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Method Validation for SPE Applied to Determination of PAH in Petroliferous Industry Effluent Water

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DOI: 10.4236/ajac.2011.28113    5,595 Downloads   9,762 Views   Citations

ABSTRACT

The presence of polycyclic aromatic hydrocarbons (PAH) in produced water is of environmental concern due to their toxic properties. PAH analysis in complex samples requires pre-treatment to enrich the fraction con- taining analytes, and eliminate matrix interferences. The objective of this work was to develop and validate an analytical methodology for determination of PAH in produced water, using solid phase extraction (SPE) and analysis by gas chromatography with flame ionization detection (GC-FID). Average recoveries of PAH from produced water enriched at two concentration levels varied from 30.9% for naphthalene to 119.1% for chrysene (RSD between 3.8% and 22.2%). The linear range was between 0.5 and 50.0 µg?mL–1, with regres- sion coefficients better than 0.998. Detection limits were between 0.01 and 0.04 µg?L–1, and quantitation lim- its were between 0.05 and 0.16 µg?L–1. The validated method was applied to samples of produced water treated for disposal, in which concentrations varied from 3.5 µg?L–1 for phenanthrene to 44.3 µg?L–1 for naphthalene ( = 177.7 μg?L–1). The method was also applied to seawater samples, in which 13 PAH compounds were detected ( = 60.27 μg?L–1), probably derived from pyrogenic sources.

Conflicts of Interest

The authors declare no conflicts of interest.

Cite this paper

J. Bispo, S. Navickiene and H. Dórea, "Method Validation for SPE Applied to Determination of PAH in Petroliferous Industry Effluent Water," American Journal of Analytical Chemistry, Vol. 2 No. 8, 2011, pp. 971-978. doi: 10.4236/ajac.2011.28113.

References

[1] H. S. Dórea, J. R. L. Bispo, K. A. S. Arag?o, B. B. Cunha, S. Navickiene, J. P. H. Alves, L. P. C. Rom?o and C. A. B. Garcia, “Analysis of BTEX, PAHs and Metals in the Oilfield Produced Water in the State of Sergipe, Brazil,” Microchemical Journal, Vol. 85, No. 2, 2007, pp. 234- 238. doi:10.1016/j.microc.2006.06.002
[2] A. Gaujac, E. S. Emídio, S. Navickiene, S. L. C. Ferreira and H. S. Dórea, “Multivariate Optimization of a Solid Phase Microextraction-Headspace Procedure for the Determination of Benzene, Toluene, Ethylbenzene and Xylenes in Effluent Samples from a Waste Treatment Plant,” Journal of Chromatography A, Vol. 1203, No. 1, 2008, pp. 99-104. doi:10.1016/j.chroma.2008.06.022
[3] E. Barbieri, C. A. B. Garcia, J. R. L. Bispo, K. A. S. Arag?o, J. P. H. Alves and H. S. Dórea, “Utiliza??o do Camar?o Sete. Barbas (Xiphopenaeus Kroyeri) na Determina??o da Toxicidade da água de Produ??o de Petróleo Caracterizada no Estado de Sergipe,” O Mundo da Saúde, Vol. 28, No. 4, 2004, p. 421.
[4] J. P. Ray and F. R. Engelhardt, “Produced Water: Technological Environmental Issues and Solutions,” Plenum Press, New York, 1992.
[5] A. H. Neilson, “PAHs and Related Compounds, Chemistry,” Springer, New York, 1998.
[6] A. Filipkowska, L. Lubecki and G. Kowalewska, “Polycyclic Aromatic Hydrocarbon Analysis in Different Matrices of the Marine Environment,” Analytica Chimica Acta, No. 547, No. 2, 2005, pp. 243-254. doi:10.1016/j.aca.2005.05.023
[7] R. M. Higashi, G. N. Cherr, C. A. Bergens and T. W.-M. Fan, “Produced Water: Technological Environmental Issues and Solutions,” Plenum Press, New York, 1992.
[8] Y. F. Song, X. Jing, S. Fleischmann and B. M. Wilke, “Comparative Study of Extraction Methods for the Determination of PAHs from Contaminated Soils and Sediments,” Chemosphere, Vol. 48, No. 9. 2002, pp. 993- 1001. doi:10.1016/S0045-6535(02)00180-7
[9] C. F. S. Filho, E. S. Emídio and H. S. Dórea, “Solid- Phase Microextraction for Determination of Anilino- Pyrimidine, Dimethylcarbamate and Thiadiazine Pesticides in Irrigation Project Surface Water,” The Journal of the Brazilian Chemical Society, Vol. 22, No. 7, 2011, p. 1371. doi:10.1590/S0103-50532011000700024
[10] T. F. Silva, D. A. Azevedo and F. R. Aquino Neto, “Distribution of Polycyclic Aromatic Hydrocarbons in Surface Sediments and Waters from Guanabara Bay, Rio de Janeiro,” The Journal of the Brazilian Chemical Society, Vol. 18, No. 3, 2007, p. 628. doi:10.1590/S0103-50532007000300021
[11] M. Toledo, F. M. Lan?as and E. Carrilho, “Solid-Phase Extraction of Nitro-PAH from Aquatic Samples and Its Separation by Reverse-Phase Capillary Liquid Chromato- graphy,” Journal of the Brazilian Chemical Society, Vol. 18, No. 5, 2007, p. 1004. doi:10.1590/S0103-50532007000500019
[12] R. M. Cavalcante, N. S. M. Filho, R. B. Viana, I. R. N. Oliveira and R. F. Nascimento, “Utilization of Solid- Phase Extraction (SPE) for the Determination of Poly- cyclic Aromatic Hydrocarbons in Environmental Aque- ous Matrices,” Química Nova, Vol. 30, No. 3, 2007, p. 560. doi:10.1590/S0100-40422007000300010
[13] R. Dong, S. Chang and Y. Sun, “Solid-Phase Micro- extraction for Determining the Distribution of Sixteen US Environmental Protection Agency Polycyclic Aromatic Hydrocarbons in Water Samples,” Journal of Chromatography A, Vol. 879, No. 2, 2000, pp. 177-188. doi:10.1016/S0021-9673(00)00347-2
[14] USEPA 3535, “Solid-Phase Extraction (SPE). Environ- mental Protection Agency. Test Methods On-Line,” 2011. http://www.epa.gov
[15] M. Thompson, S. L. R. Ellison and R. Wood, “Harmo- nized Guidelines for Single-Laboratory Validation of Methods of Analysis―(IUPAC Technical Report),” Pure and Applied Chemistry, Vol. 74, No. 5, 2002, pp. 835- 855. doi:10.1351/pac200274050835
[16] Instituto Nacional de Metrologia, Inmetro, Orienta??o Sobre Valida??o de Métodos Analíticos, Document: DOQ-CGC- RE-008, Version 03, 2010, p. 20. http://www.inmetro.gov.br/Sidoq/Arquivos/CGCRE/DOQ/DOQ-CGCRE-8_03.pdf
[17] M. Ribani, C. B. G. Bottoli, C. H. Collins, L. C. S. F. Jardim and L. F. C. Melo, “Validation for Chromatographic and Electrophoretic Methods,” Química Nova, Vol. 27, No. 5, 2004, p. 771. doi:10.1590/S0100-40422004000500017
[18] USEPA 8270, “Environmental Protection Agency. Test Methods On-Line,” 2011. http://www.epa.gov
[19] E. Martinez, M. Gros, S. Lacorte and D. Barceló, “Simplified Procedures for the Analysis of Polycyclic Aromatic Hydrocarbons in Water, Sediments and Mussels,” Journal of Chromatography A, Vol. 1047, No. 2, 2004, pp. 181-188. doi:10.1016/j.chroma.2004.07.003
[20] F. Barros, V. Hatje, M. B. Figueiredo, W. F. Magalh?es, H. S. Dórea and E. S. Emídio, “The Structure of the Benthic Macrofaunal Assemblages and Sediments Characteristics of the Paragua?u Estuarine System, NE, Brazil,” Estuarine, Coastal and Shelf Science, Vol. 78, No. 4, 2008, pp. 753-762. doi:10.1016/j.ecss.2008.02.016
[21] F. G. Prahl and R. Carpenter, “Polycyclic Aromatic Hydrocarbon (PAH)-Phase Associations in Washington Coastal Sediment,” Geochimica et Cosmochimica Acta, Vol. 47, No. 6, 1983, pp. 1013-1023. doi:10.1016/0016-7037(83)90231-4

  
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