Departamento de Química, Universidade Presbiteriana Mackenzie, São Paulo, SP, Brazil.
Talanta. 2003 Jul 4;60(4):695-705. doi: 10.1016/S0039-9140(03)00143-7.
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 anodic stripping voltammetry (ASV). The FIA-RPA peaks presented a R.S.D.<0.8% for 1.0x10(-5) mol l(-1) lead(II) (N=30, V(sample)=100 mul). The response time (0-63% of the signal maximum) to a concentration step is 1.2 s for 500 mul 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 mul. 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.
描述了一种用于汞滴电极(MDE)的简单、鲁棒且快速响应的流量适配器。将内径为 0.5 毫米的 L 形聚四氟乙烯管用硅橡胶环固定在 MDE 的玻璃毛细管上,以将流出的流动导向汞滴,距离约为 0.5 毫米。任何带有 MDE 的商业或实验室制造的批处理池都可用于此目的。通过虹吸管或侧向排水孔将池中的支持电解质的液位保持恒定。该适配器与所有不同品牌和操作模式的 MDE 兼容(自由滴落、控制滴落时间、可再生静态滴落、悬挂滴落或固着滴落)。进行了流动注射实验,并采用以下电流检测模式:取样-DC、反向脉冲安培法(RPA)和阳极溶出伏安法(ASV)。对于 1.0x10(-5) mol l(-1) 铅(II)(N=30,V(sample)=100 mul),FIA-RPA 峰的 R.S.D. <0.8%。对于在 1 ml min(-1)流速下 500 mul 进样 0.1 mmol l(-1)抗坏血酸的醋酸盐缓冲液中的浓度阶跃,响应时间(信号最大值的 0-63%)为 1.2 s,这对应于 20 mul 的响应体积。作为实际应用的示例,通过 RPA 使用标准加入法在肥料中测定了铜(II),分析频率为 90 次/小时。