Abstract: In this paper a method for the determination of sodium and potassium in butadiene styrene rubber by digestion and emulsification-flame atomic emission spectrometry was reported.The sample was first digested with concentrated nitric acid,the digested product was then dissolved in a mixed solvent of ethyl alcohol-methyl isobutyl ketone and emulsified with emulsifier Triton X-100.Barium ion was used as deionization agent for the determination for sodium and potassium.The selection of solvent and emulsifier,the consistence of viscosity of test solution and blank solution,the interferences and the detection limits were studied.The relative standard deviations were found to be less than 2.4%.The recoveries obtained were in the range of 98.0%-104.7%.