Mercury(II) is a very harmful metal, highly toxic, and carcinogenic in nature. Experiments were carried out using the emulsion liquid membrane (ELM) technique in order to evaluate the maximum extraction of mercury(II) from aqueous solutions of mercuric chloride using 3(3) factorial design. The ELM consisted of di-2-ethylhexylphosphoric acid as a carrier, toluene as an organic solvent, span 80 as a surfactant, and sulphuric acid with thiourea solution as stripping phase. The three factors for the factorial design were mercury(II) concentration in the aqueous solution, that is, feed phase concentration, carrier concentration in the membrane phase, and sulphuric acid concentration in the stripping phase. The study has also highlighted the effects of various other parameters, such as pH of the feed phase and thiourea concentration on mercury(II) extraction. The optimization of the factors to obtain maximum extraction were carried out by incorporating main effect plots, interaction plots, analysis of variance (ANOVA), normal probability plots, residual plots, surface plots, and contour plots. A reduced model developed by regression analysis was suggested in which the experimental data were fitted very well. The results showed that it is possible to extract mercury(II) up to 98% from aqueous solutions at the optimum conditions.