This article describes a more accurate, reliable, and responsive electrochemical sensor for the specific analysis of major isomers of dihydroxybenzene at binary metal oxide, nickel cobaltite (NiCo 2 O 4 ) nanosheets. In this sustainable synthesis, we report the obtention of NiCo 2 O 4 (NCO) sheets prepared through the temperature-controlled hydrothermal route which yields NCO I (stacked sheets), NCO II (multilayered sheets), and NCO III (thin sheets). Then, the structural, morphological, and chemical properties were analyzed via, microscopic, diffractive, spectral studies, while the electrocatalytic activity was examined through voltammetric analysis. The electronic structure gained via hydrothermal treatment and analytical findings reveals the appropriate band position of the produced NCO sheets to be used in electrocatalytical methods. Hence, the designed sensor was evaluated to sense the major isomers of dihydroxybenzene, which pollutes the aquatic ecosystems. Therefore, for results the hydrothermally prepared NCO sheets through the temperature-controlled hydrothermal route were employed to sense the isomers of dihydroxybenzene specifically in real-time.