An analytical method was developed and used to measure trace levels of fragrance materials (FMs) in municipal wastewater and treated wastewater. Sixteen FMs were selected as analytes because of their wide range of physical chemical properties. The analytical method included the use of nine perdeuterated FMs as internal standards, a high-flow C18 speed disk for the extraction of FMs from aqueous matrices, and an accelerated solvent extraction system for the extraction of FMs from solid matrices. For aqueous matrices, average FM recoveries (relative to the perdeuterated FM internal standard) were 97−115%, with limits of quantitation ranging from 0.5 to 35 ng/L. For activated sludge solids and primary influent solids, the average FM recovery from the extraction procedure was 81%. Concentrations and removal of FMs at an activated sludge and a trickling filter wastewater treatment plant were determined in the U.S. FM influent concentrations ranged from 0.3 to 154 μg/L, while FM effluent concentrations ranged f...