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A new catalytic spectrophotometric method was developed for the determination of trace amount of Se(Ⅳ) in microemulsion medium. The method is based on the catalytic effect of traces of Se(Ⅳ) on the oxidation of2’,4’-dichlorophenylfluorone (p-CPF) by potassium bromate with HNO3 as an activator in the presence of nonionic microemulsion medium. Under optimum conditions, the calibration graph is linear in the range of 0.4-15 μg. L-1 of Se(Ⅳ) atseparated and enriched by sulphydryl dextrane gel (SDG). The method has been applied for determination of trace selenium with satisfactory results.