A new method of preparation of nanocrystalline zinc aluminate (ZnAl2O4) powder is described in this paper. Different organic acids are used as template material and nitric acid as an oxidant. Single phase ZnAl2O4 spinel can be formed at a much lower temperature through this route which gives nanocrystalline powder with uniform particle size and morphology. The powders are characterized by thermo gravimetric analysis (TGA), X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FT-IR), BET surface area analysis and field emission scanning electron microscopy (FE-SEM). The average crystallite size of the single phase material was of 20 to 30 nm and the surface area was found to be 21 to 27 m2g−1.