Cobalt chromite (CoCr 2 O 4 ) was synthesized through the precursor method. The precursors: (NH 4 ) 3 [CoCr 2 (C 4 O 6 H 4 ) 4 (OH) 3 ]·4H 2 O, (NH 4 ) 3 [CoCr 2 (C 6 O 7 H 10 ) 4 (C 6 O 7 H 9 )]·5H 2 O were characterized by elemental chemical analysis, infrared (IR) and ultraviolet–visible (UV–vis) spectroscopy, and thermal analysis. The final oxides were characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM/TEM), UV–vis, IR, Raman spectroscopy (RS), magnetic measurements, N 2 adsorption–desorption analyses and X-ray photoelectron spectroscopy (XPS). XRD confirmed the cubic CoCr 2 O 4 phase only and determined average crystallite sizes between 14 and 21nm. Electron microscopy revealed morphology corresponding to the complete crystallization into cubic CoCr 2 O 4 . All the samples presented ferrimagnetic ordering below the Currie temperature (T c ), and a phase transition at T s ∼26K attributed to the onset of long-range spiral magnetic order. The CoCr 2 O 4 nanoparticles generated through the gluconate route following calcination at 700°C for 1h were found to have the best catalytic activity in the total oxidation of methane.