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In this scientific work, a precipitation method is followed for the synthesis of copper oxide (CuO), cobalt oxide (Co3O4) and copper cobaltite (CuCo2O4) and the viability of using these materials as electrode modifiers has been studied. A sensitive electrochemical sensor for the determination of hydroxylamine has been introduced. The morphology and physical properties of the as synthesized materials were characterized with several characterization tools. It is found that the morphology and size of CuO, Co3O4 and CuCo2O4 are nanoflakes (300–350 nm), nanoplatelet (75–100 nm) and nanobricks (20–45 nm), respectively. In addition, CuO, Co3O4 and CuCo2O4 oxidize hydroxylamine at 0.57 V, 0.53 V and 0.44 V, respectively. Electrocatalytic oxidation current of hydroxylamine was proportional to the concentration of hydroxylamine in the range 0.075 to 8.25 mM. Also, under optimized condition, limit of detection and sensitivity in the DPV measurement are 0.65 μM ± 0.05 μM and 13.1 μA cm−2 mM−1, respectively. Hence, the proposed sensor is highly sensitive, selective, simple, precise and stable for hydroxylamine detection in the real water samples. [ABSTRACT FROM AUTHOR]