Polycrystalline Li3VO4 was prepared by solid-state reaction method at 950 A degrees C for 5 h. The X-ray diffraction pattern of the material shows the formation of single phase orthorhombic beta II-type structure with no impurities. TGA measurements reveal 1.0 wt% loss in the temperature range between 25 and 120 A degrees C attributed to humidity desorption. Impedance spectroscopy measurements were carried out on pellets of polycrystalline Li3VO4 at temperatures from 25 to 500 A degrees C at 25 A degrees C steps. An anomalous behavior of the conductivity attributed to the presence of water in the temperature range between 25 and 120 A degrees C is observed. The activation energy values of the conduction process within the grains (bulk conductivity) and across grain boundaries were found to be 1.00 and 0.87 eV, respectively.