Microanalysis of organic sulfur compounds by means of combining thin layer chromatography and oxygen combustion flask method was attempted. The following procedure was found to be very simple and to give accurate results. The mixture of sulfa drugs was separated with T.L.C., and it was burned in a flask filled with oxygen, and the gas formed was absorbed in a dilute solution of sodium hydroxide. The solution was neuralized with hydrochloric acid and heated in a water bath. The sulfate ion formed was then treated with barium chromate solution and its absorbancy at 370 m.mu. was measured.