CN105842318A - Preparation method and application of graphene/polypyrrole electrochemical sensor for trace-amount lead ion detection - Google Patents
Preparation method and application of graphene/polypyrrole electrochemical sensor for trace-amount lead ion detection Download PDFInfo
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Abstract
A preparation method and an application of a graphene/polypyrrole electrochemical sensor for trace-amount lead ion detection belong to the field of environment analysis. In the invention, high selectivity is achieved through complex effect of nitrogen atoms on amino groups in the polypyrrole and lead ions and the effect of signal amplification is achieved through high-electric-conductivity of graphene nano sheets, thereby achieving the trace-amount lead ion detection. The graphene also increases space combination sites and interface electron transmission rate of the composite material, thereby improving detection effect of the sensor. Through the synergistic effect of the graphene nano sheets and polyaniline, the graphene/polypyrrole electrochemical sensing method is high in sensitivity and selectivity, is 5-750 nM in detection linear range of the lead ions, and is 0.047 nM in detection limit. The preparation method is simple and controllable and is free of secondary pollution. The electrochemical sensor has wide application prospect of trace-amount lead ion detection in in-site monitoring of water body.
Description
Technical field
The invention belongs to environmental analysis field, relate to a kind of graphene-polypyrrole electrochemical sensor for trace lead ion detection
Preparation method and applications.
Background technology
Lead ion is widely distributed in the middle of environment water as a kind of representational heavy metal contaminants, along with biological chain is enriched with, by
The lead ion that food and drinking-water are taken in accumulates in vivo along with the growth at people's age.Harm is shown kidney, nerve by it
The toxic action of system, blood and reproductive system, produces permanent injury to tissue and internal organs.Especially to child
Toxic action the severeest, can damage intelligent development, suppress function of immune system and sensory function's obstacle etc..Therefore for
In environment water, the monitoring of trace lead ion is the most necessary, and a kind of novel simple detection method of research and development is so that efficiently, examine quickly
The lead ion surveying trace becomes the most important thing.
Traditional lead ion detection method mainly have inductively coupled plasma emission spectrography, Atomic Absorption or emission spectrometry,
Fluorimetry, inductively coupled plasma mass spectrometry etc..But these methods there are disadvantages that, such as: apparatus expensive,
Be difficult to operation, sample pretreatment process complexity, consuming time, sensitivity is the highest, selectivity is general.Electrochemical sensor conduct
A kind of potential detection means has the advantage of uniqueness in lead ion context of detection.Because its equipment needed thereby is simple, low cost,
Detection efficiency is fast, highly sensitive, thus is achieved the real-time in-situ analysis to trace materials.Therefore electrochemical sensor is permissible
As one of a kind of strong candidate of detection lead ion.During preparing sensor, the choice relation of sensing element is to sensing
Device Detection results and the complexity of detection method.In view of the detection impact of environment, detection sensitivity requirement in real time, and
The factors such as sensor stability, we choose one, and preparation method is the most controlled, detection sensitivity is high, and physical chemistry
The nano composite material of stable in properties is as sensing element.Structure and the process of use of electrochemical sensor are the most quick, it is to avoid
Secondary pollution problem, and meet it to adaptation requirements such as the detection pH of environment, temperature.Therefore this height simple to operate, green
The research and development of lead ion detection method that imitate, that the suitability is strong have very important realistic meaning.
The present invention at graphene nano lamella surface aggregate, forms graphene-polypyrrole three-dimensional many by electrochemical method control pyrroles
Pore structure, utilizes the polypyrrole that high conduction performance, chemical physical property are stable, environmental protection is friendly as lead ion probe, passes through stone
The signal amplification of ink alkene nanoscale twins, constructs and has high selectivity, highly sensitive graphene-polypyrrole electricity to lead ion
Chemical sensor.
Summary of the invention
The purpose of invention: it is an object of the invention to provide a kind of novel lead ion electrochemical sensor based on graphene-polypyrrole；
The preparation method of this sensor is the most controlled, and detection process will not produce secondary pollution.
The technical scheme is that
A kind of preparation method of the graphene-polypyrrole electrochemical sensor for trace lead ion detection, following steps:
(1) the Hummers chemical method improved is used to prepare graphite oxide olefinic oxide
Concentrated sulphuric acid (98%) is slowly added in graphite powder, concentrated sulphuric acid volume: graphite powder quality=23:1；After being sufficiently stirred for,
0 DEG C of ice-water bath is slowly added to KMnO4；KMnO4It is 3:1 with graphite powder mass ratio, mixed by obtain after being sufficiently stirred for simultaneously
After compound continuous ultrasound 5～7h, obtain deep brown solution.
In deep brown solution, it is slowly added to high purity water, after heated and boiled 5～15min, is sequentially added into the peroxide of high purity water and 30%
Change hydrogen and terminate reaction, obtain jonquilleous graphene oxide aqueous solution.
After centrifugation, go the removal of impurity with dilute hydrochloric acid centrifuge washing under conditions of 8000～10000r/min, then exist with high purity water
Under conditions of 8000～10000r/min, centrifuge washing goes the removal of impurity.
Taking out the graphite oxide of purification after washing, load bag filter dialysis and within 5～7 days, go the removal of impurity further, last lyophilization obtains
To solid oxidation Graphene.
(2) electrochemical synthesis graphene oxide-polypyrrole
First prepare electrolyte solution, graphene oxide prepared by step (1) is dispersed in ultra-pure water, to 2mg/mL
Graphene oxide dispersion in be sequentially added into pyrrole monomer and H2SO4, ultimate density 0.1M of pyrrole monomer, H2SO4?
Final concentration 0.1M, obtains homogeneous electrolyte solution by above-mentioned mixed solution at room temperature magnetic agitation 3h.
Use three-electrode system to select current-vs-time method at electrochemical workstation, apply 0.5V voltage, continue 300s, at glass
Carbon electrodes synthesis graphene oxide-polypyrrole complex.
(3) graphene oxide-polypyrrole that step (2) obtains is carried out electrochemical reduction, at pH=5.7
PBS in carry out CV scanning, scanning voltage scope is: 0～-1.0V, sweeps speed for 50mV/S, and starting voltage is 0V,
The scanning number of turns is 20, and the glass-carbon electrode deionized water that the graphene-polypyrrole obtained is modified cleans, and is dried, i.e. obtains under room temperature
Graphene-polypyrrole electrochemical sensor.
(4) detection by quantitative of lead ion: add plumbi nitras configuration 0～750 in NaAc_HAc buffer solution
NM series concentration, uses the graphene-polypyrrole electrochemical sensor that step (3) obtains, and uses entering of square wave stripping voltammetry
Row detection.
In step (2), electrode needs before using to be cleaned processing, and method is as follows: by glass-carbon electrode respectively in 1 μm, 0.3 μm
5-10min is ground successively, successively with ethanol and height every time after grinding with in the suspension of the aluminum oxide polishing powder of 0.05 μm particle diameter
Pure water ultrasonic cleaning 5min, is dried under room temperature.
The present invention has the effect that
(1) highly sensitive, detection limit is up to 0.047nM (S/N=3).
(2) the controlled easy operation of preparation method, non-secondary pollution.
(3) with low cost, utilize electrochemical workstation to analyze, it is not necessary to the main equipment of complex and expensive.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of graphene-polypyrrole electrochemical sensor detection lead ion.
Fig. 2 is the SEM picture of graphene-polypyrrole nano material.
Fig. 3 is the cyclic voltammetry curve picture of graphene oxide reduction process.
Fig. 4 A is the lead ion graph of a relation with its SWASV peak current of example gained variable concentrations.
Fig. 4 B is lead ion range of linearity figure (the 5nM-750nM model with its SWASV peak current of example gained variable concentrations
Enclose interior R2=0.987, detection is limited to 0.047nM).
Fig. 5 be the graphene-polypyrrole electrochemical sensor constructed by example to the selectivity test figure of lead ion (in figure metal from
Sub-concentration is 0.5 μM, and its current value is to measure gained by SWASV).
Detailed description of the invention
Below in conjunction with accompanying drawing and technical scheme, further illustrate the detailed description of the invention of the present invention.
The present invention relates to the preparation method of a kind of graphene-polypyrrole electrochemical sensor for trace lead ion detection and answer
With, this method, based on lead ion and the selective absorption effect (shown in Fig. 1) of the nitrogen-atoms of imido grpup in polypyrrole, ensures this
The high selectivity that lead ion is detected by sensor.And graphene nanometer sheet plays signal due to its high electrical conductivity in this sensor
Amplification, strengthens interface electron transport rate, and the synthesis for polypyrrole simultaneously provides platform to promote the formation of three-dimensional porous structure,
This graphene-polypyrrole composite is made to have more effective electroactive surface and more binding site；The two is combined and plays
Synergism.
Embodiment
A kind of graphene-polypyrrole electrochemical sensor for trace lead ion detection, builds and detection process is as follows:
(1) graphene oxide is prepared: graphene oxide uses the Hummers chemical method improved to prepare.Step is as follows: take
A certain amount of concentrated sulphuric acid (98%) is slowly added in graphite powder (concentrated sulphuric acid volume: graphite powder quality=23:1), fully stirs
After mixing, in 0 DEG C of ice-water bath, it is slowly added to KMnO4(KMnO4It is 3:1 with graphite powder mass ratio), it is sufficiently stirred for simultaneously.
Then by after mixture continuous ultrasound 5～7h, deep brown solution is obtained.In deep brown solution, it is slowly added to high purity water, adds
After heat boils 5～15min, it is sequentially added into the hydrogen peroxide termination reaction of high purity water and 30%, obtains jonquilleous Graphene
Oxide water solution.After centrifugation, with dilute hydrochloric acid centrifuge washing 2～3 removals under conditions of 8000～10000r/min
Impurity, then with high purity water centrifuge washing 5～go the removal of impurity 7 times under conditions of 8000～10000r/min.Take out after washing
The graphite oxide of purification, load bag filter (MW=14000) dialyse 5～7 days to go the removal of impurity further, the coldest
Freeze and be dried to obtain solid oxidation Graphene.
(2) electrochemical method for synthesizing of graphene oxide-polypyrrole: first prepare electrolyte solution, takes graphene oxide 100mg
It is dispersed in 50mL ultra-pure water, ultrasonic about 1h, in above-mentioned solution, is sequentially added into 0.347mL pyrroles, 0.267mL
H2SO4, above-mentioned mixed solution at room temperature magnetic agitation 3h is obtained homogeneous electrolyte solution.Use classical three-electrode system
(working electrode-glass-carbon electrode；Reference electrode-saturated calomel electrode；To electrode-platinum electrode) select electricity at electrochemical workstation
Stream-time method, applies 0.5V voltage, continues 300s, synthesizes graphene oxide-polypyrrole complex in glassy carbon electrode surface.
Wherein glass-carbon electrode needs cleaning before use, and concrete grammar is as follows:
Glass-carbon electrode is ground 5 respectively in the suspension of the aluminum oxide polishing powder of 1 μm, 0.3 μm and 0.05 μm particle diameter successively
Min, respectively with ethanol and high purity water ultrasonic cleaning 5min every time after grinding, is dried under room temperature.
(3) glass-carbon electrode of the graphene oxide-polypyrrole modifying obtained is carried out electrochemical reduction, delay at the PBS of pH=5.7
Rushing and carry out CV scanning in liquid, scanning voltage scope is: 0～-1.0V, and sweeping speed is 50mV/S, and starting voltage is 0V, scanning circle
Number is 20, and the glass-carbon electrode deionized water that the graphene-polypyrrole obtained is modified cleans, and is dried, i.e. obtains Graphene under room temperature
-polypyrrole electrochemical sensor.
(4) detection by quantitative of lead ion: the glass-carbon electrode that graphene-polypyrrole step (3) obtained is modified is immersed in pH=5
NaAc_HAc buffer solution adds a certain amount of plumbi nitras and is configured to 0～750nM series concentration, use square wave stripping voltammetry
(SWASV) carrying out detects.Parameter is provided that deposition voltage is-1V, and sedimentation time is 120s.
(5) selectivity test: add a certain amount of plumbi nitras, Mercury pernitrate., nitre in pH=5 NaAc_HAc buffer solution respectively
Acid zinc, copper nitrate, cadmium nitrate are configured to the testing sample that concentration is 0.5uM, and comprise this 5 heavy metal species ion simultaneously
Mixed solution.Testing sample is detected by glass-carbon electrode that graphene-polypyrrole step (3) obtained is modified successively, side
Method, with reference to step (4), investigates the selectivity of prepared sensor.
Detect the schematic diagram of lead ion as it is shown in figure 1, work as graphene-polypyrrole and be supported on glass-carbon electrode as electrochemical probe,
Due to lead ion and the nitrogen-atoms complexation on polypyrrole imido grpup in solution, change in electric can be produced, thus reach lead ion
The purpose of detection.
The SEM picture of this example gained graphene-polypyrrole of Fig. 2, it is known that its pattern is three-dimensional porous structure, the pattern of polypyrrole
For spherical.
Fig. 3 is the cyclic voltammetry curve picture of graphene oxide reduction process.It is left that the reduction peak of graphene oxide occurs in-0.85V
The right side, along with the increase of the scanning number of turns, reduction peak tapers into until being wholly absent explanation graphene oxide and having been reduced to as graphite
Alkene.
Fig. 4 is that the SWASV of the lead ion of variable concentrations is responded by the graphene-polypyrrole electrochemical sensor constructed by this example
Figure.
Fig. 4 A is the lead ion graph of a relation with its SWASV peak current of this example gained variable concentrations.It can be seen that with
The increase of plumbum ion concentration, the peak current in SWASV curve becomes big.
Fig. 4 B is the lead ion range of linearity figure with its SWASV peak current of this example gained variable concentrations.Knowable to figure, its
The range of linearity is 5-750nM, and detection is limited to 0.047nM.
Fig. 5 is the selectivity test figure to lead ion of the graphene-polypyrrole electrochemical sensor constructed by this example, in figure other
The concentration of metal ions of interference is 0.5 μM.
Claims (3)
1. the preparation method for the graphene-polypyrrole electrochemical sensor of trace lead ion detection, it is characterised in that following steps:
(1) the Hummers chemical method improved is used to prepare graphite oxide olefinic oxide
Concentrated sulphuric acid (98%) is slowly added in graphite powder, concentrated sulphuric acid volume: graphite powder quality=23:1；Fill
After dividing stirring, in 0 DEG C of ice-water bath, it is slowly added to KMnO4；KMnO4It is 3:1 with graphite powder mass ratio, is sufficiently stirred for simultaneously
After after the mixture continuous ultrasound 5～7h that will obtain, obtain deep brown solution；
In deep brown solution, it is slowly added to high purity water, after heated and boiled 5～15min, is sequentially added into the peroxide of high purity water and 30%
Change hydrogen and terminate reaction, obtain jonquilleous graphene oxide aqueous solution；
After centrifugation, go the removal of impurity with dilute hydrochloric acid centrifuge washing under conditions of 8000～10000r/min, then exist with high purity water
Under conditions of 8000～10000r/min, centrifuge washing goes the removal of impurity；
Taking out the graphite oxide of purification after washing, load bag filter dialysis and within 5～7 days, go the removal of impurity further, last lyophilization obtains
To solid oxidation Graphene；
(2) electrochemical synthesis graphene oxide-polypyrrole
First prepare electrolyte solution, graphene oxide prepared by step (1) be dispersed in ultra-pure water,
Pyrrole monomer and H it is sequentially added in the graphene oxide dispersion of 2mg/mL2SO4, ultimate density 0.1M of pyrrole monomer,
H2SO4Ultimate density 0.1M, above-mentioned mixed solution at room temperature magnetic agitation 3h is obtained homogeneous electrolyte solution；
Use three-electrode system to select current-vs-time method at electrochemical workstation, apply 0.5V voltage, continue 300s, at glass
Carbon electrodes synthesis graphene oxide-polypyrrole complex；
(3) graphene oxide-polypyrrole that step (2) obtains is carried out electrochemical reduction, at pH=5.7
PBS in carry out CV scanning, scanning voltage scope is: 0～-1.0V, sweeps speed for 50mV/S, and starting voltage is 0V,
The scanning number of turns is 20, and the glass-carbon electrode deionized water that the graphene-polypyrrole obtained is modified cleans, and is dried, i.e. obtains under room temperature
Graphene-polypyrrole electrochemical sensor；
(4) detection by quantitative of lead ion: add plumbi nitras configuration 0～750 in NaAc_HAc buffer solution
NM series concentration, uses the graphene-polypyrrole electrochemical sensor that step (3) obtains, and uses entering of square wave stripping voltammetry
Row detection.
Preparation method the most according to claim 1, it is characterised in that in step (2), glass-carbon electrode clean method before use is such as
Under: glass-carbon electrode is ground respectively in the suspension of the aluminum oxide polishing powder of 1 μm, 0.3 μm and 0.05 μm particle diameter successively
5-10min, successively with ethanol and high purity water ultrasonic cleaning 5min every time after grinding, is dried under room temperature.
3. the application of the graphene-polypyrrole electrochemical sensor that the preparation method described in claim 1 or 2 builds, it is characterised in that
The graphene-polypyrrole electrochemical sensor prepared is immersed in the sodium acetate-acetate buffer of the lead ion containing variable concentrations
In liquid, utilizing anodic stripping square wave voltammetry to detect, wherein anodic stripping square wave voltammetry detection is the 0.1M vinegar at pH=5
Carrying out in acid-sodium acetate buffer, deposition voltage is-1.0V, and sedimentation time is 120s.
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| CN106525933A (en) * | 2016-11-03 | 2017-03-22 | 天津大学 | Method for producing polypyrrole-coated nickel cobaltate nano wire array graphene electrode and application of graphene electrode for detecting heavy metallic lead ion |
| CN109490387A (en) * | 2018-11-07 | 2019-03-19 | 上海交通大学 | The preparation method of lead ion electrochemical sensor based on aptamer |
| CN109668950A (en) * | 2018-12-03 | 2019-04-23 | 济南大学 | A kind of application of prussian blue nano particle reduction graphene oxide composite material |
| CN110436584A (en) * | 2019-07-31 | 2019-11-12 | 西安建筑科技大学 | A kind of PPy/GO combination electrode material, preparation method and applications |
| CN110746600A (en) * | 2019-09-17 | 2020-02-04 | 北京航空航天大学 | Ion rectifying device and preparation method thereof |
| CN111936854A (en) * | 2018-03-29 | 2020-11-13 | 塞洛蒂克斯公司 | Improved electrode for electrochemical devices |
| CN115728369A (en) * | 2022-11-22 | 2023-03-03 | 浙江大学绍兴研究院 | High-sensitivity flexible breathable electrode for sweat lactic acid detection |
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| CN106290534A (en) * | 2015-05-11 | 2017-01-04 | 江南石墨烯研究院 | A kind of optimization method of detection of heavy metal ion based on graphene oxide |
| CN106525933A (en) * | 2016-11-03 | 2017-03-22 | 天津大学 | Method for producing polypyrrole-coated nickel cobaltate nano wire array graphene electrode and application of graphene electrode for detecting heavy metallic lead ion |
| CN106525933B (en) * | 2016-11-03 | 2019-08-13 | 天津大学 | Polypyrrole coats the preparation method of cobalt acid nickel nano-wire array Graphene electrodes and detects the application of heavy metal lead ion |
| CN111936854A (en) * | 2018-03-29 | 2020-11-13 | 塞洛蒂克斯公司 | Improved electrode for electrochemical devices |
| CN109490387A (en) * | 2018-11-07 | 2019-03-19 | 上海交通大学 | The preparation method of lead ion electrochemical sensor based on aptamer |
| CN109668950A (en) * | 2018-12-03 | 2019-04-23 | 济南大学 | A kind of application of prussian blue nano particle reduction graphene oxide composite material |
| CN110436584A (en) * | 2019-07-31 | 2019-11-12 | 西安建筑科技大学 | A kind of PPy/GO combination electrode material, preparation method and applications |
| CN110746600A (en) * | 2019-09-17 | 2020-02-04 | 北京航空航天大学 | Ion rectifying device and preparation method thereof |
| CN115728369A (en) * | 2022-11-22 | 2023-03-03 | 浙江大学绍兴研究院 | High-sensitivity flexible breathable electrode for sweat lactic acid detection |
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Application publication date: 20160810 |