AbstractIn this work, volatile organic compounds (VOCs) in the ambient air of a secondary fiber paper mill were analyzed. For the sake of studying pollution comprehensively, four sites in the paper mill were analyzed and active sampling methods were used. Desorption was carried out with two solvents, carbon disulfide and dichloromethane. The compositions of VOCs were determined by gas chromatography-mass spectrometry (GC-MS) method. The main identified substances in the four sites were as follows: (1) waste paper sorting room: alkanes, phenols, and esters; (2) papermaking workshop: benzene series, alkanes, ethers, and phenols; (3) vacuum pump outlet: benzene series and phenols; and (4) office area: benzene series and phenols. Two main toxic substances in VOCs, the benzene series and phenols, were detected in the ambient air of the paper mill. The benzene series existed in three places along the main process of the paper mill and even existed in the office area, which was far away from the production line. Additionally, phenols were detected in all sampling locations in the paper mill.