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Detection method of trace 1-methylimidazole in imidazole ionic liquid

A detection method and technology of ionic liquids, which can be used in measurement devices, electrochemical variables of materials, instruments, etc., can solve problems such as large errors, and achieve the effect of improving detection sensitivity, rapid qualitative and quantitative detection

Inactive Publication Date: 2017-05-31
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, for the detection of trace amounts of 1-methylimidazole, this method has a large error

Method used

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  • Detection method of trace 1-methylimidazole in imidazole ionic liquid
  • Detection method of trace 1-methylimidazole in imidazole ionic liquid
  • Detection method of trace 1-methylimidazole in imidazole ionic liquid

Examples

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Effect test

Embodiment 1

[0021] 1-Ethyl-3-methylimidazolium tetrafluoroborate ([EMIm]BF 4 ) for the detection of 1-methylimidazole, the ionic liquid used in the reference electrode is [EMIm]BF 4 . 6.0982 g of [EMIm]BF 4 Remove other dissolved gases with high-purity nitrogen for 30 min, use a glassy carbon electrode that has been polished and sonicated and vacuum-dried in 6M nitric acid, acetone, deionized water, ethanol, and acetonitrile as the working electrode, platinum wire as the counter electrode, Ag / Ag + electrode as a reference electrode. Use a 10 uL microsampler to inject 1-methylimidazole, 0.2 uL each time, increasing successively. From figure 1 In a, it can be seen that 1-methylimidazole has an oxidation peak at 0.95 (peak A) and 1.26 V (peak B), respectively, and the peak current density gradually increases with the increase of 1-methylimidazole content. Such as figure 1 As shown in b, a standard curve is established according to the current density of peak A and the concentration o...

Embodiment 2

[0023] 1-Ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt ([EMIm]NTf 2 ) detection of 1-methylimidazole. The ionic liquid used in the reference electrode is [EMIm]NTf 2 . 6.3057 g of [EMIm]BF 4 Remove other dissolved gases with high-purity nitrogen for 30 min, use a glassy carbon electrode that has been polished and sonicated and vacuum-dried in 6M nitric acid, acetone, deionized water, ethanol, and acetonitrile as the working electrode, platinum wire as the counter electrode, Ag / Ag + electrode as a reference electrode. Use a 10 uL microsampler to inject 1-methylimidazole, 0.2 uL each time, increasing successively. From figure 2 In a, it can be seen that 1-methylimidazole has an oxidation peak at 1.08 (peak A) and 1.37 V (peak B), respectively, and the peak current density gradually increases with the increase of 1-methylimidazole content. Such as figure 2 As shown in b, a standard curve is established according to the current density of peak A and ...

Embodiment 3

[0025] 1-Butyl-3-methylimidazolium hexafluorophosphate ([BMIm]PF 6 ) detection of 1-methylimidazole. The ionic liquid used in the reference electrode is [BMIm]PF 6 . 4.6146 g of [BMIm]PF 6 Remove other dissolved gases with high-purity nitrogen for 30 min, use a glassy carbon electrode that has been polished and sonicated and vacuum-dried in 6M nitric acid, acetone, deionized water, ethanol, and acetonitrile as the working electrode, platinum wire as the counter electrode, Ag / Ag + electrode as a reference electrode. Use a 10 uL microsampler to inject 1-methylimidazole, 0.2 uL each time, increasing successively. From image 3 In a, it can be seen that 1-methylimidazole has an oxidation peak at 1.05 (peak A) and 1.35 V (peak B), respectively, and the peak current density gradually increases with the increase of 1-methylimidazole content. Such as image 3 As shown in b, a standard curve is established according to the current density of peak A and the concentration of 1-m...

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Abstract

The invention discloses a detection method of trace 1-methylimidazole in an imidazole ionic liquid. The detection method adopts cyclic voltammetry: a glassy carbon electrode is used as the work electrode, a platinum filament is used as the counter electrode, an Ag / Ag<+> electrode is used as the reference electrode, the internal reference solution is an imidazole ionic liquid / acetonitrile mixed solution containing 0.1M silver nitrate, and a salt bridge filled with an imidazole ionic liquid is externally connected. The operating parameters are as follows: the scanning speed is 10mV s<-1>, the scanning range relative to the Ag / Ag<+> electrode is -0.2-1.45V, the starting potential is open circuit potential, the qualitative analysis on methylimidazole is implemented according to the obtained oxidation peak potential in the circulating cyclic voltammetry curve, and the quantitative analysis is implemented according to the oxidation peak current density. Compared with the existing colorimetry, the method adopts the simple quick electrochemical process to perform qualitative and quantitative detection, and thus, is slightly influence by the variety, viscosity, electric conductivity and other properties of the negative and positive ions in the ionic liquid. The detection limit can reach 25-40 ppm, and thus, the detection sensitivity is greatly enhanced.

Description

technical field [0001] The invention relates to a method for detecting trace amounts of 1-methylimidazole in imidazole ionic liquids by means of cyclic voltammetry. Background technique [0002] Room temperature ionic liquids have many unique properties, such as large liquid range, low vapor pressure, high ionic conductivity and thermal stability, and wide electrochemical window. Therefore, ionic liquids are used as green solvents for organic and catalytic reactions, and have applications in new material preparation, extraction and separation processes, novel electrolytes in electrochemical devices, and enzymatic catalysis and biological processes. However, the content of impurities in ionic liquids, such as halide ions, water content, residual organic reaction raw materials, adsorbed gases, etc., has a great influence on their physical and chemical properties. Therefore, it is necessary to develop fast and efficient methods for detecting these impurities. [0003] For the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/48G01N27/30G01N27/38
CPCG01N27/48G01N27/308G01N27/38
Inventor 邓友全倪文鹏刘士民何昱德马祥元卢六斤
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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