DOI:https://doi.org/10.3232/SJSS.2016.V6.N3.05

Development and optimization of headspace and headspace-solid phase microextraction for the determination of volatile fuel compounds in environmental samples

María Balseiro-Romero, Raquel Chaves-Padín, Carmen Monterroso

Abstract

The application of an effective and sensitive analytical method to determine soil contaminants is a crucial step in the monitoring and remediation processes. In the present work, we optimized the analysis of volatile organic compounds (VFOC) commonly present in fuel: oxygenates (FO-MTBE and ETBE-) and monoaromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene (BTEX). Headspace (HS) and headspace-solid phase microextraction (HS-SPME) were optimized in water samples, and validated for contaminated soils, using artificially spiked soils. Contaminants were identified and quantified by gas chromatography coupled to mass spectrometry (GC/MS). Matrix effect correction with surrogate standards resulted essential when analyzing soil samples, especially when the sample exerted a strong sorption on the contaminants.

Views: 597
Downloads PDF: 582

 

References


Arambarri I, Lasa M, García R, Millán E. 2004. Determination of fuel dialkyl ethers and BTEX in water using headspace solid-phase microextraction and gas chromatography–flame ionization detection. J Chromatogr A. 1033:193-203. http://www.sciencedirect.com/science/article/pii/S0021967304001347.

Arthur CL, Pawliszyn J. 1990. Solid phase microextraction with thermal desorption using fused silica optical fibers. Anal Chem. 62:2145-2148. http://pubs.acs.org/doi/abs/10.1021/ac00218a019.

Balseiro-Romero M, Monterroso C. 2013. A headspace-analysis approach to assess the sorption of fuel volatile compounds by soils. Soil Sci Soc Am J. 77:800-808. https://dl.sciencesocieties.org/publications/sssaj/abstracts/77/3/800.

Esteve-Turrillas FA, Armenta S, Garrigues S, Pastor A, de la Guardia M. 2007. Headspace–mass spectrometry determination of benzene, toluene and the mixture of ethylbenzene and xylene isomers in soil samples using chemometrics. Anal Chim Acta 587:89-96. http://www.sciencedirect.com/science/article/pii/S0003267007001377.

Ezquerro Ó, Ortiz G, Pons B, Tena MT. 2004. Determination of benzene, toluene, ethylbenzene and xylenes in soils by multiple headspace solid-phase microextraction. J Chromatogr A. 1035:17-22. http://www.sciencedirect.com/science/article/pii/S0021967304002304.

Flórez Menéndez JC, Fernández Sánchez ML, Sánchez Urı́a JE, Fernández Martı́nez E, Sanz-Medel A. 2000. Static headspace, solid-phase microextraction and headspace solid-phase microextraction for BTEX determination in aqueous samples by gas chromatography. Anal Chim Acta 415:9-20. http://www.sciencedirect.com/science/article/pii/S000326700000862X.

García Pinto C, Herrero Martín S, Pérez Pavón JL, Moreno Cordero B. 2011. A simplified quick, easy, cheap, effective, rugged and safe approach for the determination of trihalomethanes and benzene, toluene, ethylbenzene and xylenes in soil matrices by fast gas chromatography with mass spectrometry detection. Anal Chim Acta 689:129-136. http://www.sciencedirect.com/science/article/pii/S0003267011000857.

Hiatt MH. 2010. The role of internal standards and their interaction with soils impact accuracy of volatile organics determinations. Int J Environ Anal Chem. 90:591-604. https://cfpub.epa.gov/si/si_public_record_report.cfm?dirEntryId=205118&fed_org_id=770&SIType=PR&TIMSType=Journal&showCriteria=0&address=nerl&view=citation&sortBy=pubDateYear&count=100&dateBeginPublishedPresented=.

Llompart M, Li K, Fingas M. 1999. Headspace solid phase microextraction (HSSPME) for the determination of volatile and semivolatile pollutants in soils. Talanta 48:451-459. http://www.sciencedirect.com/science/article/pii/S003991409800263X.

Louch D, Motlagh S, Pawliszyn J. 1992. Dynamics of organic compound extraction from water using liquid-coated fused silica fibers. Anal Chem. 64:1187-1199. http://pubs.acs.org/doi/abs/10.1021/ac00034a020.

Pavón JLP, Martín SH, Pinto CG, Cordero BM. 2009. Programmed temperature vaporizer based method for the sensitive determination of trihalomethanes and benzene, toluene, ethylbenzene and xylenes in soils. J Chromatogr A. 1216:6063-6070. http://www.sciencedirect.com/science/article/pii/S0021967309009558.

Rosell M, Lacorte S, Barceló D. 2006. Simultaneous determination of methyl tert-butyl ether, its degradation products and other gasoline additives in soil samples by closed-system purge-and-trap gas chromatography-mass spectrometry. J Chromatogr A. 1132:28-38. http://www.sciencedirect.com/science/article/pii/S0021967306014580.

United States Environmental Protection Agency (USEPA). 2003. Method 5021A: Volatile organic compounds in various sample matrices using equilibrium headspace analysis. Revision 1. Washington: US Environmental Protection Agency.

Zhang Z, Pawliszyn J. 1993. Analysis of organic compounds in environmental samples by headspace solid phase microextraction. J High Res Chromatogr. 16:689-692. http://onlinelibrary.wiley.com/doi/10.1002/jhrc.1240161203/abstract.





With the patronage of
Universia
Avda. de Cantabria, s/n - 28660, Boadilla del Monte
Madrid, España