Aldehydes and ketones are known as one of the hazardous air pollutants. Usually, acidified 2,4-dinitrophenylhydrazine (DNPH) solution, or DNPH-impregnated cartridges are used for automotive exhaust carbonyls collection. Then, aldehydes and ketones combined with DNPH are analyzed by HPLC/UV (High Performance Liquid Chromatography/ Ultra Violet Detection). DNPH cartridge is used widely for a good point of the handling although handling of DNPH solution is not so convienient. However, the analytical result of acrolein using DNPH cartridge was known as the low reliability. Acrolein-DNPH is changed to acrolein-DNPH-DNPH in the cartridge with acid atmosphere before extraction. And then, acrorein-DNPH-DNPH is changed to acrorein-DNPH-DNPH-DNPH with an acid atmosphere. As a result of such chemical reaction before extraction, the acrolein-DNPH is detected to low concentration.We found that at the low temperature condition, acrolein-DNPH concentration decrease speed is held down. Then, we developed new automotive exhaust aldehydes and ketones collection method using conventional DNPH cartridge. When using this automotive exhaust collection method, we can get reliable acrolein concentration and other aldehydes and ketones concentration. We would like to discuss this reliable collection method for automotive exhaust aldehydes and ketones in this paper.