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Volatile sulfur compounds (VSCs) are key odorous compounds from emissions of various odour sources because they are odorous and generally have very low odour threshold values. Identification and quantification of them through air server–thermal desorber–gas chromatography–sulfur chemiluminescence detector (AS-TD-GC-SCD) become more and more popular, although VSCs can be determined by other detectors. To find a valid, practical and quick calibration method is also an important step in their analytical processes. This study compared three different sample preparation and unity sampling methods using both gas standards (with 10 VSCs balanced in pure nitrogen gas) and liquid standards of 7 VSCs. For liquid standard sample preparation, two solvents (methanol and n-pentane) were tested and their calibration results were compared. The study revealed that the three calibration methods with both …