National Research Council of Canada. NRC Institute for National Measurement Standards
Ultraviolet irradiation of aqueous solutions of iodide/iodate ion containing low molecular weight organic acids generates volatile iodine species that are amenable to detection by atomic spectrometry. In the presence of formic, acetic or propionic acids, photo-chemical generation results in the formation of HI, methyl- and ethyl-iodide respectively, the latter two products being directly identified by gas chromatography–mass spectrometry. Deuterium and ¹³C-labeled reagents were employed to elucidate the provenance of the alkyl group. Use of ¹³CH₃–COOH produced ¹³CH₃–I; deuterated acetic acid (D₃C-COOD) resulted in the formation of CD₃–I. These observations indicate direct transfer of the alkyl group from the carboxylic acid to iodide, consistent with the suggestion that the mechanism of synthesis involves radical induced reactions.
Spectrochimica Acta Part B: Atomic Spectroscopy64, no. 7: 714–716.