Fast time-resolved micro-CT imaging of pharmaceutical tablets: Insights into water uptake and disintegration.

We use dynamic micro-computed tomography (micro-CT) with a high temporal resolution to visualize water penetration through the porous network of immediate-release pharmaceutical solid tablets and characterize dynamic swelling and disintegration mechanisms. We process the micro-CT images using two theoretical scenarios that reflect different paths of pore structure evolution: a scenario where tablet porosity remains constant during the swelling process and a scenario where the tablet porosity progressively diminishes and eventually closes during the swelling process. We calculate the time evolution of the volume of water absorbed by the tablet and, specifically, absorbed by the excipients and the pore structure, as well as the formation and evolution of cracks. In turn, the three-dimensional disintegration pattern of the tablets is reconstructed. Restricting attention to the limiting scenario where tablet porosity is assumed fixed during the swelling process, we couple liquid penetration due to capillary pressure described by the Lucas-Washburn theory with the first-order swelling kinetics of the excipients to provide a physical interpretation of the experimental observations. We estimate model parameters that are in agreement with values reported in the literature, and we demonstrate that water penetration is dominated by intra-particle porosity rather than inter-particle porosity.

Reactivity of Gypsum-Based Materials Subjected to Thermal Load: Investigation of Reaction Mechanisms.

The thermal stability of gypsum-based materials, and in this context, especially their long-term behavior, is the background of our current research activities. A comprehensive investigation program was compiled in which detailed examinations of various model materials exposed to thermal loads were carried out. The understanding of the partly not entirely consistent state of knowledge shall be sharpened especially by in situ observations of the thermally induced conversion reaction of gypsum into hemihydrate. The temporal course of the reaction was investigated non-destructively by in situ investigations in a high-resolution X-ray computed tomography setup, and the experiment was accompanied by detailed characterizations of the microstructure and composition. In this contribution, selected results of experiments with a high-purity natural gypsum rock as the model substance are presented. Studying the influence of temperature on the reaction showed that, even under supposedly dry conditions, the reaction could take place at much lower temperatures than usually reported in the literature. It was demonstrated that the transformation of gypsum into hemihydrate could take place at a temperature of already 50 °C. The results indicated that even under "classical" heating conditions in a conventional oven, the dissolution and crystallization processes in water films on the mineral surfaces could be suggested to be a driving force for the reaction. A corresponding reaction model, which took these aspects into account, was proposed in this work.

High-resolution X-ray CT for 3D petrography of ferruginous sandstone for an investigation of building stone decay.

Diestian ferruginous sandstone has been used as the dominant building stone for monuments in the Hageland, a natural landscape in east-central Belgium. Like all rocks, this stone type is sensitive to weathering. Case hardening was observed in combination with blackening of the exterior parts of the dressed stones. To determine the 3D petrography and to identify the structural differences between the exterior and interior parts, X-ray computed tomography was used in combination with more traditional research techniques like optical microscopy and scanning electron microscopy. The 3D characterization of the ferruginous sandstone was performed with a high-resolution X-ray CT scanner (www.ugct.ugent.be) in combination with the flexible 3D analysis software Morpho+, which provides the necessary petrophysical parameters of the scanned samples in 3D. Besides providing the required 3D parameters like porosity, pore-size distribution, grain size, grain orientation, and surface analysis, the results of the 3D analysis can also be visualized, which enables to understand and interpret the analysis results in a straightforward way. The complementarities between high-quality X-ray CT images and flexible 3D software and its relation with the more traditional microscopical research techniques are opening up new gateways in the study of weathering processes of natural building stones.

Three-dimensional analysis of high-resolution X-ray computed tomography data with Morpho+.

Three-dimensional (3D) analysis is an essential tool to obtain quantitative results from 3D datasets. Considerable progress has been made in 3D imaging techniques, resulting in a growing need for more flexible, complete analysis packages containing advanced algorithms. At the Centre for X-ray Tomography of the Ghent University (UGCT), research is being done on the improvement of both hardware and software for high-resolution X-ray computed tomography (CT). UGCT collaborates with research groups from different disciplines, each having specific needs. To meet these requirements the analysis software package, Morpho+, was developed in-house. Morpho+ contains an extensive set of high-performance 3D operations to obtain object segmentation, separation, and parameterization (orientation, maximum opening, equivalent diameter, sphericity, connectivity, etc.), or to extract a 3D geometrical representation (surface mesh or skeleton) for further modeling. These algorithms have a relatively short processing time when analyzing large datasets. Additionally, Morpho+ is equipped with an interactive and intuitive user interface in which the results are visualized. The package allows scientists from various fields to obtain the necessary quantitative results when applying high-resolution X-ray CT as a research tool to the nondestructive investigation of the microstructure of materials.