Poly(ethylene glycol) (PEG) residues were detected in organic solute isolates from surface water by H-1 nuclear magnetic resonance spectrometry (NMR), C-13 NMR spectrometry, and colorimetric assay. PEG residues were separated from natural organic solutes in Clear Creek, CO, by a combination of methylation and chromatographic procedures. The isolated PEG residues, characterized by NMR spectrometry, were found to consist of neutral and acidic residues that also contained poly(propylene glycol) moieties. The H-1 NMR and the colorimetric assays for poly(ethylene glycol) residues were done on samples collected in the lower Mississippi River and tributaries between St. Louis, MO, and New Orleans, LA, in July-August and November-December 1987. Aqueous concentrations for poly(ethylene glycol) residues based on colorimetric assay ranged from undetectable to approximately 28 mu-g/L. Concentrations based on H-1 NMR spectrometry ranged from undetectable to 145 mu-g/L.