CN220154338U - Rotary electrode electrochemical detection device - Google Patents
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- CN220154338U CN220154338U CN202321502709.2U CN202321502709U CN220154338U CN 220154338 U CN220154338 U CN 220154338U CN 202321502709 U CN202321502709 U CN 202321502709U CN 220154338 U CN220154338 U CN 220154338U
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Abstract
The utility model belongs to the technical field of medicine development and detection, and particularly relates to a rotary electrode electrochemical detection device. The electrochemical detection device for the rotary electrode comprises an electrolytic cell and a device for the rotary electrode, wherein a connecting port is arranged on the electrolytic cell, a connecting piece is arranged on the connecting port, a bearing is arranged on the connecting piece, the outer ring of the bearing is fixedly connected with the connecting piece, a detection electrode is fixed in the inner ring of the bearing, and the upper part of the detection electrode is connected with the device for the rotary electrode. The utility model realizes the coupling connection between the rotary electrode system and the sealed electrolytic cell, can meet the requirements of atmosphere control and electrode rotation in experiments, and has good application prospect.
Description
Technical Field
The utility model belongs to the technical field of medicine development and detection, and particularly relates to a rotary electrode electrochemical detection device.
Background
Electrochemical analysis is a commonly used analysis method, and in the research of related subjects in the biomedical field, researchers often design bioelectrodes (i.e., sensors) for sensing components of enzymes, immunity, microorganisms, cells, DNA, RNA, proteins, smell, taste and body fluids, and study related biochemical reactions by electrochemical testing methods. Thereby providing relevant information for research of diseases or development of medicines.
For electrochemical reactions, mass transfer of a substance is an important factor affecting the progress of the reaction. Mass transfer refers to the process in which the reaction substance reaches the electrode surface to react under the action of diffusion, migration or convection, or the reaction intermediate and the product leave the electrode surface under the action of diffusion, migration or convection. In the conventional electrochemical test method, the electrode is static, in this case, the simulated electrochemical reaction process is very limited, and the reaction under different mass transfer conditions cannot be studied.
In order to study the distribution of the current density on the surface of the electrode under different mass transfer conditions and reduce or eliminate the influence of factors such as a diffusion layer, a high-speed rotating electrode is developed in the field, and the end face of the electrode is like a disk, so the electrode is also called a rotating disk electrode (rotating disk electrode, RDE), namely a rotating disk electrode for short, and is also called a rotating disk electrode. And a rotating ring electrode or the like which is further improved based on the electrode, the electrochemical parameters of a more complex electrode process can be measured. RDE is characterized in that a working electrode for detecting an electrochemical reaction is rotated at a certain speed.
On the other hand, in the research of electrochemical reaction, there is often a requirement for controlling the reaction gas atmosphere, and in the existing electrochemical reaction device, a sealed electrolytic cell (for example, a thin-layer flow electrolytic cell suitable for electrochemical in-situ raman spectroscopy detection in chinese patent No. CN 201511033833.9) is often used for controlling the electrochemical reaction of the reaction gas atmosphere, however, the detection electrode in such electrolytic cell is usually fixed, and thus cannot be matched with the working electrode that needs to be rotated in the RDE system. Accordingly, it is a need in the art to provide a device that is capable of connecting an RDE system to a sealed electrolytic cell.
Disclosure of Invention
In view of the problems of the prior art, the present utility model provides a rotary electrode electrochemical detection device, with the aim of providing a device capable of connecting an RDE system with a sealed electrolytic cell.
The utility model provides a rotating electrode electrochemical detection device, includes the electrolytic cell and is used for rotating electrode's device, be provided with the connector on the electrolytic cell, be provided with the connecting piece on the connector, be provided with the bearing on the connecting piece, the outer lane and the connecting piece fixed connection of bearing, be fixed with the detecting electrode in the inner circle of bearing, detecting electrode upper portion with be used for rotating electrode's device to be connected.
Preferably, the means for rotating the electrode is a rotating disk system or a rotating ring disk system.
Preferably, the connection mode between the connection port and the connecting piece adopts threaded fit connection, frosted mouth fit connection or hot melt adhesive.
Preferably, the bearing is a sealed bearing.
Preferably, the electrolytic cell is connected with a liquid level control device;
the electrolytic cell comprises a shell, wherein an optical window sheet, at least one overflow port and a liquid leakage port are arranged on the bottom surface of the shell, the liquid leakage port is connected with a liquid outlet pipe, and the overflow port is connected with a liquid inlet pipe; a structure for introducing an electrode is arranged in the electrolytic cell;
the liquid level control device comprises a waste liquid overflow pipe and a waste liquid discharge pipe;
the liquid outlet pipe is communicated with the waste liquid overflow pipe through a hose.
Preferably, the axis of the connection port and the center of the optical window are on the same straight line.
Preferably, the structure for introducing the electrode comprises a counter electrode liquid contact tube, an outlet of the counter electrode liquid contact tube is positioned in the shell, the outlet of the counter electrode liquid contact tube is vertically downward, and a vertical distance between the outlet of the counter electrode liquid contact tube and the bottom surface of the shell is 0.05-1 mm.
Preferably, the structure for introducing the electrode comprises a reference electrode liquid contact tube, an outlet of the reference electrode liquid contact tube is positioned in the shell, the outlet of the reference electrode liquid contact tube is vertically downward, and a vertical distance between the outlet of the reference electrode liquid contact tube and the optical window sheet is 0.05-1 mm.
Preferably, an air inlet pipe is arranged in the electrolytic cell, an outlet of the air inlet pipe is positioned in the shell, and an outlet direction of the air inlet pipe faces the optical window sheet.
Preferably, the upper part or the side surface of the electrolytic cell is also provided with a structure for air outlet.
The utility model provides a connecting structure with sealing and electrode rotating functions, which can couple and connect a traditional rotating electrode system and a sealed electrolytic cell, so that the gas atmosphere in the sealed electrolytic cell can be better controlled in experiments related to the rotating electrode. Therefore, the utility model has good application prospect.
It should be apparent that, in light of the foregoing, various modifications, substitutions and alterations can be made herein without departing from the spirit and scope of the utility model as defined by the appended claims.
The above-described aspects of the present utility model will be described in further detail below with reference to specific embodiments in the form of examples. It should not be understood that the scope of the above subject matter of the present utility model is limited to the following examples only. All techniques implemented based on the above description of the utility model are within the scope of the utility model.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
FIG. 2 is a plan view of the electrolytic cell of example 2 with the upper part omitted;
FIG. 3 is a cross-sectional view of the electrolytic cell of example 2 taken along the plane of FIG. 2 A-A';
FIG. 4 is a cross-sectional view of the electrolytic cell of example 2 taken along the plane of FIG. 2B-B';
FIG. 5 is a cross-sectional view of the electrolytic cell of example 2 taken along the plane of FIG. 2C-C';
FIG. 6 is a schematic view of the liquid level control apparatus in embodiment 2;
FIG. 7 is a schematic view showing the positional relationship of the respective members in embodiment 2;
FIG. 8 is a schematic diagram showing the positional relationship between a droplet-type single crystal electrode and the solution level in example 2;
FIG. 9 is a schematic diagram showing the positional relationship between the encapsulated electrode and the solution level in example 2.
1-electrolytic cell, 101-shell, 1011-connector, 1012-connector, 1013-bearing, 102-optical window, 103-liquid outlet pipe, 104-liquid inlet pipe, 105-gas inlet pipe, 106-counter electrode liquid contact pipe, 107-reference electrode liquid contact pipe, 2-liquid level control device, 201-waste liquid overflow pipe, 202-waste liquid drain pipe, 3-support, 4-solution storage tank, 5-reference electrode, 6-counter electrode, 7-detection electrode, 701-electrode material, 702-sealed shell.
Detailed Description
Example 1
The rotary electrode electrochemical detection device of the present embodiment is shown in fig. 1, and comprises an electrolytic cell 1 and a device for rotary electrodes, wherein the electrolytic cell 1 can be selected from various existing electrolytic cells 1 with sealing function and the arrangement direction of the detection electrode 7 is downward. The means for rotating the electrode may be selected from an existing rotating disk system or a rotating ring disk system.
The electrolytic cell 1 is provided with a connecting port 1011, the connecting port 1011 is provided with a connecting piece 1012, the connecting port 1011 and the connecting piece 1012 are sealed, and the optional connecting mode comprises screw thread fit connection, frosted mouth fit connection or hot melt adhesive.
The connecting piece 1012 is provided with a bearing 1013, an outer ring of the bearing 1013 is fixedly connected with the connecting piece 1012, a detection electrode 7 is fixed in an inner ring of the bearing 1013, and the upper part of the detection electrode 7 is connected with the device for rotating the electrode. The bearing 1013 is a sealed bearing.
The device of this embodiment enables a coupled connection between the rotary electrode system and the sealed electrolytic cell.
Example 2
In this embodiment, taking a specific structure of the electrolytic cell 1 as an example, an electrochemical detection system using the rotary electrode electrochemical detection device of embodiment 1 is provided, and as shown in fig. 2 to 7, the system includes the electrolytic cell 1, a liquid level control device 2, a solution storage tank 4, a reference electrode 5, and a counter electrode 6.
The electrolytic cell 1 comprises a shell 101, wherein an optical window 102, at least one overflow port and a liquid leakage port are arranged on the bottom surface of the shell 101, the liquid leakage port is connected with a liquid outlet pipe 103, and the overflow port is connected with a liquid inlet pipe 104. The overflow and drain openings are evenly distributed on the sides of the optical window 102. In this embodiment, the number of overflow ports is three, and the number of corresponding liquid inlet pipes 104 is three, so that three different solutions can be introduced into the electrolytic cell 1 in an overflow manner, so as to meet the requirements of switching or mixing the solutions in the test. Each liquid inlet pipe 104 is connected with one solution storage tank 4 through a hose respectively, and the flow rate of the solution flowing out of the solution storage tank 4 can be controlled through a peristaltic pump or the opening of a valve at the outlet of the solution storage tank 4.
The liquid level control device 2 comprises a waste liquid overflow pipe 201 and a waste liquid discharge pipe 202; the liquid outlet pipe 103 and the waste liquid overflow pipe 201 are communicated through a hose. When the electrochemical is performed, the electrolytic cell 1 and the liquid level control device 2 form a communicating vessel through the hose, and the height of the liquid level of the solution in the electrolytic cell 1 (namely, the thickness of the solution layer) can be controlled by adjusting the height of the liquid level control device 2. The control accuracy of the conventional optical elevating table and other devices is high enough to control the height of the liquid level control device 2, and the thickness of the solution layer in the electrolytic cell 1 can be controlled within 1 mm.
The electrolytic cell 1 is provided with a structure for introducing electrodes, and a common three-electrode detection system needs to introduce a detection electrode 7, a reference electrode 5 and a counter electrode 6 into the electrolytic cell 1.
The top of the electrolytic cell 1 is provided with a connection port 1011 for connecting the detection electrode 7, and the axis of the connection port 1011 and the center of the optical window 102 are on the same line. The detection electrode 7 can be inserted into the electrolytic cell 1 through the connection port 1011 until the surface of the detection electrode 7 just contacts the solution. At this time, only a solution layer smaller than 1mm is provided from the surface of the detection electrode 7 to the surface of the optical window 102, so that the requirements of raman spectrum detection can be satisfied. Meanwhile, the solution is continuously added through the overflow port, and is continuously discharged through the liquid leakage port, so that the solution in the solution layer continuously flows, and the mass transfer requirement of biochemical reaction can be met.
When it is necessary to control the gas atmosphere in the electrolytic cell 1, the detection electrode 7 and the connection port 1011 can be sealed. The connecting port 1011 is provided with a connecting piece 1012, the connecting piece 1012 is provided with a bearing 1013, an outer ring of the bearing 1013 is fixedly connected with the connecting piece 1012, and an inner ring of the bearing 1013 is used for fixing the detection electrode 7. The connection port 1011 and the connection piece 1012 are in sealing connection, and the bearing 1013 is a sealing bearing.
The present embodiment does not need to be pressed and sealed by a large number of sealing members, so that the distance between the detection electrode 7 and the optical window 102 is more freely adjusted, and can be flexibly controlled according to the form or structure of the detection electrode 7. For example, in a preferred embodiment, the detection electrode 7 is a droplet type (bead type) single crystal electrode, which is characterized by a hemispherical shape (the upper portion of which can be connected to a cylindrical connecting member to achieve engagement with the inner race of the bearing 1013), the hemispherical plane being a single crystal surface, and the spherical surface being a non-single crystal surface. In the study, researchers were generally concerned only with the reactions that occur on the single crystal planes. However, when a hemispherical plane (single crystal face) is contacted with a solution, hemispherical spherical surfaces (non-single crystal faces) are always likely to contact the solution due to infiltration or the like of the solution, thereby generating a signal that interferes with detection. In this case, the solution is to slightly raise the drop-type monocrystal electrode, and pull a "meniscus" above the liquid surface of the solution by the action of the surface tension of the liquid (as shown in fig. 8), so that the spherical surface of the side surface is hardly contacted with the solution, and the interference signal generated by the spherical surface is almost negligible. In other embodiments, the detection electrode 7 is a packaged electrode, and the structure of the detection electrode includes an electrode material 701 and a sealing shell 702 wrapped on the side surface of the electrode material, so that the detection electrode 7 can directly control the electrode surface to be level with the solution surface (as shown in fig. 9) because the problem of water drop type single crystal electrode side interference signals does not exist. The degree of freedom in controlling the height of the detection electrode 7 cannot be achieved in the conventional sealed raman spectrum flow cell.
The structure for introducing the electrode comprises a counter electrode liquid contact tube 106, wherein an outlet of the counter electrode liquid contact tube 106 is positioned in the shell 101, the outlet of the counter electrode liquid contact tube 106 is vertically and downwards arranged, and the vertical distance between the outlet of the counter electrode liquid contact tube 106 and the bottom surface of the shell 101 is 0.05-1 mm. The electrode assembly further comprises a counter electrode 6, and the counter electrode 6 is a glass tube with two open ends, and the side surface of the glass tube is provided with a noble metal wire or a noble metal sheet in a penetrating way. One end of the glass tube is communicated with the counter electrode liquid contact tube 106 through a hose, and the other end is provided with a valve. In the detection, the glass tube and the counter electrode liquid contact tube 106 are filled with the electrolyte solution, and the electrolyte solution in the counter electrode liquid contact tube 106 is made to communicate with the solution layer in the electrolytic cell at the outlet, that is, the communication of the detection electrode 7 with the counter electrode is achieved.
The structure for introducing the electrode comprises a reference electrode liquid contact tube 107, wherein the outlet of the reference electrode liquid contact tube 107 is positioned in the shell 101, the outlet of the reference electrode liquid contact tube 107 is vertically downward, and the vertical distance between the outlet of the reference electrode liquid contact tube 107 and the optical window sheet 102 is 0.05-1 mm. The structure of the reference electrode 5 can adopt any reference electrode in the prior art, the reference electrode 5 is communicated with the reference electrode liquid contact tube 107 through a hose, and the electrolyte solution in the reference electrode liquid contact tube 107 is communicated with the solution layer in the electrolytic cell at an outlet, namely the communication between the detection electrode 7 and the reference electrode 5 is realized.
In order to control the gas atmosphere in the electrolytic cell 1, an air inlet pipe 105 is arranged in the electrolytic cell 1, an outlet of the air inlet pipe 105 is positioned in the shell 101, and an outlet direction of the air inlet pipe 105 faces the optical window sheet 102. In order to balance the gas pressure, the upper part or the side surface of the electrolytic cell 1 is also provided with a structure for discharging gas. Specifically, an air outlet or an air outlet pipe may be additionally provided on the housing 101 of the electrolytic cell 1.
In the device of the embodiment, the outer shell 101 of the electrolytic cell 1 is made of glass, so that the interior of the electrolytic cell 1 can be conveniently observed; the optical window 102 may be selected from existing raman detection windows so that a spectroscopic signal can be collected by raman spectroscopy under the electrolytic cell 1. The raman detection window may be a quartz window, and the quartz window and the glass housing 101 may be baked by a glass lamp technology, or may be bonded and sealed by a hot melt adhesive. The hose for connecting the parts is made of polytetrafluoroethylene so as to reduce pollution of the solution.
According to the embodiment, the rotatable sealed electrolytic cell with the detection electrode 7 is constructed, the rotation of the detection electrode 7 can be realized, the atmosphere of detection gas is controlled, the functions of synchronously collecting Raman spectrum and electrochemical signals and the like are performed, the requirements of various research scenes can be met, and the rotatable sealed electrolytic cell has a good application prospect in the related research of Raman spectrum and electrochemical of biological medicine.
Claims (10)
1. An electrochemical detection device for a rotary electrode, which is characterized in that: including electrolytic cell (1) and be used for rotatory electrode's device, be provided with connector (1011) on electrolytic cell (1), be provided with connecting piece (1012) on connector (1011), be provided with bearing (1013) on connecting piece (1012), the outer lane and the connecting piece (1012) fixed connection of bearing (1013), be fixed with in the inner circle of bearing (1013) and detect electrode (7), detect electrode (7) upper portion with be used for rotatory electrode's device to be connected.
2. The rotary electrode electrochemical detection device according to claim 1, wherein: the device for rotating the electrode is a rotating disc system or a rotating ring disc system.
3. The rotary electrode electrochemical detection device according to claim 1, wherein: the connection mode between the connection port (1011) and the connection piece (1012) adopts screw thread fit connection, frosted mouth fit connection or hot melt adhesive bonding.
4. The rotary electrode electrochemical detection device according to claim 1, wherein: the bearing (1013) is a sealed bearing.
5. The rotary electrode electrochemical detection device according to claim 1, wherein: the electrolytic cell (1) is connected with a liquid level control device (2);
the electrolytic cell (1) comprises a shell (101), wherein an optical window (102), at least one overflow port and a liquid leakage port are arranged on the bottom surface of the shell (101), the liquid leakage port is connected with a liquid outlet pipe (103), and the overflow port is connected with a liquid inlet pipe (104); a structure for introducing electrodes is arranged in the electrolytic cell (1);
the liquid level control device (2) comprises a waste liquid overflow pipe (201) and a waste liquid discharge pipe (202);
the liquid outlet pipe (103) is communicated with the waste liquid overflow pipe (201) through a hose.
6. The rotary electrode electrochemical detection device according to claim 5, wherein: the axis of the connection port (1011) and the center of the optical window (102) are on the same straight line.
7. The rotary electrode electrochemical detection device according to claim 5, wherein: the structure for introducing the electrode comprises a counter electrode liquid contact tube (106), wherein an outlet of the counter electrode liquid contact tube (106) is positioned in the shell (101), the outlet of the counter electrode liquid contact tube (106) is vertically downwards arranged, and the vertical distance between the outlet of the counter electrode liquid contact tube (106) and the bottom surface of the shell (101) is 0.05-1 mm.
8. The rotary electrode electrochemical detection device according to claim 5, wherein: the structure for introducing the electrode comprises a reference electrode liquid contact tube (107), wherein an outlet of the reference electrode liquid contact tube (107) is positioned in the shell (101), the outlet of the reference electrode liquid contact tube (107) is vertically downwards arranged, and the vertical distance between the outlet of the reference electrode liquid contact tube (107) and the optical window (102) is 0.05-1 mm.
9. The rotary electrode electrochemical detection device according to claim 5, wherein: an air inlet pipe (105) is arranged in the electrolytic cell (1), an outlet of the air inlet pipe (105) is positioned in the shell (101), and the outlet direction of the air inlet pipe (105) faces the optical window sheet (102).
10. The rotary electrode electrochemical detection device according to claim 9, wherein: the upper part or the side surface of the electrolytic cell (1) is also provided with a structure for air outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202321502709.2U CN220154338U (en) | 2023-06-13 | 2023-06-13 | Rotary electrode electrochemical detection device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202321502709.2U CN220154338U (en) | 2023-06-13 | 2023-06-13 | Rotary electrode electrochemical detection device |
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| CN220154338U true CN220154338U (en) | 2023-12-08 |
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| CN202321502709.2U Active CN220154338U (en) | 2023-06-13 | 2023-06-13 | Rotary electrode electrochemical detection device |
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