New oxides of general formula Ln(2/3-x)TiO(3-3x/2) (Ln = La, Pr and Nd; 0.07 <= x <= 0.13) have been prepared by a new synthetic route, starting with precursors Ln(2/3-x)Li(3x)TiO(3) with perovskite structure. Precursors were prepared by the ceramic method and a modified Pechini sol-gel process, and both were treated with nitric acid 2 M to exchange lithium ions by protons, leading to new phases Ln(2/3-x)TiO(3-3x) (OH)(3x). These phases were calcined in order to dehydrate them and obtain the anion defect oxides Ln(2/3-x)TiO(3-3x/2). All the phases showed perovskite-type X-ray powder diffraction patterns during the successive steps of the synthesis. Anionic vacancy content was calculated by an indirect method, taking into consideration the metallic relation, determined by induced coupled plasma (ICP), and the absence of Ti(III), checked by electron paramagnetic resonance (EPR). AC electric measurements carried out under different atmospheres (N-2, Ar, H-2/Ar, air and O-2) showed a conductivity increase under reducing atmosphere, due to the reduction of Ti(IV) to Ti(III). Considering their electrical behavior, these new phases become candidates for solid oxide fuel cell (SOFC) anode materials. (c) 2005 Elsevier B.V. All rights reserved.