Abstract: In this paper, the wet method using potassium chlorate and nitric acid for the destruction f organic matter in a Kjeldahl flask is studied. The sulfate formed in the decomposition product is determined by the benzidine titration method. The method has been applied to 42 different samples of 9 types of organic sulfur compounds. With the exception of sulfonal, methionine, thio-ether and poly-nuclear-sulfur compounds, all gave satisfactory results with an average deviation of ±0.13%. In comparison with the potassium hydroxide and potassium nitrate fusion method, either gravimetrically or volumetrically, the proposed method proved to be simpler, more rapid and had no need for special apparatus. Procedure: About 50-100 mg of the sample, previously dried and accurately weighed, is treated with 1 g of powdered potassium chlorate in a Kjeldahl flask, add a few drops of water to moisten the sample, then add 2 ml of nitric acid by drops with constant swirling of the flask. Heat with a small flame, until the chlorine vapor subsides. Add another gram of powdered potassium chlorate and continue heat until 1-2 ml of the liquid is left, then add enough hydrochloric acid by drops while still evaporating, in order to decompose the excess of ClO₃ and NO₃ completely, and finally evaporate the solution to dryness. Dissolve and transfer the white residue to a 250 ml beaker with 5 successive portions of about 6 ml of distilled water. Heat the clear solution to 70℃. and adjust to pH 2. Take an adequate amount of benzidine HCl reagent, also heat to 70℃. and add it slowly to the above sulfate solution with constant stirring. After cooling with tap water, filter and titrate the benzidine sulfate with NaOH standard solution as usual.