Abstract: Two methods for the determination of As and Sb in organic compounds are described: (1) Transfer about 0.2-0.3g of sample accurately weighed to an Erlenmeyer flask and add 5 ml of concentrated sulfuric acid. Heat over a small flame until the content become carbonized. Add 6-8 g ammonium persulfate in two portions, continue the heating until the solution is colorless and white fumes are evolved. Allow the liquid to cool and add 20 ml of water (in case of antimony, add 1.5 g tartaric acid in addition to the water), 5 ml of 0.1N iodine solution, 20-25 ml of saturated sulfur dioxide water. Boil the solution until the great part of sulfur dioxide is expelled. Cool, remove the residual sulfur dioxide by cautiously adding 0.1N iodine solution using starch as indicator. Dilute to 100 ml with water, neutralize to pH 8-9 by adding 6N NaOH,H₂SO₄, and sodium bicarbonate in succession and titrate with 0.1 N iodine solution. (2) Treat about 0.2-3g sample with concentrated sulfuric acid and persulfate as (1) until colorless and the excess persulfate is decomposed. Then add 0.25 g hydrazine sulfate and heat again for 5 minutes. Cool, add 30 ml of water and boil in order to remove the sulfur dioxide evolved. Dilute with 100 ml of water and titrate with 0.1N potassium bromate using methyl orange as indicator. Both (1) and (2) can be completed in 30-40 minutes and the result agree well with the standard methods described in the literature.