Éditeur(s) : HAL CCSD E Schweizerbart Science Publishers
Résumé : Mafic microgranular enclaves produced by co-mingling between minette and syenite magmas are found in the Piquiri Syenite, southern Brazil. These enclaves were crystallized under upper mantle conditions. K-clinopyroxene and pyrope are among the early-crystallized phases, suggesting an initial pressure around 5GPa. The mineralogy of minettes comprises phenocrysts of magnesium biotite and diopside, occasionally apatite, in a groundmass formed by these minerals plus alkali feldspar. Two types of apatites are observed: (i) euhedral grains, as inclusions or groundmass constituents, and (ii) aciculate crystals formed during undercooling of mafic magma. Substitutional schemes suggested for these apatites are Si ⇆ P in the tetrahedral site, and Sr and LREE replacing Ca. La, Ce, Nd, and Sr concentrations reveal that these elements are extremely enriched in apatite. Partition coefficients between early-crystallized apatites and estimated melt compositions are DLa (11.8 - 30.6), DCe (16.1-33), DNd (12-31) and DSr (5.1-8.2). Apatite concentrates the LREE up to 200 times compared to clinopyroxene, even higher values were determined for ap/mica partitioning. The ap/cpx and ap/mica partition coefficients for undercooled minerals are close to the values determined for the near-liquidus phases, which indicates constant behavior of LREE and Sr between apatite-clinopyroxene-mica parageneses and minette liquids. Furthermore, these partitioning data preclude any chemical diffusion of these elements between minette and syenite magmas during co-mingling.
ISSN: 0935-1221

hal-00407602
https://hal.archives-ouvertes.fr/hal-00407602
DOI : 10.1127/0935-1221/2007/0019-0039

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 American Chemical Society
Résumé : Absolute Mα and Mβ X-ray intensities were measured for the elements Pt, Au, Pb, U, and Th by electron impact for energies ranging from 6 to 38 keV. Experimental data were obtained by measuring the X-ray intensity emitted from bulk samples with an electron microprobe using high-resolution wavelength-dispersive spectrometers. Recorded X-ray intensities were converted into absolute X-ray yields by evaluation of the detector efficiency and then compared with X-ray intensities calculated by means of Monte Carlo simulations. Simulated Mα and Mβ X-ray intensities were found to be in good agreement with the measurements, allowing their use in standardless quantification methods. A procedure and a software program were developed to accurately obtain virtual standard values. Standardless quantifications of Pb and U were tested on standards of PbS, PbTe, PbCl2, vanadinite, and UO2.
ISSN: 0003-2700

hal-01217495
https://hal.archives-ouvertes.fr/hal-01217495
DOI : 10.1021/acs.analchem.5b01443

Éditeur(s) : HAL CCSD Cambridge University Press (CUP)
Résumé : International audience
ISSN: 1431-9276

hal-00411439
https://hal.archives-ouvertes.fr/hal-00411439

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 European Geosciences Union
Résumé : During the Neoproterozoic orogeny, the middle crust of the Araçuaí belt underwent widespread partial melting. At the regional scale, this anatectic domain is characterized by a progressive rotation of the flow direction from south to north, suggesting a 3-D deformation of the anatectic middle crust. To better determine whether melt volumes present in the anatectic middle crust of the Araçuaí orogen were large enough to allow a combination of gravity-driven and convergence-driven deformation, we used the titanium-in-quartz (TitaniQ) geothermometer to estimate the crystallization temperatures of quartz grains in the anatectic rocks. When possible, we compared these estimates with thermobarometric estimates from traditional exchange geothermobarometers applied to neighboring migmatitic kinzigites. TitaniQ temperatures range from 750 to 900 °C, suggesting that quartz starts crystallizing at minimum temperatures of ≥ 800 °C. These results, combined with the bulk-rock chemical composition of diatexites, allows the estimation of a minimum of ~ 30% melt and a corresponding viscosity of ~ 109–1010 Pa s. Such a minimum melt content and low viscosity are in agreement with interconnected melt networks observed in the field. Considering that these characteristics are homogeneous over a wide area, this supports the finding that the strength of the middle crust was severely weakened by extensive partial melting, making it prone to gravity-driven flow and lateral extrusion.
ISSN: 1869-9510

hal-01116434
https://hal.archives-ouvertes.fr/hal-01116434
DOI : 10.5194/se-5-1223-2014

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 IOP Publishing
Résumé : International audience
M-subshell ionization cross sections of U by electron impact with kinetic energies between 4 and 38 keV were determined experimentally. The cross sections have been deduced from high-resolution measurements of the M x-ray emission spectra resulting from the radiative decay of M-subshell vacancies. The experimental cross sections are compared with cross sections calculated within the plane- and distorted-wave Born approximations. The predictions of the distorted-wave Born approximation represent experimental measurements well within experimental errors.
ISSN: 0953-4075

hal-01054329
https://hal.archives-ouvertes.fr/hal-01054329
DOI : 10.1088/0953-4075/47/5/055202

Éditeur(s) : HAL CCSD Wiley-Blackwell
Résumé : International audience
Absolute Mα x-ray production cross sections have been measured and calculated for heavy elements Au, Pb, Bi, and U for electron incident energies from the ionization threshold up to 38 keV. The experimental cross sections were deduced from M x-ray intensities emitted from ultrathin samples of the elements of interest deposited onto self-supporting C films. The measurements were performed using two electron microprobes and several wavelength-dispersive spectrometers. X-ray intensities were converted into x-ray production cross sections by using estimated values of the number of incident electrons, target thickness, and spectrometer efficiency. Experimental results are compared with calculated cross sections using different predictive formulae. Good agreement is found between the measured cross sections and the predictions from the distorted-wave Born approximation, which indicates that this approximation is suited for the calculation of M-shell ionization cross sections of heavy elements.
ISSN: 0142-2421

hal-01122839
https://hal.archives-ouvertes.fr/hal-01122839
DOI : 10.1002/sia.5561

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 IOP Publishing
Résumé : We present the results of an inter-laboratory comparison of EPMA analysis at low voltage (5-6 kV) of three monophasic alloy steel samples. The aim of the work was to obtain an estimate of the present situation of low-voltage analysis of steel and identify needs for improvement. EPMA analyses of the samples were conducted by seven participant groups using electron microprobes and scanning electron microscopes of different kind, equipped with wavelength- and/or energy-dispersive X-ray spectrometers, and employing their own methodology of analysis. The results using WDS showed essentially an underestimation of the Cr contents, with relative deviations from the reference values ranging from -0.7 % to -17 %, and an overestimation of Fe and Ni, with relative deviations from the reference composition ranging from -4 % to +30 %, and from +14 % to +42 %, respectively. The relative deviations obtained by using EDS showed larger scatter, ranging from -16 % to +54 % for Cr, -0.4 % to +66 % for Fe and from +13 % to +90 % for Ni. Reasons for the differences observed and the scatter of results are discussed.
ISSN: 1757-8981

hal-00813999
https://hal.archives-ouvertes.fr/hal-00813999
DOI : 10.1088/1757-899X/32/1/012014

Éditeur(s) : HAL CCSD Springer Verlag
Résumé : International audience
A calibration method aimed at converting X-ray intensities into absolute units has been tested in different electron microprobes. The calibration requires measurement of the X-ray peak profile and measurement and calculation of the bremsstrahlung intensity emitted from a reference sample, at the energy of the X-ray line of interest. Specifically, measurements of the U M alpha and M beta lines emitted from UO2 and bremsstrahlung intensities emitted from an Al reference sample have been performed on five different instruments. The aim of the work is to determine to what accuracy X-ray intensities emitted from reference samples of actinide elements are transferable among different electron microprobes (virtual standard). The influence of the focussing geometry and different crystals and proportional counters used is analysed. Strategies to reduce the uncertainties affecting the absolute calibration of the studied lines are discussed.
ISSN: 0026-3672

hal-00411437
https://hal.archives-ouvertes.fr/hal-00411437
DOI : 10.1007/s00604-007-0856-2

Éditeur(s) : HAL CCSD American Physical Society
Résumé : International audience
Absolute M-shell x-ray production cross sections have been measured and calculated for Au and Bi for electron incident energies from close to the ionization threshold up to 38 keV. The experimental cross sections were deduced from M alpha x-ray intensities emitted from ultrathin Au and Bi samples deposited on self-supporting C films. The measurements were performed on an electron microprobe using several wavelength-dispersive spectrometers. The x-ray production cross sections were also evaluated theoretically using ionization cross sections calculated from the plane-wave and the distorted-wave Born approximations. Experimental results are compared with the calculated cross sections and also with the results of two analytical formulas widely used in many applications. Good agreement is found between the measured cross sections and the predictions from the distorted-wave Born approximation, which indicates that this approximation is suited for the calculation of M-shell ionization cross sections of heavy elements.
ISSN: 1050-2947

hal-00411432
https://hal.archives-ouvertes.fr/hal-00411432
DOI : 10.1103/PhysRevA.78.022704

Éditeur(s) : HAL CCSD Cambridge University Press (CUP)
ISSN: 1431-9276

hal-00411187
https://hal.archives-ouvertes.fr/hal-00411187
DOI : 10.1017/S1431927608083414

Éditeur(s) : HAL CCSD IOP Publishing
Résumé : Absolute L- and M-subshell x-ray production cross sections of Pb have been measured for incident electron energies ranging from 3 to 38 keV. The experimental cross sections were obtained by measuring Lα, Lβ, Mα, Mβ and Mγ x-ray intensities emitted from ultrathin Pb films deposited onto self-supporting thin C films. Measurements were performed on two electron microprobes using wavelength-dispersive spectrometers. X-ray intensities were converted into x-ray production cross sections by using estimated values of the number of incident electrons, target thickness and spectrometer efficiency. Experimental results are compared with calculated cross sections obtained using different predictive formulae, and, whenever possible, with experimental data from the literature.
ISSN: 0953-4075

hal-00858079
https://hal.archives-ouvertes.fr/hal-00858079
DOI : 10.1088/0953-4075/46/11/115202