Recent developments in gas chromatography (GC)-mass spectrometry (MS) have opened up the possibility to use the high resolution-accurate mass (HRAM) Orbitrap mass analyzer to further characterize the volatile and semivolatile fractions of environmental samples. This work describes the utilization of GC Orbitrap MS technology to characterize iodine-containing disinfection by-products (iodo-DBPs) in chlorinated and chloraminated DBP mixture concentrates. These DBP mixtures were generated in lab-scale disinfection reactions using Llobregat river water and solutions containing Nordic Lake natural organic matter (NOM). The DBPs generated were concentrated using XAD resins, and extracts obtained were analyzed in full scan mode with the GC Orbitrap MS. Integration of high resolution accurate mass information and fragment rationalization allowed the characterization of up to 11 different iodo-DBPs in the water extracts analyzed, including one new iodo-DBP reported for the first time. Overall, formation of iodo-DBPs was enhanced during chloramination reactions. As expected, NOM characteristics and iodide and bromide content of the tested waters affected the amount and type of iodo-DBPs generated. ; Peer reviewed