This research was designed to investigate the effect of cations on activated sludge characteristics and also to determine their influence on digestion performance. For this purpose, cations in solution and in floc were evaluated along with various activated sludge characteristics and the collected waste activated sludge underwent both anaerobic and aerobic digestion. It was found that large amounts of biopolymer (protein + polysaccharide) remained in the effluent of WWTP that received high influent sodium but had low iron and aluminum in floc. However, sludges from plants with high sodium and high iron and aluminum dewatered well and produced high quality effluents, suggesting that iron and aluminum have significant positive effects on floc properties. Following anaerobic digestion, a significant increase in solution protein occurred and correlations between solution protein, ammonium production, percentile volatile solids reduction and iron in floc were obtained. These data indicate that iron-linked protein is released to solution when iron is reduced and its degradation is responsible for volatile solids reduction in anaerobic digestion. In aerobic digestion, polysaccharide in solution increased along with calcium, magnesium and inorganic nitrogen. This implies that divalent cation-bound biopolymer might be the primary organic fraction that is degraded under aerobic digestion. Combined (anaerobic/aerobic) digestion was performed and produced further volatile solids destruction with discrete cation and biopolymer response during each phase of digestion. These results support the theory that two types of organic matter with different cation bindings are present in floc and each type is degraded under different digestion processes. / Master of Science