Volatile by-products during heat polymerization of soybean oil at 330degreesC were analyzed using GC-MS and NMR. Color and viscosity changes were monitored for the heat- polymerized soybean oil and the by-products. About 90% (w/w) of the by-products were decanoic, palmitic, linoleic, oleic, and stearic acids and cis-9-tricosene, The by-products also contained small amounts of 3-eicosene, 9,17-octadecadienal, and cyclotetracosene, The weight percentage of decanoic acid increased with reaction time, whereas those of other components showed no trends.