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This study evaluated the reliability of the emulsified liquid membrane (ELM) extraction technique for recovering and separating metals, focusing on Nickel (Ni(II)) and Samarium (Sm(III)), both used in electrochemical devices. Key contributions include determining optimal conditions for creating a stable water-in-oil (W/O) emulsion. The optimal conditions were found to be a 5-minute emulsification time, 4 wt.% Span 80 surfactant concentration, a 1.6 volume ratio of the internal phase to the organic phase, 1 M H2SO4 concentration for the internal phase, a 40/160 volume ratio of the emulsion to the external phase, and kerosene as the diluent. Factors affecting the separation of Ni(II) and Sm(III) included the concentrations of the internal aqueous phase, surfactant, and extractant. Under these conditions, an equimolar mixture of Ni(II) and Sm(III) was extracted within 15 min. The study emphasized the importance of phase volume ratio and surfactant concentration for emulsion stability and extraction efficiency. The response surface method (RSM) and Box-Behnken design were used to optimize influential factors, with a modified quadratic model predicting extraction yields of 83.81% for Sm(III) and 15% for Ni(II). The study demonstrates that effective separation of Ni(II) and Sm(III) ions is achievable using this technique, providing valuable insights into efficient and selective metal ion extraction, contributing to the broader field of metal recovery and recycling technologies.