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Cathodic electrochemical detection of nitrophenols at a bismuth film electrode for use in flow analysis

机译:铋膜电极上硝基酚的阴极电化学检测,用于流动分析

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摘要

The bismuth film electrode (BiFE) is presented for use in both batch voltammetric and flow injection (FI) amperometric detection of some nitrophenols (2-nitrophenol, 2-NP; 4-nitrophenol, 4-NP; 2,4-dinitrophenol, 2,4-DNP). The bismuth film was deposited ex situ (batch measurements) and in-line (FI) onto a glassy carbon substrate electrode. Batch analysis of the nitrophenols was carried out in 0.04 M Britton Robinson (BR) buffer pH 4, while for FI measurements, a carrier/electrolyte solution composed of 0.1 M BR buffer pH 4 mixed with methanol (20 + 80, v/v%) was employed to resemble media used in preconcentration/clean-up and flow separation sample pretreatment procedures. Under batch conditions, the voltammetric behavior of the nitrophenols was examined for dependence on medium pH in the range of 2 to 10. Employing the square-wave voltammetry mode, the limits of detection were 0.4 mug L-1, 1.4 mug L-1, and 3.3 mug L-1 for 2-NP, 4-NP, and 2,4-DNP, respectively. Under flow conditions, a simple in-line electrochemical bismuth film renewal procedure was tested and shown to provide very good inter- and intra-electrode reproducibility of the current signals at low mug L-1 analyte concentrations. The limits of detection for 2-NP, 4-NP and 2,4-DNP obtained using FI and amperometric detection at -1.0 V (vs. Ag/AgCl) were 0.3 mug L-1, 0.6 mug L-1 and 0.7 mug L-1, respectively, with linear ranges extending up to 20 mug L-1. The attractive performance of the BiFE under flow analysis conditions offers great promise with respect to its detection capability and to its use for a prolonged period of time with no need for inconvenient removal of the electrode from the system for mechanical surface treatment.
机译:铋膜电极(BiFE)用于批量伏安法和流动注射(FI)安培检测一些硝基苯酚(2-硝基苯酚,2-NP; 4-硝基苯酚,4-NP; 2,4-二硝基苯酚,2 ,4-DNP)。铋膜非原位沉积(批量测量)并在线(FI)沉积在玻璃碳基底电极上。在0.04 M Britton Robinson(BR)缓冲液pH 4中进行硝基苯酚的分批分析,而对于FI测量,由0.1 M BR pH 4的缓冲液与甲醇(20 + 80,v / v%)混合组成的载体/电解质溶液)类似于在预浓缩/净化和流动分离样品预处理程序中使用的介质。在分批条件下,检查了硝基酚的伏安行为对2至10范围内的中等pH值的依赖性。采用方波伏安模式,检出限为0.4马克杯L-1、1.4马克杯L-1,和3.3杯L-1分别用于2-NP,4-NP和2,4-DNP。在流动条件下,测试了简单的在线式电化学铋膜更新程序,结果表明,在低杯L-1分析物浓度下,电流信号在电极间和电极内均具有很好的重现性。使用FI和在-1.0 V(vs.Ag/AgCl)进行安培检测获得的2-NP,4-NP和2,4-DNP的检出限分别为0.3马克杯L-1、0.6马克杯L-1和0.7马克杯L-1线性范围扩展到20个杯子L-1。 BiFE在流动分析条件下的引人入胜的性能为其检测能力和长时间使用提供了广阔的前景,无需将电极从机械表面处理系统中方便地取出。

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