For the first time, iron oxide nanoparticles (NPs) with very high saturation magnetization (Ms = 283 emu/g) and superparamagnetic properties compared with other published data are successfully obtained via a facile electrochemical method. Iron oxide nanoparticles (NPs) are fabricated by electro-reduction of the ferric-triethanolamine complex in an alkaline medium but at certain optimized conditions. Here, the electro-deposition pathway of iron oxide NPs is traced and detected via cyclic voltammetry and X-ray powder diffraction (XRD) techniques. The scanning electron microscopy (SEM) and the high-resolution transmission electron microscopy (HR-TEM) are used for morphological characterization of the electrodeposits. These nanostructured iron oxides exhibited high efficiency towards the removal of lead ions. The capacity (Qm) of the removal of Pb2+ for these smart oxides is found to be 134.77 mg/g. Moreover, these materials give high uptake of about 96.58%.