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Quantification of BTEX in Soil by Headspace SPME–GC–MS Using Combined Standard Addition and Internal Standard Calibration

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Abstract

There is a great demand for simple, fast and accurate methods for quantification of volatile organic contaminants in soil samples. Solid-phase microextraction (SPME) has a huge potential for this purpose, but its application is limited by insufficient accuracy caused by a matrix effect. The aim of this research was to develop the method for BTEX quantification in soil using combined standard addition (SA) and internal standard (IS) calibration. Deuterated benzene (benzene-d6) was used as the internal standard for all analytes. The optimized method includes spiking replicate samples with different concentrations of BTEX standards and the same concentration of benzene-d6, equilibration of soil samples at 40 °C during 2 h, and SPME–GC–MS analysis. Precision and accuracy of IS and SA methods were compared on different soil matrices. Combined SA + IS method provided more precise calibration plots compared to the conventional SA calibration. The SA + IS calibration provided more precise and accurate results compared with a reference method based on solvent extraction followed by GC–MS when applied to BTEX quantification in real soil samples (spiked with diesel fuel and aged). Recoveries of BTEX from soil samples spiked with known concentrations of analytes using the developed method were in the range of 73–130% with RSD values less than 15% for all BTEX. The proposed simultaneous standard addition and internal standard approach can be advantageous and adopted for improved quantification of other toxic VOCs in soil.

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Acknowledgements

This work was conducted under the project 3661/GF4 “Development and implementation of “green” methods for determination of organic pollutants in soils” and Ph.D. project of Ms. Dina Orazbayeva both funded by the Ministry of Education and Science of Kazakhstan.

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Authors and Affiliations

  1. Faculty of Chemistry and Chemical Technology, Center of Physical Chemical Methods of Research and Analysis, Al-Farabi Kazakh National University, 96a Tole bi Street, lab. 101, 050012, Almaty, Kazakhstan

    Dina Orazbayeva, Bulat Kenessov, Dayana Nassyrova & Nadezhda V. Lyabukhova

  2. Department of Agricultural and Biosystems Engineering, Iowa State University, Ames, IA, 50011, USA

    Jacek A. Koziel

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  1. Dina Orazbayeva
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  2. Bulat Kenessov
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  3. Jacek A. Koziel
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  4. Dayana Nassyrova
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  5. Nadezhda V. Lyabukhova
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Correspondence to Bulat Kenessov.

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Orazbayeva, D., Kenessov, B., Koziel, J.A. et al. Quantification of BTEX in Soil by Headspace SPME–GC–MS Using Combined Standard Addition and Internal Standard Calibration. Chromatographia 80, 1249–1256 (2017). https://doi.org/10.1007/s10337-017-3340-0

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  • DOI: https://doi.org/10.1007/s10337-017-3340-0

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