Optimization of a microwave-assisted extraction procedure for the determination of selected alkyl, aryl, and halogenated phenols in sewage sludge and biosolids

IF 2 Q3 Environmental Science

Water Quality Research Journal of Canada Pub Date : 2016-11-02 DOI:10.2166/WQRJC.2016.002

Hing‐Biu Lee, M. Svoboda, T. Peart, S. Smyth

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引用次数: 1

Abstract

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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微波辅助萃取法测定污水污泥和生物固体中选定的烷基、芳基和卤代酚的优化

建立并优化了微波辅助萃取法测定污水污泥和生物固体样品中15种烷基、芳基和卤化酚的方法。考察了溶剂、温度、时间、水分含量、酸度、提取次数等因素对苯酚回收率的影响。结果表明，萃取溶剂对各酚类化合物的回收率影响最大，而pH对六氯酚和五氯酚的回收率影响最大。在冰醋酸存在下，用丙酮-己烷混合物提取湿污泥样品。提取液经蒸发，乙酸酐乙酰化，硅胶净化。对于干污泥样品，还提出了同时提取和乙酰化酚的可选程序。采用气相色谱-质谱法(GC-MS)分析污泥提取物中的三氯生(TCS)、烷基酚和芳基酚，采用负离子化学电离法(GC-MS)分析多卤代酚。方法对壬基酚的检出限约200 ng/g;

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来源期刊

Water Quality Research Journal of Canada WATER RESOURCES-

CiteScore

1.70

自引率

0.00%

发文量

审稿时长

>12 weeks

期刊介绍： The Water Quality Research Journal publishes peer-reviewed, scholarly articles on the following general subject areas: Impact of current and emerging contaminants on aquatic ecosystems Aquatic ecology (ecohydrology and ecohydraulics, invasive species, biodiversity, and aquatic species at risk) Conservation and protection of aquatic environments Responsible resource development and water quality (mining, forestry, hydropower, oil and gas) Drinking water, wastewater and stormwater treatment technologies and strategies Impacts and solutions of diffuse pollution (urban and agricultural run-off) on water quality Industrial water quality Used water: Reuse and resource recovery Groundwater quality (management, remediation, fracking, legacy contaminants) Assessment of surface and subsurface water quality Regulations, economics, strategies and policies related to water quality Social science issues in relation to water quality Water quality in remote areas Water quality in cold climates The Water Quality Research Journal is a quarterly publication. It is a forum for original research dealing with the aquatic environment, and should report new and significant findings that advance the understanding of the field. Critical review articles are especially encouraged.