Economou Anastasios, Voulgaropoulos Anastasios
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki 541 24, Greece.
Talanta. 2007 Feb 15;71(2):758-65. doi: 10.1016/j.talanta.2006.05.021. Epub 2006 Jun 21.
In this work, we describe an automated stripping analyzer operating on a hybrid flow-injection/sequential-injection (FIA/SIA) mode and utilizing a bismuth-film electrode (BiFE) as a flow-through sensor for on-line stripping voltammetry of trace metals. The instrument combines the advantages of FIA and SIA and is characterised by simplicity, low-cost, rapidity, versatility and low consumption of solutions. The proposed analytical flow methodology was applied to the determination of Cd(II) and Pb(II) by anodic stripping voltammetry (ASV) and of Ni(II) and Co(II) by adsorptive stripping voltammetry (AdSV). The steps of the rather complex experimental sequence (i.e. the bismuth-film formation, the analyte accumulation, the voltammetric stripping and the electrode cleaning/regeneration) were conducted on-line and the critical parameters related to the respective analytical procedures were investigated. In ASV, for a accumulation time of 180s the limits of detection for Cd(II) and Pb(II) were 2 and 1microg l(-1), respectively (S/N=3) and the relative standard deviations were 5.3% and 4.7%, respectively (n=8). In AdSV, for a total sample volume of 1000microl, the limits of detection for Ni(II) and Co(II) were 1microg l(-1) (S/N=3) and the relative standard deviations were 5.5% and 6.2%, respectively (n=8). The measurement frequency ranged between 15 and 20 stripping cycles h(-1). The results indicate that the BiFE is well suited as a flow-through detector for on-line stripping analysis and, by virtue of its low toxicity, can serve as a viable alternative to mercury-based flow-through electrodes.
在本工作中,我们描述了一种以混合流动注射/顺序注射(FIA/SIA)模式运行的自动溶出分析仪,该分析仪利用铋膜电极(BiFE)作为流通式传感器,用于痕量金属的在线溶出伏安法分析。该仪器结合了FIA和SIA的优点,具有操作简单、成本低、速度快、通用性强和溶液消耗低的特点。所提出的分析流程方法应用于通过阳极溶出伏安法(ASV)测定Cd(II)和Pb(II),以及通过吸附溶出伏安法(AdSV)测定Ni(II)和Co(II)。相当复杂的实验序列步骤(即铋膜形成、分析物积累、伏安溶出和电极清洗/再生)均在线进行,并研究了与各个分析程序相关的关键参数。在ASV中,积累时间为180s时,Cd(II)和Pb(II)的检测限分别为2和1μg l(-1)(S/N = 3),相对标准偏差分别为5.3%和4.7%(n = 8)。在AdSV中,总样品体积为1000μl时,Ni(II)和Co(II)的检测限为1μg l(-1)(S/N = 3),相对标准偏差分别为5.5%和6.2%(n = 8)。测量频率在15至20次溶出循环h(-1)之间。结果表明,BiFE非常适合作为在线溶出分析的流通式检测器,并且由于其低毒性,可以作为汞基流通式电极的可行替代品。