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A simple hydrothermal synthesis approach was used to synthesize porous MgNiO₂ Chrysanthemum Flowers (CFs) nanostructures and applied as a sensing electrode for quick detection of hazardous mercury (Hg²⁺ ions). The morphological, structural, and electrochemical properties of MgNiO₂ CFs were investigated. The morphological characteristic of MgNiO₂ CFs, with a specific surface area of 45.618 m²/g, demonstrated strong electrochemical characteristics, including cations in different oxidation states of Ni³⁺/Ni²⁺. Using a three-electrode system for electrochemical detection, the MgNiO₂ CFs based electrode revealed a good correlation coefficient (R²) of ~0.9721, a limit of detection (LOD) of ~11.7 μM, a quick response time (10 s), and a sensitivity of 8.22 μA∙μM⁻¹∙cm⁻² for Hg²⁺ ions over a broad linear range of 10–100 μM. Moreover, the selectivity for Hg²⁺ ions in tap water and drinking water was determined, and a promising stability of 25 days by MgNiO² CFs electrode was exhibited. The obtained results indicate that the developed MgNiO₂ CFs are a promising electrode for detecting hazardous Hg²⁺ ions in water and have the potential to be commercialized in the future.