串联薄层电解池研制及在血铅测定中的应用

发布时间：2018-05-06 15:30

本文选题：玻碳电极 + 薄层电解池　；参考：《齐齐哈尔大学》2012年硕士论文

【摘要】：以玻碳汞膜电极作为工作电极的阳极溶出伏安法由于灵敏度高，线性范围宽，检测速度快而成为微量分析的重要手段，但该方法仍存在峰高测量重现性差等不足。一般测量血铅时要求对血样进行稀释100倍，以减小或消除蛋白质对铅原子溶出过程的干扰，这样无形中对检测限提出了更高的要求。血铅峰高与空白峰高接近，影响定量。玻碳汞膜电极和电解池是该方法设备的核心部分。溶出时的噪音宽Wn与电极面积A成正比，铅的溶出峰高Hp也与电极面积A成正比。提高信噪比Rsn才是降低方法检测限的有效方法。本文将血液稀释10倍，在流动薄层池内，铅离子首先在大面积玻碳汞膜电极（LGCE）上预富集，溶出后在小面积玻碳汞膜电极（SGCE）上二次富集，因此提升了SGCE富集时溶出曲线的峰高，电解池内没有血液成分，只有血铅稀释剂，有利于铅的溶出，降低检测限。血液稀释倍数降低，，铅离子在血液中的的浓度相对较高，可以提高血铅峰高与空白峰高的比值。本文采用薄层大面积玻碳电解池与小面积玻碳电解池以串联方式连接。铅离子首先在大面积玻碳汞膜电极（LGCE）上被预富集，溶出后在小面积玻碳汞膜电极（SGCE）上二次富集铅，因此提升了SGCE富集时的铅离子浓度，减小电极的面积也有利于提高信噪比Rsn。
[Abstract]:Anodic stripping voltammetry with glassy carbon mercury film electrode as working electrode has become an important method for trace analysis because of its high sensitivity wide linear range and high detection speed. However the method still has some shortcomings such as poor reproducibility of peak height measurement. In order to reduce or eliminate the interference of protein on the dissolution process of lead atoms, it is required to dilute the blood sample 100 times when measuring blood lead. The peak height of blood lead was close to that of blank peak, which affected the quantification. Glassy carbon mercury film electrode and electrolytic cell are the core of the equipment. The noise width W _ n is proportional to the electrode area A, and the peak height HP is proportional to the electrode area A. Improving signal-to-noise ratio (Rsn) is an effective method to reduce the detection limit. In this paper, the hemodilution is 10 times. In the flow thin-layer cell, lead ion is preenriched on the large area glassy carbon mercury membrane electrode (LGCE), and then reenriched on the small area glassy carbon mercury membrane electrode. Therefore, the peak height of the dissolution curve during the enrichment of SGCE is raised. There is no blood component in the electrolytic cell, only blood lead diluent, which is advantageous to the dissolution of lead and lower detection limit. The ratio of blood lead peak height to blank peak height can be increased because of the decrease of hemodilution multiple and the relatively high concentration of lead ion in blood. In this paper, thin layer large area glassy carbon electrolysis cell and small area glassy carbon electrolysis cell are connected in series. Lead ion was preenriched on large area glassy carbon mercury membrane electrode (LGCE), and then reenriched on small area glassy carbon mercury membrane electrode (SGCE) after dissolution. Therefore, the lead ion concentration during SGCE enrichment was increased, and the reduction of electrode area was also beneficial to the improvement of signal-to-noise ratio (SNR).
【学位授予单位】：齐齐哈尔大学
【学位级别】：硕士
【学位授予年份】：2012
【分类号】：R131;O657.1

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