Heavy metals determination is of great importance. In this respect, a recently synthesized melamine-based covalent organic framework (Schiff base network1 (SNW1)) was used in this research as a novel modifier to alter a glassy carbon electrode for the simultaneous anodic stripping square wave voltammetric measurement of Pb2+ and Hg2+ ions. At first, the complexation of SNW1 with Pb2+ and Hg2+ ions were evaluated by density functional theory calculations. Afterward, the modified electrode was characterized by various techniques including Fourier-transform infrared spectroscopy, Scanning electron microscopy, energy dispersive X-ray analysis, cyclic voltammetry, and electrochemical impedance spectroscopy. Then, all of the effective experimental factors including pH, supporting electrolyte type, and instrumental parameters were optimized. Under optimized conditions (pH = 2.0, deposition time = 150 S, accumulation potential = -1000 (mV), pulse amplitude = 40 mV, frequency = 50 Hz, and voltage step = 7 mV) the designed sensor showed a linear response over the concentration ranges of 0.01–0.3 and 0.05–0.3 µmol/L for Pb2+ and Hg2+ respectively with a detection limit of 0.00072 and 0.01211 µmol/L. In the end, the designed electrochemical sensor was successfully employed for simultaneous measurement of Pb2+ and Hg2+ at different edible samples.
