In this work we present the utilization of the heterometallic alkoxide [FeCl{Ti-2(OPri)(9)}] as the first sol-gel single-source precursor to achieve nanocomposites made of iron and titanium oxides incorporated into Porous Vycor Glass (PVG). The nanocomposites were prepared by the impregnation of the precursor in a PVG plate followed by hydrolysis reactions. Different samples were obtained by further thermal treatment of the hydrolyzed sample. The nanocomposites were characterized by UV-vis-NIR, Raman and EPR spectroscopies, XRD and TEM. The results indicate that the room-temperature hydrolyzed samples are formed by nanoparticles of FeOOH and brookite-TiO2 embedded on a glassy matrix. After the heat treatment at temperatures above 900 degrees C, a pseudobrookite Fe2TiO5 was formed. All samples present high transparency and homogeneity. The results showed here indicate that the sol-gel process using the single-source precursor [FeCl{Ti-2(OPri)(9)}] should be a novel and efficient approach to the preparation of nanometric Fe/Ti oxides incorporated into a glassy matrix. (c) 2006 Elsevier Inc. All rights reserved.