CN101625304A - Method for evaluating cementing concrete chemical seepage by electrochemical impedance method - Google Patents
Method for evaluating cementing concrete chemical seepage by electrochemical impedance method Download PDFInfo
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- CN101625304A CN101625304A CN200910060376A CN200910060376A CN101625304A CN 101625304 A CN101625304 A CN 101625304A CN 200910060376 A CN200910060376 A CN 200910060376A CN 200910060376 A CN200910060376 A CN 200910060376A CN 101625304 A CN101625304 A CN 101625304A
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- electrochemical impedance
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Abstract
The invention discloses a method for evaluating cementing concrete chemical seepage by an electrochemical impedance method, which comprises the steps: 1) electrode wrapping: using insulated epoxy resin for wrapping working electrodes, with working faces exposed outside only, then using the cementing concrete for wrapping the working faces to ensure consistent thickness of the used cementing concrete outside the working faces every time; 2) electrochemical impedance testing: using a three-electrode system for implementing electrochemical impedance test in a working medium at certain intervals, carrying out evaluation on chemical seepage resistance of the cementing concrete in accordance with an electrochemical impedance diagram; aiming at corrosive media in cementing, such as Cl<->, SO4<2->, HCO3<->, Mg<2+>, CO2, oxygen, H2S and methane, the method of the invention can evaluate the seepage factors of the cementing concrete more intuitively and accurately.
Description
Technical field:
The present invention relates to a kind of method of using evaluating cementing concrete chemical seepage by electrochemical impedance method, belong to the corrosion electrochemistry field.It is mainly used in the evaluation of the anti-chemical seepage of cementing concrete.
Background technology:
Contained Korrosionsmedium Cl in the stratum
-, SO
4 2-, HCO
3 -, Mg
2+, CO
2, H
2S, methane etc. corrode the cementing concrete ring, destroy the structural intergrity of cement stone, cause cement mantle permeability and voidage to increase, thereby cause interlayer separation actual effect.After cement mantle wrecked, Korrosionsmedium further permeated and in the metal sleeve contact, sleeve pipe is corroded, and seriously jeopardizes the safe operation of well, influences the production life-span of oil gas well.In the China's natural gas resource, major part contains H
2S is or/and CO
2,, how to cement mantle by H
2S and CO
2, it is the problem that current oil field is very paid attention to that corrosion is effectively monitored, and also is present many acid-soluble oil gas field urgent problem.
At present, done a large amount of research for the monitoring of the seepage flow in the cement both at home and abroad, and formulated some relevant standards, its main monitoring method is:
1, the water-intake rate method of testing
By cement is immersed in the solution, test the water-intake rate of cement by the weightening finish situation of test cement.
1) method of changing of chlorine ion concentration
Similar to the water-intake rate method of testing, soak the variation of the chloride ion content in the solution of cement by test and inferred the situation of chlorion diffusion in the solution.
3) potential method
When the open circuit potential of the electrode in the reinforced concrete reaches when stablizing, the concentration of Korrosionsmedium remains unchanged around the electrode of this moment, and the expression Korrosionsmedium has diffused to electrode surface fully.
4) chloride permeability fast detection method
Electrode is immersed in the solution that contains chlorion, adds 60V voltage, chlorion quickly diffuses to the surface of electrode by effect of electric field, measures the variation that electric weight takes place in this process by the enclosed pasture method and determines the situation that chlorion spreads.
5) method and anodic polarization
After adding a voltage to electrode, determine the infiltration situation of ion by the variation of test electrode electric current.
6) linear polarization method
Determine the variation of its polarization resistance by the linear polarization curve of test electrode, thereby determine the corrosion situation of electrode.
7) electrical conductivity method
This method is the variation that can cause the resistivity of cement according to ions diffusion to the electrode surface process, determines that by the variation of resistivity total ion diffuses to the time of electrode surface fully.
From the 1980s, the electrochemical impedance method is applied to the relevant research of corrosion widely.Compare with other electrochemical techniques, the electrochemical impedance method has does not have destruction, accurate and visual, test characteristics such as simple to test bodies.
Summary of the invention:
The objective of the invention is in order to provide a kind of anti-method of galvanochemistry group of using at the Korrosionsmedium Cl in the well cementation
-, SO
4 2+, HCO
3 -, Mg
2+, CO
2, oxygen, H
2S, methane etc. carry out the method for monitoring and evaluation more intuitively, exactly to the seepage flow factor of cementing concrete.
The object of the present invention is achieved like this:
The method of evaluating cementing concrete chemical seepage by electrochemical impedance method of the present invention, this method may further comprise the steps:
1) electrode is sealed: use insulating epoxy that working electrode is sealed, have only workplace to stay the outside, use cementing concrete to seal then, guarantee each consistency of thickness that uses the cementing concrete in the workplace outside;
2) electrochemical impedance test: use three-electrode system, in actuating medium, carry out the electrochemical impedance test at regular intervals, according to electrochemical impedance figure the anti-chemical seepage of cementing concrete is estimated, the time of carrying out electrochemical impedance test is to determine according to working environment, can be 1 hour, 2 hours, 3 hours, 6 hours, 12 hours etc.
Above-mentioned method may further comprise the steps:
1) electrode is sealed:
As working electrode, with using lead to weld behind its each mirror polish, use insulating epoxy that working electrode is sealed then derby, it is not encapsulated as workplace only to stay the one side relative with face of weld;
The workplace of the working electrode after sealing is polished, cleans the back use cementing concrete that working electrode is sealed once more, the cementing concrete outside that assurance is sealed at every turn and the vertical range between the workplace remain unchanged.
2) electrochemical impedance test:
The working electrode that uses cementing concrete to seal is immersed in the actuating medium, use the carbon electrode conduct to electrode, saturated glycosides mercury electrode is as contrast electrode, form three-electrode system, wherein saturated glycosides mercury electrode uses Luggin capillary as salt bridge it to be connected indirectly with actuating medium, in actuating medium, carry out the electrochemical impedance test at regular intervals, according to electrochemical impedance figure the anti-chemical seepage of cementing concrete is estimated, the time of carrying out the electrochemical impedance test is to determine according to working environment, can be 1 hour, 2 hours, 3 hours, 6 hours, 12 hours etc.
Use open circuit potential as operating potential when carrying out the electrochemical impedance test in the above-mentioned method, amplitude is 5mV, and the test frequency scope is 0.05-100000Hz, and the testing tool of electrochemical impedance is an electrochemical workstation, as CHI 604C.
Electrochemical impedance method of the present invention is that a kind of surface state is changed responds very sensitive electrochemical method, and electrode will produce corresponding response when corrosive substance arrives the surface, reduces, occurs the feature of diffusion etc. as polarization resistance.Can utilize this kind phenomenon to come the destruction of cementing concrete is monitored.
The present invention has the following advantages:
1. use the electrochemical impedance method to not influence of working electrode surface.
The electrochemical impedance method more directly perceived, easy, exactly the anti-chemical seepage behavior of cementing concrete is estimated.
Description of drawings:
Fig. 1 is working electrode packing synoptic diagram.
The working electrode that Fig. 2 seals for No. 1 cementing concrete of use soaks the electrochemical impedance figure under the different time in 3.5%NaCl solution.
The working electrode that Fig. 3 seals for No. 2 cementing concretes of use soaks the electrochemical impedance figure under the different time in 3.5%NaCl solution
The working electrode that Fig. 4 seals for No. 1 cementing concrete of use soaks the electrochemical impedance figure under the different time in saturated carbon dioxide 3.5%NaCl solution.
The working electrode that Fig. 5 seals for No. 2 cementing concretes of use soaks the electrochemical impedance figure under the different time in saturated carbon dioxide 3.5%NaCl solution.
The working electrode that Fig. 6 seals for No. 1 cementing concrete of use is containing 0.1M Na
2Soak the electrochemical impedance figure under the different time in the 3.5%NaCl solution of S.
The working electrode that Fig. 7 seals for No. 2 cementing concretes of use is containing 0.1M Na
2Soak the electrochemical impedance figure under the different time in the 3.5%NaCl solution of S.
The working electrode that Fig. 8 seals for No. 1 cementing concrete of use soaks open circuit potential and the time relation curve under the different time in 3.5%NaCl solution.
The working electrode that Fig. 9 seals for No. 2 cementing concretes of use soaks open circuit potential and the time relation curve under the different time in 3.5%NaCl solution.
The working electrode that Figure 10 seals for No. 1 cementing concrete of use soaks open circuit potential and time relation curve under the different time in saturated carbon dioxide 3.5%NaCl solution
The working electrode that Figure 11 seals for No. 2 cementing concretes of use soaks open circuit potential and time relation curve under the different time in saturated carbon dioxide 3.5%NaCl solution
The working electrode that Figure 12 seals for No. 1 cementing concrete of use is containing 0.1M Na
2Soak open circuit potential and time relation curve under the different time in the 3.5%NaCl solution of S.
The working electrode that Figure 13 seals for No. 2 cementing concretes of use is containing 0.1M Na
2Soak open circuit potential and time relation curve under the different time in the 3.5%NaCl solution of S.
Embodiment:
The method of present embodiment evaluating cementing concrete chemical seepage by electrochemical impedance method, this method comprises:
1) electrode is sealed:
Referring to Fig. 1, with cutting into the workplace shape is that the length of side is that the foursquare derby of 1cm is as working electrode 1, use lead 2 to weld after using 800# sand paper with each mirror polish, use insulating epoxy 3 that working electrode is sealed then, it is not encapsulated as workplace only to stay the one side relative with face of weld;
The workplace of the working electrode after sealing is polished, cleans the back use cementing concrete 4 (i.e. No. 1 cementing concrete or No. 2 cementing concretes) that working electrode is sealed once more, the cementing concrete outside that assurance is sealed at every turn and the vertical range between the workplace remain unchanged.
2) electrochemical impedance test:
With use cementing concrete promptly the working electrode sealed of No. 1 cementing concrete or No. 2 cementing concretes be immersed in the different actuating mediums, use the carbon electrode conduct to electrode, saturated glycosides mercury electrode is as contrast electrode, form three-electrode system, wherein saturated glycosides mercury electrode uses Luggin capillary as salt bridge it to be connected indirectly with actuating medium, in actuating medium, carried out the electrochemical impedance test every 6 hours, according to electrochemical impedance figure to cementing concrete promptly the anti-chemical seepage of No. 1 cementing concrete or No. 2 cementing concretes estimate.
Use open circuit potential as operating potential during the electrochemical impedance test, amplitude is 5mV, and the test frequency scope is 0.05-100000Hz, and the testing tool of electrochemical impedance is CHI 604C.
1. electrochemical impedance monitoring
Fig. 2, Fig. 3 are respectively the electrochemical impedance figure of the working electrode that uses No. 1 cementing concrete and No. 2 cementing concretes to seal when soaking different time in 3.5%NaCl solution.As can be seen from the figure, when using No. 1 cementing concrete to seal, its electrochemical impedance figure began to occur diffusion phenomena in the time of the 41st hour, and still kept diffusion characteristic after 112 hours.And use in the system that No. 2 cementing concretes seal, just begin to occur faint diffusion phenomena in first hour of soaking, and 49 as a child diffusion phenomena disappear, illustrate that the corrosive deposit diffusion is complete after 49 hours.Therefore, in containing the 3.5%NaCl system, the anti-chemical seepage performance of No. 1 cementing concrete is better than No. 2 cementing concretes.
Fig. 4 and Fig. 5 are respectively the working electrode that uses No. 1 cementing concrete and No. 2 cementing concretes to seal soaks different time in containing the 3.5%NaCl solution of saturated carbon dioxide electrochemical impedance figure.As can be seen from the figure, no matter use is No. 1 cementing concrete or No. 2 cementing concretes, all is to begin at the 9th hour diffusion to occur, and keeps diffusion always.This mainly is that its voidage remains unchanged, thereby causes diffusion phenomena to remain unchanged because carbon dioxide and cementing concrete reaction generate solid-state lime carbonate.
The working electrode that Fig. 6 and Fig. 7 are respectively No. 1 cementing concrete of use No. 2 and cementing concrete is sealed is containing 0.1M Na
2Soak the electrochemical impedance figure of different time in the 3.5%NaCl solution of S.As can be seen from the figure, reach first stable hour in immersion and diffusion phenomena all occurred, that is to say that sulphion reaches electrode surface at this moment.When using No. 1 cementing concrete encapsulated electrodes, diffusion phenomena have just disappeared after 9 hours, and the increase polarization resistance value increase along with the time that is to say that the FeS that forms at electrode surface is dense, can suppress the further corrosion of reinforcing bar.And when the working electrode that No. 2 cementing concretes of use are sealed, sulphion arrives the metal surface with the phenomenon of diffusion always, that is to say that No. 2 cementing concretes can suppress the diffusion of sulphion to electrode surface.
2. open circuit potential monitoring
This method is to use the monitoring of CHI 604C electrochemical workstation.According to industry standard, spread fully and reach electrode surface when the open circuit potential of electrode changes when little Korrosionsmedium.As can be seen, the current potential of electrode has certain fluctuation from Fig. 8～Figure 13, can only by virtue of experience be similar to the time that current potential is stable of finding.As can be seen, the result of electrochemical impedance method evaluation matches from the stable time, illustrates that it is correct using the result of electrochemical impedance method evaluation.
The foregoing description is that foregoing of the present invention is further described, but this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to the foregoing description.All technology that realizes based on foregoing all belong to scope of the present invention.
Claims (3)
1, the method for evaluating cementing concrete chemical seepage by electrochemical impedance method, this method may further comprise the steps:
1) electrode is sealed:
Use insulating epoxy that working electrode is sealed, have only workplace to stay the outside, use cementing concrete to seal then, guarantee each consistency of thickness that uses the cementing concrete in the workplace outside;
2) electrochemical impedance test:
Use three-electrode system, in actuating medium, carry out the electrochemical impedance test at regular intervals, the anti-chemical seepage of cementing concrete is estimated according to electrochemical impedance figure.
2, the method for evaluating cementing concrete chemical seepage by electrochemical impedance method according to claim 1 is characterized in that this method may further comprise the steps:
1) with derby as working electrode, with using lead to weld behind its each mirror polish, use insulating epoxy that working electrode is sealed then, it is not encapsulated as workplace only to stay the one side relative with face of weld;
The workplace of the working electrode after sealing is polished, cleans the back use cementing concrete that working electrode is sealed once more, the cementing concrete outside that assurance is sealed at every turn and the vertical range between the workplace remain unchanged;
2) electrochemical impedance test:
The working electrode that uses cementing concrete to seal is immersed in the actuating medium, use the carbon electrode conduct to electrode, saturated glycosides mercury electrode is as contrast electrode, form three-electrode system, wherein saturated glycosides mercury electrode uses Luggin capillary as salt bridge it to be connected indirectly with actuating medium, in actuating medium, carry out the electrochemical impedance test at regular intervals, the anti-chemical seepage of cementing concrete is estimated according to electrochemical impedance figure.
3, the method for evaluating cementing concrete chemical seepage by electrochemical impedance method according to claim 1 and 2 uses open circuit potential as operating potential when it is characterized in that the electrochemical impedance test, and amplitude is 5mV, and the test frequency scope is 0.05-100000Hz.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102331392A (en) * | 2010-07-14 | 2012-01-25 | 中原工学院 | Method for evaluating rock permeability |
| CN102778429A (en) * | 2012-07-03 | 2012-11-14 | 天津大学 | Electrochemical transducer for atmospheric corrosion of metal materials and application thereof |
| CN103558077A (en) * | 2013-11-06 | 2014-02-05 | 上海电机学院 | Packaging method for electrochemical testing sample |
| CN113916750A (en) * | 2021-11-23 | 2022-01-11 | 南通市建筑科学研究院有限公司 | Multifunctional impermeability tester and concrete comprehensive impermeability test system comprising same |
| CN114002286A (en) * | 2021-09-26 | 2022-02-01 | 河海大学 | Method for measuring total autogenous potential of cement-based material |
| CN117147427A (en) * | 2023-10-26 | 2023-12-01 | 鲁东大学 | Sample suitable for electrochemical test in deep sea experiment and packaging method thereof |
-
2009
- 2009-08-18 CN CN200910060376A patent/CN101625304A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102331392A (en) * | 2010-07-14 | 2012-01-25 | 中原工学院 | Method for evaluating rock permeability |
| CN102778429A (en) * | 2012-07-03 | 2012-11-14 | 天津大学 | Electrochemical transducer for atmospheric corrosion of metal materials and application thereof |
| CN103558077A (en) * | 2013-11-06 | 2014-02-05 | 上海电机学院 | Packaging method for electrochemical testing sample |
| CN103558077B (en) * | 2013-11-06 | 2016-03-02 | 上海电机学院 | The method for packing of electro-chemical test sample |
| CN114002286A (en) * | 2021-09-26 | 2022-02-01 | 河海大学 | Method for measuring total autogenous potential of cement-based material |
| CN113916750A (en) * | 2021-11-23 | 2022-01-11 | 南通市建筑科学研究院有限公司 | Multifunctional impermeability tester and concrete comprehensive impermeability test system comprising same |
| CN117147427A (en) * | 2023-10-26 | 2023-12-01 | 鲁东大学 | Sample suitable for electrochemical test in deep sea experiment and packaging method thereof |
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Open date: 20100113 |