Carbonate rocks are of global importance as they contain about 50% of the world’s remaining hydrocarbon reserves and are also a major host to the world’s groundwater resources. Therefore, understanding and modelling the fluid flow processes in carbonates are of great importance. A critical problem is that, unlike homogenous media (such as sandstones), carbonates often show features, including porosity, that span across a wide spatial range, from sub-micron porosity to fractures of meters length-scale. In this study X-ray computed micro-tomography (μCT) has been utilised as a tool to monitor two phase (oil-brine) flow in porous carbonate (dolomite) plugs at ambient temperature and pressures smaller than 690 kPa. A simple, low-cost and highly X-ray transparent core-holder was utilised for which the design is introduced. Capillary end effects were recognised and avoided in data analysis. Displacement processes that occur in the dolomite under water-wet, oil-wet, and partially mixed-wet states were investigated. The experiments consisted of a series of drainage and imbibition processes occurring under capillary and viscous dominated flow regimes. Pore-scale mechanisms of piston-like displacement and snap-off (or at least clear results of them), that were previously observed in sandstones and 2D micro-models, were observed in the dolomite under study. In addition, a new pore-scale mechanism was identified which occurred at high capillary numbers, referred to as droplet-fragmentation. This new pore-scale mechanism may provide an explanation to the capillary-desaturation process for heterogeneous media. In the experiments performed on the oil-wet plug formation of a stable water in oil emulsion was observed which appears to be the first 3D observation of in situ emulsion formation made using μCT. Direct visualisation of the oil-brine-rock configurations and measurement of the contact angles are presented. A comparison was made for the contact angle distributions measured for the water-wet and oil-wet conditions. Observation of fluid displacement processes as well as oil-brine-rock contact angle distributions demonstrate that pore-scale imaging provides a promising tool for wettability characterisation on both pore and core scales. Such detailed wettability data can also be used in pore-scale flow models. For the dolomite under study multiple-scale pore network models were constructed by integrating single-scale networks extracted from μCT images acquired at different length-scales. Mercury injection capillary pressure laboratory measurements were used to evaluate the capillary pressure (vs. saturation) curves calculated using single, two-scale, and three-scale network models of this dolomite. The integrated networks displayed an improved match to the laboratory measurements in comparison with the single-scale network model. The three-scale network provided the closest simulated curve, this result confirms that a more representative model displays closer properties. While simulated capillary pressure curves are close (converging) for the integrated networks the calculated relative permeability curves show variability for different multiple-scale networks. The present work demonstrates that the pore-scale fluid displacement processes occurring in heterogeneous porous media are more complex than those occurring in homogeneous media. In addition, successful fluid flow simulations require construction of multiple-scale models as well as consideration of the pore-scale processes (such as droplet-fragmentation) that are specific to such complex pore systems.

O objetivo do presente trabalho foi avaliar, ex vivo, a eficiência dos sistemas rotatórios ProTaper Universal Retreatment Files e Mani Retreatment Files na desobturação de raízes mesiais de molares inferiores, obturadas pela técnica de ondas contínuas de condensação, determinando-se o volume percentual de material obturador remanescente no sistema de canais radiculares, utilizando-se a microtomografia de raios-X. Um total de 18 molares inferiores portadores de dois canais radiculares mesiais que possuíam curvatura entre 25° e 35° e raio de curvatura menor que 10mm, foram preparados até o instrumento 35/.04 Mtwo. Em seguida foram obturados com guta percha e cimento endodôntico AH-Plus pela técnica de ondas contínuas de condensação e mantidos em estufa a 37°C por sete dias. Imagens microtomográficas dos dentes obturados foram realizadas utilizando o microtomógrafo SkyScan 1172 e parâmetros de 100kV e 100A, gerando imagens de tamanho de 11,88m. Em seguida, os dentes foram divididos aleatoriamente em dois grupos experimentais de acordo com o tipo de instrumento de retratamento avaliado, ProTaper Retreatment Universal Files (PR) e Mani Retreatment Files (MR). De início, a desobturação dos canais radiculares foi realizada com a utilização de brocas de largo associadas a uma gota de solvente para que então os instrumentos de cada sistema fossem utilizados até que a desobturação até o nível do comprimento real de trabalho, fosse alcançada. Após novo escaneamento, as imagens foram reconstruídas utilizando-se o software NRecon e analisadas pelo software CTAn, permitindo a obtenção dos dados quantitativos das amostras. Empregou-se o teste t de Student para determinar a ocorrência de diferença estatística entre os grupos experimentais (p < 0.05). Os volumes, inicial e final médios (mm3) de material obturador remanescente foram de 17,72 e 2,12 para o grupo PR e de 16,61 e 3,71 para o grupo MR, respectivamente. O grupo PR apresentou o menor volume percentual médio de material obturador remanescente (12,76 ± 6,93%), quando comparado ao MR (23,54 ± 10,60%), observando-se diferença estatisticamente significante. Nenhum dos dois sistemas testados, foi capaz de remover completamente o material obturador do interior dos canais radiculares. O sistema rotatório ProTaper Universal Retreatment Files mostrou-se mais eficiente que o sistema Mani Retreatment Files na desobturação de canais mesiais de molares inferiores, obturados pela técnica de ondas contínuas de condensação. As características dos sistemas rotatórios de retratamento podem interferir no volume percentual de material obturador remanescente e conseqüentemente na sua eficiência de desobturação. / The objective of this study was to evaluate, ex vivo, the efficiency of rotary ProTaper Universal Retreatment Files and Mani Retreatment Files in removal procedure of the mesial roots of mandibular molars, obturated by the technique of continuous wave of condensation, determining the volume percentage of material remaining filling in root canals, using the X-Ray micro-CT. A total of 18 mandibular molars with two root canals which had mesial curvature between 25° and 35° and the radius of curvature smaller than 10mm, were prepared by the instrument Mtwo size/taper 35/.04. They were then filled with gutta-percha and sealer Ah-Plus by the technique of continuous wave of condensation and maintained at 37°C for seven days. Micro-CT images of the teeth was carried out using the device SkyScan 1172 on 100kV and 100A as parameters, generating images size 11.88 micrometers. Then the teeth were randomly divided into two groups according to the type of instrument retreatment evaluated ProTaper Universal Retreatment Files (PR) and Mani Retreatment Files (MR). Initially, the procedure for remove the root canal obturation was performed with Largo burs associated with a drop of solvent so that the instrument of each system could be used until the complete removal procedure was reached. After re-scanning, the images were reconstructed with the software used NRecon and analyzed by CTAn software, allowing to obtain quantitative data of the samples. We used the Student t test to determine the occurrence of significant differences between experimental groups (p <0.05). The mean initial and final volumes (mm3) of the remaining filling material were 17.72 and 2.12 for the P group and 16.61 to 3.71 for group MR, respectively. The PR group had the lowest average volume percentage of remaining filling material (12.76 ± 6.93%) when compared to MR (23.54 ± 10.60%), with a statistically significant difference. Neither of the systems tested were able to completely remove the filling material inside the root canals. The rotary system ProTaper Universal Retreatment Files was more efficient than the system Mani Retreatment Files in removal procedure of mesial canals, filled with the technique of continuous wave of condensation. The characteristics of rotary retreatment system may interfere with the volume percentage of remaining filling material and consequently the efficiency of removal procedure.

O objetivo do presente trabalho foi avaliar, ex vivo, a eficiência dos sistemas rotatórios ProTaper Universal Retreatment Files e Mani Retreatment Files na desobturação de raízes mesiais de molares inferiores, obturadas pela técnica de ondas contínuas de condensação, determinando-se o volume percentual de material obturador remanescente no sistema de canais radiculares, utilizando-se a microtomografia de raios-X. Um total de 18 molares inferiores portadores de dois canais radiculares mesiais que possuíam curvatura entre 25° e 35° e raio de curvatura menor que 10mm, foram preparados até o instrumento 35/.04 Mtwo. Em seguida foram obturados com guta percha e cimento endodôntico AH-Plus pela técnica de ondas contínuas de condensação e mantidos em estufa a 37°C por sete dias. Imagens microtomográficas dos dentes obturados foram realizadas utilizando o microtomógrafo SkyScan 1172 e parâmetros de 100kV e 100A, gerando imagens de tamanho de 11,88m. Em seguida, os dentes foram divididos aleatoriamente em dois grupos experimentais de acordo com o tipo de instrumento de retratamento avaliado, ProTaper Retreatment Universal Files (PR) e Mani Retreatment Files (MR). De início, a desobturação dos canais radiculares foi realizada com a utilização de brocas de largo associadas a uma gota de solvente para que então os instrumentos de cada sistema fossem utilizados até que a desobturação até o nível do comprimento real de trabalho, fosse alcançada. Após novo escaneamento, as imagens foram reconstruídas utilizando-se o software NRecon e analisadas pelo software CTAn, permitindo a obtenção dos dados quantitativos das amostras. Empregou-se o teste t de Student para determinar a ocorrência de diferença estatística entre os grupos experimentais (p < 0.05). Os volumes, inicial e final médios (mm3) de material obturador remanescente foram de 17,72 e 2,12 para o grupo PR e de 16,61 e 3,71 para o grupo MR, respectivamente. O grupo PR apresentou o menor volume percentual médio de material obturador remanescente (12,76 ± 6,93%), quando comparado ao MR (23,54 ± 10,60%), observando-se diferença estatisticamente significante. Nenhum dos dois sistemas testados, foi capaz de remover completamente o material obturador do interior dos canais radiculares. O sistema rotatório ProTaper Universal Retreatment Files mostrou-se mais eficiente que o sistema Mani Retreatment Files na desobturação de canais mesiais de molares inferiores, obturados pela técnica de ondas contínuas de condensação. As características dos sistemas rotatórios de retratamento podem interferir no volume percentual de material obturador remanescente e conseqüentemente na sua eficiência de desobturação. / The objective of this study was to evaluate, ex vivo, the efficiency of rotary ProTaper Universal Retreatment Files and Mani Retreatment Files in removal procedure of the mesial roots of mandibular molars, obturated by the technique of continuous wave of condensation, determining the volume percentage of material remaining filling in root canals, using the X-Ray micro-CT. A total of 18 mandibular molars with two root canals which had mesial curvature between 25° and 35° and the radius of curvature smaller than 10mm, were prepared by the instrument Mtwo size/taper 35/.04. They were then filled with gutta-percha and sealer Ah-Plus by the technique of continuous wave of condensation and maintained at 37°C for seven days. Micro-CT images of the teeth was carried out using the device SkyScan 1172 on 100kV and 100A as parameters, generating images size 11.88 micrometers. Then the teeth were randomly divided into two groups according to the type of instrument retreatment evaluated ProTaper Universal Retreatment Files (PR) and Mani Retreatment Files (MR). Initially, the procedure for remove the root canal obturation was performed with Largo burs associated with a drop of solvent so that the instrument of each system could be used until the complete removal procedure was reached. After re-scanning, the images were reconstructed with the software used NRecon and analyzed by CTAn software, allowing to obtain quantitative data of the samples. We used the Student t test to determine the occurrence of significant differences between experimental groups (p <0.05). The mean initial and final volumes (mm3) of the remaining filling material were 17.72 and 2.12 for the P group and 16.61 to 3.71 for group MR, respectively. The PR group had the lowest average volume percentage of remaining filling material (12.76 ± 6.93%) when compared to MR (23.54 ± 10.60%), with a statistically significant difference. Neither of the systems tested were able to completely remove the filling material inside the root canals. The rotary system ProTaper Universal Retreatment Files was more efficient than the system Mani Retreatment Files in removal procedure of mesial canals, filled with the technique of continuous wave of condensation. The characteristics of rotary retreatment system may interfere with the volume percentage of remaining filling material and consequently the efficiency of removal procedure.