Volatile organic compounds (VOCs) emitted by two wood-rotting basidiomycete fungi, Serpula lacrymans (dry rot fungus) and Coniophora puteana (cellar fungus), and the timber of Pinus sylvestris (Scots pine), were identified. Several volatile collection techniques were employed including dichloromethane solvent extraction, solid-phase microextraction (SPME) and thermal desorption of VOCs entrained on Tenax GR. In addition, a new method of solid sample injection (SSI) is described which utilises a low injector temperature and an all-glass deactivated injector liner designed to minimise both the formation of pyrolysis products and analyte degradation. All the volatile compounds collected were analysed using electron impact capillary gas chromatography-mass spectrometry (GC-MS) on HP-5, HP-Innowax and β-cyclodextrin columns. SSI and Tenax thermal desorption were found to be the most effective extraction methods. A total of 19 VOCs were observed from S. lacrymans grown on glass slides and pine, 15 from C. puteana grown on glass slides and 12 from P. sylvestris timber. S. lacrymans was found to emit, in low abundance, six unique VOCs, of which 2-methylbutanal was the greatest. The major volatile compound emitted by S. lacrymans was 1-octen-3-ol, which was also found in lower abundance from C. puteana. Six VOCs, including diethylene glycol and 4-methyl methylbenzoate, were found to be unique to C. puteana, all in medium abundance. From P. sylvestris, the major volatiles identified were S-α-pinene and 3-carene.