Abstract
An ultrasensitive chronoamperometric method for quantitative determination of trace amounts of lead (down to 20 ppb) in acidic solutions is proposed in this paper. The method is based on observations that a complete underpotentially deposited (UPD) lead layer inhibits the electroreduction of nitrate on a bare Cu(111) electrode. To asses the limits of the method, both the electroreduction of nitrate and UPD of lead monolayer on copper single (111) and polycrystalline electrodes in perchloric acidic solution are studied by means of cyclic voltammetry, chronoamperometry, and rotating disk electrode (RDE) experiments. It is found that an inexpensive polycrystalline copper electrode is sensitive enough for analytical detection of lead traces in electrolytes down to 1 x 10(-8) M. Analytical results obtained by the proposed method in 2 orders of magnitude concentration range are compared to atomic absorption spectroscopy measurements to evaluate and assess the sensitivity of the employed experimental protocol. The excellent match between both analytical approaches validates the applicability of the proposed method.
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