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Acidified 2,4-dinitrophenylhydrazine (DNPH) solution, or DNPH-impregnated cartridges are commonly used for the collection of automotive exhaust carbonyl compounds. There are some DNPH-carbonyl compounds in not in use DNPH cartridges and DNPH solution. Furthermore, concentrations of automotive exhaust carbonyl compounds are decreasing according to improvement of the purification technology for automotive exhaust. Automotive exhaust carbonyl compounds become to be difficult to be analyzed with DNPH collection method, because of these two reasons. It is thought that reliable analysis of acrolein in automotive exhaust is very difficult because concentration of DNPH-acrolein in extracted solution is not stable. Furthermore, it is found out that DNPH-acrolein in DNPH-cartridge is disappeared for short time storage in this research.