CN106556632A - A kind of preparation method of modified glassy carbon electrode - Google Patents
A kind of preparation method of modified glassy carbon electrode Download PDFInfo
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- CN106556632A CN106556632A CN201610989362.7A CN201610989362A CN106556632A CN 106556632 A CN106556632 A CN 106556632A CN 201610989362 A CN201610989362 A CN 201610989362A CN 106556632 A CN106556632 A CN 106556632A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
The invention discloses a kind of preparation method of modified glassy carbon electrode.The decorative material that the preparation method is obtained is stable, and favorable reproducibility, strong antijamming capability.The modified electrode that the preparation method of the present invention is obtained can be to the common of uric acid, xanthine and secondary purine while detection has good sensitivity.
Description
Technical field
The present invention relates to electrode technology field, more particularly to a kind of preparation method of modified glassy carbon electrode.
Background technology
Xanthine (XA) is called 2,6- xanthines, is important base in ribonucleic acid, and purine nucleotides drop
The intermediate product of solution approach.Xanthine oxidase can be catalyzed XA and generate uric acid.So, xanthic content can directly affect body
Internal uric acid content.Hypoxanthine is also called hypoxanthine, and it and xanthine are all the derivatives of purine, containing common
Purine precursors.Uric acid, xanthine and secondary purine together, are coexisted in the organ and body fluid of human body and animal.UA, XA and HX are in body
The change of interior content, can directly affect the physiological function of human body.For the measurement of three's content, it is also possible to detect and purine
The related disease of metabolism, such as gout, hyperuricemia and angiocardiopathy etc..Therefore, for uric acid, xanthine and secondary purine
Determine, it is medically significant.At present, for the detection method of uric acid, xanthine and secondary purine mainly has capillary electricity
Swimming method, high performance liquid chromatography, spectroscopic methodology etc..
Graphene film from 2004 by Novoselov etc. with mechanical stripping preparation since, its unique structure and excellent
The focus that performance is studied in being quickly become each ambit.But because Van der Waals force is susceptible to group between graphene film and piece
It is poly-, limit the extensive application of Graphene.
At present, for Graphene carries out the common method that functionalization is this defect of solution.Using functional method, in stone
Black alkene surface or edge introduce specific group Molecule, make Graphene have more performances to expand its application.Polydiene
Diallyidimethylammonium chloride (PDDA) is a kind of very strong cationic polymer, common-use words modification and functionalized nano material.
PDDA can be interacted by π-π with Graphene and is connected, and make Graphene can be good at disperseing in water, expanded Graphene
Application in Electroanalytical Chemistry.CNT (CNT) has been obtained in Electroanalytical Chemistry extensively since 1991 are found
Application.The exclusive surface electronic micro-structural of CNT, can accelerate the electronics movement on chemically modified electrode, embody excellent
Elegant chemical property.
The content of the invention
It is an object of the invention to propose a kind of preparation method of modified glassy carbon electrode, polydiene dimethylamine can be obtained
Ammonium chloride-Graphene/multi-walled carbon nano-tubes compound, is prepared into electrode, and uric acid, xanthine and secondary purine are entered simultaneously
Row is determined, and is worked well.
It is that, up to this purpose, the present invention is employed the following technical solutions：
A kind of preparation method of modified glassy carbon electrode, including：
(1), under condition of ice bath, under mechanical agitation, crystalline graphite powder is added in 98% concentrated sulfuric acid, add and account for
The sodium nitrate of graphite powder 50-80wt%, and to account for and react 30-120min under the potassium permanganate of 2-4 times of weight of Graphene, ice bath；
(2) 30-40 DEG C of constant temperature 4-5h is heated to, deionized water and hydrogen peroxide is added, 1-3h is stirred, 5% concentration is added
HCl centrifuge washings are until sulfate radical-free ion, obtains graphene oxide powder；
(3) the graphene oxide powder ultrasonic disperse is configured as the unit for uniform suspension of 0.3-1g/L, poly- two are added
Allyl dimethyl ammonium chloride, stirs, and is subsequently added hydrazine hydrate, is uniformly mixing to obtain mixed liquor；
(4) mixed liquor is warmed up to into 95-110 DEG C in closed reactor, reacts 2-5 hours, after centrifugal drying
To diallyl dimethyl ammoniumchloride-Graphene；
(5) by the diallyl dimethyl ammoniumchloride-Graphene ultrasonic disperse in water, add multi-wall carbon nano-tube
Pipe, ultrasonic vibration dispersion soln obtain diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution；
(6) with the diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution drop coating glass carbon
Electrode surface, obtains the modified glassy carbon electrode after drying.
Preferably, the glass-carbon electrode was pre-processed before drop coating, and the pretreatment is：Glass-carbon electrode is polished
The grinding of powder suspension, polishing, then it is ultrasonically treated in ethanol and secondary water successively, subsequently dried up with inert gas, obtain glass carbon
Electrode.
Using standard three electrode system, platinum electrode is the modification glass carbon that the method for the invention is prepared to electrode
Electrode is working electrode, and Ag/AgCl electrodes are reference electrode.Electrode test is carried out with cyclic voltammetric (CV), CV sweeps speed when determining
For 100mV/s, buffer solution used is the PBS (pH4.0) of 0.1mol/L, uric acid, xanthine and secondary purine is measured, continuously
After 100 circle of scanning, decorative material is stable, and favorable reproducibility, strong antijamming capability.The modification electricity that the preparation method of the present invention is obtained
Pole can be to the common of uric acid, xanthine and secondary purine while detection has good sensitivity.
Specific embodiment
Technical scheme is further illustrated below by specific embodiment.
Embodiment 1
A kind of preparation method of modified glassy carbon electrode, including：
(1), under condition of ice bath, under mechanical agitation, crystalline graphite powder is added in 98% concentrated sulfuric acid, add and account for
The sodium nitrate of graphite powder 50wt%, and to account for and react 30min under the potassium permanganate of 2 times of weight of Graphene, ice bath；
(2) 30 DEG C of constant temperature 4h are heated to, deionized water and hydrogen peroxide is added, 1h is stirred, the HCl centrifugations of 5% concentration are added
Washing is until sulfate radical-free ion, obtains graphene oxide powder；
(3) the graphene oxide powder ultrasonic disperse is configured as the unit for uniform suspension of 0.3g/L, polydiene is added
Diallyidimethylammonium chloride, stirs, and is subsequently added hydrazine hydrate, is uniformly mixing to obtain mixed liquor；
(4) mixed liquor is warmed up to into 95 DEG C in closed reactor, reacts 2 hours, after centrifugal drying, obtain poly- two
Allyl dimethyl ammonium chloride-Graphene；
(5) by the diallyl dimethyl ammoniumchloride-Graphene ultrasonic disperse in water, add multi-wall carbon nano-tube
Pipe, ultrasonic vibration dispersion soln obtain diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution；
(6) with the diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution drop coating glass carbon
Electrode surface, obtains the modified glassy carbon electrode after drying.
Embodiment 2
A kind of preparation method of modified glassy carbon electrode, including：
(1), under condition of ice bath, under mechanical agitation, crystalline graphite powder is added in 98% concentrated sulfuric acid, add and account for
The sodium nitrate of graphite powder 80wt%, and to account for and react 120min under the potassium permanganate of 4 times of weight of Graphene, ice bath；
(2) 40 DEG C of constant temperature 5h are heated to, deionized water and hydrogen peroxide is added, 3h is stirred, the HCl centrifugations of 5% concentration are added
Washing is until sulfate radical-free ion, obtains graphene oxide powder；
(3) the graphene oxide powder ultrasonic disperse is configured as the unit for uniform suspension of 1g/L, polydiene third is added
Base alkyl dimethyl ammonium chloride, stirs, and is subsequently added hydrazine hydrate, is uniformly mixing to obtain mixed liquor；
(4) mixed liquor is warmed up to into 110 DEG C in closed reactor, reacts 5 hours, after centrifugal drying, obtain poly- two
Allyl dimethyl ammonium chloride-Graphene；
(5) by the diallyl dimethyl ammoniumchloride-Graphene ultrasonic disperse in water, add multi-wall carbon nano-tube
Pipe, ultrasonic vibration dispersion soln obtain diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution；
(6) with the diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution drop coating glass carbon
Electrode surface, obtains the modified glassy carbon electrode after drying.
Embodiment 3
A kind of preparation method of modified glassy carbon electrode, including：
(1), under condition of ice bath, under mechanical agitation, crystalline graphite powder is added in 98% concentrated sulfuric acid, add and account for
The sodium nitrate of graphite powder 60wt%, and to account for and react 90min under the potassium permanganate of 3 times of weight of Graphene, ice bath；
(2) be heated to 35 DEG C of constant temperature 4.5h, add deionized water and hydrogen peroxide, stir 2h, add the HCl of 5% concentration from
Heart washing is until sulfate radical-free ion, obtains graphene oxide powder；
(3) the graphene oxide powder ultrasonic disperse is configured as the unit for uniform suspension of 0.8g/L, polydiene is added
Diallyidimethylammonium chloride, stirs, and is subsequently added hydrazine hydrate, is uniformly mixing to obtain mixed liquor；
(4) mixed liquor is warmed up to into 100 DEG C in closed reactor, reacts 3 hours, after centrifugal drying, obtain poly- two
Allyl dimethyl ammonium chloride-Graphene；
(5) by the diallyl dimethyl ammoniumchloride-Graphene ultrasonic disperse in water, add multi-wall carbon nano-tube
Pipe, ultrasonic vibration dispersion soln obtain diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution；
(6) with the diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution drop coating glass carbon
Electrode surface, obtains the modified glassy carbon electrode after drying.
The modified electrode that preparation method described in embodiment 1-3 is prepared is surveyed to uric acid, xanthine and secondary purine
Fixed, after 100 circle of continuous scanning, decorative material is stable, and favorable reproducibility, strong antijamming capability.What the preparation method was obtained repaiies
Decorations electrode can be to the common of uric acid, xanthine and secondary purine while detection has good sensitivity.
Claims (2)
1. a kind of preparation method of modified glassy carbon electrode, including：
(1), under condition of ice bath, under mechanical agitation, crystalline graphite powder is added in 98% concentrated sulfuric acid, add and account for graphite
The sodium nitrate of powder 50-80wt%, and to account for and react 30-120min under the potassium permanganate of 2-4 times of weight of Graphene, ice bath；
(2) be heated to 30-40 DEG C of constant temperature 4-5h, add deionized water and hydrogen peroxide, stir 1-3h, add the HCl of 5% concentration from
Heart washing is until sulfate radical-free ion, obtains graphene oxide powder；
(3) the graphene oxide powder ultrasonic disperse is configured as the unit for uniform suspension of 0.3-1g/L, polydiene third is added
Base alkyl dimethyl ammonium chloride, stirs, and is subsequently added hydrazine hydrate, is uniformly mixing to obtain mixed liquor；
(4) mixed liquor is warmed up to into 95-110 DEG C in closed reactor, reacts 2-5 hours, gathered after centrifugal drying
Diallyldimethylammonium chloride-Graphene；
(5) by the diallyl dimethyl ammoniumchloride-Graphene ultrasonic disperse in water, multi-walled carbon nano-tubes is added, is surpassed
Dispersion soln is swung in acoustic shock, obtains diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution；
(6) with the diallyl dimethyl ammoniumchloride-Graphene/multi-walled carbon nano-tubes complex solution drop coating glass-carbon electrode
Surface, obtains the modified glassy carbon electrode after drying.
2. the preparation method of modified glassy carbon electrode as claimed in claim 1, it is characterised in that the glass-carbon electrode drop coating it
Before pre-processed, the pretreatment is：By glass-carbon electrode polishing powder suspension grinding, polishing, then successively in ethanol and two
It is ultrasonically treated in secondary water, subsequently dried up with inert gas, obtain glass-carbon electrode.
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Cited By (2)
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| CN108930075A (en) * | 2018-07-11 | 2018-12-04 | 苏州市天翱特种织绣有限公司 | A kind of radiation-proof fabric |
| KR102455729B1 (en) | 2021-11-11 | 2022-10-18 | 경희대학교 산학협력단 | Purine metabolite detecting substance and biosensor using same |
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| US20130288155A1 (en) * | 2012-04-30 | 2013-10-31 | Samsung Sdi Co., Ltd. | Support for electrode catalyst and method of manufacturing the same, electrode catalyst and fuel cell |
| CN104525109A (en) * | 2014-12-04 | 2015-04-22 | 甘肃省商业科技研究所有限公司 | Multi-walled carbon nanotube functionalized graphene composite material and application thereof |
| CN104614527A (en) * | 2015-01-12 | 2015-05-13 | 济南大学 | Method for establishing electrochemical immunosensor for detecting carcino-embryonic antigen |
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| US20130288155A1 (en) * | 2012-04-30 | 2013-10-31 | Samsung Sdi Co., Ltd. | Support for electrode catalyst and method of manufacturing the same, electrode catalyst and fuel cell |
| CN103033548A (en) * | 2012-12-31 | 2013-04-10 | 山东理工大学 | Fabrication method of ACHE biosensor based on composite nano-material |
| CN103033548B (en) * | 2012-12-31 | 2015-02-18 | 山东理工大学 | Fabrication method of ACHE biosensor based on composite nano-material |
| CN104525109A (en) * | 2014-12-04 | 2015-04-22 | 甘肃省商业科技研究所有限公司 | Multi-walled carbon nanotube functionalized graphene composite material and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108930075A (en) * | 2018-07-11 | 2018-12-04 | 苏州市天翱特种织绣有限公司 | A kind of radiation-proof fabric |
| KR102455729B1 (en) | 2021-11-11 | 2022-10-18 | 경희대학교 산학협력단 | Purine metabolite detecting substance and biosensor using same |
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