New heterometallic complex [NiCu(NO3)2(H2O)2] (1) was prepared via the reaction of aqueoussolutions of (oxalic acid, nickel nitrate and copper nitrate). Mixed oxide CuO-NiO was suc-cessfully obtained with different morphological structures (2) and (3) through the annealingof 1 at different temperature 300◦C and 600◦C, respectively. The materials were charac-terized using FT-IR, TGA, XRD and SEM. As showed from XRD data, with increasing thecalcination temperature the crystallinity of CuO-NiO in sample 3 was improved and thediffraction peaks exhibited narrower and stronger than CuO-NiO in sample 2. The averagesize of CuO-NiO crystals obtained was calculated from Debye-Scherrer equation and foundto be 16.65 nm. To assemble the working electrode of 2-aminophenol (2-AP) chemical sensor,a thin layer of CuO-NiO NPs was deposited on glassy carbon electrode (GCE) with conduct-ing binder and used to detect 2-AP in aqueous medium successfully. The chemical sensor isexhibited the higher stability, good sensitivity (20.2729 AmM−1cm−2) and enhanced elec-trochemical activity at room conditions. Therefore, the fabricated chemical sensor withactive CuO-NiO NPs may be an effective and sensitive sensor for detection of hazardousmaterials by reliable I–V method for broad scales environmental safety of and healthcaresectors.