It is generally known that the solid char obtained from pyrolysis of scrap rubber tires can be used as an adsorbent for several applications such as wastewater treatment. In this study, scrap tires were first pyrolyzed under nitrogen (N2) or carbon dioxide (CO2) gas under various temperatures to produce char. The char was activated in situ by post-pyrolysis oxygenation (PPO) at different temperature ranges as soon as the pyrolysis process was completed. Elemental and spectroscopic analyses showed significant zinc content in the char after PPO. Batch-mode removal of aqueous copper (Cu) using the chars revealed that, for N2 and CO2, the optimum condition for pyrolysis was at 550 °C and for activation was from 550 to 250 °C. Although CO2-pyrolyzed char had lower Cu and lead (Pb) removal than N2-pyrolyzed char, it had higher char yields. For both N2- and CO2-pyrolyzed char, activation with PPO improved their heavy metal removal efficiencies significantly compared with unactivated char. PPO chars had much faster removal rates and higher Cu removal compared with both pyrolyzed, unactivated char and commercial activated carbons.