Biosorption process is considered as economical treatment to remove metal from the aqueous solution compared to other established methods. In this study, Saccharomyces cerevisiae was used as biosorbent and subject to immobilization process which consists of ethanol treatment for the removal of binary metals, lead (II) and nickel (II) from aqueous solution. Response surface methodology (RSM) was used to optimize effective parameters condition and the interaction of two or more parameters in order to obtain high removal of the binary metals. The parameters that have been studied were initial concentration of binary metals solution (10 - 60 mg/L), biosorbent dosage (0.2 - 1.0 g), pH (pH 2 - pH 6) and contact time (30 - 360 minutes) towards lead (II) and nickel (II) ions removal. Based on analysis of variance (ANOVA), biosorbent dosage, solution pH and contact time factor were found significant for both responses. Through optimization procedure, the optimum condition for lead (II) and nickel (II) ions removal were obtained at initial concentration of 10.0 mg/L, biosorbent dosage of 1.0 g, solution pH of pH 6, and contact time of 360.00 minutes, which resulted in 95.08 % and 21.09 % removal of lead (II) and nickel (II) ions respectively.