Nanopowder of La_0.75Sr_0.25Cr_0.5Mn_0.5O_3−δ (LSCM) perovskite, a potential anode material for solid oxide fuel cell (SOFC), is synthesized by a solution combustion method using metal nitrates and tartaric acid. The crystalline phases in the as-synthesized powder after calcination at various temperatures were monitored by X-ray diffraction (XRD). The results showed that increasing the molar ratio of tartaric acid to metal cations above 6 and pH 7 of the precursor solution contributed to the formation of impurity phases along with the LSCM perovskite phase. Transmission electron microscopy (TEM) analysis on the as-synthesized powders showed particle sizes in the range of 95–220nm depending on the processing conditions. A single phase LSCM perovskite obtained after calcination of dried gel at 1050°C for ≥3h was found to have crystal structure with rhombohedral symmetry with space group R-3c (167).