Nanocrystalline CuCo2O4 was synthesized in the presence of ammonium fluoride and urea. Material was characterized by the complementary combination of X-ray diffraction, N-2-adsorption, ultraviolet-visible diffuse reflectance spectroscopy, field enhanced scanning electron microscopic and transmission electron microscopic techniques. Electrochemical sensor based on CuCo2O4 was developed for the detection of organic water pollutants hydrazine and metol. For the comparative purpose, CuO and Co3O4 were synthesized and electrochemical sensors based on these materials were evaluated under the identical condition. CuCo2O4 exhibited excellent electro catalytic activity, stability, sensitivity, and selectivity in the detection of these organic pollutants. Under the optimum condition, a wide linear range was obtained from 32 nM-5000 mu M and 20 nM-1000 mu M with a limit of detection of 8 nM and 6 nM for hydrazine and metol, respectively at economical CuCo2O4 modified electrode. The analytical performance of the developed sensor was demonstrated in the determination of hydrazine and metol in different real samples such as river water, tap water and metol in photographic solution with satisfactory results. (C) 2016 Elsevier B.V. All rights reserved.