| Summary: | The Songhua River is one of the most populated and oldest industrial areas in Northeast China. To understand the sources and distribution of polycyclic aromatic hydrocarbons and their derivatives, such as 16 priority (PAHs), 33 methylated (Me-PAHs), and 12 nitrated (NPAHs) in river water and sediment, were noticed. The concentrations of ∑PAHs, ∑Me-PAHs, and ∑NPAHs in river water scaled from 135 to 563, 9.36 to 711, and 1.26 to 64.7 ng L<sup>−1</sup>, with mean values of 286, 310, and 17.9 ng L<sup>−1</sup>, and those in sediments were from 35.8 to 2000 ng g<sup>−1</sup>, 0.62 to 394 ng g<sup>−1</sup>, and 0.28 to 176 ng g<sup>−1</sup> (dry weight) with mean values of 283, 103, and 21.7 ng g<sup>−1</sup>. The compositions proved that two-ring and three-ring compounds of PAHs, NPAHs, and four-ring, six-ring of Me-PAHs were prevalent in water samples; in contrast, four-ring dominated in sediments. Principal components analysis (PCA) and diagnostic ratios confirmed that pollutant source was mixed petrogenic and pyrogenic origin. The fugacity fraction (ƒƒ) was also calculated to explain the trend of sediment–water exchange, high ƒƒ values found in summer, for most HMW PAHs and Me-PAHs that these substances acted as a secondary source of emissions from sediment to water. The risk assessment for water was categorized as high.
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