This study describes the determination of Pb(II) in wastewater by the application of solvent extraction using the halogen-free ionic liquid, 1-butyl-3-methylimidazolium octyl sulfate [BMIM][OCTSO4]. The RSM based on Box-Behnken Design (BBD) was used to optimize the experimental parameters such as extraction time, pH, feed concentration, and the amount of ionic liquid respectively, and their interaction effects that affect the extraction performance of lead. The predicted optimum working conditions are as follows: feed concentration—10 ppm, pH—4.5, shaking time—105 min, and amount of IL—3 g. Under this optimum value, the removal efficiency of lead was obtained at more than 99%. Furthermore, the statistical results revealed that the quadratic model was best fitted to the experimental data at 95% confidence level, which was analyzed by Analysis of Variance. Besides, factors like feed concentration and amount of ionic liquid and their interactions have a positive effect on Pb(II) extraction rate. Based on the analysis, the industrial effluents were treated to determine the physicochemical characteristics of lead before and after extraction. The concentration of Pb2+ in industrial effluents was reduced effectively using the ionic liquid and determined by Atomic Absorption Spectroscopy.