Halogenated Polycyclic Aromatic Hydrocarbons (X-PAHs) are ubiquitous contaminants that are thought to be generated by processes such as chemical industries and incomplete combustion, including waste incineration and electronic waste (e-waste) burning. X-PAHs are a concern for environmental and human health because they are toxic, mutagenic, and are expected to be more lipophilic than the parent compounds. To study these compounds in the environment, an analytical method was developed, utilizing large-volume injection via a programmable temperature vaporizing (PTV) inlet, using environmental samples from an e-waste area and in Guangzhou, China. The concentrations of 26 X-PAHs were measured in atmospheric particulate matter (PM), house dust (HD), and sediment. In general, the X-PAH concentrations in PM were low, with concentrations ranging from <0.078 to 41.81 pg/m³. There was no significant difference in X-PAH concentrations in PM between the e-waste area and Guangzhou. These concentrations are of the same order of magnitude as previous studies of X-PAHs in PM. These data suggest that e-waste activities are not a significant source of X-PAHs in atmospheric PM. The concentrations of X-PAHs in HD samples ranged from <0.0372 to 3575 pg/g dry weight. In general, there was no significant difference between E-waste and Guangzhou HD concentrations. The profiles of X-PAHs in PM and HD were different, suggesting that there are additional sources for X-PAHs inside homes other than outdoor air. The concentrations of X-PAHs in sediment samples from an e-waste site ranged from <104 to 2890 pg/g dry weight. The X-PAH profile in sediment more closely resembled the X-PAH profile of PM. / Graduation date: 2011