This paper investigates the treatment of zinc-cyanide electroplating rinse water using an electrocoagulation process (ECP). The effects of operating parameters such as electrode material, current density (2.5–40 A/m2), operating time (0–60 min), initial pH (5–12) and electrode connection mode (monopolar parallel (MP-P), monopolar series and bipolar series) on the ECP were evaluated to find the optimum operating conditions. At 20 A/m2, 60 min, the highest removal efficiencies were obtained with 85 and 99% for Fe and 64 and 33% for Al electrodes, for cyanide and zinc, respectively. The optimum operating conditions were found to be 30 A/m2 and 40 min, for the Fe electrode at the original pH (9.5) of the rinse water. Considering efficiency and economy, the MP-P connection mode was determined as the optimum connection mode.