radiat., 10(5):387-392, September 2003. [ doi ]

Developments in microfocus synchrotron techniques have led to new results regarding the long-term alteration of archaeological samples of biological origin. Here, ancient hair samples from two Egyptian mummies have been analyzed using a conjunction of structural and elemental synchrotron methods. In this favored context of conservation, structural analysis revealed a remarkable preservation of keratin supramolecular organization at any observed length scale. Bulk keratin structure has therefore not been modified significantly over 2000 years. However, infrared spectroscopy indicated a partial disorganization of keratins close to the hair surface through polypeptide bond breakage. Elemental mapping showed a strongly heterogeneous distribution which can be related to mummification and cosmetic treatments.

P. Walter. Molecular and structural archaeology: cosmetic and therapeutic chemicals, chap. Inventing a science of makeup, p. 1-9. Vol. 117 de Tsoucaris et Lipkowski [ .ref ], September 2003.

T. Ungár, P. Martinetto, G. Ribárik, É. Dooryhée, P. Walter, et M. Anne. Molecular and structural archaeology: cosmetic and therapeutic chemicals, chap. Microstructure determined by X-ray diffraction peak profile analysis, p. 211-220. Vol. 117 de Tsoucaris et Lipkowski [ .ref ], September 2003.

G. Tsoucaris, L. Bertrand, et P. Walter. Is supramolecular organisation a key factor for long term preservation? Dans G. Tsoucaris et J. Lipkowski, éds, Molecular and structural archaeology: cosmetic and therapeutic chemicals, vol. 117, p. 135-156. Kluwer Academic Publishers, September 2003.

E. Pantos, N. Salvadó, T. Pradell, J. Molera, M. Vendrell, A. D. Smith, I. W. Kirkman, M. Marcus, E. Gliozzo, et I. Memmi-Turbanti. Molecular and structural archaeology: cosmetic and therapeutic chemicals, chap. SR-based molecular speciation of archaeomaterials, p. 221-9. Vol. 117 de Tsoucaris et Lipkowski [ .ref ], September 2003.

Examples are presented of the use of SR modalities for the molecular characterisation of archaeomaterials. They focus on the utilisation of the most basic of synchrotron radiation properties, high brilliance and energy range that can be selected. Two techniques have been employed, X-ray diffraction and X-ray absorption spectroscopy, to characterise the mineral composition of painting pigments and pottery glazes.

P. Martinetto, M. Anne, É. Dooryhée, O. Isnard, et P. Walter. Molecular and structural archaeology: cosmetic and therapeutic chemicals, chap. A non-destructive analysis by neutron diffraction inside make-up containers of ancient Egypt, p. 107-111. Vol. 117 de Tsoucaris et Lipkowski [ .ref ], September 2003.

K. Janssens, K. Proost, I. Deraedt, E. Bulska, B. Wagner, et M. Schreiner. Molecular and structural archaeology: cosmetic and therapeutic chemicals, chap. The use of focussed X-ray beams for non-destructive characterisation of historical materials, p. 193-200. Vol. 117 de Tsoucaris et Lipkowski [ .ref ], September 2003.

In this work, the use of X-ray micro beams for non-destructive characterization of historical, archaeological and artistic materials will be described. Only the use of X-ray micro beams generated in dedicated beam lines of synchrotron storage will be discussed. Attention will be devoted to two methods of analysis: μ-XRF (X-ray fluorescence analysis) [1] and μ-XANES (X-ray absorption near-edge spectroscopy) [2]. The former method allows quantitative trace-level micro-analysis of a variety of materials while the second permits to extract information on the valence of (trace) metals in these materials. μ-XRF may be practised at synchrotron beam lines, where the polarized nature of the radiation can be used advantageously for lowering the scatter background level in the energy-dispersive X-ray spectra, leading to improved detection limits. When suitable focussing devices are employed, μ-XRF measurements can also be performed by means of compact and/or portable laboratory equipment. The latter kind of instrumentation allows for in-situ measurements (for example in a gallery, a museum etc.). In view of the requirement to employ highly monochromatic radiation, μXANES is a method that only can be employed at synchrotron facilities. The use of these methods for characterization of historical glass fragments and handwritten paper documents is briefly described.

J. Doucet. Molecular and structural archaeology: cosmetic and therapeutic chemicals, chap. New synchrotron radiation-based imaging techniques and archaeology, p. 179-192. Vol. 117 de Tsoucaris et Lipkowski [ .ref ], September 2003.

The recent emergence of synchrotron radiation-based micro-analytical techniques, like microdiffraction, microfluorescence, micro-XANES, microtomography, X-ray microscopy or IR microspectrometry, has opened extremely valuable new capabilities in the domain of material characterisation. The possibility of collecting selective images at the micrometer resolution is very attractive for looking at very small objects as well as for mapping heterogenous zones for all types of materials. The images are generally obtained in scanning mode, but sometimes also in full-field mode (X-ray microscopy). Also highly appreciated by scientists is the possibility of combining these techniques, for example tomography and fluorescence, or to successively obtain a series of images provided by these complementary techniques. The new radiation synchrotron-based imaging techniques are already exploited in archaeological investigation, for identifying pigments in paintings or ceramics. They could be also very helpful for characterising the microstructure of archeological tissues like hair, skin and bones, and thus provide physiological, pharmaceutical, medical or embalming information. The present paper is mainly dedicated to the archaeological tissues, the capabilities of synchrotron radiation-based techniques for other types of materials described in other papers of this issue.

É. Dooryhée. Molecular and structural archaeology: cosmetic and therapeutic chemicals, chap. Advances in art and archaeology using X-ray synchrotron radiation, p. 201-209. Vol. 117 de Tsoucaris et Lipkowski [ .ref ], September 2003.

L. Burgio, R. J. H. Clark, G. Martin, E. Pantos, et M. A. Roberts. Molecular and structural archaeology: cosmetic and therapeutic chemicals, chap. A multidisciplinary approach to pigment analysis: king's yellow and dragon's blood from the Winsor and Newton pigment box at the Victoria and Albert Museum, p. 61-72. Vol. 117 de Tsoucaris et Lipkowski [ .ref ], September 2003.

A 19th century box of unused watercolour pigment cakes, manufactured by Winsor and Newton and currently at the Victoria and Albert Museum, was analysed using several techniques. The box and its contents are in remarkably good condition, with most of the watercolour cakes being still intact; thus a unique opportunity was made available to study unadulterated artists' materials. Two interesting results obtained by using Raman microscopy and synchrotron radiation X-ray diffraction are reported here for the pigment cakes labelled king's yellow and dragon's blood.

G. Tsoucaris et J. Lipkowski, éds. Molecular and structural archaeology: cosmetic and therapeutic chemicals, vol. 117. Kluwer Academic Publishers, September 2003.

I. De Ryck, A. Adriaens, E. Pantos, et F. Adams. A comparison of microbeam techniques for the analysis of corroded ancient bronze objects. Analyst, 128(8):1104-1109, August 2003. [ doi ]

This paper describes the use of several microbeam analysis techniques for the chemical characterization of corrosion compounds on ancient bronze objects. They include optical microscopy, SEM-EDX, TOF-SIMS, SR-FTIR, SR-XRD, and XANES. The objective is to investigate which combination of analysis methods is most suitable for this type of application, taking into account aspects such as limited sampling and the ability of obtaining spatial information. Results show that SR-XRD in combination with optical microscopy and SEM-EDX is able to provide a complete description of the layered structure both on elemental and molecular level.

I. Reiche, M. Radtke, et C. Brouder. Antike Gläser und versteinertes Elfenbein. Phys. Unserer Zeit, 34(2):80-86, March 2003. [ doi ]

Physikalische Methoden der Archäometrie liefern den Kunsthistorikern und Archäologen wichtige Informationen. Materialspezifische Größen geben Aufschluss über Alter, Authentizität, Herkunft und Herstellungstechniken sowie Alterserscheinungen von Gegenständen. Insbesondere die Röntgenanalyse hat in jüngster Zeit wertvolle Beiträge hierzu geliefert. Dabei spannt sich ein weiter Bogen von den Mysterien ägyptischer Augenschminke über die Herstellungstechnik römischer Gläser bis zur Authentizitätsuntersuchung mittelalterlicher Silberstiftzeichnungen.

Y. Chaimanee, D. Jolly, M. Benammi, P. Tafforeau, D. Duzer, I. Moussa, et J.-J. Jaeger. A Middle Miocene hominoid from Thailand and orangutan origins. Nature, 422:61-65, March 2003. [ doi ]

L. Bertrand, G. Tsoucaris, et P. Walter. Étude de cheveux de momies égyptiennes par rayonnement synchrotron. Dans C. Leblanc, éd., Memnonia cahier supplémentaire 1, Parfums, onguents et cosmétiques dans l'Égypte ancienne, p. 21-28. Association pour la sauvegarde du Ramesseum, Le Caire, 2003.

G. D. Smith. Infrared microspectroscopy using a synchrotron source for arts-science research. J. Am. Inst. Conservation, 42(3):399-+, Fall-Winter 2003.

The nature of radiation from synchrotron storage rings is discussed with emphasis on the advantages, in particular that of brightness, that this light source offers when replacing the thermal source typically employed in a conventional infrared microscope. Specifically, synchrotron radiation allows the collection of high signal-to-noise ratio infrared spectra with diffraction-limited spatial resolution across the entire near-, mid-, and far-infrared spectral range. This level of performance permits the spatially resolved analysis of microscopic samples from artwork and artifacts down to similar to 4 mu m in the mid-infrared spectral region and potentially much smaller dimensions, for both organic and inorganic components. Conservation and archaeological scientists are alerted to the worldwide availability of these microscopy facilities for occasional use by museums and galleries free of charge.

B. L. Illman. Synchrotron applications in wood preservation and deterioration, vol. 845, chap. 19, p. 337-345. American Chemical Society, Washington, DC, USA, 2003.

Several non-intrusive synchrotron techniques are being used to detect and study wood decay. The techniques use high intensity synchrotron-generated X-rays to determine the atomic structure of materials with imaging, diffraction, and absorption. Some of the techniques are X-ray absorption near edge structure (XANES), X-ray fluorescence spectroscopy (XFS), X-ray absorption fine structure (EXAFS), and X-ray computed microtomography (XCMT). Micro-fluorescence spectroscopy was used to map the accumulation and spatial distribution of elements around hyphae at the site of decay. MicroXANES determined the valence states of metals, such as manganese and iron, during fungal colonization of wood. Microtomography was used to characterize loss of wood structural integrity. The techniques are providing information about molecular structures and compositions in the heterogeneous matrix of wood. Nondestructive methods are needed to analyze the chemistry and internal structures of wood without disturbing spatial integrity or producing structural artifacts. The methods are needed to study wood during attack by decay fungi and wood treatment with preservatives. To meet this need, we have successfully studied several systems using the X-ray facilities at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory (BNL), Upton, NY. Chemical mechanisms of fungal wood decay are dependent on transition metal redox reactions producing free radicals. Synchrotron methods are uniquely suited to detect and image metal oxidation states as probes of the decay process. The same methods have been applied to study metal-based preservatives that undergo redox reactions during fixation of wood. These methods include X-ray absorption near edge structure (XANES), X-ray fluorescence spectroscopy (XFS), extended X-ray absorption fine structure (EXAFS), and X-ray computed microtomography (XCMT). In addition to decay and preservation studies, the XCMT method has also proven to be invaluable as a tool to analyze insects and fungi that cause major diseases of forests worldwide. Microtomography was employed to study beetle structure and function, to locate fungal spores on or in beetles, to assist in identification of fungi, and to provide images depicting spatial relationships of tree-insect-fungi.

S. Gerlach, H. Römich, E. Lopéz, F. Zanini, L. Mancini, et L. Rigon. Phase contrast microtomography of archaeological glasses. Elettra Res. Highlights, 2003.

J.-L. Boutaine. Techniques de spectrométrie X et gamma appliquées à la caractérisation et l'analyse des oeuvres du patrimoine culturel. Bull. Bureau Natl Métrologie, 123:91-99, 2003.

Pour l'examen, la caractérisation et l'analyse des oeuvres d'art ou du patrimoine culturel, des matériaux constitutifs de ces oeuvres, les scientifiques de la conservation ont besoin de disposer d'une palette de méthodes non-destructives, afin de connaître les mécanismes de leur élaboration, de leur évolution / dégradation au cours du temps et d'établir des recommandations en vue de leur restauration et / ou de leur conservation. Parmi ces méthodes, celles mettant en oeuvre les rayonnements ionisants ont un rôle important. Citons : - la radiographie (<beta>, X, électrons secondaires, <gamma>, neutrons), l'émissiographie, la tomodensimètre - la diffraction X - la caractérisation à l'aide du rayonnement synchrotron - la microscopie électronique à balayage (MEB) et analyse par spectrométrie X associee - l'analyse par fluorescence X - l'analyse par activation - l'analyse par faisceaux d'ions: PIXE, PIGE, RBS et fluorescence X secondaire - la datation par thermoluminescence - la datation par mesure de la composition isotopique en carbone 14 Ces méthodes, seules ou associees à d'autres méthodes sont appliquees à des oeuvres tres diverses et des matériaux de toute nature, de toute origine et de tout age. On illustrera ces techniques par des exemples récents d'études d'objets réalisées au C2RMF. Ceci démontrera le type d'assistance que ces techniques peuvent apporter à une meilleure connaissance du patrimoine culturel de l'humanité et aussi à l'établissement de base rationnelle pour leur meilleure conservation pour les générations futures.

B. Hochleitner, M. Schreiner, M. Drakopoulos, I. Snigireva, et A. Snigirev. Analysis of paint layers by light microscopy, scanning electron microscopy and synchrotron induced x-ray micro-diffraction. Dans Proc. Conf. Art 2002, June 2003, Antwerp, Belgium, 2003.

M. Sandström, F. Jalilehvand, I. Persson, Y. Fors, E. Damian, U. Gelius, I. Hall-Roth, L. Dal, V. L. Richard, et I. Godfrey. Conservation Science 2002, p. 79-87. Archetype Books, London, UK, 2003.

M. Sandström, Y. Fors, et I. Persson. The Vasa's new battle: sulfur, acid and iron. Dans Vasa studies, vol. 19. The Vasa Museum, Stockholm, Sweden, 2003.

M. L. Carvalho, A. F. Marques, et J. Brito. Synchrotron radiation and energy dispersive X-Ray fluorescence applications on elemental distribution in human hair and bones. Dans A. Bianconi, A. Marcelli, et N. L. Saini, éds, X-Ray and inner-shell processes, AIP Conf. Proc., vol. 652, p. 522-528. AMER INST PHYSICS, January 2003. [ doi ]

This work is an application of synchrotron microprobe X-Ray fluorescence in order to study elemental distribution along human hair samples of contemporary citizens. Furthermore, X-Ray fluorescence spectrometry is also used to analyse human bones of different historical periods: Neolithic and contemporary subjects. The elemental content in the bones allowed us to conclude about environmental contamination, dietary habits and health status influence in the corresponding citizens. All samples were collected post-mortem. Quantitative analysis was performed for Mn, Fe, Co, Ni, Cu, Zn, Br, Rb, Sr and Pb. Mn and Fe concentration were much higher in bones from pre- historic periods. On the contrary, Pb bone concentrations of contemporary subjects are much higher than in pre-historical ones, reaching 100 mug g-1, in some cases. Very low concentrations for Co, Ni, Br and Rb were found in all the analysed samples. Cu concentrations, allows to distinguish Chalcolithic bones from the Neolithic ones. The distribution of trace elements along human hair was studied for Pb and the obtained pattern was consistent with the theoretical model, based on the diffusion of this element from the root and along the hair. Therefore, the higher concentrations in hair for Pb of contemporary individuals were also observed in the bones of citizens of the same sampling sites. All samples were analysed directly without any chemical treatment.

F. Quinn, N. Poolton, A. Malins, E. Pantos, C. Andersen, P. Denby, V. Dhanak, et G. Miller. The Mobile Luminescence End-Station, MoLES: a new public facility at Daresbury synchrotron. J. Synchrotron Radiat., 10:461-466, 2003. [ doi ]

A new mobile end-station is described for use on multiple beamlines at the Daresbury synchrotron radiation source (overall excitation range 5 eV to 70 keV) that allows for the detection and dispersion of photoluminescence from solid-state samples in the emission range 190-1000 nm (1.2-6.5 eV). The system is fully self-contained and includes sample-cooling facilities for the temperature range 8-330 K using a closed-cycle refrigerator, thus eliminating the need for liquid cryogens. The system also includes solid-state laser sources for use with a variety of pump-probe-type experiments, and an Ar+ surface-cleaning facility. In order to demonstrate the various capabilities of the system, the results of a variety of experiments are summarized, carried out over the excitation range 5-5000 eV on beamlines 3.2, MPW6.1 and 4.2. These include the optical detection of XAS ofL-edge structure in natural minerals and archaeological ceramics, band-gap determinations of wide-band-gap silicates, and pump-probe studies of quartz.

G. Chiari, R. Giustetto, et G. Ricchiardi. Crystal structure refinements of palygorskite and Maya Blue from molecular modelling and powder synchrotron diffraction. Eur. J. Mineral., 15(1):21-33, 2003. [ doi ]

Maya Blue, a synthetic pigment produced by the ancient Mayas, is a combination of a specific clay, palygorskite (or sepiolite), containing large channels in the crystal structure and the organic dye indigo. Little is known about the interaction of the two components to give the most stable pigment ever produced. The aim of this work is to obtain a refined model for the Mexican palygorskite used to prepare the pigment and to elucidate the structure of the clay-indigo complex, using both molecular modelling and Rietveld refinement on data collected with synchrotron radiation. Molecular modelling proved that indigo can fit into the channels without steric impediment (forming strong hydrogen bonds between the C=O group of the dye and the structural water of the clay) and produced a model, showing reasonable distances and angles, used as the starting set for the Rietveld refinement. Difference Fourier maps, calculated without indigo, showed a residual of electron density coherent with the expected disordered position of the indigo molecule. A refinement carried out using the model of palygorskite obtained in this work and a 6-fold disordered arrangement of indigo confirmed these findings. The ratio between the two polymorphs of palygorskite (monoclinic and orthorhombic) present in the natural clay was obtained for our sample and for several palygorskite specimens coming from different sites. Samples within the same outcrop show similar ratios, while samples from different locations do not. This may be used to characterize the provenance of ancient specimens, with the goal of determining whether Maya Blue was invented and produced in one place only or if the production technology was widespread in all the Mayan region.

S. Padovani, C. Sada, P. Mazzoldi, B. Brunetti, I. Borgia, A. Sgamellotti, A. Giulivi, F. D'Acapito, et G. Battaglin. Copper in glazes of Renaissance luster pottery: Nanoparticles, ions, and local environment. J. Appl. Phys., 93(12):10058-10063, 2003. [ doi ]

Following the recent finding that luster decorations in glazes of historical pottery consist of copper and silver nanoparticles dispersed in a glassy medium, the glaze in-depth composition and distribution of copper nanoparticles, copper ions, and their local environment have been studied in original samples of gold and red luster. The study has been fully carried out by nondestructive techniques such as Rutherford backscattering spectrometry, ultraviolet and visible spectroscopy, X-ray fluorescence, and extended X-ray absorption fine structure (EXAFS). Elemental analyses indicate that gold decorations are characterized by silver and copper, while red decorations by copper only. The color is determined mainly by metal nanoparticles. Specifically, silver nanoparticles determine the gold color, while the red color is determined by nanoparticles of copper. EXAFS measurements, carried out at the Cu K edge, indicate that in both gold and red luster copper is mostly the oxidized form (Cu+ and Cu2+) with a large prevalence of Cu+. States and local environment of copper ions are similar to those found in copper-alkali ion-exchanged silicate glass samples. This strongly supports the view that luster formation is mediated by a copperand silver-alkali ion exchange as a first step, followed by nucleation and growth of metal nanoparticles. (C) 2003 American Institute of Physics.

A. D. Smith, T. Pradell, J. Molera, M. Vendrell, M. A. Marcus, et E. Pantos. MicroEXAFS study into the oxidation states of copper coloured Hispano-Moresque lustre decorations. J. Phys. France IV, 104:519-522, 2003. [ doi ]

Lustreware is a traditional decorative finish applied to ceramics, giving a copper-gold metallic finish. Following an Islamic tradition, it was a highly prized luxury finish that was exported throughout the Mediterranean in medieval times. The technology required to produce the highly desired artifacts was the province of highly skilled artisans, that it was also non-trivial is evidenced by the slow development of rival production centres elsewhere and the large proportion of fragments from failed production runs found at the established centres. We have used the MicroEXAFS facility on Beamline 10.3.2 at the ALS to determine the spatial distributions of the Cu oxidation states both within areas of a constant colour and in different coloured specimens. Fluorescence microXAFS is an important technique and has enabled us to penetrate the predominately Al and Si surface layer (of the order of 100Angstrom - 200 Angstrom thick) to probe the metal glaze beneath.

M. F. Araujo, T. Pinheiro, P. Valério, A. Barreiros, A. Simionovici, S. Bohic, et A. Melo. Analysis of a roman Centaurus from Canas de Senhorim (Portugal) - Comparative study using EDXRF and SXRF. J. Phys. France IV, 104:523-526, 2003. [ doi ]

A decoration figure of a ritual bronze vase from Canas de Senhorim (Portugal) was analysed by Energy Dispersive X-ray Fluorescence (EDXRF) spectrometry and Synchrotron induced X-ray Fluorescence (SXRF) microprobe spectrometry. This artefact, a Centaurus constitutes the first evidence for a possible Roman occupation of this region of Central Portugal and it is also one of the very few artefacts of this type ever found. The determination of the Centaurus alloy composition will be important in the further comprehension of the metallurgical technologies used by the Romans in this region. EDXRF analysis of the corroded surface were made using the monochromatic radiation emitted by Ag and Gd secondary targets excited by a Rh X-ray tube at 35kV and 57 W, respectively. SXRF experiments were carried out both on the corroded surface and on a small clean area of the artefact, using both monochromatic and polychromatic excitations with 32 keV and 12 keV radiations. EDXRF results allowed the determination of the alloy bulk composition. The SXRF comparative analysis between the clean and corroded areas evidences the surface enrichment in Sn and establishes the composition of the original alloy. The Centaurus alloy is a bronze with rather high Ph content, which is characteristic of the Roman decorative artefacts.

Y. F. Hsia, H. Huang, et A. M. Ali. Mössbauer spectroscopy in China. J. Radioanal. Nucl. Chem., 255:37-45, 2003. [ doi ]

Mössbauer spectroscopy is a dynamic field with applications ranging from physics to biology. This paper gives a review of Mössbauer spectroscopy activities carried out by different groups in China. About thirty groups are distributed all over China for both fundamental and practical aspects. In-beam Mössbauer setup was established at HIRAC accelerator in Lanzhou, and the nuclear scattering facility has already been planned at Shanghai Synchrotron Radiation Light Source. In this review, some recent developments and achievements are discussed, as examples: (1) Brownian motion in anisotropic media, (2) applications to archaeology, and (3) molecule-based magnetic materials.

A. Denker, O. Hahn, B. Kanngiesser, W. Malzer, S. Merchel, M. Radtke, et S. Röhrs. Chemie der Kunst. Zerstörungsfreie Analyse von Kunst- une Kulturgütern. Materialprufung, 45(11-12):485-503, 2003.

Chemistry of arts - Non-destructive analysis of artistic and cultural heritage objects. Scientific analysis, especially the chemical composition, of artistic and cultural heritage objects reveals information, which cannot be gained from art historical investigations alone. The improvement of X-ray analytical method, like X-ray fluorescence (XRF) analysis and Particle-Induced X-ray Emission (PIXE) analysis, makes it possible to investigate even fragile and very precious objects non-destructively. In principle, two strategies are generally embarked: First, very sophisticated set-ups using particle accelerators or synchrotron-radiation sources for very sensitive or highly spatially-resolved and depth-sensitive analysis. Second, portable instrumentation for in-situ measurements at archaeological excavations, museums and collections. Highlights of investigated objects are limoges school enamels, manuscripts of Goethe and Schiller, the sceptre of Charlemagne, medieval metal objects, silverpoint drawings from the Renaissance, and Indian Mughal paintings.

M. Müller, M. Z. Papiz, D. T. Clarke, M. A. Roberts, B. M. Murphy, M. Burghammer, C. Riekel, E. Pantos, et J. Gunneweg. Identification of textiles from the Khirbet Qumran caves using microscopy and synchrotron radiation X-ray fibre diffraction, chap. 12, p. 177-188. Academic Press, Fribourg, Switzerland, 2003.

I. Reiche, G. Morin, C. Brouder, V. A. Solé, P.-E. Petit, C. Vignaud, T. Calligaro, et M. Menu. Manganese accommodation in fossilised mastodon ivory and heat-induced colour transformation: Evidence by EXAFS. Eur. J. Mineral., 14(6):1069-1073, December 2002. [ doi ]

Odontolite or bone turquoise, a turquoise-blue coloured heated fossilised mastodon ivory or bone, is an imitation of the mineral turquoise used for the decoration of medieval art objects. Its colour origin can be ascribed to Mn5+ traces in a tetrahedral environment of four oxygen atoms in an apatite matrix. The structural environment of Mn was investigated by means of extended X-ray absorption fine structure (EXAFS) in order to shed new light on the colour transformation of fossilised ivory induced by a thermal treatment. This was particularly difficult as the manganese concentration does not exceed trace amounts in fossilised ivory. EXAFS experiments confirm the presence of Mntextsuperscript2+/3+/4+ ions before and Mn5+ ions after thermal treatment in fossilised ivory and the location of Mntextsuperscript5+ ions on a P analogous site in apatite.

M. I. Cooper, P. S. Fowles, et C. C. Tang. Analysis of the laser-induced discoloration of lead white pigment. Appl. Surf. Sci., 201(1-4):75-84, November 2002. [ doi ]

The use of laser cleaning in artwork conservation is becoming increasingly important. An investigation into the effects of laser radiation on lead white pigment, considered to be historically the most important of all white pigments used in art, has been undertaken. Samples of pigment and pigment in a water-colour binding medium have been prepared and irradiated by laser radiation at 1064 mn (pulse duration 5-10 ns) at an average fluence of 0.3 J cm(-2). Irradiation under such conditions leads to the formation of an extremely thin discoloured layer. Synchrotron X-ray diffraction (XRD) and Xray photoelectron spectroscopy (XPS) have been used to characterise the altered layer. Analytical evidence for the formation of elemental lead is presented for the first time and the effect of exposure of the altered layer to air and the effect of a binding medium on the process are discussed. (C) 2002 Elsevier Science B.V. All rights reserved.

P. Dillmann, R. Balasubramaniam, et G. Béranger. Characterization of protective rust on ancient Indian iron using microprobe analyses. Corrosion Sci., 44(10):2231-2242, October 2002. [ doi ]

Local compositional and structural information was obtained from an ancient 1500-year old Indian iron and its protective scale utilizing microprobe techniques (lXRD and lPIXE). Different locations in the iron matrix and in the entrapped slag inclusions were also analyzed for P contents. The P content of the metallic iron matrix was very heterogeneous. Lower P contents were observed in the regions near slag inclusions. The surface oxide scales was layered. Enrichment of P in the metal-scale interface and in the scale adjacent to the interface was determined. The P content in the scale decreased on moving away from the interface. Microdiffraction patterns obtained at different locations in the oxide scale indicated that at locations where the P content was high (i.e. nearer the interface), the oxide was amorphous while at locations where P was low, crystalline phases were identified. The presence of crystalline phosphates was also confirmed at some regions in the scale, where the P content was relatively very high. The probable reasons for the presence of the identified phases in the atmospheric corrosion product have been discussed.

S. Quartieri, M. Triscari, G. Sabatino, F. Boscherini, et A. Sani. Fe and MnK-edge XANES study of ancient Roman glasses. Eur. J. Mineral., 14(4):749-756, August 2002. [ doi ]

The X-ray Absorption Near Edge Structure technique has been successfully applied to the study of ancient glasses from Patti Roman Villa (Messina, Sicily). From the chemical point of view, the samples are 'low-magnesia' glasses, with a composition typical of the Roman period. Fluorescence detected Fe and Mn K- edge XANES spectra and a detailed pre-edge analysis confirm that the color of the class fragments depends on the oxidation state of iron and suggest the deliberate addition of manganese oxide as decolorant during the melting procedure. This work shows that X-ray Absorption Spectroscopy is a potentially very useful nondestructive technique that can be applied in archaeological studies on many different materials.

N. Salvadó, T. Pradell, E. Pantos, M. Z. Papiz, J. Molera, M. Seco, et M. Vendrell-Saz. Identification of copper-based green pigments in Jaume Huguet's Gothic altarpieces by Fourier transform infrared microspectroscopy and synchrotron radiation X-ray diffraction. J. Synchrotron Radiat., 9(4):215-222, July 2002. [ doi ]

The scientific investigation of ancient paintings gives a unique insight into ancient painting techniques and their evolution through time and geographic location. This study deals with the identification of the green pigments used by one of the most important Catalan masters in Gothic times, Jaume Huguet. Other pigments and materials have also been characterized by means of conventional techniques such as optical microscopy, scanning electron microscopy and Fourier transform infrared spectroscopy. Synchrotron radiation X-ray diffraction has been used to produce maps of phases at a spatial resolution of 100 mum across chromatic layers.

L. A. Polette, G. Meitzner, M. J. Yacaman, et R. R. Chianelli. Maya blue: application of XAS and HRTEM to materials science in art and archaeology. Microchem J., 71(2-3):167-174, April 2002. [ doi ]

Maya blue is a famous blue pigment composed of palygorskite clay and indigo. It was used by the ancient Maya and provides a dramatic background for some of the most impressive murals throughout Mesoamerica. Despite exposure to acids, alkalis, and chemical solvents, the color of the Maya blue pigment remains unaltered. Herein, we present studies on the role of iron in authentic and synthetic samples of Maya blue using X-ray absorption spectroscopy (XAS) and high-resolution transmission electron microscopy (HRTEM). Iron nanoparticles were found outside the lattice of the crystallites of palygorskite as well as inside the channels. Iron oxide and an amorphous phase of FeO(OH) were also found in authentic samples of Maya blue, and may contribute to the optical properties of the pigment or in the characteristic brilliant color. (C) 2002 Elsevier Science B.V. All rights reserved.

T. J. Wess, I. Alberts, J. Hiller, M. Drakopoulos, A. T. Chamberlain, et M. Collins. Microfocus small angle X-ray scattering reveals structural features in archaeological bone samples: Detection of changes in bone mineral habit and size. Calcif. Tissue Int., 70(2):103-110, February 2002. [ doi ]

Microfocus X-ray scattering provides a powerful nondestructive technique capable of providing important information about the size. habit, and arrangement of mineral crystals in bone. The technique is capable of probing textural differences in a sample at a micron scale resolution. The study presented here involved the analysis of a number of archaeological bones by microfocus X-ray, scattering at the ESRF Grenoble in order to determine local changes in mineral durability. The results showed that regions of bone with a modified microscopic morphology contained a greater dispersion of crystal shape when compared with more intact regions and control contemporary bone samples. but the crystal thickness values showed similar consistency. We speculate that the persistence of collagen in the archaeological bone may allow diagenetic remodeling of bone in terms of crystallite shape but defines the size of remodelled crystallites. The ability to detect such local changes in texture has wide potential for determining crystal characteristics in healthy and diseased bone samples.

T. Ungár, P. Martinetto, G. Ribárik, É. Dooryhée, P. Walter, et M. Anne. Revealing the powdering methods of black makeup in Ancient Egypt by fitting microstructure based Fourier coefficients to the whole X-ray diffraction profiles of galena. J. Appl. Phys., 91(4):2455-2465, February 2002. [ doi ]

Galena (PbS) is a major ingredient in ancient Egyptian eye makeup. The microstructure of PbS in Egyptian cosmetic powders is used as a fingerprint and is matched with the microstructures produced artificially in geological galena minerals. The microstructure of PbS is determined by X-ray diffraction peak profile analysis in terms of dislocation density, crystallite size, and size distribution. Highresolution powder diffractograms were measured at the ESRF Grenoble synchrotron source with high resolution and high peak- to-background ratios. The Fourier coefficients of the first nine measured reflections of galena are fitted using physically based Fourier coefficients of strain and size functions. Strain anisotropy is accounted for by the dislocation model of the mean square strain. The X-ray data are supplemented by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) micrographs, and are compared with archaeological documents. It enables us to describe the procedures of eye makeup manufacturing in the Middle and New Kingdoms of Egypt some 2000 years before Christ. (C) 2002 American Institute of Physics.

M. Sandström, F. Jalilehvand, I. Persson, U. Gelius, P. Frank, et I. Hall-Roth. Deterioration of the seventeenth-century warship Vasa by internal formation of sulphuric acid. Nature, 415(6874):893-897, February 2002. [ doi ]

The seventeenth-century Swedish warship, Vasa, was recovered in good condition after 333 years in the cold brackish water of Stockholm harbour. After extensive treatment to stabilize and dry the ship's timbers, the ship has been on display in the Vasa Museum since 1990. However, high acidity and a rapid spread of sulphate salts were recently observed on many wooden surfaces, which threaten the continued preservation of the Vasa. Here we show that, in addition to concentrations of sulphate mostly on the surface of oak beams, elemental sulphur has accumulated within the beams (0.2-4 per cent by mass), and also sulphur compounds of intermediate oxidation states exist. The overall quantity of elemental sulphur could produce up to 5,000 kg of sulphuric acid when fully oxidized. We suggest that the oxidation of the reduced sulphur-which probably originated from the penetration of hydrogen sulphide into the timbers as they were exposed to the anoxic water-is being catalysed by iron species released from the completely corroded original iron bolts, as well as from those inserted after salvage. Treatments to arrest acid wood hydrolysis of the Vasa and other wooden marine-archaeological artefacts should therefore focus on the removal of sulphur and iron compounds.

C. J. Kennedy et T. J. Wess.. The structure of collagen within parchment - a review. Restaurator-International Journal for the Preservation of library and Archival Material, 70:103-110, 2002.

S. Blau, B. J. Kennedy, et J. Y. Kim. An investigation of possible fluorosis in human dentition using synchrotron radiation. J. Archaeol. Sci., 29(8):811-817, 2002. [ doi ]

Macroscopic analysis of collections of archaeological human dentition from sites in the United Arab Emirates varying in chronological age and geographical location revealed the presence of enamel defects on the buccal, lingual and occlusal surfaces of some of the teeth. The morphology of these enamel defects suggested a possible diagnoses of fluorosis. Because not all teeth in the samples studied exhibited the defect, a conclusive diagnosis could not, however, be offered. Given that fluoride can enter the crystal lattice of hydroxyapatite (the major mineral component of calcified tissue including bones and teeth), and that the uptake of higher than optimal levels of fluoride can alter the molecular structure of dentition, it was thought that the application of X-ray diffraction to this problem may aid a more archaeological problem are outlined. This is followed by a discussion of synchrotron radiation and the advantages it has over conventional X-rays. The materials and methods used in the analysis are provided, followed by a discussion of the results. While further work is required to fully attributed the enamel defects to the effects of fluoride, this paper illustrates that synchrotron radiation, in particular X-ray diffraction, can be applied to archaeological materials as a means of quickly and effectively obtaining a structural analysis.

L. Vendier, P. Sciau, et É. Dooryhée. X-ray diffraction analysis of the red varnishes in southern Gaul sigillata - Workshops in La Graufesenque. J. Phys. France IV, 12(6):189-196, 2002. [ doi ]

La Graufesenque (Millau, Aveyron) 1(rst) and 2(nd) centuries AC Sigillata red slips have been studied by X-ray diffraction at ESRF and on a conventional diffractometer. Although X-ray diffraction is a non-destructive characterisation technique adapted to surface study, it has not been used so much for Sigillata slip characterisation. The poor quality of the slip surface can be an explanation. In this work we demonstrate that it is possible to get good quality diffraction diagrams on 20- 120 AC Sigillata slips. The results confirm the productions homogeneity and the hypothesis about a non-local clay used for the slips. On a counterpart, the late (second half of 2(nd) century AC) Sigillata study needs because of their crackled surface a high quality beam, which can only be accessible on a synchrotron installation. These productions seems to be more heterogeneous: some Sigillata present similar diffraction diagrams for the slip and ceramic body (same clay'?), some others present results similar to the precedent production period ones.

P. Dillmann, D. Neff, F. Mazaudier, S. Hoerlé, P. Chevallier, et G. Béranger. Characterisation of iron archaeological analogues using micro diffraction under synchrotron radiation. Application to the study of long term corrosion behaviour of low alloy steels. J. Phys. France IV, 12(6):393-408, 2002. [ doi ]

Last progresses in synchrotron radiation focusing allow the characterisation on microscopic samples. The use of X Ray micro diffraction (muXRD) in two corrosion studies (indoor atmospheric corrosion and in soil corrosion) concerning iron archaeological artefacts is presented. This analytical method permits to locate and identify very precisely the constitutive phases of the corrosion products. For the atmospheric corrosion study, semi quantitative data were presented to assess the proportion of the different identified phases in the rust layers. For the in soil corrosion study, the precise distribution of corrosion products formed on the nine analysed artefacts is given.

L. Bertrand, P. Chevallier, J. Doucet, A. Simionovici, G. Tsoucaris, et P. Walter. Apport du rayonnement synchrotron à l'étude de cheveux archéologiques. J. Phys. France IV, 12(6):237-43, 2002. [ doi ]

La préservation dans certains contextes archéologiques des cheveux humains et des fibres animales est favorisée par leur transformation chimique au contact d'objets métalliques Afin de mieux comprendre les phénomènes complexes mis en jeu, nous avons étudié expérimentalement la fixation de cations métalliques (Cu et Pb) dans des cheveux modifiés à partir de différenties méthodes de caractérisation utilisant le rayonnement X synchrotron. Nous avons ainsi pu mettre en évidence la fixation spécifique d'une partie de ces cations au sein des lipides structurés du cheveu. La comparaison entre échantillons modèles et archéologiques apporte de nouvelles données concernant les premières étapes d'altération des cheveux archéologiques.

J. P. Veiga et M. O. Figueiredo. Sixteenth century tubular glass beads: non-destructive chemical characterization using synchrotron radiation XRF. X-ray Spectrom., 31:300-304, 2002. [ doi ]

The results of a photon microprobe (synchrotron radiation XRF) study of tubular blue glass beads of the Nueva Cadiz type uncovered by recent excavations in the center of Lisbon are reported as a contribution to the non-destructive chemical characterization of these cultural artifacts, aiming ultimately at ascertaining their provenance and manufacturing location. Either twisted or plain, with round or square cross-sections, the beads are clearly formed by two blue vitreous layers separated by an opaque white stratum, but a fourth inner transparent bluish layer is visible in the cross-section of most beads studied. These strata differ essentially in the content of colorant ions (Cu, and occasionally Co traces), fuser metals (essentially Pb) and white layer opacifier (Sn oxide). Other minor and trace elements were determined: K, Ca, Ti, Mn, Fe, Ni, Zn, Ga, As, Br, Rb, Sr, Y, Zr, Nb, Ba, Sb, Hg and Bi. The bromine increase in the outer layers was attributed to burial. Some minor elements are tentatively related to the fuser carrier compound and other chemical components are discussed in terms of raw materials and glass typology. Copyright (C) 2002 John Wiley Sons, Ltd.

E. Pantos, C. C. Tang, E. J. MacLean, K. C. Cheung, R. W. Strange, P. J. Rizkallah, M. Z. Papiz, S. L. Colston, M. A. Roberts, B. M. Murphy, S. P. Collins, D. T. Clark, M. J. Tobin, M. Zhilin, K. Prag, et A. J. N. W. Prag. Applications of synchrotron radiation to archaeological ceramics. Dans V. Kilikoglou, A. Hein, et Y. Maniatis, éds, Modern Trends in Scientific Studies on Ancient Ceramics, vol. 1011, p. 377-384. BAR International Series, 2002.

X-ray techniques have been employed widely throughout the course of advancement of Archaeological Science. It is only very recently that synchrotron radiation (SR) has been utilised for measurements on archaeological material. Synchrotron light sources are, in the main, large multidisciplinary research facilities supporting a broad research portfolio in Physics, Chemistry, Biology and Engineering. Particular emphasis has been given lately to Materials Science problems, such as microfabrication techniques or microcharacterisation studies of surfaces or small interior volumes, because of industrial applications.

The light produced by SR sources covers a wide spectral range, from the Infrared to hard X-rays. Compared to conventional laboratory sources, SR can deliver several orders of magnitude greater photon flux with a well collimated beam. The small beam cross section permits the study of localised details in materials or can be used to follow small changes in composition across a sample. The high penetration of X-rays at high photon energies (>30keV) permits the study of the interior of ceramics, non-destructively. Wavelength tunability over a continuous range allows for spectroscopy measurements (EXAFS) to be made, not feasible with conventional laboratory equipment, over small sample areas to determine oxidation state and coordination of absorbing species. Combined techniques may be used simultaneously, on the same area.

Measurements have been carried out at the Daresbury Laboratory SRS with the aim of demonstrating the advantages and evaluating the effectiveness of SR over conventional methods. High resolution powder diffraction patterns of Attic and neolithic Russian potsherds are compared with ones obtained on a conventional diffractometer. Reflections of non-plastic inclusions have a line width 5-10 times narrower in the SR case. Flat-plate XRD (fixed incident angle, variable diffraction angle) of the black gloss layer of two Attic potsherds shows that hematite, magnetite and ferrian spinel are present in one case, only spinel in the other while neither spinel or magnetite are found on the surface of the unglossed area or in powder extracted from the body of the ceramic. Other clay mineral reflections are much better resolved making phase identification less ambiguous. XRF of small areas in a calcite-rich potsherd from the Bronze Age Jordan shows variations of calcium and magnesium while the iron content is fairly constant.

Fluorescence EXAFS of a cross section of the handle of a Koan transport amphora from a shipwreck gives a spectrum characteristic of hematite the concentration of which varies with distance from the edge and with changes in the colour of the fabric. XRF of the same areas reveal a 6-fold concentration decrease of calcium and a smaller decrease in iron as the sample is traversed from edge to centre. Spatially resolved XRD (forty consecutive 250mm steps) on the same potsherd using a 2300x2300-pixel CCD detector for fast data acquisition (10 seconds per shot) reveals systematic differences in mineralogical composition across the sample. The outer, 1-2 mm wide, layer contains an unidentified micro-crystalline phase exhibiting an intense broad reflection close to the kaolinite basal reflection. This concurs with energy-dispersive XRD-Tomoscopy measurements of small volumes inside the potsherd sampling the outer 8mm in 400m steps. SAXS measurements over regions of distinct colour difference show changes in scattering density and porosity as measured by the fractal dimension values (slope of log-log SAXS pattern at low angles). These changes concur with SEM observations. Aragonite and magnesian calcite appear to be more abundant near the edge, consistent with the XRF measurements and with XRD of powder extracted from the whitish marine deposits on the surface of the amphora.

These initial measurements by no means test the limits of what can be achieved with SR. Several other SR-based techniques (FTIR, XPS, SEXAFS, glancing angle XRD, X-ray microscopy, contrast imaging and micro-tomography) can have a significant impact on characterisation of archaeomaterials such as pigments, glasses, metal surfaces and bone. Third generation SR sources can deliver thousand-fold improvements in intensity and beam cross-section offering new opportunities for novel applications and prospects for new directions in archaeological science.

B. Kanngiesser, W. Malzer, et I. Reiche. Micro-XRF goes 3D: X-ray insights into Indian Mughal paintings. Bessy highlights, 2002.

I. Reiche, C. Vignaud, B. Champagnon, G. Panczer, C. Brouder, G. Morin, V. A. Solé, L. Charlet, et M. Menu. From mastodon ivory to gemstone: the origin of turquoise color in odontolite. Am. Miner., 86(11-12):1519-1524, November-December 2001. [ doi ]

Heat-induced color changes of fossilized Miocene mastodon ivory (13-16 Ma) have been known at least since the Middle Ages. Cistercian monks are believed to have created odontolite, a turquoise-blue gemstone, by heating mastodon ivory found in Miocene geological layers next to the Pyrrenean chain, France, to use it for the decoration of medieval art objects. This material has been the object of investigations of famous European naturalists and gemmologists, among them Reaumur (1683-1757). Although vivianite [Fe-3(PO4)(2). 8H(2)O] is the commonly accepted coloring phase supposed to appear when heating fossilized mastodon ivory, our previous spectroscopic studies using PIXE/PIGE and TEM-EDX demonstrated that:the chemical composition of collection odontolite and heated mastodon ivory corresponds to well-crystallized fluorapatite [Ca-5(PO4)(3)F] containing trace amounts of Fe (230-890 ppm), Mn (220-650 ppm), Ba (160-620 ppm), Pb (40-140 ppm), and U (80210 ppm). No vivianite has been detected. To provide new insights into the physico-chemical mechanism of the color transformation of fossilized ivory, we used the combination of UV/visible/near-IR reflectance spectroscopy, time-resolved laser-induced luminescence spectroscopy (TRLIF), and X-ray absorption near-edge structure (XANES). Contrary to what had formerly been described as the color origin in odontolite, our study has conclusively identified traces of Mn5+ by UV/visible/near-IR reflectance spectroscopy, TRLIF, and XANES inside the fluorapatite. Thus, odontolite owes its turquoise- blue color to Mn5+ ions in a distorted tetrahedral environment of four O2- ions. XANES also demonstrated oxidation of disordered octahedral Mn2+ ions to tetrahedral Mn5+ species in apatite (luring the heat process. So we give the first evidence of the real color origin in odontolite.

I. Deraedt, K. Janssens, J. Veeckman, L. Vincze, B. Vekemans, et T. E. Jeffries. Trace analysis for distinguishing between Venetian and facon-de-Venise glass vessels of the 16th and 17th century. J. Anal. At. Spectrom., 16(9):1012-1017, September 2001. [ doi ]

In this paper, the differences and similarities in chemical composition between facon-de-Venise glass excavated in Antwerp and two types of Venetian glass, both from the sixteenth and seventeenth Centuries, are documented. On the basis of typological criteria alone it is not possible to distinguish imported Venetian glass from locally produced glass. For this purpose, the major element composition of Antwerp and Venetian glass was studied with EPXMA (electron probe X-ray microanalysis) and. in a second phase, these objects were also analysed for their trace element content by means of SR-XRF (synchrotron radiation induced X-ray fluorescence analysis) and LA-ICP-MS (laser ablation inductively Coupled plasma mass spectrometry). The largest group of Antwerp objects has a composition that significantly differs from truly Venetian compositions, pointing to an important local production. However, a few objects were found that have a major composition very similar to Venetian Cristallo and a larger group corresponds to the Venetian Vitrum Blanchum composition. In order to be able to make a more clear distinction between the Antwerp Cristallo and Venetian Cristallo glass types, to verify that indeed the Antwerp and Venetian Vitrum Blanchum compositions are identical and to understand better the causes of the compositional differences among the groups. the concentrations of a number of trace elements, possibly providing clues on the raw materials, were determined.

M. Bonnin-Mosbah, A. S. Simionovici, N. Métrich, J.-P. Duraud, D. Massare, et P. Dillmann. Iron oxidation states in silicate glass fragments and glass inclusions with a XANES micro-probe. J. Non-Cryst. Solids, 288(1-3):103-113, August 2001. [ doi ]

The iron oxidation states and its environment in volcanic silicate glasses have been studied by combining micro-X-ray absorption near edge structure (XANES) experiments at the iron K-edge in silicate glass fragments and glass inclusions trapped during the crystal growth. Experiments were performed at the ESRF (ID22 beam-line) - a third generation synchrotron - using a focused beam (2×10 μm^2) together with a high brilliance and a good energy resolution. The selected silicate glasses, basaltic in composition, contain between 5.5 and 8 wt% total Fe. In all XANES spectra, pre-peaks exhibit a multi-component structure, which is the convolution of information related to the valence state of iron (2^+,3^+), the site geometry and transition types. The Fe^3+/ΣFe ratio of silicate glass fragments deduced from the XANES spectra is correlated to values determined by chemistry on bulk samples within the range 0.05-0.85. XANES spectra from glass inclusions hosted in natural olivine crystals may be interpreted considering the glass fragments as reference samples.

P. Dillmann, K. Weulersse, B. Regad, G. Moulin, R. Barrett, M. Bonnin-Mosbah, S. Lequien, et P. Berger. Austenitic steel corrosion in IGCC environment. Characterisation by photon and nuclear microprobes. Nucl. Instrum. Methods B, 181(1-4):734-738, July 2001. [ doi ]

An austenitic steel sample was treated simulating particular working conditions of an integrated gasification combined cycle (IGCC) power plant. Several classical characterisation techniques were used to investigate the oxide scale. In addition ,micro-particle-induced X-ray emission (PIXE) and Rutherford backscattering spectrometry (RBS) analyses were performed and permit us to identify several phases constitutive of the oxide. Moreover, micro-X-ray absorbtion near edge structure (XANES) experiments allow us to determine the valence of the vanadium incorporated in the scale in the form of microscopic islets. The comparison of all the results leads to the proposal of a corrosion mechanism for this alloy.

P. Martinetto, M. Anne, É. Dooryhée, M. Drakopoulos, M. Dubus, J. Salomon, A. Simionovici, et P. Walter. Synchrotron X-ray micro-beam studies of ancient Egyptian makeup. Nucl. Instrum. Methods B, 181:744-748, July 2001. [ doi ]

Vases full of make-up are most often present in the burial furniture of Egyptian tombs dated from the pharaonic period. The powdered cosmetics made of isolated grains are analysed to identify their trace element signature. From this signature we identify the provenance of the mineral ingredients in the makeup and we observe different impurities in products, which have been demonstrated as synthetic substances by previous works. Focused X-ray micro-beam (2 x 5 mum(2)) is successively tuned at 11 keV, below the L-III absorption edge of Pb, and 31.8 keV for global characterisation of the metal impurities. The fluorescence signal integrated over each single grain is detected against the X-ray micro-diffraction pattern collected in transmission with a bi-dimensional detector. Furthermore, for galena grains rich in Zn, the XANES signal at the K- absorption edge of Zn shows its immediate nearest-neighbour environment.

A. Kuczumow, S. Pikus, C. Un-Ro, P. Sadowski, P. Wajnberg, et M. Jurek. Structural investigations of a series of petrified woods of different origin. Spectrochim. Acta B, 56(4):339-350, April 2001. [ doi ]

Since the investigations on petrified wood performed so far have not proved the assumption that the ring structure is coupled to the changes in the crystalline form of silica, attention was paid to other possible reasons. Using small angle X-ray scattering methods we determined the Porod curves and pore size distributions for five different samples of petrified wood, of different origin. We observed clear porosity differences in different samples. In addition, the normal X-ray diffractometric measurements were carried out, which gave a totally uniform image of the crystallographic structure of all the samples. All of them were made of pure [alpha]-quartz. The differentiation of rings in dark and bright zones should be put down to the changes in porosity rather than to other factors. The pores seem to be much more concentrated in those ring locations, which correspond to the original dark wood positions in living wood.

I. Bentchev, A. Rosenberg, et T. Sieredzki. Neue Röntgenfluorenzenzmethode für die Legierungsanalyse Zusammensetzung und Altreparaturen äthiopischer Metallkreuze (A new X-ray fluorescence method to analyze alloys composition and old repair of Ethiopian metal crosses). Restauro, 8:590-595, 2001.

How were the crosses made and do all the alloys used in the repairs date from the same period? Science offers new insight into a hitherto little noted group of objects without damaging them. In X-ray fluorescent analysis induced by synchrotron radiation (SYRFA), the sample is excited by the X-ray radiation part of the synchrotron radiation coming from an electron accelerator (synchrotron). SYRFA has advantages over RFA: tiny volumes in the trace element range can be analyzed, so-called point analyses. The SYRFA results represent the first data on the metal alloys employed for these six Ethiopian crosses. All three pectoral crosses, but only one of the hand crosses were made of an alloy containing silver, copper and only a little zinc. Little is known about the origin of these metals in Ethiopia. Probably coins served as the raw material. Despite its silver appearance, one of the crosses is made of brass. At present there is no explanation how this unusual coloring was achieved. Another hand cross is made of new silver containing 7% nickel. The diversity of the alloys supports the theory that the crosses were assembled from a supply of single pieces. All the eyes are attached to the crosses with hard silver solder of varying composition. Hard silver solder was also employed to manually join individual parts. The SYRFA method did not confirm any silver plating as assumed for some crosses. Only analysis of the top layers is possible.

P. Dillmann et R. Balasubramaniam. Characterization of ancient Indian iron and entrapped slag inclusions using electron, photon and nuclear microprobes. Bull. Mater. Sci., 24(3):317-322, 2001. [ doi ]

Compositional and structural information were obtained from an ancient 1600-year old Indian iron using microprobe techniques (EDS, mu-XRD and mu-PIXE). Several different local locations in the iron matrix and in the entrapped slag inclusions were analyzed. The P content of the metallic iron matrix was very heterogeneous. Lower P contents were observed in the regions near slag inclusions. This was correlated to the dephosphorization capacity of the slag. The crystallized phases identified in the slag inclusions were wüstite and fayalite. The compositions of the slag inclusions were relatively homogeneous.

I. Reiche. From fossilised mastodon ivory to gemstone. ESRF highlights, 2001:31-33, 2001.

T. J. Wess, M. Drakopoulos, A. Snigirev, J. Wouters, O. Paris, P. Fratzl, M. Collins, J. Hiller, et K. Nielsen. The use of small-angle X-ray diffraction studies for the analysis of structural features in archaeological samples. Archaeometry, 43(1):117-129, January 2001. [ doi ]

X-ray diffraction or scattering analysis provides a powerful non-destructive technique capable of providing important information about the state of archaeological samples in the nanometer length scale. Small-angle diffraction facilities are usually found at synchrotron sources, although the potential of a laboratory source is also described. Specific examples of analysis using X-ray diffraction of historic parchment, archaeological bone, a Central Mexico style pictograph and microdiffraction of calcified tissues are used to show the scope and versatility of the technique. Diffraction data is capable of giving fundamental structural information as well as quantifying the remodelling of structures influenced by environmental fact ors.

C. C. Tang, E. J. MacLean, M. A. Roberts, D. T. Clarke, E. Pantos, et A. J. N. Prag. The study of Attic black gloss sherds using synchrotron X-ray diffraction. J. Archaeol. Sci., 28(10):1015-1024, 2001. [ doi ]

We have studied the mineral composition of the gloss and the ceramic body of three pieces of Attic Greek pottery by applying the techniques of high-resolution powder diffraction using synchrotron X-rays. The measurements were performed on Stations 2.3 and 9.1 at the Synchrotron Radiation Source, Daresbury Laboratory. High quality powder patterns from the bulk of the ceramics and from the gloss surfaces have been obtained. The diffraction results show interesting variations of mineral composition between the gloss of the different sherds as well as variations between the bulk and the gloss. This makes phase identification and comparison between different fabrics less ambiguous. Spinel minerals are present in the gloss which are absent in the main body of the ceramics. Diffraction lines from one surface match the patterns of hematite, magnetite/maghemite and hercynite, while solid solutions of spinel structures appear to be present in the gloss layer of another sample. Crystallite particle sizes and lattice parameters of the minerals in the gloss layer of another sample. Crystallite particle sizes and lattice parameters of the minerals in the gloss layer have been accurately determined. Supplementary scanning electron microscopy (SEM) reveals the gloss thickness to be approximately 20 mum but with variations down to 5 mum. Analysis of the diffraction profile for the hematite component reveals a particle size int he order of 0.027 mum.

G. de Stasio, B. Gilbert, B. H. Frazer, K. H. Nealson, P. G. Conrad, V. Livi, M. Labrenz, et J. F. Banfield. The multidisciplinarity of spectromicroscopy: from geomicrobiology to archaeology. J. Electron Spectrosc. Relat. Phenom., 114:997-1003, 2001. [ doi ]

Synchrotron X-ray PhotoElectron Emission Microscopy (X-PEEM) is a useful tool to investigate the microchemical composition of a variety of different samples, including cells in culture, tissue sections, magnetic material, bacteria, rocks, materials science, tribology and archaeology specimens. The MEPHISTO X-PEEM, installed at the Wisconsin Synchrotron Radiation Center, reached a peak resolution of 20 nm, has been extensively used for the last 4 years to explore all of the above systems. The experiments reported here are some of the most unusual ones for this technique: ZnS precipitating bacteria, Mn and Fe oxide rocks and archaeological coins. The microchemistry of each one of these samples delivered new results.

I. Nakai, Y. Terada, M. Itou, et Y. Sakurai. Use of highly energetic (116 keV) synchrotron radiation for X-ray fluorescence analysis of trace rare-earth and heavy elements. J. Synchrotron Radiat., 8:1078-1081, 2001. [ doi ]

This study has revealed the advantages of the use of 116 keV Xrays as an excitation source of X-ray fluorescence (XRF) analyses. This technique is suitable for nondestructive multielemental analyses of heavy elements such as rare-earth elements. The lowest MDL value evaluated for the bulk analysis of a JG-1 standard reference sample (granite rock) was 0.1 ppm for W for a 500 s measurement. The spectrum of standard glass samples of SRM612 demonstrated clearly resolved K-line peaks of more than 30 elements, including all the existing rare-earth elements, at 50 ppm levels. The calibration curve for the determination of a rare-earth element shows a linear relation between the XRF intensity and concentrations from 10 to 0.03 ng. This powerful technique should be useful for nondestructive analyses of rare-earth and heavy elements in geological, geochemical and archaeological samples as well as industrial materials.

A. P. J. Stampfl, E. S. Friedman, T. J. Wilkinson, E. E. Alp, et K. A. Yener. Shedding light on the past. Nucl. Instrum. Methods A, 467-468:1305-1307, 2001. [ doi ]

The Amuq valley in southern Turkey is an important and interesting area in the Near East forming a space-time bridge for archaeologists and scientists to ancient and modern civilizations. The Lake of Antioch which evolved during the mid-late Holocene appears to have been located nearby some of the largest human settlements existing during this period. By documenting the conditions of the lake in time, using classical and modern approaches, the climate and geomorphology of the basin may be reconstructed. Synchrotron X-ray fluorescence measurements were performed on sections of a sedimentary core from the lake, representing an estimated 7500yr of history. Analysis yielded the distribution of elemental masses spanning Ca to Mo as a function of depth from the surface. We find that the elemental concentrations measured follow a number of distinct patterns that may be related to local geomorphology, climate and human activities. (C) 2001 Elsevier Science B.V. All rights reserved.

T. J. Wilkinson, E. S. Friedman, A. P. J. Stampfl, et E. E. Alp. The geoarchaeology of a lake basin: Spatial and chronological patterning of sedimentation in the Amuq plain, Turkey. Dans M. Fortin, éd., Journées d'étude du Groupe de recherches en archéométrie du CELAT (1997-1999), Cahiers d'archéologie du CELAT, Série archéométrie, vol. 10, p. 211-226. Laval University, Université Laval, Québec, Canada, 2001.

I. Reiche, A. Berger, W. Görner, S. Merchel, M. Radtke, J. Riederer, et H. Riesemeier. A closer look at Albrecht Dürer's drawings (1471-1528). Bessy highlights, 2001:32-33, 2001.

I. Deraedt, B. Vekemans, K. Janssens, et F. Adams. Synchrotron light through ancient glass. Europhysics News, 31(6):15, November 2000. [ doi ]

Synchrotron Radiation induced micro X-ray Fluorescence (m-SRXRF) can provide complementary information on trace elements when used together with EPMA (Electron Probe Micro Analysis). EPMA has a limited sensitivity with detection limits of 0.1 % in the most favourable conditions. Offering ppm level detectability for many more elements, SRXRF is considerably more powerful for quantitative fingerprint analysis in order to gain a better understanding of the provenance of archaeological objects. In this paper, after a short description of the m-SRXRF instrumentation, a study on sixteenth and seventeenth century glass objects from Antwerp will be briefly outlined.

M. Ando, J. Chen, K. Hyodo, K. Mori, H. Sugiyama, et X. Xian. Nondestructive visual search for fossils in rock using X-ray interferometry imaging. Jap. J. Appl. Phys., 39(2):L1009-L1011, October 2000. [ doi ]

Fossils inside rock have been clearly visualized utilizing an X-ray interferometer. Two types of clear images are obtained, one involves phase contrast in interference beams and the other involving refraction contrast in forward-diffracted beams. 2D monochromatic synchrotron X-ray radiation with a beam size of 10 mm × 10 mm and a photon energy of 35 keV was used. Using a stereographic pair of X-ray images, the locations of fossils inside rock can easily be determined with a precision of 0.5 mm. This method can be a powerful nondestructive tool in the fields of paleontology and paleobiology to discover and locate fossils and trace fossils inside rock.

A. Kuczumow, P. Chevallier, P. Dillmann, P. Wajnberg, et M. Rudas. Investigation of petrified wood by synchrotron X-ray fluorescence and diffraction methods. Spectrochim. Acta B, 55(10):1623-1633, October 2000. [ doi ]

Pieces of petrified wood from south-eastern Poland comprising one of the greatest European collections were investigated. The age of Miocene wood was estimated at 50 million years. Taxodioxylon sequoianum Gothan was recognised as the dominating species among the preserved samples. Silica material, basic for the petrifaction processes, was investigated by synchrotron-based microfluorescence and microdiffraction. Different distribution patterns were determined after careful examination of linear scans and elemental maps: calcium, potassium and titanium were uniformly spread in the silica matrix while the iron content was concentrated in clear inclusions; other detected elements, as Cu, Zn, Cr, As were observed mainly in the form of inclusions. There was no difference in microdiffractograms for silica between the places of original dark and light wood. One could find little difference in diffraction patterns of samples with the elevated content of iron. In general, the diffraction patterns of silica from petrified wood could be associated with quartz patterns from 1998 JCPDS-International Centre for Diffraction Data. (C) 2000 Elsevier Science B.V. All rights reserved.

P. Martinetto, M. Anne, É. Dooryhée, G. Tsoucaris, et P. Walter. Les formulations cosmétiques de l'Égypte ancienne retrouvées grâce à la diffraction des rayons X. J. Phys. France IV, 10(10):465-472, September 2000. [ doi ]

X-ray diffraction analysis of cosmetic formulations from Ancient Egypt. Funerary furniture found in Egyptian tombs is an extraordinary source for studying the customs in the everyday life during the Ancient Egypt. Some excavations of tombs have provided some genuine toilet bags, with mirrors, hairpins, eyeliner applicators and makeup receptacles, sometimes still filled with cosmetic compounds. Make-up samples have been taken from pots made of stone, ceramic, wood or reed conserved in the Department of the Egyptian Antiquities of the Louvre Museum and coming from several sites dated between 2100 and 1100 BC. The mineral phases present in the powders have been identified by X-ray diffraction, after SEM observations. Diffraction patterns have been collected in high-resolution mode at the ESRF and at the LURE and the use of a Rietveld profile refinement method has allowed the quantification of mineral phases. We will discuss the limits of this non-destructive method, applied to extremely small archaeological samples (about 1mm(3)) and to mixtures of up to ten phases. The quantitative analysis of twenty-eight cosmetic powders will allow us to think about the different eye make-up formulations elaborated 4000 years ago.

M. L. Carvalho, C. Casaca, T. Pinheiro, J. P. Marques, P. Chevallier, et A. S. Cunha. Analysis of human teeth and bones from the chalcolithic period by X-ray spectrometry. Nucl. Instrum. Methods B, 168(4):559-565, August 2000. [ doi ]

Synchrotron microprobe and X-ray fluorescence spectrometry (XRFS) were used to analyse several teeth and pieces of bone, respectively, originating from subjects of the chalcolithic period. A synchrotron microprobe with 100 mu m resolution and monochromatic photons of 18 keV were used to scan teeth from the root to the enamel. Bones were analysed by XRFS for their amount of trace elements, using a spectrometer based on a three-axial geometry and an incident beam of 17.4 keV. The detected elements for both analytical procedures were P, K, Ca, Mn, Fe, Cu, Zn, Pr, Sr and Pb. The results show high concentrations of Mn, Fe and Cu for different tooth regions when compared with data from contemporary subjects. Moreover, the high levels of Br and Sr can be associated with environment influence and dietary habits rich in protein, especially seafood. It is remarkable that lead is always of the order of magnitude of the detection limit, which is 1-2 mu g/g in all analysed teeth. Furthermore, the microprobe analysis of these samples showed that the highest concentration of the heavy metals increases from the outer enamel to the inner dentine root. For the analysed bone samples of women and men, the most important aspects concerning the elemental concentrations are the high levels of Mn and Br and the low concentrations of Pb, as found for teeth. (C) 2000 Elsevier Science B.V. All rights reserved.

P. Martinetto, M. Anne, É. Dooryhée, G. Tsoucaris, et P. Walter. Radiation in Art and Archaeology, chap. A synchrotron X-ray diffraction study of Egyptian cosmetics, p. 297-316. Dans Creagh et Bradley [ .ref ], June 2000.

W. Kockelmann, E. Pantos, et A. Kirfel. Radiation in Art and Archaeology, chap. Neutron and synchrotron radiation studies of archaeological objects, p. 347-377. Dans Creagh et Bradley [ .ref ], June 2000.

S. L. Colston, A. Jupe, et P. Barnes. Radiation in Art and Archaeology, chap. Synchrotron radiation tomographic energy-dispersive diffraction imaging, p. 129-150. Dans Creagh et Bradley [ .ref ], June 2000.

D. C. Creagh et D. A. Bradley, éds. Radiation in Art and Archaeology. Elsevier Science, June 2000.

A. Simionovici, K. Janssens, A. Rindby, I. Snigireva, et A. Snigirev. Precision micro-XANES of Mn in corroded Roman glasses. Dans W. Meyer-Ilse, T. Warwick, et D. Atwood, éds, X-ray Microscopy: Proceedings of the VIth International Conference, Berkeley, California (USA), 2-6 Aug 1999, vol. 507 de AIP conference, p. 279-283, New-York, USA, May 2000. American Institute of Physics, Melville. [ doi ]

The highest spatial resolution μ-Xanes experimental results to date were obtained on an archeological glass sample containing Mn. Both the fluorescence (SIXES) and absorption collection modes were used to record maps of the elemental distribution throughout the surface corrosion layer. By using two excitation energies near the Mn threshold at 6.5 keV, direct speciation maps were obtained. The analysis was carried out using the ESRF, ID 22 microbeam, with a 3×5 μm2 beamspot.

E. S. Friedman, Y. Sato, A. Alatas, C. E. Johnson, T. J. Wilkinson, K. A. Yener, B. Lai, G. Jennings, S. M. Mini, et E. E. Alp. An X-ray fluorescence study of lake sediments from ancient Turkey using synchrotron radiation. Dans Proc. of the 47th Annual Denver X-ray Conference, Colorado Springs, CO, August 3-7, 1998, vol. 42, p. 151-160. Plenum Press, 2000.

T. J. Wess, I. Alberts, G. Cameron, C. Laurie, J. Orgel, J. Hiller, K. Nielsen, V. de La Cruz Balthazar, M. Drakopoulos, A. M. Pollard, et M. Collins. Small angle X-ray scattering reveals changes of bone mineral habit and size in archaeological samples. Fibre Diffrac. Rev., 91:36-43, 2000.

X-ray scattering provides a powerful non-destructive technique capable of providing important information about the size, habit and arrangement of mineral crystals in bone. In the case of archaeological bone the changes in the habit of the apatite crystals and recrystallised material may reflect the changes in bone environment that have occurred since death. In the study presented here we have examined a variety of archaeological bones by small-angle X-ray scattering to show the alterations in bone habit that can be adopted after 'diagenetic remodelling'. Furthermore we show that the use of small-angle scattering microfocus technology allows us to probe into the fine structure alterations that can occur in bone as a result of microbial attack and mineral recrystallisation. The integrity of the bone crystallites has a strong correlation with the ability to extract other biomolecules from bone such as osteocalcin and DNA. Alterations in the crystallite habit may explain the success of macromolecule recovery from archaeological samples.

P. Martinetto, M. Anne, É. Dooryhée, et P. Walter. X-ray diffraction line broadening analysis of galena powders: a clue to some practices on mineral crushing in ancient Egypt. Mater. Sci. Forum, 321-323:1062-1067, 2000. [ doi ]

Galena (PbS, Fm3m) is the main mineral compound traditionally used for eye makeup in North Africa since Ancient Egypt. Archaeological excavations of galena mines have shown that Egyptians easily extracted polyhedral blocks several centimetres long 4000 years ago. The ore was crushed until a fine powder was obtained. SEM observations of cosmetics show well developed cubic crystals with a size distribution between 20 and 100 mu m. In order to determine the shape, size and strains of the crystallites in galena powders, X-ray diffraction powder patterns were collected at the ESRF (BM16). The high instrumental resolution (minimum FWHM = 0.005 degrees 2 theta) enables the line broadening, which is intrinsic to the samples, to be studied. Archaeological, geological and synthetic samples were prepared in capillaries. Natural galena (geological and archaeological) show significant anisotropic effects of microstrains and size. The archaeological interest of this study is to provide an insight into the possible methods for crushing and preparing the galena ore.

K. Janssens, G. Vittiglio, I. Deraedt, A. Aerts, B. Vekemans, L. Vincze, F. Wei, I. De Ryck, O. Schalm, F. Adams, A. Rindby, A. Knöchel, A. Simionovici, et A. Snigirev. Use of microscopic XRF for non-destructive analysis in art and archaeometry. X-ray Spectrom., 29(1):73-91, January 2000. [ doi ]

The various application possibilities of microscopic X-ray fluorescence and associated methods for the characterization and provenance analysis of objects and materials of cultural heritage value are discussed by means of a number of case studies. They include the trace analysis of historic glass, the analysis of corroded coins and statues in bronze and silver and the study of inks on historical documents. These studies are conducted by means of micro-XRF instruments installed at synchrotron beamlines and by means of laboratory equipment, some of which is easily transportable to the museum or archaeological site where the objects of interest are located. Copyright (C) 2000 John Wiley & Sons, Ltd.

W. Kockelmann, H. Kutzke, A. Kirfel, E. Pantos, M. Z. Papiz, S. E. Girdwood, E. Hähnel, M. Zhilin, A. J. N. W. Prag, et K. Prag. Quantitative phase analysis of archaeological ceramics using neutron, X-ray and synchrotron diffraction. Zeitschrift für Kristallographie, Suppl. 17:69, 2000.

Time-of-flight neutron and synchrotron X-ray diffraction were used for fingerprint determinations and quantitative mineral phase analyses of archaeological objects. Both neutron and X-ray diffraction techniques have their advantages and drawbacks when used in archaeological research. Neutron diffraction allows nondestructive analysis of complete and unprepared objects. Synchrotron X-ray diffraction can be used for fast and high resolution data collection on small amounts of powder samples, surfaces or thin sections. This paper concentrates on the introduction of the white-beam neutron diffraction technique applied on archaeological pottery. X-ray diffraction results from both laboratory and synchrotron sources are given for comparison.

K. Yamahana. Synchrotron radiation analysis on ancient Egyptian vitreous materials. Dans Proc. of the 25th Linear Accelerator Meeting in Japan, July 12-14, 2000, Himeji, Japan, 2000.

Ancient Egyptian vitreous materials, namely faience and glass, share the same elemental composition. But they appear to have originated separately. Faience objects appear as early as the Predynastic period, and glass was introduced from Mesopotamia during the New Kingdom. These faience and glass objects were not of daily use, rather they were regarded as religious symbols or luxury status goods. Most of the products were coloured blue, but we see an increased use of other colours during the New Kingdom (c.1550-1069BC). This tendency corresponds to the period of both territorial and political expansion of Egypt. A non-destructive SR-XRF experiment at Spring-8 was conducted last winter, aiming to determine the regional trait of elemental composition by examining the pattern and ratio of rare earth elements. As a result, we could observe some distinctive rare earth elements that may indicate regional variation.

A. Aerts, K. Janssens, F. Adams, et H. Wouters. Trace-level microanalysis of Roman glass from Khirbet Qumran, Israel. J. Archaeol. Sci., 26(8):883-891, August 1999. [ doi ]

A series of Roman glasses is studied using scanning electron microscopy and synchrotron radiation induced X-ray fluorescence. The glass originates from Qumrân, Israel and has been buried for about 1900 years. The major and minor as well as trace composition of the original glass was studied to obtain a better insight into the origin of these objects. The fact that the composition of this large collection is nearly the same for almost all the objects appears to support the view that Qumrân was a centre of the perfume industry in the Middle East in ancient times; the glass vials and bottles being used as receptacles for perfume, ointment, etc.

I. Nakai, C. Numako, H. Hosono, et K. Yamasaki. Origin of the red color of Satsuma copper-ruby glass as determined by EXAFS and optical absorption spectroscopy. J. Am. Ceram. Soc., 82(3):689-695, March 1999. [ doi ]

The origin of the ruby color of Satsuma glass, a famous copperruby glass produced in Japan in the mid-19th century, has been examined by electron microprobe analysis (EPMA), X-ray absorption fine structure (XAFS), and optical absorption spectroscopy analyses, CuK XAFS analysis reveals that the major component of copper in the ruby glass consists of Cu(I) ions in the glass structure. This species is distinct from Cu2O (cuprite), which we conclude is not responsible for the ruby color. Optical absorption spectra measured at 300 and 77 K clearly distinguishes the absorptions due to the colloidal particles of metallic copper and Cu2O. It is concluded that the trace amount of copper in the ruby glass, which is below the detection limit of the EPMA and XAFS techniques, exists as metallic copper particles of nanometer size and is responsible for the ruby-red appearance of the Satsuma glass.

K. Janssens, L. Vincze, B. Vekemans, C. T. Williams, M. Radtke, M. Haller, et A. Knöchel. The non-destructive determination of REE in fossilized bone using synchrotron radiation induced K-line X-ray microfluorescence analysis. Fresenius J. Anal. Chem., 363(4):413-420, February 1999. [ doi ]

The sensitivity and applicability of the synchrotron radiation induced X-ray microfluorescence (mu-SRXRF) spectrometer at the Hamburg synchrotron laboratory Hasylab for the determination of the distribution of trace concentrations of rare-earth elements (REE) in fossilized bone are discussed and critically compared to those of other trace analytical methods such as instrumental neutron activation analysis (INAA) and LAMP-ICPMS (laser ablation microprobe inductively-coupled plasma mass spectrometry). Measurements were carried out on two bone samples from contrasting terrestrial depositional environments at Olduvai Gorge (Tanzania). Results indicate that the microdistribution of the REE in these biological materials is not homogeneous and that the relative abundance of these elements can provide information on the palaeoenvironment during the fossilization process. The heterogeneous distribution of the REE can be determined in a quantitative and completely non-destructive manner provided the concentrations of individual REE are above 10 mu g/g.

A. Kuczumow, B. Vekemans, O. Schalm, W. Dorrin, P. Chevallier, P. Dillmann, C.-U. Ro, K. Janssens, et R. Van Grieken. Analyses of petrified wood by electron, X-ray and optical microprobes. J. Anal. At. Spectrom., 14(3):435-446, 1999. [ doi ]

Samples of petrified wood of different origins were analyzed by the use of the electron microprobe, capillary X-ray fluorescence microprobe, synchrotron capillary X-ray microprobe and optical microscope, applied in a microprobe manner. The main attention was given to the investigation of the ring structure of the petrified wood and the comparison of this with the ring structure of the living trees analyzed by much the same methods. The continuous X-radiation, applied in a microprobe manner, the distribution of the gray-scale representation of the secondary electron intensities and the characteristic X-ray signals, mainly from the light elements, were registered by the use of the electron microprobe method. The X-ray capillary microprobe detected the Rayleigh and Compton signals, scattered from microareas of the samples, and the characteristic X-ray signals, mainly from the heavier elements. In the synchrotron-based capillary microanalytical measurements, one of the most important results was achieved by the microprobe application of scattered synchrotron radiation. The emission and scattering results were supplemented by transmission measurements, where possible. All the methods proved to be complementary in the analysis of such periodic structures as tree rings. Both capillary microprobes were much more efficient in the detection of heavy elements and penetrated deeper than the traditional electron microprobe. Careful analysis of different signals indicated that some samples of petrified wood in the authors' possession, composed of silica of variable density, are the chemical negatives of the primordial living wood. This is the first such observation in the literature. Microdiffraction studies of the samples proved that polycrystalline cr-quartz was the main matrix component of all these samples. The elemental analysis of the petrified wood gives important indications about the petrification processes. Comparison of the particular ring structure of the petrified wood with the ring structure of living trees shows great similarities. The widths of rings, density variations and density maxima are easily readable from the microanalysis of petrified wood. These parameters potentially can be exploited for the investigation of the biological, chemical, chronological and climatic information included in the fossilized tissues.

P. Walter, P. Martinetto, G. Tsoucaris, R. Bréniaux, M. A. Lefebvre, G. Richard, J. Talabot, et É. Dooryhée. Making make-up in ancient Egypt. Nature, 397:483-484, 1999. [ doi ]

The extensive use of green, white and black make-up has been known since the earliest periods of Egyptian history,. We have investigated cosmetic powders dating from between 2000 and 1200 BC that were preserved in their original containers. Quantitative crystallographic and chemical analysis of the organic and mineral components of the powders enabled us to identify two natural lead-based compounds: crushed ore of galena (PbS) and cerussite (PbCO3). We also found two unexpected constituents: laurionite (PbOHCl) and phosgenite (Pb2Cl2CO3). Because they are neither natural extracted ores nor products resulting from subsequent ageing or chemical modification, laurionite and phosgenite appear to be synthetic products manufactured by the Egyptians using 'wet' chemistry.

P. Walter, C. Ziegler, P. Martinetto, et J. Talabot. Quand la couleur soulignait l'oeil dans l'Égypte ancienne. Technè, 9-10:9, 1999.

M. O. Figueiredo, J. P. Veiga, et T. P. Silva. Non-destructive chemical characterization of cultural material using synchrotron radiation X-ray fluorescence. Dans M. Marabelli et C. Parisi, éds, Proc. of the 6th int. conf. on non-destructive testing and microanalysis for the diagnostics and conservation of the cultural and environmental heritage, Rome, May 17th-20th 1999, vol. 3, p. 1767-1979, Rome, Italy, 1999.

Two examples of applying a photon microprobe (μ-SRXRF) to the non-destructive chemical characterization of cultural and archaeological artifacts with museologic relevance are reported:

1) the analysis of minute fragments extracted from an XVII century piece of gold-leaf carved wood with the purpose of indirectly assessing the manufacturing technique in view of establishing a correct restoration treatment;

2) the chemical study of rare Mediterranean elongated glass beads composed of five identifiable successive concentric layers with varied colouring - white, red, green, blue.

Whenever possible, the materials were previously characterized by X-ray diffraction.

Au and Hg, plus Pb and minor Cd, were identified on the external surface of the carved wood fragments. Glass beads contain Sn and are essentially Cu- and Pb- rich in all concentric constituting layers, the exact origin of the various colourings remaining an open question.

These results are briefly discusses and comments are presented on the advantages of combining non-destructive instrumental techniques for chemical analysis and phase constitution study of cultural ancient materials.

P. Dillmann, P. Fluzin, et P. Chevallier. Determination of ironmaking processes using synchrotron microprobe. Dans E. Jerem et K. T. Biró, éds, Archaeometry 98. Proceedings of the 31st Symposium, Budapest, April 26 - May 3 1998, vol. 1043, p. 327-344. British Archaeological Reports International Series, 1998.

A. Rosenberg, M. Boghardt, H. Dittmann, D. Heimermann, A. Hein, et H. Mommsen. Röntgenfluoreszenzanalyse der Druckerschwärzen des Mainzer Catholicon und anderer Frühdrucke mit Synchrotronstrahlung. Gutenberg Jahrbuch, 73:231-255, 1998. [ doi ]

F. Adams, K. Janssens, et A. Snigirev. Microscopic X-ray fluorescence analysis and related methods with laboratory and synchrotron radiation sources. J. Anal. At. Spectrom., 13(5):319-331, 1998. [ doi ]

The present status of microprobe versions of XRF analysis with tube excitation and with synchrotron radiation sources is reviewed with respect to analytical parameters such as lateral resolution and imaging capability, and achievable detection limits, precision and accuracy, The main characteristics of the method are contrasted with those of other microanalytical techniques, For laboratory source mu-XRF, results with a rotating anode tube equipped with capillary X-ray optics are discussed in terms of sensitivity and achievable lateral resolution. The possibilities of the new third generation synchrotron radiation storage rings, especially those of the European Synchrotron Radiation Facility (ESRF) and its X-ray micro-fluorescence, imaging and diffraction beamline (ID 22) are discussed and related to second generation storage rings. Some characteristic applications are given to illustrate the recent possibilities of the methodologies, in particular for the characterization of atmospheric particles, and in an analytical problem related to archaeology.

K. Janssens, I. Deraedt, O. Schalm, et J. Veeckman. Composition of 15th-17th century archaeological glass vessels excavated in Antwerp, Belgium. Mikrochim. Acta, 15:253-267, 1998.

In the beginning of the 16th century, Antwerp (Belgium) was one of the largest ports of Europe and an important centre for the manufacture and import of glassware, especially for Venetian and facon-de-Venise glass vessels. As a result, archaeological excavations in the historical centre of Antwerp have yielded a number of important glass finds from the 15th until the 17th century. Within this extensive collection, several typological categories of glass vessels can be distinguished. The major and trace composition of a series of 96 representative glass objects was determined by means of EPXMA (electron probe X-ray micro analysis) and mu-SRXRF (synchroton radiation induced Xray fluorescence analysis). Four major compositional types could be distinguished. The correlation between object composition, colour and type is discussed. Special emphasis is placed on the composition of the facon-de-Venise or Venetian glass objects found in Antwerp and on the comparison of this composition to that of glass of the same type found in other locations in Europe.

P. Barnes, S. L. Colston, A. Jupe, S. Jacques, J. K. Cockcroft, A. Bennet, et C. Hall. Novel applications of energy-dispersive diffraction in materials and industrial science. Dans Proc. 18th Eur. Cryst. Meeting, Prague, 1998.

H. Mommsen, A. Brüning, H. Dittmann, A. Hein, A. Rosenberg, et G. Sarrazin. Recent investigations of early Roman cameo glass. Part 2. X-ray fluorescence analyses induced by synchrotron radiation. Glastech. Ber. Glass. Sci. Technol., 70(7):211-219, July 1997.

The elemental composition of 14 Roman cameo grass fragments was measured quantitatively by X-ray fluorescence analysis induced by synchrotron radiation. The study was intended to learn more about the possible manufacturing techniques of these glasses. In the white cameo decor of nine fragments all belonging to vessels a higher lead oxide concentration was detected compared to the colored body. In contrast, lead oxide is not enhanced in the remaining five fragments from cameo disks or plates. The higher concentrations may be interpreted as flux added to lower the melting temperature of the white cameo layers of the vessels, thus supporting the recent hypothesis that these cameo vessels were manufactured with the help of a mold on a turning wheel, which had not to be used for the production of cameo plates.

I. Nakai, M. Matsunaga, M. Adachi, et K. I. Hidaka. Application of XAFS in archaeology. J. Phys. France IV, 7(C2):1033-1034, April 1997. [ doi ]

X-ray fluorescence XAFS technique was successfully applied to the archaeological study to find colorant elements in old glass samples and to characterize the chemical states of iron in the ceramic sherds excavated from an archaeological site in Turkey. The origin of red color of the mosaic glass is found to be due to the colloidal copper particles in the glass. Blue color is attributed to divalent cobalt. Fe K-XANES spectra revealed that the color of the sherds changes from black, gray, brown, to orange with increasing the absorption edge energy. The gray ceramics typical for Phrygia age were produced in a reducing condition. The cream color of the central Anatolian Iron Age could not be related with the oxidation tate of iron.

P. Dillmann, P. Populus, P. Fluzin, P. Chevallier, E. Elkaim, et G. Béranger. Microdiffraction du rayonnement synchrotron. Identification de phases non métalliques dans les fers anciens. Rev. Metall. Cah. Inf. Techn., 94:267-268, February 1997.

P. Dillmann, P. Populus, P. Chevallier, E. Elkaim, P. Fluzin, G. Béranger, et A. Firsov. Microdiffraction of the synchrotron radiation. Identification of non metallic phases in iron and steel. CR Acad. Sci. II-B, 324:763-772, 1997.

We present a new X-ray microdiffraction method coupled to microfluorescence for phase identification of a sample of 10 mu m in size. This method uses the high brilliance of synchrotron radiation, which allows an X-ray focus of a few square micrometers. Thus, diffraction patterns of 25-mu m inclusions are obtained. We present in this paper an example of application of this method, i.e. the identification of non metallic inclusions in an archaeological iron ingot.

F. Adams, A. Adriaens, A. Aerts, I. de Raedt, K. Janssens, et O. Schalm. Micro and surface analysis in art and archaeology. J. Anal. At. Spectrom., 12(3):257-265, 1997. [ doi ]

A variety of instrumental analytical techniques can be applied to the physical and chemical examination of works of art and archaeology, In this paper, a few examples are discussed of the application of micro-analytical chemistry in this interdisciplinary field, The following subjects from the experience of our laboratory, in collaboration with several specialized institutes, were selected: Early Bronze Age ceramic crucibles, residues and powders from Goltepe, South Central Turkey, have been analysed using surface analytical techniques to investigate potential evidence of tin smelting, The study indicates that the crucibles were used for processing of tin and gives clear evidence of a local tin industry, Roman glass from a collection of objects discovered in Qumran near the Dead Sea was used to study the corrosion of glass objects in a particularly stable environment over a period of nearly 2000 years, The corrosion of a series of glass-in-lead windows from St, Michael and St, Goedele's Cathedral, Brussels, was studied using electron probe microanalysis and micro X-ray fluorescence, New views can be formulated on the corrosion mechanism, which appears to be a complex multiphase process under the influence of atmospheric pollution, A few preliminary results are discussed for the analysis of glass paintings, in particular carnation red glass paints.

P. Dillmann, P. Populus, P. Chevallier, P. Fluzin, G. Béranger, et A. Firsov. Microdiffraction coupled with X-ray fluorescence microprobe, application in archaeometry. J. Trace Microprobe Tech., 15:251-262, 1997.

We present one of the first microdiffraction experiments performed with a photon microprobe. It allows the phase identification in 20 μm size, of inclusions collected in ancient ferrous artefacts.

H. Mommsen, A. Brüning, H. Dittmann, D. Heimermann, A. Hein, A. Rosenberg, et I. Bentchev. Zerstörungsfreie Röntgenfluoreszenzanalyse an Malschichten von Ikonen - Ziele und Möglichkeiten. Dans I. Bentchev et E. Haustein-Bartsch, éds, Ikonen. Restaurierung und Naturwissenschaftliche erforschung. Beiträge des Internationalen Kolloquiums in Recklinghausen 1994, München, Germany, 1997. Editio Maris.

F. Fassbender, H. Dittmann, A. Hein, P. Kretz, M. Lehnen, H. Mommsen, A. Rosenberg, G. Eggert, et U. Sobottka-Braun. Röntgenfluoreszenzanalyse der Lanx von Bizerta, p. 202-212. Rheinland-Verlag GmbH, Köln, Germany, 1997.

Während der Restaurierung der Lanx von Bizerta, eines römischen Silbertabletts aus der Mitte des 2. Jahrhunderts n. Chr., bestand dir Möglichkeit, Röntgenfluoreszenzanalysen am Bonner Beschleuniger ELSA des Physikalischen Institutes durchzuführen. Zielsetzung dieser zerstörungsfrei arbeitenden Elementanalysemethode war es, Beiträge zur Klärung von Fragen zu liefern wie: 1. die Identifizierung von verschiedenen Goldlegierungen und des damit verbundenen Herstellungsverfahrens (z. B. Feuervergoldung) 2. die genaue Zusammensetzung des Basismaterials der Silberplatte 3. die Verwendung von Lotmaterialien und die Bestimmung der Art des Lotverfahrens und 4. die Zusammengehörigkeit des zentralen Teiles der Silberplatte und dem Randbereich mit den zwei Griffplaten.

A. Zappala, S. Bajt, G. E. Gigante, et A. L. Hanson. Applications of EDXRF in the conservation of acid papers using a synchrotron light microbeam. Nucl. Instrum. Methods B, 117(1-2):145-150, August 1996. [ doi ]

Paper can be produced from various raw materials, which give rise to differences in the permanence and durability of the paper product, Modern paper is characterised by a tendency to discolor and become brittle, both problems being generally related to the high acidity of these papers, In order to avoid the loss of historical paper documents to this discoloration and embrittlement, many approaches have been developed to deacidify the high acid papers, However, there is a problem to verify the effectiveness of the different strategies. For this work a synchrotron X-ray microprobe was used to study the distributions of elements, related to the deacidification treatments, within papers treated with specific processes. These elemental distributions can serve as indicators of the effectiveness of each individual process. The microprobe is located at beamline X-26A at the Brookhaven National Laboratory, National Synchrotron Light Source and utilised a 7 X 10 mu m(2) collimated beam of X-rays from the synchrotron. Scans were performed transverse to paper sections to obtain elemental distribution through the sample, Some preliminary results of measurements on treated and untreated paper samples are presented.

H. Mommsen, H. Dittmann, A. Hein, et A. Rosenberg. X-ray fluorescence analysis induced by synchrotron radiation (SYXRF) and first archaeometric applications. Dans D. Dirksen et G. von Bally, éds, Optical Technologies in the Humanities, Selected Contributions to the Int. Conf. on New Technologies in the Humanities and 4th Int. Conf. on Optics Within Life Sciences OWLS IV, 9-13 July 1996, Münster, Germany, July 1996. Springer.

K. Janssens, A. Aerts, L. Vincze, F. Adams, C. Yang, R. Utui, K. Malmqvist, K. W. Jones, M. Radtke, S. Garbe, F. Lechtenberg, A. Knöchel, et H. Wouters. Corrosion phenomena in electron, proton and synchrotron X-ray microprobe analysis of Roman glass from Qumran, Jordan. Nucl. Instrum. Methods B, 109:690-695, April 1996. [ doi ]

A series of 89 glass fragments of Roman glass are studied using electron, proton and synchrotron radiation induced X-ray emission from microscopic areas on the sample surface. The glass originates from Qumran, Jordan and was buried for 1900 years. The weathering layers that result from the extended contact with ground water have been studied, next to the trace composition of the original glass of these pieces. The latter information indicates that at Qumran, large quantities of glass objects were being used in Ancient times. Cross-sectional profiles of the glass show a complex migration behaviour of various groups of major and trace elements.

H. Mommsen, T. Beier, H. Dittmann, D. Heimermann, A. Hein, A. Rosenberg, M. Boghardt, E.-M. Hanebutt-Benz, et H. Halbey. X-ray fluorescence analysis with synchrotron radiation on the inks and papers of Incunabula. Archaeometry, 38(2):347-357, 1996.

Non-destructive X-ray fluorescence analyses induced by white synchrotron radiation (SYXRF) have been performed on a page of the Gutenberg Bible and 21 other different single leaves printed in the year 1470 to 1500. Absolute elemental areal densities for the papers and inks are reported. The known high Cu and Pb content in Gutenberg's ink is confirmed. The elemental composition of the other inks, if measurable by XRF at all, are in general very low, governed only by a few additional elements and found to be not distinctive for a known printer. This will render an identification of the printer or printing offices by ink composition analysis in the period after 1470 difficult.

K. Janssens, L. Vincze, B. Vekemans, A. Aerts, F. Adams, K. W. Jones, et A. Knöchel. Synchrotron radiation induced X-ray microfluorescence analysis. Mikrochim. Acta, 13:87-115, 1996.

μ-XRF is the microscopic equivalent of the well-established multielement analytical technique. In this paper, after comparing the interaction of X-ray photons, electrons and protons with matter and an introduction to synchrotron rings and microfocussing of X-rays, the instrumentation for μ-XRF is discussed, both for laboratory source and synchrotron based setups and the analytical characteristics of μ-XRF are contrasted to that of other microanalytical techniques, Also, this issue of quantification of μ-XRF data is addressed; the applicability of the method in archeological and geological analysis is illustrated.

I. Nakai. Synchrotron radiation X-ray fluorescence analysis of cultural properties. Dans Int. Symp. on Conservation and Restoration of Cultural Property - Spectroscopic Examination in Conservation, 1996.

P. F. Schofield, G. Cressey, W. Wren Howard, et C. M. B. Henderson. Origin of color in iron and manganese containing glasses investigated by synchrotron radiation. Glass Technol., 36(3):89-94, June 1995.

The origin of colour in medieval glasses from Northern Europe has been shown to be an artifact of the oxidation states of small concentrations of Fe and Mn added as impurities in the alkali source. With a view to studying this phenomenon we have produced a sequence of Fe and Mn doped glasses, produced under different degrees of oxidation, displaying a colour range from purple through sepia, yellow, green and blue. Utilising the element specificity of X-ray absorption spectroscopy we have been able to quantify the Fe3+/Sigma Fe and Mn3+/Sigma Mn ratios by spectral simulation of 2p absorption spectra. Fe3+/Sigma Fe changes from 0.53 in the sepia glass to 0.15 in the blue glass, while it appears that the Mn3+/Sigma Mn ratio remains unaffected by the various oxidation conditions with an approximately constant value of 0.19.

L. Capasso, G. Di Tota, K. W. Jones, et C. Tuniz. Synchrotron radiation microprobe analysis of Human dental calculi from an archaeological site: a new possible perspective in palaeonutrition studies. Int. J. Osteoarchaeol., 5:282-288, 1995.

The X-ray microprobe at beamline X-26 of the National Synchrotron Light Source (Brookhaven National Laboratory) has been used to determine minor and trace elements in small fragments of dental calculi. This material was removed from 11 individuals found in the Norman necropolis discovered recently under the church of San Lorenzo di Aversa (Caserta, southern Italy, ca. AD 900-1200). the aim of these experiments is to develop new methods for non-destructive analysis of organic archaeological materials in studies of palaeonutrition and palaeopathology. These preliminary analyses show little variability in the main trace elements of dietary significance, such as Sr and Zn.

S. Li, X. J. Li, X. H. Wu, F. H. Sheng, et G. D. Li. Synchrotron-radiation study of the relic bones of Bao Zheng. Chin. Sci. Bull., 38:812-815, 1993.

I. Nakai et A. Iida. Applications of SR-XRF imaging and micro-XANES to meteorites, archaeological objects and animal tissues. Dans C. S. Barrett, J. V. Gilfrich, T. C. Huang, R. Jenkins, G. J. McCarthy, P. K. Predecki, R. Ryon, et D. Smith, éds, Advances in X-ray analysis, vol. 35, p. 1307-1315. Plenum Press, New-York, USA, 1992.

I. Brissaud, P. Chevallier, C. Dardenne, N. Deschamps, J. P. Frontier, K. Gruel, A. Taccoen, A. Tarrats, et J. X. Wang. Analysis of Gaulish coins by proton induced X-ray emission, synchrotron radiation X-ray fluorescence and neutron activation analysis. Nucl. Instrum. Methods B, 49(1-4):305-308, 1990. [ doi ]

Recent diggings in Brittany provide us with new Gaulish coins for a further study about their value and dating. The elemental analysis gives a good idea of the great variety in the monetary alloys used in Gallia in the second part of the first century B.C. Each coin was analyzed by surface and volume techniques. For some samples the discrepancy between the two types of analysis is large for Ag-rich alloys: a surface enrichment in silver is observed.

I. Brissaud, J. X. Wang, et P. Chevallier. Synchrotron radiation induced X-ray fluorescence at LURE. J. Radioanal. Nucl. Chem., 131(2):399-413, June 1989. [ doi ]

Advantages of X-ray fluorescence with the use of Synchrotron Radiation are emphasized (intensity, polarization, tunability of energy). The experimental set-up and the fast computer system for the data reduction without standards are presented. The results are in good agreement with standard references. Examples of applications are presented: old coins and potteries were studied in archaeological domain; metal alloys were analyzed; element composition of bulk samples of volcanic rocks, sublimates and aerosols were determined.

G. Harbottle, B. M. Gordon, et K. W. Jones. Use of synchrotron radiation in archaeometry. Nucl. Instrum. Methods B, 14(1):116-122, January 1986. [ doi ]

A synchrotron X-ray producing device such as the National Synchrotron Light Source at Brookhaven National Laboratory will present the research worker in the field of archaeometry with a number of new possibilities. These derive from the fundamental characteristics of the extracted X-ray beam: (a) its extraordinary intensity, four to five orders of magnitude greater than that of bremsstrahlung produced by X-ray tubes, (b) its polarization in the plane of the synchrotron ring and, (c) its energy tunability.Among the archaeometric applications one may readily identify: (a) very fast, sensitive, bulk analyses of materials such as ceramic and stone, for provenance research, (b) spot (microprobe) analytical capability, for obtaining structural information on artifacts, (c) scanning applications leading to images of the distributions of particular elements and, (d) element speciation on a micro scale. There is every reason to believe that this instrument will quickly take a prominent place in archaeometric research.