静电纺ZnO/碳复合纳米纤维修饰电极制备及对痕量铅的测定  

Preparation of Electrospun ZnO-Carbon Composite Nanofiber Modified Electrodes for the Detection of Trace Lead

作　　者：周鑫[1] 杨健茂[2] 辛萌[1] 陈梦妮[1] 王兴[1] 刘建允[1] 

机构地区：[1]东华大学环境科学与工程学院,上海201620 [2]东华大学分析测试中心,上海201620

出　　处：《分析化学》2014年第7期985-990,共6页Chinese Journal of Analytical Chemistry

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

摘　　要：以ZnCl2与聚丙烯腈（ PAN）混合液为前驱液,利用静电纺丝技术制备ZnCl2-PAN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（ ZnO-CNF）。扫描电子显微镜（ SEM）显示,ZnO纳米粒子在CNF表面均匀分散,粒径为20~30 nm。接触角测试表明,ZnO的存在使纤维表面的润湿性明显改善。将ZnO-CNF复合纤维与Nafion在乙醇中均匀分散,采用滴涂法制备ZnO-CNF修饰玻碳电极,SEM及循环伏安（ CV）证明复合物膜的成功修饰。方波溶出伏安分析（ SWV）表明,此修饰电极对痕量铅有灵敏的选择性响应。通过实验条件优化,在0.1 mol/L HAc-NaAc （pH=4.6）缓冲溶液中,-1.0 V电位下富集10 min, Pb2＋溶出峰电流与其浓度在2.4×10-10~2.4×10-7 mol/L范围内呈良好的线性关系（R=0.9980）,检出限为4.8×10-11 mol/L,抗干扰性强,稳定性好。利用本方法测定了实际水样中铅的含量,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 the electrospinning of the ZnCl2-PAN precursor, followed by preoxidation and carbonization. The ZnO nanoparticles were uniformly distributed on the surface of the carbon nanofiber with the size of 20-30 nm, confirmed by scanning electron microscopy （ SEM ） . The wettability of the ZnO-CNF was studied by water contact angle test. With Nafion as an additive, the ZnO-CNF modified electrode was successfully constructed by dip-coating. The surface morphology and electrochemical properties of the modified electrode were investigated by SEM and cyclic voltammetry. There was a sensitive response of the ZnO-CNF modified electrode on Pb ions in solution, demonstrated by square wave stripping voltammetry. Under the optimized conditions, a good linear relationship between peak current and Pb2＋concentration was obtained in the range of 2. 4×10-10-2. 4×10-7 mol/L （R=0. 998） by 10 min preconcentration at -1. 0 V in 0. 1 mol/L NaAc buffer solution （pH=4. 6）. The detection limit was 4. 8×10-11 mol/L. The practical analytical application of the ZnO-CNF modified electrode was assessed by the measurement of the actual water sample and the result was consistent with that obtained by ICP-MS.

关 键 词：静电纺丝技术 ZNO 碳复合纳米纤维修饰电极 铅 方波溶出伏安法 

分 类 号：O657.1[理学—分析化学] O614.433[理学—化学]