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The fabric of mineral liner materials that had been exposed to organic compounds over a 12-year period was investigated as part of a wider research project. Macromorphological and micromorphological changes in the fabric were identified using computed tomography and polarisation microscopy.
Special care was taken to ensure artefact free sampling and sample preparation, in particular, the drying method used, has a substantial influence on the quality of the thin sections.
Fabric changes due to contaminant permeation over several years are, by and large, relatively small and their intensity is material specific. Silty clay CML1, in particular, contains a somewhat greater number of fissures and voids in comparison with the original material. The superposition of various processes in both test procedures and sample preparation may lead to fabric changes which can impede interpretation of the results.
In this paper the characterisation of functionally graded materials is elucidated by several different methods. These methods described here are used for the quantitative analysis of materials with a local dependence of microstructure parameters. Using X-ray microscopy (computed tomography) for 3D-measurements and optical microscopy on polished sections for 1D and 2D measurements on the same sample, a ceramic filter consisting of sintered spherical particles, various mathematical evaluation methods are described and compared.
Micro-computed tomography (µCT) provides quantitative three-dimensional information of bone around titanium implants similar to classical histology. The study, based on an animal model, using cuboid-shaped biofunctionalised Ti6Al4V implants with surrounding bone after 4 weeks, is performed using 3 µCT-systems with X-ray tubes, one synchrotron-radiation-based µCT-system (SRµCT), and classical histology. Although the spatial resolution of the µCTsystems is comparable, only the results of SRµCT agree with results of classical histology. The X-ray tube sources give rise to huge artefacts in the tomograms (interface scattering, beam hardening), which impaired the quantitative analysis of bone up to about 200 µm from the implant surface. Due to the non-destructive character of µCT the specimens can be subsequently examined by classical histology
without restriction. The quantitative comparison of bone formation uncovers the strong dependence of the detected amount of newly formed bone from the selected slice. This
implies the necessity of 3D analysis. SRµCT and classical histology prove that surface modifications of the titanium implant significantly influence the bone formation. Using SRµCT, the preparation artefacts due to cutting and polishing are excluded.
Rock porosity determination by combination of X-ray computerized tomography with mercury porosimetry
(1997)
Abstract First results are described of coupling of mercury porosimetry with X-ray computerized tomography (CT) as a new combination technique for rock porosity studies. This technique is suitable for rock samples with a pronounced mercury intrusion-extrusion hysteresis and includes CT measurements before and after mercury intrusion. The entrapped portion of mercury, when the pressure after the intrusion into the rock sample is reduced to 0.1 MPa, serves as a contrast agent in the porous network to localize spatial distribution of rock porosity by CT. The results obtained show that the mercury intrusion and therefore the porosity were quite different for the separate mineral phases. Therefore the combination of mercury porosimetry and computer tomography can give 3-D data on mineral-specific porosity distributions with additional pore size information. In contrast to mercury porosimetry as a single method, results of the combination technique with CT represent a direct visualization of porosity variation and do not depend on any special pore network model.
The application of two sets of methods for the characterization of rock pore systems is reported. Both are discussed in the context of other techniques described in the literature. (i) Impregnation with labelled polymethylmethacrylate (PMMA) and autoradiography or direct measurement of the tracer activity allows the investigation of the pattern of the spatial porosity distribution and quantitative measurement of mineral-specific, local porosities, porosity gradients as well as an assessment of hydraulic and diffusive transport properties. (ii) Quantitative information on surface areas within certain pore size ranges can be achieved by combination of mercury intrusion porosimetry with X-ray absorption computertomography. As examples of applications of these techniques, the effects of weathering, alteration, mechanical stress and large diameter coring on the pore network of rocks have been studied.
Archaeological bone, ivory and antler, as well as objects manufactured from them, are largely studied to extract as much information as possible from these materials. Among others, one key question in archaeology is the exact identification of the material. Even if the identification of different kinds of osseous material seems to be trivial in many cases, it can be a difficult issue when small, heavily carved and more or less altered ancient objects are concerned. This study was focused on the determination of parameters allowing the distinction of archaeological ivory, bone and antler in order to identify the raw material used for the manufacture of prehistoric objects. The high performance of synchrotron radiation (SR) and laboratory-based micro X-ray computed tomography (microCT), providing highly resolved three-dimensional information on the micromorphology, permitted the establishment of such distinctive features of modern references of ivory, antler, land mammal and whale bones: ivory shows characteristic tubular pores with a diameter of about 1 to 2 µm, bone and antler show typical osteon structures. In our measured references, antler shows on average larger and more elongated shaped pores of the osteons compared to terrestrial mammal bone. This feature however depends very much on the original localization of the studied sample within the antler. Whale bones can be distinguished from the other osseous materials by a cancellous, osteoporotic-like structure with irregularly distributed rounded porosities with diameters reaching up to 500 µm. These characteristics have also been tested on determined Palaeolithic fragments, as diagenetic changes during burial have to be considered and may lead to the modification of the parameters established on the basis of modern bone references. In general, the chemical composition of bone objects can change drastically over time while micromorphological features, as evidenced by microCT, seem to be less susceptible to such alterations. In addition, microCT enables the comparison of inner and possibly less altered parts of the objects, and can be considered as completely non-destructive for small mineralised prehistoric objects. In this study, specific morphological features allowing the distinction of ivory and of whale bone from other bone and antler material were determined, even for altered materials dating back to Palaeolithic periods. Thus, we provide, in addition to archaeozoological, chemical and isotopic markers, a new non-destructive tool to identify some raw materials used for the fabrication of osseous objects ranging from recent to prehistoric periods.
The use of high brilliance and partial coherent synchrotron light for radiography and computed tomography (CT) allows to image micro-structured, multi-component specimens with different contrast modes and resolutions up to submicrometer range. This is of high interest for materials research, life science and non-destructive evaluation applications. An imaging setup for microtomography and radiography installed at BESSY II (a third generation synchrotron light source located in Berlin, Germany) as part of its first hard X-ray beamline (BAMline) can now be used for absorption, refraction as well as phase contrast dedicated to inhouse research and applications by external users. Monochromatic synchrotron light between 6 keV and 80 keV is attained via a fully automated double multilayer monochromator. For imaging applications the synchrotron beam transmitted by the sample is converted with a scintillator into visible light. By use of microscope optics this luminescence image is then projected onto, e.g., a CCD chip. Several scintillating materials are used in order to optimise the performance of the detector system. Different optical systems are available for imaging ranging from a larger field of view and moderate resolutions (macroscope up to 14 mm x 14 mm field of view) to high resolution (microscope down to 0.35 μm pixel size), offering magnifications from 1.8× to 40×. Additionally asymmetric cut Bragg crystals in front of the scintillator can be used for a further magnification in one dimension by a factor of about 20. Slow and fast cameras are available, with up to 16 bit dynamic range. We show the suitability of the setup for numerous applications from materials research and life science.