α-MnO2nanostructure was successfully synthesized via hydrothermal treatment of a precursorγ-MnO2. Structure, morphology, and BET surface area were characterized using X-ray powder diffraction (XRD), Scanning Electron Microscopy (SEM), and Brunauer-Emmett-Teller nitrogen adsorption (BET-N2adsorption). Thermal analysis result showed thatα-MnO2nanorods were formed fromγ-MnO2at 600°C. In addition, Pb(II) and Fe(III) adsorptive properties were investigated in an optimal condition. Results showed that equilibrium adsorption was obtained after 60 minutes for Pb(II) at pH = 4.0 and 80 minutes for Fe(III) at pH = 3.5 with 240 rpm of shaking speed overall. Experimental data was analyzed using three models: Langmuir, Freundlich, and Sips. Adsorption capacities (qm) from the Langmuir isotherm models are 124.87 mg/g for Pb(II) and 30.83 mg/g for Fe(III). Along with the highest corelation coefficients, it is clear that the adsorption of Pb(II) and Fe(III) ions onα-MnO2surface followed Sips model. Kinetic studies indicated that the uptake of Pb(II) and Fe(III) occurred in the pseudo-second-order model with two stages for Pb(II) and three stages for Fe(III).