Colloidal material in the size range 1.2 nm to 0.4 μm was isolated by ultrafiltration from Chesapeake Bay and Patuxent River waters (U.S.A.). Temperature controlled, stepwise pyrolysis of the freeze-dried material, followed by gas chromatographic-mass spectrometric analyses of the volatile products indicates that the primary organic components of this polymer are carbohydrates and peptides. The major pyrolysis products at the 450°C step are acetic acid, furaldehydes, furoic acid, furanmethanol, diones and lactones characteristic of carbohydrate thermal decomposition. Pyrroles, pyridines, amides and indole (protein derivatives) become more prevalent and dominate the product yield at the 600°C pyrolysis step. Olefins and saturated hydrocarbons, originating from fatty acids, are present only in minor amounts. These results are consistent with the composition of Chesapeake phytoplankton (approximately 50% protein, 30% carbohydrate, 10% lipid and 10% nucleotides by dry weight). The pyrolysis of a cultured phytoplankton and natural particulate samples produced similar oxygen and nitrogencontaining compounds, although the proportions of some components differ relative to the colloidal fraction. There were no lignin derivatives indicative of terrestrial plant detritus in any of these samples. The data suggest that aquatic microorganisms, rather than terrestrial plants, are the dominant source of colloidal organic material in these river and estuarine surface waters.