Abstract: A PEG600 and (NH₄)₂SO₄ two-phase aqueous filtration system was used in lab for studying the removal of lead ions from waste water. Based on the analytical data obtained from atomic absorption spectrometry, a response surface methodology was applied to optimize the technology. The optimal processing conditions included 40.25% on volume fraction of PEG600, 0.17 g·mL^-1 of (NH₄)₂SO₄, pH at 2.55, and temperature at 40.28 to render a lead removal rate of 87.47%.