Jiangsu Key Laboratory of Chemical Pollution Control and Resources Reuse, School of Environmental Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094, PR China; School of Geography Science, Nantong University, Nantong 226001, PR China.
Jiangsu Key Laboratory of Chemical Pollution Control and Resources Reuse, School of Environmental Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094, PR China.
Anal Chim Acta. 2015 Aug 12;888:85-93. doi: 10.1016/j.aca.2015.06.055. Epub 2015 Aug 10.
The present work reports preparation of ordered mesoporous carbon (OMC) film supported on a graphite fiber as a new type of solid-phase microextraction (SPME) fiber for determination of benzene series from aqueous media. The strategy for the supported OMC film preparation was combined dip-coating technology with solvent evaporation-induced self-assembly (EISA) approach. A graphite fiber was immersed in an ethanol solution containing phenolic resin and Pluronic triblock copolymer. Upon solvent evaporation and subsequent pyrolysis under 700 °C, the phenolic resin and the surfactant self-assembled on the surface of the graphite fiber to form smooth OMC film. X-ray diffraction (XRD), transmission electron microscopy (TEM) and nitrogen isothermal adsorption results indicate that the resultant OMC film possesses well-ordered two dimensional hexagonal mesostructure with pore diameters of 4.5 nm and BET surfaces of 630 m(2)/g. Scanning electron microscopy (SEM) studies show the supported OMC film with thickness at 8.5 μm is continuous and defect-free. The SPME efficiency of the OMC fiber was evaluated by analysis of five benzene series (benzene, toluene, ethylbenzene, p-xylene and m-xylene) from water samples by gas chromatography-flame ionization detection (GC-FID). The analysis results indicate that the prepared OMC fiber has wide linear ranges (0.5-500 μg/L), low detection limits (0.01-0.05 μg/L) and good repeatabilities (4.0-5.8% for one fiber, 2.9-8.7% for fiber-to-fiber). Compared with commercial counterparts, the OMC fiber exhibits improved extraction efficiency for benzene series and PAHs.
本工作报道了一种新型固相微萃取（SPME）纤维，即有序介孔碳（OMC）膜负载在石墨纤维上，用于从水介质中测定苯系物。OMC 膜负载的制备策略是将浸涂技术与溶剂挥发诱导自组装（EISA）方法相结合。将石墨纤维浸入含有酚醛树脂和 Pluronic 三嵌段共聚物的乙醇溶液中。在溶剂蒸发和随后在 700°C 下热解后，酚醛树脂和表面活性剂在石墨纤维表面自组装形成光滑的 OMC 膜。X 射线衍射（XRD）、透射电子显微镜（TEM）和氮气等温吸附结果表明，所得 OMC 膜具有良好有序的二维六方介孔结构，孔径为 4.5nm，BET 比表面积为 630m2/g。扫描电子显微镜（SEM）研究表明，负载的 OMC 膜厚度为 8.5μm，连续且无缺陷。通过气相色谱-火焰离子化检测（GC-FID）分析水样中的五种苯系物（苯、甲苯、乙苯、对二甲苯和间二甲苯），评价了 OMC 纤维的 SPME 效率。分析结果表明，所制备的 OMC 纤维具有较宽的线性范围（0.5-500μg/L）、较低的检测限（0.01-0.05μg/L）和良好的重现性（一根纤维为 4.0-5.8%，纤维间为 2.9-8.7%）。与商业产品相比，OMC 纤维对苯系物和 PAHs 的萃取效率更高。
