The conditions of technique to prepare Co3O4 by calcination from cobalt oxalate were optimized using response surface methodology. A quadratic equation model for decomposition rate was built and effects of main factors and their corresponding relationships were obtained. The statistical analysis of the results showed that in the range studied the decomposition rate of cobalt oxalate was significantly affected by the calcination temperature and calcination time. The optimized calcination conditions were as follows: the calcination temperature 680.86K, the calcination time 44.7 min, and the mass of material 3.04g, respectively. Under these conditions the decomposition rate of cobalt oxalate was 99.06%. The validity of the model was confirmed experimentally and the results were satisfactory. (C) 2010 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.