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Abstract  

An incremental integral isoconversional method for the determination of activation energy as a function of the extent of conversion is presented. The method is based on the treatment of experimental data without their transformation so that the resulting values of activation parameters should not be biased. The method was tested for recovering the activation energies from simulated data and employed for the treatment of experimental data of the NiS recrystallisation.

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Abstract  

Nickel sulphide (NiS) was characterised using X-ray diffraction, thermal gravimetric analysis (TG) and differential scanning calorimetry (DSC). The 'as received' Millerite, stoichiometric NiS, observed to be slightly nickel deficient, was found to readily decompose in a nitrogen atmosphere at elevated temperatures (450C max.) to the sulphur deficient Godlevskite, Ni7S6. DSC and X-ray measurements demonstrated that the high temperature form of the Godlevskite was readily stabilised at room temperature. The kinetics of the α-β re-transformation in Godlevskite were then investigated using DSC and were observed to be first order.

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Résumé  

Le dosage de l'oxygène par radioactivation avec les particules chargées alphas et hélions-3 a été appliqué au silicium et au germanium. Des précisions ont été apportées aux conditions opératoires en analyse non destructive qui est utilisable à l'heure actuelle en toute sécurité pour le silicium. Une méthode nouvelle d'isolement du fluor-18 est proposée en présence des activités étrangères créées à partir de la matrice dans l'irradiation du germanium.

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Abstract  

Bone provides an important source of forensic evidence. The storage conditions of bone have been recognised as a factor in maintaining the integrity of such evidence. Thermogravimetric analysis (TG) has been employed to examine the effects of storage environments and preparation methods on the structural properties of pig bones. A comparison of oven and freeze drying has been made to study the effect of storage conditions. A comparison has also been made of ground bone specimens with cut specimens. Freeze-dried hand ground specimens provided the most consistent results and, thus, this is the recommended method of preparation of bone specimens for TG analysis.

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Abstract  

Using the pulse radiolysis competition kinetic technique, OH radical rate constants with 12 metal DTPA complexes were determined in neutral aerated aqueous solutions. They are in the range of /1.3–5.9/×109 dm3 mol–1s–1. To a first approximation, the rate constant was found to decrease linearly with an increase in the field strength of the metal ion (q/r2).

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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  

The reactivity of MgO obtained from calcination of magnesium carbonate at different temperatures has been investigated by means of hydration in a constant relative humidity environment at 40°C for periods up to 24 days. Natural magnesite and AR grade basic MgCO3 calcined in the range of 500–1000°C was characterised in terms of surface area, crystallite size, morphology, and hydration rate. It was found that the hydration rate is dependent on the surface area and crystallite size where temperature was the main variable affecting them. The most reactive MgO was produced at the lowest calcination temperature with the highest surface area and the smallest crystallite size. The basic MgO specimens showed higher degree of hydration compared to the natural MgO specimens due to the smaller surface area and larger crystallite size. The low MgO content of the starting natural magnesite is also attributable to the lower reactivity. This preliminary study serves as a mean to investigate potential utilisation of reactive MgO as a supplementary cementitious material in eco-friendly cements.

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Abstract  

The hydration products of hydrothermally cured OPC-quartz blends incorporating clay-brick waste were characterised using simultaneous DTA-TG, XRD and SEM. The exotherm above 800°C on the DTA curve, due to the formation of β-wollastonite (β-CS) was related to the compressive strength. The area and/or height of the exotherm increased with compressive strength and was due primarily to the presence of calcium silicate hydrate phases including 1.1 nm tobermorite. Supporting evidence is provided by XRD and SEM.

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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  

Naturally occurring opals from three different regions in Australia were studied for their thermal characteristics. All the opals showed initial expansion followed by contraction in thermomechanical analysis (TMA) although the temperature at which the change from expansion to contraction occurred depended on their provenance. Thermogravimetric analysis (TG) revealed different rates and temperatures of dehydration for these opals. A general correlation between the temperature at which there was a zero thermal expansion and that of the maximum rate of dehydration was observed. A dehydration–sintering mechanism is proposed with the effect of sintering being more pronounced following total dehydration.

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