Reaction between PbO and TiO2 mixed in the stoichiometric ratio for the preparation of PbTiO3 has been followed using DTA and XRD techniques. Studies reveal that the reaction is initiated at approximately 800 K. Samples heat-treated at 875 K showed the characteristic X-ray pattern for crystalline PbTiO3 and, on the basis of dielectric constant measurements, a Curie transition temperature of 765 K. SEM micrographs also showed a single phase sample with well defined grains, The samples were also characterized by ac resistivity measurements. The DTA curve showed an exothermic heat effect in the temperature range 835-1020 K corresponding to the formation of lead titanate. The Curie transition in the compound so formed could be observed as another exothermic peak at 783 K in the cooling cycle. Simultaneous TG measurements confirmed that both heat effects were unattended by changes in sample weight.