ZnO-聚丙烯腈基复合碳纳米纤维修饰电极测定Pb^(2+)  

ZnO-PAN Based Carbon Composite Fiber for the Detection of Trace Pb^(2+)

作　　者：陈梦妮[1] 周鑫[1] 卢圆圆[1] 杨健茂[2] 马小玉[1] 刘建允[1] 

机构地区：[1]东华大学环境科学与工程学院国家环境保护纺织污染防治工程技术中心,上海201620 [2]东华大学分析测试中心,上海201620

出　　处：《分析科学学报》2015年第6期751-756,共6页Journal of Analytical Science

基　　金：国家自然科学基金(No.21105009;21476047);电分析化学国家重点实验室开放课题(No.SKLEAC201205)

摘　　要：以ZnO与聚丙烯腈(PAN)的混合液为前驱液,利用静电纺丝技术制备ZnOPAN纳米纤维,经预氧化和碳化处理得到ZnO纳米粒子负载碳复合纳米纤维(ZnOCNF)。扫描电镜(SEM)表征结果显示,ZnO纳米粒子在CNF表面分散均匀,且随着ZnO含量增加,纤维变细而粗糙。ZnO-PAN的比例为5∶6时,仍能得到纤维丝。接触角测试表明随着ZnO含量提高,纤维表面的水润湿性逐渐提高。同时,成功制备了ZnO-CNF复合纳米纤维修饰玻碳电极(ZnO-CNF/GCE),循环伏安(CV)法及电化学阻抗结果证明复合物膜成功修饰。方波溶出伏安(SWV)法结果表明,该修饰电极对重金属离子Pb^(2+)有灵敏的响应。在优化条件下,Pb^(2+)的溶出峰电流与其浓度在4.8×10-10~4.8×10-7 mol/L范围内呈现良好的线性关系,检出限(S/N=3)为2.4×10-10 mol/L,电极抗干扰性强、稳定性好。利用该方法测定了实际水样中Pb^(2+),并与电感耦合等离子体-质谱法(ICP-MS)进行对比,结果一致。ZnO nanoparticle-containing carbon composite nanofiber（ZnO-CNF）was prepared by electrospinning ZnO-PAN precursor,followed by pre-oxidation and carbonization.Scanning electron microscopy（SEM）was used to characterize the surface morphology of the fiber.With increasing ZnO-content,the fiber became thin and rough.At the ZnO-PAN ratio of 5∶6,the obtained ZnO/CNF composite still maintained its good fiber structure.The wettability of the ZnO-CNF was studied by water contact angle test.The ZnO-CNF composite fiber was modified on a glassy carbon electrode by dip-coating.Cyclic voltammetry and electrochemical impedance analysis demonstrated the successful fabrication of ZnO-CNF modified electrode.Square wave stripping voltammetry（SWV）showed the sensitive response of the ZnO-CNF modified electrode to Pb^2＋.Under the optimized conditions,agood linear relationship between peak current and Pb^2＋ concentration was obtained in the range of 4.8×10-10-4.8×10-7 mol/L.The detection limit was 2.4×10-10 mol/L（S/N=3）.The ZnO-CNF modified electrode possessed a good stability and reproducibility.Pb ions in real sample were analyzed,and the result was in consistent with that of ICPMS test.

关 键 词：静电纺丝 ZNO纳米粒子 碳纤维 PB2+ 

分 类 号：O657.1[理学—分析化学]