Guziejewski Dariusz, Smarzewska Sylwia, Metelka Radovan, Nosal-Wiercińska Agnieszka, Ciesielski Witold
Faculty of Chemistry, Department of Inorganic and Analytical Chemistry, University of Lodz, 92-236 Łódź, Poland.
Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Studentska 573, 53210 Pardubice, Czech Republic.
Monatsh Chem. 2017;148(3):555-562. doi: 10.1007/s00706-017-1918-8. Epub 2017 Feb 8.
The use of square wave voltammetry (SWV) and square wave adsorptive stripping voltammetry (SWAdSV) in conjunction with a cyclic renewable silver amalgam film electrode for the determination of flumetralin is presented. Poor separation of two overlapped reduction peaks is significantly improved when hexadecyltrimethylammonium bromide is used as a component of the supporting electrolyte solution (together with BR buffer pH 9.5). The SW technique parameters were investigated and found optimal as follows: frequency 50 Hz, amplitude 40 mV, and step potential 5 mV. Accumulation time and potential were studied to select the optimal conditions in adsorptive voltammetry. The analytical curve was linear for the flumetralin concentration range from 1.0 × 10 to 1.0 × 10 mol dm and from 5.0 × 10 to 1.0 × 10 mol dm for SWV and SWAdSV, respectively. Detection limit of 6.5 × 10 mol dm was calculated for accumulation time 60 s at -0.2 V. The repeatability of the method was determined at a flumetralin concentration level equal to 5.0 × 10 mol dm and expressed as %RSD = 5.0% ( = 6). The proposed method was applied and validated successfully by studying the recovery of herbicide content in spiked environmental samples.
本文介绍了使用方波伏安法（SWV）和方波吸附溶出伏安法（SWAdSV）结合循环可再生银汞膜电极测定氟乐灵的方法。当使用十六烷基三甲基溴化铵作为支持电解质溶液的成分（与pH 9.5的BR缓冲液一起）时，两个重叠还原峰的分离效果显著改善。对方波技术参数进行了研究，发现最佳参数如下：频率50Hz，振幅40mV，步长电位5mV。研究了吸附伏安法中的富集时间和电位以选择最佳条件。对于SWV和SWAdSV，氟乐灵浓度范围分别为1.0×10至1.0×10 mol dm和5.0×10至1.0×10 mol dm时，分析曲线呈线性。在-0.2V下富集时间为60s时，计算出检测限为6.5×10 mol dm。在氟乐灵浓度水平等于5.0×10 mol dm时测定了该方法的重复性，以%RSD = 5.0%（n = 6）表示。通过研究加标环境样品中除草剂含量的回收率，成功应用并验证了所提出的方法。
