On-line coupling of electrochemical preconcentration in tungsten coil electrothermal atomic absorption spectrometry for determination of lead in natural waters

被引:59
作者
Barbosa, F
Krug, FJ
Lima, EC
机构
[1] Univ Sao Paulo, Ctr Energia Nucl Agr, BR-13400970 Piracicaba, SP, Brazil
[2] Univ Sao Paulo, Inst Quim Sao Carlos, Sao Carlos, SP, Brazil
基金
巴西圣保罗研究基金会;
关键词
tungsten coil atomizer; electrothermal atomic absorption spectrometry; flow injection; lead; electrochemical preconcentration;
D O I
10.1016/S0584-8547(99)00055-5
中图分类号
O433 [光谱学];
学科分类号
0703 ; 070302 ;
摘要
A flow injection system was coupled to a tungsten coil electrothermal atomizer (150 W) for on-line separation and preconcentration of lead based on its electrochemical reduction on the atomizer surface. The electrochemical cell is built up inside the furnace by using a Pt flow-through anode and the atomizer itself as the flow-through cathode. The manifold and the tungsten coil power supply were controlled by a computer running a program written in Visual Basic, which was utilized in synchronism with the original software of the atomic absorption spectrometer. The flow-through anode (50 mm long, 0.7 mm i.d.) was inserted in tip of the autosampler arm by replacing the last section of the PTFE sample delivering tube. The tungsten coil atomizer and the counter electrode were easily connected to a d.c. power supply. An enrichment factor of 25 was obtained for lead after a 120-s electrodeposition for a sample flowing at 1.0 ml min(-1). The method detection limit was 0.2 mu g l(-1) Pb and the R.S.D. < 5% (n = 10 for 5 mu g l(-1) Pb). Up to 2% m/v NaCl or KCl and 5% m/v CaCl2 or MgCl2 did not interfere on the separation and atomization of 5 mu g l(-1) Pb. (C) 1999 Elsevier Science B.V. All rights reserved.
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页码:1155 / 1166
页数:12
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