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Techniques and Methods 5–B4

Prepared by the U.S. Geological Survey Office of Water Quality, National Water Quality Laboratory

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

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

Chapter 4
Section B, Methods of the National Water Quality Laboratory
Book 5, Laboratory Analysis
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T&M 5-B4
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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


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.

Version 1.1

Posted October 2007

Suggested citation:

Zaugg, S.D., Smith, S.G., and Schroeder, M.P., 2006, Determination of wastewater compounds in whole water by continuous liquid–liquid extraction and capillary-column gas chromatography/mass spectrometry: U.S. Geological Survey Techniques and Methods, book 5, chap. B4, 30 p.




Analytical Method

1. Scope and application

2. Method summary

3. Interferences

4. Apparatus and instrumentation

5. Reagents and consumable materials

6. Standards

7. Sample preparation

8. Safety precautions and waste disposal

9. Gas chromatograph/mass spectrometer performance

10. Instrument Calibration

11. Quality assurance and quality control

12. Calculation of results

Results and discussion of method validation

Summary and conclusions

References cited


For more information about the National Water Quality Laboratory, contact:

Laboratory Chief
U.S. Geological Survey
National Water Quality Laboratory
P.O. Box 25046, Denver Federal Center
Building 95, MS 407
Denver, CO 80225-0046
World Wide Web:

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