Our research is focused on the preparation and characterization of promising multimetal oxide ceramic materials, such as superconducting cuprates and ferroelectric materials. Results of the sol-gel synthesis of two compounds are discussed: PbTiO3 (PTO) and BaTiO3 (BTO). These are important products in the study of ferroelectric materials, with interesting applications as non-volatile ferroelectric random access memories (NVFRAMs), such as PbZr1-x, TixO3 (PZT) and BTO-stabilized PbZn1/3 Nb2/3O3 (PZN). The aim of this presentation is to show how the combination of TGA-evolved gas analysis (TGA-EGA) (i.e. mass spectrometry (MS) and Fourier transform infrared spectroscopy (FTIR) on-line coupled to TGA) gives important, but not sufficient, information for a complete identification of the intermediates that are formed during thermal decomposition. By using TGA-EGA, these intermediates can only be determined indirectly by calculation from the weight losses or by the identification of the evolved gasses. Direct information about the intermediates and the final decomposition products can be obtained by in situ high-temperature-X-ray diffraction (HT-XRD) and high-temperature-diffuse reflectance FTIR (HT-DRIFT) measurements during heat treatment.