Majid Ehsan, Hrapovic Sabahudin, Liu Yali, Male Keith B, Luong John H T
Biotechnology Research Institute, National Research Council Canada, Montreal, Quebec.
Anal Chem. 2006 Feb 1;78(3):762-9. doi: 10.1021/ac0513562.
A flow analysis electrochemical system has been developed, characterized, and optimized for the determination of arsenite (As(III)). Sensitivity was significantly improved by the electrochemical deposition of gold nanoparticles on a dual glassy carbon electrode, which was inserted into a cross-flow thin-layer electrochemical cell. The electrochemical system was linear up to 15 ppb with a detection limit of 0.25 ppb. Gold deposition was evident from cyclic voltammetry measurements, whereas atomic force microscopy and scanning electron microscopy revealed the size and distribution of deposited gold nanoparticles. The size and density of the nanoparticles were related to the gold salt concentration, deposition time, and potential as well as the electrode position. The response to arsenite was directly related to the frequency, increment, and amplitude of the square wave voltammetry as well as the deposition time and potential. Estimated reproducibility was +/-1.1% at 95% confidence interval for 40 repeated analyses of 8 ppb arsenite during continuous analysis. The reproducibility was far superior if the electrochemical reduction of arsenite was performed in nitric acid instead of hydrochloric or sulfuric acid. The electrochemical system was applicable for analysis of spiked arsenic in mineral water containing a significant amount of various ion elements.
已开发、表征并优化了一种流动分析电化学系统,用于测定亚砷酸盐(As(III))。通过在插入错流薄层电化学池的双玻碳电极上电化学沉积金纳米颗粒,显著提高了灵敏度。该电化学系统在高达15 ppb时呈线性,检测限为0.25 ppb。循环伏安法测量显示有金沉积,而原子力显微镜和扫描电子显微镜揭示了沉积金纳米颗粒的尺寸和分布。纳米颗粒的尺寸和密度与金盐浓度、沉积时间、电位以及电极位置有关。对亚砷酸盐的响应与方波伏安法的频率、增量和幅度以及沉积时间和电位直接相关。在连续分析期间,对8 ppb亚砷酸盐进行40次重复分析,在95%置信区间下估计的重现性为±1.1%。如果在硝酸而非盐酸或硫酸中进行亚砷酸盐的电化学还原,重现性会好得多。该电化学系统适用于分析含有大量各种离子元素的矿泉水中加标的砷。