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Water-Resources Investigations Report 01-4186

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Wastewater Compounds by Polystyrene-Divinylbenzene Solid-Phase Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

By Steven D. Zaugg, Steven G. Smith, Michael P. Schroeder, Larry B. Barber, and Mark R. Burkhardt

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WRI 01-4186
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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 67 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 in wastewater on aquatic organisms. This method also may be useful for evaluating the impact of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are an indicator of wastewater or that have been chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclicaromatic hydrocarbons, and high-use domestic pesticides.

Water samples are filtered to remove suspended particulate matter and then are extracted by vacuum through disposable solid-phase cartridges that contain polystyrene-divinylbenzene resin. Cartridges are dried with nitrogen gas, and then sorbed compounds are eluted with dichloromethane-diethyl ether (4:1) and determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 4 micrograms per liter averaged 74 percent ± 7 percent relative standard deviation for all method compounds. Initial method detection limits for single-component compounds (excluding hormones and sterols) averaged 0.15 microgram per liter. Samples are preserved by filtration, the addition of 60 grams NaCl, and storage at 4 degrees Celsius. The laboratory has established a sample-holding time (prior to sample extraction) of 14 days from the date of sample collection until a statistically accepted method can be used to determine the effectiveness of these sample-preservation procedures.

Version 1.1

Posted October 2007

Suggested citation:

Zaugg, S.D., Smith, S.G., Schroeder, M.P., Barber, L.B., and Burkhardt, M.R., 2007, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of wastewater compounds by polystyrene-divinylbenzene solid-phase extraction and capillary-column gas chromatography/mass spectrometry: U.S. Geological Survey Water-Resources Investigations Report 01-4186, 37 p.




Analytical Method

1. Scope and application

2. Summary of method

3. Interferences

4. Apparatus and instrumentation

5. Reagents and consumable materials

6. Standards

7. Procedure

8. Safety precautions and waste disposal

9. Gas chromatograph/mass spectrometer performance

9.1 Gas chromatograph performace evaluation

9.2 Mass spectrometer performace evaluation

10. Calibration

11. Quality assurance and quality control

12. Calculation of results

12.1 Qualitative identification

12.2 Quantitation

12.3 Reporting results

Method performance

Sample preservaton and holding times


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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