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Determination of Semivolatile Organic Compounds and Polycyclic Aromatic Hydrocarbons in Solids by Gas Chromatography/Mass Spectrometry

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Determination of Semivolatile Organic Compounds and Polycyclic Aromatic Hydrocarbons in Solids by Gas Chromatography/Mass Spectrometry Prepared by the U.S. Geological Survey Office of Water Quality, National Water Quality Laboratory Determination of Semivolatile Organic Compounds and Polycyclic Aromatic Hydrocarbons in Solids by Gas Chromatography/Mass Spectrometry Techniques and Methods 5–B3 U.S. Department of the Interior U.S. Geological Survey Determination of Semivolatile Organic Compounds and Polycyclic Aromatic Hydrocarbons in Solids by Gas Chromatography/Mass Spectrometry By Steven D. Zaugg, Mark R. Burkhardt, Teresa L. Burbank, Mary C. Olson, Jana L. Iverson, and Michael P. Schroeder Chapter 3 Section B, Methods of the National Water Quality Laboratory Book 5, Laboratory Analysis Techniques and Methods 5–B3 U.S. Department of the Interior U.S. Geological Survey U.S. Department of the Interior Dirk Kempthorne, Secretary U.S. Geological Survey P. Patrick Leahy, Acting Director U.S. Geological Survey, Reston, Virginia: 2006 For product and ordering information: World Wide Web: http://www.usgs.gov/pubprod Telephone: 1-888-ASK-USGS For more information on the USGS—the Federal source for science about the Earth, its natural and living resources, natural hazards, and the environment: World Wide Web: http://www.usgs.gov Telephone: 1-888-ASK-USGS Any use of trade, product, or firm names is for descriptive purposes only and does not imply endorsement by the U.S. Government. Although this report is in the public domain, permission must be secured from the individual copyright owners to reproduce any copyrighted materials contained within this report. Suggested citation: Zaugg, S.D., Burkhardt, M.R., Burbank, T.L., Olson, M.C., Iverson, J.L., and Schroeder, M.P., 2006, Determination of semivolatile organic compounds and polycyclic aromatic hydrocarbons in solids by gas chromatography/mass spec- trometry: U.S. Geological Survey Techniques and Methods, book 5, chap. B3, 44 p. iii Contents Abstract ...........................................................................................................................................................1 Introduction.....................................................................................................................................................1 Purpose and Scope .......................................................................................................................................3 Analytical Method..........................................................................................................................................4 1. Scope and Application ..............................................................................................................4 2. Summary of Method ...................................................................................................................5 3. Safety Precautions and Waste Disposal ................................................................................5 4. Interferences ...............................................................................................................................5 5. Apparatus and Equipment.........................................................................................................5 6. Reagents and Consumable Materials .....................................................................................6 7. Sample Preparation Procedure ...............................................................................................8 8. Instrumental Analysis ..............................................................................................................12 9. Calculation and Reporting of Results ....................................................................................17 10. Quality Assurance and Quality Control .................................................................................18 11. Results and Discussion of Method Validation .....................................................................19 Summary and Conclusions .........................................................................................................................40 References Cited..........................................................................................................................................42 Glossary .........................................................................................................................................................44 Figures 1–2. Photographs showing: 1. Solid-phase extraction assembly for accelerated solvent extracts for use in determining semivolatile organic compounds and polycyclic aromatic hydrocarbons. ......................................................................................................................11 2. Solid-phase elution module assembly used in the analytical method for deter- mining semivolatile organic compounds and polycyclic aromatic hydrocarbons. ......................................................................................................................12 3. Graph showing least squares regression plots for concentrations of naphthalene (A) and benzo[a]pyrene (B) determined in 28 sediment samples by accelerated solvent extraction (ASE) and by Soxhlet extraction. ............................................................40 4. Boxplot showing results for analysis of 28 environmental soil and sediment samples. .......................................................................................................................................41 Tables 1. Semivolatile and polycyclic aromatic hydrocarbon compounds determined using this method. ...................................................................................................................................3 2. Alkylated polycyclic aromatic hydrocarbon homolog groups determined using this method and reported with estimated concentrations. ...........................................................4 3. An example of an accelerated solvent extraction (ASE) schedule for 13 cells. ................9 iv Tables—Continued 4. An example of an accelerated solvent extraction (ASE) method for a 120°C extraction. ....................................................................................................................................10 5. Retention times, relative retention times, gas chromatography/mass spectrometry quantitation ions, confirmation ions, and percent relative abundance of confirmation ions for individual method compounds and alkylated polycyclic aromatic hydrocarbon homolog groups. ................................................................................13 6. Gas chromatography/mass spectrometry analytical sequence suggested for use with this method. .........................................................................................................................16 7. Compounds with relative response factors used for the quantitation of alkylated polycyclic aromatic hydrocarbon homolog groups. .............................................................18 8. Semivolatile and polycyclic aromatic hydrocarbon compounds detected in unfortified reagent-sand, stream-sediment, and topsoil samples. ....................................20 9. Polycyclic aromatic hydocarbon and semivolatile compound mean bias and precision of spike recovery data for nine replicates with compounds spiked at 15 micrograms per sample in reagent-sand, stream-sediment, and topsoil samples. .......................................................................................................................................21 10. Polycyclic aromatic hydrocarbons and semivolatile compound mean bias and precision of spike recovery data for nine replicates with compounds spiked at 1.5 micrograms per sample in reagent-sand, stream-sediment, and topsoil samples. .......................................................................................................................................22 11. Mean bias and precision of spike recovery data for nine replicates with compounds spiked at 1.5 and 15 micrograms per sample in reagent-sand, stream-sediment, and topsoil samples for compounds that are not included in this method. .........................................................................................................................................24 12. Initial method detection limits calculated from the precision data reported in table 10 for the nine replicate reagent-sand samples spiked at 60 micrograms per kilogram per compound. ............................................................................................................25 13. Concentrations certified by the National Institute of Standards and Technology for Standard Reference Material 1944 determined by Soxhlet extraction and this method. .........................................................................................................................................27 14. Concentrations of alkylated homolog groups detected in Standard Reference Material 1944 determined by Soxhlet extraction and this method, but not reported by the National Institute of Standards and Technology. ......................................................28 15. Replicate environmental sample results, in micrograms per kilogram, using accelerated solvent extraction. ...............................................................................................29 16. Mean average deviation and range of average deviations for compounds detected in nine duplicate sediment samples and one triplicate sample extracted using accelerated
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