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 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 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 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 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 : 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

Éditeur(s) : HAL CCSD
Résumé : Geological storage of CO2 is one of diverse technologies being explored to reduce atmospheric carbon fromindustrial processes (i.e. fossil fuel combustion). One of the specific features of CO2 injection is the possibility ofgeochemical reactions (dissolution – precipitation) between mobile reactive brine (e.g. formation water enrichedin CO2) and the host rock during the spatial and temporal evolution of CO2. That leads to modifications in thepore structure, which in turn change the flow dynamics of the reservoir (e.g. the permeability k). Then, thesesstructural modifications can largely control the injectivity, so that the pressure field in the reservoir and also theCO2 propagation. Accordingly, it is crucial to explore the changes in the reservoir properties (e.g. structural andhydrodynamic) induced during a CO2 injection and specially the relationships between them (e.g. k or reactivesurface-Sr versus porosity-φ , k versus rock heterogeneity), for developing predictive modelling tools of thetransport and reaction processes occurring during a CO2 injection and reliable risk assessment. In the case ofcarbonate rocks, the application of the predictive models of transport and reaction is still challenging, because oftheir high heterogeneity so that the incertitude in the reaction kinetics of carbonate minerals.From this perspective, we realized brine-enriched in CO2 percolation experiments through carbonate rocksamples in thermodynamic conditions expected during CO2 injection in deep reservoirs (T = 100°C et P =12MPa). The permeability changes k(t) is monitored during the experiments and the porosity variationφ (t) iscalculated from chemical analyses of the sampled outlet fluids, using ICP-EAS. The pore structure modificationsare investigated from high resolution X ray micro tomography images acquired from the synchrotron ofGrenoble (ESRF). Depending to the dissolution regime, controlled by the reservoir rock fabric and the chemicalcomposition of the brine (e.g. PCO2), we observed that a modification of pore structure can either improve(atypical result in dissolution context) or impair the value of the permeability k.
Le stockage géologique du CO2 est l’une des diverses technologies étant explorées afin deréduire les émissions de carbone atmosphérique des processus industriels (i.e. combustion del’énergie fossile). L’une des spécifiques caractéristiques de l’injection du CO2 en profondeurreste la possibilité de réactions géochimiques (dissolution-précipitation) entre la saumureréactive mobile (e.g. eau de formation enrichie en CO2) et la roche encaissante durantl’évolution spatiale et temporelle du CO2, conduisant à des modifications dans la structure despores et par conséquent dans les propriétés d’écoulement du réservoir (e.g. la perméabilité k).Donc, ces changements structuraux peuvent largement contrôler l’injectivité, ainsi que lechamp de pression dans le réservoir et aussi la propagation du CO2. Il demeure ainsi cruciald’explorer les changement dans les propriétés de réservoirs (e.g. structurales ethydrodynamiques) induits durant une injection de CO2 et explicitement les relations existantesentre eux (e.g. k ou surface réactive-Sr versus porosité-φ , k versus hétérogénéité de la roche),afin de développer des outils de modélisation prédictive des processus de transport etréactionnels se produisant durant une injection de CO2 et d’évaluer de façon fiable les risques.Dans le cas des réservoirs carbonatés, l’application des modèles prédictifs de transport réactifdemeure toujours un enjeu, car contrainte par la forte hétérogénéité en leur sein ainsi que parl’incertitude dans la cinétique de réactions des minéraux carbonatés dans ce contexte. Danscette optique, nous avons réalisé des expériences de percolation à travers des échantillons deroches carbonatées dans les conditions thermodynamiques de stockage en profondeur (T =100°C et P =12 MPa). L’évolution de la perméabilité k(t) est suivie au cours desexpériences ; et la variation de la porosité φ (t) est calculée à partir des résultats d’analyseschimiques au ICP-AES des fluides de sortie échantillonnés. L’investigation des modificationsapportées à la structure des pores est réalisée par le biais de la Micro-Tomographie hauterésolution à rayon X, acquise au synchrotron de Grenoble (e.g. ESRF).Dépendant du régime de dissolution, contrôlé par la fabrique de la roche réservoir et lacomposition chimique de la saumuré chargée en CO2 (e.g. PCO2 engagée), on a observéqu’une modification de la structure de la roche peut soit améliorer soit détériorer (résultatatypique en contexte de dissolution) la valeur de la perméabilité k.
https://hal.archives-ouvertes.fr/tel-01142136

tel-01142136
https://hal.archives-ouvertes.fr/tel-01142136
https://hal.archives-ouvertes.fr/tel-01142136/document
https://hal.archives-ouvertes.fr/tel-01142136/file/thesemangane2013.pdf

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 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