The authors have tested methods used in industrial-sanitary chemistry and have come to the conclusion that none of the colorimetric methods is suitable to analyze acrolein in the presence of aliphatic aldehydes and nitrogen oxides. They developed a fluorescent method of determining acrolein. The method involves separating and quantitatively determining acrolein with the aid of thin-layer chromatography in silicagel-gypsum. It has been established that formaldehyde, aromatic and saturated aliphatic aldehydes, amines, phenols and nitrogen peroxide do not disturb determination. Acetaldehyde and crotonic aldehyde are separated in chromatography, for the absorption of vapors of acrolein from the air a 0.25% solution of hydrochloric hydroxylamine and activated charcoal (AG-5) is recommended.