CN109060906A - The preparation method and application of the poly- complex film modified glass-carbon electrode of gold/acetylene black - Google Patents
The preparation method and application of the poly- complex film modified glass-carbon electrode of gold/acetylene black Download PDFInfo
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- CN109060906A CN109060906A CN201810736175.7A CN201810736175A CN109060906A CN 109060906 A CN109060906 A CN 109060906A CN 201810736175 A CN201810736175 A CN 201810736175A CN 109060906 A CN109060906 A CN 109060906A
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Abstract
The invention discloses a kind of preparation methods of poly- complex film modified glass-carbon electrode of gold/acetylene black, comprising the following steps: 1) ultrasonic disperse in secondary distilled water is added in acetylene black and obtains acetylene black suspension；2) glass-carbon electrode of polishing is successively cleaned by ultrasonic in dehydrated alcohol and secondary distilled water, then is rinsed well with secondary distilled water, acetylene black hanging drop is added in glassy carbon electrode surface, be placed under infrared lamp and dry to obtain acetylene black modified glassy carbon electrode；3) acetylene black modified glassy carbon electrode is placed at containing HAuCl4KNO3In solution, electric current-time sweep is carried out to obtain the final product with time 100s for -0.2V in current potential.Preparation process of the present invention is easy, convenient for application, and has positive effect to the quantitative analysis and sample detection of catechol.
Description
Technical field
Present invention relates particularly to the preparation method and applications of the poly- complex film modified glass-carbon electrode of gold/acetylene black.
Background technique
Catechol, which is called, does catechol, has compared with strong reducing property, can directly the intracorporal a variety of physiological activities of participant and
Process, and have the effects of good convergence and sterilization to skin, the base for being widely used in organic chemical industry, synthesizing fine chemicals
This raw material, while also having larger toxicity to environment and human body.Often ring is inadvertently discharged into during its manufacture and use
In border, biggish pollution is caused to water resource.Thus, the Sensitive Detection of catechol is carried out in environmental protection and human health etc.
Aspect means a great.Currently, the measuring method of catechol mainly has spectrophotometry, chemoluminescence method, electrochemical method, height
Effect liquid phase chromatogram method and capillary electrophoresis etc..However, they require to implement sample the operation such as pretreatment mostly.Therefore, it grasps
Make that step is lengthy and jumbled, amount of reagent is big, on-the-spot test is difficult to carry out.Since catechol has certain electro-chemical activity, and
It is oxidizable, so being suitble to electrochemically measure.For other measurement methods, electrochemical process has many significant
Feature, for example, fast, high sensitivity and at low cost etc., thus receive significant attention.
The advantages that biggish specific surface area, preferable catalytic activity and special physical property, makes nanoparticle in sensor
Aspect application effect is rather good.Acetylene black (acetylene black, AB) is by acetylene through thermally decomposing obtained carbon black, group
It is chain structure at the particle of this substance, microparticle surfaces are mainly graphite crystal, therefore have high specific surface area and good electronics
Transport properties.In recent years, nanogold obtains general due to special natures such as catalytic activity, biocompatibility, interface alternations
All over application, such as in terms of electrode modification, nanogold can accelerate the specific surface area of electron transmission ability and electrode.
Summary of the invention
The object of the present invention is to provide the preparation method and applications of the poly- complex film modified glass-carbon electrode of gold/acetylene black.
For achieving the above object, the technical scheme adopted by the invention is as follows:
The preparation method of the poly- complex film modified glass-carbon electrode of gold/acetylene black, comprising the following steps:
1) ultrasonic disperse in secondary distilled water is added in acetylene black and obtains acetylene black suspension；
2) glass-carbon electrode of polishing is successively cleaned by ultrasonic in dehydrated alcohol and secondary distilled water, then is rinsed with secondary distilled water
Completely, acetylene black hanging drop is added in glassy carbon electrode surface, is placed under infrared lamp and dries to obtain acetylene black modified glassy carbon electrode；
3) acetylene black modified glassy carbon electrode is placed at containing HAuCl4KNO3 It is -0.2V with the time in current potential in solution
100s carries out electric current-time sweep up to the poly- complex film modified glass-carbon electrode of gold/acetylene black；The KNO3 In solution,
HAuCl4 Content be 0.1wt%, KNO3Concentration be 1 mmol/L.
In step 2, the effective diameter of glass-carbon electrode is 3 mm.
In step 2, the glass-carbon electrode of polishing, which refers to, to be first passed through after sand paper is polished again successively with 0.5 mm and 0.05 mm
Alumina powder and chamois leather be polished to and obtained in mirror surface.
In step 2, the dripping quantity of acetylene black suspension is 6 μ L, acetylene black in acetylene black suspension on each glass-carbon electrode
Content be 1mg/mL.
The poly- complex film modified glass-carbon electrode of gold/acetylene black being prepared using the method is in catechol test
Application.
Compared with prior art, the invention has the following advantages that
In the present invention, acetylene black (AB) is dispersed in distilled water, AB modification electricity is made on the surface glass-carbon electrode (GCE) in drop coating
Then pole utilizes electro-deposition method one layer of gold on AB surface aggregate, be used for sensitive determination catechol CAT.Acetylene black (AB)
Make the poly- complex film modified glass-carbon electrode of gold/acetylene black spirit with higher in biosensor application with poly- golden film synergistic effect
Sensitivity and stability.Moreover, the poly- complex film modified glass-carbon electrode response of gold/acetylene black is fast in the present invention, preparation process is easy, just
There is positive effect in application, and to the quantitative analysis and sample detection of catechol；
It is measured using differential pulse voltammetry, catechol is 1.0 × 10-6~4.0 × 10-4 In mol/L concentration range and oxygen
Changing peak current has good linear relationship, and related coefficient is respectively 0.999.When signal-to-noise ratio is 3, catechol detection is limited to
5.0×10-7mol/L。
Detailed description of the invention
Fig. 1 is the cyclic voltammogram of different modifying electrode, wherein (a) GCE, (b) Au/GCE, (c) AB/GCE,
(d) Au/ AB/GCE, sweeping speed is 100 mV/S；
Fig. 2 is that difference sweeps influence of the speed to CAT Redox behavior, and wherein a-j is followed successively by 20,50,80,100,120,
150, 180, 200, 300, 400 mV/s；
Fig. 3 is influence of the pH to CAT peak current, and wherein a-f is successively are as follows: 5.5,6.0,6.5,7.0,7.5,8.0,
8.5；
Fig. 4 is the differential pulse voltammetry figure of various concentration CAT；Wherein a-h is followed successively by 1,5,25,50,75,100,200,400
μmol/L。
Specific embodiment
Using specific embodiment, the present invention will be further described below.
Embodiment 1
The preparation method of the poly- complex film modified glass-carbon electrode of gold/acetylene black, comprising the following steps:
1) ultrasonic disperse in secondary distilled water is added in acetylene black and obtains acetylene black suspension；Acetylene black in acetylene black suspension
Content is 1mg/mL；
2) glass-carbon electrode by the polishing that effective diameter is 3 mm is successively cleaned by ultrasonic in dehydrated alcohol and secondary distilled water, then
It is rinsed well with secondary distilled water, acetylene black hanging drop is added in glassy carbon electrode surface, is placed under infrared lamp and dries to obtain acetylene
Black modified glassy carbon electrode AB/GCE；The glass-carbon electrode of polishing refer to first pass through sand paper polishing after again successively with 0.5 mm with
The alumina powder and chamois leather of 0.05 mm is polished to be obtained in mirror surface；The dripping quantity of acetylene black suspension on each glass-carbon electrode
For 6 μ L；
3) acetylene black modified glassy carbon electrode is placed at containing HAuCl4KNO3 (it is passed through high pure nitrogen deoxygenation in advance in solution
30 min, nitrogen atmosphere protection), in -0.2V constant potential electro-deposition 100s, makes golden particle deposition in electrode surface, which is used
Water cleans up, and high pure nitrogen dries up up to the complex film modified glass-carbon electrode Au/AB/GCE of poly- gold/acetylene black；The KNO3 It is molten
In liquid, HAuCl4 Content be 0.1wt%, KNO3Concentration be 1 mmol/L.
Using application of the obtained poly- complex film modified glass-carbon electrode of gold/acetylene black in detection catechol, including with
Lower step:
A. the three-electrode system used for the poly- complex film modified glass-carbon electrode of gold/acetylene black be working electrode (d=3 mm), saturation
Calomel electrode (SCE) is reference electrode, and platinum column electrode is auxiliary electrode；
B. the PBS for being 6.5 using pH prepares the CAT of various concentration as solvent, and as electrolyte solution, three polar body systems are inserted respectively
In the electrolyte solution for entering various concentration CAT, it is -0.3 ~ 0.4 V range in current potential, carries out DPV scanning, tied according to scanning
Fruit makes the working curve of CAT concentration and peak current；
C. sample to be tested is handled as the PBS electrolyte solution that bottom liquid is pH 6.5, three-electrode system is inserted into the electricity of the sample
In electrolyte solution, DVP scanning is carried out under the conditions of step B, according to gained peak current size, in the working curve of step B
To the concentration of sample to be tested.
Comparative example 1
The preparation of decorated by nano-gold electrode:
Ready bare glassy carbon electrode is placed on containing 0.1%HAuCl4KNO3(it is passed through high pure nitrogen deoxygenation in advance in solution
30 min, nitrogen atmosphere protection), in -0.2V constant potential electro-deposition 100s, makes golden particle deposition in electrode surface, which is used
Water cleans up, and high pure nitrogen drying is made decorated by nano-gold electrode (Au/GCE).
Application effect experiment
To show invention effect, the poly- complex film modified glass-carbon electrode of gold/acetylene black being prepared using the method is in neighbour
Application in benzenediol test, in application, the three-electrode system used: the poly- complex film modified glass-carbon electrode of gold/acetylene black is work
Make electrode (d=3mm), saturated calomel electrode (SCE) is reference electrode, and platinum column electrode is auxiliary electrode.Catechol is with 0.1
The PBS solution allocation of mol/L, the disodium hydrogen phosphate of 0.2 mol/L of 0.1mol/L buffer solution of sodium phosphate (PBS), 0.2
Mol/L sodium dihydrogen phosphate and 0.1 mol/L potassium chloride mixed solution are formulated, and are then adjusted to required pH value.
When test, with cyclic voltammetry (CV) within the scope of the V of -0.3 V ~ 0.4, sweep speed is 100 mV, is surveyed
Determine electrochemical behavior of the modified electrode different obtained in embodiment 1 and comparative example 1 in CAT；In the pH 6.5 of 10 mL
PBS solution in, the desired amount of measured matter i.e. CAT is added, is then measured using differential pulse voltammetry (DPV), is swept
Retouching range is -0.3 ~ 0.4 V, and the amplitude of DPV is 0.05 V, and sampling width is 0.0167 V, and pulse width is 0.05 s, pulse
Time is 0.5 s, and quiescent time is 2 s, and all experimental operating conditions are all to carry out at normal temperature.
1, electrochemical behavior of the CAT on modified electrode
Electrochemical behavior (Fig. 1) of the different modifying electrode in PBS has been investigated with cyclic voltammetry.The concentration of CAT is 500
μmol/L.Occurs flat and wide an oxidation peak and reduction peak respectively near 0.25 V and 0.05 V in bare glassy carbon electrode
(curve a) in Fig. 2.As shown in curve b, after modifying upper gold on electrode, the oxidation peak of CAT is significantly compared to bare glassy carbon electrode
Enhancing, ratio of peak bare glassy carbon electrode improve nearly 1/2.This is because poly- gold has good conductive property, can effectively facilitate
The transmitting of CAT peak current on the electrode, improves detection sensitivity.After glass-carbon electrode modifies upper AB, the oxidation of CAT is also
Parent peak has obtained further enhancing, as shown in curve c in Fig. 2.Ratio of peak bare glassy carbon electrode of the CAT on AB/GCE improves will
Nearly 2 times.This is because AB has catalytic action, while its good conductive capability to the redox reaction of CAT on AB/GCE
Promote electron transmission speed.Furthermore AB big specific surface area is also capable of increasing its adsorption capacity to CAT.In Au/
On AB/GCE, due to the collective effect of AB and poly- golden film, the redox peaks of CAT are higher than above three electrode, oxidation peak
Electric current is nearly 3 times of bare electrode, significantly improves detection sensitivity.
, sweep speed influence
As shown in Fig. 2, having studied different speed of sweeping within the scope of 20~1000 mV ∕ s to the shadow of catechol electrochemical oxidation
It rings.It can be seen from the figure that the oxidation peak and reduction peak current of CAT increases with it with the increase for sweeping speed, spike potential difference
Slightly shuffle and bear shifting.Peak current is in good linear relationship with fast square root is swept, for oxidation peak current, linear equation are as follows:I p = 3.76 ν 1/2 - 7.13,R 2= 0.997.For reduction peak current, linear equation are as follows:I p = -3.80 ν + 7.60,R 2= 0.998.This illustrates that CAT on modified electrode surface is a diffusion controlled process.
, pH influence
Influence of the pH for CAT electrochemical behavior on the electrode is had studied in 5.5~8.0 range of pH.It can from Fig. 3
To see, in 5.5~6.5 range of pH, CAT oxidation peak current is maximum when pH is 6.5, and pH is at 5.5~6.5, oxygen
Change peak current to reduce, and pH is in 6.5~8.5 ranges, as the increase oxidation peak current of pH reduces.Therefore, pH is selected
6.5 be the pH of supporting electrolyte.As shown in figure 3, having investigated pH for the oxidation spike potential of CAT and having restored spike potential
It influences.The experimental results showed that oxidation spike potential and reduction spike potential and pH are in good linear relationship.For oxidation peak electricity
Position, linear equation are as follows:E (V) = - 0.051pH + 0.479 (R 2= 0.999).For restoring spike potential, linear equation
Are as follows:E (V) = - 0.056 pH + 0.568 (R 2= 0.996).In order to obtain higher current-responsive, select pH=
6.5 PBS is as supporting electrolyte.
, the range of linearity and detection limit
As shown in figure 4, the CAT solution for pipetting various concentration respectively utilizes differential pulse voltammetry under above-mentioned optimal conditions
Measure the oxidation peak current of CAT.The result shows that corresponding oxidation peak current is also gradually increased with the increase of CAT concentration.?
1.0×10-6~4.0 × 10-4In mol/L concentration range, the peak current of CAT and its concentration are in good linear relationship, linearly
Equation isI p (μ A)=0.0643-0.107c(μm ol/L), related coefficient 0.999, when signal-to-noise ratio is equal to 3, detection is limited to
5.0×10-7 mol/L。
As it can be seen that electrochemical sensor made of acetylene black and In Glassy Carbon Electrode Modified With Nano-gold is used for CAT sensitive determination,
It is high that it detects response performance.The complex film modified electrode there is good electricity to urge the electrochemical redox process of CAT
Change activity, the glass-carbon electrode of modified shows as its oxidation peak and reduction peak current significantly improves, and aoxidizes the negative shifting of spike potential.
This is because electric conductivity that acetylene black has excellent electric conductivity and catalytic performance and nanogold polymeric membrane excellent and at
Film properties.By the experimental results showed that, which has easy preparation, measurement accuracy, at low cost, reproducibility, stability
The advantages that good and anti-interference ability is preferable.The analysis method established also sensitivity with higher and the wider range of linearity.
Claims (5)
1. the preparation method of the poly- complex film modified glass-carbon electrode of gold/acetylene black, which comprises the following steps:
Ultrasonic disperse in secondary distilled water is added in acetylene black and obtains acetylene black suspension；
The glass-carbon electrode of polishing is successively cleaned by ultrasonic in dehydrated alcohol and secondary distilled water, then is rinsed and is done with secondary distilled water
Only, acetylene black hanging drop is added in glassy carbon electrode surface, is placed under infrared lamp and dries to obtain acetylene black modified glassy carbon electrode；
Acetylene black modified glassy carbon electrode is placed at containing HAuCl4KNO3 It is -0.2 V with the time in current potential in solution
100s carries out electric current-time sweep up to the poly- complex film modified glass-carbon electrode of gold/acetylene black；The KNO3 In solution,
HAuCl4 Content be 0.1wt%, KNO3Concentration be 1 mmol/L.
2. the preparation method of the poly- complex film modified glass-carbon electrode of gold/acetylene black as described in claim 1, which is characterized in that step
It is rapid 2) in, the effective diameter of glass-carbon electrode is 3 mm.
3. the preparation method of the poly- complex film modified glass-carbon electrode of gold/acetylene black as described in claim 1, which is characterized in that step
It is rapid 2) in, the glass-carbon electrode of polishing refer to first passes through sand paper polishing after again successively with the alumina powder of 0.5 mm and 0.05 mm
End and chamois leather are polished to and obtain in mirror surface.
4. the preparation method of the poly- complex film modified glass-carbon electrode of gold/acetylene black as described in claim 1, which is characterized in that step
It is rapid 2) in, the dripping quantity of acetylene black suspension is 6 μ L on each glass-carbon electrode, and the content of acetylene black is in acetylene black suspension
1mg/mL。
5. being existed using the poly- complex film modified glass-carbon electrode of gold/acetylene black that any method of claim 1-4 is prepared
Test the application in catechol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111725525A (en) * | 2020-06-18 | 2020-09-29 | 上海交通大学 | Carbon-supported monodisperse Pt-Ni nanoparticle catalyst prepared by electrodeposition and preparation and application thereof |
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| CN107402246A (en) * | 2017-07-13 | 2017-11-28 | 信阳师范学院 | Electrode based on nanogold/nanometer acetylene black modification and its preparation method and application |
| CN107607600A (en) * | 2017-08-18 | 2018-01-19 | 四川农业大学 | Detect catechol and NO2Sensor and its construction method and application |
Non-Patent Citations (2)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111725525A (en) * | 2020-06-18 | 2020-09-29 | 上海交通大学 | Carbon-supported monodisperse Pt-Ni nanoparticle catalyst prepared by electrodeposition and preparation and application thereof |
| CN111725525B (en) * | 2020-06-18 | 2022-03-15 | 上海交通大学 | Carbon-supported monodisperse Pt-Ni nanoparticle catalyst prepared by electrodeposition and preparation and application thereof |
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Application publication date: 20181221 |