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A deeper understanding of the role of water in dielectric-differential thermal analysis is presented.

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In mineralogical research differential thermal analysis can be applied as either a single or a combined method for three purposes:1.for the qualitative identification of minerals and the (semi-)quantitative determination of the components of rocks and soils,2.for the characterization of crystal-physical and crystal-chemical properties, including the study of kinetics and the determination of thermodynamic data, phase and reaction equilibria,3.for special petrogenetic investigations concerning the interrelation of mineralogical properties with the formation, decomposition or recrystallization of minerals.

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The effect of the addition of Ag2O on the mechanism of non-isothermal devitrification of Li2O · 2 SiO2 glass has been studied by differential thermal analysis. In both bulk and powdered samples, the presence of heterogeneous nuclei lowers the crystallization temperatures but not the value of the crystal growth activation energy.

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A study has been made of the differential thermal analysis of (i) potassium perchlorate in powdered form, (ii) potassium perchlorate in pelletized form, (iii) potassium perchlorate recrystallized from liquid NH3, and (iv) potassium perchlorate preheated for 24 hours at 375°. Pretreatment of potassium perchlorate leads to a desensitization of both endothermic and exothermic processes. Additionally, the pretreatment tends to convert the symmetric exotherm into an asymmetric exotherm due to merging of the two exotherms. An analysis of the factors causing asymmetry in the exotherm has thrown fresh light on the mechanism of thermal decomposition of potassium perchlorate.

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Abstract  

Differential thermal analysis (DTA) of low-rank coals of high lignite to subbituminous rank from coal mines of Pakistan is reported. The studies carried out in dynamic oxygen atmosphere indicate that the exothermic reactions occur between 300 and 650°C and that the samples undergo stepwise oxidation of the organic matter rather than a continuous process as indicated by the pattern of shoulders from 250 to 350°C accompanying the main peak around 450°C. The effect of heating rate, particle size and volatile content was also studied in relation to oxidation. The results show that the increase in heating rate from 10 to 80 deg min−1 results in a marked shift in all the events in the DTA curve towards higher temperatures. As for the effect of particle size, the DTA records of 100–75, 150–100, 250–150 μm and greater than 250 μm fractions show that the magnitude and position of shoulder peaks are more sensitive to changes in particle sizes compared to the main peak. The curves recorded to study the effect of changing volatile content of samples between 30–40% indicate a complex pattern of shoulders accompanying the main peak. In general, the number of shoulder peaks increases with increasing volatile content of samples but their positions do not follow any trend. The DTA curves recorded in nitrogen contain ill-de-fined oxothermic effects over the 300–750°C temperature range. These curves consist of an endothermic peak around 150°C, two exothermic shoulders in the temperature region 300–400°C and a large broad exothermic whip between 500 and 700°C. The heating rates have similar effects as in oxygen while the particle size do not influence the results. It has been concluded that the organic matter in the coals studied here is extremely heterogeneous with different burning characteristics; as a result it is very difficult to quantify energy changes associated with poorly resolved exothermic events along the DTA curve. The effects also dominate in N2 atmosphere thus making identification of mineral matter difficult. The overall pattern of DTA events in oxygen can be correlated with the heating rate, particle size and volatile content of samples.

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This article is a review of some of the results we have obtained by studying various kinds of emulsions using techniques from the simplest one, a home-made differential thermal analysis to elaborated ones such as differential scanning calorimetry commercial devices. These techniques were used not only to determine energetic values but also essentially to show and quantify physical chemical phenomena such as undercooling, freezing, melting, mass transfer between droplets and solid formation involved in hydrate formation.

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In the present paper the thermal behaviour of Mg-carbonates and -silicates is reviewed and discussed, based on own DTA investigations and data from the literature. Mg-bearing minerals in soils and sediments offer informations about the palaeoenvironment and palaeoclimatology of sediments and soils and - thus - the study of their crystal chemical compositions by means of (differential) thermal analysis informs about environmental conditions of (sedimentary Mg-) mineral (trans-) formations. The paper stresses (1) the interrelations between decomposition temperatures of (Mg-) carbonates and substitution processes and is (2) concerned with the interdependence between the dehydroxylation behaviour of Mg-bearing sheet silicates and their crystal chemical composition.

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Many chemical systems illustrating major reaction types may be conveniently studied by differential thermal analysis. The problems of vaporization and sublimation have been avoided through the use of sealed glass vials. Sample sizes are in the range of 10 to 100 milligrams. This size though small is still more than adequate for chemical analysis by instrumental methods such as infrared spectroscopy and gas chromatography.

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The melting behavior of poly(vinylidene chloride) (PVDC) was studied using differential thermal analysis (DTA). Crystals were grown isothermally from 0.1% and 0.02% dilute solutions of the polymer in 1.2-dibromoethane and monobromobenzene. Both ‘solid’ and ‘oil’ samples were used for the DTA experiments. ‘Solid’ samples are defined as dried down crystals and ‘oil’ samples are crystals which have been suspension exchanged in silicone oil without letting them dry out. Thermal curves of ‘solid’ samples are similar to those obtained previously with as-polymerized crystals, that is they show two endotherms. The lower temperature peak corresponds to the melting of lamellae as formed. The upper peak at around 200°C, may be due to the melting of crystals which have reorganized during heating. Thermal curves of ‘oil’ samples show two extra small peaks in addition to those of the ‘solid’ samples. From the results of annealing and degradation experiments, these two peaks may correspond to a small portion of the crystals which have been partially degraded to form double bonds and thus possess lower melting points. An alternative explanation is that there is an as yet unreported second crystal form of PVDC.

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Abstract  

The so-called DSP (Densified Systems containing homogenously arranged Particles) systems represent a high-performance class of inorganic binders. The hydration and hardening processes of some DSP systems, based on calcium silicates (C3S and C2S) or Portland cement/clinker with silica fume additions, were assessed, in this paper, using the thermogravimetry (TG) and differential thermal analysis (DTA). These data permit a qualitative and quantitative study of the formed hydrates as well as the estimation of hydration process kinetics.

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