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International audience; One of the challenges in the study of foam transport in 3D porous media is having an adequate spatial and temporal resolution, to get a better understanding of the local phenomenon at the pore scale in a non-destructive way. We present an experimental study in which ultra fast X-Ray microtomography is used to characterize the foam trapping while the foam is flowing in a 3D porous medium. A preformed aqueous foam is injected into a rotating cell containing a 3D granular medium made of silica grains. The use of rotating seals allows the cell to rotate continuously at the rate of one revolution per second, compatible with the fast X-ray tomography at SOLEIL synchrotron. We visualize the foam flow and track the trapping of bubbles with an acquisition time of about one second and a spatial resolution of a few microns (pixel size of one micron). This allows us to extract characteristics and reliable statistics about trapped bubbles inside the granular medium and to observe their local behavior. With this setup and technique we access to the dynamics of foam trapping during the flow and the texture variations of the foam in the trapped zones. These local trapping events are well correlated with the macroscopical measurement of the pressure gradient over the cell.

International audience; In this study, three clinopyroxene-enriched upper mantle xenoliths, petrographically classified as wehrlite,were investigated from the Nógrád–Gömör Volcanic Field with the use of X-ray microtomography. Our main goal was toquantify the volume of the glass phase and the vesicles to reveal their three-dimensional distribution. Among the studiedwehrlite xenoliths, one is weakly and two are strongly metasomatized. The two latter wehrlite xenoliths are characterizedby higher modal amount of glass and vesicles, which suggests a genetic connection between glass and concomitantvesicles, and the metasomatic agent. The glass, which was a melt at mantle conditions, forms an interconnected network.This may explain the presence of the electromagnetic anomaly with high electrical conductivity beneath the study area.Our study contributes to the better understanding of melt migration and its metasomatic effect in the lithospheric mantlebeneath monogenetic volcanic fields

In this work, unstable displacements were conducted using special equipment designed to run in-situ CT-scanner experiments. All the displacements were conducted on a homogeneous Bentheimer sandstone plug, of 10 cm in diameter and 40 cm in length. Digitations (or fingering) have been observed under varying conditions of injection flowrate, displaced fluid viscosity, and core wettability. They have been characterized at both the core scale, using the core average oil saturation and the water breakthrough; and at the local scale, using the local saturations and had-hoc image processing analysis. It was found that the effect of the different flowing conditions on the front digitations could not be interpreted independently. The oil recovery at brine breakthrough showed a good correlation with the viscous fingering number for the water-wet case. However, a different scaling was observed for the oil-wet case. The interplay of the different flowing conditions mitigates the possibility of constructing a unique scaling number to account for all experimental condition. The local saturation monitoring has provided a new insight to characterize the finger shapes and analyze the production mechanisms. It allowed to distinguish two independent contributions to early breakthrough: viscous dominated digitations and capillary dominated digitations. A two-phases diagram has been constructed to plot and compare these contributions for all flowing conditions. Their evolutions show the main production mechanisms during the flooding. We observed that the viscous digitations were not causing phase trapping at core scale: the core is completely swept after breakthrough. For the water-wet case, we found that the local oil recovery of swept zone remained constant before and after breakthrough while for the oil-wet case it is improving during all the water flooding process.

Comparative study between foams made of a pH sensitive surfactant, nonaoxyethylene oleylether carboxylic acid (AKYPO ® RO 90 VG) and a classical foaming surfactant, sodium dodecyl sulphate (SDS) was realised using simple microfluidic devices in the scope of Enhanced Oil Recovery (EOR). The influence of injecting fluid parameters such as gas and foaming liquid pressure was investigated and discussed in terms of foam morphology, and lamellae stability and curvature radii. The increasing stability of AKYPO ® foam film lamellae by increasing pH is classically explained by the electrostatic repulsive interaction of the double layer in foam film. In other hand, the addition of dodecanol (DOH) on SDS solution seems to have no effect on foam regime and lamellae stability except for high DOH concentration where the foam film shape becomes double bump. The behaviour difference between AKYPO ® and SDS lays on the lamellae shape and stability domain. While SDS lamellae stay unchanged with increasing pressure ratio between the gas and the liquid, AKYPO ® lamellae curvature radius increases which could be related to surfactants solubilities and structure. These results pointed out the relevance of solution physicochemical parameters on foam stability and flowing and help the understanding of flowing foam in EOR context.

International audience; Subduction of carbonated crust is widely believed to generate a flux of carbon into the base of the continental lithospheric mantle, which in turn is the likely source of widespread volcanic and non-volcanic CO2 degassing in active tectonic intracontinental settings such as rifts, continental margin arcs and back-arc domains. However, the magnitude of the carbon flux through the lithosphere and the budget of stored carbon held within the lithospheric reservoir are both poorly known. We provide new constraints on the CO2 budget of the lithospheric mantle below the Pannonian Basin (Central Europe) through the study of a suite of xenoliths from the Bakony-Balaton Highland Volcanic Field. Trails of secondary fluid inclusions, silicate melt inclusions, networks of melt veins, and melt pockets with large and abundant vesicles provide numerous lines of evidence that mantle metasomatism affected the lithosphere beneath this region. We obtain a quantitative estimate of the CO2 budget of the mantle below the Pannonian Basin using a combination of innovative analytical and modeling approaches: (1) synchrotron X-ray microtomography, (2) NanoSIMS, Raman spectroscopy and microthermometry, and (3) thermodynamic models (Rhyolite-MELTS). The three-dimensional volumes reconstructed from synchrotron X-ray microtomography allow us to quantify the proportions of all petrographic phases in the samples and to visualize their textural relationships. The concentration of CO2 in glass veins and pockets ranges from 0.27 to 0.96 wt.%, higher than in typical arc magmas (0–0.25 wt.% CO2), whereas the H2O concentration ranges from 0.54 to 4.25 wt.%, on the low end for estimated primitive arc magmas (1.9–6.3 wt.% H2O). Trapping pressures for vesicles were determined by comparing CO2 concentrations in glass to CO2 saturation as a function of pressure in silicate melts, suggesting pressures between 0.69 to 1.78 GPa. These values are generally higher than trapping pressures for fluid inclusions determined by Raman spectroscopy and microthermometry (0.1–1.1 GPa). The CO2/silicate melt mass ratios in the metasomatic agent that percolated through the lithospheric mantle below the Pannonian Basin are estimated to be between 9.0 and 25.4 wt.%, values consistent with metasomatism either by (1) silicate melts already supersaturated in CO2 before reaching lithospheric depths or (2) carbonatite melts that interacted with mantle peridotite to generate carbonated silicic melts. Taking the geodynamical context of the Pannonian Basin and our calculations of the CO2/silicate melt mass ratios in the metasomatic agent into account, we suggest that slab-derived melts initially containing up to 25 wt.% of CO2 migrated into the lithospheric mantle and exsolved CO2–rich fluid that became trapped in secondary fluid inclusions upon fracturing of the peridotite mineral matrix. We propose a first-order estimate of 2000 ppm as the minimal bulk CO2 concentration in the lithospheric mantle below the Pannonian Basin. This transient carbon reservoir is believed to be degassed through the Pannonian Basin due to volcanism and tectonic events, mostly focused along the lithospheric-scale regional Mid-Hungarian shear Zone.

We report an experimental study of N2-foam injection in a Bentheimer sandstone coupled with X-ray Computed Tomography (CT-scanner). The measurements of pressure drop and gas saturation at different flow rates and foam qualities allowed us to describe the foam dynamics under transient and steady-state flow conditions. The brine displacement by foam shows a transient piston-like displacement pattern taking place in two successive phases. Saturation profiles reveal permanent entrance effects related to the injection procedure, and transient downstream end effects related to the gradual foam build-up. Entrance effects are attenuated with a high foam quality and at low total flow rate. The rheological behavior of foam was studied in terms of apparent foam viscosity and foamed-gas mobility as a function of foam quality and gas interstitial velocity. In the low-quality regime, foam exhibits a shear-thinning behavior that can be modelled by a power function. Furthermore, for a fixed total velocity, the quasi-invariance of strong foam apparent viscosity values is shown to result from the slight increase of trapped gas saturation, within the commonly-admitted assumption of invariant foam texture in the low-quality regime. An increase in gas mobility was observed above a certain value of the foam quality. That transition between low-quality and high-quality regimes was related to a limiting capillary pressure of foam in the porous medium under consideration.

Currently, intraperitoneal (IP) injection of D-luciferin is the preferred method of providing substrate for bioluminescence imaging (BLI); however it has a failure rate of 3–10% due to accidental intestinal injection. The present study evaluates the quality of BLI after subcutaneous (SC) injection of D-luciferin and demonstrates the effectiveness of SC injection in anatomically disparate tumor models. Mice bearing luciferase-expressing tumors underwent BLI after SC or IP injection of D-luciferin. The average time to maximal luminescence was 6 min (range 5–9 min) after SC injection and 8 min (range 5–8 min) after IP injection. Within 7 minutes of injection, SC and IP routes yielded similar luminescence in subcutaneous, intracranial, tongue, and lung xenograft tumor models. In a model of combined subcutaneous and intracranial xenografts, SC injection resulted in proportional luminescence at all sites, confirming that preferential delivery of substrate does not occur. While tumors were occasionally not visualized with IP injection, all tumors were visualized reliably with SC injection. Thus, SC injection of D-luciferin is a convenient and effective alternative to IP injection for BLI in nude mice. It may be a preferable approach, particularly for tumors with weaker signals and/or when greater precision is required.

High Resolution 3D Reconstructions of Rocks and Composites — Ten µm resolution 3D representations of different media, were obtained with a laboratory computer microtomograph develo - ped from an electron microprobe column. From the original electron microprobe, only minor modifica - tions have been required, indeed several of the utilities of the microprobe have been used to ensure high resolution radiography (2 µm). The impact of the electron beam focused onto a thin film is used to form a "point" X-ray source and the radiographic image of the sample is acquired on a CCD camera. A speci - men rotation mechanism allows multiple radiograph acquisition and reconstruction of the X-ray attenua - tion 3D cartography. Since X-ray attenuation is directly related to density and atomic number, the microscanner provides 3D cartographs of the different phases present in the sample. System perfor - mances have been evaluated on various samples, mainly rocks and composites. Comparison with scan - ning electron micrographs was used when possible to validate the reconstructions. Results are mostly qualitative but already show the potential of the technique in describing 3D connectivity and topology of pore networks or 3D orientation of fibres in composites.

A signal loss is generally reported in electron probe microanalysis (EPMA) of porous, highly divided materials like heterogeneous catalysts. The hypothesis generally proposed to explain this signal loss refers to porosity, roughness, energy losses at interfaces, or charging effects. In this work we investigate by Monte Carlo simulation all these physical effects and compare the simulated results with measurements obtained on a mesoporous alumina. A program using the PENELOPE package and taking into account these four physical phenomena has been written. Simulation results show clearly that neither porosity nor roughness, nor specific energy losses at interfaces, nor charging effects are responsible for the observed signal loss. Measurements performed with analysis of carbon and oxygen lead to a correct total of concentration. The signal loss is thus explained by a composition effect due to a carbon contamination brought by the sample preparation and to a lesser extent by a stoichiometry of the porous alumina different from a massive alumina. For this kind of high specific surface porous sample, a little surface contamination layer becomes an important volume contamination that can produce large quantification errors if the contaminant is not analyzed.

This paper presents the rock image analysis equipment and methods available in the IFP. These images are either digital core sample images recorded at a macroscopic scale or images obtained with an electron microscope (STEM, SEM). We also show how one can study flow in porous media by the use of a medical scanner. In conclusion we expose the problems encountered and the developments that one can expect using these techniques., Cette publication présente les moyens et les méthodes d'analyse d'images de roches à l'IFP. Ces images sont soit des images numériques de carotte de forage enregistrées à l'échelle macroscopique, soit des images issues d'un microscope électronique (MEB ou MEBT). Nous montrons également comment l'écoulement de fluides dans les milieux poreux peut être étudié par un scanner médical. Nous concluons par les difficultés rencontrées dans l'utilisation de ces techniques et les développements espérés., Bieber Marie-Thérèse, Lallemand Claude, Rosenberg Elisabeth, Zinsner Bernard. Le traitement numérique d'images de roches à l'Institut Français du Pétrole. Digital processing of rock images in the Institut Français du Pétrole. In: Sciences Géologiques. Bulletin, tome 41, n°2, 1988. Traitements d'images et objets géologiques. pp. 233-240.

Foam has long been used as a mobility control agent in Enhanced Oil Recovery (EOR) processes to enhance sweep efficiency and overcome gravity segregation, viscous fingering and gas channeling, which are gas-related problems when the latter is injected alone in the reservoir. However, the systematic use of foam in reservoir engineering requires more in-depth knowledge of its dynamics in porous media. The literature shows two types of experimental approaches based either on petrophysical studies carried out on 3D porous systems and based on pressure measurements, or on microfluidic studies that allow direct visualization of foam flow but are limited to 1D or 2D model systems. The research investigated in this thesis aims to bridge the gap between these two approaches. The proposed strategy is to characterize in situ the foam flow in 3D porous media with techniques providing a wide range of temporal and spatial resolutions. A coreflood setup giving access to classical petro-physical measurements was developed and then coupled to different observation cells designed specifically for each characterization instrument. First, an X-ray CT scanner was used to describe and visualize the foam flow at the core scale. The rheological behavior of foam on this scale was studied as a function of the injection conditions such as gas velocity and foam quality. Secondly, Small Angle Neutron Scattering (SANS) was used to probe the foam structure in situ during the flow, on a wide length scale, up to three orders of magnitude in size. In situ foam texture (size and density of bubbles and lamellae) was measured for different foam qualities and at different propagation distances from the injection point. A comparison to the geometric characteristics of the porous medium was also realized. Thirdly, High Resolution Fast X-ray Micro-tomography on a Synchrotron was used to visualize the foam flow at the pore scale. This allowed to confirm visually some foam characteristics measured with SANS and to investigate on local intermittent gas trapping and mobilization. This study is an important step in the multi-scale characterization of foam flow in 3D porous media and provides some answers to certain generally accepted assumptions., L’utilisation de la mousse en récupération assistée du pétrole (Enhanced Oil Recovery, EOR) présente un avantage indéniable par rapport à l’injection du gaz seul pour pallier les problèmes de ségrégation gravitaire et de digitations visqueuses. Son utilisation systématique en ingénierie du réservoir nécessite des connaissances plus approfondies sur son comportement en milieu poreux. La littérature montre deux types d’approches expérimentales basées soit sur des études pétrophysiques effectuées sur des systèmes poreux 3D et basées sur des mesures de pressions intégrées sur l’ensemble du milieu poreux, soit sur des études micro-fluidiques qui permettent une visualisation directe de l’écoulement mais qui sont limitées à des systèmes modèles dans des géométries à 1 ou 2 dimensions. L’objectif de cette thèse est de faire le pont entre ces deux approches. La stratégie proposée consiste à caractériser in situ l’écoulement de la mousse dans des milieux poreux 3D à différentes échelles, en utilisant des techniques complémentaires permettant d’accéder à une large gamme de résolutions spatiale et temporelle. Un environnement instrumenté donnant accès aux mesures pétro-physiques classiques a été développé puis couplé à différentes cellules d’observation conçues spécifiquement pour chaque instrument de caractérisation. Dans un premier temps, un scanner X a été utilisé pour décrire et visualiser les écoulements de la mousse à l’échelle de la carotte. La rhéologie de la mousse à cette échelle a pu être étudiée en fonction des conditions d’injections comme la vitesse interstitielle du gaz et la qualité de mousse. Dans un deuxième temps, la technique de diffusion des neutrons aux petits angles (SANS) a permis de sonder la texture de la mousse en écoulement sur trois ordres de grandeurs en taille. Des informations in situ sur la texture de la mousse en écoulement (taille et densité des bulles et des lamelles) ont pu être mesurées pour différentes qualités de mousse puis en fonction de la distance au point d’injection. Une comparaison avec les caractéristiques géométriques du milieu poreux a également été effectuée. Dans un troisième temps, la micro-tomographie X rapide haute résolution sur Synchrotron a été utilisée pour visualiser la mousse en écoulement à l’échelle du pore. Cette technique a permis de confirmer de visu certaines caractéristiques de la mousse mesurées par SANS et de décrire en sus les effets d’intermittence du piégeage de la mousse. Cette étude constitue une étape importante de la caractérisation multi-échelle de l’écoulement des mousses en milieux poreux 3D et apporte des éléments de réponse à certaines hypothèses admises.