Various experimental factors, which could affect the measurement of furan by automated headspace gas chromatography/mass spectrometry, have been investigated. It was established that furan was not lost during sample heating through leakage or decomposition. Deuterium-labelled furan, used as an internal standard, was stable with respect to incubation in the presence of food and stable in model food systems at raised temperature. Saturation of the aqueous phase of the sample with ammonium sulphate improved the partitioning of furan from samples into the headspace. There was a very small decrease in the peak areas of both d0-furan and d4-furan when heated at acid pH. For food samples heated at normal headspace incubation temperature (50 degrees C), the level of furan was highest at the most acidic conditions used (pH 2.4) and did not differ significantly between pH 5 and 10. Under strong heating, production of furan decreased markedly at very high pH. Quantification based on standard additions or on external calibration gave comparable results for foods containing furan at relatively low, moderate and high levels.