Semivolatile compounds in smoke from gram-scale incomplete burning of plant materials were assessed by gas chromatography and mass spectrometry. Gas syringe sampling was shown to be adequate by comparison with adsorbent sampling. Methoxyphenols as well as 1,6-anhydroglucose were released in amounts as large as 10 mg/kg of dry biomass at 90 % combustion efficiency.Wood, twigs, bark and needles from the conifers Norway spruce and Scots pine emitted twelve reported 2-methoxyphenols in similar proportions. Grass, heather and birchwood released the same 2-methoxyphenols but also the corresponding 2,6-dimethoxyphenols which are characteristic of angiosperms. The, methoxyphenols are formed from lignin and 4iffer in structure by the group in para position relative to the phenolic OH group. Prominent phenols were those with trans-1-propenyl and ethenyl groups in that position. Vanillin, 4-hydroxy-3-methoxybenzaldehyde, was a prominent carbonyl compound from the conifer materials.