ZrO 2 decorated nanocrystalline ZSM-5 nanocomposites with different weight ratios were prepared by the calcination of physical mixture of nanocrystalline ZrO 2 and Nano-ZSM-5.Material was characterized by the complementary combination of X-ray diffraction, N 2adsorption, and transmission/scanning electron microscopic techniques. An electrochemical sensor based on ZrO 2 supported nanocrystalline zeolite was developed for the nanomolar detection of organic water pollutants metol and bisphenol A with high electrocatalytic activity, stability, sensitivity, and selectivity. Under the optimum condition, a wide linear range was obtained from 4 nM-800 µM and 6 nM-600 µM with a limit of detection of 1 nM and 3 nM for metol and bisphenol A, respectively. The analytical performance of the developed sensor was demonstrated for the determination of metol and bisphenol A in different real samples such as river water, metol in photographic solution, and bisphenol A in baby bottle with satisfactory results.