The cobalt co-ordination complexes, [Co(en)(2)Cl-2]Cl and [Co(en)(2)CO3]Cl, synthesised through literature procedures, were characterised by FTIR. Trace metallic impurities were determined by ICP-MS. Crystallinity of the samples were ascertained by preliminary X-ray powder diffraction analysis. Dark field polarised optical microscopy (OM) was used to observe particle size distribution. These compounds were subjected to temperature programmed decomposition (TPD) in thermogravimetric analyser (TGA). TPD was also carried out in a home built mass spectrometry based evolved gas analyser (EGA-MS). The complex TGA weight loss profile could be successfully explained through EGA data. Complimentary information received from both the above techniques indicated sequential decomposition, prevalence of steric effect and functional group ejection. The non-isothermal kinetic analysis of TGA and EGA data showed dominance of kinetic control mechanisms based on sigmoidal rate laws like Avarami-Erofeev (AE) and random nucleation (RN). The fraction release alpha similar to T plots were used to evaluate integral model function g(alpha) of non-isothermal kinetic rate expressions. From log[g(alpha)/T-2] similar to 1/T plots of well correlated model functions, Arrhenius parameters like activation energy and pre-exponential factors were evaluated for various decomposition steps.