Department of Chemistry, National Chung Hsing University, Taichung 402, Taiwan, R.O.C.
Talanta. 2013 Nov 15;116:852-9. doi: 10.1016/j.talanta.2013.07.063. Epub 2013 Aug 8.
A Cu(I)-ion-mediating Au reduction is proposed for preparing an Au-nanoparticle-embedded nafion (NF(Aunano)) composite. The NF(Aunano) composite consisted of highly dense, well-dispersed, and protecting-agent-free Au nanocrystals with a narrow particle size (4.8±0.1 nm) distribution. The NF(Aunano) composite was characterized as a function of composition and particle size distribution using powder X-ray diffraction, transmission electron microscopy, and electrochemical measurements. It was demonstrated that the NF(Aunano) composite provided high activity in the redox behavior of As(III), and was used as a potential sensing material with low Au loading for As(III) detection. An NF(Aunano)-composite-modified electrode is easy to prepare and regenerate. The dynamic range of a calibration curve from 0.1 to 12.0 μg L(-1) (from 1.3 to 160 nM), y=23.98x (in μA μM(-1))+0.42 (R(2)=0.999), showed linear behavior with a slope of 23.98 μA μM(-1). The detection limit is as low as 0.047 μg L(-1) (0.63 nM). The chelating agent ethylenediaminetetraacetate (EDTA) can selectively chelate with interfering metal ions, forming bulky complexes or bulky anions that are excluded from the NF film. The presence of EDTA effectively eliminated interference from several metal ions, particularly Cu(II) and Hg(II), which are generally considered to be major interferents in the electroanalysis of As(III). This method was applicable to As(III) analysis in three real water samples, namely groundwater, lake, and drinking waters.
提出了一种通过 Cu(I)离子介导的 Au 还原法来制备 Au 纳米粒子嵌入的 Nafion(NF(Aunano))复合材料。该 NF(Aunano)复合材料由高浓度、高度分散且无保护剂的 Au 纳米晶组成,其粒径分布狭窄(4.8±0.1nm)。采用粉末 X 射线衍射、透射电子显微镜和电化学测量对 NF(Aunano)复合材料的组成和粒径分布进行了表征。结果表明,NF(Aunano)复合材料在 As(III)的氧化还原行为中表现出高活性,并且可以作为一种具有低 Au 负载量的潜在传感材料,用于 As(III)检测。NF(Aunano)复合材料修饰电极易于制备和再生。从 0.1 到 12.0μg L(1.3 到 160nM)的校准曲线的动态范围,y=23.98x(以μAμM(-1)计)+0.42(R(2)=0.999)呈线性关系,斜率为 23.98μAμM(-1)。检测限低至 0.047μg L(0.63nM)。螯合剂乙二胺四乙酸(EDTA)可以与干扰金属离子选择性螯合,形成庞大的配合物或庞大的阴离子,从而被 NF 膜排除。EDTA 的存在有效地消除了来自几种金属离子的干扰,特别是 Cu(II)和 Hg(II),它们通常被认为是 As(III)电化学分析中的主要干扰物。该方法适用于地下水、湖泊和饮用水三种实际水样中 As(III)的分析。