Abstract. A new method of determination of selenium and separation of Se(IV) and Se(VI) in sea water is described. The selenium is determined by fluorometric method using Se-DAN complex in cyclohexane media. Prior to the fluorometric determination, Se(IV) is separated from sea water by means of Se(IV)-DDTC complex which is adsorbed on the macroreticular resin. As to the separation of the total selenium from sea water sample, the reduction and coprecipitation method is used. Se(VI) is determined with the same method as used for the total selenium after the separation of Se(IV). The average recoveries are 92.5±1.3% for Se(IV) and 97.4±0.9% for ∑Se. The standard deviation of analytical results is below 10%.