CN106198663B - A kind of solid contact polymer film cadmium ion electrodes selective and its application - Google Patents
A kind of solid contact polymer film cadmium ion electrodes selective and its application Download PDFInfo
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- CN106198663B CN106198663B CN201510224160.9A CN201510224160A CN106198663B CN 106198663 B CN106198663 B CN 106198663B CN 201510224160 A CN201510224160 A CN 201510224160A CN 106198663 B CN106198663 B CN 106198663B
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Abstract
The present invention relates to the method for detection heavy metal cadmium ion, specifically a kind of solid contact polymer film cadmium ion electrodes selective and its application.To have ionic-electronic conduction layers of the three-dimensional grapheme of the porous structure/mesoporous Pt as solid contact polymer film cadmium ion electrodes selective, and has sensitive membrane on ionic-electronic conduction layer.The three-dimensional porous graphene that the present invention uses/mesoporous Pt composite constructions have apparent cavernous structure, good electric conductivity, quick electronic conductivity energy and big electric double layer capacitance；The conduction velocity that can accelerate ion-electron as conducting shell improves the stability of electrode.
Description
Technical field
The present invention relates to detection heavy metal cadmium ion method, specifically a kind of solid contact polymer film cadmium from
Sub- electrodes selective and its application.
Background technology
Ion selective electrode as a kind of electrochemical sensor be potentiometry since the sixties in last century most
Important progress, it has also become the new hot spot in chemical sensor field.This method is since with high sensitivity, selectivity is good, carries
Conveniently, the features such as on-line analysis and monitoring can be used for, it is constantly subjected to the highest attention of scientific research personnel, is successfully used for environment prison
The fields such as survey, bio-medical analysis, Industrial Analysis, marine pollution monitoring, soil analysis, become in analytical chemistry one it is important
Monitoring method and means.It should be pointed out that conventional ion electrodes selective uses internal-filling liquid and internal reference electrode, in zero current
Under the conditions of there are a steady state ion flux from electrode film phase flow direction sample solution phase, and the ionic flux generated greatly limits
The development of the reduction and microelectrode of electrode detection limit.Internal-filling liquid is replaced by solid contact for this cause, to promote
Into the development of solid contact ion selective electrode.
Solid contact ion selective electrode biggest advantage is electrode without internal-filling liquid, can not only reduce detection limit,
It is durable, and be easy to minimize.In order to obtain stable potential and accelerate the conduction velocity of ion-electron, generally in electrode and polymerization
Add one layer of conducting shell between object membrane interface.Previously there is document report conducting polymer in solid contact ion selective electrode
Object, such as：Polyaniline, polypyrrole, poly- 3- octyl thiophenes etc. are used as ionic-electronic conduction layer.However, in ion selectivity sensitive film
Redox side reaction occurs due to the presence of dissolved oxygen between conducting polymer, and at the same time there is also inevitable
Water layer, these shortcomings limit the application of conducting polymer.Carbon material in recent years, including：Fullerene, graphene, carbon are received
Mitron, three-dimensional ordered macroporous carbon and crosslinking trace mesoporous carbon etc. can effectively eliminate water layer as ionic-electronic conduction layer
Presence, improve the stability of electrode, there is good application prospect, but for example three-dimensional ordered macroporous carbon of these materials, crosslinking
Trace mesoporous carbon preparation method complexity is cumbersome, need to use template, time-consuming；And fullerene, graphene, carbon nanotube are then steady in electrode
Qualitative aspect needs to be further increased.
Invention content
The purpose of the present invention is to provide a kind of solid contact polymer film cadmium ion electrodes selective and its applications.
The technical solution adopted by the present invention is to achieve the above object：
A kind of solid contact polymer film cadmium ion electrodes selective, to have the three-dimensional grapheme of porous structure/mesoporous
Ionic-electronic conduction layers of the Pt as solid contact polymer film cadmium ion electrodes selective, and in ionic-electronic conduction layer
It is upper to have sensitive membrane.
The method synthesis that the ionic-electronic conduction layer is assembled altogether using a step hydro-thermal.
The ionic-electronic conduction layer is prepared as：
1) graphene oxide (GO) is substantially soluble in water and obtains GO solution, for use；
2) by potassium chloroplatinite (K2PtCl4) it is substantially soluble in water to obtain K2PtCl4Solution, while by polyethylene glycol hexadecane
Base ether (Brij 58) makes it completely dissolved, and ascorbic acid solution is added after dissolving until solution becomes black, dark solution from
Gains in depth of comprehension black precipitate, as mesoporous Pt nano particles；
3) the mesoporous Pt nano particles of above-mentioned acquisition are dissolved in step 1) in GO solution, ultrasound makes it be uniformly mixed, mixing
Mixed liquor is placed in reaction kettle afterwards, is reacted in drying box, goes to remove water after the completion of reaction, and freeze-drying is to get to required
Three-dimensional porous graphene/mesoporous Pt composite constructions.
The content of GO is 2-3mg/mL in GO solution in the step 1).
K in the step 2)2PtCl4K in solution2PtCl4Content be 8-10mg/mL；Polyethylene glycol ten in dark solution
Containing for six alkyl ethers is 5-6mg/mL；Ascorbic acid solution content is 8-10mg/mL in dark solution.
Step 3) the mixed liquor is placed in ptfe autoclave, reacts 3-4h in 160-180 DEG C of drying box,
It goes to remove water after the completion of reaction, freeze-drying two days is to get to required three-dimensional porous graphene/mesoporous Pt composite constructions.
It will be dispersed in water after three-dimensional porous graphene/mesoporous Pt composite constructions grinding, solution drop is in glass carbon after taking dispersion
On electrode, so that aqueous solution is evaporated with infrared light irradiation, obtains uniform ionic-electronic conduction layer.
Solution concentration is 2-3mg/mL after the dispersion.
The polymer film ion selective electrode sensitive membrane that is prepared as of the sensitivity coating solution includes ionophore and sensitivity
Film basis material.Wherein ionophore is lead ion carrier.Sensitive membrane basis material includes polyvinyl chloride, poly- butylacrylic acid
Ester, butyl polyacrylate, polyetherimide, rubber or sol-gel film；Plasticizer is o- nitrobenzene octyl ether (o-NPOE), two-
2- ethylhexyls last of the ten Heavenly stems ester, dibutyl sebacate or dioctyl sebacate；Ion-exchanger is four (3,5- bis- (trifluoromethyl) benzene
Base) Boratex, dinonylnaphthalene sulfonic acid or three (dodecyl) ammonium chlorides.
A kind of preparation method of solid contact polymer film cadmium ion electrodes selective, is assembled altogether using a step hydro-thermal
Method synthesis with porous structure graphene/mesoporous Pt composite constructions, using composite construction drop coating to glassy carbon electrode surface as
Ionic-electronic conduction layer then has sensitive membrane on ionic-electronic conduction layer again.
A kind of application of solid contact polymer film cadmium ion electrodes selective, the solid contact polymer film cadmium
Among ion selective electrode is used for the detection of heavy metal cadmium ion.
The advantage of the invention is that：
1. three-dimensional grapheme/Jie of the method synthesis with porous structure that the electrode of the present invention is assembled altogether using a step hydro-thermal
Hole Pt composite constructions as ionic-electronic conduction layer, the three-dimensional material not only with the excellent performance of graphene itself and due to
With porous structure, thus there is more good electric conductivity, quick electronic conductivity energy and big electric double layer capacitance,
The conduction velocity that can accelerate ion-electron keeps response quicker, stablizes.
2. mesoporous Pt nano particles are added to three-dimensional porous graphene by the present invention using the method that a step hydro-thermal assembles altogether
In structure.Due to the difference function and synergistic effect between different nano materials, with common two-dimensional graphene and not
The three-dimensional porous graphene of mesoporous Pt nano particles is added to compare, the addition of mesoporous Pt nano particles can further increase porous stone
The chemical property of black alkene.The graphite of prepared three-dimensional porous structure can be evident that by cyclic voltammetry
Alkene/mesoporous Pt composite construction chemical properties be substantially better than common two-dimensional graphene and not plus mesoporous Pt nano particles three
Tie up porous graphene.In addition, a step hydro-thermal is total to, construction from part is easy to operate, and convenient, yield is high, is convenient for solid contact polymer film
The preparation of cadmium ion electrodes selective.
3. solid contact polymer film cadmium ion electrodes selective prepared by the present invention is to the detection sensitivity of cadmium ion
Height, detection is quick, and stability is good.It is able to detect that 10-10M nitric acid cadmium solutions, and 10-3-10-9It is in M nitric acid cadmium solutions
This spy's response of existing energy.
Description of the drawings
Fig. 1 is that the method provided in an embodiment of the present invention assembled altogether using a step hydro-thermal prepares the three-dimensional for providing porous structure
The photomacrograph of graphene/mesoporous Pt composite constructions and microcosmic electron microscope.
Fig. 2 is three prepared using the method that a step hydro-thermal assembles altogether with porous structure provided in an embodiment of the present invention
Tie up the three-dimensional porous graphene that graphene/mesoporous Pt composite constructions do not add mesoporous Pt nano particles with ordinary two dimensional graphene and
Cyclic voltammetry figure.
Fig. 3 is that solid contact polymer film cadmium ion electrodes selective provided in an embodiment of the present invention measures 10-3-10- 10The potential change response diagram of M nitric acid cadmium solutions.
Specific implementation mode
Embodiment 1
The specific preparation process of solid contact polymer film cadmium ion electrodes selective is as follows：
A. the preparation of sensitive membrane：PVC granule, o- nitrobenzene octyl ether, lead ion carrier and four (3,5- bis- (trifluoromethyl)
Phenyl) Boratex the total 250mg of mixture, the wherein o- nitrobenzene octyl ether of 32.66wt%PVC particles, 65.32wt%,
1.00wt% cadmium ions carrier and 1.02wt% tetra- (3,5- bis- (trifluoromethyl) phenyl) Boratex, are moved into 2.0mL tetrahydrochysene furans
It mutters in solution, ultrasound, stirring 2h are allowed to be uniformly dispersed.
B. the preparation of three-dimensional porous graphene/mesoporous Pt composite constructions：
1) GO for weighing 120mg is dissolved in ultrasound 1h in 40mL water, obtains the GO solution of 3mg/mL, for use；
2) K of 40mg is weighed2PtCl4It is dissolved in 5mL water, is made into the K of 20mM2PtCl4Solution.And backward K2PtCl4Solution
Middle 58 ultrasounds of Brij that 50mg is added make it completely dissolved to obtain mixed solution, the final concentration of 9mM of Brij 58 in mixed solution；
5mL0.1M ascorbic acid solutions, ultrasound is finally added into above-mentioned mixed solution again, until solution becomes black.10000rpm
Centrifuge Brij 58 extra in 15min removal solution, leaving layer black precipitate, as mesoporous Pt nano particles.
3) the mesoporous Pt nano particles that centrifugation obtains are dissolved in the GO solution of 40mL 3mg/mL, ultrasound keeps its mixing equal
It is even, it is then placed in the ptfe autoclave of 50mL, 180 DEG C of reaction 3h, go to remove water after the completion of reaction in drying box, cold
Dry two days are lyophilized to get to required three-dimensional porous graphene/mesoporous Pt composite constructions.(referring to Fig. 1)
The porous graphene prepared as shown in Figure 1/mesoporous Pt composite constructions have cylindrical exterior, have inside it bright
Aobvious porous structure and contain mesoporous Pt nano particles.
C. the three-dimensional porous graphene of drop coating/mesoporous Pt composite constructions：Take the above-mentioned synthesized three-dimensional porous graphenes of 3mg/
Mesoporous Pt composite constructions first use mortar grinder, after be scattered in 1mL water, be made into the dispersion liquid of 3mg/ml.Take 10 μ L solution drop in
On glass-carbon electrode (electrode diameter 3mm), so that aqueous solution is evaporated with infrared light irradiation, can be obtained uniformly in glassy carbon electrode surface
Three-dimensional porous graphene/mesoporous Pt composite construction conducting shells.It is multiple using the three-dimensional porous graphene of cyclic voltammetry/mesoporous Pt
Close the chemical property of structure (referring to Fig. 2).From Figure 2 it can be seen that the electric double layer electricity of three-dimensional porous graphene/mesoporous Pt composite constructions
Hold the three-dimensional porous graphene for being significantly greater than ordinary two dimensional graphene and not adding mesoporous Pt nano particles, illustrates three-dimensional structure
Porous graphene chemical property is substantially better than two-dimentional common graphite alkene, and due to the difference function between different nano materials
And synergistic effect, the addition of mesoporous Pt nano particles can then further increase the chemical property of three-dimensional grapheme.
D. the sensitive membrane that a. is prepared is dropped on the electrode that c. is prepared, and at room temperature naturally volatilization 6h to get to
Prepare the solid contact polymer film cadmium ion electrodes selective completed.
Embodiment 2
It should be first 10 before use by the above-mentioned electrode acquired-3It is activated one day in M nitric acid cadmium solutions, then again 10- 9It is activated two days in M nitric acid cadmium solutions.
Activated electrode is sequentially inserted into (cadmium nitrate solution concentration in a series of nitric acid cadmium solution containing various concentrations
Respectively 10-3, 10-4, 10-5, 10-6,10-7, 10-8, 10-9, 10-10, 5 × 10-11Mol/L), generate potential response signal (referring to
Fig. 3).
As seen from Figure 3, using porous graphene/mesoporous Pt composite constructions as the solid contact polymer film of solid contact layer
Cadmium ion electrodes selective has very sensitive potential response, finally can detect 10-10The concentration of cadmium ions of mol/L, and electricity
Position is 10-3-10-9Being presented within the scope of mol/L can this spy's response.
From the foregoing, it can be seen that the solid contact polymer film cadmium ion electrodes selective of the present invention can detect 10-10mol/L
Concentration of cadmium ions, and 10-3mol/L-10-9Presentation is good within the scope of mol/L concentration of cadmium ions can this spy's response.
Embodiment 3
Difference from Example 1 is：
A. three-dimensional porous graphene/mesoporous Pt composite constructions are prepared：The preparation of GO solution and mesoporous Pt nano particles
Journey is carried out with reference to 1 step b of embodiment.The mesoporous Pt nano particles that centrifugation obtains are dissolved in the GO solution of 40mL 2mg/mL, are surpassed
Sound makes it be uniformly mixed, and is then placed in the ptfe autoclave of 50mL, and 180 DEG C of reaction 3h, have reacted in drying box
It goes to remove water after, freeze-drying two days is to get to required three-dimensional porous graphene/mesoporous Pt composite constructions.
B. remaining implementation steps is carried out with reference to embodiment 1 step c, d and embodiment 2, can obtain solid contact polymerization
Object film cadmium ion electrodes selective measures 10-3-10-10The potential change of M nitric acid cadmium solutions responds.
Embodiment 4
Difference from Example 1 is：A. porous graphene/mesoporous Pt composite constructions are prepared：GO solution and mesoporous
The preparation process of Pt nano particles is carried out with reference to 1 step b of embodiment.The mesoporous Pt nano particles that centrifugation obtains are dissolved in 40mL
In the GO solution of 2.5mg/mL, ultrasound makes it be uniformly mixed, and is then placed in the ptfe autoclave of 50mL, in drying box
In 180 DEG C of reaction 3h, go to remove water after the completion of reaction, freeze-drying two days is to get to required three-dimensional porous graphene/mesoporous
Pt composite constructions.
B. remaining implementation steps is carried out with reference to embodiment 1 step c, d and embodiment 2, can obtain solid contact polymerization
Object film cadmium ion electrodes selective measures 10-3-10-10The potential change of M nitric acid cadmium solutions responds.
Embodiment 5
Difference from Example 1 is：A. drop coating porous graphene/mesoporous Pt composite constructions：It takes more synthesized by 3mg
Hole graphene/mesoporous Pt composite constructions first use mortar grinder, after be scattered in 1mL water, be made into the dispersion liquid of 3mg/mL.Take 5 μ L
Solution is dripped on glass-carbon electrode, so that aqueous solution is evaporated with infrared light irradiation, can be obtained in glassy carbon electrode surface uniform porous
Graphene/mesoporous Pt composite construction conducting shells.
B. remaining implementation steps is carried out with reference to 1 step d of embodiment and embodiment 2, can obtain solid contact polymer
Film cadmium ion electrodes selective measures 10-3-10-10The potential change of M nitric acid cadmium solutions responds.
Embodiment 6
Difference from Example 1 is：
A. drop coating porous graphene/mesoporous Pt composite constructions：Take porous graphene/mesoporous Pt composite junctions synthesized by 3mg
Structure first use mortar grinder, after be scattered in 1mL water, be made into the dispersion liquid of 3mg/mL.It takes 15 μ L solution drop on glass-carbon electrode, uses
Infrared light irradiation makes aqueous solution evaporate, and can obtain uniform porous graphene/mesoporous Pt composite constructions in glassy carbon electrode surface
Conducting shell.
B. remaining implementation steps is carried out with reference to 1 step d of embodiment and embodiment 2, can obtain solid contact polymer
Film cadmium ion electrodes selective measures 10-3-10-10The potential change of M nitric acid cadmium solutions responds.
Embodiment 7
Difference from Example 1 is：
A. drop coating porous graphene/mesoporous Pt composite constructions：Take porous graphene/mesoporous Pt composite junctions synthesized by 3mg
Structure first use mortar grinder, after be scattered in 1mL water, be made into the dispersion liquid of 3mg/mL.It takes 20 μ L solution drop on glass-carbon electrode, uses
Infrared light irradiation makes aqueous solution evaporate, and can obtain uniform porous graphene/mesoporous Pt composite constructions in glassy carbon electrode surface
Conducting shell.
B. remaining implementation steps is carried out with reference to 1 step d of embodiment and embodiment 2, can obtain solid contact polymer
Film cadmium ion electrodes selective measures 10-3-10-10The potential change of M nitric acid cadmium solutions responds.
Claims (6)
1. a kind of solid contact polymer film cadmium ion electrodes selective, it is characterised in that：To have the three-dimensional stone of porous structure
Ionic-electronic conduction layers of the black alkene/mesoporous Pt as solid contact polymer film cadmium ion electrodes selective, and in ion-
Has sensitive membrane on electronic conductive layer；
The method synthesis that the ionic-electronic conduction layer is assembled altogether using a step hydro-thermal；
The ionic-electronic conduction layer is prepared as：
1）By graphene oxide（GO）It is substantially soluble in water and obtains graphene oxide solution, for use；
2）By potassium chloroplatinite（K2PtCl4）It is substantially soluble in water to obtain chloroplatinous acid potassium solution, while by polyethylene glycol cetyl
Ether（Brij 58）It makes it completely dissolved, ascorbic acid solution is added after dissolving until solution becomes black, dark solution centrifugation
Obtain black precipitate, as mesoporous Pt nano particles；
3）The mesoporous Pt nano particles of above-mentioned acquisition are dissolved in step 1）In middle graphene oxide solution, ultrasound makes it be uniformly mixed,
Mixed liquor is placed in reaction kettle after mixing, is reacted in drying box, goes to remove water after the completion of reaction, and freeze-drying is to get to required
The three-dimensional porous graphene wanted/mesoporous Pt composite materials；
The step 1）The content of graphene oxide is 2-3 mg/mL in middle graphene oxide solution；
The step 2）The content of middle potassium chloroplatinite Chlorine in Solution Asia potassium platinate is 8-10 mg/mL；Poly- second two in dark solution
Containing for alcohol cetyl ether is 5-6 mg/mL；Ascorbic acid content is 8-10 mg/mL in dark solution.
2. solid contact polymer film cadmium ion electrodes selective as described in claim 1, it is characterised in that：The step
3）Mixed liquor is placed in ptfe autoclave, and 3-4 h are reacted in 160-180 DEG C of drying box, are removed after the completion of reaction
Water, freeze-drying two days is to get to required three-dimensional porous graphene/mesoporous Pt composite materials.
3. solid contact polymer film cadmium ion electrodes selective as described in claim 1, it is characterised in that：Three-dimensional is more
It is dispersed in water after hole graphene/mesoporous Pt composite materials grinding, solution drop is shone on glass-carbon electrode with infrared lamp after taking dispersion
Penetrating makes aqueous solution evaporate, and obtains uniform ionic-electronic conduction layer.
4. solid contact polymer film cadmium ion electrodes selective as described in claim 3, it is characterised in that：The dispersion
Solution concentration is 2-3 mg/mL afterwards.
5. a kind of preparation method of solid contact polymer film cadmium ion electrodes selective described in claim 1, feature
It is：Graphene/mesoporous Pt composite material of the method synthesis with porous structure assembled altogether using a step hydro-thermal, by composite wood
Gob is coated onto glassy carbon electrode surface as ionic-electronic conduction layer, then has sensitive membrane on ionic-electronic conduction layer again.
6. a kind of application of solid contact polymer film cadmium ion electrodes selective described in claim 1, it is characterised in that：
Among the solid contact polymer film cadmium ion electrodes selective is used for the detection of heavy metal cadmium ion.
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| CN109580750A (en) * | 2017-09-28 | 2019-04-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of wearable perspiration sensor chip, device and the preparation method and application thereof |
| CN109580751A (en) * | 2018-12-03 | 2019-04-05 | 中国科学院烟台海岸带研究所 | A method of realizing that molecular imprinted polymer membrane ion selective electrode updates |
| CN110243910A (en) * | 2019-06-12 | 2019-09-17 | 华东理工大学 | A kind of monimostyly ion selective electrode based on sulfhydrylation redox graphene |
| CN112213368B (en) * | 2019-07-09 | 2023-03-21 | 中国科学院烟台海岸带研究所 | Potential microelectrode sensor with universality and preparation and application thereof |
| CN113514525A (en) * | 2020-04-09 | 2021-10-19 | 中国科学院烟台海岸带研究所 | Method for measuring nitrate ions by using solid contact type ion selective electrode |
| CN111579617B (en) * | 2020-05-11 | 2022-11-15 | 中国科学院烟台海岸带研究所 | Preparation and application of solid contact type polymer film copper ion selective electrode |
| CN114544728B (en) * | 2020-11-25 | 2023-10-27 | 中国科学院烟台海岸带研究所 | Thin-layer polymer film ion selective electrode based on pulse constant current control and detection method |
| CN113008965B (en) * | 2021-03-04 | 2022-06-21 | 深圳大学 | Preparation method and application of solid film phosphate radical ion selective electrode based on cobalt/pyrrole/mesoporous carbon |
| CN113484394A (en) * | 2021-07-16 | 2021-10-08 | 香港中文大学深圳研究院 | Porous three-dimensional electrode and preparation method and application thereof |
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