This work reports the use of highly efficient nanocomposite material fabricated glassy carbon electrode (Ag(NPs)/ChS/GC) in the trace detection of Pb<sup>2+</sup> using differential pulse voltammetry (DPV). A facile method yielded the silane-grafted chitosan (ChS) using 3-trimethoxyoctylsilane, and the bioderived Ag(NPs) was <i>in situ</i> decorated on the ChS composite to obtain Ag(NPs)/ChS. X-ray Diffraction (XRD) results showed the presence of Ag(NPs) within the composite material. Spherical-shaped and uniform distribution of Ag(NPs) were observed in SEM and TEM images of the nanocomposite solid. The cyclic voltammetric studies revealed a significant increase in redox peak currents (i.e., 0.1283 mA), which was obtained using the Ag(NP)/ChS/GC compared to the bare glassy carbon electrode. Further, the electrochemical determination of Pb<sup>2+</sup> showed good linearity in anodic peak current and Pb<sup>2+</sup> concentrations (5.0-80.0 <i>μ</i>g/L), and the limit of detection was 1.97 <i>μ</i>g/L. With 10-fold increase in several cationic and anionic interfering ions, oxalic acid and glycine only show interference in determination of Pb<sup>2+</sup>. The reproducibility study showed a %RSD of 2.43%, and the electrode could be efficiently used for prolonged and repetitive detection having reasonably low %RSD of 2.55%. The real water analysis showed almost 100% recovery of Pb<sup>2+</sup> in two different real water samples.
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