CN101149353A - Carbon nano tube/ overoxidation polypyrrole composite modified electrode preparation method and uses - Google Patents
Carbon nano tube/ overoxidation polypyrrole composite modified electrode preparation method and uses Download PDFInfo
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- CN101149353A CN101149353A CNA2007100706927A CN200710070692A CN101149353A CN 101149353 A CN101149353 A CN 101149353A CN A2007100706927 A CNA2007100706927 A CN A2007100706927A CN 200710070692 A CN200710070692 A CN 200710070692A CN 101149353 A CN101149353 A CN 101149353A
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Abstract
The invention provides a kind of preparation method and its application of the carbon nanometer pipe/poly pyrrole peroxide compound modifying electrode. In the pH 7.4 solution of 0.5mg/mL multi-wall nanometer pipe and 0.2mol/L KCl containing 0.05mol/L pyrrole, it picks out the glass-carbon electrode after 8 loops of cyclic voltammetry scanning at the 0.1mV/s scanning speed in 0-1.0V electric potential range, then in 1.0mol/L NaOH solution, it gets the carbon nanometer pipe/poly pyrrole peroxide compound modifying electrode by the electrochemical polymerization through the cyclic voltammetry (0.1mV/s scanning speed, 0-1.0V scanning electric potential). The compound modifying electrode can be used to measure the dopamine, which the results show that it has the high sensitivity, good repeatability and quick response.
Description
Technical field
The invention provides a kind of preparation method and application thereof of carbon nano tube/overoxidation polypyrrole composite modified electrode.By in multi-walled carbon nano-tubes that contains 0.5mg/mL and 0.05mol/L pyrroles's 0.2mol/L KCl solution (pH7.4), sweep velocity with 0.1mV/s, after in the potential range of 0～1.0V, adopting cyclic voltammetry scanning 8 circles, after taking out glass-carbon electrode, (sweep speed and be 0.1mV/s, the scanning current potential is that 0～1.0V) scanning, 50 circle electrochemical polymerizations are prepared from carbon nano tube/overoxidation polypyrrole composite modified electrode by cyclic voltammetry in the 1.0mol/L NaOH solution that is stirring again.This composite modified electrode can be applicable to the mensuration of dopamine, and the result shows that it has highly sensitive, favorable reproducibility, responds advantage fast.
Background technology
Since carbon nano-tube was found in 1991 (S.Lijima, Nature, 1991,354:56), it has very high surface area with it, and superpower electricity is led ability, and good chemical stability and significant physical strength have caused extensive attention.It is seamless, the hollow tube body of being curled and being formed by the graphite flake that carbon atom forms, be divided into multi-walled carbon nano-tubes and Single Walled Carbon Nanotube, be a kind of new carbon with complete molecular structure of nanoscale, therefore, carbon nano-tube is considered to a kind of desirable reinforcing agent in the compound substance.Even stoped its further operation and application yet the carbon nano-tube that purifying is crossed also can be assembled bunchy rapidly in ordinary organic solvents.The compound that preparation contains carbon nano-tube is one of the best way that addresses this problem, because work as the compound tense of other materials, can significantly improve the insoluble of carbon nano-tube; Also character that can it is unique and other materials are compound.
The conducting polymer of conjugated double bond structures is because it has also obtained paying close attention to widely (Huffman in the practical application of the aspects such as carrier of modified electrode, etch-resistant coating, molecular transistors and high-performance nano catalyzer and in recent years, F.Rodriguez-Macias, Y.S.Shon, T.R.Lee, D.T.Colbert, R.E.Smalley, Science, 1998,280:1253).With nanocatalyst and conductive polymerized film compound be a kind of method of good synthesizing new nano material.When it and conducting polymer generation compound tense, both can fine combination, can give full play to advantage separately again, thereby obtain the excellent more functional composite material of performance.At present, existing report (K.Bouzek, K.M.Mangold, K.J.Uttner, Electrochim.Acta, 2000,46:661 about nano particle/polymer composites; N.Cioffi, L.Torsi, I.Losito, L.Sabbatini, P.CxZambonin, T.Bleve-Zacheo, Electrochim.Acta, 2001,46:4), its objective is that the nano particle with unique properties is compound in the conductive polymerized film that is easy to operate and control.The polymeric membrane doped carbon nanometer pipe exists potential using value owing to having new electricity, light, mechanical property.This paper adopts polypyrrole film to prepare carbon mano-tube composite and is applied in the Electroanalytical Chemistry.Polypyrrole film is a kind of very stable conductive polymerized film, and electric conductivity is all better than other a lot of conductive polymerized films.At present carbon nano-tube or polypyrrole had been seen more report as the material of modified electrode, yet there are no report and the two is made combination electrode.
Summary of the invention
One of purpose of the present invention provides a kind of preparation method of carbon nano tube/overoxidation polypyrrole composite modified electrode.
Two of purpose of the present invention is to utilize carbon nano tube/overoxidation polypyrrole composite modified electrode to be used for the mensuration of dopamine.
These purposes of the present invention will further embody and set forth by following detailed description and explanation.
The purpose of invention realizes by following technical proposals:
1, a kind of preparation method of carbon nano tube/overoxidation polypyrrole composite modified electrode, preparation process is as follows: glass-carbon electrode is polished on the aluminium oxide of 300nm to light, successively in acetone, NaOH solution (1mol/L), HNO
3Solution (1: 1, v/v) and secondary deionized water in supersound washing.Then in multi-walled carbon nano-tubes that contains 0.5mg/mL and 0.05mol/L pyrroles's 0.2mol/L KCl solution (pH 7.4), sweep velocity with 0.1mV/s, (saturated calomel electrode is a contrast electrode with three-electrode system with the CHI650b electrochemical analyser, platinum electrode is to electrode, glass-carbon electrode is a working electrode), after in 0～1.0V scope, carrying out cyclic voltammetry scanning 8 circles, take out glass-carbon electrode and immerse in the 1.0mol/L NaOH solution that is stirring that (sweep speed and be 0.1mV/s, the scanning current potential is that 0～1.0V) scanning 50 is enclosed electrochemical polymerizations and is prepared from carbon nano tube/overoxidation polypyrrole composite modified electrode by cyclic voltammetry.
2, utilize the mensuration of carbon nano tube/overoxidation polypyrrole composite modified electrode to dopamine, it is characterized in that: in the phosphate buffer solution of 0.1mol/L pH=7.0 or contain in the dopamine liquid to be measured, (saturated calomel electrode is a contrast electrode with three-electrode system with the CHI650b electrochemical analyser, platinum electrode is to electrode, working electrode is a carbon nano tube/overoxidation polypyrrole composite modified electrode) ,-0.2V～+ carry out cyclic voltammetry in the 0.6V scope.2.5 * 10
-8～5.0 * 10
-5Peak current and its concentration of dopamine have good linear relationship in the mol/L scope, are 8.0 * 10 by calculating detectability (by signal to noise ratio (S/N ratio)=3)
-9Mol/L.
Embodiment
1, instrument and reagent
CHI-650 type electrochemical analyser (Shanghai occasion China instrument company); Three electrode work systems: saturated calomel electrode (SCE) is a contrast electrode, and platinum electrode is to electrode, and working electrode is a carbon nano tube/overoxidation polypyrrole composite modified electrode, and experimental data and voltammogram are by computer acquisition, processing and record.The medical numerical control ultrasonic cleaning machine of KQ-250DE type (Kunshan ultrasonic instrument company limited), magnetic stirring apparatus 85-1B (Gongyi Ying Yu gives magnificent instrument), WS70-1 type infrared ray rapid draing type (Shanghai City U.S. river in Jiangsu Province which flows into the Huangpu River of Shanghai hardware factory).(diameter and length are respectively 10～30nm and 1～10 μ m to carbon nano-tube, Sun Nanotech Co.Ltd, DA are Sigma company product, and damping fluid is the phosphate buffer solution solution of 0.1mol/L pH=7.0, it is pure that other reagent are analysis, and water is redistilled water.
2, the preparation of carbon nano tube/overoxidation polypyrrole composite modified electrode
Preparation process is as follows: glass-carbon electrode is polished on the aluminium oxide of 300nm to light, successively in acetone, NaOH solution (1mol/L), HNO
3Solution (1: 1, v/v) and secondary deionized water in supersound washing.Then in multi-walled carbon nano-tubes that contains 0.5mg/mL and 0.05mol/L pyrroles's 0.2mol/L KCl solution (pH7.4), sweep velocity with 0.1mV/s, (saturated calomel electrode is a contrast electrode with three-electrode system with the CHI650b electrochemical analyser, platinum electrode is to electrode, glass-carbon electrode is a working electrode), after in 0～1.0V scope, carrying out cyclic voltammetry scanning 8 circles, take out glass-carbon electrode and immerse in the 1.0mol/L NaOH solution that is stirring that (sweep speed and be 0.1mV/s, the scanning current potential is that 0～1.0V) scanning 50 is enclosed electrochemical polymerizations and is prepared from carbon nano tube/overoxidation polypyrrole composite modified electrode by cyclic voltammetry.
3, utilize the mensuration of carbon nano tube/overoxidation polypyrrole composite modified electrode to dopamine, it is characterized in that: in the phosphate buffer solution of 0.1mol/L pH=7.0 or contain in the dopamine liquid to be measured, (saturated calomel electrode is a contrast electrode with three-electrode system with the CHI650b electrochemical analyser, platinum electrode is to electrode, working electrode is a carbon nano tube/overoxidation polypyrrole composite modified electrode) ,-0.2V～+ carry out cyclic voltammetry in the 0.6V scope.2.5 * 10
-8～5.0 * 10
-5Peak current and its concentration of dopamine have good linear relationship in the mol/L scope, detect and are limited to 8.0 * 10
-9Mol/L.To dopamine replicate determination 6 times, peak current does not almost change with carbon nano tube/overoxidation polypyrrole composite modified electrode, illustrates that the reappearance of electrode is better.
Claims (2)
1. the preparation method of a carbon nano tube/overoxidation polypyrrole composite modified electrode, preparation process is as follows: glass-carbon electrode is polished on the aluminium oxide of 300nm to light, successively in acetone, NaOH solution (1mol/L), HNO
3Solution (1: 1, v/v) and secondary deionized water in supersound washing.Then in multi-walled carbon nano-tubes that contains 0.5mg/mL and 0.05mol/L pyrroles's 0.2mol/L KCl solution (pH7.4), sweep velocity with 0.1mV/s, (saturated calomel electrode is a contrast electrode with three-electrode system with the CHI650b electrochemical analyser, platinum electrode is to electrode, glass-carbon electrode is a working electrode), after in 0～1.0V scope, carrying out cyclic voltammetry scanning 8 circles, take out glass-carbon electrode and immerse in the 1.0mol/L NaOH solution that is stirring that (sweep speed and be 0.1mV/s, the scanning current potential is that 0～1.0V) scanning 50 is enclosed electrochemical polymerizations and is prepared from carbon nano tube/overoxidation polypyrrole composite modified electrode by cyclic voltammetry.
2. utilize the mensuration of carbon nano tube/overoxidation polypyrrole composite modified electrode to dopamine, it is characterized in that: in the phosphate buffer solution of 0.1mol/L pH=7.0 or contain in the dopamine liquid to be measured, (saturated calomel electrode is a contrast electrode with three-electrode system with the CHI650b electrochemical analyser, platinum electrode is to electrode, working electrode is a carbon nano tube/overoxidation polypyrrole composite modified electrode) ,-0.2V～+ carry out cyclic voltammetry in the 0.6V scope.2.5 * 10
-8～5.0 * 10
-5Peak current and its concentration of dopamine have good linear relationship in the mol/L scope, detect and are limited to 8.0 * 10
-9Mol/L.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101995423A (en) * | 2009-08-19 | 2011-03-30 | 遵义师范学院 | Modified electrode for detecting iodate and preparation method |
| CN101576530B (en) * | 2009-05-21 | 2012-02-08 | 北京化工大学 | Method for measuring dopamine by utilizing graphite nano-sheet/Nafion composite film to modify electrode |
| CN101587094B (en) * | 2009-05-26 | 2012-05-23 | 上海大学 | Method for concurrent measurement of dopamine and ascorbic acid using glassy carbon electrode |
| CN101961240B (en) * | 2009-07-24 | 2012-05-30 | 瑞鼎科技股份有限公司 | Biosensor, probe, sensing device and biosensor manufacturing method |
| CN107621491A (en) * | 2017-09-22 | 2018-01-23 | 仲恺农业工程学院 | A kind of method of tyramine content in overoxidised polypyrrole modified electrode for determining tyrasamine and measure white wine |
-
2007
- 2007-09-06 CN CNA2007100706927A patent/CN101149353A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101576530B (en) * | 2009-05-21 | 2012-02-08 | 北京化工大学 | Method for measuring dopamine by utilizing graphite nano-sheet/Nafion composite film to modify electrode |
| CN101587094B (en) * | 2009-05-26 | 2012-05-23 | 上海大学 | Method for concurrent measurement of dopamine and ascorbic acid using glassy carbon electrode |
| CN101961240B (en) * | 2009-07-24 | 2012-05-30 | 瑞鼎科技股份有限公司 | Biosensor, probe, sensing device and biosensor manufacturing method |
| CN101995423A (en) * | 2009-08-19 | 2011-03-30 | 遵义师范学院 | Modified electrode for detecting iodate and preparation method |
| CN107621491A (en) * | 2017-09-22 | 2018-01-23 | 仲恺农业工程学院 | A kind of method of tyramine content in overoxidised polypyrrole modified electrode for determining tyrasamine and measure white wine |
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Application publication date: 20080326 |