Polymer nanocomposite thin films consisting of polystyrene and furnace carbon black were prepared in this study as adsorbent materials for the removal of heavy metals from industrial wastewater. The film properties were characterized, and the effect of carbon content in the nanocomposite, initial concentration, separation time, and pH on the removal efficiency were investigated. The optimal operating conditions were 120 min of separation time at pH 6 with a carbon content of 15 wt%. The adsorption equilibrium data and adsorption kinetics are also described herein. The Freundlich model best fit the equilibrium data, and the adsorption rate followed pseudo second-order kinetics.