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An analytical procedure has been developed for determining aliphatic alcohol ethoxylates (AAEs) in raw wastewater. AAEs were isolated by solid-phase extraction on a styrenedivinylbenzene disk. The maximum volume that was processed with- out plugging of the disk was 20 mL. Then AAEs were desorbed with methanol and, after evaporation to dryness, the residue was analyzed by reversed-phase liquid chromatography coupled to mass spectrometry via atmospheric pressure interface. Two des- orption temperatures (ambient and 100 °C), two organic modifiers of the mobile phase (methanol and acetonitrile) and two atmos- pheric pressure interfaces (electrospray and atmospheric pressure chemical ionization) were tested. The lowest coefficients of vari- ation for replicate measurements were obtained by desorbing AAEs from the extraction disk at 100 °C and by using methanol-based mobile phase with atmospheric pressure chemical ionization source for extract analysis. Under these conditions, all the analytes (ranging in size from 10 to 16 alkyl carbons and from 1 to 25 ethoxylate groups) were recovered at more than 70 % and the limit of quantification (signal-to-noise ratio = 10) ranged between 0.05 and 4 µg L -1.

Development of an analytical procedure for the measurement of nonionic aliphatic polyethoxylated surfactants in raw wastewater