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This study was designed to investigate the characteristics of atmospheric concentrations of toxic volatile or-ganic compounds(VOCs) in Korea. Target compounds included 1,3-butadiene, aromatics such as BTEX, anda number of carbonyl compounds. In this paper, as the first part of the study, the performance of sampling andanalytical methods was evaluated for the measurement of selected VOCs and carbonyl compounds in theambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupledwith GC/MSD analysis, while carbonyls by the DNPH-silica cartridge sampling with HPLC analysis. Themethodology was investigated with a wide range of performance criteria such as repeatability, linearity, lowerdetection limits, collection efficiency, thermal conditioning, breakthrough volume and calibration methodsusing internal standards. In addition, the sampling and analytical methods established in this study wereapplied to real field samples duplicately collected in various ambient environments. Precisions for the duplicatesamples appeared to be comparable with the performance criteria recommended by USEPA TO-17. Theoverall precision of the sampling and analytical methods was estimated to be within 2030% for majoraromatic VOCs such as BTEX, whereas the precision for major carbonyl compounds such as formaldehydeand acetaldehyde was within 1020% for field samples. This study demonstrated that the adsorbent samplingand thermal desorption method can be reliably applied for the measurement of BTEX in ppb levels frequentlyoccurred in common indoor and ambient environments.