CN106198663A - A kind of solid contact polymeric film cadmium ion electrodes selective and application thereof - Google Patents
A kind of solid contact polymeric film cadmium ion electrodes selective and application thereof Download PDFInfo
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- CN106198663A CN106198663A CN201510224160.9A CN201510224160A CN106198663A CN 106198663 A CN106198663 A CN 106198663A CN 201510224160 A CN201510224160 A CN 201510224160A CN 106198663 A CN106198663 A CN 106198663A
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Abstract
The method that the present invention relates to detect heavy metal cadmium ion, specifically a kind of solid contact polymeric film cadmium ion electrodes selective and application thereof.To have the three-dimensional grapheme/mesoporous Pt ionic-electronic conduction layer as solid contact polymeric film cadmium ion electrodes selective of loose structure, and with sensitive membrane on ionic-electronic conduction layer.Three-dimensional porous Graphene/mesoporous Pt composite construction that the present invention uses has cavernous structure clearly, good electric conductivity, quick electronic conductivity energy and big electric double layer capacitance；The conduction velocity of ion-electron can be accelerated as conducting shell, improve the stability of electrode.
Description
Technical field
The method that the present invention relates to detect heavy metal cadmium ion, specifically a kind of solid contact gathers
Compound film cadmium ion electrodes selective and application thereof.
Background technology
Ion-selective electrode is that potentiometric analysis was from 60 years last century as a kind of electrochemical sensor
Most important progress since generation, it has also become the new focus in chemical sensor field.The method is owing to having
Highly sensitive, selectivity good, easy to carry, the feature such as on-line analysis and monitoring can be used for, be subject to always
To the highest attention of scientific research personnel, be successfully used for environmental monitoring, bio-medical analysis, Industrial Analysis,
The field such as marine pollution monitoring, soil analysis, become in analytical chemistry an important monitoring method and
Means.It is pointed out that conventional ion electrodes selective uses internal-filling liquid and internal reference electrode,
There is a steady state ion flux from electrode film phase flow direction sample solution phase under the conditions of zero current, and produce
Raw ionic flux strongly limit reduction and the development of microelectrode of electrode detection limit.Due to this edge
Therefore internal-filling liquid is replaced by solid contact, thus promote solid contact ion-selective electrode
Development.
The maximum advantage of solid contact ion-selective electrode be electrode without internal-filling liquid, can not only drop
Low detection limit, durable, and it is prone to miniaturization.In order to obtain steady potential and accelerate the biography of ion-electron
Lead speed, between electrode and polymer film interface, typically add one layer of conducting shell.Document had previously been had to report
Conducting polymer in solid contact ion-selective electrode, such as: polyaniline, polypyrrole, poly-3-
Octyl thiophene etc. are as ionic-electronic conduction layer.But, at ion selectivity sensitive film and conducting polymer
There is oxidoreduction side reaction between thing due to the existence of dissolved oxygen, and there is also simultaneously and can not keep away
The water layer exempted from, these weak points limit the application of conducting polymer.Material with carbon element in recent years, including:
The conducts such as fullerene, Graphene, CNT, three-dimensional ordered macroporous carbon and crosslinking trace mesoporous carbon
Ionic-electronic conduction layer can effectively eliminate the existence of water layer, improves the stability of electrode, has very
Good application prospect, but the most three-dimensional ordered macroporous carbon of these materials, crosslinking trace mesoporous carbon preparation method
Complicated loaded down with trivial details, template need to be used, the longest；Fullerene, Graphene, CNT are then steady at electrode
Qualitative aspect needs to be improved further.
Summary of the invention
It is an object of the invention to provide a kind of solid contact polymeric film cadmium ion electrodes selective and
Its application.
The technical solution used in the present invention is for achieving the above object:
A kind of solid contact polymeric film cadmium ion electrodes selective, to have the three-dimensional stone of loose structure
Ink alkene/mesoporous Pt is as the ionic-electronic conduction of solid contact polymeric film cadmium ion electrodes selective
Layer, and with sensitive membrane on ionic-electronic conduction layer.
Described ionic-electronic conduction layer uses the method synthesis that a step hydro-thermal assembles altogether.
Described ionic-electronic conduction layer is prepared as:
1) graphene oxide (GO) is substantially soluble in water obtains GO solution, stand-by；
2) by potassium chloroplatinite (K2PtCl4) it is substantially soluble in water to obtain K2PtCl4Solution, simultaneously will be poly-
Ethylene glycol cetyl ether (Brij 58) makes it be completely dissolved, and adds ascorbic acid solution after dissolving
Until solution becomes black, dark solution is centrifuged to obtain black precipitate, is mesoporous Pt nano-particle；
3) mesoporous for above-mentioned acquisition Pt nano-particle is dissolved in step 1) in GO solution, ultrasonic make it
Mix homogeneously, during mixed liquor is placed in reactor after mixing, reacts in drying baker, goes after having reacted
Except water, lyophilization, i.e. obtain required three-dimensional porous Graphene/mesoporous Pt composite construction.
Described step 1) in GO solution the content of GO be 2-3mg/mL.
Described step 2) in K2PtCl4K in solution2PtCl4Content be 8-10mg/mL；Dark solution
Containing for 5-6mg/mL of middle Polyethylene Glycol cetyl ether；In dark solution, ascorbic acid solution content is
8-10mg/mL。
Described step 3) mixed liquor is placed in politef reactor, in the drying baker of 160-180 DEG C
Middle reaction 3-4h, removes water, lyophilization two days, i.e. obtains required three-dimensional many after having reacted
Hole Graphene/mesoporous Pt composite construction.
It is dispersed in water after three-dimensional porous Graphene/mesoporous Pt composite construction is ground, molten after taking dispersion
Drop, on glass-carbon electrode, irradiates with infrared lamp and makes aqueous solution evaporate, and obtains uniform ion-electron and passes
Conducting shell.
After described dispersion, solution concentration is 2-3mg/mL.
The polymer film ion selective electrode sensitive membrane that is prepared as of described sensitive membrane solution includes that ion carries
Body and sensitive membrane matrix material.Wherein ionophore is lead ion carrier.Sensitive membrane matrix material includes
Polrvinyl chloride, poly-butyl propyleneglycol acid esters, butyl polyacrylate, Polyetherimide, rubber or colloidal sol are solidifying
Glued membrane；Plasticizer is o-Nitrobenzol octyl ether (o-NPOE), two-2-ethylhexyl esters in the last of the ten Heavenly stems, decanedioic acid two
Butyl ester or di-n-octyl sebacate；Ion-exchanger be four (3,5-bis-(trifluoromethyl) phenyl) sodium borate,
Dinonylnaphthalene sulfonic acid or three (dodecyl) ammonium chloride.
The preparation method of a kind of solid contact polymeric film cadmium ion electrodes selective, utilizes a step water
The method synthesis that heat assembles altogether has the Graphene/mesoporous Pt composite construction of loose structure, by composite junction
Structure drop coating to glassy carbon electrode surface as ionic-electronic conduction layer, the most again at ionic-electronic conduction layer
Upper with sensitive membrane.
A kind of application of solid contact polymeric film cadmium ion electrodes selective, described solid contact
Polymeric film cadmium ion electrodes selective is among the detection of heavy metal cadmium ion.
It is an advantage of the current invention that:
1. the method synthesis that the electrode of the present invention uses a step hydro-thermal to assemble altogether has the three-dimensional of loose structure
Graphene/mesoporous Pt composite construction is as ionic-electronic conduction layer, and this three-dimensional material not only has graphite
Performance that alkene itself is excellent and owing to having loose structure, thus there is better electric conductivity,
Quickly electronic conductivity energy and big electric double layer capacitance, it is possible to accelerate the conduction velocity of ion-electron,
Make response more quick, stable.
2. it is many that mesoporous Pt nano-particle is joined three-dimensional by the method that the present invention uses a step hydro-thermal to assemble altogether
In the graphene-structured of hole.Due to the difference function between different nano materials and synergism, with
Common two-dimensional graphene and do not add the three-dimensional porous Graphene of mesoporous Pt nano-particle and compare, mesoporous
The addition of Pt nano-particle can improve the chemical property of porous graphene further.Lied prostrate by circulation
Peace test can be evident that the Graphene/mesoporous Pt composite junction of prepared three-dimensional porous structure
Structure chemical property is substantially better than common two-dimensional graphene and does not adds the three-dimensional of mesoporous Pt nano-particle
Porous graphene.It addition, step hydro-thermal construction from part altogether is simple to operate, convenient, yield is high, it is simple to Gu
The preparation of body contact polymeric film cadmium ion electrodes selective.
3. the solid contact polymeric film cadmium ion electrodes selective that prepared by the present invention inspection to cadmium ion
Surveying highly sensitive, detection is quick, good stability.It is able to detect that 10-10M cadmium nitrate solution, and
10-3-10-9Presenting in M cadmium nitrate solution can this special response.
Accompanying drawing explanation
Porous is provided in the method utilizing a step hydro-thermal to assemble the altogether preparation that Fig. 1 provides for the embodiment of the present invention
The photomacrograph of the three-dimensional grapheme of structure/mesoporous Pt composite construction and microcosmic Electronic Speculum figure.
Fig. 2 prepare for the method utilizing a step hydro-thermal to assemble altogether that the embodiment of the present invention provides have many
The three-dimensional grapheme of pore structure/mesoporous Pt composite construction and ordinary two dimensional Graphene and do not add mesoporous Pt
The three-dimensional porous Graphene cyclic voltammetry figure of nano-particle.
The solid contact polymeric film cadmium ion electrodes selective that Fig. 3 provides for the embodiment of the present invention is surveyed
Fixed 10-3-10-10The potential change response diagram of M cadmium nitrate solution.
Detailed description of the invention
Embodiment 1
The concrete preparation process of solid contact polymeric film cadmium ion electrodes selective is as follows:
A. the preparation of sensitive membrane: PVC granule, o-Nitrobenzol octyl ether, lead ion carrier and four (3,5-
Two (trifluoromethyl) phenyl) the mixture altogether 250mg of sodium borate, wherein 32.66wt%PVC granule,
65.32wt% o-Nitrobenzol octyl ether, 1.00wt% cadmium ion carrier and 1.02wt% tetra-(3,5-bis-(three
Methyl fluoride) phenyl) sodium borate, it is moved in 2.0mL tetrahydrofuran solution, ultrasonic, stirring 2h makes
Be uniformly dispersed.
The preparation of the most three-dimensional porous Graphene/mesoporous Pt composite construction:
1) GO weighing 120mg is dissolved in ultrasonic 1h in 40mL water, and the GO obtaining 3mg/mL is molten
Liquid, stand-by；
2) K of 40mg is weighed2PtCl4It is dissolved in 5mL water, is made into the K of 20mM2PtCl4Solution.
And backward K2PtCl4Solution adds the Brij 58 of 50mg is ultrasonic makes it be completely dissolved to obtain mixed solution,
The final concentration of 9mM of Brij 58 in mixed solution；Last addition 5mL in above-mentioned mixed solution again
0.1M ascorbic acid solution, ultrasonic, until solution becomes black.10000rpm is centrifuged 15min and goes
Except Brij 58 unnecessary in solution, leaving layer black precipitate, it is mesoporous Pt nano-particle.
3) the centrifugal mesoporous Pt nano-particle obtained is dissolved in the GO solution of 40mL 3mg/mL,
Ultrasonic make its mix homogeneously, be then placed in the politef reactor of 50mL, in drying baker
180 DEG C of reaction 3h, remove water, lyophilization two days, i.e. obtain required three-dimensional after having reacted
Porous graphene/mesoporous Pt composite construction.(seeing Fig. 1)
The porous graphene prepared as shown in Figure 1/mesoporous Pt composite construction has cylindrical exterior,
There is obvious loose structure and containing mesoporous Pt nano-particle inside it.
C. the three-dimensional porous Graphene of drop coating/mesoporous Pt composite construction: take 3mg above-mentioned synthesized three
Dimension porous graphene/mesoporous Pt composite construction first with mortar grinder, after be scattered in 1mL water, be made into 3
The dispersion liquid of mg/ml.Take 10 μ L solution and drip on glass-carbon electrode (electrode diameter is 3mm), with red
Outer light irradiation makes aqueous solution evaporate, it is possible to glassy carbon electrode surface obtain uniform three-dimensional porous Graphene/
Mesoporous Pt composite construction conducting shell.The three-dimensional porous Graphene of cyclic voltammetry/mesoporous Pt is used to be combined
The chemical property (seeing Fig. 2) of structure.From Figure 2 it can be seen that three-dimensional porous Graphene/mesoporous Pt is multiple
Close the electric double layer capacitance significantly greater than ordinary two dimensional Graphene of structure and do not add mesoporous Pt nano-particle
Three-dimensional porous Graphene, illustrates that the porous graphene chemical property of three dimensional structure is substantially better than two dimension general
Logical Graphene, and due to the difference function between different nano materials and synergism, mesoporous Pt
The addition of nano-particle then can improve the chemical property of three-dimensional grapheme further.
D. the sensitive membrane that a. prepares is dropped on the electrode that c. prepares, and the most naturally wave
Send out 6h, i.e. obtain the solid contact polymeric film cadmium ion electrodes selective prepared.
Embodiment 2
Before use should be first 10 by the above-mentioned electrode acquired-3M cadmium nitrate solution activates one day,
The most again 10-9M cadmium nitrate solution activates two days.
The electrode activated is sequentially inserted into (nitric acid in the cadmium nitrate solution containing a series of variable concentrations
Cadmium solution concentration is respectively 10-3, 10-4, 10-5, 10-6,10-7, 10-8, 10-9, 10-10, 5 × 10-11Mol/L),
Produce potential response signal (seeing Fig. 3).
As seen from Figure 3, the solid being solid contact layer with porous graphene/mesoporous Pt composite construction connects
Touch polymeric film cadmium ion electrodes selective has the sensitiveest potential response, finally can detect that 10-10
The concentration of cadmium ions of mol/L, and current potential is 10-3-10-9Presenting in the range of mol/L can this special response.
Be can detect that by the solid contact polymeric film cadmium ion electrodes selective of the above-mentioned visible present invention
10-10The concentration of cadmium ions of mol/L, and 10-3mol/L-10-9Mol/L concentration of cadmium ions model
This special response of good energy is presented in enclosing.
Embodiment 3
Difference from Example 1 is:
A. three-dimensional porous Graphene/mesoporous Pt composite construction is prepared: GO solution and mesoporous Pt nanometer
The preparation process of granule is carried out with reference to embodiment 1 step b.By the centrifugal mesoporous Pt nano-particle obtained
It is dissolved in the GO solution of 40mL 2mg/mL, ultrasonic makes its mix homogeneously, be then placed in 50mL's
In politef reactor, 180 DEG C of reaction 3h in drying baker, remove water after having reacted, cold
Dry two days of lyophilizing, i.e. obtains required three-dimensional porous Graphene/mesoporous Pt composite construction.
B. remaining implements step reference embodiment 1 step c, and d and embodiment 2 are carried out, and can obtain solid
Contact polymeric film cadmium ion electrodes selective measures 10-3-10-10The potential change of M cadmium nitrate solution
Response.
Embodiment 4
Difference from Example 1 is: a. prepares porous graphene/mesoporous Pt composite construction: GO
The preparation process of solution and mesoporous Pt nano-particle is carried out with reference to embodiment 1 step b.Will be centrifugal
To mesoporous Pt nano-particle be dissolved in the GO solution of 40mL 2.5mg/mL, ultrasonic make it mix
Uniformly, it is then placed in the politef reactor of 50mL, 180 DEG C of reaction 3h in drying baker,
Remove water, lyophilization two days after having reacted, i.e. obtain required three-dimensional porous Graphene/mesoporous
Pt composite construction.
B. remaining implements step reference embodiment 1 step c, and d and embodiment 2 are carried out, and can obtain solid
Contact polymeric film cadmium ion electrodes selective measures 10-3-10-10The potential change of M cadmium nitrate solution
Response.
Embodiment 5
Difference from Example 1 is: a. drop coating porous graphene/mesoporous Pt composite construction: take
Porous graphene synthesized by 3mg/mesoporous Pt composite construction first with mortar grinder, after be scattered in 1mL
In water, it is made into the dispersion liquid of 3mg/mL.Take 5 μ L solution and drip on glass-carbon electrode, shine with infrared lamp
Penetrate and make aqueous solution evaporate, it is possible to obtain uniform porous graphene/mesoporous Pt in glassy carbon electrode surface multiple
Close structure conduction layer.
B. remaining enforcement step is carried out with reference to embodiment 1 step d and embodiment 2, can obtain solid
Contact polymeric film cadmium ion electrodes selective measures 10-3-10-10The potential change of M cadmium nitrate solution
Response.
Embodiment 6
Difference from Example 1 is:
A. drop coating porous graphene/mesoporous Pt composite construction: take the porous graphene synthesized by 3mg/
Mesoporous Pt composite construction first with mortar grinder, after be scattered in 1mL water, be made into 3mg/mL point
Dissipate liquid.Take 15 μ L solution and drip on glass-carbon electrode, irradiate with infrared lamp and make aqueous solution evaporate, it is possible to
Uniform porous graphene/mesoporous Pt composite construction conducting shell is obtained in glassy carbon electrode surface.
B. remaining enforcement step is carried out with reference to embodiment 1 step d and embodiment 2, can obtain solid
Contact polymeric film cadmium ion electrodes selective measures 10-3-10-10The potential change of M cadmium nitrate solution
Response.
Embodiment 7
Difference from Example 1 is:
A. drop coating porous graphene/mesoporous Pt composite construction: take the porous graphene synthesized by 3mg/
Mesoporous Pt composite construction first with mortar grinder, after be scattered in 1mL water, be made into 3mg/mL point
Dissipate liquid.Take 20 μ L solution and drip on glass-carbon electrode, irradiate with infrared lamp and make aqueous solution evaporate, it is possible to
Uniform porous graphene/mesoporous Pt composite construction conducting shell is obtained in glassy carbon electrode surface.
B. remaining enforcement step is carried out with reference to embodiment 1 step d and embodiment 2, can obtain solid
Contact polymeric film cadmium ion electrodes selective measures 10-3-10-10The potential change of M cadmium nitrate solution
Response.
Claims (10)
1. a solid contact polymeric film cadmium ion electrodes selective, it is characterised in that: many to have
The three-dimensional grapheme of pore structure/mesoporous Pt is as solid contact polymeric film cadmium ion electrodes selective
Ionic-electronic conduction layer, and with sensitive membrane on ionic-electronic conduction layer.
2. the solid contact polymeric film cadmium ion electrodes selective as described in claim 1, it is special
Levy and be: the method synthesis that described ionic-electronic conduction layer uses a step hydro-thermal to assemble altogether.
3. the solid contact polymeric film cadmium ion electrodes selective as described in claim 2, it is special
Levy and be: described ionic-electronic conduction layer is prepared as:
1) graphene oxide (GO) is substantially soluble in water obtains GO solution, stand-by；
2) by potassium chloroplatinite (K2PtCl4) it is substantially soluble in water to obtain K2PtCl4Solution, simultaneously will be poly-
Ethylene glycol cetyl ether (Brij 58) makes it be completely dissolved, and adds ascorbic acid solution after dissolving
Until solution becomes black, dark solution is centrifuged to obtain black precipitate, is mesoporous Pt nano-particle；
3) mesoporous for above-mentioned acquisition Pt nano-particle is dissolved in step 1) in GO solution, ultrasonic make it
Mix homogeneously, during mixed liquor is placed in reactor after mixing, reacts in drying baker, goes after having reacted
Except water, lyophilization, i.e. obtain required three-dimensional porous Graphene/mesoporous Pt composite construction.
4. the solid contact polymeric film cadmium ion electrodes selective as described in claim 3, it is special
Levy and be: described step 1) in GO solution the content of GO be 2-3mg/mL.
5. the solid contact polymeric film cadmium ion electrodes selective as described in claim 3, it is special
Levy and be: described step 2) in K2PtCl4K in solution2PtCl4Content be 8-10mg/mL；Black
In solution, Polyethylene Glycol cetyl ether contains for 5-6mg/mL；In dark solution, ascorbic acid content is
8-10mg/mL。
6. the solid contact polymeric film cadmium ion electrodes selective as described in claim 3, it is special
Levy and be: described step 3) mixed liquor is placed in politef reactor, dry in 160-180 DEG C
Dry case reacts 3-4h, removes water, lyophilization two days after having reacted, i.e. obtain required three
Dimension porous graphene/mesoporous Pt composite construction.
7. the solid contact polymeric film cadmium ion electrodes selective as described in claim 1, it is special
Levy and be: be dispersed in water after three-dimensional porous Graphene/mesoporous Pt composite construction is ground, take dispersion
Rear solution drips on glass-carbon electrode, irradiates with infrared lamp and makes aqueous solution evaporate, obtains uniform ion-electricity
Sub-conducting shell.
8. the solid contact polymeric film cadmium ion electrodes selective as described in claim 7, it is special
Levy and be: after described dispersion, solution concentration is 2-3mg/mL.
9. the system of the solid contact polymeric film cadmium ion electrodes selective described in a claim 1
Preparation Method, it is characterised in that: the method synthesis utilizing a step hydro-thermal to assemble altogether has the stone of loose structure
Ink alkene/mesoporous Pt composite construction, passes composite construction drop coating to glassy carbon electrode surface as ion-electron
Conducting shell, the most again with sensitive membrane on ionic-electronic conduction layer.
10. the solid contact polymeric film cadmium ion electrodes selective described in a claim 1 should
With, it is characterised in that: described solid contact polymeric film cadmium ion electrodes selective is for a huge sum of money
Belong among the detection of cadmium ion.
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