For efficient and accurate speciation analysis of I in the nitric acid solution of spent nuclear fuel in its reprocessing process, a sequential procedure for stepwise separation of different iodine species in 3 mol/L HNO was proposed based on the solvent extraction using CCl and mesitylene. Molecular iodine (I) was first separated by solvent extraction using CCl, and iodide (I) remaining in the aqueous phase was oxidized to I by adding NaNO and then extracted to mesitylene. Finally, iodate (IO) was reduced to I using NHOH·HCl and extracted to mesitylene. The separation efficiency of 98-99% for tracer amounts of I, I, and IO in 3 mol/L HNO and less than 2% crossover among different iodine species were achieved. The extraction process and mechanism of different iodine species in CCl and mesitylene were investigated, and the problem of crossover of different iodine species due to the low extraction efficiency of low concentration of iodine in nitric acid solution was solved. A direct transfer of IO from HNO to the mesitylene phase without conversion to I was observed, which was attributed to the iodination of mesitylene in the HNO medium. Addition of a stable iodine species carrier and repeated extraction significantly improved the separation efficiency of iodine species, making their quantitative separation achievable. This method provides an approach for speciation analysis of I in the acidic spent nuclear fuel solution, enabling us to investigate and control the behavior of volatile I in the spent nuclear fuel reprocessing process.
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