{"title":"Calixarene films on QCM via electrospin coating for real-time monitoring of phenolic species in aqueous media","authors":"Farabi Temel","doi":"10.1007/s11164-024-05422-2","DOIUrl":null,"url":null,"abstract":"<div><p>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 <i>p</i>-nitrophenol (PNP), phenol (PHE), <i>p</i>-chlorophenol (PCP), and <i>m</i>-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 (<sup>1</sup>H-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<sup>–5</sup> 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 <i>p</i>-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.</p><h3>Graphical abstract</h3>\n<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":753,"journal":{"name":"Research on Chemical Intermediates","volume":"50 12","pages":"6031 - 6052"},"PeriodicalIF":2.8000,"publicationDate":"2024-10-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Research on Chemical Intermediates","FirstCategoryId":"92","ListUrlMain":"https://link.springer.com/article/10.1007/s11164-024-05422-2","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
引用次数: 0
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.
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.
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