The single-step synthesis of nanosized MgFe2O4 via mechanochemical processing of binary oxide precursors is reported. The mechanochemical route is followed by X-ray diffraction and Fe-57 Wossbauer spectroscopy. The nanoscale nature of the mechanosynthesized material is evidenced by transmission electron microscopy. Quantitative information is provided on both ionic and spin configurations in nanosized MgFe2O4. (c) 2006 Elsevier B.V. All rights reserved.