Method of measurement and collection of benzene, toluene and xylenes in the air of urban residential district was studied. The air samples was absorbed by charcoal from an unpolluted residential district and a polluted residential district, The samples were analysed by gas chromatography. Absorbance of charcoal, separation of bezene hydrocarbon, accuracy and precision are discussed. The separate values of benzene, toluene and xylene were 0.032, 0.048, 0.040mg/m3.