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Abstract: A photocolorimetric microtechnique is described, by which it is possible to determine the real amount of iodine in carrier-free solutions of131INa. The method is conceptually based on the well-known effect of iodine, by which the rate of reduction of ceric sulfate by arsenious acid in sulfuric acid solutions is proportional to the iodide concentration. The tittration and the preparation of its corresponding calibration graph require approximately 90 min; thus, it seems possible to use this technique as a routine analysis. Under the stated conditions of temperature and reaction time, it is possible to determine samples of iodine with concentrations ranging between 20 and 160 ng/ml. The standard error between different determinations is less than ±5%. The application of the method in production control and utilization of carrier-free131I solutions, free from reducing agent, are discussed.