CN105548309B - The purposes of polycarbazole/nitrogen-doped graphene modified electrode - Google Patents
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Abstract
The invention discloses a kind of polycarbazole/nitrogen-doped graphene modified electrode and preparation method and purposes, electrode is made up of glass-carbon electrode as substrate, conducting polymer polycarbazole with nitrogen-doped graphene.The present invention makes two kinds of components of PCZ and N GE produce more obviously synergy using drop coating and polymerization two-step method acquisition PCZ/N GE modified glassy carbon electrodes so that its reduction to p-nitrophenol has stronger catalytic action, and reduction potential increase is substantially.Raw material used is easy to get, and drug dosage is few.Preparation method is simple and quick, reproducible, and the electrode environmental stability being prepared is good.
Description
The application is application number：201410360297.2, the applying date：2014.7.25, title " polycarbazole/N doping graphite
The divisional application of alkene modified electrode and preparation method and purposes ".
Technical field
The present invention relates to a kind of polycarbazole/nitrogen-doped graphene modified electrode and preparation method and purposes.
Background technology
It by the crystal structure of the compact arranged hexagonal honeycomb shape of carbon atom, thickness is only 0.35nm that graphene, which is, its base
This construction unit is most stable of benzene hexatomic ring in organic material.Preferable graphene has good electric conductivity, has relatively large
Specific surface area characteristic, thus with many unique physics, chemistry and mechanical performances, be widely used in electrochemical sensor
Field.Some hetero atoms such as N, B etc. are doped into the mechanism of graphene, destroy the preferable SP2 hydridization of carbon atom, thus is drawn
Play graphene electronic property and great change occurs for chemism.And nitrogen-atoms due in the periodic table of elements with carbon atom phase
Neighbour, and have a pair of lone pair electrons, therefore after doping, equally with good electric conductivity.And polycarbazole is as a kind of superior performance
Conducting polymer, have been widely used for multiple fields.The copolymer of polycarbazole and its derivative is already used to as electricity
Chemical sensor is used to detect dopamine.Lei Wu etc. is realized pair using the compound modified glassy carbon electrode of polycarbazole and graphene
The detection of pesticide imidacloprid.With relatively low test limit and sensitivity.Therefore, polycarbazole has more in electrochemical sensing field
It is widely applied prospect.
One of p-nitrophenol, the environmental contaminants as most serious, have been widely used for dyestuff, insecticide explosive
Deng field.Because it is to people, the special toxicity of animal and plant, and be difficult by traditional treatment method degraded, therefore
P-nitrophenol and its derivative are classified as one of 114 kinds of organic pollutions by Environmental Protection Agency.It is very must that it, which is detected,
Must.There are many methods to be used for detecting paranitrophenol, such as gas chromatography, high performance liquid chromatography, spectroscopic methodology etc. at present.
But these methods are all very complicated.It is time-consuming and costly, it is unsuitable for popularization and application.
The content of the invention
It is an object of the invention to provide a kind of excellent performance, prepare simple and rapid polycarbazole/nitrogen-doped graphene and repair
Adorn electrode and preparation method and purposes.
The present invention technical solution be：
A kind of polycarbazole/nitrogen-doped graphene modified electrode, it is characterized in that：By glass-carbon electrode as substrate, conducting polymer
Thing polycarbazole forms with nitrogen-doped graphene.
A kind of preparation method of polycarbazole/nitrogen-doped graphene modified electrode, it is characterized in that：Comprise the following steps：
(1) glass-carbon electrode is ground on 0.1 and 0.03 μm of aluminum oxide respectively smooth, done with water and acetone rinsing
Only, it is standby；
(2) a certain amount of nitrogen-doped graphene is dissolved in NN- dimethylformamides, it is scattered equal that dark-brown is formed after ultrasound
Even mixed solution；Above-mentioned mixed solution is taken, is dropped on the glass-carbon electrode handled well through step (1).Dried under infrared lamp standby
With；
(3) electrochemical polymerization selects cyclic voltammetry, and using three-electrode system, saturated calomel electrode is reference electricity
Pole, platinum electrode is that glass-carbon electrode is working electrode to electrode, and in the boron trifluoride ether solution containing carbazole, regulation is low
Current potential is -0.2~0.4V, and high potential is 1.4~1.8V, and sweep speed is 50~200mV s-1, the circle of scanning 4~12, is obtained
Modified electrode is rinsed repeatedly using second alcohol and water, and is dried up with nitrogen, and PCZ/N-GE modified electrodes are made.
A kind of polycarbazole/nitrogen-doped graphene modified electrode is used to detect p-nitrophenol, it is characterized in that：Detection method bag
Include the following steps：
PCZ/N-GE modified glassy carbon electrodes are positioned in the cushioning liquid of pH value 4.6, lead to nitrogen 10 minutes, added to nitre
Base phenol, using cyclic voltammetry, the electrochemical response of detecting electrode p-nitrophenol to environmental pollutants.
Cushioning liquid selects acetic acid and sodium acetate.P-nitrophenol concentration range is 0.8~20 μM.
Compared with prior art, its remarkable advantage is the present invention：(1) PCZ/N-GE is obtained using drop coating and polymerization two-step method
Modified glassy carbon electrode, two kinds of components of PCZ and N-GE are made to produce more obviously synergy so that its reduction to p-nitrophenol
With stronger catalytic action, reduction potential increase is obvious.Raw material used is easy to get, and drug dosage is few.Preparation method is simple
Quickly, reproducible, the electrode environmental stability being prepared is good.(2) modified electrode prepared has strong electricity on CV curves
Stream response, the Electrochemical Detection applied to p-nitrophenol have relatively low detection limit (~10-8M), and linearly dependent coefficient is
0.9971.Detection method is quick and accurate.
Brief description of the drawings
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is 1PCZ/N-GE of embodiment of the present invention preparation (carbazole gathering on nitrogen-doped graphene modified glassy carbon electrode
Close curve).
Fig. 2, Fig. 3 are the scanning electron microscope (SEM) photographs of PCZ/N-GE modified electrodes prepared by the embodiment of the present invention 1.
Fig. 4 is PCZ/N-GE modified electrodes prepared by the embodiment of the present invention 1 and other modified electrodes to p-nitrophenol
Cyclic voltammetry curve.
Fig. 5, Fig. 6 are the PCZ/N-GE modified electrodes of the preparation of the embodiment of the present invention 1 respectively to p-nitrophenol current-responsive
Cyclic voltammetry curve (0.8~20 μM), linear relationship chart.
Embodiment
Embodiment 1：
(1) glass-carbon electrode is ground on 0.1 and 0.03 μm of aluminum oxide respectively smooth, done with water and acetone rinsing
Only, it is standby.
(2) nitrogen-doped graphene (N-GE) is dissolved in N,N-dimethylformamide (DMF) middle rank and forms 2mg ml-1It is molten
Liquid.10 μ L are pipetted with accurate pipettor to drop on the glass-carbon electrode handled well, infrared lamp drying.
(3) electrochemical polymerization selects cyclic voltammetry, and using three-electrode system, saturated calomel electrode is reference electricity
Pole, platinum electrode are that the glass-carbon electrode of N-GE modifications is working electrode, in the boron trifluoride second containing 0.5mM carbazoles to electrode
In ethereal solution, regulation low potential is 0V, and high potential 1.4V, sweep speed is 100mV s-1, the circle of scanning 8, obtained modification electricity
Pole is rinsed repeatedly using second alcohol and water, and is dried up with nitrogen, and PCZ/N-GE modified electrodes are made (see Fig. 1).By N-GE and PCZ/
The glass-carbon electrode of N-GE modifications is scanned Electronic Speculum and tested (see Fig. 2, Fig. 3) respectively.Figure it is seen that N-GE has graphite
The same structure of the typical thin paper of alkene, there is larger surface area.A strata it has been polymerize on N-GE from figure 3, it can be seen that working as
After carbazole, surface has loose structure, in order to which analyte and electronics are mutually transmitted between solution and electrode.
Embodiment 2：
(1) glass-carbon electrode is ground on 0.1 and 0.03 μm of aluminum oxide respectively smooth, done with water and acetone rinsing
Only, it is standby.
(2) nitrogen-doped graphene (N-GE) is dissolved in N,N-dimethylformamide (DMF) middle rank and forms 0.5mg ml-1's
Solution.10 μ L are pipetted with accurate pipettor to drop on the glass-carbon electrode handled well, infrared lamp drying.
(3) electrochemical polymerization selects cyclic voltammetry, and using three-electrode system, saturated calomel electrode is reference electricity
Pole, platinum electrode are that the glass-carbon electrode of N-GE modifications is working electrode, in the boron trifluoride second containing 0.5mM carbazoles to electrode
In ethereal solution, regulation low potential is -0.2V, and high potential 1.4V, sweep speed is 200mV s-1, the circle of scanning 8, obtained modification
Electrode is rinsed repeatedly using second alcohol and water, and is dried up with nitrogen, and PCZ/N-GE modified electrodes are made.
Embodiment 3：
(1) glass-carbon electrode is ground on 0.1 and 0.03 μm of aluminum oxide respectively smooth, done with water and acetone rinsing
Only, it is standby.
(2) nitrogen-doped graphene (N-GE) is dissolved in a certain amount of N,N-dimethylformamide (DMF) middle rank and forms 1mg
ml-1Solution.10 μ L are pipetted with accurate pipettor to drop on the glass-carbon electrode handled well, infrared lamp drying.
(3) electrochemical polymerization selects cyclic voltammetry, and using three-electrode system, saturated calomel electrode is reference electricity
Pole, platinum electrode are that the glass-carbon electrode of N-GE modifications is working electrode, in the boron trifluoride second containing 0.5mM carbazoles to electrode
In ethereal solution, regulation low potential is 0V, and high potential 1.8V, sweep speed is 50mV s-1, the circle of scanning 8, obtained modified electrode
Rinsed using second alcohol and water, and dried up with nitrogen repeatedly, PCZ/N-GE modified electrodes are made.
Embodiment 4：By the electrode and N-GE prepared by embodiment 1, graphene (GE), polycarbazole (PCZ) and naked glass carbon electricity
Pole carries out cyclic voltammetry in 0.1mM p-nitrophenyl phenol solution.See Fig. 4.It can be seen that N-GE and PCZ are repaiied
More a lot of than naked glass carbon times of the current-responsive of the electrode of decorations, and on the electrode of N-GE modifications, the current potential of its reduction peak than
Naked glass carbon potential is big, shows also original very strong catalytic action of the N-GE to p-nitrophenol.And the electricity of PCZ/N-GE modifications
Pole is corrected than both in the strong manyfold of electric current, reduction potential again, and catalytic action is stronger, and this is mainly due to PCZ's and N-GE
Caused by synergy.Allow PCZ/N-GE modified glassy carbon electrodes to be used as a kind of electrochemical sensor, quickly and easily examine
Survey p-nitrophenol.
Embodiment 5：
PCZ/N-GE modified glassy carbon electrodes prepared by embodiment 1 are being detected into the application of environmental contaminants p-nitrophenol,
Detection method is as follows：
Obtained PCZ/N-GE modified glassy carbon electrodes are positioned in the acetate buffer solution of pH value 4.6, lead to nitrogen 10
Minute, different amounts of p-nitrophenyl phenol solution is added, using cyclic voltammetry, detecting electrode p-nitrophenol to environmental pollutants
Electrochemical response.Experimental result is shown in Fig. 5, Fig. 6.Fig. 5 is cyclic voltammetry curve.Fig. 6 be in the range of 0.8~20 μM electric current with
The concentration of p-nitrophenol is in good linear relationship.Linear relationship is Ipc (μ A)=0.6549+1.6531C (μM), phase relation
Number is limited to 0.062 μM (S/N=3) for 0.9971. detections.Show that the modified electrode has good linear pass to p-nitrophenol
System and low test limit.
Claims (4)
1. a kind of polycarbazole/nitrogen-doped graphene modified electrode is used to detect p-nitrophenol, it is characterized in that：The polycarbazole/
Nitrogen-doped graphene modified electrode is made up of glass-carbon electrode as substrate, conducting polymer polycarbazole with nitrogen-doped graphene；Inspection
Survey method comprises the following steps：
PCZ/N-GE modified glassy carbon electrodes are positioned in the cushioning liquid of pH value 4.6, lead to nitrogen 10 minutes, add p-nitrophenyl
Phenol, using cyclic voltammetry, the electrochemical response of detecting electrode p-nitrophenol to environmental pollutants；
The polycarbazole/nitrogen-doped graphene modified electrode, its preparation method comprise the following steps：
(1) glass-carbon electrode is ground on 0.1 and 0.03 μm of aluminum oxide respectively it is smooth, it is clean with water and acetone rinsing, it is standby
With；
(2) a certain amount of nitrogen-doped graphene is dissolved in NN- dimethylformamides, it is finely dispersed that dark-brown is formed after ultrasound
Mixed solution；Above-mentioned mixed solution is taken, is dropped on the glass-carbon electrode handled well through step (1)；It is dried for standby under infrared lamp；
(3) electrochemical polymerization selects cyclic voltammetry, and using three-electrode system, saturated calomel electrode is reference electrode, platinum
Silk electrode is that glass-carbon electrode is working electrode to electrode, in the boron trifluoride ether solution containing carbazole, adjusts low potential
For -0.2~0.4V, high potential is 1.4~1.8V, and sweep speed is 50~200mv/s, the circle of scanning 4~12, obtained modification electricity
Pole is rinsed repeatedly using second alcohol and water, and is dried up with nitrogen, and PCZ/N-GE modified electrodes are made.
2. polycarbazole according to claim 1/nitrogen-doped graphene modified electrode is used to detect p-nitrophenol, its feature
It is：Cushioning liquid selects acetic acid and sodium acetate.
3. polycarbazole according to claim 1/nitrogen-doped graphene modified electrode is used to detect p-nitrophenol, its feature
It is：P-nitrophenol concentration range is 0.8~20 μM.
4. polycarbazole according to claim 1/nitrogen-doped graphene modified electrode is used to detect p-nitrophenol, its feature
It is：P-nitrophenol concentration is 20 μM.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196985A (en) * | 2013-04-26 | 2013-07-10 | 黑龙江大学 | Method for measuring p-nitrophenol in water system |
| WO2013160719A8 (en) * | 2012-04-26 | 2014-01-09 | Indian Institute Of Technology Madras | Metal-alloy graphene nanocomposites and methods for their preparation and use |
| CN103808779A (en) * | 2014-01-22 | 2014-05-21 | 西北师范大学 | Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013160719A8 (en) * | 2012-04-26 | 2014-01-09 | Indian Institute Of Technology Madras | Metal-alloy graphene nanocomposites and methods for their preparation and use |
| CN103196985A (en) * | 2013-04-26 | 2013-07-10 | 黑龙江大学 | Method for measuring p-nitrophenol in water system |
| CN103808779A (en) * | 2014-01-22 | 2014-05-21 | 西北师范大学 | Method for detecting p-nitrophenol by using PDDA (Poly Diallyldimethylammonium) functionalized graphene modified glassy carbon electrode |
Non-Patent Citations (2)
| Title |
|---|
| Electrochemical determination of imidacloprid using poly(carbazole)/chemically reduced graphene oxide modified glassy carbon electrode;Wu Lei,Qiuju Wu,Weimeng Si,Zhenyan Gu,Yuehua Zhang et al.;《Sensors and Actuators B: Chemical》;20130406;第183卷;全文 * |
| Nitrogen-Doped Graphene and Its Application in Electrochemical Biosensing;Ying Wang,Yuyan Shao,Dean W. Matson,Jinghong Li and Yuehe Lin;《Acs Nano》;20100407;第4卷(第4期);全文 * |
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