The level of microplastics (MPs) in wastewater treatment plants (WWTPs) has been well evaluated by the particle number, while the mass concentration of MPs and especially nanoplastics (NPs) remains unclear. In this study, pyrolysis gas chromatography–mass spectrometry was used to determine the mass concentrations of MPs and NPs with different size ranges (0.01–1, 1–50, and 50–1000 μm) across the whole treatment schemes in two WWTPs. The mass concentrations of total MPs and NPs decreased from 26.23 and 11.28 μg/L in the influent to 1.75 and 0.71 μg/L in the effluent, with removal rates of 93.3 and 93.7% in plants A and B, respectively. The proportions of NPs (0.01–1 μm) were 12.0–17.9 and 5.6–19.5% in plants A and B, respectively, and the removal efficiency of NPs was lower than that of MPs (>1 μm). Based on annual wastewater effluent discharge, it is estimated that about 0.321 and 0.052 tons of MPs and NPs were released into the river each year. Overall, this study investigated the mass concentration of MPs and NPs with a wide size range of 0.01–1000 μm in wastewater, which provided valuable information regarding the pollution level and distribution characteristics of MPs, especially NPs, in WWTPs.

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