Ultra-simple adaptor to convert batch cells with mercury drop electrodes in voltammetric detectors for flow analysis

摘要

A simple, robust and fast-responding flow adaptor for mercury drop electrodes (MDEs) is described. An L-shaped PTFE tube with an internal diameter of 0.5 mm is fixed with a silicone ring on the glass capillary of a MDE, in such a way as to direct the outcoming flow onto the mercury drop, from a distance of about 0.5 mm. Any commercial or laboratory-made batch cell, provided with an MDE, serves for the purpose. The level of supporting electrolyte in the cell is maintained constant through a siphon or a lateral draining orifice. The adaptor is compatible with all the different brands and operating modes of the MDEs (free dropping, controlled drop time, renewable static drop, hanging drop or sessile drop). Flow injection experiments were conducted with the following amperometric detection modes: sampled-DC, reverse pulse amperometry (RPA), and anoidc stripping voltammetry (ASV). The FIA-RPA peaks presented a R.S.D. <0.8% for 1.0 * 10~(-5) mol l~(-1) lead(II) (N = 30, V_(sample) = 100 μl). The response time (0-63% of the signal maximum) to a concentration step is 1.2 s for 500 μl injections of 0.1 mmol l~(-1) ascorbic acid in acetate buffer at a flow rate of 1 ml min~(-1), which corresponds to a response volume of 20 μl. As an example of practical application, copper(II) was determined in fertilizers by RPA using the standard addition method, at an analytical frequency of 90 injections per h.