In this paper, the recovery of nickel ions from a simulated Watts electroplating rinse solution by solvent extraction and liquid surfactant membrane (LSM) was studied, in which di(2-ethylhexyl)phosphoric acid was selected as a mobile carrier. Important variables affecting the LSM permeation process, including the membrane viscosity (surfactant concentration), volume ratios of internal to organic phase and of W/O emulsions to external phase, carrier concentration, internal droplet size, and nickel concentration in the external phase, were systematically investigated. The effectiveness of this LSM technique for nickel recovery was demonstrated with better use of carrier over a comparable solvent extraction operation.