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A new three-angle energy-dispersive (ED) diffractometer has been successfully commissioned on station 16.4 SRS, Daresbury, England. The diffractometer facilitates the simultaneous collection of three spectra at three Bragg scattering angles. This enables the sampling of a far greater range of reciprocal space as compared to conventional single-angle diffractometers. Additionally the arrangement allows changes in sample density to be monitored. A protocol has been developed to align the diffractometer such that the origins of the diffracting volume are coincident on the diffractometer axis. Spectra obtained from the diffractometer were improved by the construction and placement of shielding. Experimental determination of components of the resolution function show that the resolution is close to the instrumental limit. The flux distribution of station 16.4 was determined experimentally. A novel whole pattern method has been developed for the quantitative analysis of synchrotron ED diffraction data. The method, which accounts for the differential absorption across the ED spectrum, was developed using spectra collected from a set of test binary phase mixtures and pure phases. Parameters relating to the proposed models were determined using linear and non-linear least-squares methods. Although the final model is the most physically complete it does not take account of certain non-diffraction derived events which appear as counts within the test spectra. A novel application of synchrotron ED diffraction, energy-dispersive diffraction tomography (EDD-T), is described. The method facilitates the non-destructive examination of the interior of crystalline and semi-crystalline objects. The resolution and limitations of this technique have been demonstrated using test objects. The method has been used to map the phase distributions of a variety of materials in a range of different samples. Quantitative EDD-T was used to determine the invasion of calcite into simulated oil-reservoir rocks.

Sixteen percent of New Zealand’s power comes from geothermal sources which are primarily located within the Taupo Volcanic Zone (TVZ). The TVZ hosts twenty three geothermal fields, seven of which are currently utilised for power generation. Ngatamariki Geothermal Field is the latest geothermal power generation site in New Zealand, located approximately 15 km north of Taupo. This was the location of interest in this project, with testing performed on a range of materials to ascertain the physical properties and microstructure of reservoir rocks. The effect of burial diagenesis on the physical properties was also investigated. Samples of reservoir rocks were taken from the Tahorakuri Formation and Ngatamariki Intrusive Complex from a range of wells and depths (1354-3284 mbgl). The samples were divided into four broad lithologies: volcaniclastic lithic tuff, primary tuff, welded ignimbrite and tonalite. From the supplied samples twenty one small cylinders (~40-50mm x 20-25mm) were prepared and subjected to the following analyses: dual weight porosity, triple weight porosity, dry density, ultrasonic velocity (saturated and dry) and permeability (over a range of confining pressures). Thin sections impregnated with an epoxy fluorescent dye were created from offcuts of each cylinder and were analysed using polarised light microscopy and quantitative fluorescent light microstructural microscopy. The variety of physical testing allowed characterisation of the physical properties of reservoir rocks within the Ngatamariki Geothermal Field. Special attention was given to the petrological and mineralogical fabrics and their relation to porosity and matrix permeability. It was found that the pore structures (microfractures or vesicles) had a large influence on the physical properties. Microfractured samples were associated with low porosity and permeability, while the vesicular samples were associated with high porosity and permeability. The microfractured samples showed progressively lower permeability with increased confining pressure whereas samples with a vesicular microstructure showed little response to increased confining pressure. An overall trend of decreasing porosity and permeability with increasing density and sonic velocity was observed with depth, however large fluctuations with depth indicate this trend may be uncertain. The large variations correlate with changes in lithology suggest that the lithology is the primary control of the physical properties with burial diagenesis being a subsidiary factor. This project has established a relationship between the microstructure and permeability, with vesicular samples showing high permeability and little response increased confining pressure. The effects of burial diagenesis on the physical properties are subsidiary to the observed variations in lithology. The implications of these results suggest deep drilling in the Tahorakuri Formation may reveal unexploited porosity and permeability at depth.

Este trabalho foi desenvolvido utilizando-se rochas reservatório siliciclásticas provenientes de afloramentos brasileiros, pertencentes ao Grupo Guaritas (Caçapava do Sul e Pinheiro Machado - RS) e à Formação Pirambóia (Rio Claro - SP), com o objetivo de se obter suas características petrofísicas. As amostras são provenientes de diferentes fácies eólicas e pluviais, com características semelhantes a reservatórios de água e hidrocarbonetos. Foram utilizados experimentos de Ressonância Magnética Nuclear (RMN), intrusão de mercúrio, susceptibilidade magnética, análise de lâmina petrográfica e Espectroscopia de Fluorescência de Energia Dispersiva de Raios-X (EDX) para a análise das amostras. Apesar de serem provenientes de sistemas deposicionais similares, a correlação entre os resultados demonstrou que a diagênese tem importante papel no desenvolvimento dos reservatórios, influenciando na porosidade e permeabilidade das amostras. Foi demonstrado que a susceptibilidade magnética possui correlação com as quantidades de Fe 203, Al 203 e SiO2, onde o Al 203 está relacionado com a quantidade de argila das amostras (aluminossilicatos). Através dos resultados de RMN foi possível estimar a susceptibilidade magnética das amostras através da largura de linha espectral em baixo campo. As estimativas de porosidade e tamanhos de poros via RMN demonstraram compatibilidade com as análises das lâminas e experimentos de intrusão de mercúrio. Com os experimentos de RMN bidimensionais T1xT2, foi mostrado que há uniformidade na relaxação, devido aos mapas de correlação serem aproximadamente paralelos à diagonal dos mapas 2D. Nos experimentos DxT2 há a correlação entre a distribuição de tempos de relaxação e coeficientes de difusão, demonstrando que, em muitos casos, há restrição de difusão translacional das moléculas do fluido. Para estimar a permeabilidade das rochas foi utilizado o modelo desenvolvido por pesquisadores da Schlumberger Doll Research (SDR), amplamente aplicado na previsão da permeabilidade através de resultados obtidos pela RMN. Aplicando-o de maneira clássica, os resultados não foram plenamente satisfatórios, em função das características magnéticas das rochas estudadas. O coeficiente relaxatividade superficial foi calculado pela convolução entre a distribuição de tamanhos de poros da intrusão de mercúrio e a distribuição de tempos de relaxação transversal. Este parâmetro foi utilizado como correção ao modelo SDR, entretanto, os resultados obtidos continuaram não satisfatórios. Foi proposta então a correção através da susceptibilidade magnética, tanto medida pelo susceptômetro quanto estimada pela RMN. As utilizações dessas duas informações culminaram em melhores resultados para o valor das permeabilidades, com destaque para a RMN, desta maneira, propondo um novo método para estimar esse importante parâmetro das rochas reservatório. Com estes resultados podemos verificar a coesão entre os aspectos geológicos das amostras e a RMN, porém, as técnicas de RMN existentes empregadas ao estudo devem ainda ser aperfeiçoadas e novas devem ser desenvolvidas para o estudo de rochas reservatório que apresentam alta susceptibilidade magnética, um problema comum encontrado no estudo de rochas sedimentares por RMN. / The petrophysical characterization of siliciclastic reservoir rocks from Brazilian outcrops was the objective of this work. The samples were obtainded from different eolian and pluvial facies of the Guaritas Group (Caçapava do Sul and Pinheiro Machado - RS) and Pirambóia Formation (Rio Claro -SP). Different methods were applied in order to study these samples: Nuclear Magnetic Resonance (NMR), mercury injection, magnetic susceptibility, petrographic thin sections analysis and Energy Dispersive X-ray Fluorescence Spectroscopy (EDX). Despite the depositional similarities, the results indicate that permeability and porosity are affected by diagenetic processes which show that the diagenesis plays an important role at the development of these reservoirs. It was shown the correlation between magnetic susceptibility and the amounts of Fe 2O3 , Al 203 and Si0 2 were the amount of Al 203 is related with the quantity of clay (aluminosilicates). Magnetic susceptibilities were estimated using the linewidth obtained from NMR spectra (by FFTs of the FIDs) measured at low and homogeneous magnetic fields, obtaining good agreement with the bulk magnetic susceptibility. Porosity and pore size distributions determined by NMR, mercury injection and petrographic analysis were compatible. In the two-dimensional NMR experiment T 1xT2 a diagonal behavior of relaxation time distributions was observed, indicating uniformity of relaxation mechanisms inside the samples. With DxT 2 measurements, the transverse relaxation times were correlated with diffusion coefficients showing restricted diffusion in most samples. In order to predict permeability the model proposed by researchers from Schlumberger Doll Research (SDR), which uses NMR parameters, was applied. With the classical permeability SDR predictor the obtained results were not fully satisfactory, as consequence of the magnetic characteristics of the samples. In order to correct this predictor, surface relaxivity coefficients were determined by the superposition of T2 and mercury injection pore diameter distributions nevertheless, these results were again unsatisfactory. Thus, a new correction method for the SDR permeability predictor was proposed using NMR and bulk magnetic susceptibilities. This approach improved considerably the permeability prediction, especially when using NMR-derived magnetic susceptibilities. The consistency between NMR and geological properties of the samples was verified nevertheless, the used NMR techniques still need to be improved and new ones must be developed, in order to allow the study of reservoir rocks with high magnetic susceptibility.

Este trabalho foi desenvolvido utilizando-se rochas reservatório siliciclásticas provenientes de afloramentos brasileiros, pertencentes ao Grupo Guaritas (Caçapava do Sul e Pinheiro Machado - RS) e à Formação Pirambóia (Rio Claro - SP), com o objetivo de se obter suas características petrofísicas. As amostras são provenientes de diferentes fácies eólicas e pluviais, com características semelhantes a reservatórios de água e hidrocarbonetos. Foram utilizados experimentos de Ressonância Magnética Nuclear (RMN), intrusão de mercúrio, susceptibilidade magnética, análise de lâmina petrográfica e Espectroscopia de Fluorescência de Energia Dispersiva de Raios-X (EDX) para a análise das amostras. Apesar de serem provenientes de sistemas deposicionais similares, a correlação entre os resultados demonstrou que a diagênese tem importante papel no desenvolvimento dos reservatórios, influenciando na porosidade e permeabilidade das amostras. Foi demonstrado que a susceptibilidade magnética possui correlação com as quantidades de Fe 203, Al 203 e SiO2, onde o Al 203 está relacionado com a quantidade de argila das amostras (aluminossilicatos). Através dos resultados de RMN foi possível estimar a susceptibilidade magnética das amostras através da largura de linha espectral em baixo campo. As estimativas de porosidade e tamanhos de poros via RMN demonstraram compatibilidade com as análises das lâminas e experimentos de intrusão de mercúrio. Com os experimentos de RMN bidimensionais T1xT2, foi mostrado que há uniformidade na relaxação, devido aos mapas de correlação serem aproximadamente paralelos à diagonal dos mapas 2D. Nos experimentos DxT2 há a correlação entre a distribuição de tempos de relaxação e coeficientes de difusão, demonstrando que, em muitos casos, há restrição de difusão translacional das moléculas do fluido. Para estimar a permeabilidade das rochas foi utilizado o modelo desenvolvido por pesquisadores da Schlumberger Doll Research (SDR), amplamente aplicado na previsão da permeabilidade através de resultados obtidos pela RMN. Aplicando-o de maneira clássica, os resultados não foram plenamente satisfatórios, em função das características magnéticas das rochas estudadas. O coeficiente relaxatividade superficial foi calculado pela convolução entre a distribuição de tamanhos de poros da intrusão de mercúrio e a distribuição de tempos de relaxação transversal. Este parâmetro foi utilizado como correção ao modelo SDR, entretanto, os resultados obtidos continuaram não satisfatórios. Foi proposta então a correção através da susceptibilidade magnética, tanto medida pelo susceptômetro quanto estimada pela RMN. As utilizações dessas duas informações culminaram em melhores resultados para o valor das permeabilidades, com destaque para a RMN, desta maneira, propondo um novo método para estimar esse importante parâmetro das rochas reservatório. Com estes resultados podemos verificar a coesão entre os aspectos geológicos das amostras e a RMN, porém, as técnicas de RMN existentes empregadas ao estudo devem ainda ser aperfeiçoadas e novas devem ser desenvolvidas para o estudo de rochas reservatório que apresentam alta susceptibilidade magnética, um problema comum encontrado no estudo de rochas sedimentares por RMN. / The petrophysical characterization of siliciclastic reservoir rocks from Brazilian outcrops was the objective of this work. The samples were obtainded from different eolian and pluvial facies of the Guaritas Group (Caçapava do Sul and Pinheiro Machado - RS) and Pirambóia Formation (Rio Claro -SP). Different methods were applied in order to study these samples: Nuclear Magnetic Resonance (NMR), mercury injection, magnetic susceptibility, petrographic thin sections analysis and Energy Dispersive X-ray Fluorescence Spectroscopy (EDX). Despite the depositional similarities, the results indicate that permeability and porosity are affected by diagenetic processes which show that the diagenesis plays an important role at the development of these reservoirs. It was shown the correlation between magnetic susceptibility and the amounts of Fe 2O3 , Al 203 and Si0 2 were the amount of Al 203 is related with the quantity of clay (aluminosilicates). Magnetic susceptibilities were estimated using the linewidth obtained from NMR spectra (by FFTs of the FIDs) measured at low and homogeneous magnetic fields, obtaining good agreement with the bulk magnetic susceptibility. Porosity and pore size distributions determined by NMR, mercury injection and petrographic analysis were compatible. In the two-dimensional NMR experiment T 1xT2 a diagonal behavior of relaxation time distributions was observed, indicating uniformity of relaxation mechanisms inside the samples. With DxT 2 measurements, the transverse relaxation times were correlated with diffusion coefficients showing restricted diffusion in most samples. In order to predict permeability the model proposed by researchers from Schlumberger Doll Research (SDR), which uses NMR parameters, was applied. With the classical permeability SDR predictor the obtained results were not fully satisfactory, as consequence of the magnetic characteristics of the samples. In order to correct this predictor, surface relaxivity coefficients were determined by the superposition of T2 and mercury injection pore diameter distributions nevertheless, these results were again unsatisfactory. Thus, a new correction method for the SDR permeability predictor was proposed using NMR and bulk magnetic susceptibilities. This approach improved considerably the permeability prediction, especially when using NMR-derived magnetic susceptibilities. The consistency between NMR and geological properties of the samples was verified nevertheless, the used NMR techniques still need to be improved and new ones must be developed, in order to allow the study of reservoir rocks with high magnetic susceptibility.

[pt] O presente trabalho apresenta um estudo paramétrico de alguns fatores intervenientes no processo de entupimento de formações rochosas por sólidos em suspensão, sob injeção de água. Primeiramente se fez uma revisão das formulações mais comumente utilizadas em se tratando de modelos de redução de permeabilidade na literatura técnica especializada. Em seguida, a partir de dois simuladores numéricos, executou- se vários casos de injeção de água,e tais resultados foram comparados entre si e comentários foram feitos a respeito da validade das informações por eles fornecidas. Uma campanha de ensaios foi executada de forma a avaliar alguns parâmetros intervenientes na retenção de partículas em suspensão quando injetadas em um meio poroso, como a rocha. Inicialmente foi feita uma revisão bibliográfica sobre ensaios de injeção já realizados em diversos centros de pesquisas do mundo. Os resultados desses experimentos de injeção, conjugados a análises complementares de microscopia eletrônica, fornecem informações bastantes úteis para determinados aspectos a serem considerados na execução de injeção de água produzida em poços offshore. / [en] The present work presents a parametric study of some intervening factors in the blockage process of rocky formations for solids in suspension, under injection of water.Firstly it was made a review in the specialized technical literature on the formulations more commonly used for modelling the permeability reduction. Next, using two numeric simulators, several examples of water injection were executed, and the results were compared amongst each other. A series of laboratory tests was performed in order to evaluate some intervening parameters in the retention of particles in suspension when injected in a porous medium. Initially it was made a bibliographical review on injection tests carried out in several research centers of the world. The results of the injection experiments, with associated analyses of electronic microscopy, were able to supply useful information for certain aspects to be considered when injecting produced water in offshore wells.

Au cours de la production d'hydrocarbures, l'extraction de fluides fait décroître la pression de pore dans les réservoirs (« depletion »). Ceci induit un changement du champ de contraintes qui résulte en une augmentation des contraintes effectives appliquées sur le réservoir. Les mesures in situ montrent que les variations de contraintes peuvent être décrites par un paramètre appelé chemin de chargement (stress path), défini comme le rapport entre la variation de contrainte effective horizontale et la variation de contrainte effective verticale par rapport aux conditions initiales dans le réservoir. La compaction induite par la production d'hydrocarbures peut avoir de graves conséquences dans le cas de roches faiblement consolidées car elle induit des variations des propriétés pétrophysiques des roches in situ, notamment de la perméabilité, un des paramètres les plus importants pour estimer la performance d'un réservoir mais aussi un des plus difficiles à mesurer. Pour compliquer encore les choses, la perméabilité est souvent anisotrope dans les réservoirs avec de forts contrastes entre la perméabilité horizontale kh et la perméabilité verticale kv.L'objectif de cette étude est de comprendre l'influence des chemins de chargement sur le comportement mécanique et les évolutions couplées de perméabilité pour un sable quartzeux (Sable de la Durance, DS) et un grès faiblement consolidé (grès d'Otter Sherwood, OSS, qui constitue la roche réservoir du champ pétrolier de Wytch Farm en Angleterre). Nos résultats montrent que le grès peu consolidé présente un comportement mécanique similaire à celui de roches consolidées. Au contraire, le sable présente un comportement différent, avec une transition plus graduelle entre les régimes de déformation qui nécessite d'utiliser un critère basé sur l'évolution du rayon de courbure des courbes contraintes-déformations pour déterminer les contraintes limites : cette méthode a été validée par une étude d'analyse des émissions acoustiques pour caractériser l'endommagement. Les domaines de déformation élastique et plastique ont été bien définis et les contraintes limites ont été comparées aux prédictions du modèle Cam-Clay modifié et du modèle d'enveloppe limite normalisée. Les perméabilités horizontale et verticale ont été mesurées sous contraintes. Pour analyser l'influence des effets de bord dans les essais mécaniques, les perméabilités mesurées soit classiquement sur toute la longueur de l'échantillon, soit entre deux points intermédiaires ont été comparées. Pour l'écoulement horizontal, les facteurs géométriques et facteurs d'anisotropie ont été déterminés par des simulations numériques en éléments finis afin de pouvoir déterminer les vraies valeurs de perméabilité horizontale. L'évolution de la perméabilité suit l'évolution de la déformation des matériaux et est contrôlée aussi bien par la déformation volumique que par la déformation en cisaillement. A partir de nos mesures il est possible de séparer l'effet de la pression moyenne de l'effet de la contrainte déviatorique sur l'évolution de la perméabilité en construisant des cartes d'isoperméabilités dans l'espace des contraintes. Enfin une modélisation élasto-plastique a été réalisée pour prédire le comportement hydro-mécanique du grès faiblement consolidé. L'approche utilisée permet de prédire de manière satisfaisante l'évolution de la perméabilité avec les contraintes, à partir d'une loi exponentielle fonction de la déformation effective. Au contraire, pour le sable de la Durance le lien entre l'évolution de la perméabilité et la déformation est loin d'être évidente, notamment aux faibles contraintes où la réduction de perméabilité est très rapide. Pour mieux comprendre ces évolutions de perméabilité, une analyse de l'endommagement a été réalisée par des mesures sur échantillons et en utilisant des techniques d'imagerie à plusieurs échelles. / During hydrocarbon production, the extraction of fluid induces a decrease of pore pressure called depletion. This depletion causes a change in the stress field that results in an increased stress on the rock by enhancement of the effective stress in the reservoir. In situ measurements show that the stress variations can be described by the so-called stress path parameter, defined as the ratio of the change in effective horizontal stress by the change in effective overburden stress from initial reservoir conditions. This production induced compaction can have severe consequences in the case of poorly consolidated reservoirs. Compaction induces variations of petrophysical properties of in situ rocks and particularly permeability variations, one of the most important parameters controlling reservoir performance. Yet it is one of the most difficult property to measure. To complicate matters further, permeability anisotropy is often found in reservoirs. Therefore the horizontal permeability kh, may be different from the vertical permeability kv.The aim of this study is to understand the influence of stress paths on the mechanical behavior and coupled permeability evolutions of a Quartz sand (Durance Sand, DS) and a weakly consolidated sandstone (Otter Sherwood Sandtone, OSS which is the reservoir rock of the Wytch Farm oil field, UK). We found that the weakly consolidated rock presents a mechanical behavior similar to that of consolidated rocks. However, the sand shows a different behavior, with a gradual transition regime which requires the use of a curvature criterion to peak yield stresses on the stress-strain evolution plot; this criterion has been validated on the basis of Acoustic Emission analysis. The elastic and plastic deformation regimes are well identified and the determined yield stresses are fitted using the modified Cam-Clay and Elliptic Cap models for all observed onsets of plastic yielding. Both vertical and horizontal permeability have been measured during loading. To analyze the influence of end effects during loading in the triaxial cell, permeabilities measured over the mid-section and over the total core length were compared. For the horizontal flow, the geometrical and anisotropy factors were determined using Finite Element simulations in order to calculate the correct horizontal permeability. Permeability evolution follows closely the material deformation and is controlled by both volumetric and shear strains. It is possible to infer the effect of the mean pressure and/or the deviatoric stress on the permeability evolution by building isopermeability maps in the stress space. Finally, an application of elasto-plastic modeling to predict the hydromechanical behavior of the weakly consolidated rock is presented. This approach allows a satisfying prediction of the permeability evolution with stresses, using an exponential function of an effective strain. Reversely for DS, the link between strain and permeability is not obvious as permeability reduction is pronounced at early stage of loading. To understand these permeability evolutions, a damage analysis has been performed using core analysis measurements and multi-scale imaging.