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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

Saber, Ayman N., Zhang, Haifeng, Yang, Min
Environmental monitoring and assessment 2019 v.191 no.7 pp. 411
BTEX (benzene, toluene, ethylbenzene, xylene), additives, desorption, detection limit, exposure duration, gas chromatography-mass spectrometry, headspace analysis, industrial wastewater, pH, phenols, polycyclic aromatic hydrocarbons, solid phase microextraction, standard deviation, tandem mass spectrometry, temperature, volatile organic compounds, wastewater treatment
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.