Two MgO samples were prepared from home-made magnesium galactarate hemihydrate (MgCHO·0.5HO) and magnesium oxalate dihydrate (MgCO·2HO) by calcination at 500 °C for 3 h in air. Thermal decompositions of both Mg salts were studied by TG and DSC analyses. Selected samples were chosen during thermal decomposition of galactarate salt to examine its decomposition steps by FTIR, as well as the original salt. The resulted oxides at 500 °C from both precursors were characterized by FTIR and XRD analyses as pure periclase MgO nanoparticles, between 11.5 and 12.6 nm. SEM micrographs of oxides showed substantial differences between the particles' shapes. It was stick-like particles in case of MgO-Gala and aggregates of small cubic crystals in case of MgO-Oxal. Results of surface area and porosity measurements showed, also, great differences in their surface characterizations. The decomposition of isopropyl alcohol, as a test reaction, was applied to compare the catalytic activity of such samples with the distribution of both acidic and basic sites over their surfaces.