Phosphorus (P) in sediments plays an important role in shallow lake ecosystems and has a major effect on the lake environment. The mobility and bioavailability of P primarily depend on the contents of different P forms, which in turn depend on the sedimentary environment. Here, sediment samples from Baiyangdian (BYD) lake were collected and measured by the Standards, Measurements, and Testing procedure and Phosphorus-31 nuclear magnetic resonance spectroscopy (31P NMR) to characterize different P forms and their relationships with sediment physicochemical properties. The P content in the sediments varied in different areas and had characteristics indicative of exogenous river input. Inorganic P (334–916 mg/kg) was the dominant form of P. The 31P NMR results demonstrated that orthophosphate monoesters (16–110 mg/kg), which may be a source of P when redox conditions change, was the dominant form of organic P (20–305 mg/kg). The distribution of P forms in each region varied greatly because of the effects of anthropogenic activities, and the regions affected by exogenous river input had a higher content of P and a higher risk of P release. Principal component analysis indicated that P bound to Fe, Al, and Mn oxides and hydroxides (NaOH-P) and organic P were mainly derived from industrial and agricultural pollution, respectively. Redundancy analysis indicated that increases in pH lead to the release of NaOH-P. Organic matter plays an important role in the organic P biogeochemical cycle, as it acts as a sink and source of organic P.