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tIn this work, a new catalyst based on carbon paste (CP) modified by spinel NiCo2O4nanoparticles and zeolite-4A was proposed and used for the electrochemical oxidation ofmethanol. NiCo2O4@zeolite-4A was obtained through the calcination of the physical mix-ture of NiCo2O4and zeolite-4A. Their physicochemical properties were characterized byX-ray diffraction (XRD), scanning electron microscopy-energy dispersive X-ray spectra (SEM-EDS), and FT-IR techniques. The electrocatalytic performance of modified electrode basedon NiCo2O4@zeolite-4A was tested using cyclic voltammetry (CV) and chronoamperomerty(CA). The result of cyclic voltammetry indicated a significant rise in the oxidation currenton the surface of NiCo2O4@zeolite-4A/CPE modified electrode. The rate constant for the cat-alytic reaction (k) of methanol was calculated by means of a chronoamperometric technique.To sum up, the incorporation of NiCo2O4nanoparticles into zeolite-4A provided the binaryelectroactive sites for catalysis of methanol oxidation as it exhibited a long-term stabilityfor catalytic reaction, and thus a promising application.