静电纺丝法制备氧化锆纳米纤维修饰玻碳电极用于甲基对硫磷的检测

Electrospun Zirconia Nanofibre-modified Glassy Carbon Electrode for Determination of Methyl Parathion

通过静电纺丝技术制备含有锆盐的纳米纤维,经煅烧制得结构均匀的氧化锆(ZrO_2)纳米纤维。纤维直径约为(194 030) nm,透射电镜及X-射线衍射分析结果表明,纤维主要由单斜相纳米ZrO_2微晶组成。将ZrO_2纤维和导电炭黑Super P及粘结剂混合,采用滴涂法制备ZrO_2纳米纤维薄膜修饰玻碳电极,并成功应用于甲基对硫磷(MP)的检测。利用循环伏安(CV)及差分脉冲伏安法(DPV)研究MP在电极表面的电化学行为。在最优条件下,响应电流信号与MP的浓度在0.1～1.2μg/L的范围内呈良好的线性关系,检出限为0.06μg/L(S/N=3.0)。此修饰电极具有良好的稳定性、重现性和选择性。使用此传感器检测实际水样,MP的回收率为96.7%～102.4%,相对标准偏差为2.3%～4.5%,可望用于MP的高灵敏传感。

Zirconia(ZrO 2)nanofibers with a diameter of(194±30)nm were successfully fabricated by electrospinning zirconium salt-containing nanofibers followed by calcination.Scanning electron microscopy,transmission electron microscopy and X-ray diffraction characterization results revealed that the fibers were mainly composed of monoclinic nano-crystallite of ZrO 2.The ZrO 2 nanofiber-modified glassy carbon electrode(GCE)was prepared by drop-coating the mixture of ZrO 2 nanofibre,Super P and polyvinylidenefluoride(PVDF),were successfully applied to the detection of methyl parathion(MP).Cyclic voltammetry(CV)and differential pulse voltammetry(DPV)were used to study the electrochemical behavior of MP on the modified electrode surface.Under the optimal conditions,the DPV peak current of the electrode showed a linear relationship with MP concentration in the range of 0.1-1.2 mg/L with a detection limit of 0.06μg/L(S/N=3).The sensor had good stability,reproducibility and anti-interference property.The real water samples were analyzed,with MP recovery of 96.7%-102.4%and relative standard deviation of less than 5%.This electrode could be used as a highly sensitive sensor for MP measurement.