CN102253163A - Electrochemistry continuously regenerated CO2 suppressor - Google Patents

Electrochemistry continuously regenerated CO2 suppressor Download PDF

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Publication number
CN102253163A
CN102253163A CN2010101802073A CN201010180207A CN102253163A CN 102253163 A CN102253163 A CN 102253163A CN 2010101802073 A CN2010101802073 A CN 2010101802073A CN 201010180207 A CN201010180207 A CN 201010180207A CN 102253163 A CN102253163 A CN 102253163A
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Prior art keywords
chamber
rejector
degasser
cyclic regeneration
devolatilizing
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CN2010101802073A
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Chinese (zh)
Inventor
李选培
马志斌
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East & West Analytical Instruments Inc
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East & West Analytical Instruments Inc
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Priority to CN2010101802073A priority Critical patent/CN102253163A/en
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Abstract

The invention relates to a device which is used for ion chromatographic analysis, and has an ion exchange function and an electrochemical reaction function, and discloses an electrochemistry continuously regenerated CO2 suppressor. The electrochemistry continuously regenerated CO2 suppressor comprises two suppressor external pressure plates, a suppression chamber clamped between two ion exchange membranes, an electrode chamber composed of two ion exchange membranes and two electrodes at the two sides and a CO2 degasser, wherein, the two suppressor external pressure plates are positioned at the two sides of the two electrodes; one end of the degasser is communicated with the suppression chamber, and the other end of the degasser is communicated with the electrode chamber through a conductance cell; and the two ends of the suppression chamber are in a V shape. The electrochemistry continuously regenerated CO2 suppressor provided by the invention has a small dead volume, an inter-membrane low voltage, a CO2 degassing function, high suppression capacity and stable performance, and no regeneration liquid (acid or base) needs to be filled additionally.

Description

Galvanochemistry cyclic regeneration CO＜sub〉2＜/sub〉rejector
Technical field
The present invention relates to a kind of device that is used for ion chromatography, be specifically related to a kind of galvanochemistry cyclic regeneration CO with ion exchanging function and electrochemical reaction function 2Rejector.
Background technology
As everyone knows, chromatography of ions has become the moon, the conventional analysis technology of cation analysis, and " rejector " played vital role therein, because in the flow system of chromatography of ions, analysans and leacheate (acid or alkali) all are just to have necessarily, the form of negative charge exists, electric conductivity detector is exactly that conductivity power according to these ions shows it respectively, but, because electric conductivity detector is to the moon, kation does not have selectivity, its detection be that total electricity of effects of ion is led, therefore, for correct the detection treated measured ion, just must be with the gegenion in the solution (to anion analysis, kation promptly is a gegenion, to cation analysis, negative ion promptly is a gegenion) remove, simultaneously, for obtaining to treat the sensitivity of measured ion, needs will be reduced to minimum from the background conductance of leacheate, and this function is called " inhibition " in chromatography of ions, and the device with this function is called as rejector.The performance of rejector directly influences the analysis result of chromatography of ions, and wherein background conductance is one of important technical parameter of its performance of reflection, and unit is μ S/cm (every centimetre of little Siemens).
At present, existing multiple commercial rejector, as Chinese patent application number be 85102998 and publication number be disclosed continuous regenerative ion exchange column in 1033109, all be to constitute by two amberplexes to suppress chamber (volume is 5ml), the opposite side of two amberplexes is respectively anode chamber and cathode chamber, in anode chamber and cathode chamber, be provided with electrode and be used to support the sponge plastics or the ceramic wafer of amberplex, and filled acid or alkali regenerative agent as amberplex.According to the electrodialysis principle, under the double action of electric field and amberplex, ion is made directional migration and is optionally seen through amberplex, thereby makes leacheate be converted into the form (H that low electricity is led 2O or H 2CO 3).And the U.S. wears SRS (self-regenerationsuppressor) rejector of peace (DIONEX), different with above-mentioned two kinds of devices: it is to be respectively equipped with in anode chamber and the cathode chamber platinum plating POROUS TITANIUM PLATE, plays the supporting role of electrode, flow passage and film.This device has been eliminated above-mentioned two kinds of devices because the mensuration that the thermal effect of using the intermembranous overtension of insulation porous material enable to bring causes is disturbed, and also need not to fill regenerated liquid (acid or alkali), make produce more convenient, use safety and reliability, life-span longer.
Yet above-mentioned rejector does not possess CO 2Degassing function is though in the anion analysis of using the carbonate leacheate, carbonate is converted into light current and hangs down the H that electricity is led from promptly after suppressing 2CO 3Form, but than H 2O (experimental water of chromatography of ions is the deionized water of conductivity less than 1 μ S/cm), its conductivity still higher (being generally about 15 μ S/cm), secondly, H 2CO 3In the conductance cell that volume for stream increases suddenly, might separate out CO 2Gas, this will produce serious the interference to measuring.In above-mentioned SRS rejector, adopted the method for back-pressure pipe to stop CO 2Separating out of gas, but because this method has increased the pressure that rejector bears, thereby also increased the possibility of rejector leakage, in addition, the conductivity of solution is subjected to Temperature Influence bigger, H 2CO 3Existence, baseline will be fluctuateed with variation of temperature, simultaneously baseline noise also increases thereupon, and stability and the sensitivity of measuring is had a negative impact.And can't realize the gradient elution of carbonate system.
Summary of the invention
The purpose of this invention is to provide little, the intermembranous voltage of a kind of dead volume low, need not additionally to fill regenerated liquid (acid or alkali), have CO 2The degassing function, the gradient elution that can realize carbonate system, inhibition capacity are big, the galvanochemistry cyclic regeneration CO of stable performance 2Rejector.
The technical scheme of taking for the present invention that achieves the above object is:
A kind of galvanochemistry cyclic regeneration CO of the present invention 2Rejector, the electrode chamber, the CO that comprise two rejector outer plates, be clipped in inhibition chamber in the middle of two amberplexes, form between two electrodes of two amberplexes and both sides 2Degasser, described two rejector outer plates are positioned at the both sides of two electrodes, and degasser one end is communicated with the inhibition chamber, and the other end is communicated with electrode chamber by conductance cell, and two ends, described inhibition chamber are " V " font.
Wherein, indoor filling anion exchange resins of described inhibition or Zeo-karb are perhaps filled anion-exchange fibre or cation exchange fibre.
Wherein, described CO 2One end of degasser exports by its devolatilizing chamber inlet and leacheate on the outer plate and is communicated with CO 2The other end of degasser is communicated with the regenerated liquid inlet by conductance cell with its devolatilizing chamber outlet.
Wherein, described CO 2Degasser is by four CO 2Devolatilizing chamber, four CO 2The degassing film pipe is formed, and four degassing film pipes lay respectively at four CO 2In the devolatilizing chamber, described four CO 2Devolatilizing chamber adopts the PEEK material.
Wherein, described CO 2Pressure in the devolatilizing chamber chamber is less than 1.37 mm Hg.
Wherein, described CO 2The degassing film pipe adopts Teflon AF material.
Wherein, the dead volume of described inhibition chamber is less than 60 μ l.
Wherein, described electrode is that the aperture is the platinum plating POROUS TITANIUM PLATE of 0.1-0.3mm.
Advantage of the present invention is as follows:
1, voltage is low between little, the amberplex of dead volume;
2, need not additionally to fill regenerated liquid (acid or alkali);
3, has CO 2Degassing function, big, the stable performance of inhibition capacity.
Description of drawings
Fig. 1 is the synoptic diagram of inner structure of the present invention;
Fig. 2 is that the present invention is used for the principle schematic that anion chromatographic is analyzed;
Fig. 3 is the principle schematic that the present invention is used for cation analysis.
1 suppresses supporter 4 rejector outer plate 5 electrodes, 6 ion exchange resin of chamber 2 amberplexes, 3 films or ion-exchange fibre 7 leacheates 8 leacheates that enter the mouth exports 9 regenerated liquids, 10 waste liquid outlets, 11 devolatilizing chambers, 12 degassing film pipes, 13 devolatilizing chambers, 14 devolatilizing chambers that enter the mouth that enter the mouth and exports 15 negative electrodes, 16 anodes, 17 cation-exchange membranes, 18 cation exchange fibre 20CO 2Exhausr port 23 anion-exchange fibres 24 anion-exchange membranes 25 conductance cells.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
A kind of galvanochemistry cyclic regeneration CO of the present invention 2Rejector, by two electrode chambers that are clipped in inhibition chamber 1 in the middle of two amberplexes 2 and two amberplex 2 opposite sides and with four that suppress that chamber 1 links to each other CO independently 2Degasser constitutes.The dead volume that suppresses chamber 1 is less than 60 μ l, suppressing chamber 1 is made by teflon, indoor filling anion exchange resins or Zeo-karb, also can fill anion-exchange fibre or cation exchange fibre, electrode chamber or be called regeneration passage the electrode 5 that the platinum plating POROUS TITANIUM PLATE is made is housed, its aperture 0.1-0.3mm, opposite through the liquid flow path direction of regeneration passage with inhibition chamber 1 liquid flow path direction, four CO independently 2CO in the degasser 2Devolatilizing chamber 13 is made by the PEEK material, four CO independently 2It is the CO of 100 μ l that the volume of being made by Teflon AF material is housed respectively in the devolatilizing chamber 13 2Degassing film pipe 12.
Referring to Fig. 1, leacheate and sample mix solution enter the inlet 7 on the rejector outer plate 4, flow into the inhibition chamber 1 of making by PTFE with the direction of arrow, suppress to have filled ion exchange resin or ion-exchange fibre 6 in the chamber 1, leacheate after suppressing is flowed out by outlet 8 with the direction of arrow, enters four independences and the continuous CO that is made by the PEEK material through the inlet 11 of degas passage then 2Devolatilizing chamber 13, CO 2TeflonAF CO is housed in the devolatilizing chamber 13 2Degassing film pipe 12, each CO 2CO in the devolatilizing chamber 2The degassing film pipe volume is 100 μ l, leacheate and sample mix solution after the degassing enter conductance cell 25 through exporting 14, the regenerated liquid that the solution that is flowed out by conductance cell 25 is recycled on the rejector outer plate 4 enters the mouth 9, as the regenerated liquid process electrode (platinum plating POROUS TITANIUM PLATE) 5 of film, discharge by waste liquid mouth 10 at last.
Referring to Fig. 2, as with Na 2CO 3+ NaHCO 3When carrying out anion analysis, together enter from the sample NaX of anion separation column and leacheate and to suppress chamber 1, following reaction takes place with wherein cation exchange fibre 18 as leacheate:
(1)2R-H+Na 2CO 3→2R-Na+H 2CO 3
(2)R-H+NaHCO 3→R-Na+H 2CO 3
(3)R-H+NaX→R-Na+HX
Subsequently, H 2CO 3Together enter degassing film pipe 12 with sample HX, and following reaction take place:
(4)H 2CO 3→CO 2↑+H 2O
CO in the equation (4) 2By CO 2Exhausr port 20 is discharged.
From above-mentioned reaction as can be seen, leacheate be converted into light current from H 2CO 3After, the overwhelming majority is with CO 2Form discharge, make background conductance approach H 2O, and sample is converted into the form of acid by the form of salt, has strengthened its conductance signal greatly, thereby has improved detection sensitivity (H +Limiting molar is the highest in all kations, is 350 μ S/cm, and Na +Limiting molar only is 50 μ S/cm).
In addition, be circulated to the H of regeneration passage (electrode chamber) by conductance cell 2Following reaction, take place in O therein:
(5)2H 2O→4H ++O 2↑+4e
(6)2H 2O+2e→2OH -+H 2↑
H in the equation (5) +Under the double action of electric field and cation-exchange membrane 17, enter and suppress chamber 1, cation-exchange membrane 17 is added under the situation of regenerated liquid (acid) need not, forever regenerated, and the OH in the equation (6) -With Na from the inhibition chamber +In conjunction with, generate NaOH (entering waste liquid), kept charge balance.
Referring to Fig. 3, when carrying out cation analysis as leacheate, together enter from the sample (is example with NaX) and the leacheate of cation separation post and to suppress the chamber with Loprazolam (MSA), following reaction takes place with wherein anion-exchange fibre 23:
(7)R-OH+MSA→R-MSA+H 2O
(8)R-OH+NaX→R-X+NaOH
By above-mentioned reaction as can be seen, leacheate is converted into H by the Loprazolam of dense ionization 2O, and sample is converted into the form of corresponding alkali with the form of salt, has strengthened its conductance signal greatly, thereby has improved detection sensitivity (OH -Limiting molar is the highest in all negative ion, is 198 μ S/cm).
In addition, be circulated to the H of regeneration passage (electrode chamber) by conductance cell 2The reaction of equation (7) and equation (8) takes place respectively in O therein, wherein the OH in the equation (8) -Under the double action of electric field and anion-exchange membrane 24, enter and suppress the chamber, anion-exchange membrane 24 is added under the situation of regenerated liquid (alkali) need not, forever regenerated, and the H in the equation (7) +With Loprazolam root and X from the inhibition chamber -In conjunction with, generate corresponding acid (entering waste liquid), kept charge balance.At last, sample solution is removed wherein through degassing film pipe (as shown in Figure 1) and is entered detecting device behind the dissolved gases.
Described PEEK is a polyether-ether-ketone resin, is a kind of special engineering plastics of excellent performance.Described Teflon AF is a high performance Teflon fluorocarbon resin of new generation.Complete amorphous TeflonAF has many outstanding advantages, as the complete transparency in 190nm thickness, and low-refraction (1.29～1.31); Outstanding dielectric properties (in plastics family, having minimum specific inductive capacity); The good mechanical performance; The thermal behavior of wide warm area and excellent in chemical inertia reach restricted dissolubility or the like in selected perfluorinated solvents.TeflonAF is with a wide range of applications in high-tech area.As being used as in the important materials aspect optical fiber and the integrated optics semiconductor and process materials, dielectric and releasable material, the chemical industrie material of property and biomedical material etc.
Experiment condition and result
As shown in Figure 1, suppress chamber 1 and make, for reducing dead volume by teflon, two ends should be " V " font, indoor filling ion-exchange resin, for guaranteeing the chromatographic performance of rejector, the amount of the ion exchange resin of filling in the inhibition chamber should be able to produce the back-pressure of 0.7-1.0MPa.Condition of work and result are as follows:
Anion analysis
Leacheate: 1.8mmol/L Na 2CO 3+ 1.7mmol/L NaHCO 3
Flow: 2.0ml/min
Electric current: 30mA
Background conductance before the degassing: 12.82 μ S/cm
Degassing rear backdrop electricity is led: 2.03 μ S/cm
Cation analysis
Leacheate: 4.0mmol/L MSA (Loprazolam)
Flow: 1.5ml/min
Electric current: 20mA
Background conductance before the degassing: 0.36 μ S/cm
Degassing rear backdrop electricity is led: 0.14 μ S/cm
When the present invention works:
A is converted into the form that corresponding light current is led from low electricity by ion-exchange and electrochemical reaction dual-use function with leacheate.
The H that b is produced by brine electrolysis +(hydrogen ion) and OH -(hydroxide ion) finishes the automatic cyclic regeneration of amberplex.
C passes through CO 2Degasser is with the H of inhibitory reaction generation 2CO 3With CO 2Form remove, simultaneously dissolved gases in the water is removed.
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be qualification to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.

Claims (8)

1. galvanochemistry cyclic regeneration CO 2Rejector is characterized in that: the electrode chamber, the CO that comprise two rejector outer plates, be clipped in inhibition chamber in the middle of two amberplexes, form between two electrodes of two amberplexes and both sides 2Degasser, described two rejector outer plates are positioned at the both sides of two electrodes, and degasser one end is communicated with the inhibition chamber, and the other end is communicated with electrode chamber by conductance cell, and two ends, described inhibition chamber are " V " font.
2. a kind of galvanochemistry cyclic regeneration CO according to claim 1 2Rejector is characterized in that: indoor filling anion exchange resins of described inhibition or Zeo-karb, perhaps fill anion-exchange fibre or cation exchange fibre.
3. a kind of galvanochemistry cyclic regeneration CO according to claim 1 2Rejector is characterized in that: described CO 2One end of degasser exports by its devolatilizing chamber inlet and leacheate on the outer plate and is communicated with CO 2The other end of degasser is communicated with the regenerated liquid inlet by conductance cell with its devolatilizing chamber outlet.
4. a kind of galvanochemistry cyclic regeneration CO according to claim 1 2Rejector is characterized in that: described CO 2Degasser is by four CO 2Devolatilizing chamber, four CO 2The degassing film pipe is formed, and four degassing film pipes lay respectively at four CO 2In the devolatilizing chamber, described four CO 2Devolatilizing chamber adopts the PEEK material.
5. a kind of galvanochemistry cyclic regeneration CO according to claim 4 2Rejector is characterized in that: described CO 2Pressure in the devolatilizing chamber chamber is less than 1.37 mm Hg.
6. a kind of galvanochemistry cyclic regeneration CO according to claim 4 2Rejector is characterized in that: described CO 2The degassing film pipe adopts the TeflonAF material.
7. a kind of galvanochemistry cyclic regeneration CO according to claim 1 2Rejector is characterized in that: the dead volume of described inhibition chamber is less than 60 μ l.
8. a kind of galvanochemistry cyclic regeneration CO according to claim 1 2Rejector is characterized in that: described electrode is that the aperture is the platinum plating POROUS TITANIUM PLATE of 0.1-0.3mm.
CN2010101802073A 2010-05-18 2010-05-18 Electrochemistry continuously regenerated CO2 suppressor Pending CN102253163A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN102735792A (en) * 2012-07-13 2012-10-17 青岛盛瀚色谱技术有限公司 Resin filling type ion chromatography electrolysis self-regeneration suppressor
CN104020226A (en) * 2014-05-16 2014-09-03 安徽皖仪科技股份有限公司 Apparatus with improved CO2 inhibiting performance and special for ion chromatograph instruments and method for improving CO2 inhibiting performance of apparatus
CN104237450A (en) * 2014-09-30 2014-12-24 华南理工大学 Multifunctional ion chromatography suppressor for cations and anions
CN104569280A (en) * 2013-10-18 2015-04-29 戴安公司 Multielectrode electrolytic device and method
CN105259279A (en) * 2015-11-25 2016-01-20 华东理工大学 Ion chromatography suppressor-charge detector integrated device
CN108254415A (en) * 2018-03-06 2018-07-06 西安西热电站化学科技有限公司 A kind of hydrogen conductivity measuring system

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102735792A (en) * 2012-07-13 2012-10-17 青岛盛瀚色谱技术有限公司 Resin filling type ion chromatography electrolysis self-regeneration suppressor
CN102735792B (en) * 2012-07-13 2014-08-13 青岛盛瀚色谱技术有限公司 Resin filling type ion chromatography electrolysis self-regeneration suppressor
CN104569280A (en) * 2013-10-18 2015-04-29 戴安公司 Multielectrode electrolytic device and method
US9625430B2 (en) 2013-10-18 2017-04-18 Dionex Corporation Multielectrode electrolytic device and method
CN104569280B (en) * 2013-10-18 2017-06-30 戴安公司 Multi-electrode electrolysis unit and method
CN104020226A (en) * 2014-05-16 2014-09-03 安徽皖仪科技股份有限公司 Apparatus with improved CO2 inhibiting performance and special for ion chromatograph instruments and method for improving CO2 inhibiting performance of apparatus
CN104020226B (en) * 2014-05-16 2016-05-04 安徽皖仪科技股份有限公司 The special CO of a kind of ion chromatograph2TVS performance raising method and device
CN104237450A (en) * 2014-09-30 2014-12-24 华南理工大学 Multifunctional ion chromatography suppressor for cations and anions
CN105259279A (en) * 2015-11-25 2016-01-20 华东理工大学 Ion chromatography suppressor-charge detector integrated device
CN108254415A (en) * 2018-03-06 2018-07-06 西安西热电站化学科技有限公司 A kind of hydrogen conductivity measuring system

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Application publication date: 20111123