高温红外光谱电化学薄层池的制作与表征
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摘要
为了拓宽光谱电化学研究范围,开展高温下电化学反应过程,本文研制了一种高温红外光谱电化学薄层池(HTC)。研制的HTC清洗方便,操作简单,适用于水体系和有机体系。该HTC可在室温至373 K(根据溶剂沸点,控温精度为±0. 5 K)温度范围内使用,具有良好的电化学性能,红外光谱采集谱图清晰信噪比好。利用铁氰化钾水溶液和对苯醌离子液体溶液的红外光谱电化学行为对HTC进行了表征,得到较满意的结果。
In order to investigate electrochemical process at elevated temperature,a high temperature thinlayer cell (HTC) was constructed for in situ infrared (IR) spectroelectrochemistry. It works very well in the temperature range from ambient to 373 K (depend on boiling point of solvent) with the control precision within± 0. 5 K to apply for room-temp and high-temp in situ IR spectroelectrochemistry. The cell can be facilely cleaned and conveniently manipulated in both aqueous and non-aqueous system. The electrochemical and IR performance were characterized with K_3[Fe(CN)_6]in aqueous and with benzoquinone (BQ) in ionic liquid BMIMPF_6 by cyclic voltammetry and in situ IR spectroelectrochemistry at various temperature. Experimental results suggest that the cell has an excellent electrochemical performance within wider range of temperature,and good signal-noise ratio for IR absorption peaks during cyclic voltammetry (CV) scan. In conclusion,HTC has a promising application in electrochemical process in which the temperature plays an important role.
In order to investigate electrochemical process at elevated temperature,a high temperature thinlayer cell (HTC) was constructed for in situ infrared (IR) spectroelectrochemistry. It works very well in the temperature range from ambient to 373 K (depend on boiling point of solvent) with the control precision within± 0. 5 K to apply for room-temp and high-temp in situ IR spectroelectrochemistry. The cell can be facilely cleaned and conveniently manipulated in both aqueous and non-aqueous system. The electrochemical and IR performance were characterized with K_3[Fe(CN)_6]in aqueous and with benzoquinone (BQ) in ionic liquid BMIMPF_6 by cyclic voltammetry and in situ IR spectroelectrochemistry at various temperature. Experimental results suggest that the cell has an excellent electrochemical performance within wider range of temperature,and good signal-noise ratio for IR absorption peaks during cyclic voltammetry (CV) scan. In conclusion,HTC has a promising application in electrochemical process in which the temperature plays an important role.
引文
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[18]Jin B K,Huang J L,Zhao A K,et al.Direct Evidence of Hydrogen-bonding and/or Protonation Effect on p-Benzoquinone Electrochemical Reduction by in situ IR Spectroelectrochemical Study[J].J Electroanal Chem,2010,650(1):116-126.
[19]Kim Y O,Jung Y M,Kim S B,et al.Two-Dimensional Correlation Analysis of Spectroelectrochemical Data for p-Benzoquinone Reduction in Acetonitrile[J].Anal Chem,2004,76(17):5236-5240.
[20]LI Tong,JIN Baokang.Electrochemical Redox of Benzoquinone in Ionic Liquids[J].Chem J Chinese Univ,2014,35(4):847-852(in Chinese).李彤,金葆康.离子液体中对苯醌的电化学行为[J].高等学校化学学报,2014,35(4):847-852.
[21]Wang Y J,Rogers E I,Belding S R,et al.The Electrochemical Reduction of 1,4-Benzoquinone in 1-Ethyl-3-methylimidazolium Bis(trifluoromethane-sulfonyl)-imide,C(2)mim NTf2:A Voltammetric Study of the Comproportionation Between Benzoquinone and the Benzoquinone Dianion[J].J Electroanal Chem,2010,648(2):134-142.
[2]Jin B K,Li L,Huang J L,et al.IR Spectroelectrochemical Cyclic Voltabsorptometry and Derivative Cyclic Voltabsorptometry[J].Anal Chem,2009,81(11):4476-4481.
[3]Liu P,Jin B K,Cheng F L.A Low Temperature in situ Infrared Reflected Absorbance Spectroelectrochemical(LT IRRAS)Cell[J].J Electroanal Chem,2007,603(2):269-274.
[4]Zavarine I S,Kubiak C P.A Versatile Variable Temperature Thin Layer Reflectance Spectroelectrochemical Cell[J].JElectroanal Chem,2001,495(2):106-109.
[5]Mahabiersing T,Luyten H,Nieuwendam R C,et al.Synthesis,Spectroscopy and Spectroelectrochemistry of Chlorocarbonyl{1,2-Bis[(2,6-diisopropylphenyl)imino]acenaphthene-κ2-N,N'}rhodium(I)[J].Collect Czec Chem Commun,2003,68(9):1687-1709.
[6]Laviron E.The Use of Polarography and Cyclic Voltammetry for the Study of Redox Systems with Adsorption of the Reactants.Heterogeneous vs.Surface Path[J].J Electroanal Chem,1995,382(1995):111-127.
[7]Brown A P,Ason F C.Cyclic and Differential Pulse Voltammetric Behavior of Reactants Confined to the Electrode Surface[J].Anal Chem,1977,49(11):1589-1595.
[8]ZHAO Zhi,TIAN Peng,CHEN Qingyang,et al.Study of the Application of Ionic Liquids[J].Chinese J Shandong Chem Ind,2017,46(2):42-43(in Chinese).赵智,田鹏,陈庆阳,等.离子液体应用概述[J].山东化工,2017,46(2):42-43.
[9]Da Silva L C O,Soares B G.New all Solid-state Polymer Electrolyte Based on Epoxy Resin and Ionic Liquid for High Temperature Applications[J].J Appl Polym Sci,2018,135(9):45838.
[10]Paravannoor A,Augustine C A.Interfacial Properties of Alloy Anodes in Combination with Room Temperature Ionic Liquid Electrolytes:A Review Based on Li Secondary Batteries[J].J Electroanal Chem,2017,805:98-109.
[11]Seyedlar A O,Martins J P D,Sebastiao P J,et al.Dynamics of Binary Mixtures of an Ionic Liquid and Ethanol by NMR[J].Magn Reson Chem,2018,56(2):108-112.
[12]Wu T Y,Su S G,Chiu C L,et al.Impact of Polyethyleneglycol Addition on Diffusion Coefficients in Binary Ionic Liquid Electrolytes Composed of Dicationic Ionic Liquid and Polyethyleneglycol[J].Magn Reson Chem,2018,56(2):86-94.
[13]YAN Hua,ZHANG Hongmei,ZHANG Lijing,et al.Research Progress of Ionic Liquids[J].Chinese J Shandong Chem Ind,2016,45(23):55-57(in Chinese).闫华,张红梅,张丽静,等.离子液体研究进展[J].山东化工,2016,45(23):55-57.
[14]ZHANG Suojiang,XU Chunming,LV Xingmei,et al.Ionic Liquids and Green Chemistry[M].Beijing:Science Press,2008:524-533(in Chinese).张锁江,徐春明,吕兴梅,等.离子液体与绿色化学[M].北京:科学出版社,2008:524-533.
[15]ZHUANG Qiankun,CHEN Hongyuan.The Temperature Effect of Microelectrode and Its Applications to the Determination of Kinetic Parameters[J].Chem J Chinese Univ,1996,17(2):224-226(in Chinese).庄乾坤,陈洪渊.微电极的温度效应及其在动力学参数测定中的应用[J].高等学校化学学报,1996,17(2):224-226.
[16]Pons S,Datta M,Mcaieer J F,et al.Infrared Spectroelectrochemical of the Fe(CN)4-6/Fe(CN)3-6Redox System[J].JElectroanal Chem,1984,160:369-376.
[17]Astuti Y,Topoglidis E,Briscoe P B,et al.Proton-Coupled Electron Transfer of Flavodoxin Immobilized on Nanostructured Tin Dioxide Electrodes:Thermodynamics Versus Kinetics Control of Protein Redox Function[J].J Am Chem Soc,2004,126(25):8001-8009.
[18]Jin B K,Huang J L,Zhao A K,et al.Direct Evidence of Hydrogen-bonding and/or Protonation Effect on p-Benzoquinone Electrochemical Reduction by in situ IR Spectroelectrochemical Study[J].J Electroanal Chem,2010,650(1):116-126.
[19]Kim Y O,Jung Y M,Kim S B,et al.Two-Dimensional Correlation Analysis of Spectroelectrochemical Data for p-Benzoquinone Reduction in Acetonitrile[J].Anal Chem,2004,76(17):5236-5240.
[20]LI Tong,JIN Baokang.Electrochemical Redox of Benzoquinone in Ionic Liquids[J].Chem J Chinese Univ,2014,35(4):847-852(in Chinese).李彤,金葆康.离子液体中对苯醌的电化学行为[J].高等学校化学学报,2014,35(4):847-852.
[21]Wang Y J,Rogers E I,Belding S R,et al.The Electrochemical Reduction of 1,4-Benzoquinone in 1-Ethyl-3-methylimidazolium Bis(trifluoromethane-sulfonyl)-imide,C(2)mim NTf2:A Voltammetric Study of the Comproportionation Between Benzoquinone and the Benzoquinone Dianion[J].J Electroanal Chem,2010,648(2):134-142.
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