The synthesis of high T c superconducting YBa 2Cu 3O 7−δ powders obtained by three different schemes has been i investigated. The decomposition of metal carboxylates, mixed metal oxalates, and the conventional ceramic method of mixed oxide/carbonate are contrasted. Thermal analysis (TGA, DTA) results as well as X-ray diffraction data are used to follow the progress of the decomposition and solid state reactions leading to the formation of the required perovskite. The effect of cation mixing at the molecular level in the carboxylates and oxalates is compared to the physical mixing of coarser particles in the conventional approach. In the case of the carboxylates and mixed oxalate it is suggested that Ba and Y form a double carbonate that decomposes into barium carbonate and yttrium oxide in the progress of the reaction.