CN103018304A - Glassy carbon electrode modified by nickel oxide-graphene nano material, preparation method and application thereof - Google Patents
Glassy carbon electrode modified by nickel oxide-graphene nano material, preparation method and application thereof Download PDFInfo
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- CN103018304A CN103018304A CN2013100056197A CN201310005619A CN103018304A CN 103018304 A CN103018304 A CN 103018304A CN 2013100056197 A CN2013100056197 A CN 2013100056197A CN 201310005619 A CN201310005619 A CN 201310005619A CN 103018304 A CN103018304 A CN 103018304A
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Abstract
The invention belongs to the technical field of electrochemistry and nano materials and especially relates to a glassy carbon electrode modified by nickel oxide-graphene nano material, a preparation method and an application of the electrode for detecting acetaminophen. The preparation method comprises the following steps of: firstly, dispersing graphene oxide ultrasonically in ultrapure water to obtain a graphene oxide colloidal solution; subsequently, mixing the prepared graphene oxide colloidal solution with a nickel sulfate solution ultrasonically to prepare an electrolyte; and then dipping a clean electrode in the prepared electrolyte, electrically depositing graphene and nickel oxide on the surface of the electrode at an even and constant electric potential, drying and washing to obtain the needed glassy carbon electrode. The glassy carbon electrode has the advantages of simple preparation process, short preparation time, non-toxicity and environmental protection and low cost; meanwhile, the glassy carbon electrode can be used for detecting the acetaminophen and also has the advantages of fast response, wide linear range, good reproducibility and high stability; and the glassy carbon electrode is not interfered by the coexisting electro-active material, so that the glassy carbon electrode is an excellent detection electrode.
Description
Technical field
The invention belongs to galvanochemistry and technical field of nano material, particularly a kind of glass-carbon electrode of modifying based on nickel oxide-graphene nano material and preparation method thereof and this electrode are used for the detection of paracetamol.
Background technology
Paracetamol (paracetamol, acetaminophen, acetaminophen) has antipyretic effect, is used for cat fever, arthralgia, neuralgia, antimigraine, pain caused by cancer and the rear pain relieving of operation etc.Yet the excessive use paracetamol can cause liver damage, and severe patient can cause stupor even dead.The hepatotoxicity wind agitation of paracetamol comes from the problem that occurs in the drug metabolism processes; in biotransformation, it can produce a kind of metabolite, i.e. N-acetyl 1,4-benzoquinone imines; its characteristic is larger, need to the protection factors such as reductive glutathione in body be combined to reduce toxicity.If it is excessive to take paracetamol dosage, or the protection such as the glutathione factor is when reducing, and causes the important large molecule of the larger intermediate metabolites of this toxicity and other to be combined, and hepatic injury will occur.Therefore, a kind of reliable, quick and economic method detects accurately paracetamol and has great importance.The detection method of paracetamol has a lot, such as: analysis by titration, spectrophotometric method, chemoluminescence method and electrochemical method.But, in these methods, electrochemical method because of its have that easy, accurate, highly sensitive, cost is low and detect before the advantage such as pre-service work weak point consuming time, be widely used in the detection of paracetamol, so the stability of detecting electrode and reappearance are vital to testing result.But the detecting electrode reappearance of present used sensor is relatively poor, the response time is slower.
Nano particle is owing to it has larger specific surface area, good conductivity and biocompatibility plays a very important role at tool aspect the raising sensor performance.Especially metal or metal oxide nanoparticles have caused the great interest of researcher, and they utilize gold, carbon nano-tube and other nano particles to make up the acetparaminosalol phenol sensor.Meanwhile, Graphene is because its unique structure, high physical strength, tuneable optical property and electric conductivity enjoy liking of researcher.Yet traditional preparation method, especially chemical reduction method tend to cause the pollution of product.Because chemical reduction method often uses the poisonous or expensive reagent such as hydrazine or sodium borohydride as reductive agent.Therefore, a kind of green method for preparing Graphene of exploitation is very significant.The method that studies show that in recent years, Direct electrochemical reduction graphene oxide prepare Graphene is very effective, and the Graphene of electrochemical reduction has been applied to many fields: such as sensor, capacitor and fuel cell etc.
Summary of the invention
The purpose of this invention is to provide the glass-carbon electrode that a kind of nickel oxide-graphene nano material is modified, this electrode has response time weak point, favorable reproducibility, the high and good catalytic oxidation activity of stability for the detection of paracetamol.
Another object of the present invention provides the preparation method of the glass-carbon electrode of a kind of above-mentioned nickel oxide-graphene nano material modification.
Purpose of the present invention can realize by following scheme:
A kind of method for preparing the glass-carbon electrode of nickel oxide-graphene nano material modification, its step comprises:
(1) is dispersed in the ultrapure water graphene oxide is ultrasonic, obtains graphene oxide colloidal solution, then the graphene oxide colloidal solution and the NiSO that make
46H
2The ultrasonic electrolytic solution that is mixed of O solution;
(2) with in the prepared electrolytic solution in the clean electrode immersion step (1), behind electrode surface constant potential electro-deposition Graphene and nickel oxide, dry, wash.Preferably, first with electrode with the polishing of the aluminium powder of 0.3 μ m, then successively ultrasonic processing 3-5 minute in ultrapure water, absolute ethyl alcohol, ultrapure water namely gets clean electrode after drying.
In the electrolytic solution of described step (1), the proportioning of graphene oxide and Ni ion is 1g:3-20mmol.Preferably, in the electrolytic solution in the described step (1), the proportioning of graphene oxide and Ni ion is 1g:5-10mmol.
The graphene oxide content of the electrolytic solution in the described step (1) is 1～4mg/ml.
Also contain 0.02～0.05mol/L sodium sulphate in the electrolytic solution in the described step (1).
In the described step (2), the used current potential of potentiostatic electrodeposition is-1.0 ~-1.8V, the used time of potentiostatic electrodeposition is 50 ~ 2100 seconds.Preferably, the used current potential of potentiostatic electrodeposition is-1.5V that the used time of potentiostatic electrodeposition is 150-200 second.
The invention still further relates to the application of glass-carbon electrode in detecting paracetamol that nickel oxide-graphene nano material is modified.
Graphene oxide used in the present invention is to adopt improvement Hummers method to prepare.
The invention has the beneficial effects as follows: 1, the preparation method of the glass-carbon electrode of described nickel oxide-graphene nano material modification adopts galvanochemistry one stage reduction method to obtain, and preparation technology is simple, preparation time is short, asepsis environment-protecting, and cost is low.2, the even electro-deposition of described glass-carbon electrode outside surface has Graphene and nickel oxide, can be used for the detection of paracetamol, and it is active that the detected representation of paracetamol is gone out good catalytic oxidation, and the tool response time is fast, the range of linearity is wide, favorable reproducibility, stable high, and the interference of the electroactive material that is not coexisted, detection is limited to 2 * 10 to paracetamol
-8Mol/L is a kind of good detecting electrode.
Description of drawings
Fig. 1 is nickel oxide-graphene nano particle (a), the Graphene (b) of electrochemical reducing preparation and the Raman spectrogram of graphene oxide (c), and interior illustration is the raman signatures spectrum of nickel oxide.
Fig. 2 is the field emission scanning electron microscope figure of the glass-carbon electrode of nickel oxide-graphene nano material modification.
Fig. 3 is the photoelectron spectroscopy figure of the glass-carbon electrode of nickel oxide-graphene nano material modification.
Fig. 4 is the photoelectron spectroscopy figure (a) of graphene oxide, the photoelectron spectroscopy figure (b) of the Graphene of electrochemical reducing preparation.
Fig. 5 is the photoelectron spectroscopy figure of electro-deposition gained nickel oxide.
Fig. 6 is that the glass-carbon electrode of nickel oxide-graphene nano material modification is to the cyclic voltammogram of paracetamol.
Fig. 7 be the glass-carbon electrode modified of nickel oxide-graphene nano material to the differentiated pulse volt-ampere curve figure of paracetamol, interior illustration is that this glass-carbon electrode is to the peak current of the detection of paracetamol and the graph of a relation of concentration.
Fig. 8 is that the glass-carbon electrode modified of nickel oxide-graphene nano material and common graphite alkene glass-carbon electrode are to the differentiated pulse volt-ampere curve figure of the interference test of paracetamol.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
The used equipment of present embodiment: the shooting of Hitachi S-4800 type scanning electron microscope, pHS-3C acidity meter for laboratory, KQ3200E type ultrasonic cleaner, PHI5000ESCA x-ray photoelectron spectroscopy, LabRam Π, Dilor(France) spectrometer.
With glass-carbon electrode with the polishing of the aluminium powder of 0.3 μ m, more successively at ultrapure water, absolute ethyl alcohol, ultrasonic processings is 3-5 minute in the ultrapure water, makes the glass carbon of cleaning, then dries at ambient temperature, for subsequent use;
Take by weighing 4mg graphene oxide (this graphene oxide adopts the Hummers method to synthesize) and be dissolved in the 1ml ultrapure water, ultrasonic processing 6 hours, so that graphene oxide is dispersed in the ultrapure water, obtaining concentration is the graphene oxide colloidal solution of 4mg/mL;
Be the NiSO of 40mmol/L with concentration
46H
2O solution (the Na that wherein contains 0.1mol/L in the solution
2SO
4As supporting electrolyte) and the graphene oxide colloidal solution of the above-mentioned preparation ratio take volume ratio as 1:1.5 mix, ultrasonic processing 5 minutes makes electrolytic solution; The clean glass-carbon electrode of processing is immersed in this electrolytic solution, and electro-deposition is 150 seconds under-1.5V constant potential, then glass-carbon electrode is dried in air, and washing namely gets the glass-carbon electrode that nickel oxide-graphene nano material is modified.
Embodiment 2
With glass-carbon electrode with the polishing of the aluminium powder of 0.3 μ m, more successively at ultrapure water, absolute ethyl alcohol, ultrasonic processings is 3-5 minute in the ultrapure water, makes the glass carbon of cleaning, then dries at ambient temperature, for subsequent use;
Take by weighing 5mg graphene oxide (this graphene oxide adopts the Hummers method to synthesize) and be dissolved in the 1mL ultrapure water, ultrasonic processing 6.5 hours, so that graphene oxide is dispersed in the ultrapure water, obtaining concentration is the graphene oxide colloidal solution of 5mg/mL;
Be the NiSO of 50mmol/L with concentration
46H
2O solution (the Na that wherein contains 0.1mol/L in the solution
2SO
4As supporting electrolyte) and the graphene oxide colloidal solution of the above-mentioned preparation ratio take volume ratio as 1:2 mix, ultrasonic processing 5 minutes makes electrolytic solution; The clean glass-carbon electrode of processing is immersed in this electrolytic solution, and electro-deposition is 200 seconds under-1.5V constant potential, then glass-carbon electrode is dried in air, and washing namely gets the glass-carbon electrode that nickel oxide-graphene nano material is modified.
Performance characterization: the glass-carbon electrode that the used nickel oxide of following test-graphene nano material is modified is the glass-carbon electrode for preparing among the embodiment 1.
(1), Raman spectrum detects
Nickel oxide-graphene nano particle is carried out Raman spectrum to be detected, a among Raman spectrogram such as Fig. 1, the Graphene that again electrochemical process is reduced simultaneously, b among Raman spectrogram such as Fig. 1 and the graphene oxide that adopts the Hummers method to synthesize, c among Raman spectrogram such as Fig. 1 compares, and the result shows: the Graphene of graphene oxide and electrochemical process reduction has all shown stronger D peak (because defective peak that intervalley scattering forms) and strong G peak.But the Graphene of comparing the electrochemical process reduction with graphene oxide has shown a slightly strong 2D peak.And the intensity of the D/G of the Graphene of electrochemical process reduction shows that thus the number at electrochemical reduction Graphene small-medium size particle increases greater than graphene oxide.These all illustrate graphene oxide successful be reduced to Graphene.And we can observe at 400-500cm in a of Fig. 1
-1There is the raman signatures spectrum of nickel oxide in the scope, the existence of nickel oxide is described, specifically see the interior illustration among Fig. 1.
(2), the glass-carbon electrode surface topography map of nickel oxide-graphene nano material modification
Field emission scanning electron microscope is a kind of means that can be used for characterizing the electrode surface pattern.Adopt field emission scanning electron microscope to take the surface topography of glass-carbon electrode, specifically as shown in Figure 2, can observe from Fig. 2, nickel oxide is evenly distributed on the glass-carbon electrode, and the Graphene that does not occur to reunite covers on the nickel oxide surfaces.
(3), the composition detection of the glass-carbon electrode of nickel oxide-graphene nano material modification
Can see that from x-ray photoelectron spectroscopy shown in Figure 3 (XPS) figure the glass-carbon electrode that prepared nickel oxide-graphene nano material is modified only has 3 kinds of elements to form: carbon, oxygen, nickel.
For the prepared material of further sign is Graphene and nickel oxide compound, adopt the x-ray photoelectron power spectrum that the Graphene of graphene oxide and electrochemical process reduction is characterized, specifically as shown in Figure 4, Fig. 4 a is the XPS figure of graphite oxide, and Fig. 4 b is the XPS figure of the Graphene of electrochemical process reduction.Result surface: graphene oxide C1s photoelectron spectroscopy figure in contain the significantly oxygen-containing functional group of very large and degree of oxidation, belong to respectively the different functional groups of carbon: the ring-type carbon of anaerobic, epoxy carbon, hydroxyl carbon and carbonyl carbon.Although, also have identical functional group in the Graphene of electrochemical process reduction, yet their peak intensity is significantly than a little less than the graphene oxide.Thereby the method for electrochemical reduction provides a kind of feasible method for preparing graphene film at electrode.
The valence state of nickel that adopted the XPS map analysis, specifically as shown in Figure 5, the Ni(2p of the nickel oxide among Fig. 5 (NiO)) feature is in conjunction with can be as follows: 855.8eV(2p
3/2), 861.6eV (2p
3/2), 873.6eV (2p
1/2) and 879.0eV (2p
1/2), show the existence of nickel oxide, and testing result is also corresponding with the Raman spectrogram among Fig. 1.
(4), the glass-carbon electrode of nickel oxide-graphene nano material modification is to the detection of paracetamol (AP)
A, electrocatalysis characteristic
The glass-carbon electrode that the nickel oxide-graphene nano material of preparation is modified is that the AP solution of 1mmol/L has carried out the electro-catalysis test to concentration, specifically see Fig. 6, do not having the PBS(pH=7.0 of AP) solution in be a level and smooth curve, shown in a detection line among the figure, when having added after concentration is the AP of 1mmol/L, can observe a pair of obvious redox peak occurs, shown in the b detection line among the figure, hence one can see that: the glass-carbon electrode that nickel oxide-graphene nano material is modified has good catalytic performance to AP.
B, detectability
Adopt Differential Pulse Voltammetry, the glass-carbon electrode that the test nickel oxide-the graphene nano material is modified is to detectability and the range of linearity of AP, and concrete test result is 2 * 10 in concentration as shown in Figure 7
-8Mol/L to 1 * 10
-4In the mol/L scope, prepared glass-carbon electrode has good linearity to AP, detects and is limited to 2 * 10
-8Mol/L.
C, selectivity and disturbed test
In the analysis experiment of actual sample, the electroactive material of some coexistences may disturb the testing result to AP, so carried out selectivity and interference experiment.The glass-carbon electrode that nickel oxide-graphene nano material is modified is tested as agent interfering adding respectively dopamine, ascorbic acid and uric acid in the AP testing process, and the dopamine, ascorbic acid and the uric acid that add same concentrations when detecting AP with common Graphene electrodes are tested as a comparison.Concrete outcome is as follows:
The glass-carbon electrode that utilizes nickel oxide-graphene nano material to modify to the AP testing process in, add concentration and be dopamine, ascorbic acid and the uric acid of 0.1mmol/L, but detection does not cause obvious interference to AP, shown in a detection line of Fig. 8, and the detected peaks when utilizing common Graphene electrodes to detect AP is compared (the b detection line of Fig. 8), the peak is strong obviously to become large, illustrates that prepared glass-carbon electrode detects AP and has good selectivity.
Simultaneously, also the AP content in the actual sample (day and night hundred clothes are given repeated exhortations) is measured, the result is as shown in table 1, day, the sheet recovery was 95.93% ~ 103.5%, the relative standard deviation (RSD) of measuring for 5 times is 3.373%, because night sheet with day sheet compared a kind of composition of chlorphenamine maleate many, thereby to night sheet also carried out corresponding analysis, the result shows: chlorphenamine maleate does not disturb the detection of AP, night, the recovery of sheet was 98.24% ~ 102.4%, RSD=2.079%(n=5), illustrate that this glass-carbon electrode is very high to the Detection accuracy of AP.
Table 1
D, stability test
The glass-carbon electrode that same nickel oxide-graphene nano material modified is that the AP of 1mmol/L carries out 5 parallel experiments to concentration, the result shows that the relative standard deviation of these 5 times experiments is less than 1.489%, prepare the AP that 5 identical electrodes detect 1mmol/L simultaneously, relative standard deviation is 2.622%, and the above results has illustrated that this glass-carbon electrode has good reappearance.This glass-carbon electrode is preserved at normal temperatures and was that the AP of 1mmol/L measures to concentration in per 5 days, the peak current of finding this glass-carbon electrode after one month is original 91.40%, has illustrated that thus the glass-carbon electrode that nickel oxide-the graphene nano material is modified that adopts this law preparation has good stability.
Claims (10)
1. the glass-carbon electrode modified of a nickel oxide-graphene nano material, it is characterized in that: the even electro-deposition of described glass-carbon electrode outside surface has nickel oxide and graphene nano particle.
2. the preparation method of the glass-carbon electrode modified of a nickel oxide as claimed in claim 1-graphene nano material, its step comprises:
(1) is dispersed in the ultrapure water graphene oxide is ultrasonic, obtains graphene oxide colloidal solution, then the graphene oxide colloidal solution that makes and the ultrasonic electrolytic solution that is mixed of nickel sulfate solution;
(2) with in the prepared electrolytic solution in the clean electrode immersion step (1), behind electrode surface constant potential electro-deposition Graphene and nickel oxide, dry, wash.
3. the method for the glass-carbon electrode modified of preparation nickel oxide according to claim 2-graphene nano material, it is characterized in that: in the electrolytic solution of described step (1), the proportioning of graphene oxide and Ni ion is 1g:3-20mmol.
4. the method for the glass-carbon electrode modified of preparation nickel oxide according to claim 3-graphene nano material, it is characterized in that: the graphene oxide of the electrolytic solution in the described step (1) and the proportioning of Ni ion are 1g:5-10mmol.
5. the method for the glass-carbon electrode modified of preparation nickel oxide according to claim 2-graphene nano material, it is characterized in that: the graphene oxide content of the electrolytic solution in the described step (1) is 1～4mg/mL.
6. the method for the glass-carbon electrode of preparation nickel oxide according to claim 2-graphene nano material modification is characterized in that: also contain 0.02～0.05mol/L sodium sulphate in the electrolytic solution in the described step (1).
7. the method for the glass-carbon electrode modified of preparation nickel oxide according to claim 2-graphene nano material is characterized in that: in the described step (2), the used current potential of potentiostatic electrodeposition is-1.0 ~-1.8V, the used time of potentiostatic electrodeposition is 50 ~ 2100 seconds.
8. the method for the glass-carbon electrode modified of preparation nickel oxide according to claim 7-graphene nano material, it is characterized in that: in the described step (2), the used current potential of potentiostatic electrodeposition is-1.5V that the used time of potentiostatic electrodeposition is 150-200 second.
9. the method for the glass-carbon electrode modified of preparation nickel oxide according to claim 2-graphene nano material, it is characterized in that: in the described step (2), first with the aluminium powder polishing of electrode with 0.3 μ m, then successively ultrasonic processing 3-5 minute in ultrapure water, absolute ethyl alcohol, ultrapure water namely gets clean electrode after drying.
10. the application of glass-carbon electrode in detecting paracetamol of nickel oxide claimed in claim 1-graphene nano material modification.
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