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Abstract  

Hydrogen sulphate, nitrate and perchlorate salts of diphenylamine have been prepared and characterized by elemental, spectral and gravimetric analyses. Thermal decomposition of these salts has been evaluated by TG (static air) and DSC (inert atmosphere). The proton transfer reaction plays a major role during thermolysis of these salts. The diphenylammonium hydrogen sulphate under thermal and microwave irradiation forms 4-(phenylamino) benzenesulphonic acid by sulphonation process, whereas nitrate and perchlorate salts do not form corresponding nitro and perchloro derivatives, rather they ignite and explode, respectively, to form gaseous products along with a residual carbon .

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Abstract  

Phenylenediammonium dibromide (PDADBr) salts have been prepared and characterized by X-ray crystallography. The thermal decomposition of PDADBr has been studied by thermogravimetry (TG) and differential thermal analysis (DTA). Kinetic parameters have been evaluated using model fitting and isoconversional methods. The thermolytic pathways have also been suggested which involve proton transfer as a primary step to regenerate parent amine and HBr. Interaction between amine and HBr at higher temperature yields gaseous products.

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Abstract

Recent work has described the preparation and characterization of the two complexes [Fe2(C10H8N2)4O(OH2)2](NO3)4 and [Co(C10H8N2)3]2[Co(OH2)6]·7(OH2) (NO3)8 in which both the nitrogen atoms of 2,2′-bipyridine are directly bonded with the metals. Their structures were determined by single-crystal X-ray diffraction at 296 K. Thermolysis of these complexes has been detailed by the use of TG–DTA and ignition delay measurements. Kinetics of thermal decomposition has also been established. Model free isoconversional and model fitting kinetic approaches have been applied to isothermal TG data for the decomposition of these complexes.

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Journal of Thermal Analysis and Calorimetry
Authors: Gurdip Singh, A. K. Shrimal, Inder Pal Singh Kapoor, Chandra Prakash Singh, Dinesh Kumar, and Manan S. Mudi

Abstract

Three transition metal perchlorate complexes of general formula [M(dah)2)](ClO4)2 (where M = Zn, Cu, and Ni; dah = 1,6-diaminohexane) have been prepared, and characterized by elemental analysis, infrared spectroscopy (IR), and gravimetric method. The thermal decomposition has been studied by thermogravimetry (TG), differential thermal analysis (DTA), and differential scanning calorimetry (DSC). Kinetics parameters of their thermolysis were evaluated by model-fitting and isoconversional methods using isothermal TG data. Model-fitting method has given the single value of activation energy (E) whereas; isoconversional method yields a series of E values which vary with the extent of conversion. Further ignition delay of these complexes was measured to see the response toward rapid heating with varying amounts. The thermal stability of the complexes decreases in the order as: [Zn(dah)2)](ClO4)2 > [Cu(dah)2)](ClO4)2 > [Ni(dah)2)](ClO4)2

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