The main objective of this research was to test the hypothesis that bioavailable protein and, more specifically, the sulfurcontaining amino acids within the protein, can be degraded by proteolytic enzymes to produce odor-causing compounds-mainly volatile sulfur compounds (VSCs)-during biosolids storage. To achieve these objectives, samples of digester effluent and cake solids were collected at 11 different wastewater treatment plants in North America, and the samples were analyzed for protein and amino acid content and general protein-degrading enzyme activity. At the same time, cake samples were stored using headspace bottles, the concentration of VSCs were measured using gas chromatography, and olfactometry measurements were made by a trained odor panel. The results showed that the bound cake protein content and methionine content was well-correlated with VSC production and the detection threshold measured by the odor panel. Water Environ. Res., 80, 127 (2008).