NH2-Fe2O3 and NH2-Fe2O3/chitosan (NH2-Fe2O3/CS) with excellent physical properties and high adsorption capacities for several heavy metal ions were synthesized using a one-pot hydrothermal method. The materials were characterized by scanning electron microscopy (SEM), electron dispersive spectroscopy (EDS), transmission electron microscopy (TEM), and X-ray diffraction (XRD). Physicochemical properties were determined by the Fourier transform infrared spectra (FTIR) and nitrogen adsorption analysis (Brunauer–Emmett–Teller (BET) method). The results of the characterization studies show that the material is uniformly dispersed and has good crystallinity and well-defined porous particles. The material is mesoporous, and the particles have a specific surface area of 55.41–233.03 m2·g−1, a total pore volume of 0.24–0.54 cm3·g−1, and a diameter of 3.83–17.56 nm. Additional results demonstrate that NH2-Fe2O3 and NH2-Fe2O3/CS are effective adsorbents for the removal of heavy metal ions from solution. In a ternary system, the order of their selective adsorption was determined to be Pb(II) > Cu(II) > Cd(II), and the adsorption rate of Pb(II) was much higher than that of Cu(II) and Cd (II). The metal ion adsorption capacity of NH2-Fe2O3 and NH2-Fe2O3/CS makes them promising adsorbents for wastewater cleanup.