Odor pollution as an environmental nuisance has attracted a lot of public attention. A great number of volatile organic compounds are capable of causing odor problems, most of which are accompanied by adverse health effects. Volatile organic compound samples were collected from different sites in the high-tech industry development zone in Hefei, including various kinds of factories and residential areas. The samples were analyzed by gas chromatography and mass spectrometry detection, and the analysis results showed that the concentrations of total volatile organic compounds ranged from 285.30 to 1802.30 ppbv. Among the 80 specific volatile organic compounds studied, 46 compounds detected could lead to odor pollution according to the odor threshold. To provide comprehensive characterization of odor pollution, instrumental analysis combined with olfactory measurement were conducted in this study. Odor volatile organic compounds were characterized by using olfactory odor concentration, odor index and coefficient of divergence analysis methods. According to the results, the automobile components manufacturing plants and electric products plants exhibited the highest concentrations of odor volatile organic compounds among all the major emission sites, especially during the injection molding and spraying. Specifically, 1,4-diethylbenzene was the most abundant odorous contributor in this study. Furthermore, the profiles of each volatile organic compounds at the industrial sites were quite different from those at the residential sites, which can be deduced that the surrounding residential zones were not strongly affected by the volatile organic compounds emission from the industrial zones.