Speciation of Iodide, Iodine, and Iodate in Environmental Matrixes by Inductively Coupled Plasma Atomic Emission Spectrometry Using in situ Chemical Manipulation

Abstract

Abstract Dissolved iodine, iodide, and iodate are determined in environmental matrixes by in situ chemical manipulation and inductively coupled plasma atomic emission spectrometry (ICPAES). The method uses equipment commonly available to most laboratories involved in environmental inorganic analysis. Total dissolved iodine, iodide, and iodate are determined by ICPAES using iodine vapor generation. Total iodine is determined directly by ICPAES after filtration. Total dissolved iodide (I−) is oxidized in situ to iodine by the addition of sodium nitrite in sulfuric acid in a simplified continuous flow manifold. Iodate is determined by prereduction at the instrument before analysis by the in situ oxidation ICPAES procedure. A standard nebulizer produces the gas–liquid separation of the total iodine, which is then quantified by ICPAES at 206.16 nm. The instrument detection limit for the iodine analysis was 0.04 μg/mL. Recoveries from seawater, saltwater, and freshwater standard reference materials ranged from 85 to 118% and averaged 98%. For samples containing both iodine and iodide, the total is determined with in situ oxidation, iodine is determined without the oxidizing reagents, and iodide is calculated from the difference. For samples containing all 3 species, pre-reduction is used and the iodine and iodide concentrations are subtracted for quantitation of iodate. The analysis is selective for these 3 species (I−, I2, and IO−3). A group of 20–30 samples may be analyzed and quantitated for all 3 individual, commonly occurring iodide species in less than 1 h. The procedure is considerably faster than any other reported techniques. This method is especially well-suited to the analysis of small environmental samples.