Grabarczyk Malgorzata, Adamczyk Marzena
Faculty of Chemistry, Maria Curie-Sklodowska University 20-031 Lublin Poland
RSC Adv. 2018 Apr 23;8(27):15215-15221. doi: 10.1039/c8ra01160e. eCollection 2018 Apr 18.
An analytical procedure regarding the voltammetric determination of germanium(iv) by adsorptive stripping voltammetry (AdSV) exploiting the plated bismuth film electrode (BiFE) is described. The use of mercury free electrode as a working electrode is the first time proposed in AdSV germanium determination. The method is based on adsorptive accumulation of the Ge(iv)-chloranilic acid complex at a BiFE by a nonelectrochemical process followed by the cathodic stripping step. Experimental variables, including bismuth and chloranilic acid concentrations, deposition potential and time were carefully optimized. Under optimized conditions the cathodic stripping peak current was directly proportional to the concentration of Ge(iv) in the range from 3 × 10 to 1.5 × 10 mol L with the correlation coefficient 0.997. Because the AdSV technique could be invalidated due to real samples matrix the influence of foreign ions, surface active substances, and humic substances on the Ge(iv) signal was precisely examined. The satisfying minimization of potential matrix interferences was also suggested. Analytical results of natural water samples analysis showed that the proposed procedure of trace germanium(iv) determination is suitable for direct environmental water analysis.
描述了一种利用镀铋膜电极(BiFE)通过吸附溶出伏安法(AdSV)伏安测定锗(IV)的分析方法。首次在AdSV锗测定中提出使用无汞电极作为工作电极。该方法基于Ge(IV)-氯冉酸络合物通过非电化学过程在BiFE上的吸附积累,随后进行阴极溶出步骤。仔细优化了包括铋和氯冉酸浓度、沉积电位和时间在内的实验变量。在优化条件下,阴极溶出峰电流与Ge(IV)浓度在3×10至1.5×10 mol/L范围内成正比,相关系数为0.997。由于实际样品基质可能使AdSV技术失效,因此精确研究了外来离子、表面活性物质和腐殖质对Ge(IV)信号的影响。还提出了令人满意的潜在基质干扰最小化方法。天然水样分析的结果表明,所提出的痕量锗(IV)测定方法适用于直接环境水分析。