In the present study, we demonstrate the synergistic effect of copper nanoparticles, tungsten disulfide, and diamond nanoparticles on the electrochemical detection of cyanuric acid, a compound conventionally employed for disinfection in aquatic recreational facilities such as swimming pools. First, copper nanoparticles were synthesized in-situ on a glassy carbon electrode through the electrochemical reduction of copper nitrate and their response towards cyanuric acid was assessed. In order to improve this response, we evaluated the inclusion of transition metal dichalcogenides nanosheets (MoS2, ReS2 or WS2), as well as diamond nanoparticles in the electrochemical sensor construction. These nanomaterials were incorporated onto the electrode via drop-casting from their respective suspensions. Specifically, the 2D transition metal dichalcogenide suspensions were obtained through a top-down exfoliation method, facilitated by ultrasonic assistance. After optimizing the arrangement of nanomaterials on the glassy carbon electrode to enhance cyanuric acid detection, we characterized the morphology of the resulting surfaces at each stage of electrode surface modification by atomic force microscopy and scanning electron microscopy. The optimized methodology revealed that the sensor response exhibited a linear relationship with cyanuric acid concentrations ranging from 0.077 to 0.70 mM with a detection limit of 23 µM. The sensor was applied to cyanuric acid determination in a swimming pool water sample, obtaining very good recoveries. The results are in good agreement with those obtained by HPLC-UV–vis measurements.
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