CN106442306B - Electrochemical corrosion testing device and method capable of realizing different dissolved oxygen content conditions - Google Patents
Electrochemical corrosion testing device and method capable of realizing different dissolved oxygen content conditions Download PDFInfo
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Abstract
An electrochemical corrosion testing device and method capable of realizing different dissolved oxygen content conditions. The device comprises an electrochemical workstation, a beaker, a nitrogen cylinder, an oxygen glass rotameter, a nitrogen glass rotameter, a gas outlet disc, a dissolved oxygen measuring instrument and a digital signal controller. The oxygen bottle and the nitrogen bottle supply oxygen and nitrogen for the test solution, so that the purpose of increasing or reducing the content of dissolved oxygen is achieved. The dissolved oxygen measuring instrument measures the dissolved oxygen content of the test solution in the beaker in real time, and transmits a monitoring signal to the digital signal controller, and the signal controller adjusts the glass rotameter through the rotation of the valve controller, so as to control the flow of oxygen and nitrogen entering the test solution. The gas outlet disk is used for evenly flowing out oxygen and nitrogen. The method and the device ensure that the content of the dissolved oxygen in the test solution is accurately, stably and automatically controlled, and provide preconditions for measuring the influence of the dissolved oxygen on metal corrosion by using an electrochemical method.
Description
Technical Field
The invention relates to a corrosion testing device, in particular to an electrochemical corrosion testing device and method capable of realizing different dissolved oxygen content conditions.
Background
Currently, known corrosion testing devices involving dissolved oxygen content consist of nitrogen cylinders and beakers. Only the dissolved oxygen inherent in the test solution can be removed by the nitrogen cylinder, so that the dissolved oxygen content in the solution is limited by the initial dissolved oxygen content of the solution, and the measurement range is limited. And the gas flow is regulated only through an outlet valve on the nitrogen cylinder, so that the outlet pressure is difficult to control, larger bubbles can appear in the test solution, and the solution can splash out of the beaker when serious. The nitrogen flows out from a single pipeline, and the amount of the nitrogen absorbed by the solution is limited in the process that the bubbles rise to the surface of the beaker from the bottom of the beaker, so that waste is caused. In the test process, the content of dissolved oxygen in the test solution cannot be controlled in a stable value in real time, and the accuracy of the test result is affected.
Disclosure of Invention
In order to overcome the defects of small dissolved oxygen content range, difficult control of gas flow, unstable bubbles and the like in the existing electrochemical corrosion testing method and device under different dissolved oxygen content conditions, the invention provides the electrochemical corrosion testing device capable of realizing different dissolved oxygen content conditions, which not only can widen the controllable dissolved oxygen content range, but also can automatically adjust the gas flow, and enables the bubbles to flow out carefully and uniformly at an outlet, thereby providing a stable and reliable electrochemical testing environment.
It is another object of the present invention to provide an electrochemical corrosion test method that can achieve different dissolved oxygen content conditions.
The technical scheme adopted for solving the technical problems is as follows:
the device comprises an electrochemical workstation, a beaker, a nitrogen cylinder, an oxygen glass rotameter, a nitrogen glass rotameter, a gas outlet disc, a dissolved oxygen meter and a digital signal controller, wherein the oxygen cylinder, the oxygen glass rotameter and the gas outlet disc are sequentially communicated; the nitrogen cylinder, the nitrogen glass rotameter and the gas outlet disc are sequentially communicated; the beaker is filled with test solution, a gas outlet disc is arranged at the bottom of the beaker, and the beaker mouth is sealed by a beaker cover; the electrochemical working station is connected with the working electrode, the reference electrode and the auxiliary electrode, and the working electrode, the reference electrode and the auxiliary electrode extend into the test solution in the beaker; one end of the dissolved oxygen measuring instrument is connected with the probe, the probe stretches into the test solution, the other end of the dissolved oxygen measuring instrument is connected with the digital signal controller, the digital signal controller is connected with the valve controller, and the valve controller controls the flow of the oxygen glass rotameter and the nitrogen glass rotameter.
The gas outlet disc is disc-shaped, the diameter of the gas outlet disc is smaller than the inner diameter of the beaker, the gas outlet disc is divided into two layers of spaces which are mutually separated from each other up and down, and the upper layer is connected with the oxygen inlet and is provided with a plurality of outlets with the size smaller than that of the inlet; the lower layer is connected with a nitrogen inlet, and nitrogen is discharged from the upper surface of the outlet disc through a plurality of fine vertical pipes.
The bottom surface of the gas outlet plate is provided with a sucker, and the sucker is adsorbed at the bottom of the beaker.
The beaker cover is provided with a plurality of holes, and the beaker cover seals the edges of the holes through silica gel.
The digital signal controller is a microcomputer with programmable function.
The test method of the invention comprises the following steps:
setting a numerical value of the content of dissolved oxygen required by the test in a digital signal controller, and opening valves on an oxygen cylinder and a nitrogen cylinder; in the test process, the dissolved oxygen measuring instrument reads the content of the dissolved oxygen in the current test solution, transmits the content of the dissolved oxygen to the digital signal controller in the form of an electric signal, and increases the flow of the oxygen in the oxygen glass rotameter by controlling the valve controller and simultaneously closes the nitrogen valve to enable the dissolved oxygen in the test solution to rise to the concentration required by the test if the measured content of the dissolved oxygen is lower than a preset value; if the measured dissolved oxygen content is higher than the preset value, the flow of nitrogen in the nitrogen glass rotameter is increased by controlling the valve controller, and meanwhile, the oxygen valve is closed, so that the dissolved oxygen in the test solution is reduced to the concentration required by the test.
The invention has the advantages that:
1. the oxygen circulation pipeline and the nitrogen circulation pipeline are introduced into the beaker, and the change of the dissolved oxygen content in a larger concentration range can be realized by controlling the relative flow of oxygen and nitrogen, so that conditions are provided for researching the influence of the change of the dissolved oxygen content on the corrosion of the material.
2. The dissolved oxygen measuring instrument probe is introduced into the beaker, so that the dissolved oxygen content in the test solution can be monitored in real time, and the flow of nitrogen and oxygen can be adjusted by feedback of the digital signal controller and the valve controller according to the reading of the measuring instrument.
3. The beaker cover is drilled with a plurality of holes for connecting the three electrodes, the gas inlet pipeline and the dissolved oxygen measuring instrument wire, and can isolate the internal solution from air through silica gel sealing.
4. The nitrogen cylinder and the oxygen cylinder are respectively connected with the gas outlet disc after passing through the glass rotameter, and the valve of the glass rotameter is controlled by the valve controller, so that the stable control of the gas outflow pressure and flow can be realized.
5. The gas outlet disc is provided with two inlets and a plurality of outlets, so that the flow of an inlet pipeline can be evenly and evenly halved, gas can evenly and finely flow out at different positions at the bottom of the beaker, the gas can be rapidly dissolved in a test solution, and the interference to a test system is reduced.
Drawings
Fig. 1 is a general schematic of the present invention.
Fig. 2 is a top view of the cap of the present invention.
Fig. 3 is a schematic diagram of the working principle of the gas outlet plate in the present invention.
Wherein the down arrow indicates a gas inlet, the up arrow indicates a gas outlet, the solid arrow indicates oxygen, and the open arrow indicates nitrogen.
The device is composed of: 1. an electrochemical workstation; 2. an auxiliary electrode interface; 3. a working electrode interface; 4. a reference electrode interface; 5. dissolved oxygen measuring instrument; 6. a probe; 7. an auxiliary electrode; 8. a reference electrode; 9. a working electrode; 10. a gas outlet plate; 11. a beaker; 12. a beaker cover; 13. nitrogen gas glass rotameter; 14. an oxygen glass rotameter; 15. a flowmeter bracket; 16. a nitrogen inlet pipe; 17. an oxygen inlet pipe; 18. a nitrogen outlet pipe; 19. an oxygen outlet pipe; 20. a nitrogen cylinder; 21. an oxygen cylinder; 22. a digital signal controller; 23. a valve controller; 24. working electrode jack; 25. auxiliary electrode insertion holes; 26. a reference electrode jack; 27. a probe jack of the dissolved oxygen measuring instrument; 28. an oxygen inlet pipe insertion hole; 29. nitrogen inlet pipe insertion holes; 30. and a sucking disc.
Detailed Description
The patent of the invention is described in further detail below with reference to the accompanying drawings and examples.
Examples
As shown in fig. 1, the electrochemical workstation comprises an electrochemical workstation 1, a beaker 11, a nitrogen bottle 20, an oxygen bottle 21, an oxygen glass rotameter 14, a nitrogen glass rotameter 13, a gas outlet disk 10, a dissolved oxygen meter 5 and a digital signal controller 22, wherein the oxygen bottle 21, the oxygen outlet pipe 19, the oxygen glass rotameter 14, an oxygen inlet pipe 17 and the gas outlet disk 10 are sequentially communicated; the nitrogen cylinder 20, the nitrogen outlet pipe 18, the nitrogen glass rotameter 13, the nitrogen inlet pipe 16 and the gas outlet disk 10 are sequentially communicated, and the oxygen glass rotameter 14 and the nitrogen glass rotameter 13 are fixed on a flowmeter bracket; the beaker 11 is filled with test solution, the gas outlet disc 10 is arranged at the bottom of the beaker 11, and the beaker mouth is sealed by the beaker cover 12; the electrochemical workstation 1 is respectively connected with a working electrode 9, a reference electrode 8 and a platinum sheet auxiliary electrode 7 through a working electrode interface 3, a reference electrode interface 4 and an auxiliary electrode interface 2, and the working electrode, the reference electrode and the auxiliary electrode extend into a test solution in a beaker; one end of the dissolved oxygen measuring instrument 5 is connected with the probe 6, the probe 6 stretches into the test solution, the other end of the dissolved oxygen measuring instrument 5 is connected with the digital signal controller 22, the digital signal controller 22 is connected with the valve controller 23, and the valve controller controls the flow of the oxygen glass rotameter and the nitrogen glass rotameter.
The electrochemical workstation 1 is connected with a working electrode 9, a reference electrode 8 and a platinum sheet auxiliary electrode 7 and is used for measuring electrochemical response parameters of the working electrode under a given voltage or current signal so as to judge the corrosion behavior rule of the sample. The nitrogen 20 and oxygen 21 cylinders provide a stable source of gas for the test solution, and the gas supply pressure is controlled to a relatively small stable level by valves on the cylinders. The oxygen glass rotameter 14 and the nitrogen glass rotameter 13 are used for measuring the flow of oxygen and nitrogen on one hand and regulating the flow of gas in real time through a regulating valve on the other hand under the transmission control of a valve controller. The dissolved oxygen measuring instrument 5 stretches the probe into the test solution, and the content of the dissolved oxygen is measured in real time through a sensor on the probe. The dissolved oxygen meter analyzes and converts the measurement signal, displays the dissolved oxygen content on a panel, and transmits the calculation result to the digital signal controller 22 in the form of an electric signal. The digital signal controller is a microcomputer with programmable function, which allows the user to input the set value in advance, compares the set value with the value transmitted by the dissolved oxygen controller, and then sends out instructions to the valve controller to adjust the opening and closing of the valve. In order to avoid frequent opening or closing of the valve during the test, an allowable concentration deviation value of the dissolved oxygen is also set in the digital signal controller, so as to ensure that the content of the dissolved oxygen in the solution is maintained at a relatively stable value. The gas outlet disk 11 is a plastic product and operates on the principle shown in fig. 3. The shape of the cup is disc-shaped, the diameter of the cup is slightly smaller than the inner diameter of the beaker, the cup is divided into two layers of spaces which are mutually separated from each other up and down, and the upper layer is connected with an oxygen inlet and is provided with a plurality of outlets with smaller sizes; the lower layer is connected with a nitrogen inlet, and nitrogen is discharged from the upper surface of the outlet disc through a plurality of fine vertical pipes. During the test, the disc is adsorbed at the bottom of the beaker through the sucker below, and nitrogen or oxygen uniformly and finely flows out from the upper surface, so that the dissolution process of the gas in the test solution is accelerated.
The test procedure of the invention is as follows:
as shown in fig. 1, two pipelines, namely an oxygen bottle 21, an oxygen glass rotameter 14, a gas outlet disk 10 and a nitrogen bottle 20, a nitrogen glass rotameter 13 and a gas outlet disk 10, are respectively communicated, and in the connecting process, a nitrogen inlet pipe 16 and an oxygen inlet pipe 17 pass through a nitrogen inlet pipe jack 29 and an oxygen inlet pipe jack 28 in the beaker cover 12 to check whether the air tightness of a passage is good. The electrochemical measurement working electrode 9, the reference electrode 8 and the platinum sheet auxiliary electrode 7 pass through a working electrode jack 24, a reference electrode jack 26 and an auxiliary electrode jack 25 on the beaker cover, the relative positions of the three electrodes are adjusted, then the dissolved oxygen measuring instrument probe 6 passes through a dissolved oxygen measuring instrument probe jack 27 on the beaker cover 12, and the edge of the hole of the beaker cover is sealed by silica gel. Pouring test solution into a beaker 11, putting all the components passing through a beaker cover 12 into the solution together, enabling a gas outlet disc 10 to fall on the bottom of the beaker, placing a dissolved oxygen measuring instrument probe 6, a working electrode 9, a reference electrode 8 and a platinum sheet auxiliary electrode 7 in the middle of the beaker, and covering the beaker cover. And setting the value of the content of the dissolved oxygen required by the test in the digital signal controller, and opening valves on the oxygen cylinder and the nitrogen cylinder. In the test process, the dissolved oxygen measuring instrument reads the content of the dissolved oxygen in the current test solution, transmits the content of the dissolved oxygen to the digital signal controller in the form of an electric signal, and increases the flow of the oxygen in the glass rotameter by controlling the valve controller and simultaneously closes the nitrogen valve to enable the dissolved oxygen in the test solution to rise to the concentration required by the test if the measured content of the dissolved oxygen is lower than a preset value; if the measured dissolved oxygen content is higher than the preset value, the flow rate of nitrogen in the glass rotameter is increased by controlling the valve controller, and meanwhile, the oxygen valve is closed, so that the dissolved oxygen in the test solution is reduced to the concentration required by the test.
The invention controls the dissolved oxygen content in the test solution by the flow of the nitrogen and the oxygen into the test solution. The dissolved oxygen content can be preset in the digital signal controller according to the corrosion test requirements. The dissolved oxygen content in the beaker is controlled to be equal to a preset value by combining a dissolved oxygen measuring instrument, a digital signal controller and a valve controller. The gas outlet plate can make the nitrogen and the oxygen flow out evenly and finely.
The foregoing detailed description of the invention is merely illustrative of the invention and is not limited to the embodiments of the invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or equivalents substituted for elements thereof to achieve the same technical effect. As long as the use requirement is met, the invention is within the protection scope of the invention.
Claims (4)
1. The electrochemical corrosion testing device is characterized by comprising an electrochemical workstation, a beaker, a nitrogen cylinder, an oxygen glass rotameter, a nitrogen glass rotameter, a gas outlet disc, a dissolved oxygen measuring instrument and a digital signal controller, wherein the oxygen cylinder, the oxygen glass rotameter and the gas outlet disc are sequentially communicated; the nitrogen cylinder, the nitrogen glass rotameter and the gas outlet disc are sequentially communicated; the beaker is filled with test solution, a gas outlet disc is arranged at the bottom of the beaker, and the beaker mouth is sealed by a beaker cover; the electrochemical working station is connected with the working electrode, the reference electrode and the auxiliary electrode, and the working electrode, the reference electrode and the auxiliary electrode extend into the test solution in the beaker; one end of the dissolved oxygen measuring instrument is connected with the probe, the probe stretches into the test solution, the other end of the dissolved oxygen measuring instrument is connected with the digital signal controller, the digital signal controller is connected with the valve controller, and the valve controller controls the flow of the oxygen glass rotameter and the nitrogen glass rotameter;
the gas outlet disc is disc-shaped, the diameter of the gas outlet disc is smaller than the inner diameter of the beaker, the gas outlet disc is divided into two layers of spaces which are mutually separated from each other up and down, and the upper layer is connected with the oxygen inlet and is provided with a plurality of outlets with the size smaller than that of the inlet; the lower layer is connected with a nitrogen inlet, and nitrogen is discharged from the upper surface of the outlet disc through a plurality of fine vertical pipes;
the testing method of the electrochemical corrosion testing device capable of realizing the conditions of different dissolved oxygen contents comprises the following steps:
setting a numerical value of the content of dissolved oxygen required by the test in a digital signal controller, and opening valves on an oxygen cylinder and a nitrogen cylinder; in the test process, the dissolved oxygen measuring instrument reads the content of the dissolved oxygen in the current test solution, transmits the content of the dissolved oxygen to the digital signal controller in the form of an electric signal, and increases the flow of the oxygen in the oxygen glass rotameter by controlling the valve controller and simultaneously closes the nitrogen valve to enable the dissolved oxygen in the test solution to rise to the concentration required by the test if the measured content of the dissolved oxygen is lower than a preset value; if the measured dissolved oxygen content is higher than the preset value, the flow of nitrogen in the nitrogen glass rotameter is increased by controlling the valve controller, and meanwhile, the oxygen valve is closed, so that the dissolved oxygen in the test solution is reduced to the concentration required by the test.
2. The electrochemical corrosion testing device capable of realizing different dissolved oxygen contents according to claim 1, wherein the bottom surface of the gas outlet plate is provided with a sucker, and the sucker is adsorbed at the bottom of the beaker.
3. The electrochemical corrosion testing apparatus according to claim 1, wherein the beaker cover is provided with a plurality of holes, and the beaker cover seals the edges of the holes by silica gel.
4. The electrochemical corrosion testing device capable of realizing different dissolved oxygen contents according to claim 1, wherein the digital signal controller is a microcomputer with a programmable function.
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| CN106841019B (en) * | 2017-03-14 | 2023-03-24 | 西安热工研究院有限公司 | Full-automatic oxygen-enriched corrosion test device and method |
| CN107138108A (en) * | 2017-06-21 | 2017-09-08 | 合肥学院 | A kind of device and method for preparing ferrous hydroxide precipitation |
| CN108896474B (en) * | 2018-08-01 | 2023-07-25 | 中国石油天然气集团有限公司 | Corrosion evaluation device and method for monitoring concentration of dissolved oxygen at high temperature in real time |
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