To explore the potential of micellar enhanced ultrafiltration (MEUF) process for the treatment of industrial effluent, herein, we report the surfactant-based separation of a metal ion [Ni(II)] from the aqueous solution using two different anionic surfactants viz. dioctyl sodium sulfosuccinate (DSS) and sodium dodecyl sulfate (SDS). By following a systematic investigation, we utilized two membranes with different pore sizes viz. 10,000 MWCO (molecular weight cutoff) and 30,000 MWCO and determined the rejection coefficient and permeate flux of the Ni(II) from aqueous at 1.5 bar trans-membrane pressure. The experimental results showed higher percentage of Ni(II) retention upon using the micellar solution of SDS compared with the solution containing DSS surfactant. In addition, the retention of Ni(II) ions incorporated in the micelles of surfactants was also found to be higher upon using 10,000 MWCO membrane compared with 30,000 MWCO membrane. Hence, we suggest that the combination of SDS surfactant and 10,000 MWCO membrane is a potent solution for the removal of metal ions from aqueous solutions via MEUF process.