This study was carried out to provide the stable and homogeneous sample for the proficiency test which was applied for the olfactory dilution method of the offensive odor. For this purpose, the relationship between VOCs concentration and air dilution test results were analysed. As the results, the mixture of 7.1 ppm of toluene and m-xylene were suitable as a low level of PTM(proficiency test material) for air dilution olfactory method. In addition, time stability and homogeneity between samples were investigated through the time of 6 hr ~ 48 hr. As the results, the stability of sample concentration with GC analysis was shown as 5.1% RSD for toluene and 6.8 %RSD for xylene, respectively. The stability of sample was 5.4 %RSD in terms of air dilution olfactory method.