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Journal of Thermal Analysis and Calorimetry
Authors: N. R. Sperandeo, C. V. Mattia, and Maria M. de Bertorello

The tautomeric binary system consisting of N-(3,4-dimethyl-5-isoxazolyl)-4-amino-1,2-naphthoquinone (1),m.p. 156‡C, and 2-hydroxy-N-(3,4-dimethyl-5-isoxazolyl)-1,4-naphthoquinon-4-imine (2),m.p. 218‡C, was studied by DTA-TG-DTG and IR spectrometry. Crystals of 1, left in contact with their mother liquor during 4 months, exhibited thermal behaviour similar to that of physical mixtures of 1 and 2, which reveal the presence of a eutectic at about 146‡C.

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The mechanochemical solid-state adsorption of the cationic dye crystal violet (CV) by montmorillonite was investigated by XRD and simultaneous DTA-TG. Solid CV was ground with the clay for 5 min and four different varieties of CV mechanochemically treated clay were investigated. X-ray and DTA data were compared with those of CV-montmorillonite obtained from an aqueous suspension. X-ray and DTA studies of a ground mixture and a ground mixture heated at 110°C suggest that the mechanochemical adsorption of organic cations takes place on the external surfaces of the clay. The study of a ground mixture washed with water, and washed with water and acetone reveal that water is essential for the penetration of CV into the interlayer space.

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This study reports experimental investigations by DTA/TG analysis of (1−x)SnO2xCuO compositions, up to 1773 K and at two oxygen partial pressures (i.e. air and argon). In air, DTA/TG results showed thermal effects due exclusively to CuO presence in the initial mixture. No binary compounds were formed. The reduction process of CuO to Cu2O over 1273 K as well as the formation over 1373 K of the liquid phase, have been evidenced. In argon atmosphere, CuO to Cu2O reduction reaction is shifted toward 1205 K, while the liquid phase appears in the studied mixtures over 1473 K. The formation of an eutectic composition between SnO2−Cu2O, melting at 1491 K, coordinates:0.932Cu2O+0.068SnO2, has been experimentally established in argon.

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DTA/TG coupling

Applications in the field of superconducting materials with high critical temperature

Journal of Thermal Analysis and Calorimetry
Author: J. L. Jorda

With the discovery of high temperature superconductivity an extraordinary field for investigations on new materials containing up to (more than) 8 or 9 components has been open. But, in addition to problems specifically related to superconductivity, we are faced with a prelimary difficulty: the preparation of well defined compounds which may have reproducible properties. This difficulty is smoothed out when the phase relations in the relevant systems are known. Differential Thermal Analysis (DTA) contributes to their establishment. However, in multicomponent systems, an isopletic line is expected to intercept various boundary surfaces and the analysis is obviously complicated, compared to low order systems. In addition, by the nature of high temperature superconductors the oxygen partial pressure used for their preparation is an important thermodynamic parameter which contributes to fix the oxygen content in the solid state. During heat treatments, the composition of the systems may change, due to oxygen or volatile oxides (Tl2O3, PbO2 or HgO) release. A permanent composition control then requires thermogravimetric (TG) measurements associated to DTA.

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best tool which allows to determine the thermal decomposition of organic substances in ceramic samples and the proper heating program seems to be DTA/TG measurements [ 20 ]. The important information from thermal analysis is the temperature at which

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In order to get insight in some of the yet unanswered questions about the formation process of the (Bi,Pb)2Sr2Ca2Cu3O10+δ superconducting compound, coupled DTA-TG measurements have been performed in parallel with other techniques such as X-ray diffraction, Scanning Electron Microscopy and Energy Dispersive X-ray Microanalysis. The path leading to the formation of the (Bi,Pb)2Sr2Ca2Cu3O10+δ compound, starting from coprecipitated oxalates powders was studied. The activation energy of some of the involved transformation processes were determined. Relationships between the differences induced in the DTA traces by various sample nominal compositions and the intergranular magnetic properties of the superconductor will be discussed.

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Simultaneous DTA-TG is an excellent technique for evaluating phases formed in hydrothermally treated CaO-SiO2-H2O and CaO-Al2O3-SiO2-H2O systems. Thermal analysis in combination with XRD and SEM, revealed that in the CaO-Al2O3-SiO2-H2O system the amount of hydrogarnet formed was the largest when gibbsite was used as the Al source, smallest for kaolin and intermediate for metakaolin. The endotherm peak temperature of the hydrogarnet dehydration endotherm was affected by the amount of hydrogarnet and the Si content of hydrogarnet. The thermal stability and structural order of 11 Å tobermorite were reduced with the incorporation of Al and, as a result, 11 Å tobermorite transformed into 9.3 Å tobermorite at lower temperatures while the transformation of the latter into beta-wollastonite required more energy. There exists a direct relationship between the 9.3 Å tobermorite and beta-wollastonite formation temperatures. Solid-state 29Si and 27Al MAS NMR data support these findings.

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Reactivity in the solid-state between ZnWO4 and some RE2MoO6 (RE=Y, Sm, Eu, Gd, Dy, Ho, Er and Lu) was investigated by XRD and DTA-TG methods. Four new compounds with the formula ZnRE2MoWO10 (RE=Sm, Eu, Gd, Dy) were synthesized. The obtained compounds are isostructural and crystallize in the monoclinic system. They melt incongruently within the temperature range of 1016–1033°C. The solid product of melting is an adequate of rare-earths molybdate.

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X-ray, magnetic and differential thermal analysis and thermogravimetric (DTA-TG) measurements of Fe2O3 nanoparticles surrounded by amorphous SiO2were carried out. The mass loss above 370 K could be attributed to the dehydration. The broadened exothermic peak around 900 K was observed by the DTA analysis. Considering the results of the X-ray and magnetic analyses, this anomaly was interpreted as due to the g- to a-transition in the present Fe2O3nanoparticle system. The broadness of the peak and thus the gradual progress of the transformation would be attributed to the stress caused by the amorphous SiO2 network surrounding extremely small particles.

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