Nickel molybdate (NiMoO4) nanopowders were prepared by a new method in low temperature. For the first time, we used carboxymethyl cellulose as a new capping agent in synthesis procedure. The formed nickel molybdate products have been characterized by means of UV-vis diffuse reflectance spectroscopy, X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and energy dispersive X-ray microanalysis (EDX). Glassy carbon electrode modified with NiMoO4 nanopowders was prepared and used for oxidation of ethanol and methanol. The study of the different scan rates indicates a diffusional process for oxidation of ethanol. The detection limit obtained for ethanol was also 3.8 mM.