CN109709178A - A kind of preparation method and application of nanometer of platinum/graphen flexible electrode - Google Patents
A kind of preparation method and application of nanometer of platinum/graphen flexible electrode Download PDFInfo
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- CN109709178A CN109709178A CN201910151118.7A CN201910151118A CN109709178A CN 109709178 A CN109709178 A CN 109709178A CN 201910151118 A CN201910151118 A CN 201910151118A CN 109709178 A CN109709178 A CN 109709178A
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Abstract
The invention belongs to technical field of food safety detection, and in particular to the preparation method and application of a kind of nanometer of platinum/graphen flexible electrode；The preparation method of nanometer platinum/graphen flexible electrode, comprising the following steps: Step 1: preparing the precursor solution of graphene oxide solution and platinum respectively；Step 2: preparation graphene oxide paper；Step 3: carrying out electronation to graphene oxide paper redox graphene flexible electrode is made；Step 4: redox graphene flexible electrode is connected to an electrochemical workstation, the precursor solution of platinum is added in electrolyte, is scanned using cyclic voltammetry, nanometer platinum/graphen flexible electrode is made.Compared with traditional electrode testing result, nanometer platinum/graphen flexible electrode detection sensitivity is higher, and hydrogen is not precipitated in detection process, as a result more stable, while detection range is also wider；And electrode is more flexible in structure, it is easier to be miniaturized, be suitble to the quick detection under various occasions to gallic acid.
Description
Technical field
The invention belongs to technical field of food safety detection, and in particular to the system of a kind of nanometer of platinum/graphen flexible electrode
Preparation Method and application.
Background technique
Gallic acid (Galic acid, GA) is a kind of main natural phenolic ingredient, a kind of important organic fine
Product, are widely used in pharmacy and food industry.Gallic acid have powerful anti-oxidizing activities, have anticancer, anti-inflammatory,
The various biologicals such as anti-oxidant, antimicrobial, anti-cardiovascular disease and pharmaceutical use.
There are chemoluminescence method, high performance liquid chromatography (HPLC), liquid chromatogram-string for gallic acid detection method at present
Join mass spectrography (LC-MS/MS), reflux injection method (Reverse Flow Injection, RFI) etc..These technologies have very high
Sensitivity, but need expensive instrument, complicated pre-treatment step and professional operator.And in numerous electrochemistry
It is traditional modification and detection method based on solid electrode mostly in detection method, has in these electrochemical detection methods
One or more disadvantages, detection sensitivity is poor, and the range of linearity is narrow, detection environmental suitability difference etc..
Summary of the invention
In view of the above shortcomings of the prior art, the present invention provides a kind of nanometer of platinum/graphen flexible electrode and application.
In order to achieve the above object of the invention, the invention adopts the following technical scheme:
A kind of preparation method of nanometer of platinum/graphen flexible electrode, comprising the following steps:
Step 1: preparing the precursor solution of graphene oxide solution and platinum respectively；
Step 2: preparation graphene oxide paper；
Step 3: carrying out electronation to graphene oxide paper redox graphene flexible electrode is made；
Step 4: redox graphene flexible electrode is connected to an electrochemical workstation, by the precursor solution of platinum
It is added in electrolyte, is scanned using cyclic voltammetry, nanometer platinum/graphen flexible electrode is made.
Preferably, in the nanometer platinum/graphen flexible electrode mass ratio of Platinum Nanoparticles and graphene be (1~
3): 200.
Preferably, the preparation graphene oxide paper, specifically includes:
Graphene oxide solution is uniformly mixed with ascorbic acid solution, is protected from light sealing and standing after ultrasonic setting time；
Mixed liquor after standing is poured into the vacuum filtration tank equipped with aqueous filter paper and is filtered, is covered on aqueous filter paper
Lid film layer；
Aqueous filter paper is transferred to freeze drier to be freeze-dried, the graphene oxide paper tentatively restored is made.
Preferably, the mass ratio of the graphene oxide and ascorbic acid is 1:(1~2).
Preferably, described that graphene flexible electrode is made, it specifically includes:
The front that graphene oxide paper is clung by adhesive tape is cut into target size and removes aqueous filter paper, obtains
Desirable oxidation graphene paper；
Desirable oxidation graphene paper is placed in hydroiodic acid solution and submerges and carries out oscillation preset time, is then taken out clear
It washes, air-dry, redox graphene flexible electrode is made.
Preferably, the sweep parameter of the cyclic voltammetry includes: voltage scan range -1.3~0.8V, scanning
Speed 50mV/s, scanning circle number 10~15 enclose.
The present invention also provides the applications of nanometer platinum/graphen flexible electrode made from above-mentioned preparation method, are used for galla turcica
The Concentration Testing of acid.
Preferably, the Concentration Testing of the gallic acid, comprising the following steps:
(a) nanometer platinum/graphen flexible electrode is determined with electrode is clamping, with platinum electrode, three electricity of saturated calomel electrode composition
Polar body system；
(b) it takes the phosphate buffer solution of certain volume, gallic acid titer to be placed in electrolytic cell, carries out square wave voltammetry
Scanning, and be stirred before each scanning, record the scanning curve of square wave voltammetry；
(c) linear relationship between the various criterion concentration and peak current of gallic acid titer is compared, obtains electrode pair
In the correction equation of gallic acid；
(d) it takes the phosphate buffer solution of certain volume, prepare liquid to be placed in electrolytic cell, carries out square wave voltammetry scanning, and
It is stirred before each scanning, records the scanning curve of square wave voltammetry to obtain the peak current of prepare liquid, and according to correction
Equation obtains the concentration of gallic acid in prepare liquid.
Preferably, the sweep parameter of the square wave voltammetry are as follows: scanning voltage range 0.2-0.7V, quiet hour
3s, amplitude 0.025V, period 40ms, pulsewidth 5ms.
Compared with prior art, the present invention having the following technical effect that
Compared with traditional electrode testing result, nanometer platinum/graphen flexible electrode detection sensitivity is higher, and detection process does not have
There is precipitation hydrogen, it is as a result more stable, while detection range is also wider；And electrode is more flexible in structure, it is easier to miniature
Change, is suitble to the quick detection under various occasions to gallic acid.
Detailed description of the invention
Fig. 1 is the pictorial diagram of the nanometer platinum/graphen flexible electrode of the embodiment of the present invention；
Fig. 2 is the nanometer platinum/graphen flexible electrode of the embodiment of the present invention and the electric conductivity pair of graphene flexible electrode
Than figure；
Fig. 3 is that the content of Platinum Nanoparticles in the nanometer platinum/graphen flexible electrode of the embodiment of the present invention is swept with cyclic voltammetry
Retouch the relational graph of circle number；
Fig. 4 is following for the gallic acid for the various concentration that the nanometer platinum/graphen flexible electrode of the embodiment of the present invention measures
Ring volt-ampere curve；
Fig. 5 be the various concentration that the nanometer platinum/graphen flexible electrode of the embodiment of the present invention measures gallic acid with it is dense
Linear graph between degree.
Specific embodiment
In order to illustrate the embodiments of the present invention more clearly, Detailed description of the invention a specific embodiment of the invention will be compareed below.
It should be evident that drawings in the following description are only some embodiments of the invention, those of ordinary skill in the art are come
It says, without creative efforts, is also possible to obtain other drawings based on these drawings, and obtain other real
Apply mode.
The preparation method of the nanometer platinum/graphen flexible electrode of the embodiment of the present invention, includes the following steps:
1) the use of liquid-transfering gun is that 2mg/mL graphene oxide solution is placed in 50mL centrifuge tube by 5mL concentration, 15mL is added
Deionized water shakes up；Then will be added 5mL concentration be 2mg/mL ascorbic acid solution after shake up, ultrasonic 2h, after be protected from light sealing it is quiet
It sets for 24 hours；
2) pouring into above-mentioned black mixed liquor equipped with diameter is 50mm, the vacuum filtration for the aqueous filter paper that aperture is 0.22 μm
Tank filters, and obtains black gelatinous membrane；
3) dry 12h under the conditions of above-mentioned gelatinous membrane and aqueous filter paper being put into 40 DEG C of freeze drier simultaneously
The graphene oxide paper tentatively restored；
4) front of above-mentioned graphene oxide paper is clung with adhesive tape, crops filter paper around, will gently aoxidize stone
Black alkene paper and filter paper separate；Graphene oxide paper is then cut into the specification of 0.5 × 1cm, is put into 10mL centrifuge tube, is added
Hydroiodic acid is until graphene oxide paper is totally submerged；
5) above-mentioned centrifuge tube is put into shaking table, is rocked at 25 DEG C with 60rmp rate and react 6h, finally takes out graphene paper,
Using washes of absolute alcohol, until cleaning solution be it is colourless, be dried with nitrogen and be prepared into redox graphene flexible electrode；
6) take the NaCl that 100 μ L concentration are 7.5mmol/L platinum acid chloride solution and 9900 μ L concentration are 0.5~0.6mol/L molten
Liquid is configured to electrolyte；
7) above-mentioned redox graphene flexible electrode is connected to electrochemical workstation, and in above-mentioned electrolyte into
Nanometer platinum/graphen flexible electrode is made in row cyclic voltammetry scan.Cyclic voltammetric parameter is as follows: voltage scan range is -1.3
~0.8V, scanning speed 50mV/s, scanning circle number 10 enclose.Wherein, Platinum Nanoparticles and graphene in nanometer platinum/graphen flexible electrode
Mass ratio be 1:100.
Stone Platinum Nanoparticles made from the preparation method of the nanometer platinum/graphen flexible electrode of the embodiment of the present invention/ink alkene paper, such as
Shown in Fig. 1.Platinum Nanoparticles/graphene paper made from the preparation method of the nanometer platinum/graphen flexible electrode of the embodiment of the present invention with
The electric conductivity of simple graphene paper compares, as shown in Fig. 2, it is apparent that compared to simple graphene paper, nanometer
The electric conductivity of platinum/graphen paper significantly improves.
Graphene flexible electrode made from the preparation method of the nanometer platinum/graphen flexible electrode of the present embodiment has splendid
Mechanical performance, have wide-angle bending without there is the ability damaged；Carry out surface mixing Platinum Nanoparticles chemical treatment it
Afterwards, electric conductivity has obtained great promotion, has great advantages compared with traditional solid electrode；And preparation method work
Skill is simple.Wherein, graphene oxide is tentatively restored using ascorbic acid, it can be by can not be by hydrogen iodine in graphene oxide
The oxygen-containing group reduction of acid reduction, is thoroughly restored later using hydroiodic acid, so that the electric conductivity of graphene is more preferably.Oxidation
The mass ratio of graphene and ascorbic acid is the proportion such as 1:1.2,1:1.5,1:1.8,1:2；Ratio will cause lower than mass ratio 1:1
Restoring incomplete electric conductivity reduces；Ratio is higher than 1:2, and the difficulty in washes of absolute alcohol can be made to increase, can be to electrode
Accuracy when detection interferes.
In addition, the content of the Platinum Nanoparticles in the nanometer platinum/graphen flexible electrode of the embodiment of the present invention exists with graphene paper
In chloroplatinic acid & sodium chloride mixed electrolytic solution carry out cyclic voltammetry scan when circle number variation and change, as shown in figure 3, into
When row cyclic voltammetry scan early period, the circle number of scanning is more, and the content of Platinum Nanoparticles is higher；When scanning circle number reaches 12 circle,
The content of Platinum Nanoparticles reaches peak.Therefore, with the variation of cyclic voltammetry scan circle number, in nanometer platinum/graphen flexible electrode
The mass ratio of Platinum Nanoparticles and graphene can also be 1:200,1.5:200,2.5:200,3:200 etc..
The nanometer platinum/graphen flexible electrode obtained of the above embodiment of the present invention is applied in gallic acid quantitative measurment.
Specifically, the Concentration Testing of the gallic acid of the embodiment of the present invention, includes the following steps:
1, nanometer platinum/graphen flexible electrode is determined with electrode is clamping, form three electrodes with platinum electrode, saturated calomel electrode
System；
2, above-mentioned nanometer platinum/graphen flexible electrode system is connected into an electrochemical workstation, in phosphate buffer solution
In the electrolytic cell of (0.1mol/L, pH=2.5), swept in 0.2~0.7V of voltage scan range of setting using cyclic voltammetry
It retouches to stabilization；
3,10mL phosphate buffer solution (0.1mol/L, pH=2.5) is added in electrolytic cell, is surveyed using square wave voltammetry
Amount, specifically: it is measured within the scope of 0.2~0.7V using square wave voltammetry, record current response；Square wave voltammetry parameter
It is as follows: scanning voltage 0.2~0.7V of range, quiet hour 3s, amplitude 0.025V, period 40ms, pulsewidth 5ms；
4,30 μ L, 50 μ L, 70 μ L, the gallic acid solution that 100 μ L concentration are 10 μm of ol/L is added into electrolytic cell respectively,
In addition, 10 μ L, 30 μ L, 50 μ L, the gallic acid solution that 70 μ L concentration are 100 μm of ol/L is also added into electrolytic cell respectively, adopt
The response of the Stripping Voltammetry under each concentration (i.e. the scanning curve of square wave voltammetry) is recorded with the method in step 3, such as Fig. 4 institute
Show, with the increase of the concentration of gallic acid solution, peak current is improved.
5. analyzing the linear relationship between peak current and the gallic acid concentration of addition, electrode is obtained for gallic acid
Correction equation: y=0.0024x-0.073, as shown in figure 5, wherein the accuracy of correction equation is R2=0.9925.
6. it is similar with step 3, it takes the phosphate buffer solution of certain volume, prepare liquid to be placed in electrolytic cell, carries out square wave volt
Peace method scanning, and being stirred before each scanning, records the scanning curve of square wave voltammetry to obtain the peak current of prepare liquid,
And the concentration of gallic acid in prepare liquid is obtained according to correction equation.
It should be noted that the above is only that the preferred embodiment of the present invention and principle are described in detail, it is right
For those skilled in the art, the thought provided according to the present invention will change in specific embodiment, and
These changes should also be regarded as the scope of the invention.
Claims (10)
1. the preparation method of a kind of nanometer of platinum/graphen flexible electrode, which comprises the following steps:
Step 1: preparing the precursor solution of graphene oxide solution and platinum respectively；
Step 2: preparation graphene oxide paper；
Step 3: carrying out electronation to graphene oxide paper redox graphene flexible electrode is made；
Step 4: redox graphene flexible electrode is connected to an electrochemical workstation, the precursor solution of platinum is added
It in electrolyte, is scanned using cyclic voltammetry, nanometer platinum/graphen flexible electrode is made.
2. the preparation method of a kind of nanometer of platinum/graphen flexible electrode according to claim 1, which is characterized in that described
The mass ratio of Platinum Nanoparticles and graphene is (1~3) in nanometer platinum/graphen flexible electrode: 200.
3. the preparation method of a kind of nanometer of platinum/graphen flexible electrode according to claim 1, which is characterized in that described
Graphene oxide paper is prepared, is specifically included:
Graphene oxide solution is uniformly mixed with ascorbic acid solution, is protected from light sealing and standing after ultrasonic setting time；
Mixed liquor after standing is poured into the vacuum filtration tank equipped with aqueous filter paper and is filtered, is covered on aqueous filter paper thin
Film layer；
Aqueous filter paper is transferred to freeze drier to be freeze-dried, the graphene oxide paper tentatively restored is made.
4. the preparation method of a kind of nanometer of platinum/graphen flexible electrode according to claim 3, which is characterized in that described
The mass ratio of graphene oxide and ascorbic acid is 1:(1~2).
5. the preparation method of a kind of nanometer of platinum/graphen flexible electrode according to claim 3, which is characterized in that described
Graphene flexible electrode is made, specifically includes:
The front that graphene oxide paper is clung by adhesive tape is cut into target size and removes aqueous filter paper, obtains target
Graphene oxide paper；
Desirable oxidation graphene paper is placed in hydroiodic acid solution and submerges and carries out oscillation preset time, then takes out cleaning, wind
It is dry, redox graphene flexible electrode is made.
6. the preparation method of a kind of nanometer of platinum/graphen flexible electrode according to claim 1, which is characterized in that described
The sweep parameter of cyclic voltammetry includes: voltage scan range -1.3~0.8V, scanning speed 50mV/s, scanning circle number 10~15
Circle.
7. the preparation method of a kind of nanometer of platinum/graphen flexible electrode according to claim 1, which is characterized in that described
Electrolyte is NaCl solution；The precursor solution of the Platinum Nanoparticles is platinum acid chloride solution.
8. the application of nanometer platinum/graphen flexible electrode, feature made from the preparation method as described in claim any one of 1-7
It is, the Concentration Testing for gallic acid.
9. application according to claim 8, which is characterized in that the Concentration Testing of the gallic acid, comprising the following steps:
(a) nanometer platinum/graphen flexible electrode is determined with electrode is clamping, form three electrode bodies with platinum electrode, saturated calomel electrode
System；
(b) it takes the phosphate buffer solution of certain volume, gallic acid titer to be placed in electrolytic cell, carries out square wave voltammetry and sweep
It retouches, and is stirred before each scanning, record the scanning curve of square wave voltammetry；
(c) linear relationship between the various criterion concentration and peak current of gallic acid titer is compared, obtains electrode for not having
The correction equation of gallate-based；
(d) it takes the phosphate buffer solution of certain volume, prepare liquid to be placed in electrolytic cell, carries out square wave voltammetry scanning, and every
It is stirred before secondary scanning, records the scanning curve of square wave voltammetry to obtain the peak current of prepare liquid, and according to correction equation
Obtain the concentration of gallic acid in prepare liquid.
10. application according to claim 9, which is characterized in that the sweep parameter of the square wave voltammetry are as follows: scanning voltage
Range 0.2-0.7V, quiet hour 3s, amplitude 0.025V, period 40ms, pulsewidth 5ms.
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| CN113311029A (en) * | 2021-06-09 | 2021-08-27 | 宁波海通食品科技有限公司 | Impedance rapid detection method of escherichia coli in food based on nano magnetic beads |
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Application publication date: 20190503 |