Toxic heavy metal ions, such as lead ions, significantly threaten human health and the environment. This work introduces a novel method for the simple and sensitive detection of lead ions based on biochar-loaded titanium dioxide nanoparticles (BC@TiO2NPs) nanocomposites. Eco-friendly biochar samples were prepared from spent coffee grounds (500 °C, 1 h) that were chemically activated with TiO2 nanoparticles (150 °C, 24 h) to improve their conductivity. Structural characterizations showed that BC@TiO2NPs have a porous structure. The BC@TiO2NPs material was evaluated for lead ion determination by assembling glassy carbon electrodes. Under optimal conditions, the sensor was immersed in a solution containing the analyte (0.1 M NaAc-HAc buffer, pH = 4.5) for the detection of lead ions via differential pulse voltammetry. A linear dynamic range from 1 pM to 10 μMwas achieved, with a detection limit of 0.6268 pM. Additionally, the analyte was determined in tap water samples, and a satisfactory recovery rate was achieved.
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