This paper presents an approach to the preparation of LaCoO3 perovskite and nickel doped LaCoO3 in A and B site both, to see the effect of nickel doping in both the site catalyst synthesized by co-precipitation method. The novelty of the experiment is nickel doped in A-site of LaCoO3 Perovskite to see effect of nickel doping into their physical properties (i.e. crystalline phase and microstructure). Samples have been characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), Branauer-Emmett-Teller (BET) nitrogen adsorption technique.