This work reports the use of highly efficient nanocomposite material fabricated glassy carbon electrode (Ag(NPs)/ChS/GC) in the trace detection of Pb²⁺ 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 Pb²⁺ showed good linearity in anodic peak current and Pb²⁺ 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 Pb²⁺. 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 Pb²⁺ in two different real water samples.

Fabrication of a working electrode with silane grafted chitosan (CHTMS) employed in the sensitive detection of Pb(II) in aqueous media is presented. Several advanced analytical methods have extensively characterized the nanocomposite material. The prepared material was subsequently employed for modification of a glassy carbon electrode (GCE) and characterized using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS), which show a 3-fold enhancement in surface area compared with the bare GCE, and a charge transfer resistance of 678.7 Ω. The modified electrode was employed in the sensitive determination of Pb(II) in aqueous media using differential pulse anodic stripping voltammetry (DPASV), where optimization of experimental parameters such as pH, deposition time, and deposition potential was carried out. Under optimized conditions, the linear regression and correlation coefficient were obtained, which show that Pb(II) can be detected over a wide concentration range with a calculated limit of detection (LOD) of 3.47 µg/L, which is lower than the permissible limit set by the WHO. For practical applicability, reproducibility and stability tests, as well as real water sample analyses were further performed, with the obtained recovery rates showing promising results.