CN106198844A - A kind of utilize Graphene as the ion chromatographic eliminator of proton transport passage - Google Patents
A kind of utilize Graphene as the ion chromatographic eliminator of proton transport passage Download PDFInfo
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- CN106198844A CN106198844A CN201610527747.1A CN201610527747A CN106198844A CN 106198844 A CN106198844 A CN 106198844A CN 201610527747 A CN201610527747 A CN 201610527747A CN 106198844 A CN106198844 A CN 106198844A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
- G01N2030/965—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange suppressor columns
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Abstract
The invention discloses a kind of utilize Graphene as the ion chromatographic eliminator of proton transport passage, including positive pole porous platinum electrode sheet；The proton-conductive films built based on Graphene, its upper surface is pressed into contact with positive pole porous platinum electrode sheet lower surface；Anode regenerated liquid supports screen, is arranged between positive pole porous platinum electrode sheet and proton-conductive films；Leacheate supports screen, and its upper surface is pressed into contact with proton-conductive films lower surface；Cation exchange membrane, its upper surface and leacheate support screen lower surface and are pressed into contact with；Negative pole porous platinum electrode sheet, its upper surface is pressed into contact with cation exchange membrane lower surface；Cathode regenerative liquid supports screen, is arranged between negative pole porous platinum electrode sheet and cation exchange membrane.The present invention utilizes Graphene to carry out the hydrion exchange of suppressor anode region as proton exchange medium, it is possible to the suppression efficiency of suppressor is greatly improved.
Description
Technical field
The present invention relates to chromatography of ions fields of measurement, a kind of utilize Graphene as the ion of proton transport passage
Chromatographic eliminator.
Background technology
Ion chromatography is one of most important three big chromatographic separation technologies.Along with becoming increasingly popular of chromatographic technique, just
Gradually it is applied to every field, has become as inorganic anion and the cation analysis means of routine at present, and also apply
In the qualitative of organic molecule or quantitative analysis, such as organic acid, organic amine, aminoacid etc..Due to most of ionization thing
Matter can occur ionization to produce conductance in the solution, and electrical conductivity is corresponding to the concentration of ion.So the mensuration of electrical conductivity has become as
The quantitative analysis method of topmost solion.But problem is not only to treat that measured ion has a conductance, and general leacheate itself
Also there is high conductance, produce strong background conductance, treat that the conductance signal of measured ion can be annihilated, greatly have impact on the standard of detection
Really property and detectable limit.Then people attempt suppressing the background conductance that chromatography of ions is high, effectively solve this and ask
Topic.
Develop into today, one of suppression system core component having become as chromatography of ions.The quality of suppressor is related to
The baseline stability of chromatography of ions instrument system, the key index such as repeatability and detection sensitivity.The Main Function of suppressor is fall
The detection sensitivity of measured ion is treated in the background conductance of low leacheate and raising.First, (as a example by anion) change sample cloudy from
Son is corresponding acid, and owing to hydrionic limiting molar is 7 times of other cationes, substantially increases and surveyed the moon
The detection sensitivity of ion.Second, it is the most weak acid (carbonic acid) or water by leacheate ion transit so that it is detection sensitivity is significantly
Reduce.Both the above effect improves signal to noise ratio simultaneously, greatly improves the detection sensitivity of the chromatography of ions.
Fig. 1 is the chromatography of ions Cleaning Principle figure using background conductance suppressing method.As a example by Anionic recognition, treat test sample
Product enter chromatographic column with leacheate and separate.Leacheate is sodium carbonate (or sodium bicarbonate or NaOH).Go out from chromatographic column
The testing sample that separated of solution come and the mixed solution of leacheate.Eluent concentration is higher also has high electrical conductivity,
The usual concentration of ion to be measured is relatively low, and corresponding electrical conductivity is the highest, directly this mixed solution is carried out Conductivity detection, the color obtained
Spectrogram often baseline is the highest, and the chromatographic peak treating measured ion being superimposed upon on baseline easily reaches the saturated electric conductivity value of detector, leads
Cause measure inaccurate, high background conductance makes noise amplify the most in proportion, cause concentration the lowest treat that measured ion is difficult at Gao Ji
In line conductance measured accurately.Fig. 2 is the contrast of the chromatogram that Direct Conductivity detection obtains with Suppressor conductivity detection.
The principle of this suppression background of suppressor and amplification measured signal achieves ion exchange in being suppressor, as
Shown in Fig. 3, being converted into hydrion after the sodium ion in leacheate and the inhibited device of the anionic current in sample, carbonate becomes
Carbonic acid, background conductance is the most significantly lowered, and treats that measured ion and hydrion are combined into strong acid, ionic conductivity quilt to be measured simultaneously
Amplify.The principle of cation suppressor is similar to, and simply the anion of background is exchanged by hydroxyl.What Fig. 3 represented is based on ion
The electrolysis suppressor schematic diagram of exchange (document chromatography of ions instrument, Zhu Yan, Chemical Industry Press, 2006), suppressor is deposited
At three passages, be two regenerated liquid passages and a leacheate passage respectively, after powering up under the driving of electromotive force positive and negative electrode
Producing water electrolysis reaction, positive pole produces hydrion and oxygen, and negative pole produces hydroxide ion and hydrogen, and hydrion passes through cation
Exchange membrane enters leacheate passage, has the sodium ion of same charge to enter negative pole district by cation exchange membrane, it is achieved to drench simultaneously
Washing liquid background conductance suppression function.
By to be electrolysed based on ion exchange suppressor principles and methods it can be seen that cathode chamber proton (i.e. hydrogen from
Son) performance of exchange membrane has decisive meaning to the inhibition of suppressor.Actual application requires that PEM is not
Only have the highest proton conductivity, but also remaining cation in passage can effectively be shielded, the most only allow proton by and
Water and other cation is stoped to be passed through.The most also there is higher chemical stability, heat stability and enough mechanical strengths
(resistant to liquid pressure).The most the most frequently used PEM is the Nafion membrane of E.I.Du Pont Company.Its subject matter is to exist except matter
The infiltration problem of son remaining cation outer, i.e. selective penetrated property is bad.Suppressor requires that only hydrion leads under certain electric current
Cross, to neutralize the hydroxyl in leacheate and the conductance of measured ion is treated in amplification.Other ions outside if there is proton free
Infiltration, then the efficiency of reduction suppressor that can be the biggest.It is to reach same inhibition can only strengthen further when generally using
Electric current, thus produce the series of problems such as device heating, membrane poisoning.In addition to minimizing fuel infiltration, it has to increase proton
The thickness of conductive membranes, but proton conductivity declines the most therewith.
Graphene (Graphene) is as a kind of most typical two dimensional crystal material, since within 2004, being invented, respectively
Individual field has obtained paying close attention to widely, becomes science and the focus of engineering field research.It it is the two dimension of Graphene as shown in Fig. 4
Structure and utilize Colloidal particles (document ultracapacitor based on Graphene and the lithium sulfur of Graphene that transmission electron microscope photographed
Battery preparation and performance study, thesis for the doctorate in 2014, Yang Xi, Nankai University).Its feature is at carbon atom two dimensional surface
On according to hexagon network structure arrange, the thickness of only one of which atomic layer on the direction be perpendicular to this two dimensional surface
(0.335nm), be equivalent to a hair 200,000/.The structure of Graphene is highly stable, and the connection of carbon-carbon bond is the most pliable and the toughest
(bond distance 1.42), the carbon atom face meeting flexural deformation when external force puts on Graphene so that carbon atom need not be rearranged to fit
Answer external force, thus keep Stability Analysis of Structures (defect will not be produced).It is outstanding that this stable lattice structure makes Graphene have
Heat conductivity.The heat conductivity of Graphene is up to 5300W/ (m*k), higher than CNT and diamond.Electronics is in track simultaneously
Time mobile, will not scatter because of lattice defect or introducing foreign atom, make Graphene have high electric conductivity.Its resistance
Rate is 10^-6 Ω * cm, lower than copper or silver, is the room temperature material that resistivity is minimum in the world.
Summary of the invention it is an object of the invention to provide and a kind of utilizes Graphene to press down as the chromatography of ions of proton transport passage
Device processed, the problem low to solve prior art suppressor suppression efficiency.
In order to achieve the above object, the technical solution adopted in the present invention is:
A kind of utilize Graphene as the ion chromatographic eliminator of proton transport passage, it is characterised in that: including:
Positive pole porous platinum electrode sheet；
The proton-conductive films built based on Graphene, its upper surface is pressed into contact with positive pole porous platinum electrode sheet lower surface；
Anode regenerated liquid supports screen, is arranged between positive pole porous platinum electrode sheet and proton-conductive films, and this anode regenerated liquid props up
Support screen is screen net structure, and anode regenerated liquid supports in screen and is provided with anode regenerated liquid passage, and anode regenerated liquid passage two ends are divided
Lian Jie not have and all be exported by the regenerated liquid entrance of positive pole porous platinum electrode sheet, regenerated liquid, regenerated liquid enters from regenerated liquid entrance
Anode regenerated liquid passage, finally flows out from regenerated liquid outlet, forms anode regenerated liquid stream；
Leacheate supports screen, and it is that scion grafting has the stereo silk-screen structure of ionic functional group and can conduct electricity, leacheate supporting network
Shielding its upper surface to be pressed into contact with proton-conductive films lower surface, leacheate supports in screen and is provided with leacheate passage, and leacheate leads to
Two ends, road are connected to leacheate entrance, leacheate outlet, the testing sample ion separated flowed out from chromatographic column and pouring
The mixed liquor of washing liquid, after leacheate entrance enters leacheate passage, finally flows out from leacheate outlet, forms drip washing liquid stream
Road；
Cation exchange membrane, its upper surface and leacheate support screen lower surface and are pressed into contact with, and cation exchange membrane is available for sun
Ion passes through；
Negative pole porous platinum electrode sheet, its upper surface is pressed into contact with cation exchange membrane lower surface；
Cathode regenerative liquid supports screen, is arranged between negative pole porous platinum electrode sheet and cation exchange membrane, this cathode regenerative liquid
Support screen is screen net structure, and cathode regenerative liquid supports in screen and is provided with cathode regenerative liquid passage, cathode regenerative liquid passage two ends
Being connected to all be exported by the regenerated liquid entrance of negative pole porous platinum electrode sheet, regenerated liquid, regenerated liquid connects from regenerated liquid entrance
After entering cathode regenerative liquid passage, finally flow out from regenerated liquid outlet, form cathode regenerative liquid stream road.
Described a kind of utilize Graphene as the ion chromatographic eliminator of proton transport passage, it is characterised in that: based on
The proton-conductive films that Graphene builds, it is the porous type proton-conductive films with SiO2 as substrate, and at substrate hole, deposition has list
Layer graphene, then forms parcel at two sides deposition Nafion material, and proton passes through Nafion medium under the effect of electric potential difference
And single-layer graphene.
Described a kind of utilize Graphene as the ion chromatographic eliminator of proton transport passage, it is characterised in that: drip washing
It is the stereo silk-screen structure that scion grafting has ionic functional group that liquid supports screen, and leacheate supports at the silk screen hole of screen cross section
Permission liquid passes through, and it is ultra-high molecular weight polyethylene that this leacheate supports the material of screen, web lines footpath 0.2-0.3mm；Silk screen
Count is 50-60 mesh.
The present invention utilizes Graphene to carry out the hydrion exchange of suppressor anode region as proton exchange medium, it is possible to significantly
Improve the suppression efficiency of suppressor.
Accompanying drawing explanation
Fig. 1 is the chromatography of ions Cleaning Principle figure using background conductance suppressing method in prior art.
Fig. 2 is the comparison diagram of the chromatogram that Direct Conductivity detection and Suppressor conductivity detection obtain in prior art.
Fig. 3 is electrolysis suppressor schematic diagram based on ion exchange in prior art.
Fig. 4 is the structure chart of Graphene, wherein:
Fig. 4 a is the two-dimensional structure figure of Graphene, and Fig. 4 b is the Colloidal particles figure of the Graphene utilizing transmission electron microscope to photograph.
Fig. 5 is the preparation process figure of proton-conductive films based on single-layer graphene in the present invention.
Fig. 6 is suppressor structure chart of the present invention.
Detailed description of the invention
As shown in Figure 6, a kind of utilize Graphene as the ion chromatographic eliminator of proton transport passage, including:
Positive pole porous platinum electrode sheet 1；
The proton-conductive films 2 built based on Graphene, its upper surface is pressed into contact with positive pole porous platinum electrode sheet 1 lower surface；
Anode regenerated liquid supports screen 3, is arranged between positive pole porous platinum electrode sheet 1 and proton-conductive films 2, this anode regenerated liquid
Supporting screen 3 is screen net structure, and anode regenerated liquid supports in screen 3 and is provided with anode regenerated liquid passage 4, anode regenerated liquid passage 4
Two ends are connected to all be exported by the regenerated liquid entrance of positive pole porous platinum electrode sheet 1, regenerated liquid, and regenerated liquid enters from regenerated liquid
Mouth enters anode regenerated liquid passage 4, finally flows out from regenerated liquid outlet, forms anode regenerated liquid stream；
Leacheate supports screen 5, and it is that scion grafting has the stereo silk-screen structure of ionic functional group and can conduct electricity, leacheate supporting network
Screen 5 its upper surfaces are pressed into contact with proton-conductive films 2 lower surface, and leacheate supports in screen 5 and is provided with leacheate passage 6, drip washing
Liquid passage 6 two ends are connected to leacheate entrance, leacheate outlet, the testing sample ion separated flowed out from chromatographic column
With the mixed liquor of leacheate, after leacheate entrance enters leacheate passage 6, finally flow out from leacheate outlet, form drip washing
Liquid stream road；
Cation exchange membrane 7, its upper surface and leacheate support screen 5 lower surface and are pressed into contact with, and cation exchange membrane 7 is available for
Cation is passed through；
Negative pole porous platinum electrode sheet 8, its upper surface is pressed into contact with cation exchange membrane 7 lower surface；
Cathode regenerative liquid supports screen 9, is arranged between negative pole porous platinum electrode sheet 8 and cation exchange membrane 7, this cathode regenerative
It is screen net structure that liquid supports screen 9, and cathode regenerative liquid supports in screen 9 and is provided with cathode regenerative liquid passage 10, and cathode regenerative liquid leads to
Two ends, road 10 are connected to all be exported by the regenerated liquid entrance of negative pole porous platinum electrode sheet 8, regenerated liquid, and regenerated liquid is from regeneration
After liquid entrance accesses cathode regenerative liquid passage 10, finally flow out from regenerated liquid outlet, form cathode regenerative liquid stream road.
The proton-conductive films 2 built based on Graphene, it is the porous type proton-conductive films with SiO2 as substrate, substrate via
At gap, deposition has single-layer graphene, then forms parcel at two sides deposition Nafion material, and proton is logical under the effect of electric potential difference
Cross Nafion medium and single-layer graphene.
It is the stereo silk-screen structure that scion grafting has ionic functional group that leacheate supports screen 5, and it is transversal that leacheate supports screen 5
Allowing liquid to pass through at the silk screen hole in face, it is ultra-high molecular weight polyethylene that this leacheate supports the material of screen 5, web lines footpath
0.2-0.3mm；Screen knitting density is 50-60 mesh.
In the present invention, as anode regenerated liquid support screen and cathode regenerative liquid support screen have with leacheate support screen
Structure.
The Wu Heng of nearest Chinese University of Science and Technology pacifies seminar and cooperates with An Deliehaimu seminar of Univ Manchester UK
(the proton transport characteristic of document Graphene class two-dimensional material, Wang Fengchao, Wu Hengan, physics, 7 phases of volume 44 (2015)；Document Hu
S, Lozada-Hidalgo M, Wang FC et al, Nature, 2014,516:227；), have studied the two-dimensional material such as Graphene
Proton transport characteristic find, under room temperature, the proton conductivity of unit plane JISHI ink alkene is about 5mS/cm^2, and single-layer silicon nitride boron
The proton conductivity of (the two-dimensional structure crystal of another kind of similar Graphene) is about 100 mS/cm^2.By to this two dimension knot
Structure crystal cloud density distribution calculating find, the most all exist cloud density relatively low " hole " (document Hu S,
Lozada-Hidalgo M, Wang FC et al, Nature, 2014,516:227；).And the electron cloud in two dimension boron nitride
Density Distribution is more sparse than Graphene, and this makes proton can pass through these holes under potential field effect, and remaining ion
But can not pass through.Further, the proton transport ability of Graphene raises the most rapidly along with the rising of temperature does not the most reduce,
When 250 DEG C, the proton conductivity of single-layer graphene is up to 1000 mS/cm^2.The Geiger team of Northwestern Univ USA have studied
Proton transport containing defective Graphene (document Achtyl JL et al, Nature Communications, 2015,6:
6539；).In aqueous, Graphene not biasing can allow substantial amounts of proton to pass through.
Can be seen that the proton transport characteristic that the two-dimension nano materials such as Graphene are outstanding, have again chemical stability good simultaneously,
The advantage such as high mechanical properties and Heat stability is good.This is so that it can substitute existing PEM, and makes proton exchange properties
Can be substantially improved, and can effectively cut off remaining cation outside oxygen, water and proton free.
Specific embodiments is as follows:
1, the preparation of the proton-conductive films of single-layer graphene
The technique not yet having large-area manufacturing due to mono-layer graphite, the present invention takes porous SiN as substrate.Aperture position covers
Double-sided deposition is carried out with Nafion medium after mono-layer graphite；Owing to Nafion has proton transport characteristic, so obtain is compound
Structure can both keep the excellent proton conduction property of Graphene, realizes again the preparation of large area film under existing technique.SiN has
There are good chemical stability and mechanical strength, are insulating barrier more common in semiconductor technology and substrate layer, photoetching can be passed through
Equally distributed porous-substrates (this is maturation process) is generated with etch process.Single-layer graphene is covered by vapour deposition process
The hole position of SiN.Then the two dimensional crystal of plus substrate makes Nafion be deposited on two dimensional crystal in placing into Nafion environment
Tow sides, form parcel.Making step is illustrated in fig. 5 shown below: 1, forms the sedimentary of two-sided SiO in silicon wafer surface, simultaneously
Coating photoresist；2, select suitable light shield to be exposed and etch, form equally distributed porous-substrates structure at SiO2 layer；3,
The etching of Si substrate；4, the development of wafer rear and etching, form pore structure；5, there is the mono-layer graphite of two dimensional crystal structure
Alkene moves to gap；6；Nafion deposits to the two sides of wafer, forms parcel.
2, Graphene proton-conductive films is utilized to carry out suppressor anode hydrogen ion transport
Proton-conductive films based on Graphene is utilized to carry out the suppressor structure of anode hydrogen ion transport as shown in Figure 6 (still with the moon
As a example by suppressor ion).This suppressor is equally based on electrochemical suppressors, utilizes electric field to produce electrolysis and the migration of ion of water
Gesture. the regenerated liquid passage of negative electrode and anode uses the thin conduction screen passed through only for gas or liquid, thus reduces suppressor
Running voltage, reduce heat produce.The hydrion that electricity anolyte water produces is under electric field action, by by single-layer graphene
The proton-conductive films made, owing to this proton-conductive films has the highest selection ratio and low operating resistance rate, hydrion obtains
With rapidly and efficiently by this layer enter leacheate passage.Cation in leacheate is then by the cation near negative electrode simultaneously
Exchange membrane enters the regenerated liquid passage of negative pole.Realize conductance by above procedure to suppress.
Claims (3)
1. one kind utilizes Graphene as the ion chromatographic eliminator of proton transport passage, it is characterised in that: including:
Positive pole porous platinum electrode sheet；
The proton-conductive films built based on Graphene, its upper surface is pressed into contact with positive pole porous platinum electrode sheet lower surface；
Anode regenerated liquid supports screen, is arranged between positive pole porous platinum electrode sheet and proton-conductive films, and this anode regenerated liquid props up
Support screen is screen net structure, and anode regenerated liquid supports in screen and is provided with anode regenerated liquid passage, and anode regenerated liquid passage two ends are divided
Lian Jie not have and all be exported by the regenerated liquid entrance of positive pole porous platinum electrode sheet, regenerated liquid, regenerated liquid enters from regenerated liquid entrance
Anode regenerated liquid passage, finally flows out from regenerated liquid outlet, forms anode regenerated liquid stream；
Leacheate supports screen, and it is the stereo silk-screen structure that scion grafting has ion-type functional group, and leacheate supports screen on it
Surface is pressed into contact with proton-conductive films lower surface, and leacheate supports in screen and is provided with leacheate passage, leacheate passage two ends
It is connected to leacheate entrance, leacheate outlet, the testing sample ion separated flowed out from chromatographic column and leacheate
Mixed liquor, after leacheate entrance enters leacheate passage, finally flows out from leacheate outlet, forms leacheate stream；
Cation exchange membrane, its upper surface and leacheate support screen lower surface and are pressed into contact with, and cation exchange membrane is available for sun
Ion passes through；
Negative pole porous platinum electrode sheet, its upper surface is pressed into contact with cation exchange membrane lower surface；
Cathode regenerative liquid supports screen, is arranged between negative pole porous platinum electrode sheet and cation exchange membrane, this cathode regenerative liquid
Support screen is screen net structure, and cathode regenerative liquid supports in screen and is provided with cathode regenerative liquid passage, cathode regenerative liquid passage two ends
Being connected to all be exported by the regenerated liquid entrance of negative pole porous platinum electrode sheet, regenerated liquid, regenerated liquid connects from regenerated liquid entrance
After entering cathode regenerative liquid passage, finally flow out from regenerated liquid outlet, form cathode regenerative liquid stream road.
The most according to claim 1 a kind of utilizing Graphene as the ion chromatographic eliminator of proton transport passage, it is special
Levy and be: the proton-conductive films built based on Graphene, it is the porous type proton-conductive films with SiO2 as substrate, substrate hole
Place's deposition has single-layer graphene, then forms parcel at two sides deposition Nafion material, and proton passes through under the effect of electric potential difference
Nafion medium and single-layer graphene.
The most according to claim 1 a kind of utilizing Graphene as the ion chromatographic eliminator of proton transport passage, it is special
Levying and be: it is the stereo silk-screen structure that scion grafting has ionic functional group that leacheate supports screen, leacheate supports screen cross section
Silk screen hole at allow liquid pass through, this leacheate support screen material be ultra-high molecular weight polyethylene, web lines footpath
0.2-0.3mm；Screen knitting density is 50-60 mesh.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111214848A (en) * | 2020-01-20 | 2020-06-02 | 青岛盛瀚色谱技术有限公司 | Ion chromatography inhibitor |
-
2016
- 2016-07-06 CN CN201610527747.1A patent/CN106198844A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111214848A (en) * | 2020-01-20 | 2020-06-02 | 青岛盛瀚色谱技术有限公司 | Ion chromatography inhibitor |
| US11808743B2 (en) | 2020-01-20 | 2023-11-07 | Qingdao Shenghan Chromatograph Technology Co., Ltd. | Ion chromatography (IC) suppressor |
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Application publication date: 20161207 |