The comparative study of the thermal analysis (thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and derivative thermogravimetry (DTG)) and de electrical conductivity measurements of copper(II) and zinc(II) malonate, maleate and succinate complexes have been carried out using the atmospheres of static air and dynamic dry nitrogen. The isothermally heated products at each decomposition stage have been characterized by C and H analyses, infrared spectra and X-ray powder diffraction data. The electrical conductivity measurements were found to give additional information on the solid-state reaction as compared to that obtained from conventional thermal techniques (such as TGA, DTG and DSC).