Phosphorus (P) compounds in three different lake surface sediments were extracted by sequential P extraction and identified by P-31 nuclear magnetic resonance (P-31 NMR) spectroscopy. The extraction procedure primarily discriminates between inorganic P-binding sites but most extraction steps also contained P not reacting (nrP) with the molybdenum complex during P analyses. In all three lakes, the nrP dominated in the NaOH extracts. Nonreactive P from the dystrophic lake was dominated by potentially recalcitrant P groups such as orthophosphate monoesters, while the nrP in the two more productive lakes also contained polyphosphates, pyrophosphate, and organic P groups such as P lipids and DNA-P that may be important in remineralization and recycling to the water column. In addition, polyphosphates showed substantial dynamics in settling seston. The Humic-P pools (P associated with humic acids) showed strong signals of orthophosphate monoesters in all three lakes, which supported the assumption that P-containing humic compounds are indeed recovered in this fraction, although other organic P forms are also present. Thus, in addition to expanding the understanding of which organic P forms that are present in lake sediments, the P-31 NMR technique also demonstrated that the chemical extraction procedure may provide some quantification of recalcitrant versus labile organic P forms.