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Perfluoroalkyl acids (PFAAs) are widely used as multi-purpose surfactants or water/oil repellents. In order to understand the contamination level and compositional profiles of PFAAs in aqueous environment in textile, leather, and paper making industrial areas, surface waters and tap waters were collected along the watershed of the Qiantang River where China's largest textile, leather, and paper making industrial bases are located. For comparison, surface water and tapwater samples were also collected in Hangzhou and its adjacent areas. 17 PFAAs were analyzed by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry. The results show that the total concentrations of PFAAs (ΣPFAAs) in the Qiantang River waters ranged from 106.1 to 322.9 ng/L, averaging 164.2 ng/L. The contamination levels have been found to be extremely high, comparable to the levels of the most serious PFAA contamination in surface waters of China. The PFAA composition profiles were characterized by the dominant PFOA (average 58.1% of the total PFAAs), and PFHxA (average 18.8%). The ΣPFAAs in tap water ranged from 9.5 to 174.8 ng/L, showing PFAA compositional pattern similar to the surface waters. Good correlations between PFAA composition profiles in tap waters and the surface waters were observed.