A thermal desorption-gas chromatography/mass spectrometric method was developed for the determination of methyl bromide in fumes formed during preservation of cultural materials from insects. Methyl bromide in lunes was collected by drawing 10ι of air through the adsorbent tube filled with a solid adsorbent (Chromosorb). The air samples were analyzed by using a special thermal desorption device and GC/MS determination. The recovery of methyl bromide by air sampling was 88% and the detection limit of the assay was 0.1 pptv based upon assayed air of 10ι. The method was applied to the determination of fumed methyl bromide used for the preservation of papers in a library. The mean concentration of methyl bromide determined in a library was 280.2 $pm$ 25.4 pptv.