In this study, the effect of difference in gas phase media (between nitrogen and air) used for standard gas preparation was evaluated with respect to relative recovery of carbonyl compounds (CC). To this end, calibration analysis was carried out using gaseous CC standards (with the two media) containing five different CCs (acetaldehyde (AA), propionaldehyde (PA), butyraldehyde (BA), isovaleraldehyde (IA), and valeraldehyde (VA)). Derivatization of CCs was made, and the carbonyl hydrazones eluted via acetonitrile were analyzed by reverse phase HPLC for UV detection. As a result, the CC standards in N2 medium showed about 10% higher recovery than that of air medium. However, the difference in their relative recovery is in most cases not statistically significant. Consequently, it is concluded that the difference in gaseous media like N2 or air is unlikely to affect derivatization efficiency of CCs.