CN107315039A - CNT/Jenner's nano composite material modified electrode and preparation method and application - Google Patents
CNT/Jenner's nano composite material modified electrode and preparation method and application Download PDFInfo
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Abstract
The present invention relates to electrochemical analysis detection field, and more particularly to a kind of CNT/Jenner's nano composite material modified electrode and preparation method and application.The CNT that the present invention is provided/Jenner's nano composite material modified electrode, it is prepared by the preparation method of above-mentioned CNT/Jenner's nano composite material modified electrode.The modified electrode is a kind of highly sensitive electrochemical sensor.The advantages of modified electrode has shorter response time, the wider range of linearity, relatively low test limit, good selectivity and higher stability.CNT/Jenner's nano composite material modified electrode that the present invention is provided is applied in the detection of lemon yellow, and detection is accurate easy.
Description
Technical field
The present invention relates to electrochemical analysis detection field, and more particularly to a kind of CNT/Jenner's nano composite material is repaiied
Adorn electrode and preparation method and application.
Background technology
Synthetic dyestuff, is an a kind of very important class for food additives, is commonly added in food, for example fruit juice
Beverage, soda, fructose etc. are commonly used to change its outward appearance and color.In general, the azo collection contained in these materials
, there is potential threat to the health of the mankind, so must have strict law supervision in group and fragrant link structure.Lemon yellow this
Allergy, asthma, eczema, anxiety, antimigraine can be caused or even induce the generation of cancer and other diseases by planting azo colouring agent.People
The daily acceptable intake of body is 0.75mg kg-1(FAO (Food and Agriculture Organization of the United Nation) and the World Health Organization provide 1994).
China, according to the property of dyestuff, content of tartrazine changes according to the maximum of authorized synthetic dyestuffs.Generally all from 0 to
100 milligrams, but many commercial products are not inconsistent, and dye content exceedes the content allowed.However, some (European associations of university of country
Can and some European countries) prohibited these colouring agents, such as in Finland and Norway's lemon yellow be considered as carcinogenic and prohibit
Only use.Therefore, content of the lemon yellow in food is accurately determined extremely urgent.
In recent years, shown according to substantial amounts of document report, grasped substantial amounts of technology to determine food additives lemon
Lemon is yellow, such as AAS, HPLC MS, fluorescence emission spectrometry, capillary electrophoresis.However, its
In certain methods Technical comparing it is costly and time-consuming, or need complicated pretreatment, should which has limited their further development
With.Compared with these methods, electrochemical measuring method is considered as a selection well, because it is low, simple easy to play cost
Operate, stability is good and sensitivity is high.In recent years, it has been proposed that with various Electrochemical Modification determination of electrode lemon yellows
Different technologies.In addition, also carried out deep discussion to the electrochemical reaction mechanism of lemon yellow, including diffusion coefficient is estimated
Meter and standard isomery speed Changshu.But these methods want accurate easy measure lemon yellow to be still a challenge.
The content of the invention
It is an object of the invention to provide a kind of preparation method of CNT/Jenner's nano composite material modified electrode, energy
Enough environmental protection, quickly and easily synthetic modification electrode.
The second object of the present invention is to provide a kind of CNT/Jenner's nano composite material modified electrode, with good
Chemical property.
The third object of the present invention is to provide a kind of CNT/Jenner's nano composite material modified electrode in lemon yellow
Detection in application, detection is accurate easy.
The present invention is solved its technical problem and realized using following technical scheme：
Present invention also offers a kind of preparation method of CNT/Jenner's nano composite material modified electrode.Including following
Step：
The dispersion liquid that CNT/Jenner's nano composite material is added dropwise in the surface of basal electrode after polishing, cleaning is carried out
Modification, wherein, CNT/Jenner's nano composite material is by by carbon nano-tube solution, HAuCl4Solution and strong base solution
Heating is prepared after mixing.
The present invention proposes a kind of CNT/Jenner's nano composite material modified electrode, and it is by above-mentioned CNT/gold
The preparation method of nano composite material modified electrode is prepared.The CNT/Jenner's nano composite material modified electrode includes
Basal electrode and the decorative layer being attached on the basal electrode.
Present invention also offers it is a kind of according to above-mentioned CNT/Jenner's nano composite material modified electrode in lemon yellow
Detection in application.
Present invention has the advantages that：
The preparation method of the CNT that the present invention is provided/Jenner's nano composite material modified electrode, in alkaline heating condition
Under, by gold chloride and CNT hybrid reaction, abandon traditional poisonous hydrazine 24h reduction, environmental protection.This method it is only
Special part is its simplicity and nontoxicity, and the mild condition time is short, and low in raw material price is easy to get, and is in industrial production
Controllable prepare with scale add possibility.
The CNT that the present invention is provided/Jenner's nano composite material modified electrode, it is by above-mentioned CNT/Jenner
The preparation method of nano composite material modified electrode is prepared.The modified electrode is a kind of highly sensitive electrochemical sensor.Should
Modified electrode has a shorter response time, the wider range of linearity, relatively low test limit, good selectivity and higher
The advantages of stability.
The application of the CNT that the present invention is provided/Jenner's nano composite material modified electrode, is prepared into by using above-mentioned
The CNT arrived/Jenner's nano composite material modified electrode, there is good electro-catalysis ability, detection limit (3S/N) to lemon yellow
For 0.34 μm of ol/L, the gold electrode less than individual layer MMB modifications determines TT detection limit (44 μm of ol/L).Applied in lemon
In yellow detection, detection is accurate easy.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be in embodiment
The required accompanying drawing used is briefly described.
Fig. 1 is CNT/Jenner's nano composite material modified electrode (WNTs/Au/ that the embodiment of the present invention 1 is prepared
GCE), bare electrode and Au/GCE are in the 0.1mol/L PBS cushioning liquid (pH 5.0) containing 50 μm of ol/L lemon yellows (TT)
In cyclic voltammogram；
Fig. 2 is CNT/Jenner's nano composite material modified electrode (WNTs/Au/ that the embodiment of the present invention 2 is prepared
GCE) 50 μm of ol/L TT are carried out in 0.1mol/L PBS (pH 5.0) solution to detect obtained cyclic voltammogram, speed is swept：
100mV s-1, enrichment time is from the inside to surface：0th, 30,60,90,120,180,210,240,270,300,330,360s, and
TiN/GCE (b), RGO/GCE (c), RGO-TiN/GCE (d) are in the 0.1mol/L PBSs (pH containing 50 μm of ol/L TT
7.0) cyclic voltammogram in, sweeps speed：100mV/s；
Fig. 3 is CNT/Jenner's nano composite material modified electrode (WNTs/Au/ that the embodiment of the present invention 2 is prepared
GCE Fig. 2 peak current) is corresponded to the change curve of enrichment time；
Fig. 4 is CNT/Jenner's nano composite material modified electrode (WNTs/Au/GCE) prepared by the embodiment of the present invention 3
The TT, a f of various concentrations are detected in 0.1mol/L PBS (pH 5.0) solution：1、3、5、8、10、30、50、80、100μ
Mol/L, sweeps speed：100mV s-1, enrichment time 270s；
Fig. 5 is CNT/Jenner's nano composite material modified electrode (WNTs/Au/GCE) prepared by the embodiment of the present invention 3
Corresponding to Fig. 4 TT concentration and the linear relationship chart of electric current.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person in embodiment, according to normal condition or manufacturer
It is recommended that condition carry out.Agents useful for same or the unreceipted production firm person of instrument, are the routine that can be obtained by commercially available purchase
Product.
In the description of the invention, it is necessary to which explanation, term " first ", " second " etc. are only used for distinguishing description, without
It is understood that to indicate or imply relative importance.
Below to CNT/Jenner's nano composite material modified electrode of the embodiment of the present invention and preparation method thereof with answering
With being specifically described.
A kind of preparation method of CNT provided in an embodiment of the present invention/Jenner's nano composite material modified electrode.Including
Following steps：
The dispersion liquid that CNT/Jenner's nano composite material is added dropwise in the surface of basal electrode after polishing, cleaning is carried out
Modification, CNT/Jenner's nano composite material is by by carbon nano-tube solution, HAuCl4Solution and strong base solution mixing
Heating is prepared afterwards.
S1, prepare CNT/Jenner's nano composite material.
S1.1, preparation carbon nano-tube solution.
CNT is a kind of new material for the individual layer laminated structure being made up of carbon atom, is that known world is most thin, most
Hard nano material, it has many unusual performances, and thermal conductivity factor is up to 4000W/m ﹒ K, higher than graphite and diamond,
Its electron mobility is again higher than most metals more than 10000cm2/V ﹒ s under normal temperature, and resistivity only has 10-6 Ω ﹒ cm,
It is lower than most of metal, it is the minimum material of world resistivity.
Therefore, selection carbon nano-tube material is used to prepare electrochemical sensor, can perform well in electrochemical measurement.
Accurate easy determine for being used for lemon yellow so as to the electrode modified for the composite of carbon nano-tube material provides favorably
Ensure.
In an optional embodiment of the invention, the concentration 2.5-1.8g/L of carbon nano-tube solution.Further, to upper
State obtained carbon nano-tube solution and be also an option that carry out sonic oscillation.
Sonic oscillation helps so that the degree of scatter of carbon nano-tube solution is more uniform, so as to further be conducive to
Follow-up experimental implementation.
S1.2, preparation carbon nano-tube solution, HAuCl4The mixed solution of solution.
The composite species of CNT is various, including noble metal (Pt, Au, Ag etc.), metal oxide, quantum dot
Material and polymer etc..But metallic and CNT are combined as the less of contact material.Your gold gold is used as
Category is represented, and is that one kind has the advantages that corrosion resistance is strong, stability is good, electric conductivity is strong.And combined with CNT, can be with
Greatly reduce or eliminate resistance during CNT transmission electronics.
Gold chloride is the compound of gold, soluble in water in the crystallization of yellow, easily deliquescence.It is heated to be decomposed into gold.Chlorine gold
Acid can be used in preparing nanometer grade gold.Therefore, selection gold chloride is used to prepare CNT/Jenner's nano composite material, can make
For the CNT/Jenner's nano composite material modified electrode gone out for accurately being detected in electrochemical measurement.So as to being carbon
Accurate easy determine that the electrode of the composite modification of nano-tube material is used for lemon yellow provides favourable guarantee.
Further, CNT, HAuCl are being prepared4During the mixed solution of solution, HAuCl4The concentration selection of solution
0.020-0.025mol/L.In above-mentioned volume range and concentration range, good composite wood can be formed with CNT
Material.
In an optional embodiment of the invention, specifically, 21.00 mg CNT is accurately weighed with electronic balance,
It is put into round-bottomed flask, adds 10.00ml deionized water.Into the foregoing carbon nano-tube solution prepared, add
20 μ L, 0.024mol/L HAuCl4Solution, it is this under the conditions of, good CNT/gold nano composite wood can be formed
Material.
S1.3, strong base solution regulation carbon nano-tube solution, HAuCl4The pH of the mixed solution of solution.
Under strong alkali environment, it can effectively ensure that gold chloride is reduced into nanogold, so as to form carbon with CNT
Nanotube/Jenner's nano composite material.
Specifically, carbon nano-tube solution, HAuCl4The pH value 11- of solution and the mixed mixed solution of strong base solution
14.When the pH value of mixed solution is in 11-14, good CNT formation CNT/gold nano composite wood can be formed
Material.Further, the pH value 13 of above-mentioned mixed solution., can be more efficient when the pH value of mixed solution is adjusted to 13
Ground forms good CNT formation CNT/Jenner's nano composite material.
Further, the concentration 0.4-0.6mol/L of above-mentioned strong base solution.As the concentration 0.4- of strong base solution
During 0.6mol/L, it can not only effectively ensure that whole mixed solution is combined in the basic conditions, and can be formed good
Good CNT formation CNT/Jenner's nano composite material.
Further, the concentration selection 0.5mol/L of above-mentioned strong base solution.As the concentration 0.5mol/L of strong base solution
When, it can further ensure that whole mixed solution is combined in the basic conditions, form good CNT formation carbon
Nanotube/Jenner's nano composite material, does not result in the excessive waste or very few of raw material.
Further, above-mentioned strong base solution includes at least one of sodium hydroxide solution or potassium hydroxide solution.
Specifically, above-mentioned strong base solution can select single sodium hydroxide solution, single potassium hydroxide solution or
The strong base solution of person's sodium hydroxide solution and potassium hydroxide solution compounding.
S1.3, heating carbon nano-tube solution, HAuCl4Solution and the mixed mixed solution of strong base solution.
By heating carbon nano-tube solution, HAuCl4Solution and the mixed mixed solution of strong base solution ensure that
Form good CNT/Jenner's nano composite material.
Specifically, in an optional embodiment of the invention, heating carbon nano-tube solution, HAuCl4Solution and highly basic
The mixed mixed solution of solution is the oil bath heating in 98-100 DEG C of 2-4 hour of progress of temperature.
Further, the dispersion liquid of CNT/Jenner's nano composite material is to be combined the CNT/gold nano
Material carries out ultrasonic vibration after being mixed with water and is made.
Specifically, after oil bath terminates, flask is taken out, cools down at normal temperatures, mixed carbon nano-tube solution is surpassed
Sound oscillation, is made the dispersion liquid of CNT/Jenner's nano composite material.
Further, in an optional embodiment of the invention, by CNT obtained above/gold nano composite wood
The dispersion liquid of material pours into lucifuge in 10mL plastic tubes and is put into refrigerator with standby, if product is excessively dilute, can carry out centrifugal concentrating.
S2, polishing, cleaning after basal electrode surface be added dropwise CNT/Jenner's nano composite material dispersion liquid
Modified.
It should be understood that above-mentioned basal electrode can select appropriate basal electrode according to the actual needs.
Above-mentioned specific polishing, the specific method of clean substrate electrode, this area can be selected according to the actual needs
Conventional polishing, the specific method of clean substrate electrode.
The specific method of the dispersion liquid of above-mentioned dropwise addition CNT/Jenner's nano composite material can also be according to reality
Need to select dropwise addition method commonly used in the art.
In an optional embodiment of the invention, above-mentioned basal electrode selection glass-carbon electrode (GCE).
Specifically, first, the glass-carbon electrode (GCE) of 3mm diameters is polished on chamois leather, then 0.05 μm of ol/L's
Obtained by alumina slurry mirror finish, successively with ultrasound 2min in water and ethanol, and dried up with nitrogen.Finally, by 5 μ L
0.1mg mL-1 CNT/Jenner's nano composite material dispersant liquid drop is applied to the electrode surface polished, then at room temperature
Dry, that is, obtain CNT/gold nano nano composite material modified electrode (WNTs/Au/GCE).
Some embodiments of the present invention also provide a kind of CNT/Jenner's nano composite material modified electrode.
The modified electrode is prepared into using the preparation method of above-mentioned CNT/Jenner's nano composite material modified electrode
Arrive, CNT/Jenner's nano composite material modified electrode includes basal electrode and the decorative layer being attached on basal electrode.
The modified electrode has a shorter response time, the wider range of linearity, relatively low test limit, good selectivity and higher
Stability the advantages of.
Some embodiments of the present invention also provide a kind of CNT/Jenner's nano composite material modified electrode in lemon
Application in yellow detection.Applied in the detection of lemon yellow, detection is accurate easy.There is good electricity to urge to lemon yellow
Change ability, detection limit (3S/N) is 0.34 μm of ol/L, less than detection limit (44 μ that the gold electrode that individual layer MMB is modified determines TT
mol/L)。
The feature and performance to the present invention are described in further detail with reference to embodiments：
Embodiment 1
A kind of CNT/Jenner's nano composite material modified electrode that the present embodiment is provided, is made by following steps：
21.00mg CNT is accurately weighed with electronic balance, is put into round-bottomed flask, adds 10.00ml's
Deionized water, carries out sonic oscillation.The mol/L of 20 μ L 0.024 HAuCl4 solution is added, with 0.5mol/L NaOH solution
Adjust its pH to 13；The solution prepared is carried out to the oil bath of 3 hours, temperature is 100 DEG C；After oil bath terminates, flask is taken out,
Cool down at normal temperatures, carry out sonic oscillation, you can make CNT/Jenner's nano composite material standby.
The glass-carbon electrode (GCE) of 3mm diameters is polished on chamois leather, then in 0.05 μm of ol/L alumina slurry minute surface
Polishing gained, successively with ultrasound 2min in water and ethanol, and is dried up with nitrogen.Finally, by 5 μ L 0.1mg mL-1 carbon nanometer
Pipe/Jenner's nano composite material dispersant liquid drop is applied to the electrode surface polished, and then dries at room temperature, that is, obtains carbon nanometer
Pipe/Jenner's nano composite material modified electrode (WNTs/Au/GCE).
Embodiment 2
A kind of CNT/Jenner's nano composite material modified electrode that the present embodiment is provided, is made by following steps：
18.00mg CNT is accurately weighed with electronic balance, is put into round-bottomed flask, adds 8.00ml's
Deionized water, carries out sonic oscillation.Add 18 μ L 0.020mol/L HAuCl4Solution, with 0.4mol/L KOH solution
Adjust its pH to 11；The solution prepared is carried out to the oil bath of 2 hours, temperature is 98 DEG C；After oil bath terminates, flask is taken out,
Cool down at normal temperatures, carry out sonic oscillation, you can make CNT/Jenner's nano composite material standby.
The glass-carbon electrode (GCE) of 3mm diameters is polished on chamois leather, then in 0.05 μm of ol/L alumina slurry mirror
Obtained by mirror polish, successively with ultrasound 2min in water and ethanol, and dried up with nitrogen.Finally, by 5 μ L 0.1mg mL-1Carbon receive
Mitron/Jenner's nano composite material dispersant liquid drop is applied to the electrode surface polished, and then dries at room temperature, that is, obtains carbon nanometer
Pipe/Jenner's nano composite material modified electrode (WNTs/Au/GCE).
Embodiment 3
A kind of CNT/Jenner's nano composite material modified electrode that the present embodiment is provided, is made by following steps：
20.00mg CNT is accurately weighed with electronic balance, is put into round-bottomed flask, adds 12.00ml's
Deionized water, carries out sonic oscillation.Add the mol/L of 22 μ L 0.020 HAuCl4Solution, with 0.4mol/L NaOH and
KOH solution adjusts its pH to 11；The solution prepared is carried out to the oil bath of 4 hours, temperature is 99 DEG C；After oil bath terminates, take
Go out flask, cool down at normal temperatures, carry out sonic oscillation, you can make CNT/Jenner's nano composite material standby.
The glass-carbon electrode (GCE) of 3mm diameters is polished on chamois leather, then in 0.05 μm of ol/L alumina slurry mirror
Obtained by mirror polish, successively with ultrasound 2min in water and ethanol, and dried up with nitrogen.Finally, by 5 μ L 0.1mg mL-1Carbon receive
Mitron/Jenner's nano composite material dispersant liquid drop is applied to the electrode surface polished, and then dries at room temperature, that is, obtains carbon nanometer
Pipe/Jenner's nano composite material modified electrode (WNTs/Au/GCE).
Embodiment 4
A kind of CNT/Jenner's nano composite material modified electrode that the present embodiment is provided, is made by following steps：
22.00mg CNT is accurately weighed with electronic balance, is put into round-bottomed flask, adds 11.00ml's
Deionized water, carries out sonic oscillation.Add the mol/L of 22 μ L 0.020 HAuCl4Solution, with 0.4mol/L NaOH solution
Adjust its pH to 11；The solution prepared is carried out to the oil bath of 3 hours, temperature is 99 DEG C；After oil bath terminates, flask is taken out,
Cool down at normal temperatures, carry out sonic oscillation, you can make CNT/Jenner's nano composite material standby.
The glass-carbon electrode (GCE) of 3mm diameters is polished on chamois leather, then in 0.05 μm of ol/L alumina slurry mirror
Obtained by mirror polish, successively with ultrasound 2min in water and ethanol, and dried up with nitrogen.Finally, by 5 μ L 0.1mg mL-1Carbon receive
Mitron/Jenner's nano composite material dispersant liquid drop is applied to the electrode surface polished, and then dries at room temperature, that is, obtains carbon nanometer
Pipe/Jenner's nano composite material modified electrode (WNTs/Au/GCE).
Experimental example one
CNT/Jenner's nano composite material is prepared using cyclic voltammetric technical research embodiments of the invention 1 to repair
Adorn electrode (WNTs/Au/GCE) and the chemical property of other contrast materials.
Specifically, in the 0.1mol/L PBS cushioning liquid (pH 5.0) containing 50 μm of ol/L lemon yellows (TT), investigate naked
The chemical property of electrode, Au/GCE, WNTs/Au/GCE.Specifically, refer to Fig. 1, wherein, curve a represent for naked electricity
The cyclic voltammogram of pole, curve b represents Au/GCE cyclic voltammogram, (curve a and curve b are essentially coincided), and curve c is represented
WNTs/Au/GCE cyclic voltammogram.
From the graph, it is apparent that the bare electrode that curve a is represented, peak current minimum is almost nil, curve b is represented
Au/GCE peak current does not almost have yet.The peak current for the SWNTs-Au/GCE that curve c is represented is maximum, and this shows successfully to make
For SWNTs/Au nano materials, and the nano-complex has good electrocatalysis characteristic to lemon yellow.
Experimental example two
Embodiments of the invention 2 are prepared with CNT/Jenner's nano composite material modified electrode (WNTs/Au/
GCE the influence of enrichment time) is investigated.Fig. 2 and Fig. 3 are refer to, it is molten in 50 μm of ol/L TT 0.1M PBS (pH 5.0) bufferings
In liquid, (A) be 5 μ L SWNTs-Au/GCE under different enrichment times, 50 μm of ol/L TT 0.1M PBS (pH 5.0) bufferings
Cyclic voltammogram in solution, (B) be change curve of the peak current with enrichment time, as can be seen from Figure modified electrode
Electrochemical behavior is influenceed by enrichment time, and when enrichment time is 270s, peak current is maximum, when enrichment time exceedes
During 270s, peak current tends to be steady, and illustrates that the TT of electrode surface absorption reaches saturation.Therefore, the optimal richness selected in experiment
Integrate the time as 270s.
Experimental example three
Embodiments of the invention 3 are prepared with CNT/Jenner's nano composite material modified electrode (WNTs/Au/
GCE the range of linearity and detection limit) are investigated.
Fig. 4 is refer to, as can be seen from the figure peak current increases with the increase of TT concentration.Fig. 5 is refer to, is peak
The linear relationship chart of electric current and concentration, as can be seen from the figure in 5-100 μm of ol/L, lemon yellow concentration and peak current are presented
Outlet sexual intercourse, equation of linear regression is：Ip/ μ A=0.825+0.714C TT, coefficient correlation is R=0.9941, detection limit
(3S/N) is 0.34 μm of ol/L, and showing the modified electrode has preferable catalytic activity to lemon yellow, its range of linearity also compared with
Extensively.
Experimental example four
Embodiments of the invention 4 are prepared with CNT/Jenner's nano composite material modified electrode (WNTs/Au/
GCE interference experiment) is carried out.
Specifically, fixed TT concentration is 50 μm of ol/L, it is allowed to which evaluated error is controlled within 5%, is surveyed in optimal experiment
Under fixed condition, it is the influence that 50 μm of ol/L TT are determined to concentration to have investigated some materials that may be present.
Test result indicates that：Citric acid, glucose, Vc, amaranth are dry to the measure nothing that concentration is 50 μm of ol/L TT
Disturb.
Experimental example five
Embodiments of the invention 1 are prepared with CNT/Jenner's nano composite material modified electrode (WNTs/Au/
GCE repeatability and stability) are investigated.
CNT/Jenner's nano composite material modified electrode is placed on the 0.1 mol/L PBS cushioning liquid that pH is 5.0
In, under optimum experimental condition, with same 50 μm of branch electrode pair ol/L TT parallel determinations three times, obtained relative standard deviation
For 1.80%.The modified electrode is soaked in pH 5.0 0.1M PBS cushioning liquid again, is placed in refrigerator.After 20 days,
It is 50 μm of ol/L TT METHOD FOR CONTINUOUS DETERMINATIONs 5 times to concentration, oxidation peak current has declined than initial value but change little, relative standard
Deviation is 6.02%, illustrates that the modified electrode has good stability.
Experimental example six
Embodiments of the invention 1 are prepared with CNT/Jenner's nano composite material modified electrode (WNTs/Au/
GCE sample analysis and recovery experiment) are carried out.
TT measure in the true fruit of table 1 grain (pigeon)
In order to evaluate the actual application value of this method, the TT in true fruit grain is measured simultaneously using the modified electrode
Carry out recovery testu.Recovery experiment result table 1, the TT measured content is 9.0mmol/L, with buy true fruit grain in
The mmol/L of concentration 7.7 that lemon yellow is indicated is approached.Determine satisfaction, detection and the control of quality available for impurity of the drug.
In summary, CNT/Jenner's nano composite material modified electrode that the present invention is provided, it is received by above-mentioned carbon
The preparation method of mitron/Jenner's nano composite material modified electrode is prepared.The modified electrode is a kind of highly sensitive electrochemistry
Sensor.The modified electrode has shorter response time, the wider range of linearity, relatively low test limit, good selectivity
The advantages of higher stability.CNT/Jenner's nano composite material modified electrode that the present invention is provided is applied in lemon
In the yellow detection of lemon, detection is accurate easy.Detection limit (3S/N) is 0.34 μm of ol/L, is surveyed less than the gold electrode that individual layer MMB is modified
Determine TT detection limit (44 μm of ol/L).
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected reality of the present invention
Apply example.Based on the embodiment in the present invention, those of ordinary skill in the art are obtained under the premise of creative work is not made
Every other embodiment, belong to the scope of protection of the invention.
Claims (10)
1. the preparation method of a kind of CNT/Jenner's nano composite material modified electrode, it is characterised in that comprise the following steps：
The dispersion liquid that CNT/Jenner's nano composite material is added dropwise in the surface of basal electrode after polishing, cleaning is modified,
The CNT/Jenner's nano composite material is by by carbon nano-tube solution, HAuCl4After solution and strong base solution mixing
Heating is prepared.
2. the preparation method of CNT according to claim 1/Jenner's nano composite material modified electrode, its feature exists
In the concentration 2.5-1.8g/L of the carbon nano-tube solution.
3. the preparation method of CNT according to claim 2/Jenner's nano composite material modified electrode, its feature exists
In the HAuCl4The concentration 0.020-0.025mol/L of solution.
4. the preparation method of CNT according to claim 3/Jenner's nano composite material modified electrode, its feature exists
In the strong base solution includes at least one of sodium hydroxide solution or potassium hydroxide solution.
5. the preparation method of CNT according to claim 4/Jenner's nano composite material modified electrode, its feature exists
In the concentration 0.4-0.6mol/L of the strong base solution.
6. the preparation method of CNT according to claim 1/Jenner's nano composite material modified electrode, its feature exists
In the carbon nano-tube solution, the HAuCl4The pH value of solution and the mixed mixed solution of the strong base solution is 11-
14。
7. the preparation method of CNT according to claim 6/Jenner's nano composite material modified electrode, its feature exists
In the heating carbon nano-tube solution, the HAuCl4Solution and the mixed mixed solution of the strong base solution are
In the oil bath heating of 98-100 DEG C of 2-4 hour of progress of temperature.
8. the preparation method of CNT according to claim 1/Jenner's nano composite material modified electrode, its feature exists
In the dispersion liquid of the CNT/Jenner's nano composite material is to mix the CNT/Jenner's nano composite material with water
Ultrasonic vibration is carried out afterwards to be made.
9. a kind of CNT/Jenner's nano composite material modified electrode, it is characterised in that it is any one by such as claim 1-8
The preparation method of CNT/Jenner's nano composite material modified electrode described in is prepared, the CNT/gold nano
Composite modified electrode includes basal electrode and the decorative layer being attached on the basal electrode.
10. a kind of CNT according to claim 9/Jenner's nano composite material modified electrode is in the detection of lemon yellow
Application.
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| CN201710509104.9A CN107315039A (en) | 2017-06-28 | 2017-06-28 | CNT/Jenner's nano composite material modified electrode and preparation method and application |
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| CN109324097A (en) * | 2018-10-11 | 2019-02-12 | 大连大学 | A kind of electrode and its application for melamine measurement |
| CN110744067A (en) * | 2019-09-29 | 2020-02-04 | 济南大学 | Method for preparing carbon nano tube loaded gold nano by ultrasonic spraying |
| CN112881486A (en) * | 2021-01-15 | 2021-06-01 | 柳州市质量检验检测研究中心 | Method for detecting lemon yellow content of bean product in snail rice noodles by using mesoporous carbon modified electrode |
| CN113008962A (en) * | 2021-02-23 | 2021-06-22 | 南通大学 | PDMS-based flexible electrode and preparation method thereof |
| CN115055672A (en) * | 2022-06-15 | 2022-09-16 | 安徽理工大学 | Method for preparing coral-shaped gold nano/carbon nano tube composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109324097A (en) * | 2018-10-11 | 2019-02-12 | 大连大学 | A kind of electrode and its application for melamine measurement |
| CN110744067A (en) * | 2019-09-29 | 2020-02-04 | 济南大学 | Method for preparing carbon nano tube loaded gold nano by ultrasonic spraying |
| CN110744067B (en) * | 2019-09-29 | 2022-06-07 | 济南大学 | Method for preparing carbon nano tube loaded gold nano by ultrasonic spraying |
| CN112881486A (en) * | 2021-01-15 | 2021-06-01 | 柳州市质量检验检测研究中心 | Method for detecting lemon yellow content of bean product in snail rice noodles by using mesoporous carbon modified electrode |
| CN113008962A (en) * | 2021-02-23 | 2021-06-22 | 南通大学 | PDMS-based flexible electrode and preparation method thereof |
| CN115055672A (en) * | 2022-06-15 | 2022-09-16 | 安徽理工大学 | Method for preparing coral-shaped gold nano/carbon nano tube composite material |
| CN115055672B (en) * | 2022-06-15 | 2023-10-24 | 安徽理工大学 | Method for preparing coral-shaped gold nano/carbon nano tube composite material |
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