Environmental safety is of paramount importance for human well‐being, imposing significant demands for affordable, rapid, portable, and robust analytical tools for real‐time and on‐site water monitoring. In this context, we have developed an analytical method to efficiently detect heavy metal ions, particularly Pb2+ ions, in water samples. This method employs a stepwise‐prepared electrode comprised of a thin film of poly(methyl orange) (pMO) electrochemically deposited onto reduced graphene oxide (erGO), which is in turn coated on a glassy carbon electrode (GCE). The resulting pMO/erGO/GCE electrode was characterized using Raman spectroscopy, scanning electron microscopy (SEM), and electrochemical techniques. Square wave anodic stripping voltammetry (SWASV) was subsequently employed to detect the target ions. Importantly, the pMO/erGO/GCE electrode exhibits excellent analytical performance, featuring a broad linear concentration range spanning from 14 to 595 parts per billion (ppb), a sensitivity of 5.60 μA ppb−1 cm−2, and a theoretical calculated value of the detection limit of 0.82 ppb. The effectiveness of this sensor was validated through successful testing of aqueous samples from dissolved ores containing both lead(II) and cadmium(II) cations, as determined by atomic absorption spectroscopy.