CN110133092A - Hydrogen peroxide electrochemical sensor and method based on the catalysis of ultralight silver nanowires aeroge - Google Patents
Hydrogen peroxide electrochemical sensor and method based on the catalysis of ultralight silver nanowires aeroge Download PDFInfo
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- CN110133092A CN110133092A CN201910359032.3A CN201910359032A CN110133092A CN 110133092 A CN110133092 A CN 110133092A CN 201910359032 A CN201910359032 A CN 201910359032A CN 110133092 A CN110133092 A CN 110133092A
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Abstract
A kind of hydrogen peroxide electrochemical sensor based on the catalysis of ultralight silver nanowires aeroge of the present invention, including electrode and electrolyte；The electrode includes working electrode, to electrode and reference electrode；The working electrode is ultralight silver nanowires aeroge；The electrolyte is the mixed solution of NaOH and NaCl, is provided with magnetic stirring apparatus in the electrolyte.Pass through current-vs-time (I-t) module of electrochemical workstation, obtain the curve that restore current value of the hydrogen peroxide on silver nanowires aeroge changes with concentration of hydrogen peroxide, determine the functional relation between current value and concentration of hydrogen peroxide, hydrogenperoxide steam generator concentration to be measured can be calculated according to the stabling current value of unknown concentration hydrogenperoxide steam generator.The device and method simple process, it is easy to operate, have many advantages, such as low cost, short route, efficiently it is convenient, be easy to heavy industrialization application.
Description
Technical field
The invention belongs to sensor fields, and in particular to a kind of hydrogen peroxide based on the catalysis of ultralight silver nanowires aeroge
Electrochemical sensor and method.
Background technique
On October 27th, 2017, international cancer research institution, the World Health Organization announce carcinogenic substance inventory in hydrogen peroxide
(H2O2) belong to third class carcinogenic substance, but hydrogen peroxide has Strong oxdiative, disinfecting properties, has in our daily lifes and production
Very extensive application.In daily life, hydrogen peroxide is prevalent in the lives such as shampoo, toothpaste, bleaching textiles use
In product, also it is widely used in vessel disinfection, food sterilization and wastewater treatment, material and eliminates the unusual smell；Meanwhile hydrogen peroxide is
The intermediate synthetic agent of many raw materials technologies is essential intermediate reaction in biology, drug, clinic and environmental analysis
Object；In health monitoring, the oxidizing ferment in human body cell mitochondria is at every moment all generating hydrogen peroxide, while hydrogen peroxide
Molecule, which can penetrate various intercellular membranes easily and act on cell, to be integrally metabolized, and then influences human health.Intracellular peroxidation
Hydrogen should maintain fixed concentration, and excessive hydrogen peroxide can cause the biology such as cell ageing, nerve degeneration and cancer irreversible
Damage.It can be seen that either environmental monitoring or human body cell health monitoring, hydrogen peroxide realizes low concentration on-line checking
It is extremely important.
Existing hydrogen peroxide detection is broadly divided into six classes: titration, spectrophotometry, fluorescence according to testing principle difference
Method, chemoluminescence method, electrochemical process and chromatography.Wherein electrochemical detection method is since its is easy to operate, low cost, not vulnerable to
Impurity interfere the advantages that and received significant attention in chemical detection.The basic principle of Electrochemical Detection is to utilize catalyst
Hydrogen peroxide generates catalytic current, establishes the linear functional relation formula between electric current and concentration of hydrogen peroxide, is closed according to this function
It is formula, the concentration of hydrogenperoxide steam generator to be measured is determined by the electric current of hydrogenperoxide steam generator to be measured.Such method have it is easy to operate,
The features such as detecting quick, low consumption, the high detection limit and high sensitivity, there is more traditional method high market to apply valence
Value.The key of Electrochemical Detection hydrogen peroxide technology is to improve hydrogen peroxide catalyzed dose of specific surface area, makes hydrogen peroxide can
Faster, to be more effectively catalyzed, to improve catalytic current, enhance the sensitivity and detectable limit of Electrochemical Detection.
Based on this, applicant team is proposed using the ultralight silver nanowires aeroge with superhigh specific surface area, as mistake
Hydrogen oxide catalysis electrode, produces hydrogen peroxide electrochemical sensor.
Summary of the invention
Technical problems to be solved:
In order to avoid the shortcomings of the prior art, a kind of peroxide based on the catalysis of ultralight silver nanowires aeroge of the present invention
Change hydrogen electrochemical sensor and passes through electrochemical workstation using ultralight silver nanowires aeroge as the catalysis electrode of hydrogen peroxide
Current-vs-time (I-t) module, obtain restore current value of the hydrogen peroxide on silver nanowires aeroge with concentration of hydrogen peroxide
The curve of variation determines the functional relation between current value and concentration of hydrogen peroxide, can be molten according to unknown concentration hydrogen peroxide
The stabling current value of liquid calculates hydrogenperoxide steam generator concentration to be measured.The device and method simple process, easy to operate, tool
Have the advantages that low cost, short route, efficiently it is convenient, be easy to heavy industrialization application.
The technical scheme is that a kind of hydrogen peroxide electrochemical sensing based on the catalysis of ultralight silver nanowires aeroge
Device, including electrode and electrolyte；It is characterized by: the electrode includes working electrode, to electrode and reference electrode；The work
Electrode is ultralight silver nanowires aeroge；The electrolyte is the mixed solution of NaOH and NaCl, NaOH concentration >=0.1M, NaCl
Concentration >=5g/L；Magnetic stirring apparatus is provided in the electrolyte.
A further technical solution of the present invention is: the preparation method specific steps of the ultralight silver nanowires aeroge are such as
Under:
Step 1: utilizing polyol process synthesis of silver nano-wire solution, and by precipitating, centrifugation purification solution, removal is wherein
Silver nano-grain；
Step 2: it after mixing evenly using turbula shaker by the silver nanowires solution of purification, is immediately placed on cold in liquid nitrogen
But it crystallizes, after crystallization completely, is placed in freeze drier and handles 24~48 hours；
Step 3: complete silver nanowires solution will be crystallized after freeze drier taking-up, heat is carried out in atmosphere of hydrogen
Processing 1~2.5 hour, heat treatment temperature are 200~400 DEG C, obtain ultralight silver nanowires aeroge.
A further technical solution of the present invention is: described is platinum guaze to electrode, reference electrode is Ag/AgCl saturated solution.
Hydrogen peroxide is detected by the above-mentioned hydrogen peroxide electrochemical sensor based on the catalysis of ultralight silver nanowires aeroge
The method of the concentration of solution, comprising the following steps:
Step 1: three-electrode electro Chemical detection architecture is established: using the ultralight silver nanowires aeroge as work electricity
Pole, using platinum guaze as to electrode, using Ag/AgCl saturated solution as reference electrode, connection electrode and electrochemical workstation are described
Electrochemical workstation is for recording data；
Step 2: NaOH solution and NaCl solution being mixed and are used as electrolyte, NaOH concentration >=0.1M, and NaCl concentration >=
5g/L；Magnetic stirring apparatus, revolving speed >=200rpm/min of magnetic stirring apparatus are added in the electrolyte；
Step 3: interval same time instills the isometric and identical peroxide of concentration with liquid-transfering gun into the electrolyte
Change hydrogen solution；The concentration of hydrogen peroxide after electric current stationary value and corresponding dilution after each instillation hydrogenperoxide steam generator of fitting
Linear relationship；On the basis of electric current stationary value and the linear relationship of concentration of hydrogen peroxide, body is detected by three-electrode electro Chemical
System obtains the I-t electric current stationary value of hydrogenperoxide steam generator to be measured, substitutes into the linear relationship expression formula of fitting, finally calculates mistake to be measured
The concentration of hydrogen peroxide solution.
Beneficial effect
The beneficial effects of the present invention are: in hydrogen peroxide electrochemical sensor proposed by the invention, ultralight silver nanoparticle
Line aeroge can greatly increase the specific surface area of catalyzing hydrogen peroxide, so that the current value of hydrogen peroxide I-t curve is improved,
The corresponding sensitivity and detectable limit that hydrogen peroxide detector can be improved.
Equipment of the present invention only has an electrochemical workstation and magnetic stirring apparatus, device are simple, it is only necessary to adopt
It is easy to operate with the I-t plate of electrochemical workstation, while result has very high repeatability.
Electrolyte used in the present invention contains NaOH and NaCl, NaOH concentration >=0.1M, NaCl concentration >=5g/L, alkali
Property environment can increase catalytic current of the hydrogen peroxide on silver nanowires silica aerogel electrode, at the same NaCl ion can be enhanced it is molten
The electric conductivity of liquid.
Detailed description of the invention
Fig. 1 is the preparation method flow chart of the ultralight silver nanowires aeroge of the present invention；
Fig. 2 is the microscopic appearance figure of the ultralight silver nanowires aeroge of the present invention；
Fig. 3 is the ultralight silver nanowires aeroge typical cyclic voltammetric response curve under hydrogenperoxide steam generator of the present invention；
Between the current-responsive peak of curve and concentration of hydrogen peroxide of the ultralight silver nanowires aeroge of Fig. 4 (a) present invention
I-t curve；Its linear fit relationship of Fig. 4 (b)；
Fig. 5 is Hydrogen Peroxide Disinfectant residue detection example.
Specific embodiment
The embodiments described below with reference to the accompanying drawings are exemplary, it is intended to be used to explain the present invention, and cannot understand
For limitation of the present invention.
It is an object of the invention to propose a kind of hydrogen peroxide electrochemical detector based on ultralight silver nanowires aeroge.
The preparation of silver nanowires solution: preparing silver nanowires aqueous solution using improved polyol process first, specifically: will
0.05mM NaCl, 0.017mM CuCl are added in 100mL ethylene glycol2, 0.19M polyvinylpyrrolidone (PVP), 0.0014mM
AgNO3, 1 hour of 185 DEG C of oil bath heatings prepares 30mL when heating dissolved with the ethylene glycol solution of 0.12M silver nitrate, and dissolution is equal
It is even, after to be heated, the ethylene glycol solution for the silver nitrate newly prepared is added dropwise to mixing with the rate of 0.3 mL/min
In liquid, and strong stirring；Again by mixed liquor oil bath heating 20 minutes after being added dropwise completely, takes out be cooled to room temperature later.
Silver nanowires purified solution: silver nanowires solution after cooling is diluted with water to 500mL, is stood for 24 hours, with injection
Device gentle aspiration supernatant repeats aforesaid operations and acquired solution is mixed into third with the ratio of 1:4 after second removes supernatant
Ketone solution is placed in centrifuge and carries out separating-purifying with the revolving speed of 2000r/min, supernatant is gently removed after centrifugation, weight
Multiple centrifugally operated 3~4 times, the silver nanowires solution of purification can be obtained.
The preparation of silver nanowires aeroge: the silver nanowires solution after gained is purified, which is placed on vortex oscillation machine, to be vibrated, and is made
Silver nanowires is evenly distributed in the solution, after oscillation is completed, is immediately placed on iron block cooling in liquid nitrogen in advance, solution
It crystallizes, after crystallization completely, is immediately placed in freeze drier from bottom to top, be lyophilized 36 hours to get ultralight silver nanowires is arrived
Aeroge, the connection between silver nanowires is mainly by Van der Waals force at this time.Gained silver nanowires aeroge is placed in atmosphere of hydrogen
In furnace, 250 DEG C of 1 hours of heat treatment remove the PVP in silver nanowires, and the welding of silver nanowires intersection may be implemented, most
Ultralight, the silver nanowires aeroge of high-specific surface area and high electron conductivity can be obtained eventually.
Electro-chemical test is done using ultralight silver nanowires aeroge: being established traditional electrochemistry three-electrode system, is received with silver
As working electrode, platinum guaze is used as to electrode rice noodles aeroge, and for Ag/AgCl as reference electrode, electrolyte is 50mL NaOH
The mixed solution of (1M) and NaCl (20g/L) are often separated by 50s with micropipette rifle, the 0.1M H of 50 μ L are added2O2Solution, mistake
Hydrogen peroxide solution can be diluted and be uniformly dispersed in the electrolytic solution rapidly, and the I-t curve of three-electrode system is obtained, such as Fig. 4 institute
Show；The of short duration time after hydrogenperoxide steam generator is added every time, step can all occur in the obtained I-t current value of electrochemical workstation
Formula decline, as shown in Figure 4 and Figure 5, the hydrogen peroxide after electric current stationary value and corresponding dilution after being fitted decline every time are dense
The linear relationship of degree can be fitted to obtain the relational expression of electric current and concentration of hydrogen peroxide to be I (μ A)=- 37.6m according to Fig. 4
(mM) -1.27, so as to which according to the I-t curve stabling current value of hydrogenperoxide steam generator to be measured, substitution above-mentioned relation formula is obtained
The concentration of hydrogenperoxide steam generator to be measured.
In this example, silver nanowires aeroge is 2.1 μM (signal-to-noise ratio=3) to the detectable limit of hydrogen peroxide, detection
Sensitivity is 4.178 μ A/ (μM mm).
Detection example: taking common Hydrogen Peroxide Disinfection Solution in family, dilutes 2500 times, the I-t of the test gained solution is bent
Line such as Fig. 5, can be obtained stabling current in 1 minute, stabling current value be substituted into relational expression, the hydrogen peroxide for obtaining the solution is dense
Degree is 0.3mM.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (4)
1. a kind of hydrogen peroxide electrochemical sensor based on the catalysis of ultralight silver nanowires aeroge, including electrode and electrolyte；
It is characterized by: the electrode includes working electrode, to electrode and reference electrode；The working electrode is ultralight silver nanowires gas
Gel；The electrolyte is the mixed solution of NaOH and NaCl, NaOH concentration >=0.1M, NaCl concentration >=5g/L；The electrolysis
Magnetic stirring apparatus is provided in liquid.
2. the hydrogen peroxide electrochemical sensor according to claim 1 based on the catalysis of ultralight silver nanowires aeroge, special
Sign is: steps are as follows for the preparation method of the ultralight silver nanowires aeroge:
Step 1: utilizing polyol process synthesis of silver nano-wire solution, and by precipitating, centrifugation purification solution, removes silver therein
Nano particle；
Step 2: after mixing evenly using turbula shaker by the silver nanowires solution of purification, cooling knot is immediately placed in liquid nitrogen
Crystalline substance after crystallization completely, is placed in freeze drier and handles 24~48 hours；
Step 3: complete silver nanowires solution will be crystallized after freeze drier taking-up, heat treatment 1 is carried out in atmosphere of hydrogen
~2.5 hours, heat treatment temperature was 200~400 DEG C, obtained ultralight silver nanowires aeroge.
3. the hydrogen peroxide electrochemical sensor according to claim 1 based on the catalysis of ultralight silver nanowires aeroge, special
Sign is: described is platinum guaze to electrode, and reference electrode is Ag/AgCl saturated solution.
4. being detected using the hydrogen peroxide electrochemical sensor based on the catalysis of ultralight silver nanowires aeroge described in claim 1
The method of the concentration of hydrogen peroxide solution, feature is specific step is as follows:
Step 1: three-electrode electro Chemical detection architecture is established: using the ultralight silver nanowires aeroge as working electrode, with
Platinum guaze is used as to electrode, using Ag/AgCl saturated solution as reference electrode, connection electrode and electrochemical workstation, and the electrification
Work station is learned for recording data；
Step 2: NaOH solution and NaCl solution are mixed and are used as electrolyte, NaOH concentration >=0.1M, NaCl concentration >=5g/L；
Magnetic stirring apparatus, revolving speed >=200rpm/min of magnetic stirring apparatus are added in the electrolyte；
Step 3: interval same time instills the isometric and identical hydrogen peroxide of concentration with liquid-transfering gun into the electrolyte
Solution；The line of the concentration of hydrogen peroxide after electric current stationary value and corresponding dilution after each instillation hydrogenperoxide steam generator of fitting
Sexual intercourse；On the basis of electric current stationary value and the linear relationship of concentration of hydrogen peroxide, obtained by three-electrode electro Chemical detection architecture
To the I-t electric current stationary value of hydrogenperoxide steam generator to be measured, the linear relationship expression formula of fitting is substituted into, peroxidating to be measured is finally calculated
The concentration of hydrogen solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111380917A (en) * | 2020-03-23 | 2020-07-07 | 艾感科技(广东)有限公司 | Air quality monitoring sensor and monitoring system based on nanofiber membrane |
| CN114951679A (en) * | 2022-05-05 | 2022-08-30 | 西安建筑科技大学 | Conductive nano silver wire ink with good conductivity and preparation method and application thereof |
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| KR20190015644A (en) * | 2017-07-13 | 2019-02-14 | 한국과학기술연구원 | Peroxide detecting sensor, peroxide detecting device comprising the same, and method for manufacturing the same |
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| KR20190015644A (en) * | 2017-07-13 | 2019-02-14 | 한국과학기술연구원 | Peroxide detecting sensor, peroxide detecting device comprising the same, and method for manufacturing the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111380917A (en) * | 2020-03-23 | 2020-07-07 | 艾感科技(广东)有限公司 | Air quality monitoring sensor and monitoring system based on nanofiber membrane |
| CN114951679A (en) * | 2022-05-05 | 2022-08-30 | 西安建筑科技大学 | Conductive nano silver wire ink with good conductivity and preparation method and application thereof |
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Effective date of registration: 20210118 Address after: 710072 No. 127 Youyi West Road, Shaanxi, Xi'an Applicant after: Northwestern Polytechnical University Applicant after: Shenzhen Research Institute of Xi'an University of Technology Address before: 710072 No. 127 Youyi West Road, Shaanxi, Xi'an Applicant before: Northwestern Polytechnical University |
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Application publication date: 20190816 |