Soil is a fundamental resource in the environment, its sustainable use is vital to food supply and, consequently, life continuity on the Earth. However, the currently status of this resource in the world is critical and, therefore, the need of soil recovery measures and methods to evaluate it is urgent. The aim of this study is to provide a holistic evaluation about soil architecture at different recovery states, as well as its interaction with fluid in the environment by using nonconventional methods. It was organized a tool package that allows to analyze soil physical at geometric, morphometric and energy scope, to show in a more efficient way, which physical parameters indicate the physical and environmental quality. Subsequently, this package was applied to the study of six types of managements in different stages of development by using of physical parameter derived from the package; It was also analyzed the efficiency of recovery techniques under different perspectives. In addition, the soil-water dynamic was evaluated in a particular condition by using the same tools, offering knowledge about this interaction in the environment along the time. Finally, it is expected that this work can bring new insight on preservation and recovery of this environmental resource. / O solo é um recurso fundamental no meio ambiente, seu uso sustentável é vital para prover alimentos e consequentemente a continuidade da vida na Terra. No entanto, estado atual desse recurso no mundo encontra-se em condição crítica, logo as medidas de recuperação devem ser adotadas urgentemente, consequentemente a necessidade de métodos adequados para avaliação dessas medidas. O objetivo desse estudo é proporcionar uma avaliação holística sobre a arquitetura do solo em diferentes estados de recuperação, assim como sua interação com fluido no meio ambiente utilizando métodos não convencionais. Logo, foi organizado um pacote de ferramentas que permitam analisar a física solo no âmbito de geometria, morfometria e energia, proporcionando parâmetros físicos que indicam a qualidade física e ambiental; Em seguida esse pacote foi aplicado no estudo de seis tipos de manejos com diferentes estágios de desenvolvimento, envolvendo os parâmetros físicos derivados do pacote, mostrando assim a eficiência das técnicas de recuperação sob diferentes perspectivas; Assim foi realizado também a avaliação da dinâmica da água no solo em uma situação particular utilizando as mesmas ferramentas, proporcionando conhecimentos sobre o essa interação no meio ambiente ao longo do tempo. Finalmente, espera-se com esse trabalho novos olhares sobre esse recurso precioso no meio ambiente.

Universidade de São Paulo, Faculdade de Medicina; 2015. Introdução: Diante de uma rotura traumática do manguito rotador, não há evidência direta que comprove que os reparos realizados precocemente são mais eficazes que aqueles realizados tardiamente. Para abordar essa questão, ensaios biomecânicos e de morfometria óssea foram realizados após roturas extensas do manguito rotador realizadas precocemente (lesões agudas) e tardiamente (lesões crônicas), mediante a utilização de um modelo experimental em ratos. Método: 30 ratos adultos da raça Wistar foram aleatoriamente divididos em três grupos (I, II e III) e submetidos à secção completa dos tendões do supraespinal e infraespinal nos ombros esquerdos. Após oito semanas, nos animais dos grupos I e II, os tendões rotos pertencentes aos ombros esquerdos foram cirurgicamente reparados, e os tendões equivalentes nos ombros direitos foram seccionados e imediatamente reparados. Quatro semanas após os reparos (para os ratos do grupo II) ou oito semanas após os reparos (para os ratos do grupo I), os animais foram submetidos à eutanásia. Os ratos do grupo III foram submetidos à eutanásia oito semanas após a cirurgia de secção tendínea sem que houvesse ocorrido o reparo dos tendões rotos. Os ombros direitos dos animais do grupo III permaneceram intactos e serviram como controles. Após a eutanásia, todos os ratos tiveram seus ombros dissecados e os espécimes foram encaminhados para a realização de testes biomecânicos e de microtomografia computadorizada. Resultados: Para todos os parâmetros biomecânicos analisados, foram encontradas interações significantes referentes aos fatores tempo de cicatrização e reparo, considerando os reparos precoces e tardios. Com relação ao tendão supraespinal para o período de oito semanas de cicatrização, a força máxima até a falha foi significantemente maior nos reparos precoces em comparação aos reparos tardios (31,81 ± 3,86N vs 19,36 ± 6,14N; p < 0,001), bem como a rigidez (17,22 ± 4,35N/mm vs 10,85 ± 4,25N/mm; p=0,034), a tensão máxima até a falha (4,49 ± 2,02N/mm2 vs 1,97 ± 0,61N/mm2; p < 0,001) e o módulo de elasticidade (13,72 ± 5,29N/mm2 vs 6,47 ± 2,42 N/mm2; p=0,033). Com relação ao tendão infraespinal com oito semanas de cicatrização, a força máxima até a falha foi significantemente maior nos reparos precoces em comparação aos reparos tardios (21,26 ± 3,94N vs 12,74 ± 2,87N; p=0,005), assim como a rigidez (12,86 ± 2,65N/mm vs 7,21 ± 3,30N/mm; p=0,014). O grupo com reparo tardio com oito semanas de cicatrização obteve resultados nos testes biomecânicos semelhantes aqueles obtidos nos testes do grupo com lesão sem reparo com oito semanas de cicatrização. A avaliação microtomográfica não apresentou diferenças significantes na microarquitetura óssea entre os reparos realizados precocemente e tardiamente. Conclusões: Os resultados desse estudo demonstram que as roturas extensas do manguito rotador reparadas precocemente produzem um tecido cicatricial na junção ósteo-tendínea com melhores propriedades biomecânicas que as roturas reparadas tardiamente. Porém, ao analisar a morfometria óssea da porção proximal do úmero, verificou-se que os efeitos são equivalentes, tanto para os reparos realizados tardiamente quanto para os reparos realizados precocemente / Introduction: In the event of a traumatic rotator cuff tear, there is no direct evidence that supports early over late surgical repair. To address this knowledge gap, biomechanical and bone morphometry outcomes were assessed following early (acute) and late (chronic) massive rotator cuff tear repairs in an experimental rat model. Methods: 30 adult Wistar rats were randomly divided into three groups (I, II and III), then subjected to combined supraspinatus and infraspinatus tendon tears of the left shoulder. Eight weeks following the injury, animals from groups I and II had the tendons of the injured shoulder surgically repaired. In addition, these animals were subjected to the same injury on the contralateral shoulder, which was immediately repaired. The rats were euthanized four weeks (group II) or eight weeks (group I) following the repairs. Group III was euthanized eight weeks following the injury, without surgical repair of the left shoulder, and the intact right shoulders of this group were used as controls. Tissues from all groups were harvested and subjected to biomechanical testing and bone morphometry analysis. Results: In all biomechanical parameters analyzed, a significant interaction was observed between healing and repair timing. For the supraspinatus tendon with eight weeks healing time, biomechanical properties were significant increased in the early repair group compared to the late repair group, including maximum load to failure (31,81 ± 3,86N vs 19,36 ± 6,14N; p < 0,001), stiffness (17,22 ± 4,35N/mm vs 10,85 ± 4,25N/mm; p=0,034), maximum stress to failure (4,49 ± 2,02N/mm2 vs 1,97 ± 0,61N/mm2; p < 0,001) and modulus of elasticity (13,72 ± 5,29N/mm2 vs 6,47 ± 2,42 N/mm2; p=0,033). For the infraspinatus tendon with eight weeks healing time, biomechanical properties were also significantly increased in the early repair group, including maximum load to failure (21,26 ± 3,94N vs 12,74 ± 2,87N; p=0,005) and stiffness (12,86 ± 2,65N/mm vs 7,21 ± 3,30N/mm; p=0,014). There were no significant differences between the late repair with eight weeks of healing time and the group without surgical repair for supraspinatus and infraspinatus tendons. Concerning bone morphometry of the humeral head, no significant differences were observed when comparing early and late repair groups. Conclusions: The results from this study indicate that early surgical repair of a massive rotator cuff tear leads to increased biomechanical properties of the tissue after healing. However, proximal humerus bone morphometry was unaffected by surgical repair timing

A técnica de levantamento de seio maxilar (LSM) visa aumentar a altura óssea junto à superfície sinusal de maxila posterior atrófica utilizando diferentes materiais de preenchimento, para possibilitar a instalação de implantes dentários. Esses materiais de preenchimento podem variar quanto à origem e às propriedades físicoquímicas, resultando em diferentes respostas biológicas. O objetivo do atual trabalho foi avaliar a eficiência do Gen-Ox®inorg e GenPhos XP® na técnica de elevação do seio maxilar em comparação ao Bio-Oss®. Em 24 coelhos foi realizado o levantamento bilateral dos seios maxilares (SMs) utilizando 200 mm3 de material de preenchimento por seio, conforme os grupos experimentais Bio-Oss (6SMs/período), Gen-Ox (5SMs/período) e GenPhos (5SMs/período), e a janela óssea de acesso foi recoberta com uma membrana reabsorvível. Os animais de cada grupo foram eutanasiados aos 15, 30 e 60 dias e a região dos SMs foi coletada e fixada em formalina a 10% tamponada. As peças foram submetidas à análise microtomográfica para determinação do volume total do SM elevado e em seguida ao processamento histológico, sendo cortes coronais dos SMs obtidos e avaliados morfometricamente pelo método de volumetria de pontos. Todos os três materiais apresentaram excelente biocompatibilidade e promoveram a manutenção do volume do seio preenchido ao longo do tempo, sendo em média de 214,1 mm3. Em todos os grupos a formação óssea ocorreu em íntimo contato com as partículas de material. Ao término de 60 dias, o tecido ósseo formado mostrava-se maduro e preenchia parcialmente os espaços entre as partículas. A forma e tamanho das partículas de Gen-Ox gerou maior espaço entre as partículas que pode ter levado a formação de maior volume de tecido ósseo e de tecido conjuntivo (53,0 ± 10,1 mm3 e 74,1 ± 21,5 mm3) comparado ao Bio-Oss (43,7 ± 11,6 mm3 e 61,2 ± 23,3 mm3) e GenPhos (47,5 ± 10,4 mm3 e 58,5 ± 25,7 mm3). Baseado na estabilidade do volume sinusal elevado, na capacidade osteocondutora e na formação e maturidade óssea ao longo do tempo promovidos pelo Gen-Ox®inorg e GenPhos®, comparável ao do Bio-Oss®, conclui-se que esses dois biomateriais significam uma alternativa segura na técnica de LSM. / Maxillary sinus augmentation (MSA) for implant placement using bone graft or bone substitutes is a common procedure to increase the bone volume in the atrophic posterior part of the maxilla. Various bone substitutes have been used in sinus floor elevation procedures. Nonetheless, the biological performance of bone substitutes may vary according to origin, physical and chemical properties. The goal of this study was to evaluate the efficiency of both Gen-Ox®inorg and GenPhos XP® in maxillary sinus augmentation technique compared to Bio-Oss®. In 24 rabbits, it was conducted a bilateral lifting of the maxillary sinuses (MSs) using 200 mm3 of filling material for sinus in accordance with the experimental groups Bio-Oss (6SMs/period), Gen-Ox (5MSs/period) and GenPhos (5MSs/period). The sinus access window was covered with a resorbable membrane. The animals of each group were euthanized at 15, 30 and 60 days and the MSs were collected and fixed in 10% buffered formalin. The samples were submitted to microtomographic analysis to calculate the MS augmentation volume. Histological coronal sections of MS augmentation were used for morphological analysis and determination of volume density of each structure by point counting volumetry method. All three materials had excellent biocompatibility and promoted maintenance of the MS augmentation volume over time, averaging 214.1 mm3. In all groups the bone formation occurred in close contact with the material particles. At the end of 60 days, the bone tissue formed was mature and it partially filled the spaces between the particles. The shape and size of Gen-Ox particles generated greater space between the particles that may have led to a higher formation of bone volume and connective tissue (53.0 ± 10.1 mm3 and 74.1 ± 21.5 mm3) than Bio-Oss (43.7 ± 11.6 mm3 and 61.2 ± 23.3 mm3) and GenPhos (47.5 ± 10.4 mm3 and 58.5 ± 25.7 mm3). Based on the stability of the MS volume, the osteoconductive capacity and the bone formation and maturation over time promoted by Gen-Ox®inorg and GenPhos®, and comparable to Bio-Oss®, it is concluded that these two biomaterials may be a safe alternative in MSA technique.

Objectives: We compared a novel porous biphasic calcium phosphate (pBCP) containing 70% HA and 30% -TCP with autogenous bone (AB) regarding bone formation, graft granular size influence (0.7, 1.0 or 1.5 mm), physicochemical properties, and volumetric changes of the total grafted area as well its components (newly formed bone, graft particle stability and soft tissue). Materials and methods: Article 1 used a critical size defect in rats. Analyzes included XRD (X-ray diffraction), SEM (scanning electron microscope) and EDS (Energy-dispersive X-ray spectroscopy) in vitro and then histomorphometry of biopsies collected from rat skull. Article 2 used a bilateral MSFA by lateral wall surgery in 12 patients in a split-mouth design. Analyses of three-dimensional (3D) cone beam computed tomography (CBCT) scans at different periods (T0, T1 and T2), and of micro-CT scans and histological slides of graft core biopsies were performed. Results: In the preclinical approach, similar physicochemical characteristics among pBCPs with different granular sizes were found. Besides, osteopromotion regarding pBCP granular sizes of 0.7 and 1.0 were higher than AB. In the clinical approach, pCBP was similar to AB. However, in both approaches, the volume of the total grafted area and particles within the grafted area were more reduced for AB (45% and 37%, respectively, in article 1 and 31% and 33%, respectively, in Article 2). For pBCP these volumetric changes did not occur, except for 1.5 mm size group in the preclinical approach, which showed a significant reduction in the last period (24 weeks). Conclusion: pBCP70:30 physicochemical characteristics, such as slow resorption, creates a favorable microenvironment for bone formation that is directly influenced by the granule size. pBCP70:30 promotes greater preservation of the grafted volume than AB, thus being a good alternative for MSFA and bone regeneration procedures. / Objetivos: Nós comparamos um novo fosfato de cálcio bifásico poroso (pBCP contendo 70% HA e 30% -TCP com o osso autógeno (AB) quanto à formação óssea, influência do tamanho granular do enxerto (0,7, 1,0 ou 1,5 mm), propriedades físico-químicas e alterações volumétricas da área total enxertada, bem como seus componentes (osso recém-formado, estabilidade das partículas do enxerto e tecido mole). MATERIAIS E MÉTODOS: O artigo 1 usou um defeito de tamanho crítico em ratos. As análises in vitro incluíram XRD (difração de raios X), SEM (microscopia eletrônica de varredura) e EDS (espectroscopia de dispersão de energia por raios X) e depois análise histomorfometria de biópsias coletadas da calvária de ratos. O artigo 2 envolveu utilização do material para elevação bilateral de seio maxilar em 12 pacientes, em um desenho split-mouth. Análise de tomografia computadorizada tridimensional (3D) de feixe cônico (TCFC) em diferentes períodos (T0, T1 e T2), micro-CT scans e lâminas histológicas de biópsias do enxerto foram realizadas. Resultados: Na abordagem pré-clínica, foram encontradas características físico-químicas semelhantes entre os pBCPs com diferentes tamanhos granulares. Em adição, a osteopromoção, para os tamanhos granulares do pBCP de 0,7 e 1,0 mm foram maiores que para o AB. Na abordagem clínica, o pBCP foi semelhante ao AB. No entanto, em ambas as abordagens, o volume total da área enxertada e o volume das partículas dentro da área enxertada foram menores para o AB (45% e 37% respectivamente no artigo 1 e 31% e 33% respectivamente no Artigo 2). Para o pBCP mudanças volumétricas não ocorreram, exceto para o grupo tamanho 1,5 mm na abordagem pré-clínica, que mostrou uma redução significativa no último período (24 semanas). Conclusão: As características físico-químicas do pBCP, como a lenta reabsorção, criam um microambiente favorável para a formação óssea e isso é diretamente influenciado pelo tamanho dos grânulos. O pBCP70: 30 promove maior preservação do volume enxertado em comparação ao AB, sendo uma boa alternativa para o aumento do seio maxilar e para os procedimentos de regeneração óssea.

[pt] Na indústria do petróleo, problemas como dano mecânico causam redução da porosidade e permeabilidade de uma formação rochosa, reduzindo a produtividade e injetividade de poços de sistemas de produção de óleo e gás. Na perfuração do poço há alteração do estado de tensões no seu entorno, causando uma deformação na rocha que pode induzir a uma perda significativa da permeabilidade. Nesta dissertação foi realizado um estudo da influência do dano mecânico na porosidade de rochas do tipo arenito. Para isso, utilizou-se a técnica não-destrutiva de microtomografia de raios-x, que permite a visualização da estrutura interna de materiais, acoplada a uma célula desenvolvida para aplicação, in situ, de tensão hidrostática. Uma amostra de arenito como 8 mm de diâmetro foi tomografada em 3 condições: sem carregamento, após a aplicação de tensão hidrostática de 3300 psi e após o descarregamento. A célula permitiu que as variações de carga fossem realizadas sem retirar a amostra do tomógrafo, permitindo uma comparação quantitativa entre as imagens 3D. Nas 3 condições foram obtidos dados como porosidade total, variação da área porosa em cada camada, volume e forma dos poros. / [en] In the oil industry, problems such as mechanical damage reduce the porosity and permeability of a rock formation, reducing the productivity and injectivity of wells in oil and gas production systems. During the well drilling there is a change in the state of the stress in its surroundings, causing a deformation in the rock that can induce a significant loss of permeability. In this dissertation, it was carried out a study regarding the influence of mechanical damage on the porosity of sandstone rocks. In order to do this, the non-destructive technique of x-ray microtomography was used, which allows the visualization of the materials internal structure, coupled to a cell developed for in situ application of hydrostatic stress. A sandstone sample of 8 mm in diameter was scanned under 3 conditions: without load, after application of 3300 psi hydrostatic stress and after unloading. The cell allowed the load variations to be performed without removing the sample from the tomograph, allowing a quantitative comparison between the 3D images in the 3 conditions. Data such as total porosity, variation of the porous area in each layer, volume and shape of the pores were obtained.

Avaliação da \"qualidade\" da microarquitetura óssea contribui na prevenção e risco de fraturas associado a osteoporose. Amostras de ossos trabeculares de corpos vertebrais da região T12, L1 e L4 de 30 de indivíduos (cadáveres humanos), classificados pela técnica de ultrassonometria de calcâneo como normais, osteopênicos e osteoporóticos foram utilizadas. Os parâmetros histomorfométricos, físicos e mecânicos da microarquitetura analisados pela técnica de microtomografia de raios-X, ensaios mecânicos de compressão axial e nanoindentação. Baseado nestes parâmetros, constantes elásticas efetivas globais foram obtidas pela técnica homogeneização assintótica para estrutura tipo-placa. Teste ANOVA apresentou diferenças, muito e extremamente significativas para densidade linear estrutural (p = 0,017), grau de anisotropia (p = 0,042), auto valor (p = 0,045), número de Euler (p = 0,016), idade (p = 0,009), separação trabecular (p = 0,009), densidade de conectividade (p = 0,006), módulo de elasticidade (p = 0,001), tensão máxima no limite de resistência a fratura (0,001), índice de qualidade óssea do calcâneo (p = 0,0001), fração de volume ósseo (p = 0,0001), espessura trabecular (p = 0,0002), dimensão fractal (p = 0,0002), momento de inércia polar médio (p = 0,00005), excentricidade (p = 0,0002), fração de porosidade (p = 0,0001) e densidade mineral óssea aparente (p = 0,00005) entre os grupos. O teste de Spearman identificou correlação moderada, alta e muito alta dos valores da tensão máxima no limite de resistência a fratura com os parâmetros de idade (r = -0,684), fração de volume ósseo (r = 0,762), fator de forma trabecular (r = -0,754), espessura trabecular (r = 0,675), densidade linear trabecular (r = 0,622), autos valores (r = -0,615), dimensão fractal (r = 0,855), momento de inércia polar médio (r = 0,816), excentricidade (r = -0,569) e fração de porosidade (r = -0,762). Estes parâmetros são indicadores da qualidade da microarquitetura óssea trabecular e risco de fratura associado a osteoporose. / Evaluation of the \"quality\" of bone microarchitecture can contribute to the prevention and risk of fractures associated with osteoporosis. Samples of trabecular bone from the vertebral regions T12, L1 and L4 from the bodies of 30 individuals (human cadavers), classified by ultrasonometry technique calcaneus as normal, osteopenic and osteoporotic were used. The histomorphometric, physical and mechanical parameters of the microarchitecture were analyzed by X-ray microtomography technique, mechanical tests of axial compression and nanoindentation. Based on these parameters, globally effective elastic constants were obtained by asymptotic homogenization technique for type-plate structure. ANOVA test showed differences that were very and extremely significant for the following: structural linear density (p = 0.017) anisotropy (p = 0.042), auto value (p = 0.045), Euler number (p = 0.016), age (p = 0.009), trabecular separation (p = 0.009), connectivity density (p = 0.006), elastic modulus (p = 0.001), maximum stress fracture strength limit (0.001), bone quality score of the calcaneus (p = 0.0001), bone volume fraction (p = 0.0001), trabecular thickness (p = 0.0002), fractal dimension (p = 0.0002), mean polar moment of inertia (p = 0.00005), eccentricity (p = 0.0002), porosity fraction (p = 0.0001) and apparent bone mineral density (p = 0.00005) between groups. The Spearman test identified moderate correlation, high and very high values of maximum stress fracture resistance limit for the following parameters: age (r = -0.684), bone volume fraction (r = 0.762), trabecular bone pattern factor (r = -0.754), trabecular thickness (r = 0.675), trabecular linear density (r = 0.622), auto value (r = -0.615), fractal dimension (r = 0.855), mean polar moment of inertia (r = 0.816), eccentricity (r = -0.569) and porosity fraction (r = -0.762). These parameters are quality indicators of the microarchitecture of trabecular bone and fracture risk associated with osteoporosis.

Les roches mantelliques exposées sur le plancher océanique et/ou en contact avec l’atmosphère au niveau d’une ophiolite, sont en déséquilibre et s’altèrent, via les réactions de serpentinisation (i.e. d’hydratation et oxydo-réduction) et les réactions de carbonatation. Ces réactions d’altération jouent un rôle important dans les échanges chimiques entre la Terre profonde et les enveloppes externes, en particulier dans le cycle des volatils (C, H et O) via la minéralisation du CO2 atmosphérique, la production d’hydrogène et la formation d’hydrocarbures et de molécules prébiotiques. L’ophiolite d’Oman est un « laboratoire naturel » idéal pour étudier ces réactions depuis l’hydrothermalisme océanique jusqu’à l’altération continentale actuelle.Cette thèse présente les résultats d’une étude multi-technique et multi-échelle réalisée sur une série de péridotites serpentinisées et carbonatées échantillonnées sur deux sites, Wadi Dima et Batin (Massif de Wadi Tayin), considérés comme représentatifs des processus d’altération affectant l’ophiolite d’Oman. Ces travaux combinent caractérisations (micro-)structurales (EBSD, µ-tomographie), pétrographiques et minéralogiques (Raman, Cathodoluminescence, (3D-)XANES), et analyses géochimiques (EPMA, (LA)-ICPMS) et isotopiques (isotopes du O, C micro-bulk et in-situ).L’étude des harzburgites de Wadi Dima a permis d’identifier la succession des épisodes de serpentinisation et de carbonatation qui ont affecté les péridotites lors du refroidissement de la lithosphère jusqu’à la mise en place de l’Ophiolite d’Oman. La serpentinisation commence en domaine océanique (appauvrissement en REE, anomalie négative en Ce) durant le refroidissement initial de la lithosphère océanique et/ou au début du détachement intra-océanique à < 200-220°C, par la formation des veines de lizardite. Cette serpentinisation continue avec la formation de chrysotile au centre de la structure maillée, remplaçant l’olivine. Le dernier stade de serpentinisation a lieu simultanément au premier stade de carbonatation et engendre l’altération complète de la péridotite à < 100°C. Le système est contrôlé par des hétérogénéités locales (anomalies en Ce et variation de la composition isotopique en carbone). La carbonatation continue à < 50°C lors de la transition en domaine continental. Des veines de carbonates se forment par interaction avec des fluides issus des sédiments durant la convergence et avec des fluides de surface et de sub-surface durant l’altération actuelle de l’ophiolite. Ce processus marque le passage d’un régime hydrothermal océanique dont la chimie est dominée par la composition de la roche, à un régime hydrothermal continental dont la chimie est contrôlée par la composition du fluide dans des fractures. Paradoxalement, la structure initiale du manteau contrôle l’orientation et la distribution des veines de carbonate.Le site de Batin se distingue par sa structure complexe avec la présence de nombreux filons de gabbros et de pyroxénites et des évidences d’imprégnation magmatique. La serpentinisation y est marquée par la formation de textures atypiques en anneau ("fingerprint") caractérisées par des variations des teneurs en Fe-Mg et du redox à micro-échelle et par des compositions isotopiques en oxygène en déséquilibre. Ces caractéristiques sont interprétées comme résultant de déséquilibres locaux dans les processus de transport-nucléation-réaction pouvant être liés à plusieurs paramètres : forts gradients de température, redox, composition du fluide, et de perméabilité.Cette thèse apporte de nouvelles données vis-à-vis des relations temporelles et spatiales entre les réactions de serpentinisation et de carbonatation, les hétérogénéités chimiques à micro-échelle et l’impact de ces réactions d’altération sur les bilans globaux des volatils (C, H et O) en Oman. Elle met particulièrement en évidence la possibilité de stocker du CO2 et de produire de l’H2 simultanément lors de l’altération du plancher océanique. / Mantle rocks exposed in seafloor and/or directly in contact with atmosphere in ophiolite system are thermodynamically and chemically in disequilibrium. Mantle alteration is driven by serpentinization (ie, hydration and oxidation-reduction reactions) and carbonatization reactions. These reactions play an major role in the chemical exchanges between the deep mantle and the outer envelops, especially in the global mass budget of volatiles (C, H and O) via CO2 mineralization, hydrogen production and formation of hydrocarbons and prebiotic molecules. Oman ophiolite is an ideal "natural laboratory" for studying alteration reactions in mantle rocks from ocean hydrothermalism to modern continental weathering.This thesis presents the results of a multi-technical and multi-scale study on carbonate-hosted serpentinized peridotites in two sites, Wadi Dima and Batin (Wadi Tayin massif), considered representative of the alteration processes affecting the Oman ophiolite. This work combines (micro-) structural (EBSD, µ-tomography), petrographical (EPMA), mineralogical (Raman, Cathodoluminescence, (3D-)XANES), geochemical ((LA)-ICPMS) and isotopic studies (O, C in situ and micro-bulk).Studies in Wadi Dima harzburgites have highlighted successive episodes of serpentinization and carbonatization in Oman peridotites from oceanic lithosphere cooling to Oman Ophiolite emplacement. Serpentinization occurs in oceanic setting (REE depletion, negative Ce anomalies), probably during the onset of the oceanic lithosphere cooling and / or of the intra-oceanic detachment, at < 200-220°C, driven by the formation of lizardite veins constituting the mesh structure. Serpentinization continues at lower temperature with the formation of chrysotile in the center of the mesh structure, replacing olivine. The last stage of serpentinization is concurrent with early carbonatization and generates the complete peridotite alteration at < 100°C. In this rock-dominated system, fluid flow paths are controlled by nano-porosity (etch pits), by pore scale weakness and by local heterogeneity in permeability, generating local chemical heterogeneities (Ce anomalies variability and carbon isotope heterogeneity). Carbonatization continues at < 50°C during the transition in continental setting. Carbonate veins are formed during interaction with sediment-derived fluids during intra-oceanic detachment at the onset of obduction and with surface and sub-surface fluids during modern continental Ophiolite weathering. This process records the transition from oceanic diffuse-flow rock-dominated to cooler continental fluid-focused-flow fluid-dominated hydrothermal systems. Paradoxically, initial mantle structure controls orientation and distribution of carbonate veins.Batin site is distinguished by its complex structure with the presence of abundant gabbros and pyroxenites dikes, evidence of magmatic impregnation peridotites. Serpentinization is charcheterized by the formation of an uncommon texture in rings ("fingerprint") at the expense of olivine, marked by chemically variation in Fe-Mg and redox at microscale and by disequilibrium oxygen isotopic composition. These features are interpreted as resulting from local disequilibrium in the transport-nucleation-reaction processes that may be related to several parameters: high temperature gradient, redox, fluid composition, and permeability.This thesis brings new constraints on temporal and spatial relations between serpentinization and carbonatization reactions, on local chemical heterogeneities at micro-scale and on the global chemical budget of volatiles (C, H and O) in Oman peridotites. It has highlighted the possibility to store CO2 and producing H2 simultaneously during subseafloor alteration.

Submitted by Daniella Santos (daniella.santos@ufma.br) on 2017-06-20T14:13:09Z No. of bitstreams: 1 Lauber Jose.pdf: 935752 bytes, checksum: 4853ee9a573d926513f92f2560f03c9a (MD5) / Made available in DSpace on 2017-06-20T14:13:10Z (GMT). No. of bitstreams: 1 Lauber Jose.pdf: 935752 bytes, checksum: 4853ee9a573d926513f92f2560f03c9a (MD5) Previous issue date: 2017-06-12 / FAPEMA / The polymerization shrinkage (PS) and the detrimental effects have been the focus of studies with the aim of improving the performance of composite resins. The simplicity of technique due to the possibility of single fill in large quantities have allowed bulk fill composite resins (BFC) to be indicated to minimize this shrinkage. This thesis, divided in two chapters, aimed to evaluate the behavior of bulk fill composite resins in class I restorations by mans computerized microtomography (μCT) and microtensile bond strength (μTBS). Chapter I evaluated the PS and μTBS in BFC and conventional class I restorations composite resins, and the correlation between these factors. Class I cavities (4 x 5 x 4 mm), (factor-C = 4.2), were created in human third molars that were free of caries, which were randomized and divided into 4 groups (n = 6): Z350 XT(+): incremental insertion (II) and manual fill (MF); Z350 XT(-): single insertion (SI) and MF; TBF (Tetric N-Ceram Bulk Fill: SI and MF); and SFU [SonicFill: SI and ultrasonic fill (UF) ]. The teeth were scanned and analyzed in μCT at two times: T0- after the filling of the cavity with composite resins and T1- after the polymerization for PS. After 1 week, the teeth were sectioned crosswise in the buccolingual and mesiodistal directions to obtain specimens with approximately 1 mm² thickness and fixed to universal test machine device to perform μTBS. The data showed a statistically significant difference for PS between the groups Z350 XT(+) e Z350 XT(-), and between SF e Z350 XT(-) (Kruskal-Wallis and Dunn, p<0.05). he μTBS was higher for Z350 XT (+) than the other groups (p <0.05) and there was no correlation between PS and μTBS (p> 0.05). It was concluded that the BFC type present a PS similar to that of the conventional nanoparticulate composite resin inserted using the incremental technique. The bond strength was higher for the composite resin incrementally inserted, which presented a lower number of pre-test failures when compared to bulk fill composites. No correlation was observed between the PS and bond strength when bulk fill and conventional composites were used. Chapter II evaluated the volume of polymerization shrinkage (VS), gap (VG) and void (VV) using μCT in BFC and conventional class I restorations, and their correlations. Class I cavities (4 x 5 x 4 mm), factor-C = 4.2, were created in human third molars that were free of caries, which were randomized and divided into 5 groups (n = 6): Z350 XT(+) (II/MF); Z350 XT(-) (SI/MF); TBF (SI/MF); SFM [ (SonicFill: SI and MF) ] and SFU (SI/UF). The teeth were scanned and analyzed in μCT at two times: T0- after the filling of the cavity with composite resins and T1- after the polymerization for VG and VV, and for VS (T1-T0). After 1 week, the teeth were sectioned crosswise in the buccolingual and mesiodistal directions to obtain specimens with approximately 1 mm² thickness and fixed in a universal testing machine to perform μTBS. Kruskal-Wallis and Dunn tests showed statistically significant difference in VS for groups Z350 XT(+) and Z350 XT (-), and between SFU and Z350 XT(-), and difference between VV for Z350 XT(+) and BFC (p <0.05). There was no difference in VG between the conventional and BFC (p>0.05). There is a positive correlation between VS versus VG and between VS versus VV (Spearman, p <0.05). It was concluded that BFCs of both sonic and manual insertion showed polymerization shrinkage and gap formation similar to the incrementally inserted nanoparticulate conventional resin. There is a positive correlation between polymerization shrinkage and final gap formation, as well as between polymerization shrinkage and void in composite resins. The final gap was formed mainly by the initial gap generated during the insertion/filling of the composite in the cavity and not to the polymerization shrinkage. / A contração de polimerização (CP) e seus efeitos prejudiciais vêm sendo o foco de estudos com o intuito de melhorar o desempenho das resinas compostas. A simplicidade da técnica devido a possibilidade de preenchimento único em grande quantidade tem permitido que resinas bulk fill (RBF) sejam indicadas para minimizar essa contração. Esta tese, dividida em dois capítulos, teve por objetivo avaliar o comportamento de resinas bulk fill em restaurações classe I por meio de microtomografia computadorizada (μCT) e resistência de união por microtração (μTBS). O capítulo I avaliou a CP por μCT e a μTBS em restaurações classe I de RBF e convencional, e a correlação entre esses fatores. Cavidades classe I (4x5x4 mm), (fator-C=4,2) foram realizadas em terceiros molares livres de cárie, que foram randomizados e divididos em 4 grupos (n=6): Z350 XT(+): inserção incremental(II) e preenchimento manual (PM); Z350 XT(-): inserção única (IU) e PM; TBF (Tetric N Ceram Bulk Fill: IU e PM); e SFU [SonicFill: IU e preenchimento ultrassônico (PU) ]. Os dentes foram escaneados e analisados em μCT em dois tempos: T0- após o preenchimento da cavidade com resinas compostas e T1- depois da polimerização para CP. Após 1 semana os dentes foram seccionados transversalmente no sentido vestíbulo-lingual e mesio-distal para obtenção de espécimes com aproximadamente 1mm² de espessura, e fixados em dispositivo para máquina de ensaio universal para realizar μTBS. Os dados demonstraram diferença estatisticamente significante para a CP entre os grupos Z350 XT(+) e Z350 XT(-) e entre SFU e Z350 XT(-) (Kruskal-Wallis e Dunn, p<0.05). A μTBS foi maior para Z350 XT(+) em relação aos demais grupos (p<0.05) e não houve correlação entre CP e a μTBS (p>0.05). Concluiu-se que RBF apresentaram CP semelhante à resina convencional nanoparticulada inserida de forma incremental. A resistência de união foi maior para a resina convencional inserida pela técnica incremental que apresentou menor falhas pré-teste, quando comparada às RBF. Não foi observada correlação entre a CP e a resistência de união quando utilizadas RBF e convencionais. O capítulo II avaliou o volume de contração de polimerização (VC), gap (VG) e poro (VP) usando μCT em restaurações classe I de RBF e convencional, e suas correlações. Cavidades classe I (4x5x4 mm), fator-C=4,2, foram realizadas em terceiros molares humanos livres de cárie que foram randomizados e divididos em 5 grupos (n=6): Z350 XT(+) (II/PM); Z350 XT (-) (IU/PM); TBF (IU/PM); SFM [ (SonicFill (IU/PM) ] e SFU (IU/PU). Os dentes foram escaneados e analisados em μCT em dois tempos: T0- após o preenchimento da cavidade com resinas compostas e T1- depois da polimerização para VG e VP, e VC (T1-T0). Após 1 semana os dentes foram seccionados transversalmente no sentido vestíbulo-lingual e mesio-distal para obtenção de espécimes com aproximadamente 1mm² de espessura, e fixados em máquina de ensaio universal para realizar μTBS. Os testes de Kruskal-Wallis e Dunn, demonstraram diferença estatisticamente significante no VC em μCT para os grupos Z350 XT(+) e Z350 XT (-) e entre SFU e Z350 XT(-), e diferença entre o VP para Z350 XT(+) e as RBF (p<0.05). Não houve diferença para o VG entre as RBF e convencional (p>0.05). Houve correlação positiva entre a VC versus VG e entre VC versus VP (Spearman, p<0.05). Concluiu-se que as RBF tanto de inserção sônica quanto manual mostraram contração de polimerização e formação de gap semelhante à resina convencional nanoparticulada inserida de forma incremental. Há uma correlação positiva entre a contração de polimerização e a formação de gap final, assim como entre a contração de polimerização e poro nas resinas compostas. O gap final foi formado principalmente pelo gap inicial gerado durante a inserção/preenchimento da resina na cavidade e não à contração de polimerização.

Cette thèse sinscrit dans une dynamique de recherche qui a vu le jour assez récemment dans le domaine du séchage des boues de station dépuration. Conscientes des problèmes de gestion que va entraîner laugmentation des quantités de boue produites suite à lapplication de la législation européenne, différentes équipes de recherche se sont lancées dans létude du séchage des boues. Considérant que lépandage agricole et la valorisation énergétique demeureront les principales filières délimination pour les boues, le séchage constitue, dans les deux cas, une étape essentielle après la déshydratation mécanique. Lambition de ce travail est de contribuer à améliorer les connaissances dans le domaine du séchage convectif des boues et à mieux appréhender les changements de texture qui surviennent au cours du séchage à laide de la microtomograhie à rayons X. Le chapitre I décrit le contexte général dans lequel se situe le travail, cest-à-dire lépuration des eaux usées et la production de boues qui en résulte. La place du séchage dans les différentes filières de valorisation, compte tenu des exigences de la législation européenne, est présentée. Ensuite, un état des connaissances dans le domaine du séchage des boues ainsi quune présentation des technologies de séchage actuellement mises en oeuvre sont effectués. Ce chapitre met en évidence que létat divisé de la matière se situe au cur du travail et pose les objectifs majeurs de la présente étude. Le chapitre II est consacré à la définition des notions essentielles à létude du séchage. Le concept disotherme de sorption à leau est présenté avant de passer en revue les différents types deau que lon trouve dans les boues. Les modes de transport deau pendant le séchage sont ensuite rappelés. La suite du chapitre se concentre sur la manière dont les données de séchage sont exploitées et reprend, brièvement, les progrès effectués en modélisation de la cinétique. La fin du chapitre décrit le retrait qui constitue un phénomène indissociable du séchage des matériaux déformables dont font partie les boues. Lensemble des dispositifs expérimentaux et des méthodes utilisés au long de ce travail sont décrits dans le chapitre III. Les principaux dispositifs expérimentaux sont la cellule de filtration sous pression, le système dextrusion des échantillons, le microsécheur convectif et le microtomographe à rayons X. Les méthodes décrites concernent la caractérisation des boues, la déshydratation des boues, le filtrage des courbes de séchage, lexploitation des coupes tomographiques par analyse dimages et la manière de rassembler les informations issues du séchage et de la microtomographie. Le chapitre IV est consacré au développement dune procédure de conditionnement et de déshydratation permettant dobtenir une boue déshydratée dont la siccité est la plus élevée et la plus reproductible possible. La mise au point de cette procédure permet deffectuer cette étude sur des boues réelles. Les boues sont prélevées après létape dépaississement dans deux stations dépuration gérées par lAIDE, à Retinne et à Embourg. Les gâteaux de boue obtenus sont ensuite caractérisés : les propriétés rhéologiques sont déterminées ainsi que le taux deau liée par lintermédiaire des isothermes de désorption à leau. Des essais de séchage sur des échantillons extrudés à partir du gâteau de filtration montrent que les conditions opératoires de conditionnement et de déshydratation des boues nont pas dinfluence significative sur la cinétique. La procédure de production déchantillons mise au point (conditionnement-filtration-extrusion) est utilisée dans toute la suite du travail. Tout au long du chapitre V, linfluence de trois variables opératoires (la température, la vitesse superficielle et lhumidité absolue de lair) sur le retrait, la cinétique de séchage, la fissuration et le développement de profils dhumidité au cours du séchage dextrudats de chacune des deux boues est étudiée. Pour ce faire, les données issues du microsécheur et du microtomographe sont exploitées conjointement. Une analyse multi-zones permet de relier différents phénomènes observés se produisant de manière simultanée. Le développement de résistances intragranulaires au transfert, lapparition de gradients dhumidité à la paroi et le phénomène de fissuration sont en effet liés. Le chapitre VI aborde une caractérisation plus détaillée de la texture des échantillons, principalement dans leur état séché. À cet effet, des techniques telles la microscopie électronique à balayage, la mesure des isothermes dadsorption-désorption dazote et la porosimétrie au mercure sont utilisées en plus de la microtomographie. Le travail se termine par une conclusion rassemblant lensemble des résultats et par lénoncé de perspectives qui pourraient constituer une suite intéressante à cette étude. This thesis comes within a recent research dynamic in the field of sludge drying, according to European requirements concerning urban wastewater treatment and landfilling of biodegradable materials. Considering landspreading and utilization for energy purposes as the two major issues to eliminate sludges, drying constitutes, in both cases, an essential step after mechanical dewatering. Despite obvious economic, industrial and environmental interests, rather few studies have been devoted to wastewater sludge drying till lately. This work aims to improve the knowledge in the field of sludge drying and to better apprehend the textural changes that occur during drying by using X-ray microtomography. A first part of the work is dedicated to the development of a method allowing the production of sludge samples with a reproducible dryness, in order to realize the study on real sludges. Sludges are collected after secondary settling and thickening in two domestic wastewater treatment plants near university. Conditioning and mechanical dewatering are realized in the laboratory. Filtration cakes are characterized by different techniques : rheology, sorption isotherms, Rheological measurements indicate that, for a same sludge, elastic and viscous modulus only depends on the cake dryness. Drying experiments performed on individual cylindrical extrudates obtained from the cake show that operating conditions used for conditioning (polyelectrolyte dose) and dewatering (filtration pressure drop) have no significant influence on drying kinetics. The next part of the work shows that X-ray microtomography, despite this technique is still few used in chemical engineering, is a choice tool to follow the textural changes of individual samples submitted to convective drying. Contrary to methods traditionally or newly used (caliper, volume displacement methods, NMR,), X-ray microtomography is a non destructive, accurate and easy to use technique. The analysis of the images obtained by microtomography allows quantifying the shrinkage of the sample, the cracks and the moisture gradients at the sample wall at successive drying levels. The study of the influence of three operating variables (temperature, superficial velocity and absolute humidity of air) on the shrinkage, the development of cracks and moisture gradients is performed in a convective microdryer specially designed in the laboratory. Extragranular heat and mass transfer coefficients, intragranular diffusion coefficient and the water evaporation capacity are estimated from experimental data. A multi-zone analysis proposes to relate the different phenomena observed. Moisture gradients are induced by internal diffusional limitations and cause mechanical stresses. Cracks appear when mechanical stress exceeds the breakage level. Results show clearly that the crack extent depends on the value of the moisture gradients. The last part of the work deals with a detailed textural characterization of the dried samples. Several characterization techniques (scanning electron microscopy, mercury porosimetry, analysis of N2 adsorption-desorption isotherms, X-ray microtomography) show that the two sludges considered in the study present very different final textures. 3D images and binary images of cross sections indicate, among others, that the cracks developed during drying have different shapes and configurations. Morphological analysis of these cracks gives some ideas about the way cracks develop and brings to the fore a relation between texture and drying kinetics. Although the presence of cracks is not of the highest importance for the final quality of dried sludges, the methodology developed in this thesis can be applied to a large variety of other soft materials (food, ceramics,) for which crack formation has to be avoided because it impairs the final quality of the dried material. In the future, a fully coupled thermo-hydro-mechanical model will be implemented in a Finite Element code to quantify the evolution of the stress tensor versus the drying level especially at the onset of cracks formation. Results obtained in this thesis will allow validating the model.

Orientador: Osmir Batista de Oliveira Junior / Abstract: A regeneração óssea caracteriza-se por ser um processo fisiológico complexo que envolve a participação coordenada entre angiogênese e osteogênese. Envolve um processo de múltiplas etapas que inclui migração, proliferação e diferenciação de vários tipos de células, como células endoteliais, fibroblastos, osteoblastos e osteoclastos. Sabe-se que os biomateriais sintéticos têm demonstrado ser uma excelente alternativa ao reparo ósseo. Assim, o objetivo deste estudo foi avaliar o efeito do Biosilicato de sódio (BS) e dos compósitos 3D de 30% de hidroxiapatita e ácido poliláctico (3D 30% HA / PLA) e 30% hidroxiapatita e ácido poli (ácido láctico-co-glicólico) (30% HA / PLGA), e em defeitos críticos na calvária de ratos. Cento e vinte ratos machos de 90 dias com 350g de massa corporal em média foram aleatoriamente divididos em grupos de acordo com materiais de enxerto e tempo de análise, apresentando 6 animais em cada um. Os defeitos de tamanho crítico foram criados empregando-se uma trefina de 8 mm de diâmetro interno e preenchidos com os materiais mencionados ou apenas o coágulo sanguíneo como controle. Após 14 (T1), 30 (T2), 60 (T3), 90 (T4) e 120 dias (T5) dias do procedimento cirúrgico, a regeneração óssea foi avaliada por radiografia, microtomografia computadorizada (μ-CT) e histologia. A avaliação macroscópica mostrou biocompatibilidade em torno da área de interesse entre os biomateriais e ossos adjacentes. As imagens de μ-CT e de raios-x revelaram uma considerável formação ... (Complete abstract click electronic access below) / Resumo: The process of bone regeneration requires a coordinated coupling between osteogenesis and angiogenesis involveing a multistep process that includes migration, proliferation, and differentiation of several types of cells such as endothelial, fibroblasts, osteoblasts and osteoclasts. It is known that synthetic biomaterials have been proven to be an excellent alternative to bone repair. Thus, the aim of this study is to evaluate the effect of calcium and sodium Biosilicate (BS), a 3D scaffold of hydroxyapatite and polylactic acid (30% HA / PLA) and a hydroxyapatite and poly (lactic-co-glycolic acid) (30% HA / PLGA) composites in critical-sized calvarial defects. One hundred and twenty 90 days old male rats with 350g of body mass on average were randomly divided into groups (n = 6) according to graft materials and analysis time. Critical-size defects were created by means of a 8 mm inner diameter trephine bur and were filled with a 3D 30% HA/PLGA scaffold, 30% HA/PLA, BS or blood clot as control. After 15 (T1), 30 (T2), 60 (T3), 90 (T4) and 120 (T5) days of the cirurgical procedure, bone regeneration was evaluated by histology, x-ray and micro-computed tomography (µ-CT). Macroscopic evaluation showed no significant inflamation around the interest area. µ-CT results indicates that 30% HA/PLA and 3D 30% HA/PLGA composites were not fully degraded and images revealed considerable bone formation in 90 days and 120 days in relation to these materials. On the other hand, BS presented a ... (Resumo completo, clicar acesso eletrônico abaixo) / Doutor