With good correlation with methylene chloride (CH2Cl2) and ethylene dichloride (EDC), abundant CH3Cl in urban Shanghai, was mainly associated with industrial activities, although biomass burnings exist widely in rural areas of east China. The high concentrations and large variation of CH3Cl and EDC simultaneously appeared at Liyang site. Spikes of CH3Cl and EDC concentrations as well as toluene/benzene (T/B) ratios frequently present in easterly airflows indicated an important contribution from emissions of chemical plants clustering in the east of Liyang. Different emission sources may contribute to ambient CH3Cl at Taizhou site, which was suggested by the two kinds of linear regressions of CH3Cl to some other compounds detected. The substantially elevated CH3Cl levels suggest significant influence of intensive industrial activities on the YRD atmosphere.