期刊
ELECTROANALYSIS
卷 16, 期 19, 页码 1616-1621出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/elan.200402979
关键词
bismuth film electrode; nitrophenol; cathodic reduction; electrochemical detection; voltammetry; amperometry
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.
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