E. Matthijs, M. D. Burford, G. Cassani, M. H. I. Comber, C. V. Eadsforth, P. Haas, H. Klotz, R. Spilker, H. Waldhoff, H.-P. Wingen
May 1, 2013
An analytical method has been developed for the determination of alcohol ethoxylate (AE) components in sewage sludge. The method has been extensively ring tested in several industrial laboratories and concentrations in sludge samples from a number of EU countries have been obtained. The method is based on a methanol soxhlet extraction of centrifuged sludge, which is then cleaned up using an alumina column, followed by derivatisation with naphthoyl chloride and a further alumina column clean-up. The extract is analysed using high performance liquid chromatography (HPLC) with fluorescence detection. The method is capable of determining alcohol ethoxylate components in the range of C12–C18 alkyl chain lengths with an ethoxylate chain of EO4 up to approximately EO20 in sludge samples. The detection limit is approximately 20–30 mg kg −1 of total AEs in dry weight of sludge. Using the method, sludges from several European Sewage Treatment Plants (STP) were analysed. The concentration of the AEs, which are primarily linear, in digestor inlet averaged 1164 mg kg −1 (550–2947 mg kg −1 ) and in outlet sludges the mean value obtained was 167 mg kg −1 (<22–468 mg kg −1 ). At those plants in which concentrations were monitored in both inlet and outlet sludges, removal of the AEs by anaerobic digestion at the STP averaged 82% (range 61–93%). The interlaboratory relative standard deviation of the procedure was around 40% for the digester sludges analysed. The method developed provides a more accurate estimate of the environmental level of AE components compared to existing colorimetric approaches, but the method will over-estimate the concentration of alcohol ethoxylates in sludges due to the non-specific nature of the detection. However, it is sufficiently robust and accurate to estimate alcohol ethoxylates in sludges and hence concentrations that could be applied to soil.