Abstract: Two ends of the 2,4-dinitrophenylhydrazine (DNPH) sampling tube were connected separately with the outlet of climatic chamber and the suction tube of the constant current air sampler, which was adjusted to have an air flow-rate of 0.50 L·min^-1, and a sampling time of 20 min. Blank test was made as the chamber is empty. The chamber was opened and the testing sample, such as the furnitures which may liberate those organic pollutants of aldehydes and ketones, should be put into the chamber as quick as possible and the chamber was closed immediately. Sampling of the air from the climatic chamber was started at this moment. Air sample at the 24th hour was collected for analysis. The organic pollutants in air sample were adsorbed by DNPH and transformed to stable hydrazone derivatives, which were eluted from the sampling tube by SPE with 5 mL of acetonitrile, and the eluate obtained was analyzed by HPLC and the pollutants of aldehydes and ketones were separated by HPLC and detected by PDA detector at the wavelength of 360 nm. As shown by the results, linear relationships between values of peak area and mass concentration of 15 kinds of aldehyde-DNPH and ketone-DNPH were found in the same range of 0.20-20 mg·L^-1, with detection limits (3s) in the range of 0.011-0.054 μg·m^-3. Test for recovery was made by standard addition method, giving results in the range of 84.6%-113%, and RSDs (n=6) were found in the range of 0.40%-3.6%.