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National Water Quality Laboratory

Friday December 15, 2017

Techniques and Methods 5-B4

Determination of Wastewater Compounds in Whole Water by Continuous Liquid-Liquid Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

Steven D. Zaugg, Steven G. Smith, and Michael P. Schroeder

July 2006

Quality assurance reviews during May 2007 at USGS NWQL detected an error by which the identifications of Acetyl-hexamethyl-tetrahydronaphthalene (AHTN) and Hexahydrohexamethylcyclopentabenzopyran (HHCB) were reversed. This error affected data published in this report. The results in this revised publication reflect correct data reporting for these two compounds.

For more information on this issue see the National Water Quality Laboratory Technical Memorandum 2007.03 at http://nwql.usgs.gov/Public/tech_memos/nwql.2007-03.pdf

A method for the determination of 69 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals on aquatic organisms in wastewater. This method also is useful for evaluating the effects of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are indicators of wastewater or have endocrine-disrupting potential. These compounds include the alkylphenol ethoxylate nonionic surfactants, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides.

Wastewater compounds in whole-water samples were extracted using continuous liquid–liquid extractors and methylene chloride solvent, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 0.5 microgram per liter averaged 72 percent ± 8 percent relative standard deviation. The concentration of 21 compounds is always reported as estimated because method recovery was less than 60 percent, variability was greater than 25 percent relative standard deviation, or standard reference compounds were prepared from technical mixtures. Initial method detection limits averaged 0.18 microgram per liter. Samples were preserved by adding 60 grams of sodium chloride and stored at 4 degrees Celsius. The laboratory established a sample holding-time limit prior to sample extraction of 14 days from the date of collection.

This report is available on the USGS Publishing Network.

VIEW the report.


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