A study was made on the radioiodination of organic compounds in presence of hydrogen peroxide both in aqueous and organic solvent systems. In case of the reaction of rosebengal, Hippuran, and 5-iodo-uracil the aqueous reaction system could give high labelling yield within a relatively short reaction time. Labelling yield of average 50% could be obtained within 30 minutes of reaction sequence. In cases of organic solvent systems (D.M.S.O., D.M.F., and Dioxane) the solvent system of D.M.S.O. could give better yield for neutral organic compounds, where as D.M.F. and Dioxane gave better labelling result for acidic materials. Especially, o-iodobenzoic acid, o-iodotoluene, and pentachlorophenol could be labelled better in organic solvent system.