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The synthesis of barium metastannate, BaSnO3, by heating mixtures of metal oxalates, either physically mixed or subjected to a phase of mechanical activation, up to temperatures in the range 750- 1200 °C has been studied. Simultaneous thermogravimetric-differential scanning calorimetric (TGDSC) analyses and powder X-ray diffractometry have been applied to check the advancement of the reactions. BaSnO3, though slightly contaminated by BaCO3, can be obtained by heating the activated mixture up to T ≥ 1000 °C while heating a sample of a physical mixture at temperature as high as 1200 °C resulted in a mixture of BaSnO3, SnO2 and Ba2SnO4. The heat capacities of BaSnO3 samples prepared at temperatures between 1000 and 1200 °C have been measured by modulated temperature differential scanning calorimetry (MTDSC) in the temperature range 50-400 °C.