Xanthoceras Sorbifolia Bunge hull activated carbon (XSA) was prepared and characterized by Brunauer-Emmett-Teller analysis, scanning electron microscopy and energy dispersive X-ray (EDX) spectroscopy. The ability of XSA as an adsorbent was investigated for the removal of the iron group ions Fe(III), Co(II), and Ni(II) from aqueous solution. Optimum adsorption parameters were determined based on the initial concentrations of the iron group ions, pH, adsorption temperature, and adsorption time in adsorption studies. The maximum monolayer adsorption capacities were 241.13 mg/g for Fe(III), 126.05 mg/g for Co(II), and 187.96 mg/g for Ni(II), respectively. Adsorption kinetics and isotherms showed that the adsorption process best fitted the nonlinear pseudo-second-order and Langmuir models, and the affinity of the ions for XSA decreased as follows: Fe(III) > Ni(II) > Co(II). Regeneration studies indicated that XSA could be used after several consecutive adsorption/desorption cycles using HNO3. Fourier transform infrared and EDX spectra revealed the chemical adsorption value of XSA as an adsorbent for removing iron group ions from aqueous solutions.