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  • Author or Editor: P. Thomas x
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Abstract  

A complex oxalate precursor, CaCu3(TiO)4(C2O4)8·9H2O, (CCT-OX), was synthesized and the precipitate that obtained was confirmed to be monophasic by the wet chemical analyses, X-ray diffraction, FTIR absorption and TG/DTA analyses. The thermal decomposition of this oxalate precursor led to the formation of phase-pure calcium copper titanate, CaCu3Ti4O12, (CCTO) at ≥680°C. The bright-field TEM micrographs revealed that the size of the as synthesized crystallites to be in the 30–80 nm range. The powders so obtained had excellent sinterability resulting in high density ceramics which exhibited giant dielectric constants upto 40000 (1 kHz) at 25°C, accompanied by low dielectric losses, <0.07.

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Abstract  

Thermal analysis has been employed in a study of the degradation of heritage Sydney sandstone used in St Mary’s Cathedral in Sydney, Australia. TG and DSC have been used to characterise the clay components removed from weathered and unweathered sandstone. Two types of kaolin clays — kaolinite and its polymorph, dickite — have been identified. A higher amount of dickite present in the clay of weathered sandstone indicates that a kaolinite-to-dickite transformation occurs upon weathering. XRD hot stage analysis was also used to demonstrate the presence of a more thermally stable polymorph of the kaolinite.

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Abstract  

The utilisation of fired clay-brick waste is of interest in the manufacture of building products due to both socio-economic and technological reasons. Autoclaving is an established process for manufacturing calcium silicate-based building products that affords rapid strength development. Clay-brick waste represents a source of alternative silica, which is more reactive than conventionally used silica and also contains alumina. This paper presents data on the effect of lowering the autoclaving temperature from commonly practised 180 to 170°C on OPC-quartz blends containing clay-brick fines as direct replacement of quartz at 4.3, 8.6 and 12.9 mass percentages. The hydration products of autoclaved OPC-quartz blends with clay-brick fines were characterised using simultaneous DTA-TG in combination with other methods.

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Abstract  

The thermal properties are presented for a precious opal sourced from Coober Pedy, South Australia and a moldavite from Bohemia, Czech Republic whose origins differ significantly as opal is derived from the slow isothermal diagenesis of silica, while the tektites are specimens of vitreous silica formed from the terrestrial impact of asteroids. The differences between the two glassy silicates are presented through measurement of the TG–DSC, TMA and high-vacuum-hot-extraction DEGAS analysis.

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Abstract  

The degradation of poly(vinyl alcohol) was investigated using TG analysis and Fourier transform infrared spectroscopy to determine the effect of atmosphere on the process of degradation. In the spectra, four vibrational modes were identified that characterised the major steps of the degradation process. These were the O-H, C-H, C=O and C=C stretching modes. The mechanism observed for degradation in an inert atmosphere was in accordance with the accepted mechanism of elimination followed by pyrolisation. Evidence of conjugated polyenes, however, was not observed. For the air atmosphere, oxidation in both steps of the degradation process was observed.

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Abstract  

The thermal decomposition of electrolytic manganese dioxide (EMD), in an inert atmosphere, and the effect of chemical reduction on EMD, using 2-propanol under reflux (82C), was investigated by differential scanning calorimetry (DSC). This study is an extension of a study investigating the thermal decomposition of EMD and reduced EMD by TG-MS (J. Therm. Anal. Cal., 80 (2005)625)). The DSC characterisation was carried out up to 600C encompassing the water loss region up to 390C and the first thermal reduction step. Water removal was observed in two distinct endothermic peaks (which were not deconvolved in the TG-MS) associated with the removal of bound water. For the lower degrees of chemical reduction, thermal reduction resulted in the formation of Mn2O3; for higher degrees of chemical reduction, the thermal reduction resulted in Mn3O4 at 600C. In the DSC the thermal reduction of the EMD and chemically reduced specimen was observed to be endothermic. The reduced specimens, however, also showed an exothermic structural reorganisation.

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Abstract  

The deleterious interaction of some traditional sulphide artists pigments and copper ions results in the formation of black copper sulphides, in particular, covellite (CuS), and, hence, the discolouration of valuable artworks. In this paper the interaction of malachite, a source of copper(II) ions, with the pigment cadmium yellow, a sulphide pigment comprising of a solid solution of cadmium and zinc sulphides, is investigated by XRD and TG-MS. XRD showed the presence of the copper sulphide and cadmium carbonate phases, produced by a simple ion exchange mechanism. TG-MS showed the complexity of the range of metastable phases produced. The identification of these phases, however, requires further work.

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Abstract  

An accurate means of determining bone age is a goal for forensic scientists. In this study, thermogravimetric analysis (TGA) has been used to examine pig bone specimens of different post-mortem age. Analysis of bone in both air and nitrogen atmospheres reveals a decrease in total mass loss as the bones age. Two mass loss steps due to the decomposition of the organic bone components were observed and show decreasing trends with age for decomposition in an air atmosphere. In a nitrogen atmosphere the decomposition was observed to be more complex and age dependence of the mass loss for each step was not identified. The TGA data, however, demonstrates the potential of the technique as a means of estimating post-mortem age of forensic bone specimens.

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Résumé  

Une méthode d'étude de la composition stoéchiométrique de couches minces (10 à 500 μg/cm2) de verres chalcogénures est développée. L'étude des réactions nucléaire; induites par bombardement de protons de basse énergie (<4 MeV) sur les éléments constitutifs Ge, As, Te et S, conduit à choisir la diffusion élastique et la détection de gammas prompts pour le dosage simulatené. La précision et la sensibilité de la méthode sont discutées à partir des résultats obtenus. L'utilisation de la résonance fine sur le soufre (p, p'γ) est appliquée à l'étude de l'homogénéité des cibles.

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Abstract  

Analytical procedures for measuring various radionuclides in the238U and232Th chains in briney waters are described. Using methods such as mass spectrometry, and alpha, beta and gamma spectrometry, the desired measurement sensitivity required for each of the radionuclides is achieved.233U,228Th,208Po,212Pb, and133Ba are used as tracers for chemical yield recoveries. Typical precision of the results range from 5–20%.

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