A comparative analysis of the results, obtained by differential thermal analysis (DTA), high temperature X-ray diffraction (XRD), and temperature programmed electrical conductivity measurements (TPEC), in the study of the polymorphic transition (a to B form) of a mixed ferrous and cobaltous molybdate is reported. In order to p r o m in the interpretation of the curves obtained using TPEC, the results obtained with these techniques, used at different heating rates, have been compared. This comparison enables one to evidence the occurrence of the phase transition on the surface and in the bulk of the sample particles.