Mettakoonpitak Jaruwan, Miller-Lionberg Dan, Reilly Thomas, Volckens John, Henry Charles S
Department of Chemistry, Colorado State University, Fort Collins, Colorado 80523, USA.
Access Sensor Technologies LLC, 430 N College Ave St. 410, Fort Collins, Colorado 80524, USA.
J Electroanal Chem (Lausanne). 2017 Nov 15;805:75-82. doi: 10.1016/j.jelechem.2017.10.026. Epub 2017 Oct 12.
A low-cost electrochemical sensor with Nafion/Bi modification using adsorptive stripping voltammetry for Co and Ni determination in airborne particulate matter and welding fume samples is described. Carbon stencil-printed electrodes (CSPEs) manufactured on low-cost PET films were utilized. Dimethylglyoxime (DMG) was used as a Co(II) and Ni(II) chelator with selective chemical precipitation for trace electrochemical analysis. Electrochemical studies of the Nafion/Bi-modified CSPE indicated a diffusion-controlled redox reaction for Co and Ni measurements. The Nafion coating decreased the background current and enhanced the measured peak current. Repeatability tests based on changes in percent relative standard deviation (RSD) of peak current showed the electrode could be used at least 15 times before the RSD exceeded 15% (the reported value of acceptable repeatability from Association of Official Analytical Chemists (AOAC)) due to deterioration of electrode surface. Limits of detection were 1 μg L and 5 μg L for Co and Ni, respectively, which were comparable to electrochemical sensors requiring more complicated modification procedures. The sensor produced a working range of 1-250 and 5-175 μg L for Co and Ni, respectively. Interference studies showed no other metal species interfered with Co and Ni measurements using the optimized conditions. Finally, the developed sensors were applied for Co and Ni determination in aerosol samples generated from Co rods and a certified welding-fume reference material, respectively. Validation with ICP-MS showed no statistically different results with 95% confidence between sensor and the ICP methods.
描述了一种低成本的电化学传感器,该传感器采用Nafion/铋修饰,利用吸附溶出伏安法测定空气中颗粒物和焊接烟尘样品中的钴和镍。使用了在低成本PET薄膜上制造的碳模板印刷电极(CSPE)。丁二酮肟(DMG)用作钴(II)和镍(II)的螯合剂,通过选择性化学沉淀进行痕量电化学分析。Nafion/铋修饰的CSPE的电化学研究表明,在测量钴和镍时存在扩散控制的氧化还原反应。Nafion涂层降低了背景电流并增强了测量的峰值电流。基于峰值电流相对标准偏差(RSD)百分比变化的重复性测试表明,由于电极表面的劣化,在RSD超过15%(官方分析化学家协会(AOAC)报告的可接受重复性值)之前,该电极至少可使用15次。钴和镍的检测限分别为1μg/L和5μg/L,这与需要更复杂修饰程序的电化学传感器相当。该传感器对钴和镍的工作范围分别为1 - 250μg/L和5 - 175μg/L。干扰研究表明,在优化条件下,没有其他金属物种干扰钴和镍的测量。最后,将开发的传感器分别应用于钴棒和气溶胶样品以及经认证的焊接烟尘参考物质中钴和镍的测定。与电感耦合等离子体质谱(ICP-MS)的验证表明,传感器和ICP方法之间在95%置信度下没有统计学上的显著差异。