CN106770602A - The detection method of micro 1 methylimidazole in a kind of glyoxaline ion liquid - Google Patents
The detection method of micro 1 methylimidazole in a kind of glyoxaline ion liquid Download PDFInfo
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- CN106770602A CN106770602A CN201710154632.7A CN201710154632A CN106770602A CN 106770602 A CN106770602 A CN 106770602A CN 201710154632 A CN201710154632 A CN 201710154632A CN 106770602 A CN106770602 A CN 106770602A
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Abstract
The invention discloses a kind of detection method of micro 1 methylimidazole in glyoxaline ion liquid, the detection method uses cyclic voltammetry, with glass-carbon electrode as working electrode, platinum filament be to electrode, Ag/Ag+Electrode is reference electrode, and interior reference liquid is the mixed solution of the glyoxaline ion liquid containing 0.1M silver nitrates and acetonitrile, an external salt bridge for being built-in with glyoxaline ion liquid；Operating parameter：Sweep speed is 10 mV s‑1, relative to Ag/Ag+Electrode sweep limits is 0.2 to 1.45 V, and take-off potential is OCP, and the oxidation spike potential in the cyclic voltammetry curve of gained realizes the qualitative analysis to methylimidazole, and quantitative analysis is realized according to oxidation peak current density.It is of the invention compared with existing colorimetric method, qualitative and quantitative determination is carried out using easy, quick electrochemical method, the properties such as species, viscosity, electrical conductivity by ionic liquid zwitterion are influenceed smaller, and detection limit can reach 25 to 40 ppm, substantially increase detection sensitivity.
Description
Technical field
The present invention relates to the method for micro 1- methylimidazoles in a kind of utilization cyclic voltammetry detection glyoxaline ion liquid.
Background technology
Ionic liquid at room temperature has many unique properties, such as larger liquid journey, relatively low vapour pressure, ion-conductance higher
Conductance and heat endurance and electrochemical window wider etc..Therefore, ionic liquid is used as organic and catalytic reaction
Green solvent, and new material prepare, extraction and separation process, electrochemical device in novel electrolyte and enzymatic and
All applied in bioprocess.However, the impurity content in ionic liquid, such as halide ion, water content, residual it is organic anti-
Raw material, gas of absorption etc. is answered to have a very big impact its physics and chemical property.Therefore, development is fast and efficiently examined
The method for surveying these impurity is extremely necessary.
For the detection of halide ion, there are the methods such as chloride ion-selective electrode, chromatography of ions and Electrochemical Detection at present.
Wherein, the feasibility of electrodes selective detection is relatively low, and although chromatography of ions has comparing sensitivity high, but its price higher
Infringement with ionic liquid to chromatographic column all limits the extensive use of this method.Thus, electrochemical method receives more
Concern, especially the context of detection in trace impurity achieve the pretty good effect of comparing.For example, document 1 report by
The detection of ppb grades of chlorion is realized using stripping voltammetry on silver disk electrode（Anal. Chem. 2004, 76, 1998-
2003.）.However, the detection of Organic Ingredients for being remained in ionic liquid is but rarely reported, just include among these imidazoles from
1- methylimidazoles in sub- liquid.Because 1- methylimidazoles can occur complex reaction with the copper chloride of ethanol, using in electronics
The position of maximum absorption band can realize the detection qualitative and quantitative to its in absorption spectra（Document 2, Green Chemistry,
2001, 3, 33-36）.However, for the detection of micro 1- methylimidazoles, this method just has larger error.And
And, in reality, a process for purifying is had for the villaumite or bromide of precursor during prepared by ionic liquid, this
The content of the 1- methylimidazoles remained in product can be wherein reduced, so the 1- methylimidazoles remained in most of product are all micro-
Amount.
In sum, the detection side of 1- methylimidazoles micro in detection glyoxaline ion liquid efficiently, easy is developed
Method has very great meaning, especially with the method for electrochemistry.
The content of the invention
It is an object of the invention to provide a kind of detection method of micro 1- methylimidazoles in glyoxaline ion liquid.
The present invention is working electrode using glass-carbon electrode, and cyclic voltammetry is detection technique.Because 1- methylimidazoles have admittedly
Fixed oxidizing potential, with Ag/Ag+When electrode is reference electrode, its oxidation spike potential is 1 ± 0.05 V, can be realized accordingly
The qualitative analysis of 1- methylimidazoles, and oxidation peak current density can set up standard song with 1- methylimidazoles in the range of finite concentration
Line, realizes the quantitative analysis to 1- methylimidazoles.
The detection method of micro 1- methylimidazoles in a kind of glyoxaline ion liquid, it is characterised in that the detection method is used
Cyclic voltammetry, with glass-carbon electrode as working electrode, platinum filament be to electrode, Ag/Ag+Electrode is reference electrode, and interior reference liquid is
The mixed solution of glyoxaline ion liquid and acetonitrile containing 0.1M silver nitrates, external one is built-in with glyoxaline ion liquid
Salt bridge；Operating parameter：Sweep speed is 10 mV s-1, relative to Ag/Ag+Electrode sweep limits is -0.2 to 1.45 V, starting
Current potential is OCP, and the oxidation spike potential in the cyclic voltammetry curve of gained realizes the qualitative analysis to methylimidazole,
Quantitative analysis is realized according to oxidation peak current density.
The glass-carbon electrode through 30-50 nm alumina powder polishing, salpeter solution successively in 6M, acetone, deionization
It is cleaned by ultrasonic in water, ethanol and acetonitrile 30-40 minutes, then 80-90 degree makes after drying 20-30 minutes in the vacuum drying chamber
With.
The glyoxaline ion liquid containing 0.1M silver nitrates is 9 with the volume ratio of acetonitrile：1.
In the detection method, test system is placed in glove box, and wherein water content and oxygen content are below 1 ppm.
In the detection method, to being passed through in system high pure nitrogen 30-40 minutes before test.
The lowest detection of the 1- methylimidazoles is limited to 25-40 ppm.
Implementation process of the present invention is：Volt-ampere test is circulated in glove box using three-electrode system.Wherein, glass carbon electricity
Pole（A diameter of 2 mm）Used as working electrode, platinum filament is used as to electrode, Ag/Ag+Electrode is used as reference electrode.Working electrode is being surveyed
Before examination, it is processed by shot blasting using the alumina powder of 30-50 nm, salpeter solution then successively in 6M, acetone, deionization
Ultrasonically treated 30 minutes in water, ethanol and acetonitrile, then 80 degree of dryings 30 minutes in vacuum drying chamber.The interior reference of reference electrode
Liquid is the mixed solution of the acetonitrile containing 0.1 M silver nitrates and ionic liquid to be measured（Volume ratio is 1：9）, it is external equipped with it is to be measured from
The salt bridge of sub- liquid.Before test, testing sample first leads to high pure nitrogen 30 minutes, is then tested.Take-off potential is set to
OCP, sweep speed is 10 mV s-1, sweep limits is -0.2 to 1.45 V.The determination of detection limit and building for standard curve
It is vertical to use standard addition method, pure 1- methylimidazoles are injected in testing sample using the microsyringe of 10 uL.
The present invention can realize the decomposition electricity of the decomposition voltage higher than 1- methylimidazoles of the anion based on glyoxaline cation
The detection of 1- methylimidazoles in the ionic liquid of pressure.
It is of the invention that qualitative and quantitative determination is carried out using easy, quick electrochemical method compared with existing colorimetric method,
The properties such as species, viscosity, electrical conductivity by ionic liquid zwitterion are influenceed smaller, and detection limit can reach 25 to 40
Ppm, substantially increases detection sensitivity.
Brief description of the drawings
Fig. 1：（a）[EMIm]BF4In containing different 1- methylimidazoles concentration cyclic voltammetry curve（Abbreviation CV）；（b）First
The current density of individual oxidation peak and the linear relationship of 1- methylimidazole concentration.
Fig. 2：（a）[EMIm]NTf2In containing different 1- methylimidazoles concentration CV curves；（b）First electric current of oxidation peak
The linear relationship of density and 1- methylimidazole concentration.
Fig. 3：（a）[BMIm]PF6In containing different 1- methylimidazoles concentration CV curves；（b）First electric current of oxidation peak
The linear relationship of density and 1- methylimidazole concentration.
Specific embodiment
In order to be better understood from the present invention, further it is illustrated with reference to embodiment, but these embodiments should not be managed
It is any limitation of the invention to solve.
Embodiment 1
1- ethyl-3-methylimidazole tetrafluoroborates（[EMIm]BF4）The detection of middle 1- methylimidazoles, used in reference electrode
Ionic liquid is [EMIm] BF4.[EMIm] BF of 6.0982 g4Other gases 30 minutes for dissolving are removed with high pure nitrogen, is used
By polishing and the ultrasonically treated and vacuum drying glass-carbon electrode conduct in 6M nitric acid, acetone, deionized water, ethanol and acetonitrile
Working electrode, platinum filament is used as to electrode, Ag/Ag+Electrode is used as reference electrode.1- first is injected using the microsyringe of 10 uL
Base imidazoles, 0.2 uL, increases successively every time.Be can see from Fig. 1 a, 1- methylimidazoles are 0.95（Peak A）With 1.26 V（Peak
B）There is an appearance of individual oxidation peak at place respectively, and peak current density gradually increases with the increase of 1- methylimidazole contents.Such as Fig. 1 b
Shown, the concentration of current density and 1- methylimidazoles according to peak A is set up has good line in standard curve, 28-669 ppm
Sexual intercourse（y=0.217x+11.336, R2=0.9994）, and lowest detection is limited to 28 ppm.
Embodiment 2
1- ethyl-3-methylimidazoles are double（Fluoroform sulphonyl）Inferior amine salt（[EMIm]NTf2）The detection of middle 1- methylimidazoles.Ginseng
It is [EMIm] NTf than ionic liquid used in electrode2.[EMIm] BF of 6.3057 g4Remove what other dissolved with high pure nitrogen
Gas 30 minutes, using ultrasonically treated and vacuum is dry by polishing and in 6M nitric acid, acetone, deionized water, ethanol and acetonitrile
, used as working electrode, platinum filament is used as to electrode, Ag/Ag for dry glass-carbon electrode+Electrode is used as reference electrode.Use the micro- of 10 uL
Amount injector injection 1- methylimidazoles, 0.2 uL, increases successively every time.Be can see from Fig. 2 a, 1- methylimidazoles are 1.08
（Peak A）With 1.37 V（Peak B）Place has individual oxidation peak to occur respectively, and peak current density is with the increase of 1- methylimidazole contents
Gradually increase.As shown in Figure 2 b, according to peak A current density and the concentration of 1- methylimidazoles sets up standard curve, 74-700
There is good linear relationship in ppm（y=0.065x+7.6073, R2=0.9982）, there is another in the concentration less than 74 ppm
One linear relationship occurs（y=0.3076x+9.9987, R2=0.935）, and lowest detection is limited to 28 ppm.
Embodiment 3
1- butyl -3- methylimidazole hexafluorophosphates（[BMIm]PF6）The detection of middle 1- methylimidazoles.Used in reference electrode
Ionic liquid is [BMIm] PF6.[BMIm] PF of 4.6146 g6Other gases 30 minutes for dissolving are removed with high pure nitrogen, is used
By polishing and the ultrasonically treated and vacuum drying glass-carbon electrode conduct in 6M nitric acid, acetone, deionized water, ethanol and acetonitrile
Working electrode, platinum filament is used as to electrode, Ag/Ag+Electrode is used as reference electrode.1- first is injected using the microsyringe of 10 uL
Base imidazoles, 0.2 uL, increases successively every time.Be can see from Fig. 3 a, 1- methylimidazoles are 1.05（Peak A）With 1.35 V（Peak
B）There is an appearance of individual oxidation peak at place respectively, and peak current density gradually increases with the increase of 1- methylimidazole contents.Such as Fig. 3 b
Shown, the concentration of current density and 1- methylimidazoles according to peak A is set up has good line in standard curve, 34-680 ppm
Sexual intercourse（y=0.036x+1.9985, R2=0.9991）, and lowest detection is limited to 34 ppm.
Claims (6)
1. in a kind of glyoxaline ion liquid micro 1- methylimidazoles detection method, it is characterised in that the detection method is using following
Ring voltammetry, with glass-carbon electrode as working electrode, platinum filament be to electrode, Ag/Ag+Electrode is reference electrode, interior reference liquid be containing
There are the glyoxaline ion liquid of 0.1M silver nitrates and the mixed solution of acetonitrile, the external salt for being built-in with glyoxaline ion liquid
Bridge；Operating parameter：Sweep speed is 10 mV s-1, relative to Ag/Ag+Electrode sweep limits is -0.2 to 1.45 V, starting electricity
Position is OCP, and the oxidation spike potential in the cyclic voltammetry curve of gained realizes the qualitative analysis to methylimidazole, root
Quantitative analysis is realized according to oxidation peak current density.
2. detection method as claimed in claim 1, it is characterised in that the glass-carbon electrode is thrown through the alumina powder of 30-50 nm
It is cleaned by ultrasonic 30-40 minutes in light, salpeter solution successively in 6M, acetone, deionized water, ethanol and acetonitrile, then in vacuum
80-90 degree is used after drying 20-30 minutes in drying box.
3. detection method as claimed in claim 1, it is characterised in that the glyoxaline ion liquid containing 0.1M silver nitrates
It is 9 with the volume ratio of acetonitrile：1.
4. detection method as claimed in claim 1, it is characterised in that in the detection method, test system is placed in glove box
Interior, wherein water content and oxygen content are below 1 ppm.
5. detection method as claimed in claim 1, it is characterised in that in the detection method, to being passed through height in system before test
Pure nitrogen gas 30-40 minutes.
6. detection method as claimed in claim 1, it is characterised in that the lowest detection of the 1- methylimidazoles is limited to 25-40
ppm。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111349047A (en) * | 2020-03-03 | 2020-06-30 | 扬州大学 | Carbon paste ion selective electrode and preparation method and application thereof |
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| CN101284211A (en) * | 2008-06-02 | 2008-10-15 | 中国科学院过程工程研究所 | Glyoxaline ion liquid reclaiming agent regeneration and cyclic utilization method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349047A (en) * | 2020-03-03 | 2020-06-30 | 扬州大学 | Carbon paste ion selective electrode and preparation method and application thereof |
| CN111349047B (en) * | 2020-03-03 | 2022-06-14 | 扬州大学 | Carbon paste ion selective electrode and preparation method and application thereof |
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