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Abstract  

Solid state Ln–L compounds, where Ln stands for light trivalent lanthanides (L–Gd) and L is tartrate, have been synthesized. Thermogravimetry and differential thermal analysis (TG/DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration and thermal decomposition of the isolated compounds.

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Journal of Thermal Analysis and Calorimetry
Authors: Konstantin Gavrichev, Mikhail Ryumin, Alexander Tyurin, Andrey Khoroshilov, Larisa Mezentseva, Alexander Osipov, Valeriy Ugolkov, and Viktor Gusarov

Abstract  

Thermal behavior of LaPO4·nH2O and NdPO4·nH2O nanopowders from room temperature to 973 K was investigated by DSC, TA/DTG, ESM, and X-ray study. Mass loss due to the release of adsorbed and hydrate water was found in the range from 323 to 623 K. Phase transitions from hexagonal structure nanopowders to monoclinic one for bulk specimens were found above 873 K.

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The investigations concerning the thermal behaviour of a series of Ni(II) and Cu(II) complexes of type [MLCln]· mH2O ((1) M:Ni, L:L(1), n=1, m=2; (2) M:Cu, L:L(2), n=1, m=2; (3) M:Ni, L:L(3), n=2, m=0; (4) M:Cu, L:L(3), n=1, m=2) are presented in this paper. The ligands L(1)-L(3) have been synthesised by template condensation of 1,2-diaminoethane with formaldehyde and 2-amino-1,3,4-thiadiazole-5-thiole or 2-acetamino-1,3,4-thiadiazole-5-sulfonamide. The bonding and stereochemistry of the complexes have been characterised by IR, electronic and magnetic studies at room temperature. The thermal behaviour provided confirmation of the complex composition as well as the number and the nature of water molecules and the intervals of thermal stability. The different nature of the ligands and/or the metallic ions generates a different thermal behaviour for complexes. The complexes do not show biological activity against HIV virus.

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Abstract  

In order to obtain a better understanding of thermal substituent effects in 1,2,4-triazole-3-one (TO), the thermal behavior of 1,2,4-triazole, TO, as well as urazole and the decomposition mechanism of TO were investigated. Thermal substituent effects were considered using thermogravimetry/differential thermal analysis, sealed cell differential scanning calorimetry, and molecular orbital calculations. The onset temperature of 1,2,4-triazole was higher than that of TO and urazole. Analyses of evolved decomposition gases were carried out using thermogravimetry–infrared spectroscopy and thermogravimetry–mass spectrometry. The gases evolved from TO were determined as HNCO, HCN, N2, NH3, CO2, and N2O.

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Abstract  

The thermal behaviour of 2- and 4-biphenylmethanol were studied by differential scanning calorimetry (DSC). It was found that the 2-isomer shows a relatively strong resistance to crystallisation, and that it easily vitrifies on cooling. Oppositely, 4-biphenylmethanol readily crystallizes on cooling. The slow molecular mobility of 2-biphenylmethanol in the amorphous solid state was studied by DSC and by thermally stimulated depolarisation currents (TSDC). Both techniques indicate that 2-biphenylmethanol is a relatively strong glass-former, with a fragility index of ~50 in the Angell's scale.

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Abstract  

The thermal behavior of montmorillonite and organically modified montmorillonite, both treated with heavy metal cations [Cu(II), Cd(II) and Hg(II)], was characterized via thermal analyses (TG, DTG and DTA) combined with evolved species gas mass spectrometry (MS-EGA), and X-ray diffraction at in situ controlled temperature (HTXRD). The reactions involving Cu(II)- and Cd(II)-montmorillonite samples are mostly related to H2O and OH loss, unlike Hg(II)-montmorillonite, where effects associated to Hg(II) loss are also present. Finally reactions related to dehydration, dehydroxylation and to organic matter decomposition can be observed in montmorillonite samples treated with cysteine.

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The mono- and di-imines of some diaminonaphthalenes were prepared using a solid solid reaction technique. Their structures were studied using elemental analysis, infrared and electronic spectra. The thermal behaviour of the obtained compounds and their solid solid preparation reactions have also been studied. The energies of activation as well as the reaction orders of those reactions were determined.

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Abstract  

Poly(2-hydroxyethoxybenzoate), poly(ε-caprolactone), and random poly(2-hydroxyethoxybenzoate/e-caprolactone) copolymers were synthesized and characterized in terms of chemical structure and molecular mass. The thermal behavior was examined by DSC. All the samples appear as semicrystalline materials; the main effect of copolymerization was lowering in the amount of crystallinity and a decrease of melting temperature with respect to homopolymers. Flory's equation described well the T m-composition data. Amorphous samples (in the 20–100%2-hydroxyethoxybenzoate unit concentration range) obtained by quenching showed amonotonic decrease of the glass transition temperature T g as the content of caprolactone units is increased. The Wood's equation described the T g-composition data well.

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Abstract  

Thermal investigation has allowed us to show the changes undergone by a sort of nitrile-butadiene rubber (NBR) as a consequence ofγ-radiation-induced ageing. The parameters of the processes, which occur at progressive heating of the investigated samples, were determined. It was shown that for γ-irradiated samples the activation parameters corresponding to the thermo-oxidative process leading to solid products are correlated through the relation of compensation effect. Also, it was shown that, by γ-irradiation, NBR undergoes a relatively rapid change of its thermal behaviour which can be due to structural changes.

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Abstract  

The influence of additions of 2, 4, 6, 8, 10 and 12 mass% Ag on the thermal behavior of the Cu–8 mass% Al alloy was studied using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffractometry (XRD). The results indicate that the presence of silver introduces new thermal events, due to the formation of a silver-rich phase and, for additions of 10 and 12 mass% Ag, it is possible to verify the formation of the γ1 phase (Cu9Al4) and the metastable transitions which are only observed in alloys with a minimum of 9 mass% Al.

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