Thermal behaviour of nickel amine complexes containing SO42−, NO3−, Cl− and Br− as counter ions and ammonia and ethylenediamine as ligands have been investigated using simultaneous TG/DTA coupled with mass spectroscopy (TG/DTA–MS). Evolved gas analyses detected various transient intermediates during thermal decomposition. The nickel ammonium sulphate complex produces NH, N, S, O and N2 species. The nickel ammonium nitrate complex generated fragments like N, N2, NO, O2, N2O, NH2 and NH. The halide complexes produce NH2, NH, N2 and H2 species during decomposition. The ligand ethylenediamine is fragmented as N2/C2H4, NH3 and H2. The residue hexaamminenickel(II) sulphate produces NiO with crystallite size 50 nm. Hexaammine and tris(ethylenediamine)nickel(II) nitrate produce NiO in the range 25.5 nm and 23 nm, respectively. The halide complexes produce nano sized metallic nickel (20 nm) as the residue. Among the complexes studied, the nitrate containing complexes undergo simultaneous oxidation and reduction.
This is a preview of subscription content, log in to check access.
The authors are grateful to Prof. T. Ichikawa, the Institute for Advanced Materials Research, Hiroshima University, Japan, for the TG–MS analyses.
Mathew S, Nair CGR, Ninan KN. Thermal decomposition kinetics: kinetics and mechanism of thermal decomposition of tetraamminecopper(II) sulphate monohydrate. Thermochim Acta. 1989;144:33–43.CrossRefGoogle Scholar
Kapoor IPS, Kapoor M, Singh G, Singh UP, Goel N. Preparation, characterization and thermolysis of nitrate and perchlorate salts of 2,4,6-trimethylaniline. J Hazard Mater. 2010;173:173–80.CrossRefGoogle Scholar
Mathew S, Nair CGR, Ninan KN. Thermal decomposition kinetics: kinetics and mechanism of thermal decomposition of bis(ethylenediamine)copper(II) halide monohydrate. Thermochim Acta. 1991;181:253–8.CrossRefGoogle Scholar
Alcolea A, Ibarra I, Caparrós A, Rodríguez R. Study of the MS response by TG–MS in an acid mine drainage efflorescence. J Therm Anal Calorim. 2010;101:1161–5.CrossRefGoogle Scholar
Yu Z, Sun Y, Wei W, Lu L, Wang X. Preparation of NdCrO3 nanoparticles and their catalytic activity in the thermal decomposition of ammonium perchlorate by DSC/TG-MS. J Therm Anal Calorim. 2009;97:903–9.CrossRefGoogle Scholar
Vogel AI. A text book of quantitative inorganic analysis. 4th ed. New York: Longmann; 1978.Google Scholar
Mockenhaupt C, Eßmann R, Lutz HD. [Ni(NH3)6]SO4: crystal structure and infra red spectra. Z Naturforsch. 1999;54b:843–8.Google Scholar
Cotton FA, Wilkinson G. Advanced inorganic chemistry. 5th ed. New York: Wiley; 1988.Google Scholar
Skoczylas ML, Mikuli E, Szklarzewicz J, Hetmańczyk J. Thermal behaviour, phase transition and molecular motions in [Co(NH3)6](NO3)2. Thermochim Acta. 2009;496:38–44.CrossRefGoogle Scholar
Madarász J, Bombicz P, Mátyás C, Réti F, Kiss G, Pokol G. Comparative evolved gas analytical and structural study on trans-diammine-bis(nitrito)-palladium(II) and platinum(II) by TG/DTA-MS, TG-FTIR, and single crystal X-ray diffraction. Thermochim Acta. 2009;490:51–9.CrossRefGoogle Scholar
Norris AC, Pope MI, Selwood M. The determination of kinetic parameters for reactions involving solids. Thermochim Acta. 1980;41:357–60.CrossRefGoogle Scholar
Frost AA, Pearson RG. Kinetics and mechanism. New York: Wiley; 1961.Google Scholar