New combustion synthetic route for the synthesis of nanosized 𝛾-Fe₂O₃ by microwave-assisted route is reported. X-ray density, tap density and powder density of prepared 𝛾-Fe₂O₃ are calculated. Adsorption study of Pb²⁺ on combustion derived nanosized 𝛾-Fe₂O₃ is studied by dynamic method. The 𝛾-Fe₂O₃ structure and lead adsorbed 𝛾-Fe₂O₃ (Pb-𝛾-Fe₂O₃) are studied by X-ray diffraction (XRD). Additional lead peaks in Pb-𝛾-Fe₂O₃ sample pattern confirm the lead adsorption. Morphology of as prepared 𝛾-Fe₂O₃ and Pb-𝛾-Fe₂O₃ is studied by scanning electron micrograph (SEM) technique. Varied morphology for Pb-𝛾-Fe₂O₃ compared to its 𝛾-Fe₂O₃ is observed. Variation of bonding in Pb-𝛾-Fe₂O₃ sample due to lead adsorption is viewed by infrared spectroscopic (IR) technique. Energy dispersive X-ray microanalysis (EDX) is scanned for the lead adsorbed 𝛾-Fe₂O₃ to know the presence of lead on 𝛾-Fe₂O₃ surface. The eluent lead solution is characterized by atomic absorption spectroscopy (AAS) and solution conductivity (SC). Reduction in the concentration and increase in conductance of eluent lead solution is observed. The potential use of solid adsorbents for the adsorption of heavy metal pollutants is envisaged in the present work.