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首页> 外文期刊>Electroanalysis >Multicommutated Anodic Stripping Voltammetry at Tubular Bismuth Film Electrode for Lead Determination in Gunshot Residues
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Multicommutated Anodic Stripping Voltammetry at Tubular Bismuth Film Electrode for Lead Determination in Gunshot Residues

机译：管状铋薄膜电极上的多交换阳极溶出伏安法测定枪支残留物中的铅

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摘要

This work describes the construction of a miniaturized flow-through electrochemical cell and its application to the determination of lead in gunshot residues (GSR) by differential-pulse anodic stripping voltammetry at bismuth films co-deposited on-line on a tubular carbon paste electrode. The developed detector was coupled to a multicommutated flow system which was designed to allow medium exchange prior to the stripping step thus reducing interferences from the analytical matrix, and to implement the standard additions method in an automatic way, using only one standard solution. For a deposition time of 60 s at - 1.5 V at a flow rate of 0.5 mL min(-1) without oxygen removal, the detection limit of the method was 0.2 mg L-1. Under these conditions the linear dynamic range was 0.3-10.0 mg L-1 with a sampling rate of 15.0 samples h(-1). Repeatability of lead concentration was 3% (n = 3). The method was applied to the analysis of lead in GSR on hands of shooters and concentrations up to 16.5 mu g and 6.7 mu g were found in palms and backs, respectively. No statistically significant differences between the results obtained by the proposed and the comparative method (F-AAS) were found, at a 95% confidence level.
机译：这项工作描述了一种微型流通式电化学电池的构造及其在在线沉积在管状碳糊电极上的铋膜上的微分脉冲阳极溶出伏安法测定枪支残留物（GSR）中的铅的应用。研发的检测器与多换向流系统相连，该系统设计成可在汽提步骤之前进行介质交换，从而减少了来自分析基质的干扰，并仅使用一种标准溶液即可自动实施标准添加方法。对于在0.5 mL min（-1）的流速下在-1.5 V下60 s的沉积时间而没有除氧的情况，该方法的检测极限为0.2 mg L-1。在这些条件下，线性动态范围为0.3-10.0 mg L-1，采样率为15.0个样本h（-1）。铅浓度的重复性为3％（n = 3）。该方法用于分析射手手上的GSR中的铅，在手掌和背部分别发现浓度分别为16.5和6.7微克。在95％的置信水平下，在提议的方法和比较方法（F-AAS）之间没有发现统计学上的显着差异。

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