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

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

Abstract:

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.

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USGS Numbered Series

ProdID:

79258

Citation Author:

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

Citation Contributing Office:

USGS National Water Quality Laboratory

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Version 1.1

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ENGLISH

Citation Larger Work Title:

Chapter 4 of Section B, Methods of the National Water Quality Laboratory of Book 5, Laboratory Analysis

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Citation Month:

Oct

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v, 30 p.

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Geological Survey (U.S.)

Citation Series:

Techniques and Methods

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Citation Series Number:

5-B4

Citation Search Results Text:

Determination of Wastewater Compounds in Whole Water by Continuous Liquid-Liquid Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry; 2006; TM; 5-B4; Chapter 4 of Section B, Methods of the National Water Quality Laboratory of Book 5, Laboratory Analysis; Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.