ABSTRACT In this study, an innovative hybrid process was proposed and examined as an alternative for nickel/cobalt separation from a synthetic pregnant leach solution. The first step was carried out by employing electrodeionization of a feed solution containing 950 ppm of nickel and 100 ppm of cobalt after adding EDTA to form (Ni-EDTA)−2 complex to suppress migration of nickel cations toward cathodic compartment. This process increased nickel percentage from 90.47 to 97 in the diluted feed solution. This solution was then subjected to cation exchanging process to adsorb the remaining cobalt cations, leading to a nickel purity of 99.7 wt% with an overall recovery 71.1%. On the other hand, the cathode rinse solution of EDI process which contained a major portion of the cobalt cations underwent three stages of extraction process using cyanex 272, resulting in recovery of 65.5 wt% of cobalt with a purity of 100%. It was seen that six stages of solvent extraction process were needed to reach the same purity of cobalt cations by the traditional extraction method. These findings highlight the superior performance of the proposed hybrid process, which not only yielded a relatively high recovery ratio but also ensured excellent purity of nickel and cobalt.