CN102735604B - Electrolytic cell for corrosion electrochemical measurement - Google Patents

Electrolytic cell for corrosion electrochemical measurement Download PDF

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Publication number
CN102735604B
CN102735604B CN201210193921.5A CN201210193921A CN102735604B CN 102735604 B CN102735604 B CN 102735604B CN 201210193921 A CN201210193921 A CN 201210193921A CN 102735604 B CN102735604 B CN 102735604B
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China
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electrolytic cell
working electrode
electrode
pond body
temperature
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Expired - Fee Related
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CN201210193921.5A
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CN102735604A (en
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李谋成
韩沛洪
马荣耀
王士栋
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The invention discloses an electrolytic cell for corrosion electrochemical measurement, comprising an electrolytic cell body with sealed inner cavity, wherein the exterior of the electrolytic cell body is provided with a temperature controller to keep the temperature of the electrolyte at a preset temperature level, the top of the electrolytic cell is provided with a plurality of electrolytic cell top nozzles, a reference electrode, an auxiliary electrode and a temperature measuring device are respectively arranged, side vertical face of the electrolytic cell is provided with an electrolytic cell side wall opening, a clamping member of a clamp is made from insulating materials, the clamping member clamps a working electrode, the working electrode, the reference electrode and the auxiliary electrode are externally connected with an electrochemical workstation, the temperature-sensing end of the temperature measuring device is dipped in the electrolyte to measure the temperature of the electrolyte at real time, when conducting electrochemical measurement, the electrolyte in the electrolytic cell body submerges the electrode end of the reference electrode and the electrode end of the auxiliary electrode. According to the invention, the rapid preparation of working electrode measurement experimental device assembly can be realized, good leakproofness of the working electrode is achieved, and simultaneously the requirements of constant temperature electrochemical measurement from room temperature to boiling condition are satisfied.

Description

For the electrolytic cell of electrochemical corrosion measurement
Technical field
The present invention relates to a kind of electrolysis unit, particularly a kind of electrolysis experimental apparatus for testing for electrochemical measurement.
Background technology
In material corrosion research, often use electrolytic cell, quality prepared by working electrode directly has influence on accuracy and the correctness of experimental result, epoxy resin approved sample Chang Yi leaves micro gap or the bubble between working electrode and epoxy resin, many times naked eyes cannot be discovered, result, in when test situations such as corrosion that gap, affects experimental result.On the other hand, loaded down with trivial details approved sample process often expends the longer time, and preparation work electrode can improve the efficiency of corrosion electrochemistry research greatly quickly and easily.Many test requests carry out under the condition higher than room temperature, and for example, stainless steel intercrystalline corrosion testing requirements test is carried out in the sulfuric acid-copper-bath of boiling, realizes the research that electro-chemical test contributes to material corrosion under above-mentioned environment.Therefore, at preparation work electrode quickly and easily, ensure working electrode sealing in, realize the constant temperature electrochemical measurement of material from room temperature to boiling condition and seem particularly crucial, and that the electrolysis experimental apparatus for testing of existing electrochemical measurement uses is convenient not, structural design is also not ideal enough.
Summary of the invention
In order to solve prior art problem, the object of the present invention is to provide a kind of electrolytic cell for electrochemical corrosion measurement, can realize the assembling of quick preparation work electrode test experimental provision, there is working electrode sealing good, meet from room temperature to boiling condition simultaneously constant temperature electrochemical measurement.
To achieve the above object of the invention, the present invention adopts following technical proposals:
A kind of electrolytic cell for electrochemical corrosion measurement, there is the electrolytic cell pond body of bore seal, the outside of electrolytic cell pond body is provided with temperature control equipment, make the temperature of the electrolytic solution in the body of electrolytic cell pond remain on preset temperature level, body top, electrolytic cell pond is at least provided with three electrolytic cell top mouths of pipe, electrolytic cell head tube opening's edge lineal layout, each electrolytic cell top mouth of pipe all seals, the side elevation of electrolytic cell pond body is also provided with electrolytic cell sidewall opening, the centerline of the center line of electrolytic cell sidewall opening and three electrolytic cell top mouths of pipe is in the same space plane, a working electrode is fixed on the outside of electrolytic cell sidewall opening by fixture, the compacting part of the fixture directly contacting with working electrode is made up of insulating material, compacting part compresses working electrode, gasket ring is arranged at the edge of electrolytic cell sidewall opening, the shape and size of the endoporus of gasket ring and electrolytic cell sidewall opening are suitable, gasket ring is installed between the external wall of working electrode and electrolytic cell pond, and make electrolytic cell sidewall opening in seamless sealing state, the test surfaces of working electrode is exposed in the inner chamber of electrolytic cell pond body, the size of the corresponding electrolytic cell sidewall opening of area of the test surfaces of working electrode, the test surfaces of working electrode contacts with the electrolytic solution in the body of electrolytic cell pond completely, also have a contrast electrode to be installed on the position near working electrode by first electrolytic cell top mouth of pipe, the most advanced and sophisticated alignment work electrode of Luggin capillary of contrast electrode, also have an auxiliary electrode to be placed in the position of maintenance level between working electrode by second electrolytic cell top mouth of pipe, and relative with the test surfaces of working electrode, separately there is a temperature measuring equipment to install by the 3rd the electrolytic cell top mouth of pipe, working electrode, the external electrochemical workstation of contrast electrode and auxiliary electrode, the temperature-sensitive test lead of temperature measuring equipment immerses in the electrolytic solution in the body of electrolytic cell pond, temperature to electrolytic solution is measured in real time, in the time carrying out electro-chemical test, electrolytic solution in the body of electrolytic cell pond floods the electrode tip of contrast electrode and the electrode tip of auxiliary electrode.
As the optimal technical scheme of technical solution of the present invention, body top, electrolytic cell pond is provided with four electrolytic cell mouths of pipe, and air-breather or condensing unit are installed in the 4th the electrolytic cell top mouth of pipe; Or body top, electrolytic cell pond is provided with five electrolytic cell mouths of pipe, air-breather is installed in the 4th the electrolytic cell top mouth of pipe, condensing unit is installed in the 5th the electrolytic cell top mouth of pipe; Air-breather passes into inert gas in the intracoelomic cavity of electrolytic cell pond, and condensing unit makes water vapor condense into aqueous water, is again back in the electrolytic solution in the body of electrolytic cell pond.
Said temperature control device is constant temperature water bath apparatus, and electrolytic cell pond body is installed in the water bath containers of constant temperature water bath apparatus.
Said temperature control device is heating arrangement, and heating arrangement heats the electrolytic solution in the body of electrolytic cell pond, realizes the constant temperature electro-chemical test from room temperature to electrolytic solution boiling temperature condition.
Above-mentioned working electrode is also preferably sheet, and the area of working electrode is greater than the size of electrolytic cell sidewall opening, the direct compacting gasket ring of working electrode.
The shape of above-mentioned working electrode preferably adopts circle, square, pentagon or hexagon.
The compacting part of above-mentioned fixture preferably passes through bolted.
The material of above-mentioned electrolytic cell pond body preferably selects simple glass, quartz glass or the polytetrafluoroethylmaterial material of printing opacity to make.
Each electrolytic cell top mouth of pipe of above-mentioned electrolytic cell pond body preferably seals by sealing-plug respectively.
Above-mentioned gasket ring and sealing-plug preferably select nitrile rubber or silicon rubber to make.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. to be placed in pond external for working electrode of the present invention, only makes the area that is exposed to pond body opening contact with solution, and sample is easy to prepare, without approved sample.
2. the present invention can realize the corrosion test under solution boiling condition with heating by electric cooker electrolytic cell, configure reflux condenser to prevent moisture evaporation simultaneously, in preparing quickly and easily electrode assembling and ensureing working electrode sealing, can realize room temperature to the constant temperature electro-chemical test under fluidized state.
3. opening part of the present invention is equipped with the gasket ring of good airproof performance, contacts well with working electrode, has ensured sealing and insulativity, has avoided the impact of crevice corrosion on electro-chemical test.
4. the present invention, for the fixture of steady job electrode with bolt, can mount and dismount easily.
5. electrolytic cell of the present invention pond body has multiple mouths of pipe, except for installing contrast electrode, auxiliary electrode, can equip temperature measuring equipment, gas device, condensing unit etc., alternative good.
Brief description of the drawings
Fig. 1 is the electrolyser construction schematic diagram of the embodiment of the present invention one for electrochemical corrosion measurement.
Fig. 2 is the electrolytic cell pond body side surface structural representation of installment work electrode in the embodiment of the present invention one.
Fig. 3 is clamp structure schematic diagram in the embodiment of the present invention one.
Embodiment
By reference to the accompanying drawings, to the preferred embodiments of the present invention, details are as follows:
embodiment mono-:
Referring to Fig. 1, Fig. 2 and Fig. 3, a kind of electrolytic cell for electrochemical corrosion measurement, there is the electrolytic cell pond body 1 of bore seal, the outside of electrolytic cell pond body 1 is provided with temperature control equipment, make the temperature of the electrolytic solution in electrolytic cell pond body 1 remain on preset temperature level, body 1 top, electrolytic cell pond is at least provided with three electrolytic cell top mouths of pipe, electrolytic cell head tube opening's edge lineal layout, each electrolytic cell top mouth of pipe all seals, the side elevation of electrolytic cell pond body 1 is also provided with electrolytic cell sidewall opening 2, the centerline of the center line of electrolytic cell sidewall opening 2 and three electrolytic cell top mouths of pipe is in the same space plane, a working electrode 5 is fixed on the outside of electrolytic cell sidewall opening 2 by fixture 4, the compacting part 12 of the fixture 4 directly contacting with working electrode 5 is made up of insulating material, compacting part 12 compresses working electrode 5, gasket ring 3 is arranged at the edge of electrolytic cell sidewall opening 2, the shape and size of the endoporus of gasket ring 3 and electrolytic cell sidewall opening 2 are suitable, gasket ring 3 is installed between working electrode 5 and electrolytic cell pond body 1 outer wall, and make electrolytic cell sidewall opening 2 in seamless sealing state, the test surfaces of working electrode 5 is exposed in the inner chamber of electrolytic cell pond body 1, the size of the corresponding electrolytic cell sidewall opening 2 of area of the test surfaces of working electrode 5, the test surfaces of working electrode 5 contacts with the electrolytic solution in electrolytic cell pond body 1 completely, also have a contrast electrode 6 to be installed on the position near working electrode 5 by first electrolytic cell top mouth of pipe, the most advanced and sophisticated alignment work electrode 5 of Luggin capillary of contrast electrode 6, also have an auxiliary electrode 7 to be placed in the position of maintenance level between working electrode 5 by second electrolytic cell top mouth of pipe, and relative with the test surfaces of working electrode 5, separately there is a temperature measuring equipment 8 to install by the 3rd the electrolytic cell top mouth of pipe, working electrode 5, contrast electrode 6 and the external electrochemical workstation of auxiliary electrode 7, the temperature-sensitive test lead of temperature measuring equipment 8 immerses in the electrolytic solution in electrolytic cell pond body 1, temperature to electrolytic solution is measured in real time, in the time carrying out electro-chemical test, electrolytic solution in electrolytic cell pond body 1 floods the electrode tip of contrast electrode 6 and the electrode tip of auxiliary electrode 7.Can realize the electro-chemical test to institute's research material under condition of different temperatures at the present embodiment electrolytic cell.
In the present embodiment, body 1 top, electrolytic cell pond is provided with four electrolytic cell mouths of pipe, and air-breather is installed in the 4th the electrolytic cell top mouth of pipe, and air-breather passes into inert gas in body 1 inner chamber of electrolytic cell pond.
In the present embodiment, temperature control equipment is constant temperature water bath apparatus, and electrolytic cell pond body 1 is installed in the water bath containers of constant temperature water bath apparatus, the present embodiment electrolytic cell is placed in to thermostat water bath and can realizes the electro-chemical test of constant temperature.
Referring to Fig. 1 and Fig. 3, in the present embodiment, the compacting part 12 of above-mentioned fixture 4 passes through bolted.Be used for the fixture 4 of steady job electrode 5 with bolt, can mount and dismount easily.Working electrode 5, without the approved sample process through loaded down with trivial details, is directly installed on electrolytic cell sidewall opening 2 places by fixture 4, has greatly improved the efficiency of Experiment in Erosive Electrochemistry research.
In the present embodiment, simple glass, quartz glass or the polytetrafluoroethylmaterial material of the material selection printing opacity of electrolytic cell pond body 1 are made, and are convenient to observation experiment phenomenon and monitoring experiment effect, and the cost of material is low, easily manufactured.
Referring to Fig. 1, in the present embodiment, three electrolytic cell top mouths of pipe of electrolytic cell pond body 1, respectively by sealing-plug 9,10,11 sealings, adopt the packaging structure of sealing-plug sealing simple, are convenient to installation and removal and safeguard.
In the present embodiment, gasket ring 3 and sealing-plug 9,10,11 select nitrile rubber or silicon rubber to make, and material is easy to get, and seal low cost of manufacture, when experimental temperature requires when higher or lower, can select the wider silicon rubber of temperature resistant range to make.
In the present embodiment, first working electrode 5 use are fixed on to electrolytic cell sidewall opening 2 places with the fixture 4 of bolt, ensure sealing, insulation.Contrast electrode 6 is installed on the position near working electrode 5 by first electrolytic cell top mouth of pipe of electrolytic cell, the most advanced and sophisticated alignment work electrode 5 of its Luggin capillary.Auxiliary electrode 7 is placed in and the position of working electrode 5 levels by second electrolytic cell top mouth of pipe, relative with working electrode 5.Back to back the 3rd the electrolytic cell top mouth of pipe installed temperature measuring equipment 8.When test, solution floods working electrode 5, contrast electrode 6 and auxiliary electrode 7.
embodiment bis-:
The technical scheme of the present embodiment and embodiment mono-is basic identical, and special feature is:
In the present embodiment, body 1 top, electrolytic cell pond is provided with four electrolytic cell mouths of pipe, and condensing unit is installed in the 4th the electrolytic cell top mouth of pipe, and condensing unit makes water vapor condense into aqueous water, is again back in the electrolytic solution in electrolytic cell pond body 1.In the present embodiment, when done requirement of experiment temperature is during higher than room temperature, while even reaching boiling temperature, can be four mouths of pipe by cell design, contrast electrode 6, auxiliary electrode 7, temperature measuring equipment 8 and condenser pipe are installed respectively.Be that contrast electrode 6 is installed on the position near working electrode 5 by first electrolytic cell top mouth of pipe of electrolytic cell, the most advanced and sophisticated alignment work electrode 5 of its Luggin capillary.Auxiliary electrode 7 is placed in and the position of working electrode 5 levels by second electrolytic cell top mouth of pipe, relative with working electrode 5.Back to back two electrolytic cell top mouths of pipe are installed respectively temperature measuring equipment 8 and condenser pipe.In the present embodiment, can realize the corrosion test under solution boiling condition with heating by electric cooker electrolytic cell, configure reflux condenser to prevent moisture evaporation simultaneously, can realize room temperature to the constant temperature electro-chemical test under fluidized state by electro-chemical test instrument.
In the present embodiment, temperature control equipment is heating arrangement, and heating arrangement heats the electrolytic solution in electrolytic cell pond body 1, realizes the constant temperature electro-chemical test from room temperature to electrolytic solution boiling temperature condition.Now, whole device can be placed in to thermostat water bath, be adjusted to and test temperature required and test, water-bath middle water level line should be lower than the extreme lower position of working electrode 5 lower edges and electrolytic cell sidewall opening 2, and working electrode 5 is not contacted with water in water-bath.Heating can realize the test under solution boiling condition to electrolytic cell to adopt the adjustable electric furnace of power, can realize room temperature to the constant temperature electro-chemical test under fluidized state by electro-chemical test instrument.
In the present embodiment, can carry out the electro-chemical test of stainless steel in the sulfuric acid-copper-bath of boiling.Electrolytic cell is established 4 mouths of pipe, and contrast electrode 6, auxiliary electrode 7, reflux condenser and temperature measuring equipment 8 are installed respectively.First working electrode 5 use fixtures 4 are fixed on to electrolytic cell sidewall opening 2 places, ensure sealing, insulation.When test, sulfuric acid-copper-bath floods working electrode 5, contrast electrode 6 and auxiliary electrode 7.The present embodiment electrolytic cell is placed on the adjustable electric furnace of power and is heated, install external electrochemical workstation, the electrochemical behavior of test stainless steel in the sulfuric acid-copper-bath of boiling.
embodiment tri-:
The technical scheme of the present embodiment and previous embodiment is basic identical, and special feature is:
In the present embodiment, body 1 top, electrolytic cell pond is provided with five electrolytic cell mouths of pipe, and air-breather is installed in the 4th the electrolytic cell top mouth of pipe, and condensing unit is installed in the 5th the electrolytic cell top mouth of pipe; Air-breather passes into inert gas in body 1 inner chamber of electrolytic cell pond, and condensing unit makes water vapor condense into aqueous water, is again back in the electrolytic solution in electrolytic cell pond body 1.In the present embodiment, when done requirement of experiment temperature is during higher than room temperature, pass into inert gas as also needed to remove the oxygen in solution.At this moment can be four mouths of pipe by cell design, contrast electrode 6, auxiliary electrode 7, temperature measuring equipment 8 and gas device are installed respectively.Be that contrast electrode 6 is installed on the position near working electrode 5 by first electrolytic cell top mouth of pipe of electrolytic cell, the most advanced and sophisticated alignment work electrode 5 of its Luggin capillary.Auxiliary electrode 7 is placed in and the position of working electrode 5 levels by second electrolytic cell top mouth of pipe, relative with working electrode 5.Back to back two electrolytic cell top mouths of pipe are installed respectively temperature measuring equipment 8 and gas device.
embodiment tetra-:
The technical scheme of the present embodiment and previous embodiment is basic identical, and special feature is:
In the present embodiment, working electrode 5 is sheet, and the area of working electrode 5 is greater than the size of electrolytic cell sidewall opening 2, the direct compacting gasket ring 3 of working electrode 5.In the present embodiment, when test, working electrode 5 use fixtures 4 are fixed on electrolytic cell sidewall opening 2 places, test area is electrolytic cell sidewall opening 2 sizes, working electrode 5 assembling preparations fast, simply, without epoxy resin approved sample, specimen size does not have too high requirement, all can use as long as not excessive or too small.Opening part is equipped with the gasket ring 3 of good airproof performance, contacts well with working electrode 5, has ensured sealing and insulativity, has avoided the impact of crevice corrosion on electro-chemical test.
In the present embodiment, working electrode 5 be shaped as circular, square, pentagon or hexagon.
By reference to the accompanying drawings the embodiment of the present invention is illustrated above, but the invention is not restricted to above-described embodiment, can also make multiple variation according to the object of innovation and creation of the present invention.The change made under all Spirit Essences according to technical solution of the present invention and principle, modification, substitute, combination, simplify; all should be equivalent substitute mode; as long as goal of the invention according to the invention; only otherwise deviate from know-why and the inventive concept of the present invention for the electrolytic cell of electrochemical corrosion measurement, all belong to protection scope of the present invention.

Claims (10)

1. the electrolytic cell for electrochemical corrosion measurement, there is the electrolytic cell pond body (1) of bore seal, the outside of described electrolytic cell pond body (1) is provided with temperature control equipment, make the temperature of the electrolytic solution in described electrolytic cell pond body (1) remain on preset temperature level, it is characterized in that: described electrolytic cell pond body (1) top is at least provided with three electrolytic cell top mouths of pipe, described electrolytic cell head tube opening's edge lineal layout, each described electrolytic cell top mouth of pipe all seals, the side elevation of described electrolytic cell pond body (1) is also provided with electrolytic cell sidewall opening (2), the centerline of the center line of described electrolytic cell sidewall opening (2) and described three electrolytic cell top mouths of pipe is in the same space plane, a working electrode (5) is fixed on the outside of described electrolytic cell sidewall opening (2) by fixture (4), the compacting part (12) of the described fixture (4) directly contacting with described working electrode (5) is made up of insulating material, described compacting part (12) compresses described working electrode (5), gasket ring (3) is arranged at the edge of described electrolytic cell sidewall opening (2), the shape and size of the endoporus of described gasket ring (3) and described electrolytic cell sidewall opening (2) are suitable, described gasket ring (3) is installed between described working electrode (5) and electrolytic cell pond body (1) outer wall, and make described electrolytic cell sidewall opening (2) in seamless sealing state, the test surfaces of described working electrode (5) is exposed in the inner chamber of described electrolytic cell pond body (1), the size of the corresponding described electrolytic cell sidewall opening of area (2) of the test surfaces of described working electrode (5), the test surfaces of described working electrode (5) contacts with the electrolytic solution in described electrolytic cell pond body (1) completely, also have a contrast electrode (6) to be installed on the position near described working electrode (5) by first electrolytic cell top mouth of pipe, the most advanced and sophisticated described working electrode (5) of aiming at of Luggin capillary of described contrast electrode (6), also have an auxiliary electrode (7) to be placed in by second electrolytic cell top mouth of pipe the position that keeps level between described working electrode (5), and relative with the test surfaces of described working electrode (5), separately there is a temperature measuring equipment (8) to install by the 3rd the electrolytic cell top mouth of pipe, described working electrode (5), contrast electrode (6) and the external electrochemical workstation of auxiliary electrode (7), the temperature-sensitive test lead of described temperature measuring equipment (8) immerses in the electrolytic solution in described electrolytic cell pond body (1), temperature to electrolytic solution is measured in real time, in the time carrying out electro-chemical test, electrolytic solution in described electrolytic cell pond body (1) floods the electrode tip of described contrast electrode (6) and the electrode tip of described auxiliary electrode (7).
2. the electrolytic cell for electrochemical corrosion measurement according to claim 1, is characterized in that: described electrolytic cell pond body (1) top is provided with four electrolytic cell mouths of pipe, and air-breather or condensing unit are installed in described the 4th the electrolytic cell top mouth of pipe; Or described electrolytic cell pond body (1) top is provided with five electrolytic cell mouths of pipe, air-breather is installed in described the 4th the electrolytic cell top mouth of pipe, condensing unit is installed in described the 5th the electrolytic cell top mouth of pipe; Described air-breather passes into inert gas in described electrolytic cell pond body (1) inner chamber, and described condensing unit makes water vapor condense into aqueous water, is again back in the electrolytic solution in described electrolytic cell pond body (1).
3. the electrolytic cell for electrochemical corrosion measurement according to claim 2, is characterized in that: described temperature control equipment is constant temperature water bath apparatus, and described electrolytic cell pond body (1) is installed in the water bath containers of described constant temperature water bath apparatus.
4. the electrolytic cell for electrochemical corrosion measurement according to claim 2, it is characterized in that: described temperature control equipment is heating arrangement, described heating arrangement heats the electrolytic solution in described electrolytic cell pond body (1), realizes the constant temperature electro-chemical test from room temperature to electrolytic solution boiling temperature condition.
5. according to the electrolytic cell for electrochemical corrosion measurement described in any one in claim 1~4, it is characterized in that: described working electrode (5) is sheet, the area of described working electrode (5) is greater than the size of described electrolytic cell sidewall opening (2), and described working electrode (5) is gasket ring (3) described in compacting directly.
6. the electrolytic cell for electrochemical corrosion measurement according to claim 5, is characterized in that: being shaped as of described working electrode (5) is circular, square, pentagon or hexagon.
7. according to the electrolytic cell for electrochemical corrosion measurement described in any one in claim 1~4, it is characterized in that: the compacting part (12) of described fixture (4) passes through bolted.
8. according to the electrolytic cell for electrochemical corrosion measurement described in any one in claim 1~4, it is characterized in that: simple glass, quartz glass or the polytetrafluoroethylmaterial material of the material selection printing opacity of described electrolytic cell pond body (1) are made.
9. according to the electrolytic cell for electrochemical corrosion measurement described in any one in claim 1~4, it is characterized in that: each electrolytic cell top mouth of pipe of described electrolytic cell pond body (1) seals by sealing-plug respectively.
10. the electrolytic cell for electrochemical corrosion measurement according to claim 9, is characterized in that: described gasket ring (3) and sealing-plug select nitrile rubber or silicon rubber to make.
CN201210193921.5A 2012-06-13 2012-06-13 Electrolytic cell for corrosion electrochemical measurement Expired - Fee Related CN102735604B (en)

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