Superconducting Bi–Pb–Sr–Ca–Cu–O (BPSCCO) thin films were grown on MgO substrates by a spray pyrolysis technique, followed by a solid-state reaction. The thin films with nominal composition Bi1.65Pb0.4Sr1.2Ca1.2Cu2.5(NO3)δ were grown varying mainly the annealing temperature between 835 and 855 °C in order to observe the influence on the critical temperature Tc. At 855 °C the higher Tc was obtained for the 2212 phase. The thin films were then analyzed by X-ray diffraction, R-T measurements and atomic absorption spectroscopy.