Calixarene films on QCM via electrospin coating for real-time monitoring of phenolic species in aqueous media

IF 2.8 3区化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Research on Chemical Intermediates Pub Date : 2024-10-19 DOI:10.1007/s11164-024-05422-2

Farabi Temel

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Abstract

This study includes the synthesis of 11 different calixarene derivatives, the preparation of thin film sensors on quartz crystal microbalance (QCM) crystals, and the specification of sensor-analyte pairs by examining the sensing properties of these sensors against different phenolic compounds such as p-nitrophenol (PNP), phenol (PHE), p-chlorophenol (PCP), and m-nitrophenol (MNP) in the aqueous medium. For this purpose, calixarene derivatives with different structures were first synthesized and characterized using spectroscopic methods such as Proton nuclear magnetic resonance (¹H-NMR) and Fourier-transform infrared spectroscopy (FTIR). Detection studies were carried out for proposed phenolic compounds with calixarene-based QCM sensors obtained by electrospinning. At the beginning of the experiments, sensor-analyte pairs were determined according to the values at which the highest sensor frequencies were observed. Therefore, according to the highest sensor responses towards 5 × 10^–5 M analytes, the sensor-analyte pairs were determined as QCM-5 for PNP (17.8 Hz) and MNP (3.8 Hz). Also, for PHE and PCP, the highest responses were observed as 4.1 Hz and 4.0 Hz in the QCM-11 and QCM-1 sensors, respectively. In further experiments, determined sensor-analyte pairs were tested at different analyte concentrations. In addition, the limits of detection (LOD) of the sensors were calculated from different analyte concentration studies such as 0.580 (QCM-5), 0.659 (QCM-11), 0.490 (QCM-1), and 0.466 (QCM-5) mM against PNP, PHE, PCP, and MNP, respectively. Interactions between sensor-analyte pairs were evaluated in terms of adsorption kinetics. It was observed that the relationships between the sensor responses and the analyte concentration were highly consistent with the Freundlich isotherm. In addition, repeatability and stability tests of the sensors were performed, and it was observed that they exhibited good repeatability and stability properties. Finally, selectivity between analytes was assessed, and the highest selectivity was observed as with the QCM-4 sensor versus p-nitrophenol. It was found that the selectivity of the sensor to PNP was 21.1 times compared to PHE and PCP and 74 times compared to MNP.

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通过电纺丝涂层在 QCM 上形成 Calixarene 薄膜，用于实时监测水介质中的酚类物质

本研究包括合成 11 种不同的咔唑烯衍生物，在石英晶体微天平 (QCM) 晶体上制备薄膜传感器，以及通过检测这些传感器对水介质中不同酚类化合物（如对硝基苯酚 (PNP)、苯酚 (PHE)、对氯苯酚 (PCP) 和间硝基苯酚 (MNP)）的传感特性来确定传感器-分析物对的规格。为此，首先合成了不同结构的萼片烯衍生物，并利用质子核磁共振（1H-NMR）和傅立叶变换红外光谱（FTIR）等光谱方法对其进行了表征。利用通过电纺丝获得的基于卡利沙蕾烯的 QCM 传感器对提议的酚类化合物进行了检测研究。实验开始时，根据观察到的最高传感器频率值确定传感器-分析物对。因此，根据对 5 × 10-5 M 分析物的最高传感器响应，PNP（17.8 Hz）和 MNP（3.8 Hz）的传感器-分析物对被确定为 QCM-5。此外，对于 PHE 和 PCP，QCM-11 和 QCM-1 传感器的最高响应分别为 4.1 Hz 和 4.0 Hz。在进一步的实验中，确定的传感器-分析物对在不同的分析物浓度下进行了测试。此外，根据不同的分析物浓度研究计算出了传感器的检测限 (LOD)，如针对 PNP、PHE、PCP 和 MNP 的检测限分别为 0.580（QCM-5）、0.659（QCM-11）、0.490（QCM-1）和 0.466（QCM-5）毫摩尔。根据吸附动力学评估了传感器-分析物对之间的相互作用。结果表明，传感器响应与分析物浓度之间的关系与 Freundlich 等温线高度一致。此外，还对传感器进行了可重复性和稳定性测试，结果表明传感器具有良好的可重复性和稳定性。最后，对分析物之间的选择性进行了评估，观察到 QCM-4 传感器对对硝基苯酚的选择性最高。研究发现，该传感器对对硝基苯酚的选择性是 PHE 和 PCP 的 21.1 倍，是 MNP 的 74 倍。

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来源期刊

Research on Chemical Intermediates 化学-化学综合

CiteScore

5.70

自引率

18.20%

发文量

229

审稿时长

2.6 months

期刊介绍： Research on Chemical Intermediates publishes current research articles and concise dynamic reviews on the properties, structures and reactivities of intermediate species in all the various domains of chemistry. The journal also contains articles in related disciplines such as spectroscopy, molecular biology and biochemistry, atmospheric and environmental sciences, catalysis, photochemistry and photophysics. In addition, special issues dedicated to specific topics in the field are regularly published.