The work presented in this paper describes the preparation and the electrochemical application of functionalized chitosan-entrapped carbon paste electrodes (CH/CPE) for lead ions (Pb2+) detection in industrial wastewater. The chitosan was first functionalized using TiO2 and CuO, which were both metal oxides that were obtained by extracting it from waste products derived from shrimp shells. The analytical performance of the as-prepared electrodes, CH/CPE, TiO2-CH/CPE, and NiO-CH/CPE, for the detection of lead (II) was examined using electrochemical impedance spectroscopy (EIS) technique in the 0.1 M KNO3 electrolyte solution. The effect of experimental conditions, including polarization potential, frequency, and pH, are optimized to maximize the sensitivity of the measurements. The developed impedimetric sensors provided a linear response over a concentration range of 10−6 to 10−4 M with a detection limit of 3.10−7 M based on S/N = 3. The DFT computational analysis demonstrated that chitosan biopolymer possesses the ability to adsorb Pb (II) ions that are present in wastewater. Chitosan and the derivatives of chitosan, have the potential to remove heavy metals from industrial effluent in a manner that is both economical and eco-friendly to the environment. Chitosan is a biopolymer that is abundantly renewable.