This study investigated the solution combustion synthesis technique to obtain the nanostructured magnesioferrite (MgFe2O4) spinel powder. The reaction was performed in an electric muffle furnace. Considering the characteristics of the as-synthesized powders, the 30% fuel-deficient formulation was selected for synthesis temperature evaluation. This formulation was synthesized at different furnace temperatures. Powder characterization was carried out by X-ray diffraction (XRD) to evaluate crystallographic analysis and crystallite size; Transmission Electron Microscopy (TEM) was done to assess the morphology and crystallite size; and Mossbauer spectroscopy and vibrational sample magnetometer (VSM) were performed to obtain magnetic measurements. Crystallite sizes estimated from the XRD technique increased with furnace temperature values, which were consistent with the results obtained by TEM. The characterized samples of MgFe2O4 had an average crystallite size of 42.8 nm using the DRX method, average saturation magnetization of 25.6 emu/g and coercive field not higher than 11 Oe. (C) 2011 Elsevier B.V. All rights reserved.