The electrochemical activities of hydroxylamine (HX) as a pollutant compound at a 1,1-bis(phenylacetyl)ferrocenele/NiO/CNTs modified carbon paste electrode (1,1-BPF/NiO/CNTs/CPE) has been studied. 1,1-BPF was used as a suitable mediator for elecrocatalytic interaction with HX. The voltammetric properties of HX at the 1,1-BPF/NiO/CNTs/CPE was investigated by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), chronoamperometry, and square wave voltammetry (SWV) methods. The oxidation peak current increases linearly with HX concentration in the range 0.5–250.0 μM and the detection limit for HX was 0.2 μM. The sensor was applied to wastewater samples with excellent performance.
