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Determination of BTEX Compounds by Dispersive Liquid–Liquid Microextraction with GC–FID

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Abstract

Rapid, inexpensive, and efficient sample-preparation by dispersive liquid–liquid microextraction (DLLME) then gas chromatography with flame ionization detection (GC–FID) have been used for extraction and analysis of BTEX compounds (benzene, toluene, ethylbenzene, and xylenes) in water samples. In this extraction method, a mixture of 25.0 μL carbon disulfide (extraction solvent) and 1.00 mL acetonitrile (disperser solvent) is rapidly injected, by means of a syringe, into a 5.00-mL water sample in a conical test tube. A cloudy solution is formed by dispersion of fine droplets of carbon disulfide in the sample solution. During subsequent centrifugation (5,000 rpm for 2.0 min) the fine droplets of carbon disulfide settle at the bottom of the tube. The effect of several conditions (type and volume of disperser solvent, type of extraction solvent, extraction time, etc.) on the performance of the sample-preparation step was carefully evaluated. Under the optimum conditions the enrichment factors and extraction recoveries were high, and ranged from 122–311 to 24.5–66.7%, respectively. A good linear range (0.2–100 μg L−1, i.e., three orders of magnitude; r 2 = 0.9991–0.9999) and good limits of detection (0.1–0.2 μg L−1) were obtained for most of the analytes. Relative standard deviations (RSD, %) for analysis of 5.0 μg L−1 BTEX compounds in water were in the range 0.9–6.4% (n = 5). Relative recovery from well and wastewater at spiked levels of 5.0 μg L−1 was 89–101% and 76–98%, respectively. Finally, the method was successfully used for preconcentration and analysis of BTEX compounds in different real water samples.

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Acknowledgments

Financial support from Iran University of Science and Technology is gratefully acknowledged. The authors thank Dr Khorasani and Dr Jalali Haravi for providing the capillary column.

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Authors and Affiliations

  1. Department of Analytical Chemistry, Faculty of Chemistry, Iran University of Science and Technology, Tehran, Iran

    Yaghoub Assadi, Fardin Ahmadi & Mohammad Reza Milani Hossieni

  2. Electroanalytical Chemistry Research Center, Iran University of Science and Technology, Tehran, Iran

    Yaghoub Assadi & Mohammad Reza Milani Hossieni

Authors
  1. Yaghoub Assadi
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  2. Fardin Ahmadi
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  3. Mohammad Reza Milani Hossieni
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Correspondence to Fardin Ahmadi.

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Assadi, Y., Ahmadi, F. & Hossieni, M.R.M. Determination of BTEX Compounds by Dispersive Liquid–Liquid Microextraction with GC–FID. Chroma 71, 1137–1141 (2010). https://doi.org/10.1365/s10337-010-1616-8

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