An experimental program was conducted to evaluate the relative accuracy of differential ignition and nitric acid solubilization methods for determining the amount of biomass in activated sludge to which powdered activated carbon was added. The results showed the nitric acid method gave better results over a wider range of carbon and biomass concentrations. The nitric acid method was then used in an additional study to determine the ratio of carbon to biomass solids in both the mixed liquor and effluent from a bench scale reactor. The results of this study indicated that there was little difference in the carbon to biomass ratios and supports the concept that solids residence times determined with total suspended solids can be used to control process operation.