A major disadvantage of precipitation removal of heavy metals is the disposal of sludge having a high concentration of heavy metals, sometimes requiring disposal in hazardous waste landfills. A sorption based polishing step using natural sorbents; following precipitation may be feasible to avoid costly disposal of hazardous sludge. This study investigates the applicability of the use of a natural zeolite, namely clinoptilolite, obtained from a Western Anatolian deposit, in removing copper and nickel from aqueous solutions. Maximum achievable capacities were found as 0.31 meq Cu2+/g and 0.32 meq Ni2+/g for as-received, and 0.55 meq Cu2+/g and 0.43 meq Ni2+/g for conditioned clinoptilolite samples, respectively. Use of clinoptilolite for the removal of Cu2+ from precipitation effluents holds more potential for the purpose of meeting discharge standards. Metal removal mechanisms are also investigated via examination of exchangeable cations (Na+, K+, Mg2+, Ca2+) in the aqueous phase.