| Summary: | Nowadays, heavy metal ion pollution in water is becoming more and more common, especially arsenic, which seriously threatens human health. In this work, we used Fe<sub>3</sub>O<sub>4</sub>–rGO nanocomposites to modify a glassy carbon electrode and selected square wave voltametric electrochemical detection methods to detect trace amounts of arsenic in water. Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) showed that Fe<sub>3</sub>O<sub>4</sub> nanoparticles were uniformly distributed on the rGO sheet, with a particle size of about 20 nm. Raman spectroscopy and electrochemical impedance spectroscopy (EIS) showed that rGO provides higher sensitivity and conductive substrates. Under optimized experimental conditions, Fe<sub>3</sub>O<sub>4</sub>–rGO-modified glassy carbon electrodes showed a higher sensitivity (2.15 µA/ppb) and lower limit of detection (1.19 ppb) for arsenic. They also showed good selectivity, stability, and repeatability.
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