FeMn mixed oxides were prepared by the citrate method with Fe:Mn atomic ratio equal to 1:1, 1:3 and 3:1. The sample was characterized by means of specific surface area measurements, X-ray diffractometry (XRD), temperature programmed desorption of oxygen (O-2-DTP), temperature programmed reduction (TPR), X-ray fluorescence (XRF), transmission electron microscopy (TEM and SAED) and high resolution TEM (HREM). The characterization results demonstrated the formation of a Mn2O3-Fe2O3 solid solution. The catalytic performance in ethanol, ethyl acetate and toluene total oxidation on these samples was better than on Fe2O3 and Mn2O3 pure oxides. (C) 2009 Elsevier B.V. All rights reserved.