Mixed Mg-V oxides have been prepared following three different methods (calcination of precursors constituted by a layered double hydroxide, impregnation of MgO with vanadate, or mechanical MgO-V2O5 mixtures), and have been characterized following powder X-ray diffraction, X-ray absorption spectroscopy, vis-UV and FT-IR spectroscopies, thermal analysis, temperature-programmed reduction, and specific surface area assessment. Mg3V2O8 is mainly formed, although small amounts Of alpha-Mg2V2O7 are detected in some cases, in addition to MgO. (C) 2004 Elsevier B.V. All rights reserved.