Low molecular weight components of both an acid-polymerized and a γ-alumina polymerized furfuryl alcohol polymer were separated by gas chromatography utilizing a Porapak type P-S column packing. The identities of the separated polymer components were established by infrared spectroscopy, mass spectrometry, and nuclear magnetic resonance analysis. Volatile constituents found to be common to both furfuryl alcohol resin types were: furfuryl alcohol, water, difurylmethane, difurfuryl ether, and 2,5-difurfurylfuran. Also, 5-furfurylfurfuryl alcohol was found to be present only in the acid-polymerized resin, and 4-furfuryl-2-pentenoic acid γ-lactone was a constituent only of the γ-alumina-polymerized resin. Contrary to expectation, no esters of levulinic acid were found among the low molecular weight components of the γ-alumina-polymerized furfuryl alcohol polymer.