Citation: JIANG Ming-Yue, LI Jian-Sheng, JIANG Hui, QI Jun-Wen, LIU Chao, WANG Lian-Jun. Ordered Mesoporous Carbon as Solid-phase Microextraction Coating for Determination of Some Chlorobenzenes in Water[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(1): 1-7. doi: 10.11895/j.issn.0253-3820.150564
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A novel ordered mesoporous carbon (OMC) coating supported on graphite fiber for solid phase microextraction (SPME) was prepared by combining evaporation-induced self-assembly process with dip-coating method for determination of chlorobenzenes in aqueous media. Scanning electron microscopy (SEM) studies showed that the obtained OMC film was defect free and well integrated with the substrate. The thickness of the film was about 7.0 μm. Transmission electron microscopy (TEM), X-ray diffraction (XRD), and nitrogen isothermal adsorption results indicated that the resultant OMC film possessed well-ordered two dimensional hexagonal mesostructure with pore volume of 0.28 cm3/g and BET surfaces of 369.7 m2/g. The SPME performance of the OMC coating was evaluated by analysis of four kinds of chlorobenzenes from water samples with gas chromatography-flame ionization detection (GC-FID). The analysis conditions, including extraction time and temperature, desorption time, stirring rate, ionic strength and headspace volume, were optimized. Moreover, the SPME performance home-made coating was compared with the commercial coatings. The analysis results indicated that the optimum extraction conditions were extraction time of 30 min, extraction temperature of 50℃, desorption time of 2 min, ionic strength of 0.35 g/mL, headspace volume of 15 mL. The prepared OMC fiber demonstrated wide linear ranges (1-1000 μg/L) and low detection limits (0.05-0.15 μg/L) under the optimal conditions. The relative standard deviations were 4.1%-6.4% for seven parallel samples. The peak areas of the OMC coating were 2 times more than those of polydimethylsiloxane/divinylbenzene (PDMS/DVB) coating and 18 times those of more than polyacrylate (PA) coating. The OMC coating was applied to analysis of two real water, and four chlorobenzenes were not detected. The recoveries of two samples spiked at 20 μg/L were in the range of 99.4%-114.5% and 92.3%-97.0%, respectively.
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