有序介孔碳固相微萃取涂层测定水中氯苯类有机污染物  

Ordered Mesoporous Carbon as Solid-phase Microextraction Coating for Determination of Some Chlorobenzenes in Water

作　　者：江明月[1] 李健生[1] 蒋慧[1] 齐俊文[1] 刘超[1] 王连军[1] 

机构地区：[1]南京理工大学环境与生物工程学院,南京210094

出　　处：《分析化学》2016年第1期1-7,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No.51478224)~~

摘　　要：采用溶剂挥发自组装结合提拉法,在石墨纤维表面制备有序介孔碳(Ordered nlesoporous cabon OMC)涂层,并开展其对水中氯苯类有机污染物的固相微萃取(SPME)测定。扫描电镜(SEM)结果显示,制备的OMC涂层完整与基体结合紧密,厚度约为7μm。透射电镜(TEM)、X射线衍射(XRD)和氮吸附脱附结果证实,OMC涂层具有规整二维六方特征,比表面积和孔容分别为369.7 m^2/g和0.28 cm^3/g。以氯苯类污染物为分析对象,采用顶空固相微萃取与氢火焰气相色谱联用法对OMC涂层的萃取性能进行全面的评价,优化萃取时间和温度、解吸时间、搅拌速率、离子强度及顶空体积等萃取条件,并与商品化涂层进行比对。结果表明最佳萃取条件为:萃取时间30 min萃取温度50℃,脱附时间2 min,盐浓度0.35 g/mL,顶空体积15 mL。在最佳萃取条件下,检出限在0.05~0.15μg/L之间;在1~1000μg/L线性范围内,线性关系良好;7次平行样测定的相对标准偏差为4.1%~6.4%。制备的OMC涂层的峰面积是商用聚二甲基硅氧烷/二乙烯基苯(Polydimethylsiloxane/divinylbenzene,PDMS/DVB)涂层的2倍,商用聚丙烯酸酯(Polyacrylate,PA)涂层的18倍。将此涂层应用于两种实际水样中,4种氯苯均未检出,添加浓度为20μg/L时,样品回收率分别为99.4%~114.5%和92.3%~97.0%。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 dipcoating 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 wellordered two dimensional hexagonal mesostructure with pore volume of 0.28 cm^3/g and BET surfaces of369.7 m^2/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 of0.35 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 of99.4%-114.5%and 92.3%-97.0%,respectively.

关 键 词：有序介孔碳 涂层 固相微萃取 氯苯 

分 类 号：X832[环境科学与工程—环境工程] O658.2[理学—分析化学]