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使用响应面法-中心复合设计优化,实现 TNT 的灵敏和选择性阻抗测定。

Sensitive and selective impedimetric determination of TNT using RSM-CCD optimization.

机构信息

Faculty of Chemistry, Bu-Ali Sina University, Hamedan, Iran.

Faculty of Chemistry, Bu-Ali Sina University, Hamedan, Iran; D-8 International University, Hamedan, Iran.

出版信息

Talanta. 2023 May 15;257:124381. doi: 10.1016/j.talanta.2023.124381. Epub 2023 Feb 17.

Abstract

Detection of trace amounts of 2,4,6-Trinitrotoluene as a widely used explosive in the military and industrial sectors is of vital importance due to security and environmental concerns. The sensitive and selective measurement characteristics of the compound still is considered a challenge for analytical chemists. Unlike conventional optical and electrochemical methods, the electrochemical impedance spectroscopy technique (EIS), has a very high sensitivity, but it faces a significant challenge in that it requires complex and expensive steps to modify the electrode surface with selective agents. We reported the design and construction of an inexpensive, simple, sensitive, and selective impedimetric electrochemical TNT sensor based on the formation of a Meisenheimer complex between magnetic multiwalled carbon nanotubes modified with aminopropyl triethoxysilane (MMWCNTs @ APTES) and TNT. The formation of the mentioned charge transfer complex at the electrode-solution interface blocks the electrode surface and disrupts the charge transfer in [(Fe (CN) )] redox probe system. Charge transfer resistance changes (ΔR) were used as an analytical response that corresponded to TNT concentration. To investigate the influence of effective parameters on the electrode response, such as pH, contact time, and modifier percentage, the response surface methodology based on central composite design (RSM-CCD) was used. The calibration curve was achieved in the range of 1-500 nM with a detection limit of 0.15 nM under optimal conditions, which included pH of 8.29, contact time of 479 s, and modifier percentage of 12.38% (w/w). The selectivity of the constructed electrode towards several nitroaromatic species was investigated, and no significant interference was found. Finally, the proposed sensor was able to successfully measure TNT in various water samples with satisfactory recovery percentages.

摘要

检测痕量 2,4,6-三硝基甲苯(TNT)作为一种广泛应用于军事和工业领域的爆炸物,由于安全和环境方面的考虑,具有至关重要的意义。尽管化合物具有敏感和选择性的测量特性,但对于分析化学家来说,仍然是一个挑战。与传统的光学和电化学方法不同,电化学阻抗谱技术(EIS)具有非常高的灵敏度,但它面临着一个重大挑战,即需要复杂且昂贵的步骤来用选择性试剂修饰电极表面。我们报告了一种基于磁性多壁碳纳米管修饰的氨丙基三乙氧基硅烷(MMWCNTs@APTES)与 TNT 之间形成 Meisenheimer 配合物的廉价、简单、灵敏和选择性的阻抗电化学 TNT 传感器的设计和构建。在电极-溶液界面形成的所述电荷转移配合物会阻碍电极表面并破坏 [(Fe(CN) )] 氧化还原探针系统中的电荷转移。电荷转移电阻变化(ΔR)被用作与 TNT 浓度相对应的分析响应。为了研究有效参数(如 pH 值、接触时间和修饰剂百分比)对电极响应的影响,使用了基于中心复合设计(RSM-CCD)的响应面法。在最佳条件下,校准曲线在 1-500 nM 范围内实现,检测限为 0.15 nM,最佳条件包括 pH 值为 8.29、接触时间为 479 s 和修饰剂百分比为 12.38%(w/w)。还研究了构建的电极对几种硝基芳烃的选择性,未发现明显的干扰。最后,该传感器能够成功地测量各种水样中的 TNT,回收率令人满意。

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