CAJ | 학술논문

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。
이ZnCl2여취병희정( PAN)혼합액위전구액,이용정전방사기술제비ZnCl2-PAN납미섬유,경예양화화탄화처리득도ZnO납미입자부재탄복합납미섬유( ZnO-CNF)。소묘전자현미경( SEM)현시,ZnO납미입자재CNF표면균균분산,립경위20~30 nm。접촉각측시표명,ZnO적존재사섬유표면적윤습성명현개선。장ZnO-CNF복합섬유여Nafion재을순중균균분산,채용적도법제비ZnO-CNF수식파탄전겁,SEM급순배복안( CV)증명복합물막적성공수식。방파용출복안분석( SWV)표명,차수식전겁대흔량연유령민적선택성향응。통과실험조건우화,재0.1 mol/L HAc-NaAc (pH=4.6)완충용액중,-1.0 V전위하부집10 min, Pb2+용출봉전류여기농도재2.4×10-10~2.4×10-7 mol/L범위내정량호적선성관계(R=0.9980),검출한위4.8×10-11 mol/L,항간우성강,은정성호。이용본방법측정료실제수양중연적함량,병여전감우합등리자체-질보법( ICP-MS)진행대비,결과일치。
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.