Siriangkhawut Watsaka, Pencharee Somkid, Grudpan Kate, Jakmunee Jaroon
Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200, Thailand.
Talanta. 2009 Sep 15;79(4):1118-24. doi: 10.1016/j.talanta.2009.03.032. Epub 2009 Mar 25.
A cost-effective sequential injection monosegmented flow analysis (SI-MSFA) with anodic stripping voltammetric (ASV) detection has been developed for determination of Cd(II) and Pb(II). The bismuth film working electrode (BiFE) was employed for accumulative preconcentration of the metals by applying a fixed potential of -1.10 V versus Ag/AgCl electrode for 90 s. The SI-MSFA provides a convenient means for preparation of a homogeneous solution zone containing sample in an acetate buffer electrolyte solution and Bi(III) solution for in situ plating of BiFE, ready for ASV measurement at a flow through thin layer electrochemical cell. Under the optimum conditions, linear calibration graphs in range of 10-100 microg L(-1) of both Cd(II) and Pb(II) were obtained with detection limits of 1.4 and 6.9 microg L(-1) of Cd(II) and Pb(II), respectively. Relative standard deviations were 2.7 and 3.1%, for 11 replicate analyses of 25 microg L(-1) Cd(II) and 25 microg L(-1) Pb(II), respectively. A sample throughput of 12h(-1) was achieved with low consumption of reagent and sample solutions. The system was successfully applied for analysis of water samples collected from a draining pond of zinc mining, validating by inductively coupled plasma-optical emission spectroscopy (ICP-OES) method.
已开发出一种具有阳极溶出伏安法(ASV)检测的经济高效的顺序注射单段流动分析(SI-MSFA)方法,用于测定镉(II)和铅(II)。采用铋膜工作电极(BiFE),通过相对于Ag/AgCl电极施加-1.10 V的固定电位90 s,对金属进行累积预富集。SI-MSFA提供了一种便捷的方法,可在醋酸盐缓冲电解质溶液和Bi(III)溶液中制备含有样品的均匀溶液区,用于BiFE的原位镀覆,准备好在流通式薄层电化学池中进行ASV测量。在最佳条件下,获得了镉(II)和铅(II)浓度在10 - 100 μg L⁻¹范围内的线性校准曲线,镉(II)和铅(II)的检测限分别为1.4和6.9 μg L⁻¹。对于25 μg L⁻¹镉(II)和25 μg L⁻¹铅(II)的11次重复分析,相对标准偏差分别为2.7%和3.1%。实现了12 h⁻¹的样品通量,试剂和样品溶液消耗低。该系统成功应用于从锌矿排水池中采集的水样分析,并通过电感耦合等离子体发射光谱法(ICP-OES)进行了验证。