Investigations on the thermal behaviour of [Ni(NH3)6](NO3)2 and [Ni(en)3](NO3)2 using TG–MS and TR-XRD under inert condition

Abstract

Thermal behaviour of hexaamminenickel(II) nitrate and tris(ethylenediamine)nickel(II) nitrate have been investigated by means of simultaneous thermogravimetry/DTA coupled online with mass spectral (MS) studies and temperature resolved X-ray diffraction (TR-XRD) techniques under inert atmospheric condition. Both the complexes produce highly exothermic reactions during heating due to the oxidation of the evolved ammonia or ethylenediamine by the decomposition products of Ni(NO3)2. Evolved gas analysis by MS studies detected fragments like NH2 and NH ions with weak intensity. The decomposition of nitrate group generates N, N2, NO, O2 and N2O species. Ethylenediamine (m/z 60) is fragmented to H2 (m/z 2), N (m/z 14), NH3 (m/z 17) and CH2=CH2/N2 (m/z 28) species. The formation of the intermediates was monitored by in situ TR-XRD. The residue of thermal decomposition for both the complexes was found to be crystalline NiO in the nano range.