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Optimization and validation of headspace solid-phase microextraction method coupled with gas chromatography–triple quadrupole tandem mass spectrometry for simultaneous determination of volatile and semi-volatile organic compounds in coking wastewater treatment plant

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Abstract

Industrial wastewater could be an important source for the emission of volatile (VOCs) and semi-volatile organic compounds (SVOCs), but little is known about it. In this study, a method for the identification and quantitation of 43 VOCs and SVOCs in coking wastewater was developed using a solvent-free equilibrium extraction method on the basis of headspace solid-phase microextraction accompanied by gas chromatography–triple quadrupole tandem mass spectrometry (HS-SPME-GC-MS/MS). To ensure good extraction efficiency, the parameters that have an effect on the HS-SPME-GC-MS/MS process were carefully optimized, in terms of fiber exposure time and temperature, pH, salt additives, sample volume, and desorption time. The HS-SPME method showed good linearity range with coefficients of determination (R2) ≥ 0.991 and achieving a satisfactory recoveries value (70–120%) with good relative standard deviations (RSDs) < 20% (precision). Furthermore, the purposed approach proved to be sensitive with low detection limits, where the values ranged from 0.03 to 3.01 μg/L. The real sample analysis result showed that 43 of VOCs and SVOCs were detected in raw coking wastewater, with 3-cresol as the dominant ones. Further, the method revealed that seven phenols, 11 polycyclic aromatic hydrocarbons, and five BTEX were detected even in the treated effluent. In conclusion, the HS-SPME method developed in this study is simple in sample preparation, convenient, sensitive, and could satisfy the requirement of the analysis of VOCs and SVOCs in coking wastewater.

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Funding

This work was partially supported by Chinese Academy of Sciences (Grant No. Y273). The first author (A.N. Saber) is financially supported by the CAS-TWAS president’s Fellowship for International Ph.D. Students (CAS-TWAS Fellowship No. 2017CTF086).

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Authors and Affiliations

  1. State Key Laboratory of Environmental Aquatic Chemistry, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, 100085, China

    Ayman N. Saber, Haifeng Zhang & Min Yang

  2. University of Chinese Academy of Sciences, Beijing, 100049, China

    Ayman N. Saber, Haifeng Zhang & Min Yang

  3. Pesticide Residues and Environmental Pollution Department, Central Agricultural Pesticide Laboratory, Agricultural Research Center, Dokki, Giza, 12618, Egypt

    Ayman N. Saber

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  1. Ayman N. Saber
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  2. Haifeng Zhang
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Correspondence to Min Yang.

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Saber, A.N., Zhang, H. & Yang, M. Optimization and validation of headspace solid-phase microextraction method coupled with gas chromatography–triple quadrupole tandem mass spectrometry for simultaneous determination of volatile and semi-volatile organic compounds in coking wastewater treatment plant. Environ Monit Assess 191, 411 (2019). https://doi.org/10.1007/s10661-019-7554-5

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