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National Water Quality Laboratory

Saturday March 17, 2018

Techniques and Methods 5-B2

Determination of Wastewater Compounds in Sedment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

Mark R. Burkhardt, Steven D. Zaugg, Steven G. Smith, and Rhiannon C. ReVello

May 2005

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 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were 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, polycyclic aromatic hydrocarbons, and high-use domestic pesticides.

Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry.

Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent 13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the E remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance (greater than 25 percent relative standard deviation), (2) reference standards prepared from technical mixtures, or (3) potential blank contamination.

Samples were preserved by freezing to 20 degrees Celsius. The U.S. Geological Survey National Water Quality Laboratory has established a 1-year sample-holding time limit (prior to sample extraction) from the date of sample collection (if the sample is kept at 20C) until a statistically accepted method can be used to determine the effectiveness of the sample-freezing procedure.

This report is available on the USGS Publishing Network.

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