In kerosene samples from nuclear fuel reprocessing, iodoalkanes with chain-lengths from C4 to C13 have been identified. The kerosene samples were purified by means of solid-phase extraction. By this method other fission products like125Sb and106Ru were quantitatively removed from the solution. The only remaining radioactive nuclide was thus129I. The iodoorganic compounds in the kerosene from the solvent were enriched from 6000 Bq/L to 100 000 Bq/L129I by vacuum distillation. Chromatographic separation by HPLC, fractionation, and -measurement of the fractions showed that at least one polar and one nonpolar iodoorganic compound were present. Derivatisation of the iodoorganic compounds with, 1,4-diazabicyclo-2,2,2-octane to quatermary ammonium salts and252Cf plasma desorption mass spectrometry of the products revealed that the main iodoorganic constituents in the kerosene were iodobutane as polar and iodododecane as nonpolar compound in approximately equal concentrations.