Rojas-Romo Carlos, Serrano Núria, Ariño Cristina, Arancibia Verónica, Díaz-Cruz José Manuel, Esteban Miquel
Departament de Química Analítica, Facultat de Química, Universitat de Barcelona, Martí i Franquès 1-11, E-08028 Barcelona, Spain; Facultad de Química, Pontificia Universidad Católica de Chile, Vicuña Mackenna 4860, Santiago 7820436, Chile.
Departament de Química Analítica, Facultat de Química, Universitat de Barcelona, Martí i Franquès 1-11, E-08028 Barcelona, Spain.
Talanta. 2016 Aug 1;155:21-7. doi: 10.1016/j.talanta.2016.04.015. Epub 2016 Apr 6.
The determination of Sb(III) on an ex-situ bismuth screen-printed carbon electrode (ex-situ BiSPCE) by means of adsorptive stripping voltammetry (AdSV) using quercetin-5'-sulfonic acid as chelating agent was optimized. The effect of different experimental parameters such pH, ligand concentration (CQSA), accumulation potential (Eacc) and accumulation time (tacc) were studied to obtain a wide linear range, the highest sensitivity and the lowest detection limit. Ex-situ BiSPCE was analytically compared with a sputtered bismuth screen-printed electrode (BispSPE) under optimal conditions. The obtained analytical parameters suggest that ex-situ BiSPCE behaves much better than BispSPE and the first was selected for this study. Optimal parameters were pH=4.6; CQSA=10.0 to 20.0×10(-6)molL(-1); Eacc=-0.5V and tacc=60s. Peak area is proportional to Sb(III) concentration up to 100.0μgL(-1) (tacc 60s) and 45.0μgL(-1) (tacc 120s) range, with detection limits of 1.2μgL(-)(1) (tacc 60s) and 0.8μgL(-1) (tacc 120s). The relative standard deviation for a Sb(III) solution (20.0μgL(-1)) was 3.9% for ten successive assays. Thus, the effect of various interfering metal ions was studied and the methodology was validated using a spiked groundwater reference material with very satisfactory results.
采用槲皮素 - 5'-磺酸作为螯合剂，通过吸附溶出伏安法（AdSV）在异位铋丝网印刷碳电极（异位BiSPCE）上对Sb(III)的测定进行了优化。研究了不同实验参数如pH值、配体浓度（CQSA）、富集电位（Eacc）和富集时间（tacc）的影响，以获得较宽的线性范围、最高灵敏度和最低检测限。在最佳条件下，将异位BiSPCE与溅射铋丝网印刷电极（BispSPE）进行了分析比较。获得的分析参数表明，异位BiSPCE的性能比BispSPE好得多，因此选择前者进行本研究。最佳参数为pH = 4.6；CQSA = 10.0至20.0×10(-6)molL(-1)；Eacc = -0.5V和tacc = 60s。在tacc为60s时，峰面积与Sb(III)浓度在高达100.0μgL(-1)范围内成正比，在tacc为120s时，在45.0μgL(-1)范围内成正比，检测限分别为1.2μgL(-1)（tacc 60s）和0.8μgL(-1)（tacc 120s）。对于20.0μgL(-1)的Sb(III)溶液，连续十次测定的相对标准偏差为3.9%。因此，研究了各种干扰金属离子的影响，并使用加标地下水参考物质对该方法进行了验证，结果非常令人满意。
