基于有序介孔碳涂层的固相微萃取法测定水中多环芳烃  

Determination of polycyclic aromatic hydrocarbons in water using solidphase microextraction with ordered mesoporous carbon coating

作　　者：蒋慧[1,2] 李健生[1] 胡兴茹 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 [2]南通大学地理科学学院,南通226001

出　　处：《环境化学》2017年第6期1288-1294,共7页Environmental Chemistry

基　　金：国家自然科学基金(51478224)资助~~

摘　　要：采用溶剂挥发诱导自组装结合提拉法在不锈钢丝表面制备了以有序介孔碳(Ordered mesoporous carbon,OMC)为涂层的固相微萃取(Solid phrase microextraction,SPME)纤维,考察了该纤维的萃取效果和在高温下的稳定性,建立了水中多环芳烃(Polycyclic aromatic hydrocarbons,PAHs)污染物的固相微萃取测定分析方法.扫描电镜(Scanning electron microscopy,SEM)结果表明,制备的OMC涂层连续完整且与不锈钢基体紧密结合,厚度约为11μm.氮吸附脱附结果证明,涂层材料具有规整的二维六方特征,孔径集中分布在3.8 nm,比表面积和孔容分别为522 m^2·g^(-1)和0.36 cm3·g^(-1).以水中多环芳烃类污染物作为分析对象,采用固相微萃取与气相色谱联用法探讨了OMC涂层对多环芳烃类污染物的萃取效果,对萃取方式、萃取时间、萃取温度、搅拌速度等条件进行了优化,并与商品化涂层进行了对比.结果表明,采用直接固相微萃取方式,萃取时间30 min,萃取温度50℃,搅拌速率800 r·min-1萃取效率最高;在最佳萃取条件下,OMC涂层分析5种PAHs的检测限范围是0.004—0.012μg·L^(-1),定量限范围0.010—0.025μg·L^(-1);萘和苊在0.1—250μg·L^(-1)范围内,芴、荧蒽和芘在0.25—100μg·L^(-1)范围内线性关系良好;单根纤维相对标准偏差(RSD)为3.9%—7.4%,多根纤维相对标准偏差为6.7%—9.8%.自制OMC纤维在350℃高温热解析80次后萃取效率不变,且对PAHs的萃取效率优于商用聚二甲基硅氧烷/二乙烯基苯(Polydimethylsiloxane/divinylbenzene,PDMS/DVB)涂层.将自制纤维应用于两种实际水样的固相微萃取分析中,分别添加0.25μg·L^(-1)和100μg·L^(-1)的样品回收率分别为81.3%—92.8%和89.3%—108.8%.This work reports the preparation of ordered mesoporous carbon（OMC） film supported on stainless steel wires using solvent evaporation-induced self-assembly approach combined with dipcoating technique and its application in solid-phase microextraction（SPME） of polycyclic aromatic hydrocarbons（PAHs） in water samples. The extraction efficiency and the thermal stability of the OMC fiber were investigated. A SPME method based on the OMC coating for the analysis of PAHs inwater samples was established. Characterization results of N2adsorption-desorption and SEM showed the OMC film had a highly ordered mesostructure with a specific surface area of 522 m^2·g^-1and a pore volume of 0. 36 cm^3·g^-1. The film was dense and continuous with a thickness of 11μm. The OMC fiber showed high resistance under thermal conditions. Five PAHs were analyzed by the SPME method using the OMC fiber. The fiber showed wide linear ranges,low detection limits（0.004—0.012 μg·L^-1）,low quantify limits（0.010—0.025 μg·L^-1） and good repeatabilities（3.9%—7.4% for one fiber,6.7%—9.8% for fiber-to-fiber）. The extraction efficiency remained unchanged after 80 desorption at 350 ℃. Compared with commercial fibers,the new fiber presented significantly improved extraction efficiencies with good stability at high temperatures. Under the optimum conditions,the OMC fiber was successfully applied to detect five PAHs in two water samples and achieved satisfactory results with the recoveries of 81.3%—92.8% and 89.3%—108.8%

关 键 词：有序介孔碳 固相微萃取 多环芳烃 

分 类 号：X832[环境科学与工程—环境工程]