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Environmental Monitoring and Assessment

, Volume 184, Issue 5, pp 2893–2907 | Cite as

HS-SPME/GC–MS analysis of volatile and semi-volatile organic compounds emitted from municipal sewage sludge

  • Urszula KotowskaEmail author
  • Maciej Żalikowski
  • Valery A. Isidorov
Open Access
Article

Abstract

The aim of the research involved identification and semi-quantitative determination of unknown volatile and semi-volatile organic compounds emitted to air by sewage sludge formed in the process of municipal wastewater treatment in a sewage treatment plant. Samples taken directly after completion of the technological process as well as the sludge stored on the premise of the sewage treatment plant were analyzed. A simple method using off-line headspace solid-phase microextraction combined with gas chromatography–mass spectrometry has been proposed for extraction and detection of organic pollutants. For reliable identification of compounds, combination of two independent parameters: mass spectra and linear temperature programmed retention indices were employed. Over 170 compounds of different structure were identified including aliphatic and aromatic hydrocarbons, alcohols, esters, carbonyls, as well as sulfur, nitrogen, and chlorine containing compounds. The prevailing substances included: ethyl ether, n-hexane, p-xylene, o-xylene, mesitylene, m-ethylbenzene, limonene, n-decane, n-undecane, and n-dodecane. A few compounds such as methanetiol, dimethyl polisulfide, octaatomic sulfur, phthalic anhydride, and indoles were identified in the sludge for the first time.

Keywords

Sewage sludge Organic compounds HS-SPME GC–MS 

References

  1. Adams, R. P. (1995). Identification of essential oil components by GC/MS. Carol Stream (IL): Allured.Google Scholar
  2. Arcadi, R., Costa, C., & Imperatore, C. (1998). Oral toxicity of DEHP during pregnancy and sucking in the long-evans rat. Food and Chemical Toxicology, 36, 963–974.CrossRefGoogle Scholar
  3. Arthur, C. L., & Pawliszyn, J. (1990). Solid phase microextraction with thermal desorption using fused silica optical fibers. Analytical Chemistry, 62, 2145–2148.CrossRefGoogle Scholar
  4. ASTM (1998). ASTMD6169: Standard practice for selection of sorbents, sampling and thermal desorption analysis procedures for volatile organic chemicals in air. West Conshohocken: ASTM.Google Scholar
  5. Basheer, C., & Lee, H. K. (2004). Hollow fiber membrane-protected solid-phase microextraction of triazine herbicides in bovine milk and sewage sludge samples. Journal of Chromatography A, 1047, 189–194.Google Scholar
  6. Blount, B. C., Kobelski, R. J., McElprang, D. O., Ashley, D. L., Morrow, J. C., Chambers, D. M., et al. (2006). Quantification of 31 volatile organic compounds in whole blood using solid-phase microextraction and gas chromatography–mass spectrometry. Journal of Chromatography B, 832, 292–301.CrossRefGoogle Scholar
  7. Bravo-Linares, C. M., Mudge, S. M., & Loyola-Sepulveda, R. H. (2007). Occurrence of volatile organic compounds (VOCs) in Liverpool Bay, Irish Sea. Marine Pollution Bulletin, 54(11), 1742–1753.CrossRefGoogle Scholar
  8. Cai, Q.-Y., Mo, C.-H., Wu, Q.-T., Zeng, Q.-Y., & Katsoyiannis A. (2007) Occurrence of organic contaminants in sewage sludges from eleven wastewater treatment plants, China. Chemosphere, 68, 1751–1762.CrossRefGoogle Scholar
  9. de Zeeuw, R. A., Franke, J. P., Maurer, H. H., & Pfleger, K. (1992). Gas chromatographic retention indices of toxicologically relevant substances on packed or capillary columns with dimethylsillicone stationary phases (2nd ed.). Weinheim: VCH Verlag.Google Scholar
  10. Domeño, C., Martínez-García, F., Campo, L., & Nerín, C. (2004). Sampling and analysis of volatile organic pollutants emitted by an industrial stack. Analytica Chimica Acta, 524, 51–62.CrossRefGoogle Scholar
  11. Eitzer, B. D. (1995). Emissions of volatile organic chemicals from municipal solid waste composting facilities. Environmental Science and Technology, 29, 896–902.CrossRefGoogle Scholar
  12. Escalasa, L., Guadayola, J. M., Cortinab, M., Riverab, L., & Caixach, J. (2003). Time and space patterns of volatile organic compounds in a sewage treatment plant. Water Research, 37, 3913–3920.CrossRefGoogle Scholar
  13. Fang, J., Lovanh, N., & Alvarez, P. J. (2004). The use of isotopic and lipid analysis techniques linking toluene degradation to specific microorganisms: Applications and limitations. Water Research, 38, 2529–2536.CrossRefGoogle Scholar
  14. Gu, Y.-Q., Mo, M.-H., Zhou, J. P., Zou, C. S., & Zhang, K. Q. (2007). Evaluation and identification of potential organic nematicidal volatiles from soil bacteria. Soil Biology and Biochemistry, 39(10), 2567–2575.CrossRefGoogle Scholar
  15. Harrison, E. Z., Oakes, S. R., Hysell, M., & Hay, A. (2006). Organic chemicals in sewage sludges. Science of the Total Environment, 367, 481–497.CrossRefGoogle Scholar
  16. Hippelein, M. (2006). Analysing selected VVOCs in indoor air with solid phase microextraction (SPME): A case study. Chemosphere, 65, 271–277.CrossRefGoogle Scholar
  17. Isidorov, V. A., Kotowska, U., & Vinogorova, V. T. (2005a). GC identification of organic compounds based on partition coefficients of their TMS derivatives in a hexane-acetonitrile system and retention indices. Analytical Sciences, 21, 483–489.CrossRefGoogle Scholar
  18. Isidorov, V., Vinogorova, V., & Rafałowski, K. (2005b). Gas chromatographic determination of extractable compounds composition and emission rate of volatile terpenes from larch needle litter. Journal of Atmospheric Chemistry, 50(3), 263–273.CrossRefGoogle Scholar
  19. ISO (2000). ISO EN 16017–1: Air quality—sampling and analysis of volatile organic compounds in ambient air, indoor air and workplace air by sorbent tube/thermal desorption/capillary gas chromatography. Part 1: Pumped sampling.Google Scholar
  20. ISO (2003). ISO EN 16017-2: Air quality—sampling and analysis of volatile organic compounds in ambient air, indoor air and workplace air by sorbent tube/thermal desorption/capillary gas chromatography. Part 2: Diffusive sampling.Google Scholar
  21. Janssen, A., Ma, S., Lens, P., & Lettinga, G. (1997). Performance of a sulfide-oxidizing expanded-bed reactor supplied with dissolved oxygen. Biotechnology and Bioengineering, 53, 32–40.CrossRefGoogle Scholar
  22. Jönsson, S., Gustavsson, L., & van Bavel, B. (2007). Analysis of nitroaromatic compounds in complex samples using solid-phase microextraction and isotope dilution quantification gas chromatography–electron-capture negative ionisation mass spectrometry. Journal of Chromatography A, 1164, 65–73.CrossRefGoogle Scholar
  23. Kim, K.-H., Choi, Y. J., Jeon, E. C., & Sunwoo, Y. (2005). Characterization of malodorous sulfur compounds in landfill gas. Atmospheric Environment, 39, 1103–1112.CrossRefGoogle Scholar
  24. Koe, L. C. C., & Shen, W. (1997). High resolution GC–MS analysis of VOCs in wastewater and sludge. Environmental Monitoring and Assessment, 44, 549–561.CrossRefGoogle Scholar
  25. Llompart, M., García-Jares, C., Salgado, C., Polo, M., & Cela R. (2003). Determination of musk compounds in sewage treatment plant sludge samples by solid-phase microextraction. Journal of Chromatography A, 999, 185–193.CrossRefGoogle Scholar
  26. Llop, A., Borrull, F., & Pocurull, E. (2010). Pressurised hot water extraction followed by simultaneous derivatization and headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry for the determination of aliphatic primary amines in sewage sludge. Analytica Chimica Acta, 665, 231–236.CrossRefGoogle Scholar
  27. Lu, R., Wu, J., Turco, R. P., Winer, A. M., Atkinson, R., Arey, J., et al. (2005). Naphthalene distributions and human exposure in Southern California. Atmospheric Environment, 39, 489–507.CrossRefGoogle Scholar
  28. Mangani, G., Berloni, A., & Maione, M. (2003). “Cold” solid-phase microextraction method for the determination of volatile halocarbons present in the atmosphere at ultra-trace levels. Journal of Chromatography A, 988, 167–175.CrossRefGoogle Scholar
  29. Matysik, S., Herbarth, O., & Mueller, A. (2009) Determination of microbial volatile organic compounds (MVOCs) by passive sampling onto charcoal sorbents. Chemosphere, 76, 114–119.CrossRefGoogle Scholar
  30. NSAI (2011). prEN 13649: Stationary source emissions—determination of the mass concentration of individual gaseous organic compounds—test methods. Dublin: NSAI.Google Scholar
  31. Pagans, E., Front, X., & Sanchez A. (2006). Emission of volatile organic compounds from composting of different solid wastes: Abatement by biofiltration. Journal of Hazardous Materials, 131, 179–186.CrossRefGoogle Scholar
  32. Parke, D. V., & Lewis, D. F. (1992). Safety aspects of food preservatives. Food Additives and Contaminants, 9(5), 561–577.CrossRefGoogle Scholar
  33. Pawliszyn, J. (1997). Solid-phase microextraction, theory and practice. New York: Wiley.Google Scholar
  34. Pawliszyn, J., & Liu, S. (1987). Sample introduction for capillary gas chromatography with laser desorption and optical fibers. Analytical Chemistry, 59, 1475–1478.CrossRefGoogle Scholar
  35. Sadtler Research Laboratory (1986). Standard GC retention index library. Philadelphia: Sadtler Research Laboratory.Google Scholar
  36. Safer, A. M., & al-Nughamish, A. J. (1999). Hepatotoxicity induced by the anti-oxidant food additive, butylated hydroxytoluene (BHT), in rats: An electron microscopical study. Histology and Histopathology, 14, 391–406.Google Scholar
  37. Simonich, S. L., Begley, W. M., Debaere, G., & Eckhoff, W. S. (2000). Trace analysis of fragrance materials in wastewater and treated wastewater. Environmental Science and Technology, 34, 959–965.CrossRefGoogle Scholar
  38. Spinhirne, J. P., Koziel, J. A., & Chirase, N. K. (2004). Sampling and analysis of volatile organic compounds in bovine breath by solid-phase microextraction and gas chromatography–mass spectrometry. Journal of Chromatography A, 1025, 63–69.CrossRefGoogle Scholar
  39. Tryphonas, H., Lacroix, F., Lok, E., Jee, P. D., Clayson, B., Hayward, S., et al. (1999). The effect of butylated hydroxytoluene on selected immune surveillance parameters in rats bearing enzyme-altered hepatic preneoplastic lesions. Food and Chemical Toxicology, 37(7), 671–681.CrossRefGoogle Scholar
  40. US EPA (1996). US EPA Method 5041a: Desorption and analysis of sorbent cartridges from volatile organic sampling train (VOST). Washington, DC: US EPA.Google Scholar
  41. Van den Dool, H., & Kratz, P. (1963). A generalization of retention index system including linear temperature programmed gas-liquid partition chromatography. Journal of Chromatography, 11, 463–471.CrossRefGoogle Scholar
  42. Van Durme, G. P., McNamara, B. F., & McGinley, C. M. (1992). Bench-scale removal of odor and volatile organic compounds at a composting facility. Water Environment Research, 64, 19–27.CrossRefGoogle Scholar
  43. Villaverde, M. L., Juárez, M. P., & Mijailovsky, S. (2007). Detection of Tribolium castaneum (Herbst) volatile defensive secretions by solid phase microextraction–capillary gas chromatography (SPME-CGC). Journal of Stored Products Research, 43(4), 540–545.CrossRefGoogle Scholar
  44. Webber, M. D., Rogers, H. R., Watts, C. D., Boxall, A. B. A., Davis, R. D., & Scoffin, R. (1996). Monitoring and prioritisation of organic contaminants in sewage sludges using specific chemical analysis and predictive, non-analytical methods. Science of the Total Environment, 185, 27–44.CrossRefGoogle Scholar
  45. Wilson, S. C., Duarte-Davidson, R., & Jones, K. C. (1996a). Screening the environmental fate of organic contaminants in sewage sludges applied to agricultural soils: 1. The potential for downward movement to groundwaters. Science of the Total Environment, 185, 45–57.CrossRefGoogle Scholar
  46. Wilson, S. C., Duckham, C., & Jones, K. C. (1996b). Quantification of volatile organic compound losses from sludge amended soil: A pilot scale study. Chemosphere, 33, 1261–1272.CrossRefGoogle Scholar
  47. Woolfenden, E. (2010a). Sorbent-based sampling methods for volatile and semi-volatile organic compounds in air. Part 1: Sorbent-based air monitoring options. Journal of Chromatography A, 1217, 2674–2684.CrossRefGoogle Scholar
  48. Woolfenden, E. (2010b). Sorbent-based sampling methods for volatile and semi-volatile organic compounds in air. Part 2: Sorbent-based air monitoring options. Journal of Chromatography A, 1217, 2685–2694.CrossRefGoogle Scholar
  49. Wu, S.-F., & Ding, W.-H. (2010) Fast determination of synthetic polycyclic musks in sewage sludge and sediments by microwave-assisted headspace solid-phase microextraction and gas chromatography–mass spectrometry. Journal of Chromatography A, 1217, 2776–2781.CrossRefGoogle Scholar
  50. Wu, B.-Z., Feng, T.-Z., Sree, U., Chiu, K.-H., & Lo, J.-G. (2006). Sampling and analysis of volatile organics emitted from wastewater treatment plant and drain system of an industrial science park. Analytica Chimica Acta, 576, 100–111.CrossRefGoogle Scholar
  51. Zeng, J., Chen, J., Chen, L., Wang, Y., Chen, W., Huang, X., et al. (2009). The extraction performance of methacrylic acid–trimethylolpropanetrimethacrylate solid-phase microextraction fibers in aqueous solutions. Analytica Chimica Acta, 648, 194–199.CrossRefGoogle Scholar

Copyright information

© The Author(s) 2011

Authors and Affiliations

  • Urszula Kotowska
    • 1
    Email author
  • Maciej Żalikowski
    • 1
  • Valery A. Isidorov
    • 1
  1. 1.Institute of ChemistryUniversity of BialystokBialystokPoland

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