The thermal decomposition of FeC 2 O 4 Á2H 2 O prepared by solid-state method was investigated in air using TG-DTG/DSC. The precursor and its decomposition products formed at various temperatures were characterized by FT-IR and XRD. As evidenced by the results, the thermal decomposition proceeds in two steps with DSC peaks closely corresponding to the mass loss. The decomposition of FeC 2 O 4 Á2H 2 O and the kinetic analysis of the second step were performed under non-isothermal conditions, and the activation energies were estimated by the Ozawa integral method and the Coats-Redfern integral method. In order to make the kinetic calculation much more accurate, the temperature was risen by variable acceleration in the different stages of the decomposition to help distinguish the two steps from each other, and this is an innovation point that is deserved to be mentioned in this study. After calculation and comparison, the decomposition conforms to the nucleation and growth model and the physical interpretation is summarized. The activation energy and kinetic mechanism function were determined to be 113.90 kJ mol -1 and G(a) = [-ln(1 -a)] 2/3 , respectively.