Volatile organic compounds (VOCs) are critical components in the generation of secondary organic aerosol (SOA) as well as ozone. In this study, the compositions of VOC emissions from two dyestuff plants were sampled and quantitatively analyzed using SUMMA canister sampling, a pre-concentrator, and GC-MS. Based on the organized emission concentrations, the two plants generated an estimated 443.0 kg a–1 and 667.8 kg a–1 of VOCs, which were dominated by halogenated hydrocarbons. The differences in composition between the plants, plant workshops, and production chains were remarkable. The average removal rate of the VOCs was calculated to be 86.1%, with alkanes and alkenes exhibiting the maximum rate, followed by halogenated hydrocarbons and OVOCs. Our research establishes the characteristics of VOCs—including their EFs, which have hitherto remained unassessed—generated by dyestuff production and offers supporting air quality data for emission inventories of relevant industries as well as policy making.