CN104965013A - Self-compensation and pollution-resistant reference electrode - Google Patents
Self-compensation and pollution-resistant reference electrode Download PDFInfo
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- CN104965013A CN104965013A CN201510337861.3A CN201510337861A CN104965013A CN 104965013 A CN104965013 A CN 104965013A CN 201510337861 A CN201510337861 A CN 201510337861A CN 104965013 A CN104965013 A CN 104965013A
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Abstract
The invention discloses a self-compensation and pollution-resistant reference electrode which comprises a shell and a silver-silver chloride electrode arranged in the shell. The upper end of the silver-silver chloride electrode is connected with a cable while the lower portion of the same is soaked in a reference electrolyte in the shell, a liquid junction is arranged at the lower end of the shell, the reference electrolyte is mixed liquid prepared by silver chloride, potassium chloride, liquid colloid gel and distilled water, the mixed liquid is liquid colloid, solid potassium chloride which is solidified after being molten is added into the reference electrolyte, and the liquid junction is hydrophobic microporous polytef. The self-compensation and pollution-resistant reference electrode has the advantages of high long-term stability and high pollution resistance.
Description
Technical field
The present invention relates to a kind of contrast electrode, particularly relate to a kind of self compensation, anti-pollution contrast electrode.
Background technology
Contrast electrode is used in many electrochemical sensors or chain tape, and such as form potentiometric sensor with ion-selective electrode, platinum electrode etc., it has extensive utilization in laboratory and multiple industrial circle, such as petrochemical field, environmental monitoring field etc.Different according to environment for use, also not identical to the performance requirement of contrast electrode, use for laboratory contrast electrode requires that the repeatability of electrode is better; And the reference potential that industrial contrast electrode requires electrode to provide is steady in a long-term, electrodes maintenance workload is little, especially water environment on-line monitoring field, there is long-term field to measure, water quality situation is complicated, the features such as maintenance difficulties is large, requires higher to electrode long-time stability and anti-fouling performance.
Silver-silver chloride reference electrode covers one deck silver chloride on silver metal silk, and it in stable electrode potential, has stability and reversibility good, the advantages such as temperature coefficient is low in certain density electrolyte solution.Conventional silver-silver chloride reference electrode is many, and in housing, add certain density Klorvess Liquid be reference electrolyte, and connect with solution to be measured through liquid junction (porous separator), form Measure Channel, silver-silver chloride electrode one end is placed in electrolytic solution, leadout electrode current potential after the other end and wire bonds.
Existing industrial contrast electrode mainly comprises biliquid and connects form and single liquid connects form two kinds of versions, the contrast electrode that single liquid connects form does not have independently salt bridge, its reference electrolyte is connected by liquid junction with solution to be measured, as paper: Lu Bo, Zhao Jianjun etc. the contrast electrode of design in " industrial contrast electrode Developing Application ".Biliquid connects form independently salt bridge, its reference electrolyte is communicated with solution to be measured by salt bridge electrolytic solution, reference electrolyte is all connected by liquid junction with salt bridge electrolytic solution and between salt bridge electrolytic solution with solution to be measured, as paper: the contrast electrode of design in the paper " preparation of Ag/AgCl high temp. reference electrode " that Zhang Qing, Li Ping etc. deliver.
The advantages such as it is good that silver-silver chloride reference electrode has stability and reversibility, and temperature coefficient is low are a kind of good contrast electrodes, in laboratory and to be industrially all widely used.The silver-silver chloride reference electrode of prior art is generally single liquid and connects form, is made up of housing, reference electrolyte, silver-silver chloride electrode and liquid junction.Its principle is that the argent being coated with silver chloride exports in stable electrode potential in certain density chlorion electrolytic solution (normally Klorvess Liquid).Its housing can select the material be suitable for as required, as glass, teflon etc.; Silver-silver chloride electrode is usually by electrolytic process or cladding process preparation; Liquid junction is communicated with electrolytic solution and measured medium, is generally the porosints such as ceramic core; Electrolytic solution is generally certain density Klorvess Liquid.Silver-silver chloride reference electrode can be divided into use for laboratory and industry to use contrast electrode online according to environment for use, laboratory reference electrode slowly can ooze out electrolytic solution at liquid junction place usually, simultaneously, electrode body top is provided with filling opening, maintain electrolytic solution stable (as patent 94246790.6), repeatedly need add electrolytic solution during use, electrode repeatability is good but use trouble; Industrial contrast electrode often adds gel (as agar etc.) in the electrolytic solution, be solid gel, not there is mobility, electrolytic solution can be avoided to ooze out contrast electrode, and only make ion move freely, avoid the trouble of repetition liquid feeding, but because industrial electrode uses for a long time, especially water environment on-line monitoring field, in its reference electrolyte, electrolyte generation loss, causes electrode potential to drift about.In addition, because contrast electrode on-line monitoring environment is usually comparatively complicated, especially monitoring water environment field, common liq connects the very easily contaminated material attachment in boundary, causes liquid junction to block, affects sensor measurement.
Summary of the invention
For solving the deficiencies in the prior art, the object of the invention is to, provide a kind of self compensation, anti-pollution contrast electrode, this electrode has the advantages such as long-time stability are good, anti-pollution ability is strong.
Technical scheme of the present invention is: a kind of self compensation, anti-pollution contrast electrode, comprise housing and be arranged on the silver-silver chloride electrode in housing, described silver-silver chloride electrode upper end is connected with cable, described silver-silver chloride electrode bottom is immersed in the reference electrolyte in housing, the lower end of described housing is provided with liquid junction, it is characterized in that, described reference electrolyte is the formulated mixed liquor of silver chloride, potassium chloride, the agent of liquid colloidal gel and distilled water, described mixed liquor is liquid shape colloid, adds the solid potassium chloride of melting after coagulation in described reference electrolyte; Described liquid junction is hydrophobic micropore teflon.
Aforesaid a kind of self compensation, anti-pollution contrast electrode, it is characterized in that, the lower end of described housing is provided with salt bridge, the upper/lower terminal of described salt bridge is respectively equipped with internal liquid and meets boundary and outside liquid meets boundary, salt bridge electrolytic solution is provided with in described salt bridge, described salt bridge electrolytic solution is the formulated mixed liquor of potassium chloride, the agent of liquid colloidal gel and distilled water, and described mixed liquor is liquid shape colloid, and in described salt bridge electrolytic solution, add the solid potassium chloride of melting after coagulation.
Aforesaid a kind of self compensation, anti-pollution contrast electrode, is characterized in that, the below that described outside liquid meets boundary is provided with antifouling ring.
Aforesaid a kind of self compensation, anti-pollution contrast electrode, is characterized in that, it is ceramic core liquid junction that described internal liquid meets boundary, comprises internal liquid and connect boundary's pedestal and be bonded in internal liquid and connect ceramic core on boundary's pedestal.
Aforesaid a kind of self compensation, anti-pollution contrast electrode, is characterized in that, described housing upper end is provided with electrode cap.
Aforesaid a kind of self compensation, anti-pollution contrast electrode, is characterized in that, the agent of described liquid colloidal gel is high acyl gellan gum.
Aforesaid a kind of self compensation, anti-pollution contrast electrode, is characterized in that, is also provided with ion-selective electrode in described housing, and described ion-selective electrode and contrast electrode form measuring circuit.Aforesaid a kind of self compensation, anti-pollution contrast electrode, is characterized in that, in described reference electrolyte silver chloride and potassium chloride saturated, the mass ratio of the agent of liquid colloidal gel and distilled water is 0.2 ~ 10:100.
Aforesaid a kind of self compensation, anti-pollution contrast electrode, is characterized in that, in described salt bridge electrolytic solution, potassium chloride is saturated, and the mass ratio of the agent of liquid colloidal gel and distilled water is 0.2 ~ 10:100.
The beneficial effect that the present invention reaches:
1, the present invention adopts liquid shape colloidal electrolyte to be reference electrolyte, ensures that silver-silver chloride electrode fully contacts with electrolytic solution, ensures electrode measurement reliability;
2, the present invention adopts the liquid shape colloidal electrolyte of the solid potassium chloride adding melting after coagulation as salt bridge electrolytic solution or reference electrolyte, this solid potassium chloride energy auto-compensation contrast electrode measures the electrolyte of institute's loss, reduce contrast electrode drift, improve the long-time stability that it is measured;
3, the present invention adopts hydrophobic micropore teflon to be that outside liquid meets boundary, and is designed with antifouling ring, contributes to improving electrode contamination resistance, improves electrode measurement reliability.
Accompanying drawing explanation
Fig. 1 is that biliquid of the present invention connects contrast electrode structural representation;
Fig. 2 is that in Fig. 1 of the present invention, internal liquid connects boundary's structural representation;
Fig. 3 is that list liquid of the present invention connects contrast electrode structural representation;
Fig. 4 is combined electrode structure schematic diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
embodiment 1
As shown in Figure 1, for biliquid connects contrast electrode structural representation, the silver-silver chloride electrode 104 comprising housing 103 and be arranged in housing 103, described silver-silver chloride electrode 104 upper end is connected with cable 101, described silver-silver chloride electrode 104 bottom is immersed in the reference electrolyte in housing 103, described housing 103 upper end is provided with electrode cap 102, described reference electrolyte is silver chloride, potassium chloride, the agent of liquid colloidal gel and the formulated mixed liquor (agent of described liquid colloidal gel is high acyl gellan gum) of distilled water, described mixed liquor is liquid shape colloid, silver chloride and potassium chloride saturated (25 DEG C) in described reference electrolyte, the mass ratio of the agent of liquid colloidal gel and distilled water is 0.2 ~ 10:100.The solid potassium chloride of melting after coagulation is added in described reference electrolyte.
The lower end of described housing 103 is provided with salt bridge housing 106, the upper/lower terminal of described salt bridge housing 106 is respectively equipped with internal liquid and meets boundary 105 and outside liquid meets boundary 107, salt bridge electrolytic solution is provided with in described salt bridge housing 106, described salt bridge electrolytic solution is potassium chloride, the agent of liquid colloidal gel and the formulated mixed liquor (agent of described liquid colloidal gel is high acyl gellan gum) of distilled water, described mixed liquor is liquid shape colloid, in described salt bridge electrolytic solution, potassium chloride is saturated, and the mass ratio of the agent of liquid colloidal gel and distilled water is 0.2 ~ 10:100.The solid potassium chloride of melting after coagulation is added in described salt bridge electrolytic solution.
Described outside liquid meets boundary 107 for hydrophobic micropore teflon, and large-area liquid junction effectively can improve reference salt bridge and the efficiency that is communicated with of liquid to be measured, reduces resistivity, improves measuring accuracy, and the hydrophobicity of material can effectively decreasing pollution thing attachment.
The below that described outside liquid meets boundary 107 is provided with antifouling ring 108, contributes to improving electrode contamination resistance, improves electrode measurement reliability.
As shown in Figure 2, described internal liquid meets boundary 105 for ceramic core liquid junction, comprises internal liquid and connects boundary's pedestal 202 and be bonded in internal liquid and connect ceramic core 201 on boundary's pedestal 202.
Contrast electrode of the present invention meets boundary 107 by outside liquid and forms path with solution to be measured, welds rear output potential signal by cable 101 with silver-silver chloride electrode 104.
The present invention each parts preparation method and electrode assembling process as follows:
1, silver-silver chloride electrode: silver-silver chloride electrode 104 is conductors that the current potential of contrast electrode produces and exports, and makes by multiple methods such as electrolytic process.
2, reference electrolyte: reference electrolyte is the stable basis of contrast electrode.In the present invention, reference electrolyte is the formulated mixed liquor of silver chloride, potassium chloride, liquid colloidal gel agent (as high acyl gellan gum) and distilled water, and mixed liquor is liquid shape colloid, wherein potassium chloride and silver chloride saturated (25 DEG C).This electrolytic solution is liquid shape colloid, and electrolytic solution can be made fully to contact with silver-silver chloride electrode.The solid potassium chloride of melting after coagulation is added in reference electrolyte.
3, internal liquid meets boundary: internal liquid meets boundary 105 and adopts ceramic core liquid junction, ceramic core 201 and internal liquid is connect boundary's pedestal 202 bonding, as shown in Figure 2.
4, outside liquid meets boundary: outside liquid meets boundary 107 for hydrophobic micropore teflon.Large-area expanded microporous polytetra fluoroethylene-EPTEE is as liquid junction, can effectively improve liquid junction ducting capacity, reduce resistivity, improve the reliability that contrast electrode is measured, the hydrophobic performance of material effectively can reduce the adhesive ability of polluter in solution to be measured, improves electrode antifouling property.
5, salt bridge: outside liquid is connect boundary 107 and salt bridge housing 106 fluid sealant bonding, to be solidified complete after, salt bridge electrolytic solution is injected liquid junction, make liquid junction at least in part fill by electrolytic solution.Then assemble antifouling ring 108, antifouling ring 108 can effectively stop polluter to be attached on liquid junction, as attachments such as the thread algae in monitoring water environment occasion, improves the long-time stability of electrode.
6, salt bridge electrolytic solution: salt bridge electrolytic solution is the intermediate medium being communicated with reference electrolyte and liquid to be measured, formulated by potassium chloride, liquid colloidal gel agent (as high acyl gellan gum) and distilled water, is liquid shape colloid, wherein, potassium chloride saturated (25 DEG C).
7, salt bridge assembling: add appropriate salt bridge electrolytic solution in salt bridge cavity, and add the solid potassium chloride of appropriate melting after coagulation in this electrolytic solution.After completing above step, internal liquid is met boundary 105 bonding with it by fluid sealant, solidify stand-by.The solid potassium chloride of condensation after melting, in order to the electrolyte of additional survey loss, becomes block, common crystal shape potassium chloride can be avoided to be deposited on salt pars basilaris pontis, affect electrode measurement.The solid gel (solid gel is difficult to add solid potassium chloride and supplements loss electrolyte) that the reference electrolyte (or salt bridge electrolytic solution) of general industry contrast electrode is finite concentration Klorvess Liquid, along with service time extends, electrolyte meeting loss in salt bridge, and then cause reference electrolyte concentration to reduce, affect potential measurement.In the present invention, the solid potassium chloride meeting auto-compensation electrode in salt bridge electrolytic solution measures the potassium chloride of loss for a long time, makes concentration of electrolyte keep saturated, reduces the drift of electrode, improve electrode stability.
8, contrast electrode assembling: the reference salt bridge completed is connected by sealing thread with electrode shell 103, appropriate reference electrolyte is added by electrode shell 103 top after connection, again silver-silver chloride electrode 104 is fixed by fluid sealant and electrode shell 103, sealing reference electrolyte.Solidify rear assembling electrode cap 102, complete contrast electrode assembling.
embodiment 2
In the occasion that environment is not too severe, without the need to salt bridge, single liquid can be formed and connects form contrast electrode, as shown in Figure 3.Reference electrolyte is the formulated mixed liquor of silver chloride, potassium chloride, the agent of liquid colloidal gel and distilled water, mixed liquor is liquid shape colloid, in reference electrolyte, add the solid potassium chloride of melting after coagulation, liquid junction adopts expanded microporous polytetra fluoroethylene-EPTEE liquid junction.
embodiment 3
This contrast electrode, on the basis of embodiment 1, by amendment structural design mode, forms combination electrode, as ion-selective electrode 401 and contrast electrode 402 are combined into combination electrode, as shown in Figure 4.Ion-selective electrode 401 and contrast electrode 402 form measuring circuit.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and distortion, these improve and distortion also should be considered as protection scope of the present invention.
Claims (9)
1. a self compensation, anti-pollution contrast electrode, comprise housing and be arranged on the silver-silver chloride electrode in housing, described silver-silver chloride electrode upper end is connected with cable, described silver-silver chloride electrode bottom is immersed in the reference electrolyte in housing, the lower end of described housing is provided with liquid junction, it is characterized in that, described reference electrolyte is the formulated mixed liquor of silver chloride, potassium chloride, the agent of liquid colloidal gel and distilled water, described mixed liquor is liquid shape colloid, adds the solid potassium chloride of melting after coagulation in described reference electrolyte; Described liquid junction is hydrophobic micropore teflon.
2. a kind of self compensation according to claim 1, anti-pollution contrast electrode, it is characterized in that, the lower end of described housing is provided with salt bridge, the upper/lower terminal of described salt bridge is respectively equipped with internal liquid and meets boundary and outside liquid meets boundary, salt bridge electrolytic solution is provided with in described salt bridge, described salt bridge electrolytic solution is the formulated mixed liquor of potassium chloride, the agent of liquid colloidal gel and distilled water, and described mixed liquor is liquid shape colloid, and in described salt bridge electrolytic solution, add the solid potassium chloride of melting after coagulation.
3. a kind of self compensation according to claim 2, anti-pollution contrast electrode, is characterized in that, the below that described outside liquid meets boundary is provided with antifouling ring.
4. a kind of self compensation according to claim 2, anti-pollution contrast electrode, is characterized in that, it is ceramic core liquid junction that described internal liquid meets boundary, comprises internal liquid and connect boundary's pedestal and be bonded in internal liquid and connect ceramic core on boundary's pedestal.
5. a kind of self compensation according to claim 1 and 2, anti-pollution contrast electrode, is characterized in that, described housing upper end is provided with electrode cap.
6. a kind of self compensation according to claim 1 and 2, anti-pollution contrast electrode, is characterized in that, the agent of described liquid colloidal gel is high acyl gellan gum.
7. a kind of self compensation according to claim 1 and 2, anti-pollution contrast electrode, is characterized in that, is also provided with ion-selective electrode in described housing, and described ion-selective electrode and contrast electrode form measuring circuit.
8. a kind of self compensation according to claim 1, anti-pollution contrast electrode, is characterized in that, in described reference electrolyte silver chloride and potassium chloride saturated, the mass ratio of the agent of liquid colloidal gel and distilled water is 0.2 ~ 10:100.
9. a kind of self compensation according to claim 2, anti-pollution contrast electrode, is characterized in that, in described salt bridge electrolytic solution, potassium chloride is saturated, and the mass ratio of the agent of liquid colloidal gel and distilled water is 0.2 ~ 10:100.
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Cited By (5)
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| WO2017071320A1 (en) * | 2015-10-29 | 2017-05-04 | 广州道动新能源有限公司 | Battery utilizing ion exchange membrane and microfluidic technique to realize multi-electrolyte structure |
| WO2017071321A1 (en) * | 2015-10-29 | 2017-05-04 | 广州道动新能源有限公司 | Method utilizing conduction of electrolytes to realize turning on/off of cell of battery having multiple electrolytes |
| CN109298037A (en) * | 2018-12-25 | 2019-02-01 | 中国科学院烟台海岸带研究所 | A kind of micro-volume device and its application method for Copper diethlydithiocarbamate measurement |
| CN109884148A (en) * | 2019-04-03 | 2019-06-14 | 南方科技大学 | Reference electrode and using method thereof |
| CN114441618A (en) * | 2020-10-30 | 2022-05-06 | 南京农业大学 | Solid ion selective electrodes and method for rapidly determining soil nutrient ion concentration by using solid ion selective electrodes |
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| CN114441618B (en) * | 2020-10-30 | 2023-11-24 | 南京农业大学 | Solid ion selective electrode and method for rapidly determining concentration of soil nutrient ions by using same |
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