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-controlled simultaneous TG, DTG, DTA, TD and EGA apparatus. Part I. - Journal of Thermal Analysis, 32, pp. 301--310. Derivatograph-C. A microcomputer-controlled simultaneous TG, DTG, DTA, TD and EGA apparatus. Part I

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Thermal decomposition kinetics of some aromatic azomonoethers

Part III. Non-isothermal study of 4-[(4-chlorobenzyl)oxy]-4′-chloroazobenzene in dynamic air atmosphere

Journal of Thermal Analysis and Calorimetry
Authors: A. Rotaru, Anca Moanţă, P. Rotaru, and E. Segal

Abstract  

Thermal analysis of 4-[(4-chlorobenzyl)oxy]-4′-chloro-azobenzene dye, exhibiting liquid crystalline properties, was performed in dynamic air atmosphere. The compound behavior was investigated using TG, DTG, DTA and DSC techniques, under non-isothermal linear regime. The evolved gases were analyzed by FTIR spectroscopy. Kinetic parameters of the first decomposition step were obtained by means of multi-heating rates methods, such as isoconversioanl methods, IKP method and Perez-Maqueda et al. criterion.

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Mesoporous materials MCM-41 with the hexagonal arrangement of pores were obtained using dodecyltrimethylammonium bromide and octadecyltrimethylammonium bromide as templating surfactants. Adsorption of toluene and propan-1-ol on the as-synthesized MCM-41 silica samples was investigated using the TG-DTG, DTA and DSC techniques. The sorption mechanism of used adsorptives is discussed in terms of hydrophobicity of pore interior filled with template as well as pore dimensions.

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Thermal analysis of some fly ashes

I. Gastitrimetric determination of carbon and sulfur contents of fly ashes

Journal of Thermal Analysis and Calorimetry
Authors: K. Szécsényi, M. Arnold, K. Tomor, and F. Gaál

Abstract  

The thermal behavior of different fly ashes from the electrical precipitators of various pulverized carbon fuel-fired boilers was investigated by means of simultaneous TG, DTG, DTA and EGA analysis. The carbon and sulfur contents of the samples were determined by gastitrimetry. The compositions of the samples were examined by X-ray diffraction. The quantitative oxide analysis of the ashes was carried out by means of a classical method.

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The thermolysis of zinc bis(citrato)ferrate(III)dodehydrate has been investigated from ambient temperature to 600 °C using various physico-chemical techniques, i.e., simultaneous TG-DTG-DTA, XRD, Mössbauer and I.R. spectroscopy. After dehydration at 200 °C, the anhydrous complex undergoes oxidative decomposition to yield -Fe2O3 and ZnO at 350 °C. Subsequently, the cations remix to yield fine particles of zinc ferrite, ZnFe2O4 as a result of solid state reaction between -Fe2O3 and ZnO at a temperature (450 °C) much lower than for ceramic method.

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Abstract  

Thermal decomposition of ammonium tris (malonato) ferrate (III) tetrahydrate, i. e. (NH4)3[Fe(CH2C2O4)3]·4H2O has been studied up to 973 K in static air atmosphere employing Mössbauer and infrared spectroscopies, and non-isothermal techniques (TG, DTG, DTA). The anhydrous complex decomposes into an iron (II) intermediate at 453 K. The iron (II) species on further heating is reoxidized to -Fe2O3 as the final thermolysis product. An increase in particle size of -Fe2O3 with increasing decomposition temperature has been observed. The results are compared with the analogous oxalate complex.

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Abstract  

Thermal behaviors of two mixed-ligand complexes, [Ni(PMPP-SAL)(Py)3] and [Cu(PMPP-SAL)Py]·MeOH, (PMPP-SAL=1-phenyl-3-methyl-4-(salicylidene hydrazide)-propenylidene-pyrazolone-5, Py=pyridine), were studied by TG-DTG-DTA in dynamic air atmosphere. The complexes show the loss of pyridine molecule is followed by the decomposition of the PMPP-SAL anion and give respective metal oxides as residues. Meanwhile, the Ozawa-Flynn-Wall model-free analyses and multivariate non-linear regressions were applied to perform single and overall steps optimization. Kinetic parameters were given and the most probable mechanism functions were suggested in this study.

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Abstract  

The thermal behaviour of ordered kaolinites from Hungary and Australia intercalated with potassium acetate, cesium acetate and urea has been investigated by simultaneous TG-DTG-DTA, TG-MS, Raman microscopy and XRD. Remarkable changes in the thermal decomposition pattern of the intercalates were obtained as a function of the nature of the intercalating re-agents. Replacing the potassium cation to cesium leads to a change in the OH environments resulting in a more complicated dehydroxylation pattern. The urea intercalates can be decomposed completely without dehydroxylating the mineral, although further treatments are necessary to restore the original d-spacing.

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Abstract  

A novel AB2-type monomer diethyl 5-(4-hydroxyethoxyphenylazo)isophthalate for preparing hyperbranched azo polymers (HBPAZO) was synthesized. The monomer obtained was characterized by IR spectra, UV–Vis spectra, 1H NMR spectrum and C NMR spectrum. The TG-DTG/DTA curves show that the decomposition of the monomer proceeds in four steps. During the second-step decomposition, the mass loss occurs between 480.5 K and 579.0 K and the phenomena of condensing to HBPAZO for the melted monomer was found. So it is inferred that this temperature range is the best for polycondensation of the melted monomer, which is very important for synthesizing of HBPAZO.

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Abstract  

Thermal decomposition of M(mal/fum)�xH2O (M=Mn, Co, Ni) has been studied in static air atmosphere from ambient to 500�C employing TG-DTG-DTA, XRD and IR spectroscopic techniques. After dehydration the anhydrous maleate salts decompose to metal oxalate in the temperature range of 320–360�C, which at higher temperature undergo an abrupt oxidative pyrolysis to oxides. The anhydrous fumarate salts have been found to decompose directly to oxide phase. A comparison of thermal analysis reveals that fumarates are thermally more stable than maleates.

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