Kinetic analysis of thermogravimetric data on some nickel(II) N-alkyldithiocarbamates
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Thermogravimetric and derivative thermogravimetric curves of some complexes [Ni(S2CNHR)2] (R=Me, Et, Pri, Bui, But, Bz,p-MePh,p-MeOPh,p-ClPh,p-NO2Ph) in a dynamic nitrogen atmosphere were studied to determine their modes of decomposition. All these complexes show similar TG profiles. The weight losses in the main decomposition stages indicate conversion of the nickel(II) dithiocarbamates to sulphide. Reaction orders were estimated via the shape characteristics of the corresponding derivative thermogravimetric curves and kinetic analysis of the thermogravimetric data was performed by using the Coats-Redfern and Horowitz-Metzger methods.Keywords:
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Abstract The Ni(II), Cu(II) Co(II) and Zn(II) complexes of 2,3‐hydroxyimino‐4‐phenyl‐6‐phenyazo‐1‐thia‐4,5‐diaza‐ cyclohexa‐5‐diene (H 2 L) were synthesized. Thermal behavior of these complexes was studied in dynamic nitrogen atmosphere by TA (thermogravimetric analysis), DTA (differential thermal analysis) and DTG (differential thermal gravimetry) techniques. The reaction order, the activation energies, the entropies, the enthalpies, the free energies, and the pre‐exponential factors of the thermal decomposition reactions were calculated from the thermogravimetric curves. The kinetic analysis of the thermogravimetric data was performed by using several methods such as MacCallum‐Tanner (MT), van Krevelen (vK), Madhusudanan‐Krishnan‐Ninan (MKN), Wanjun‐Yuwen‐Hen‐Cunxin (WYHC), Horowitz‐Metzger (HM) and Coats‐Redfern method (CR) based on the single heating rate. Most appropriate methods were determined for each decomposition step according to the least‐square linear regression. The Ni(II), Cu(II) Co(II) and Zn(II) complexes displayed one‐ or two‐stage decomposition pattern when heating in a dynamic nitrogen atmosphere and metal oxides remained as end products of the complexes. The characterization of the end products of the decomposition was performed by X‐ray diffraction.
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Thermal decomposition of [Cu4O(Cl+Br)6(OPPh3)4], starts at temperatures about 200°C. The decomposition proceeds in several steps. The intermediate formed in the first decomposition step (weight loss 2–4%) is a new crystalline phase with slightly different structure but with preserved central unit Cu4O. The only crystalline phases found in the further decomposition products was CuBr in all cases when the bromine atoms were present, the presence of CuCl was only observed at the decomposition of the hexachlorocomplex.
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Experiments on the thermal decomposition of CuSe were carried out by using a thermogravimetric analyzer (TGA) at different heating rates. The kinetic parameters and mechanisms were discussed based on model-free and model-based analyses. The decomposition rate and decomposition behavior of CuSe were investigated by using a vacuum thermogravimetric furnace. The results showed that the R3 model was identified as the most probable mechanism function under the present experimental conditions. The average values of activation energy and the pre-exponential factor were 12.344 J/mol and 0.152 s-1, respectively. The actual decomposition rate of CuSe was found to be 0.0030 g/(cm2·min).
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Abstract Thermal decomposition of ZnHg(SCN) 4 (ZMTC) in air was investigated by means of thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The intermediates and final products of the thermal decomposition were identified by X‐ray powder diffraction at room temperature. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)
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