Nanotechnology is offering solutions to water contamination issues, as new techniques are needed to improve the removal of harmful compounds from water bodies. Despite previous reviews on this topic, nanotechnology is paving the way for more effective water treatment methods. Understanding the substitute influence of divalent Co2+ and rare earth elements Sm3+ on the structure, magnetic, and removal efficiency of hexagonal ferrites requires an understanding of a sequence of SrFe12O19, SrFe11.5Co0.5O19, Sr0.95Sm0.05Fe12O19, and Sr0.95Sm0.05Fe11.5Co0.5O19 M-type hexagonal ferrites were prepared using the flash technique. The XRD examination revealed that the crystallized material formed a single M-type hexagonal phase. The characteristics of M-type hexagonal ferrites include absorption bands with low wavenumbers in the FTIR curves between 400 to 1000 cm−1. There was a variation in magnetic characteristics with the replacement of Sm3+ and Co2+ doping, possibly due to the spin canting impact created by rare earth Sm3+ and Co2+ ions. The goal of the research is to explore the potential of doping magnetic hexaferrites and its influence in wastewater treatment. Various parameters, such as pH and contact duration, that influence the adsorption of lead ions from aqueous solutions were also examined. At pH 7 and 25 °C after 70min, the maximal removal efficiency of the Sr0.95Sm0.05Fe11.5Co0.5O19 was found to be 99%. Magnetic separation was carried out by applying an external magnetic field using a permanent magnet. The strong magnetization of the ferrites (51–58 emu/g) enabled the rapid separation of the magnetic particles from the solution, with over 95% of the ferrite particles being recovered within 10 to 70 min. The Freundlich isotherm model fitted all the isotherm data. Adsorption kinetics were explained by the pseudo-first-order, pseudo-second order, and intraparticle diffusion models. The investigated samples’ adsorption capacity remained efficient till 5 cycles.