Studying the effects of extreme conditions, such as high temperatures and low humidity, on soil properties is important to various disciplines, including geotechnical engineering, soil science, waste management, crop management, and ceramics. The goal of this research is to investigate the effect of environmental and geometrical factors on microstructure, desiccation cracking, and CO2 flux in clays. The objectives of this research are threefold. (1) Understand the effects of temperature on the microstructure of clay soils; (2) develop a standardized procedure for studying desiccation cracking in a laboratory setting with reliable and repeatable results; and (3) develop an environmental chamber capable of monitoring CO2 flux through a soil sample large enough to accommodate a fully developed crack network. To accomplish these objectives, an array of laboratory testing was conducted. First, this study examines the effects of extreme temperatures on the microstructural properties of clay using FESEM, cation-exchange capacity (CEC) tests, thermal gravimetric analysis (TGA), and Brunauer–Emmett–Teller (BET) surface area analyzer. Second, a standardized procedure for producing accurate and repeatable laboratory tests on the desiccation cracking of soils is presented. The procedure includes specifications for sample collection, material preparation and characterization (including microstructural properties), and the determination of a representative elemental area (REA) for a fully developed crack network. Finally, a new climatic chamber capable of controlling temperature and relative humidity is designed and tested. The chamber can monitor CO2 flux through a fully developed crack network, enabling fundamental research on the relationship between desiccation cracking and the oxidation of soil organic carbon. The key findings indicate a dependency of soil microstructure on temperature changes. CEC and BET surface area significantly decrease with temperatures beyond 100ºC, indicating a relationship that needs further study. Additionally, compacted and slurry cracking behavior was found to be sensitive to boundary geometry and sample thickness. A REA was identified for each slurry sample thickness. The procedures of this research can be repeated for other soil types and used to connect existing and future research to improve understanding of desiccation cracking behavior, and to study the effects of desiccation cracking on other important geo-environmental phenomena.

[pt] Rochas carbonáticas possuem atributos únicos que as distinguem das siliciclasticas e necessitam de diferentes métodos de estudo para caracterizar sua textura. Rochas carbonáticas são resultado de interações entre processos deposicionais químicos e biológicos. Os processos diagenéticos que formam e alteram estas rochas contribuem para o acúmulo de heterogeneidades. Devido ao alto teor de heterogeneidade, as propriedades medidas (e.g. porosidade e permeabilidade) variam com a escala de investigação e estudos com o compromisso a significância dos detalhes e representação espacial. Ampliar uma escala menor para maior, exige procedimentos que preservem a essência dos processos físicos de um nível mais detalhada para um mais grosseiro. Métodos simplificados para dimensionar propriedades não aditivas em outras escalas, tal como permeabilidade, geralmente não honram a heterogeneidade presente em sistemas complexos. Com isso a dinâmica dos fluidos em rochas complexas exige abordagens e métodos mais sofisticados. Este estudo é focado em desenvolver uma metodologia de avaliação da permeabilidade como parâmetro de escala para meios porosos heterogêneos. A permeabilidade é retro calculada ao emular o experimento de Darcy e resolver o fluxo no meio poroso utilizando uma formulação de elementos finitos para equação de Brinkman. O estudo iniciou com foco em sistemas paramétricos de células periódicas e posteriormente a duas microtomogra fia de rochas carbonáticas, do qual uma foi selecionada para um estudo de representatividade espacial. As células periódicas foram utilizadas para avaliar os efeitos da formação de canais e espaços vazios, em analogia a fraturas e vugos, assim como os efeitos da permeabilidade da matriz porosa. As amostras carbonáticas consistem de casos nos quais é possível observar a presença de uma combinação dos fenômenos estudadas. Por fim um estudo de representatividade foi conduzido segmentando uma amostra de micro-tomografia em suficientes sub-amostras que capazes de reproduzir a heterogeneidade espacial da amostra original. / [en] Carbonate rocks have unique attributes that distinguish them from siliciclastics and that require diferent methods of study to characterize their texture. Carbonates rocks are formed as a result of close interactions between biological and chemical depositional processes. The underlying diagenetic processes that form and alter these rocks contribute to a build-up of heterogeneities. Because of the high heterogeneity content measured properties (e.g. porosity and permeability) change with the scale of investigation and studies have struggle with a trade-off between significance of details and space representativeness. Extending a smaller scale to a larger requires scaling up procedures that preserves the essence of physical processes at one level to be summarized at the coarser level. Simplistic methods for scaling-up non-additive properties such as permeability generally do not honour the original heterogeneity present in complex systems. Therefore the dynamics of fluid flow in complex rocks demand more sophisticate methods and approaches. This study was focused in developing a methodology to evaluate the permeability as a scaling-up parameter for heterogeneous porous media. The permeability is back-calculated by emulating Darcy s experiment and solving the pore-scale ow using a Finite element formulation of Brinkman flow equation. The study was initially focused on parametric systems of periodic cells and later extended to two micro-tomography carbonate samples in which one has been selected for a spatial representativeness study. The parametric cells were used to evaluate the shape effects of channels and void spaces in an analogy to geological fractures and vugs as well as the permeability of the porous matrix. The micro-tomography carbonate samples consisted of a real case scenario in which, to a certain degree, could be observed a combination of the previously studied periodic cells. Finally a representativeness study was conducted segmenting the micro-tomography sample into suficiently sub-samples that would be capable of reproducing the spatial heterogeneity of the sample.