Method 524.2, Revision 3.0, is a laboratory analytical method for the determination of 59 volatile organic compounds (VOCs) in water. The method uses purge-and-trap techniques to isolate VOCs from a water matrix, and capillary column gas chromatography-mass spectrometry (GC/MS) for the identification and measurement of the analytes. This study evaluated 48 additional compounds of environmental interest as candidates for possible inclusion in the method. The new candidate VOCs include many polar, water soluble compounds that are very difficult to remove from the water matrix. The initial evaluation tested the candidate VOCs in fortified reagent water for sensitivity and linearity of response. Results indicated that 28 of the compounds had sufficient potential to warrant further study. Additional studies Investigated purging efficiency, precision and accuracy, method detection limits (MDLs), sample preservation and storage, and possible matrix effects. Final results demonstrated that Method 524.2, Revision 3.0, was capable of determining 24 of the candidate VOCs with acceptable accuracy and precision. MDLs were generally 1 µg/L or lower. © 1992 Journal of Chromatographic Science.