CN103969318A - Novel carbon nano tube electrochemical sensing interface and preparation method thereof - Google Patents
Novel carbon nano tube electrochemical sensing interface and preparation method thereof Download PDFInfo
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- CN103969318A CN103969318A CN201410175736.2A CN201410175736A CN103969318A CN 103969318 A CN103969318 A CN 103969318A CN 201410175736 A CN201410175736 A CN 201410175736A CN 103969318 A CN103969318 A CN 103969318A
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Abstract
The invention discloses a novel carbon nano tube electrochemical sensing interface and a preparation method thereof. The novel carbon nano tube electrochemical sensing interface is characterized in that based on a novel functional carbon nano tube static compound monomolecular layer and a modified electrode electrochemical sensing interface analysis system of a polymer film, and through the use of surface negative charge activity of the anion conducting polymer film and the adoption of layered electrostatic self-assembly, a novel poly sulfanilic acid/quaternary ammonium functional carbon nano tube/monomolecular layer sulfanilic acid nano-composite film modified electrode sensing interface is prepared. Through the electrostatic self-assembly of the poly sulfanilic acid/quaternary ammonium cation functional carbon nano tube/monomolecular layer sulfanilic acid nano-composite film electrode sensing interface, the whole preparation process is simple and time-saving, the condition is controllable, the prepared sensing interface is good in stability and repeatability, the repeatability of the preparation process of the sensing interface is high, and the problem that the stability and the repeatability of an electrochemical sensor are poor in practical application is solved to a great degree.
Description
Technical field
The invention belongs to Electroanalytical Chemistry technical field, specifically, is the preparation of the film modified electrode electro Chemical sensing interface of a kind of novel poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/individual layer sulfanilic acid electrostatic self-assembled nano-complex.
Background technology
Modified electrode electrochemical methods has highly sensitive, and instrument equipment is simple and easily realize microminiaturization, without any need for sample pretreatment and detachment process, simplifies routine analyzer and shortens the outstanding advantages such as analysis time.Carbon nano-tube (CNTs) is large because having specific surface area, and good conductivity and promotion electronics transmission capacity, be widely used in the preparation at Electrochemical Modification electrode sensing interface.But up to now, the dispersion of carbon nano-tube and the ordered fabrication at electrode surface are difficult problems for this research field always.Once there were report surfactant sodium dodecylsulphonate and organic polymer reagent etc. to improve to a certain extent the dispersiveness [1-5] of carbon nano-tube, but simple painting preparation method etc. cannot be realized the ordered fabrication of carbon nano-tube at electrode surface, and disperse reagent to transmit performance at the residual electronics that can hinder sensing interface of electrode surface, thereby greatly reduce chemical property and the electro catalytic activity of carbon nano tube modified electrode.How research allows CNTs is orderly at electrode surface height of formation, structure is controlled and directed intensive stable laminate structure, and building sensitive, stable electrochemical sensing interface is current divination by means of the milfoil key issue to be solved.By quaternary ammonium cation group on covalent bonding, the dispersiveness of carbon nano-tube in environmentally friendly solvent water improved dramatically; Simultaneously, utilize the strong adsorptive power of static of the carbon nano-tube after new functionalization, sulfanilic acid unimolecular layer modified glassy carbon electrode surface by the quaternary ammonium cation functionalized carbon nano-tube electrostatic self-assembled of high degree of dispersion at surface band negative charge, make that CNTs disperses in order, stable modified electrode, electrochemical activity and electro catalytic activity that this modified electrode can intact maintenance carbon nano-tube.The poly-sulfanilic acid conductive polymer membrane of bear electricity on electrostatic self-assembled more afterwards.This layer upon layer electrostatic self assembly technology of preparation method is simple, and consuming time short, condition is controlled, can improve dramatically the order of carbon nano-tube in the time that electrode surface is assembled, and can greatly improve repeatability prepared by sensing interface.
The present invention utilizes the surface negative charge activity of anionic electroconductive polymer film, and quaternary ammonium cation functionalized carbon nano-tube positive surface charge activity, large specific surface area and superior electronic conduction performance, prepare a kind of novel poly-sulfanilic acid/quaternized cationic functional carbon nano-tube/unimolecular layer sulfanilic acid nano-complex membrane electrochemical sensing interface by layer upon layer electrostatic self assembly.Up to now, this preparation method has no report at present.Taking dopamine as example, study the electrochemical oxidation behavior of dopamine (DA) on this modified electrode, the unique three-D space structure having due to this electrode and the negative charge active group surface of high concentration, and the collaborative enhancing electro catalytic activity that has of nano-complex film, greatly increase the electronics transfer rate of DA, reduce oxidation overpotential, thereby greatly improved the sensitivity of measuring.
ZhangJ,GaoL,Dispersionofmutiwallcarbonnanotubesbysodiumdodecylsulfateforpreparationofmodifiedelectrodestowarddetectinghydrogenperoxide,Mater.Lett.,61,3571-3574,2007.
WuKB,SunYY,HuSS,Developmentofanamperometricindole-3-aceicacidsensorbasedoncarbonnanotubesfilmcoatedglassycarbonelectrode,Sensor.Actuat.B-Chem.,96,658-662,2003.
WangJ,MuamehM,LinYH,SolubilizationofcarbonnanotubebyNafiontowardthepreparationofamperometricbiosensors,J.Am.Chem.Soc.,125,2408-2409,2003.
RubianesMD,RivasGA,Dispersionofmulti-wallcarbonnanotubesinpolyethylenimine:anewalternativeforpreparingelectrochemicalsensors,Electrochem.Commun.,9,480-484,2007.
BolloS,FerreyraNF,RivasGA,ElectrooxidationofDNAatglassycarbonelectrodemodifiedwithmultiwallcarbonnanotubesdispersedinchitosan,Electroanalysis,19,833-840,2007.
Summary of the invention
The present invention is pin improvements over the prior art just, build a kind of novel film modified electrode electro Chemical sensing interface of poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex.This sensing interface is successfully for high stability, the high sensitivity Electrochemical Detection of dopamine.Concrete technical scheme of the present invention is as follows:
The invention discloses a kind of preparation method of novel carbon nano-tube electrochemical sensing interface, modified electrode electrochemical sensing interface analytic system based on the compound unimolecular layer of new function carbon nano tube static and polymer film, utilize the surface negative charge activity of anionic electroconductive polymer film, and quaternary ammonium functionalized carbon nano-tube positive surface charge activity, large specific surface area and superior electronics transmit performance, prepare a kind of novel poly-sulfanilic acid/quaternary ammonium functionalized carbon nano-tube/unimolecular layer film modified electrode sensing of sulfanilic acid nano-complex interface by layer upon layer electrostatic self assembly.
The preparation method of novel carbon nano-tube electrochemical sensing interface of the present invention, concrete preparation process is as follows:
(1), by electrochemical method, sulfanilic acid unimolecular layer is covalently bonded to glass-carbon electrode surface, the sulfanilic acid electrostatic interaction that quaternary ammonium cation functionalized carbon nano-tube with a large amount of positive charges and electrode surface are electronegative, that self assembly makes is stable, the carbon nano tube modified electrode of orderly dispersion;
(2), on carbon nano-tube/unimolecular layer sulfanilic acid modified electrode of preparation by electrochemical method polymerization sulfanilic acid, obtain the poly-film modified electrode electro Chemical sensor of sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex by layer upon layer electrostatic self assembly.
The invention also discloses the electrochemical detection method that the film modified electrode electro Chemical sensing interface of a kind of poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex is applied to dopamine.Be chosen under best current potential, dopamine carried out to electrochemical gaging by electric current-time curve method, in very wide linear concentration range, this sensor has rapid sensitive, stable current-responsive to dopamine.
The advantage that the present invention has and effect:
1. the present invention utilizes after carbon nano-tube quaternary ammonium cation functionalization the dispersiveness in water fabulous: water is the friendly solvent of electrochemical gaging system, use water as spreading agent and easily obtain the CNTs membrane material of purifying at electrode surface, thereby avoided the introducing of the even non-conductive organic solvent of poorly conductive and organic polymer spreading agent to affect electric conductivity and the electronics transmission performance of sensing interface; In addition, due to the repulsive interaction between a large amount of quaternary ammonium cations of carbon nano tube surface after functionalization, effectively avoided the reunion between carbon nano-tube.By bear electricity sulfanilic acid unimolecular layer, quaternary ammonium cation functionalized carbon nano-tube aqueous solution easily obtains the CNTs film of high-sequential assembling at electrode surface.These for CNTs the application in electrochemical sensor very crucial.
2. the present invention has very strong Electrostatic Absorption characteristic to bear electricity unimolecule and polymkeric substance after utilizing carbon nano-tube quaternary ammonium cation functionalization, many in conjunction with the electroactive site of poly-sulfanilic acid bear, the collaborative advantages such as electrochemical signals that strengthen, the film modified electrode sensing interface stability of the poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex degree of preparation improves greatly; Electronics transmits medium carbon nano-tube and poly-sulfanilic acid order degree improves greatly; Nano-complex film electro catalytic activity improves greatly.
The poly-whole preparation process of sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex membrane electrochemical sensing interface of electrostatic self-assembled simple, save time, condition is controlled, the sensing interface stability of preparation, favorable reproducibility; The preparation process repeatability of sensing interface is high, and this has solved the problem of electrochemical sensor stability and poor reproducibility in the time of practical application to a great extent.
Brief description of the drawings
Fig. 1 is the building process mechanism schematic diagram of poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex membrane electrochemical sensing interface;
Fig. 2 is the scanning electron microscope figure of poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex membrane electrochemical sensing interface;
Fig. 3 (A) is naked glass-carbon electrode response cycle volt-ampere (CV) figure to DA in pH7.0PBS;
In figure, the blank PBS buffer solution of a-; B-is containing the PBS buffer solution of 0.1mMDA;
Fig. 3 (B) is poly-sulfanilic acid modified electrode response cycle volt-ampere (CV) figure to DA in pH7.0PBS;
In figure, the blank PBS buffer solution of a-; B-is containing the PBS buffer solution of 0.1mMDA;
Fig. 3 (C) is quaternary ammonium cation functionalized carbon nano-tube modified electrode response cycle volt-ampere (CV) figure to DA in pH7.0PBS;
In figure, the blank PBS buffer solution of a-; B-is containing the PBS buffer solution of 0.1mMDA;
Fig. 3 (D) is the poly-film modified electrode of sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex response cycle volt-ampere (CV) figure to DA in the PBS of pH7.0;
In figure, the blank PBS buffer solution of a-; B-is containing the PBS buffer solution of 0.1mMDA;
Fig. 4 (A) is adding curve electric current-time response of variable concentrations DA continuously for gathering the film modified electrode of sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex;
Fig. 4 (B) is the linear relationship chart of response current and DA concentration, operating potential: 0.20V;
Embodiment
The invention discloses the film modified electrode electro Chemical sensing interface of a kind of novel poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/individual layer sulfanilic acid nano-complex and prepare and stablize the electricity analytical method of sensitive determination dopamine, it is a kind of modified electrode electrochemical sensor analytic system based on the compound unimolecular layer of new function carbon nano tube static and polymer film, first by electrochemical process, sulfanilic acid unimolecular layer is covalently bonded to glass-carbon electrode surface, the sulfanilic acid electrostatic interaction that positively charged quaternary ammonium cation functionalized carbon nano-tube and electrode surface are electronegative, make stable carbon nano tube modified electrode.On carbon nano-tube/unimolecular layer sulfanilic acid modified electrode of preparation, by electrochemical method polymerization sulfanilic acid, obtain the poly-film modified electrode electro Chemical sensing interface of sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex by layer upon layer electrostatic self assembly.
Study the electrochemical behavior of dopamine (DA) on this modified electrode, the unique three-D space structure having due to this modified electrode electrochemical sensing interface and the negative charge active group surface of high concentration, greatly increase the electronics transfer rate of DA on this interface, and the collaborative enhancing catalytic oxidation DA activity that has of nano-complex film, thereby greatly improve the sensitivity while measuring DA taking it as sensing interface electrochemical methods.
The film modified electrode of poly-sulfanilic acid/quaternary ammonium cation carbon nano-tube/unimolecular layer sulfanilic acid nano-complex prepared by the present invention is compared with quaternary ammonium cation functionalized carbon nano-tube modified electrode with naked glass-carbon electrode, poly-sulfanilic acid modified electrode, electro catalytic activity obviously increases, and has greatly improved the electrochemical gaging sensitivity to dopamine.Be chosen under optimal response current potential, dopamine carried out to electrochemical gaging by electric current-time curve method.In very wide linear concentration range, this sensor has the current-responsive of rapid sensitive to dopamine, and excellent stability.
The film modified electrode of poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex prepared by the present invention, preparation process repeatability is fine, greatly reduces the deviation of electrochemical sensing interface in each preparation.
Below in conjunction with Figure of description, technical scheme of the present invention is described in further detail:
Naked glass-carbon electrode (GCE) is polished on deerskin with the alumina powder of 0.3 μ m and 0.05 μ m successively, be polished to minute surface.With absolute ethyl alcohol, the each 5min of distilled water ultrasonic cleaning.The three-electrode system that is working electrode pretreated glass-carbon electrode is put into the 0.1MKCl solution containing 0.003M sulfanilic acid, between 0.6～1.2V, enclose with the fast cyclic voltammetry scan 10 of sweeping of 0.05V/s, after taking out and cleaning with redistilled water, dry, drip the laboratory self-control quaternary ammonium cation functionalization CNT aqueous dispersion (1mg/mL) of 4 μ L, dry, rinse with redistilled water, then containing in the 0.1MKCl solution of 0.005M sulfanilic acid, potential region in-0.2～2.0V encloses with the fast cyclic voltammetry scan 5 of sweeping of 0.05V/s, after taking-up, rinse with redistilled water, dry.Obtain the film modified electrode of poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex.
Fig. 1 is the whole modification mechanism schematic diagram of the poly-film modified electrode of sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex.The unimolecular layer sulfanilic acid electrostatic interaction that positively charged quaternary ammonium cation functionalized carbon nano-tube and electrode surface are electronegative, makes directed stable carbon nano tube modified electrode; Form afterwards poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex film, make this electrode surface form the negative charge active group surface of unique three-D space structure and high concentration, thereby can greatly improve mass transfer rate and the electronics transfer rate of DA on electrochemical sensing interface.
Fig. 2 is the scanning electron microscope figure of poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex membrane electrochemical sensing interface.From figure, can obviously find out, thin layer carbon nano tube surface is covered by one deck organic polymer, has confirmed the interfacial assembly process mechanism shown in Fig. 1.
Fig. 3 is in the different modifying electrode PBS buffer solution that is 7.0 at pH, the cyclic voltammogram while having or not DA.As can be seen from the figure, DA is at naked glass-carbon electrode (A), oxidation peak current potential on poly-sulfanilic acid modified electrode (B) and quaternary ammonium functionalized carbon nano-tube modified electrode (C) is respectively 0.307V, 0.227V, 0.269V, current-responsive value is 3.25 μ A, 5.73 μ A, 10.56 μ A, and the oxidation peak current potential that records DA on poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer film modified electrode of sulfanilic acid nano-complex (D) is reduced to 0.197V, current-responsive value is 18.49 μ A, illustrate under the collaborative electrocatalysis of poly-sulfanilic acid and carbon nano-tube, make DA oxidized under lower current potential, obtain higher current-responsive simultaneously.
Fig. 4 (A) adds continuously curve electric current-time response of variable concentrations DA under the set potential of 0.2V for gathering the film modified electrode of sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex, Fig. 4 (B) is the linear relationship chart of response current and DA concentration.Sensor has the response of rapid sensitive to DA, in 2.0～102.0 μ M concentration ranges, the concentration of response current and DA is fine linear relationship, and linear concentration range is wide.Press S/N=3 and calculate, this method is measured detecting of DA and is limited to 0.02 μ M, lower than what report in many documents.To 50 μ MDA METHOD FOR CONTINUOUS DETERMINATION 10 times, current-responsive relative standard deviation (RSD) is 0.23%.Modified electrode is placed in pH7.0 phosphate buffer and redeterminates DA after 4 DEG C of refrigerators is preserved 1 month, and current-responsive only declines 3%.Repeat to prepare sensing interface 6 times, current-responsive relative standard deviation (RSD) is only 1.5%.
What more than enumerate is only part specific embodiment of the present invention; obviously, the invention is not restricted to above embodiment, can also have many distortion; all distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (3)
1. a novel carbon nano-tube electrochemical sensing interface, it is characterized in that, modified electrode electrochemical sensing interface analytic system based on the compound unimolecular layer of novel quaternary ammonium cation functionalized carbon nano-tube static and polymer film, utilize the surface negative charge activity of anionic electroconductive polymer film, and quaternary ammonium functionalized carbon nano-tube positive surface charge activity, large specific surface area and superior electronics transmit performance, prepare a kind of novel poly-sulfanilic acid/cationation of quaternary ammonium function carbon nano-tube/unimolecular layer sulfanilic acid nano-complex membrane electrochemical sensing interface by layer upon layer electrostatic self assembly.
2. the preparation method of novel carbon nano-tube electrochemical sensing interface according to claim 1, is characterized in that, concrete preparation process is as follows:
(1), by electrochemical method, sulfanilic acid unimolecular layer is covalently bonded to glass-carbon electrode surface, the sulfanilic acid unimolecular layer electrostatic interaction that positively charged quaternary ammonium cation functionalized carbon nano-tube and electrode surface are electronegative, makes the carbon nano tube modified electrode of steady ordered;
(2), on carbon nano-tube/unimolecular layer sulfanilic acid modified electrode of preparation by electrochemical method polymerization sulfanilic acid, obtain the poly-film modified electrode electro Chemical sensor of sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex by layer upon layer electrostatic self assembly.
3. the film modified electrode electro Chemical sensor application of poly-sulfanilic acid/quaternary ammonium cation functionalized carbon nano-tube/unimolecular layer sulfanilic acid nano-complex that a preparation method according to claim 1 and 2 is prepared from is in the Electrochemical Detection of dopamine, it is characterized in that, prepared New Type of Carbon nanotube electrochemical sensing interface has significant catalytic oxidation effect to dopamine, by comparing the response signal to noise ratio (S/N ratio) to dopamine under different potentials, be chosen under optimal response current potential, dopamine carried out to electrochemical gaging by electric current-time curve method.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104831277A (en) * | 2015-04-13 | 2015-08-12 | 济南大学 | Preparation method and application of poly-sulfosalicylic acid / titanium dioxide / carbon nanotube nanocomposite with electrode as substrate |
| CN105548313A (en) * | 2016-01-06 | 2016-05-04 | 辽宁大学 | Modified electrode for detecting low-concentration dopamine and making method and application thereof |
| CN108169298A (en) * | 2017-12-19 | 2018-06-15 | 江南大学 | A kind of preparation method for the disposable sensor for detecting dopamine |
| CN114544720A (en) * | 2022-01-12 | 2022-05-27 | 肇庆学院 | Electrochemical sensor for ultra-sensitive detection of enrofloxacin and preparation method thereof |
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| CN1395094A (en) * | 2002-07-18 | 2003-02-05 | 武汉大学 | Electrochemical sensor for determining dopamine |
| CN102141536A (en) * | 2010-12-10 | 2011-08-03 | 北京化工大学 | Composite material electrode based on carbon nano tubes as well as preparation method and application thereof |
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2014
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Patent Citations (2)
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| CN1395094A (en) * | 2002-07-18 | 2003-02-05 | 武汉大学 | Electrochemical sensor for determining dopamine |
| CN102141536A (en) * | 2010-12-10 | 2011-08-03 | 北京化工大学 | Composite material electrode based on carbon nano tubes as well as preparation method and application thereof |
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| LEI ZHANG ET AL.: "Fabrication of poly(orthanilic acid)–multiwalled carbon nanotubes composite film-modified glassy carbon electrode and its use for the simultaneous determination of uric acid and dopamine in the presence of ascorbic acid", 《J SOLID STATE ELECTROCHEM》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104831277A (en) * | 2015-04-13 | 2015-08-12 | 济南大学 | Preparation method and application of poly-sulfosalicylic acid / titanium dioxide / carbon nanotube nanocomposite with electrode as substrate |
| CN105548313A (en) * | 2016-01-06 | 2016-05-04 | 辽宁大学 | Modified electrode for detecting low-concentration dopamine and making method and application thereof |
| CN108169298A (en) * | 2017-12-19 | 2018-06-15 | 江南大学 | A kind of preparation method for the disposable sensor for detecting dopamine |
| CN114544720A (en) * | 2022-01-12 | 2022-05-27 | 肇庆学院 | Electrochemical sensor for ultra-sensitive detection of enrofloxacin and preparation method thereof |
| CN114544720B (en) * | 2022-01-12 | 2023-09-05 | 肇庆学院 | Electrochemical sensor for ultra-sensitively detecting enrofloxacin and preparation method thereof |
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