CN103884753B - A kind of preparation method of rhodamine 6G/oxine film modified electrod and application - Google Patents
A kind of preparation method of rhodamine 6G/oxine film modified electrod and application Download PDFInfo
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- CN103884753B CN103884753B CN201310705672.8A CN201310705672A CN103884753B CN 103884753 B CN103884753 B CN 103884753B CN 201310705672 A CN201310705672 A CN 201310705672A CN 103884753 B CN103884753 B CN 103884753B
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Abstract
The invention discloses preparation method and the application of a kind of rhodamine 6G/oxine film modified electrod, is 5.0 × 10 in pH7.0 rhodamine 6G concentration
-3cyclic voltammetry is utilized to be aggregated in ITO electrode by Rh6G in the solution of mol/L, after rhodamine 6G film is completely dry, recycling cyclic voltammetric, modifies oxine on electrode, has so just prepared the rhodamine 6G/oxine film modified electrod of surface uniform, good stability.This modified electrode preparation method is simple, and good stability is highly sensitive, reusable, has certain application prospect in hydrogen peroxide context of detection.
Description
Technical field
The invention belongs to technical field of chemistry, relate to preparation method and the application of a kind of rhodamine 6G/oxine film modified electrod.
Background technology
Chemically modified electrode be the mid-1970s one of growing up emerging, be also the Disciplinary Frontiers of current most active galvanochemistry and Electroanalytical Chemistry.Chemically modified electrode carries out MOLECULE DESIGN at electrode surface, forms certain microstructure, and by having the molecule of excellent chemical character, ion, polymer design be fixed on electrode surface, makes electrode have certain specific chemistry and electrochemical properties.It grows up on Conventional electrochemical electrode base, is improving the superiority in selectivity and sensitivity with uniqueness.In mid-term in 19 end of the centurys to 20th century, know and known that a lot of substance adsorbs at electrode surface, and started to carry out electrode modification on a molecular scale.The Chinese Academy of Sciences at the beginning of the eighties answers in Changchun chemistry institute Dong Shao person of outstanding talent to take the lead in leading and carried out the systematic study of chemically modified electrode at home.Over nearly 20 years, chemically modified electrode obtains remarkable development especially.Nowadays application is more and more extensive, as in all many-sides such as life science, environmental science, analysis science, energy science, material science and electronics.
Many dyestuffs all have good electrochemical activity, the conjugated structure feature of dyestuff is conducive to the absorption of molecule on electrode, and the group carried can promote that some molecules are at the electronic transfer process of electrode surface, be therefore the focus that people study in electrode modification field always
[10].If organic dyestuff is amino or hydroxyl with electron donor, and when having at least one unsubstituted ortho position or contraposition, on electrode, electrochemical polymerization can occur.The method preparing dye Modified Electrode generally includes absorption method, the methods such as polymkeric substance investment and directly electropolymerization dye molecule.
Rhodamine 6G, English name Rhodamine6G, has another name called rose-red 6G, rhodamine 6G, rhodamine 6G.It is a kind of a kind of dyestuff derived by triphenylmethane that can be used as bioluminescence coloring agent, water-soluble in scarlet colour band green fluorescence; Be dissolved in alcohol to take on a red color band yellow fluorescence or yellowish red color band green fluorescence.By etc. the rhodamine B of weight and aniline hydrochloride be heated to 185 ~ 190 DEG C and keep 1.5 ~ 2h, by products therefrom ethanol and mineral acid in addition esterification obtain.
Hydrogen peroxide is commonly called as hydrogen peroxide, and aqueous solution is colourless transparent liquid, has faint special odor.Pure hydrogen peroxide is nattier blue oily liquids.In acid condition, hydrogen peroxide is more stable, but in the basic conditions, then very unstable, can fast decoupled.Oxidation or reducing action can be had in different situations, can be used as oxygenant, bleaching agent, sanitizer, dechlorinating agent etc., so be all widely used in fields such as textile industry, paper-making industry, electronics industry, grocery trade, environmental protection; In addition, with enzyme as molecular recognition elements, have good selectivity, now existing multiple enzyme is for measuring micro constitutent in biosome, and when wherein using oxidase to measure, final product is hydrogen peroxide, therefore, develops H that is sensitive, quick, low cost
2o
2detection method meaning is important.At present, H
2o
2detection method comprises titrimetry, spectrophotometric method, chromatography, chemoluminescence method and electrochemical process etc.
The dyestuff great majority studied at present are quinone imides dyestuff, as methylenum careuleum, methylene green, meldola blue etc.They have good catalytic effect to the material such as protein, cytochrome.But the preparation of this kind of electrode many employings absorption method, the stability of electrode, repeatability and serviceable life are all undesirable.In ITO electrode, only polymerization has the modified electrode stability of rhodamine 6G film also poor, but the stability that modified electrode is put after being polymerized upper oxine film is again greatly improved, and can preserve for a long time and reuse.Hydrogen peroxide is all widely used in the field such as commercial production, environmental analysis, and it is also the important by-products of a series of enzymatic reaction such as cholesterol oxidase, glucose oxidase.Therefore, the H that development cost is low, quick, highly sensitive
2o
2detection method is significant.
Summary of the invention
In order to overcome defect of the prior art, the invention provides the preparation method of a kind of rhodamine 6G/oxine film modified electrod, utilize rhodamine 6G (Rh6G) electrochemical properties, prepare rhodamine 6G/oxine film modified electrod, establish a kind of new method to hydrogen peroxide determination.Its technical scheme is:
A kind of preparation method of rhodamine 6G/oxine film modified electrod, comprises the following steps:
(1) successively by ITO electrode ultrasonic cleaning 2min in acetone, absolute ethyl alcohol, intermediate water, dry, stand-by;
(2) pretreated electrode puts into 5 × 10
-4in mol/LRh6G+0.1mol/LPBS, pH=7.0+0.1mol/LNaCl system, connect three-electrode system, utilize cyclic voltammetry to carry out scanning polymerization rhodamine 6G film, scanning potential range is-1.1 ~ 1.6V; Sweep speed is 50mV/s; Scanning hop count is 20 sections;
(3), after completing polymerization, take out the electrode modified, rinse well with redistilled water, dry, for subsequent use;
(4) the rhodamine 6G modified electrode after drying is put into 5 × 10
-4in the oxine+0.1mol/LNaCl system of mol/L, connect three-electrode system, in-0.9 ~ 1.4V potential range, with 100mV/s sweep speed electrochemical polymerization 14 sections, rhodamine/oxine film modified electrod can be obtained.
Application in the quantitative test of rhodamine 6G of the present invention/oxine film modified electrod hydrogen peroxide in actual sample.
Beneficial effect of the present invention:
The present invention has prepared rhodamine 6G/oxine film modified electrod, establishes a kind of new method to hydrogen peroxide determination.Have studied pH value, potential range, Rh6G concentration, buffer solution, oxine film thickness to the impact measured.Be 5.0 × 10 in pH7.0 rhodamine 6G concentration
-3cyclic voltammetry is utilized to be aggregated in ITO electrode by Rh6G in the solution of mol/L, after rhodamine 6G film is completely dry, recycling cyclic voltammetric, modifies oxine on electrode, has so just prepared the rhodamine 6G/oxine film modified electrod of surface uniform, good stability.Then utilize differential pulse voltammetry to measure rhodamine 6G/oxine film to the response of hydrogen peroxide, experimental result shows, the concentration of hydrogen peroxide is 5 × 10
-5~ 7.5 × 10
-3within the scope of mol/L with peak current be good linear relationship, detectability can reach 5 × 10
-6mol/L, related coefficient is 0.9991, and the recovery, between 96.4% ~ 104.8%, can be used for the quantitative test of hydrogen peroxide in actual sample.This modified electrode preparation method is simple, and good stability is highly sensitive, reusable, has certain application prospect in hydrogen peroxide context of detection.
In a word, compared with the present invention detects with one hydrogen peroxide detection method, there is following advantage: the instrument of use is easy to operate, reagent type and consumption few, modified electrode is easily prepared, modified electrode stability, favorable reproducibility, can long storage time and recycling; Highly sensitive to hydrogen peroxide determination, interfering material is few, so this modified electrode has certain practical value.
Accompanying drawing explanation
Cyclic voltammogram when Fig. 1 is polymerization rhodamine 6G film;
Cyclic voltammogram when Fig. 2 is polymerization oxine film;
Fig. 3 is the different modified electrode electric current at blank solution: (a) blank electrode; (b) rhodamine 6G film modified electrod; (c) oxine film modified electrod; (d) rhodamine 6G/oxine film modified electrod;
Fig. 4 is the electric current of electrode in blank solution of poly-rhodamine 6G film: the scanning of (a) first time; The scanning of (b) second time;
Fig. 5 is the electric current of electrode in blank solution of poly-rhodamine 6G/8 hydroxyquinoline film: the scanning of (a) first time; The scanning of (b) second time;
Fig. 6 be rhodamine/oxine modified electrode to the response of hydrogen peroxide: (a) is in blank in solution; B () is in superoxol;
Fig. 7 is the uv-visible absorption spectra of rhodamine 6G: the uv-visible absorption spectra of (a) rhodamine 6G solution; The uv-visible absorption spectra of (b) electropolymerization rhodamine 6G modified electrode;
When Fig. 8 is different pH, electropolymerization electrode soaks the absorbance log of front and back at 540nm place wavelength: before (a) soaks; B () soaks after;
Fig. 9 be same buffer solution in the impact on DPV current peak: (a) PBS; (b) sodium hydrogen phosphate-citrate buffer solution; (c) sodium hydrogen phosphate-potassium phosphate buffer; (d) potassium dihydrogen phosphate-sodium hydrate buffer solution;
Figure 10 is the absorbance log at 540nm place wavelength of the electrode immersion front and back that same rhodamine 6G solution concentration is modified: before (a) soaks; B () soaks after;
Figure 11 is that oxine film thickness is on the impact measured;
Figure 12 is that rhodamine 6G/oxine film is to the response of hydrogen peroxide;
Figure 13 is the funtcional relationship of concentration of hydrogen peroxide and peak current in solution.
Embodiment
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is described in more detail.
The present invention adopts the method for electropolymerization to modify rhodamine 6G in ITO electrode, because rhodamine 6G is soluble in water, when modified electrode soaks for a long time in water, film can come off from electrode, less stable.And oxine is insoluble in water, and be easily polymerized in ITO electrode, therefore on the electrode being polymerized rhodamine 6G, be polymerized one deck oxine film again, the stability of modified electrode will improve greatly.The accuracy of result just can be improved widely when measuring hydrogen peroxide.
CHI660b electrochemical workstation (Shanghai Chen Hua instrument company; Three electrode work system: ITO are working electrode, and platinum electrode is auxiliary electrode, and Ag/AgCl is contrast electrode); Cary ultraviolet spectrophotometer (U.S. UARIAN); KAWH9050 ultrasonic cleaning machine; 8S-1 type magnetic stirring apparatus.
Rhodamine 6G (Xi Long Chemical Co., Ltd. of Shantou City, AR), is mixed with 2.5 × 10
-3mol/L aqueous solution; Oxine (AR), is mixed with 2.5 × 10 in the ethanol water of 1: 1
-3the solution of mol/L; Sodium chloride (Xi Long Chemical Co., Ltd., AR); 30% hydrogen peroxide (AR), is mixed with 5 × 10
-2mol/L standard reserving solution; Acetone; Absolute ethyl alcohol; Ascorbic acid (Xi Long Chemical Co., Ltd. of Shantou City); Glucose (Xi Long Chemical Co., Ltd., AR); NaOH (1Guanghua Chemical Plant Co., Ltd., Guangdong); Citric acid; Sodium hydrogen phosphate, sodium dihydrogen phosphate (Xi Long Chemical Co., Ltd., AR), two reagent are mixed with respectively pH=5.0,5.5,6.0,6.5,7.0,7.5, the 2mol/LNaH of 8.0
2pO
4-Na
2hPO
4buffer solution (PBS); Other reagent are formulated by analytical reagent, and experimentation all adopts redistilled water.
The pre-service of 1ITO electrode
Successively by ITO electrode ultrasonic cleaning 2min in acetone, absolute ethyl alcohol, intermediate water, dry, stand-by.
The preparation of rhodamine/oxine film
Pretreated electrode puts into 5 × 10
-4in mol/LRh6G+0.1mol/LPBS (pH=7.0)+0.1mol/LNaCl system, connect three-electrode system, utilize cyclic voltammetry to carry out scanning polymerization rhodamine 6G film.Scanning potential range is-1.1 ~ 1.6V; Sweep speed is 50mV/s; Scanning hop count is 20 sections.After completing polymerization, take out the electrode modified, rinse well with redistilled water, dry, for subsequent use.Cyclic voltammogram when Fig. 1 is electropolymerization rhodamine 6G, as can be seen from Figure rhodamine 6G oneself be aggregated in ITO electrode.
Rhodamine 6G modified electrode after drying is put into 5 × 10
-4in the oxine+0.1mol/LNaCl system of mol/L, connect three-electrode system, in-0.9 ~ 1.4V potential range; With 100mV/s sweep speed electrochemical polymerization 14 sections, rhodamine/oxine film modified electrod can be obtained, take out electrode redistilled water wash clean, soak after 4 hours in the PBS of pH=7.0, for subsequent use.Cyclic voltammogram when Fig. 2 is electropolymerization oxine, as can be seen from Figure oxine oneself be aggregated in ITO electrode.
Electrochemical gaging
In 0.1mol/LNaCl+5mL0.2mol/LPBS system, using the film modified ITO electrode of rhodamine/oxine as working electrode, platinum electrode is auxiliary electrode, and Ag/AgCl is contrast electrode, carries out differential pulse voltammetry (DPV) scanning.Scanning potential range: 0 ~-1.1V; Current potential increment: 0.01v, amplitude: 0.05V, time of repose: 15s.20,40,60,80,100,120,140 μ L0.1mol/L Hydrogen peroxide standard storing solutions are added in the solution successively, the peak point current of each scanning of record after peak current is stable.In order to make dissolution homogeneity, before each scanning, all utilize magnetic stirrer 5 second.
The optical characteristics of electropolymerization rhodamine 6G film modified electrod
5 × 10
-4in mol/LRh6G+0.1mol/LPBS (pH=7.0)+0.1mol/LNaCl system, using ITO electrode as working electrode, scan by cyclic voltammetry.Scanning potential range is-1.1 ~ 1.6V; Sweep speed is 500mV/s; Scanning hop count is 20 sections.Rinse well with redistilled water, dry.Cary ultraviolet spectrophotometer is adopted to scan in the wavelength coverage of 300 ~ 800nM again.Contrast with the uv-visible absorption spectra figure of Rh6G solution.
Differential pulse is to the sign of modified electrode
Fig. 3. be respectively blank electrode, the film modified ITO electrode of rhodamine 6G, the film modified ITO electrode of oxine, the differential pulse voltammetry figure of the film modified ITO electrode of rhodamine 6G/oxine in blank solution.The modified electrode of rhodamine 6G film is only had not have current peak at-0.3 ~ 0.3V, and oxine film modified electrod and rhodamine 6G/oxine film modified electrod have two small area analysis peaks between-0.3 ~ 0.3V, it can thus be appreciated that oxine oneself be aggregated on rhodamine 6G film modified electrod.Fig. 4 is the map of current that only polymerization has the electrode of rhodamine 6G film first time scanning and the 5th scanning differential pulse in blank solution, Fig. 5 is the map of current of electrode first time scanning and the 5th scanning differential pulse in blank solution of polymerization rhodamine/oxine film, relatively two figure can reach a conclusion, on rhodamine film again polymerization to have the electrode of oxine much more stable than only having the electric current of the electrode of rhodamine film.Fig. 6 be rhodamine/oxine modified electrode to the response of hydrogen peroxide, the existence of hydrogen peroxide can cause the reduction peak current of rhodamine to change as can be seen from Figure, along with concentration of hydrogen peroxide increase, peak current reduces gradually.
Uv-visible absorption spectra is to the sign of rhodamine 6G modified electrode
As can be seen from Fig. 7 uv-visible absorption spectra figure, there occurs red shift at the absorption peak (b) of the rhodamine 6G on ITO electrode surface through electropolymerization compared with uv-visible absorption spectra peak (a) of rhodamine 6G solution.This shows that the rhodamine in ITO electrode there occurs electropolymerization, and poly-rhodamine 6G increases due to molecule internal double bond conjugated degree, causes maximum absorption band red shift.
The optimization of pH value during electropolymerization rhodamine 6G film
Respectively 5 × 10
-4electropolymerization rhodamine 6G film in the PBS system of the pH that mol/LRh6G+0.1mol/LNaCl+0.1mol/L is different, film after being polymerized first measures uv-visible absorption spectra, then soak in redistilled water after 4 hours and measure a uv-visible absorption spectra again, investigate the impact of different pH value on rhodamine thin film stability with this.The rhodamine 6G film polymerize when the pH value of PBS is 7.0 in solution is as shown in Figure 8 the most stable.
Different buffer solution is on the impact of poly-rhodamine 6G/oxine modified electrode DPV current peak
Respectively 5 × 10
-4in the different buffer systems (phosphate buffered solution (PBS), sodium hydrogen phosphate-citrate buffer solution, sodium hydrogen phosphate-potassium phosphate buffer, potassium dihydrogen phosphate-sodium hydrate buffer solution) of mol/LRh6G+0.1mol/LNaCl+0.1mol/LpH=7.0, take ITO electrode as working electrode polymerization rhodamine 6G film.After rhodamine 6G film is dry, then 5 × 10
-4oxine film is polymerized in mol/L8-hydroxyquinoline+0.1mol/LNaCl system.With the electrode modified for working electrode respectively be polymerized rhodamine film time buffer solution in scan differential pulse voltammetry.As Fig. 9, the peak shape that the peak shape of the DPV current peak of modified electrode in sodium hydrogen phosphate-citrate buffer solution, sodium hydrogen phosphate-potassium phosphate buffer, potassium dihydrogen phosphate-sodium hydrate buffer solution is all not so good as in PBS is good.
Polymerization rhodamine membrane potential scope
When preparing polymer thin film modified electrode by cyclic voltammetry, scanning potential range all has considerable influence to the formation of polymer film and character.Experimental result shows, when current potential is lower than-1.1V, in PBS buffer solution, electrode can be damaged, when current potential is increased to 1.7V, between 1.3 ~ 1.5V, occurs a peak, peak current reduces along with the increase of the polymerization number of turns, when the current potential upper limit controls to be 1.6 ~ 1.8V, stable polymerization can be carried out, therefore, during electropolymerization, to be chosen as-1.1 ~ 1.6V comparatively suitable for scan round potential range, in literary composition rhodamine 6G film used all in this potential range electropolymerization be prepared from.
Polymerization rhodamine film Rh6G concentration
Respectively at 0.1mol/LNaCl+0.1mol/LPBS (pH=7.0)+variable concentrations Rh6G (1.25 × 10
-4~ 7.5 × 10
-4mol/L) rhodamine 6G film is prepared in system, film after being polymerized first measures uv-visible absorption spectra, then soak in intermediate water after 4 hours and measure a uv-visible absorption spectra again, investigate the impact of variable concentrations Rh6G on rhodamine film with this.In solution, rhodamine liquor concentration is 5 × 10 as shown in Figure 10
-4the rhodamine film be polymerized during mol/L is the thickest also the most stable.
Oxine film thickness
The thickness of oxine film by scanning hop count to control, so investigate oxine thickness to measuring the impact of hydrogen peroxide to be polymerized hop count.Be 5 × 10 in oxine concentration respectively
-3in mol/L solution, be supporting electrolyte with NaCl, the electrode having modified rhodamine film is working electrode, and be-0.9 ~ 1.4V at current potential, speed is 0.05V/s, scans different hop counts.Modified electrode after being polymerized soaks the standard solution measuring hydrogen peroxide after 4 hours respectively in the buffer solution of pH=7.0.The calibration curve slope that the hop count being polymerized oxine as shown in Figure 11 measures Hydrogen peroxide standard solution 14 sections time is maximum, judges that sensitivity is maximum with this, so the hop count of final selective polymerization oxine is 14 sections.
The selection of base electrode
Under same experimental technique, step and condition, be working electrode with glass-carbon electrode, glass-carbon electrode is polymerized rhodamine/oxine film.The results show, the rhodamine that the ratio that ITO electrode is polymerized is polymerized on the glass-carbon electrode/sensitivity of oxine film to hydrogen peroxide determination is high.So the final base electrode selected of experiment is ITO electrode.
H
2o
2concentration is on the impact of modified electrode DPV peak current
Figure 12 is rhodamine/oxine modified electrode when to scan potential range be 0 ~-1.1V, and containing variable concentrations H
2o
2pBS (pH7.0,0.1mol/LNaCl) in differential pulse voltammetry figure.In this test system, rhodamine/oxine film is to H
2o
2have strong response, the reduction peak current of rhodamine is with all with H
2o
2concentration increase and reduce.Work as H
2o
2concentration 5 × 10
-5mol/L ~ 7.5 × 10
-3time within the scope of mol/L, its reduction peak current and concentration have good linear relationship, equation of linear regression and related coefficient y=0.0137x-6.1663, R=0.9991 respectively.
Interference test
Under the test condition optimized, to 5 × 10
-4mol/L superoxol measures, when relative error is ± 5%, the uric acid of 50 times, glucose, ethanol and other common inorganic ions as potassium, sodium, magnesium, calcium etc. all on mensuration without impact.There is certain interference in ascorbic acid, according to ascorbic acid instability in the basic conditions, before the assay the acidity adjustment of sample solution is caused alkalescence, places a period of time, measures again, can eliminate the interference of ascorbic acid after ascorbic acid decomposes.
The recovery is tested
Rhodamine/oxine film modified electrod is placed in mensuration system, measures Hydrogen peroxide standard solution, draw typical curve, then the compound sample of replicate determination 5 parts of synthetic samples and synthesis sample and standard specimen, utilize mark-on method to calculate the recovery.The results are shown in Table, the recovery is between 96.4 ~ 104.8%.The preparation of synthesis sample: H
2o
2(4 × 10
-3mol/L)+KCl (10
-3mol/L)+MgCl
2(10
-3mol/L)+glucose (10
-3mol/L)+uric acid (5 × 10
-3mol/L)+ascorbic acid (5 × 10
-3mol/L).
Table 1 sample analysis and the recovery (n=5)
The above; be only the present invention's preferably embodiment; protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses, the simple change of the technical scheme that can obtain apparently or equivalence are replaced and are all fallen within the scope of protection of the present invention.
Claims (2)
1. a preparation method for rhodamine 6G/oxine film modified electrod, is characterized in that, comprise the following steps:
(1) successively by ITO electrode ultrasonic cleaning 2min in acetone, absolute ethyl alcohol, intermediate water, dry, stand-by;
(2) pretreated electrode puts into 5 × 10
-4mol/L rhodamine 6G+0.1mol/LNaH
2pO
4-Na
2hPO
4in buffer solution, pH=7.0+0.1mol/LNaCl system, connect three-electrode system, utilize cyclic voltammetry to carry out scanning polymerization rhodamine 6G film, scanning potential range is-1.1 ~ 1.6V; Sweep speed is 50mV/s; Scanning hop count is 20 sections;
(3), after completing polymerization, take out the electrode modified, rinse well with redistilled water, dry, for subsequent use;
(4) the rhodamine 6G modified electrode after drying is put into 5 × 10
-4in the oxine+0.1mol/LNaCl system of mol/L, connect three-electrode system, in-0.9 ~ 1.4V potential range, with 100mV/s sweep speed electrochemical polymerization 14 sections, rhodamine/oxine film modified electrod can be obtained.
2. according to claim 1 preparation method obtain rhodamine 6G/oxine film modified electrod hydrogen peroxide in actual sample quantitative test in application.
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