Waste citrus peel-based activated carbon (WCAC) was prepared from waste citrus peels by activation with KOH. The removal of Cu and Pb ions from aqueous solution by the prepared WCAC was investigated in batch experiments. The solution pH significantly influenced Cu and Pb adsorption capacity and the optimum pH was 4 to 6. The adsorption of Cu and Pb ions by WCAC followed pseudo-second-order kinetics and the Langmuir isotherm model. The maximum adsorption capacity calculated by Langmuir isotherm model was 31.91 mg/g for Cu and 92.22 mg/g for Pb. As the temperature was increased from 303 K to 323 K, the ΔG˚ value decreased from –7.01 to –8.57 kJ/mol for Cu ions and from –0.87 to –2.06 kJ/mol for Pb ions. These results indicated that the adsorption of Cu and Pb by WCAC is a spontaneous process.