NMR methods suitable for the analysis of organic contaminants in water have been demonstrated and applied to two untreated aqueous product streams from a coal liquefaction process. A range of NMR techniques (including 1H-13C two-dimensional correlation, distortionless enhancement via polarization transfer (DEPT), and water attenuation by T2 relaxation (WATR) H2O peak suppression) is applied to one sample to establish unequivocal resonance assignment and organic compound identification. For subsequent samples, simpler methods (conventional 13C NMR or WATR 1H NMR) are sufficient. Sample preparation is minimal and does not prejudice detection of volatile organics. Various alcohols, ketones, and phenols have been identified in the samples investigated. Relative abundances have been measured. © 1990, American Chemical Society. All rights reserved.