Iodinated glycerol (CAS no. 5634-39-9), therapeutically used as an expectorant and source of organically bound iodine, was analyzed to determine the purity and composition of the chemical samples used in carcinogenicity and toxicity studies. The manufactured product is described by the patent and chemical literature as a mixture of two isomeric iodopropylideneglycerols (structures 1 and 2). The results of our studies, however, indicate that the two principal components of the product were 3-iodo-1,2-propanediol (IPD) and glycerol (GLY). Analyses from GC-MS (full scan electron impact) and carbon-13 nuclear magnetic resonance spectrometry provided conclusive identification of these components. The quantification of IPD and GLY in one of two samples of commercial product using GC-flame ionization detection indicated concentrations of 33 and 17%, respectively (Sample A). Similar concentrations were determined for a second sample from the same source (Sample B), which was a gratis sample procured approximately nine years after Sample A. Numerous minor components were also observed in these two samples. These components were tentatively identified as condensation products of glycerol and iodine-containing analogues. The iodopropylideneglycerol compounds, described in the patent, were not observed in either of the two samples.