Éditeur(s) : HAL CCSD Institute of Electrical and Electronics Engineers (IEEE) Institute of Electrical and Electronics Engineers
Résumé : International audience
Conventional quantitative electron probe microanalysis of actinides requires the use of reference standard samples. However, for such elements, standards are generally not available. To overcome this difficulty, standardless methods of analysis are used, in which the x-ray intensity emitted by the standard is calculated. To be reliable, such calculations require accurate knowledge of physical data such as the x-ray production cross section. However, experimental data of this quantity are not always available for actinide elements. In the present work, experimental L and M x-ray production cross sections were measured for elements uranium and lead. Measurements were performed with two electron microprobes using wavelength-dispersive spectrometers using thin self-supporting targets. Experimental results are compared with calculated cross sections obtained from different analytical formulae, and, whenever possible, with experimental data obtained from the literature.
ISSN: 0018-9499

hal-01122820
https://hal.archives-ouvertes.fr/hal-01122820
DOI : 10.1109/TNS.2014.2321016

Éditeur(s) : HAL CCSD
Résumé : Submitted to the Journal of Mathematical Analysis and Applications
International audience
We present new types of regularity for nonlinear generalized functions, based on the notion of regular growth with respect to the regularizing parameter of Colombeau's simplified model. This generalizes the notion of G^{ infty }-regularity introduced by M. Oberguggenberger. A key point is that these regularities can be characterized, for compactly supported generalized functions, by a property of their Fourier transform. This opens the door to microanalysis of singularities of generalized functions, with respect to these regularities. We present a complete study of this topic, including properties of the Fourier transform (exchange and regularity theorems) and relationship with classical theory, via suitable results of embeddings.
J. Math. Anal. Appl.

Droits : info:eu-repo/semantics/OpenAccess
hal-00020280
https://hal.archives-ouvertes.fr/hal-00020280
https://hal.archives-ouvertes.fr/hal-00020280/document
https://hal.archives-ouvertes.fr/hal-00020280/file/ADelcroixGRegularJan27.pdf
ARXIV : math/0603183

Éditeur(s) : HAL CCSD Wiley
Résumé : We report new measurements of the surface ionization Phi(0) for Ge K alpha and L alpha X-rays on an Fe substrate, Ga K alpha and L alpha X-rays on an Ni substrate, and Au M alpha X-rays on Si, W and Ta substrates. The measurements were performed using the tracer technique for electron incident energies ranging from the ionization threshold up to about 40 keV. Improvements in sample preparation and in the X-ray measurement technique enabled surface ionization values to be obtained with uncertainties less than 2%. Simulations of Phi(0) for the studied cases were performed using the general-purpose Monte Carlo (MC) code PENELOPE. Experimental measurements are compared with simulation results and with the results of several predictive formulae widely used in electron probe microanalysis and Auger electron spectroscopy (AES). The accuracy of the reported measurements makes it possible to assess the reliability of the different calculations for incident electron energies below 10 keV.
ISSN: 0049-8246

hal-00617775
https://hal.archives-ouvertes.fr/hal-00617775
DOI : 10.1002/xrs.1294

Éditeur(s) : HAL CCSD Royal Society of Chemistry
Résumé : International audience
Low-level water measurements of geological materials are fundamental in understanding the volatile inventories of the Earth from the mantle to crustal reservoirs. Here we describe the development of microanalytical techniques using the new SHRIMP SI ion microprobe to measure the abundances of OH− (as a proxy for water) in volcanic glass and nominally anhydrous minerals (NAMs). Samples were first analysed at the Carnegie Institute of Washington (CIW) on their Cameca ims-6f with calibrations based on previous FTIR and manometry analyses. SHRIMP SI is a large geometry ion microprobe and is currently mainly used for O and S isotope analyses. The analytical protocol used here incorporates multiple collection of 16O− and 16O1H− allowing rapid measurements. A single calibration line incorporating all glasses and NAMs for the SHRIMP SI allows calibration of 16O1H−/16O− to H2O over a wide range in concentration (50 to 15 000 ppm H2O). This calibration line has around a 10% uncertainty, which appears to be limited only by sample heterogeneity. The current background for SHRIMP analysis is between 20–40 ppm but this is expected to improve with improved pumping on the source chamber. A current limitation to water analysis of NAM samples, by any technique, is having a range of standard materials to enable OH− calibration to absolute H2O concentrations. Data are presented for 7 NAM samples (2 olivines, 2 orthopyroxenes and 3 clinopyroxenes) that appear to be promising as potential standards for international laboratory H2O measurements. These NAM samples have been analysed and characterised here by SHRIMP SI, FTIR, EMP and the Cameca ims-6f ion microprobe at CIW. Four of these samples have previously been measured by manometry to determine absolute H2O concentrations.
ISSN: 0267-9477

hal-01243514
https://hal.archives-ouvertes.fr/hal-01243514
DOI : 10.1039/c5ja00047e

Éditeur(s) : HAL CCSD Cambridge University Press (CUP)
Résumé : International audience
XFILM is a computer program for determining the thickness and composition of thin films on Substrates and multilayers by electron probe microanalysis. In this study, we describe the X-ray emission model implemented in the latest version of XFILM and assess its reliability by comparing measured and calculated k-ratios from thin-film samples available in the literature. We present and discuss examples of applications of XFILM that illustrate the capabilities of the program.
ISSN: 1431-9276

hal-00475542
https://hal.archives-ouvertes.fr/hal-00475542
DOI : 10.1017/S1431927609991218

Éditeur(s) : HAL CCSD SAGE Publications (UK and US)
Résumé : International audience
In this article, we focus on hypomaturation autosomal-recessive-type amelogenesis imperfecta (type IIA2) and describe 2 new causal Matrix metalloproteinase 20 (MMP20) mutations validated in two unrelated families: a missense mutation p.T130I at the expected homozygous state, and a compound heterozygous mutation having the same mutation combined with a nucleotide deletion, leading to a premature stop codon (p.N120fz*2). We characterized the enamel structure of the latter case using scanning electron microscopy analysis and microanalysis (Energy-dispersive X-ray Spectroscopy, EDX) and confirmed the hypomaturation-type amelogenesis imperfecta as identified in the clinical diagnosis. The mineralized content was slightly decreased, with magnesium substituting for calcium in the crystal structure. The anomalies affected enamel with minimal inter-rod enamel present and apatite crystals perpendicular to the enamel prisms, suggesting a possible new role for MMP20 in enamel formation.
ISSN: 0022-0345

hal-01545484
https://hal.archives-ouvertes.fr/hal-01545484
DOI : 10.1177/0022034513488393

Éditeur(s) : HAL CCSD IOP Publishing
Résumé : The use of electron probe microanalysis (EPMA) at low voltage allows improvements in the lateral resolution and surface sensitivity of the technique down to the sub-micrometre scale, and it is also useful in minimizing X-ray absorption (for the analysis of ultra-light elements), charging effects and secondary fluorescence. However, EPMA at low voltage is accompanied by a number of problems which may affect the accuracy of quantitative results. A large number of these problems arise from the need of using low-energy X-ray lines such as L- and M-lines, which have low fluorescence yields, large uncertainties in the mass attenuation coefficients, and are affected by several spectroscopic difficulties (e.g., peak shifts and overlaps). Other factors that play an important role at low voltage are carbon contamination, surface oxidation, the quality of sample polishing, the influence of a conductive coating and the limitations of matrix correction procedures. In this paper, we illustrate the capabilities of EPMA at low voltage and we examine in detail the different sources of uncertainty that may affect the accuracy of quantitative results.
ISSN: 1757-8981

hal-00767564
https://hal.archives-ouvertes.fr/hal-00767564
DOI : 10.1088/1757-899X/32/1/012016

Éditeur(s) : HAL CCSD American Geophysical Union
Résumé : International audience
We performed 31 friction experiments on glassy basalts (GB) and glass-free basalts (GFB) at slip rates up to 6.5 m s−1 and normal stress up to 40 MPa (seismic conditions). Frictional weakening was associated to bulk frictional melting and lubrication. The weakening distance (Dw) was about 3 times shorter in GB than in GFB, but the steady state friction was systematically higher in GB than in GFB. The shorter Dw in GB may be explained by the thermal softening occurring at the glass transition temperature (Tg ~500°C), which is lower than the bulk melting temperature (Tm ~1250°C) of GFB. Postexperiment microanalyses suggest that the larger crystal fraction measured in GB melts results in the higher steady state friction value compared to the GFB melts. The effect of interstitial glass is to facilitate frictional instability and rupture propagation in GB with respect to GFB.
ISSN: 0094-8276

hal-01054139
https://hal.archives-ouvertes.fr/hal-01054139
DOI : 10.1002/2013GL058601

Éditeur(s) : HAL CCSD Elsevier
Résumé : International audience
The oxygen fugacity and therefore the iron redox state of a melt is known to have a strong influence on the liquid line of descent of magmas and thus on the composition of the coexisting melts and crystals. We present a new method to estimate this critical parameter from electron probe microanalyses of two of the most common minerals of basaltic series, plagioclase and clinopyroxene. This method is not based on stoichiometric calculations, but on the different partitioning behaviour of Fe3+ and Fe2+ between both minerals and a melt phase: plagioclase can incorporate more Fe3+ than Fe2+, while clinopyroxene can incorporate more Fe2+ than Fe3+. For example, the effect of oxidizing a partly molten basaltic system (Fe3+ is stabilized with respect to Fe2+) results in an increase of FeOtotal in plagioclase, but a decrease in the associated clinopyroxene. We propose an equation, based on published partition coefficients, that allows estimating the redox state of a melt from these considerations. An application to a set of experimental and natural data attests the validity of the proposed model. The associated error can be calculated and is on average <1 log unit of the prevailing oxygen fugacity.;In order to reduce the number of different variables influencing the Fe2+/Fe3+ mineral/melt equilibrium, our model is restricted to basaltic series with SiO2<60% that have crystallized at intermediate to low pressure (<0.5 GPa) and under relatively oxidizing conditions (Delta FMQ>0; where FMQ is the fayalite-magnetite-quartz oxygen buffer equilibrium), but it may be parameterized for other conditions. A spreadsheet is provided to assist the use of equations, and to perform the error propagation analysis.
ISSN: 0377-0273

hal-00475550
https://hal.archives-ouvertes.fr/hal-00475550
DOI : 10.1016/j.jvolgeores.2009.11.023

Éditeur(s) : HAL CCSD Royal Society of Chemistry
Résumé : International audience
LA-ICP-MS analysis of the chemical composition of biogenic carbonate has many applications in the environmental sciences but the characteristics of the material produced by the ablation process are largely unknown. To fill this gap, we have undertaken a study of the chemical and physical nature of particles produced by laser ablation of biogenic carbonates. SEM imaging suggests that laser ablation produces two distinct particle populations, one consisting of microsize particles and the other of nanosize particles. A 213 nm laser gives rise to a higher proportion of microsize particles than a 193 nm laser, probably because the 213 nm laser couples less completely with carbonate material. The microsize particles appear to form by photomechanical fracturing along lines of cleavage or weakness, rather than by hydrodynamic sputtering (as is generally observed for silicates). Chemical analysis of the carbonate particles suggests that little chemical fractionation of biogenic carbonates occurs during the ablation process or during transport to the plasma. This is supported by the constancy of the fractionation factor ([X/Ca](measured)/[X/Ca] true) during the course of an ablation of a carbonate standard. In contrast, changes in the fractionation factor during the first few seconds of ablation of the NIST 612 are observed for some elements. This difference in fractionation is likely to result from the different formation mechanisms of the microsize particles.
ISSN: 0267-9477

hal-00411933
https://hal.archives-ouvertes.fr/hal-00411933
DOI : 10.1039/b706727e

Éditeur(s) : HAL CCSD AGU and the Geochemical Society
Résumé : International audience
The ODP/IODP multileg campaign at ODP Site 1256 (Cocos plate, eastern equatorial Pacific) provides the first continuous in situ sampling of fast spreading ocean crust from the extrusive lavas, through the sheeted dikes and down into the uppermost gabbros. This paper focuses on a detailed petrographic and microanalytical investigation of the gabbro section drilled during IODP Expedition 312. The marked patchy and spotty features that can be observed in many Hole 1256D gabbros is mostly due to a close association of two different lithological domains in variable amounts: (1) subophitic domains and (2) a granular matrix. Major and trace element mineral compositions, geothermometry, and petrological modeling suggest that subophitic and granular domains follow one single magma evolution trend formed by in situ fractionation. The subophitic domains correspond to the relative primitive, high-temperature end-member, compositionally similar to the basalts and dikes from the extrusive unit upsection, while the granular domains fit with a magma evolution by crystal fractionation to lower temperatures, up to a degree of crystallization of similar to 80%. Our results support the following scenario for the fossilization of the axial melt lens at ODP Site 1256: relatively primitive MORB melts under near-liquidus conditions fill the melt lens and feed the upper, extrusive crust. Near the melt lens-sheeted dike boundary at lower temperatures, crystallization starts with first plagioclase before clinopyroxene in a mushy zone forming the subophitic domains. At decreasing temperatures, the subophitic domains continue to crystallize, finally forming a well-connected framework. Evolved, residual melt is finally trapped within the subophitic network, crystallizing at near-solidus conditions to the granular matrix. Another important textural feature in Hole 1256D gabbros is the presence of microgranular domains which are interpreted as relics of stoped/assimilated sheeted dikes (transformed to "granoblastic dikes" by contact metamorphism). All these different domains can be observed in close association, often at the thin section scale, demonstrating the extremely complex petrological record of combined crystallization/assimilation processes ongoing in the axial melt lens. Very similar gabbros with a marked spotty/patchy appearance, and bearing the same close association of lithological domains as observed at Site 1256, are known in the so-called "varitextured gabbro" unit from the Oman Ophiolite located at the same structural level, between cumulate gabbros and granoblastic dikes. The close petrological similarity of the gabbro/dike transition between both IODP Hole 1256D and the Oman ophiolite suggests that in situ fractionation and dike assimilation/contamination are major magmatic processes controlling the dynamics and fossilization of the axial melt lens at fast spreading oceanic ridges.
ISSN: 1525-2027

hal-00644798
https://hal.archives-ouvertes.fr/hal-00644798
DOI : 10.1029/2011GC003655