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Optimization of a microwave-assisted extraction procedure for the determination of selected alkyl, aryl, and halogenated phenols in sewage sludge and biosolids
Author(s) -
HingBiu Lee,
Miloš Svoboda,
Thomas E. Peart,
Shirley Anne Smyth
Publication year - 2016
Publication title -
water quality research journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.339
H-Index - 44
eISSN - 2408-9443
pISSN - 1201-3080
DOI - 10.2166/wqrjc.2016.002
Subject(s) - chemistry , phenols , biosolids , extraction (chemistry) , sewage sludge , chromatography , acetic anhydride , acetic acid , solvent , organic chemistry , sewage , waste management , engineering , catalysis
A microwave-assisted extraction method for the determination of 15 alkyl, aryl, and halogenated phenols in sewage sludge and biosolids samples was developed and optimized. The effects of solvent, temperature, time, moisture content, acid, and number of extractions on the recovery of phenols were evaluated. Results indicated that extraction solvent had the greatest impact on the recovery of all phenols while pH had the largest effect on recovery of hexachlorophene and pentachlorophenol. Wet sludge samples were extracted with acetone-hexane mixture in the presence of glacial acetic acid. The extract was evaporated, acetylated by acetic anhydride and cleaned up by silica gel. For dry sludge samples, an optional procedure for the simultaneous extraction and acetylation of phenols was also proposed. Triclosan (TCS) and the alkyl and aryl phenols in sludge extracts were analyzed by gas chromatography-mass spectrometry (GC-MS) in electron-impact mode while polyhalogenated phenols were analyzed by GC-MS in negative ion chemical ionization mode. Method detection limits were ca. 200 ng/g for nonylphenol,

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