Three-electrode testing apparatus and testing method

Abstract

This invention relates to a three-electrode testing device and method. The testing device includes a solution container, a worktable, a working electrode, a reference electrode, and a counter electrode. The worktable is provided with an adjusting screw, a moving block, a counter electrode mounting hole, a reference electrode mounting hole, and a scale. The moving block is provided with a working electrode mounting hole. The working electrode mounting hole, the counter electrode mounting hole, and the reference electrode mounting hole are used to install the working electrode, the counter electrode, and the reference electrode, respectively. The adjusting screw is threadedly engaged with the moving block. The rotation of the adjusting screw can precisely adjust the position of the moving block on the worktable, away from or closer to the counter electrode mounting hole. The position of the moving block can be reflected in the reading of the scale. In this way, the distance between the working electrode and the counter electrode can be quantified, which is beneficial for three-electrode testing. The testing method using this device is simple to operate and can reproduce three-electrode tests.

Description

Technical Field

[0001] This invention relates to the field of electrochemical testing technology, and in particular to a three-electrode testing device and testing method. Background Technology

[0002] The so-called three-electrode system is designed to eliminate the large errors in electrode potential caused by polarization current. It introduces a reference electrode to stabilize the working electrode, based on the ordinary two-electrode system (working electrode and counter electrode). The electrolytic cell consists of three electrodes: the working electrode, the counter electrode, and the reference electrode. The working electrode is the main object of electrode research and operation, the reference electrode is the comparison standard for the potential electrode, and the counter electrode is mainly used to polarize the counter electrode by passing polarization current. Different working electrodes are used depending on the test object. When testing the electrode sheet, electrode clamps are used to hold the electrode sheet in place. See [link to relevant documentation]. Figure 1 When testing powders, a glassy carbon electrode is selected as the working electrode. See [link / reference]. Figure 2 The counter electrode is usually a platinum sheet counter electrode, see [reference needed]. Figure 3 Existing three-electrode testing devices often exhibit errors in single measurements under the same conditions, leading to difficulties in reproducing three-electrode tests and raising questions about the accuracy of single measurements. After careful observation, the inventors discovered that the main reason for this result is that existing three-electrode testing devices do not quantify the distance between the working electrode and the counter electrode. Summary of the Invention

[0003] The purpose of this invention is to solve the above-mentioned problems and provide a three-electrode testing device and testing method.

[0004] The technical solution of this invention is: a three-electrode testing device, comprising a solution container, a worktable, a working electrode, a reference electrode, and a counter electrode; wherein the working electrode is further divided into two forms depending on the test object: electrode clamping electrode sheet and glassy carbon electrode; while the counter electrode is a commonly used platinum sheet counter electrode; the worktable is mounted on the solution container; the worktable is provided with an adjusting screw and a moving block; the top surface of the worktable is provided with a horizontally arranged T-shaped groove A; the T-shaped groove A includes a horizontally arranged sliding hole A and a vertically arranged through hole A on the upper and lower surfaces of the worktable; the adjusting screw passes through the sliding hole A along the direction of the through hole A; the end of the adjusting screw extends beyond the side of the worktable and is provided with an operating end; operating the operating end can drive the adjusting screw to rotate; the moving block is embedded in the sliding hole A, and its bottom slides in cooperation with the inner end face of the sliding hole A; the moving block is provided with a vertically arranged... The working electrode mounting hole is used to install the working electrode; this working electrode mounting hole is located directly above the through hole A, allowing the working electrode to enter the solution container through the through hole A; the moving block is threadedly engaged with the adjusting screw on one side of the working electrode mounting hole; the moving block is restricted by the rotating adjusting screw and the inner end face of the sliding hole A, and can only move laterally along the axis of the adjusting screw; a vertical counter electrode mounting hole is provided on the worktable directly opposite the end of the through hole A, used to install the counter electrode; the lateral movement of the moving block can just be converted into the working electrode moving closer to or further away from the counter electrode; a scale is provided on the worktable on one side of the T-shaped groove A, set in the direction of the through hole A; the distance between the working electrode and the counter electrode can be directly reflected on the scale; a vertical reference electrode mounting hole is also provided on the worktable, used to install the reference electrode.

[0005] Preferably, the operating end of the adjusting screw is a hexagonal prism, which is convenient for hand-held rotation to drive the adjusting screw to rotate.

[0006] Preferably, the bottom of the workbench is provided with a step for embedding the port of the solution container; the step and the port of the solution container form a tight fit to prevent the solution from splashing out from the edge of the solution container.

[0007] Preferably, the working electrode includes mounting rod A; the reference electrode includes mounting rod B; and the counter electrode includes mounting rod C. Mounting rods A, B, and C respectively allow the working electrode, counter electrode, and reference electrode to extend below the liquid surface in the solution container. Mounting rods A, B, and C are all vertically hollow, with wires extending from their upper ends to their lower ends, used to connect the test points of the working electrode, counter electrode, and reference electrode, respectively. The diameter of mounting rod A matches the diameter of the working electrode mounting hole, used to lock mounting rod A in place. The diameter of mounting rod B matches the diameter of the reference electrode mounting hole, used to lock mounting rod B in place. The diameter of mounting rod C matches the diameter of the counter electrode mounting hole, used to lock mounting rod C in place.

[0008] Furthermore, rubber sleeves are fitted at the same axial positions on mounting rods A, B, and C; the rubber sleeves of mounting rods A, B, and C respectively mate with the inner walls of the working electrode mounting hole, reference electrode mounting hole, and counter electrode mounting hole; the maximum outer diameter of the rubber sleeves is larger than the corresponding electrode mounting holes; because the rubber sleeves have a certain radial shrinkage capacity and a certain friction on their outer surface, they can be inserted into the corresponding electrode mounting holes to form a stable connection.

[0009] Preferably, the working electrode is a glassy carbon electrode; the glassy carbon section of this glassy carbon electrode is horizontally oriented towards the mounting hole of the counter electrode; when testing powder materials, the powder needs to be loaded onto the glassy carbon electrode; the powder needs to be ground off after the glassy carbon electrode has been used; as the number of uses of the glassy carbon electrode increases, the glassy carbon electrode is also forced to undergo a certain amount of grinding; the length of the glassy carbon section of the glassy carbon electrode becomes shorter, and the test results show errors; the moving block is provided with a mounting block, a hexagonal block, and an eccentric cylinder; the top surface of the moving block is provided with a horizontally arranged T-shaped groove B; the T-shaped groove B includes a horizontally arranged sliding hole B and a vertical through hole B arranged above and below the moving block; the through hole B coincides with the through hole A; the mounting block and the hexagonal block are installed. Inside the sliding hole B; the working electrode mounting hole is set on the mounting block for mounting the glassy carbon electrode; one side of the mounting block is in contact with the side wall of the sliding hole B; the other side of the mounting block is provided with a hexagonal block; the bottom of the mounting block and the bottom of the hexagonal block both abut against the inner end of the sliding hole B; this allows the mounting block to be manually adjusted so that the mounting block carries the glassy carbon electrode along the sliding hole B, thereby adjusting the position of the glassy carbon electrode; the eccentric cylindrical body is cylindrical and is vertically fitted inside the hexagonal block at the eccentric position; the top of the eccentric cylindrical body is provided with an insertion hole; this insertion hole is used to insert a columnar object, which can drive the eccentric cylindrical body to rotate; the bottom end of the eccentric cylindrical body extends downward with a threaded column; The threaded column engages with the inner thread of the sliding hole B and is offset from the axis of the eccentric cylinder. The hexagonal block and the eccentric cylinder constitute an eccentric clamping mechanism. Within this eccentric clamping mechanism, the rotation of the eccentric cylinder body can be controlled through the insertion hole. The rotation of the eccentric cylinder body can change the shape and position of the hexagonal block. This change in shape and position allows the hexagonal block's side to clamp or release the mounting block. Because this eccentric clamping mechanism has two eccentric settings—the eccentricity of the eccentric cylinder body relative to the hexagonal block and the eccentricity of the threaded column relative to the eccentric cylinder body—the reaction force of the mounting block cannot directly act on the threaded column, let alone drive its rotation. Therefore, this eccentric clamping mechanism... The structure has good self-locking capability; the moving block has a downward-extending calibration plate on the side facing the electrode mounting hole; the calibration plate passes downward through through hole B and through hole A; the bottom of the calibration plate penetrates the solution container to a depth not exceeding the test depth of the glassy carbon electrode; periodically, the moving block is moved to the position closest to the electrode mounting hole by adjusting the screw, then the clamping state of the hexagonal block on the mounting block is released, the position of the mounting block in the sliding hole B is manually adjusted so that the glassy carbon segment end of the glassy carbon electrode abuts against the end face of the calibration plate, and finally the hexagonal block is driven to clamp the mounting block, thus completing the calibration work of the glassy carbon segment end of the glassy carbon electrode; the interval between two adjacent calibration work can also be the corresponding number of uses.

[0010] Preferably, the helix angle of the adjusting screw is smaller than the friction angle of the adjusting screw, thereby achieving the self-locking function between the adjusting screw and the moving block.

[0011] A testing method using the above-described three-electrode testing apparatus includes the following steps:

[0012] ① Install the working electrode, reference electrode, and counter electrode.

[0013] Locate the working electrode mounting hole, reference electrode mounting hole, and counter electrode mounting hole on the worktable; insert the working electrode, reference electrode, and counter electrode into the corresponding working electrode mounting hole, reference electrode mounting hole, and counter electrode mounting hole from bottom to top to the appropriate extent;

[0014] ② Attach the workbench to the port of the solution container;

[0015] ③ Connect the working electrode wire, the reference electrode wire, and the counter electrode wire to the electrochemical workstation.

[0016] ④ Perform three-electrode testing

[0017] The operating terminal drives the adjusting screw to rotate; the adjusting screw moves the moving block and the working electrode closer to or away from the counter electrode; after the working electrode moves to a suitable distance, the reading of the electrochemical workstation and the reading reflected on the scale by the moving block are recorded.

[0018] ⑤ Reproduce the three-electrode test

[0019] The working electrode is moved back and forth by controlling the operation terminal; when the reading reflected on the scale by the moving block is consistent with the reading in step ④, the reading of the electrochemical workstation is recorded for verification.

[0020] Preferably, the electrode in step ① is a glassy carbon electrode; the glassy carbon segment of the glassy carbon electrode faces the counter electrode; the moving block is provided with a mounting block, a hexagonal block, an eccentric cylinder, and a calibration plate; the working electrode mounting hole is provided on the mounting block;

[0021] Between steps ② and ③, the following process also takes place:

[0022] The operating end drives the adjusting screw to rotate; the adjusting screw moves the moving block and the working electrode to the position closest to the counter electrode; the eccentric cylinder releases the clamping state of the hexagonal block on the mounting block; the position of the mounting block is manually adjusted so that the glassy carbon section end of the carbon electrode is in close contact with the calibration plate; and the eccentric cylinder restores the clamping state of the hexagonal block on the mounting block.

[0023] The beneficial effects of the present invention are as follows: The three-electrode testing device of the present invention has the following advantages:

[0024] (1) The present invention adjusts the screw and the moving block to make the working electrode move closer to or away from the counter electrode, thereby minimizing external interference; the position of the working electrode can be reflected on the scale, thereby quantifying the distance between the working electrode and the counter electrode; the present invention can realize the reproduction of three-electrode test and has high accuracy in a single measurement.

[0025] (2) The rubber sleeve of the present invention can form a stable connection with the working electrode mounting hole, the reference electrode mounting hole and the counter electrode mounting hole by means of its own elastic properties, and can limit the working electrode, the reference electrode and the counter electrode to the same depth in the solution container;

[0026] (3) The working electrode of the present invention is a glassy carbon electrode; the moving block of the present invention is provided with a mounting block, a hexagonal block, an eccentric cylinder and a calibration plate; the working electrode mounting hole is set on the mounting block; the eccentric cylinder can cooperate with the hexagonal block to clamp the mounting block; when the glassy carbon section of the glassy carbon electrode is worn, the position of the mounting block can be manually adjusted so that the end of the glassy carbon section abuts against the side of the calibration plate and then clamped; this can avoid the glassy carbon section of the glassy carbon electrode from being worn and causing inaccurate three-electrode testing;

[0027] The testing method using this three-electrode testing device is simple to operate. The adjusting screw and the moving block precisely move the working electrode, and the positional changes of the working electrode can be reflected on the scale of the worktable; thus, the three-electrode test can be reproduced. Attached Figure Description

[0028] Figure 1 It is a three-dimensional view of the working electrode clamping the electrode plate;

[0029] Figure 2 This is a 3D view of a glassy carbon electrode;

[0030] Figure 3 This is a three-dimensional view of the platinum sheet electrode;

[0031] Figure 4 This is a perspective view of the three-electrode testing device of the present invention in Embodiment 1;

[0032] Figure 5 This is a perspective view of the three-electrode testing device of the present invention in use in Embodiment 1;

[0033] Figure 6 yes Figure 5 Top view;

[0034] Figure 7 yes Figure 6 AA section view;

[0035] Figure 8 This is a perspective view of the three-electrode testing device of the present invention in Embodiment 2;

[0036] Figure 9 This is a perspective view of the three-electrode testing device of the present invention in use in Embodiment 2;

[0037] Figure 10 yes Figure 9 Top view;

[0038] Figure 11yes Figure 10 BB cross-sectional view;

[0039] Figure 12 yes Figure 11 A magnified view of the I-shaped image;

[0040] Figure 13 It is a 3D view of the mounting block and the hexagonal block in contact;

[0041] In the diagram: 1. Solution container, 2. Workbench, 21. Adjusting screw, 211. Operating end, 22. Moving block, 221. Working electrode mounting hole, 222. Mounting block, 223. Hexagonal block, 224. Eccentric cylinder, 2241. Insertion hole, 2242. Threaded column, 225. T-slot B, 2251. Sliding hole B, 2252. Through hole B, 226. Calibration plate, 23. T-slot A, 231. Sliding hole A, 232. 24. Through hole A, 25. Counter electrode mounting hole, 26. Scale, 27. Reference electrode mounting hole, 28. Step, 3. Working electrode, 311. Electrode clamp, 3111. Eccentric wheel clamping mechanism, 3112. Electrode sheet, 3113. Concave seat, 312. Glassy carbon segment, 313. Mounting rod A, 314. Mounting rod C, 315. Wire, 316. Rubber sleeve, 4. Reference electrode, 5. Counter electrode, 51. Inverted L-shaped plate, 52. Platinum sheet. Detailed Implementation

[0042] Example 1: See Figure 1-7 A three-electrode testing device includes a solution container 1, a worktable 2, a working electrode 3, a reference electrode 4, and a counter electrode 5. The working electrode 3, depending on the test object, is further divided into two forms: an electrode clamp 311 clamping an electrode sheet 3112 and a glassy carbon electrode. The counter electrode 5 uses a commonly used platinum sheet 52. In this embodiment, the working electrode 3, which uses an electrode clamp 311 to clamp the electrode sheet 3112, includes an eccentric wheel clamping mechanism 3111, an electrode sheet 3112, and a concave seat 3113. The electrode sheet 3112 is disposed in the concave seat. Inside seat 3113; eccentric wheel clamping mechanism 3111 is located on one side of concave seat 3113 and acts on electrode plate 3112; working electrode 3 using glassy carbon electrode is a glassy carbon section 312 with one end horizontal; platinum sheet 52 to electrode 5 includes inverted L-shaped plate 51 and platinum sheet 52; the end of the inverted L-shaped plate 51 is connected to platinum sheet 52; the inner side of the inverted L-shaped plate 51 matches the outer side of concave seat 3113; in this way, the inner side of the inverted L-shaped plate 51 can be fastened to the outer edge of concave seat 3113, so that the distance between platinum sheet 52 and electrode plate 3112 is minimized. See Figure 7 As shown.

[0043] A workbench 2 is mounted on a solution container 1. The workbench 2 is equipped with an adjusting screw 21 and a moving block 22. The top surface of the workbench 2 is provided with a horizontally arranged T-shaped groove A 23. This T-shaped groove A 23 includes a horizontally arranged sliding hole A 231 and a vertically arranged through hole A 232. The adjusting screw 21 passes through the sliding hole A 231 along the direction of the through hole A 232. The end of the adjusting screw 21 extends beyond the side of the workbench 2 and is provided with an operating end 211. Operating the operating end 211 can drive the adjusting screw 21 to rotate. The moving block 22 is embedded in the sliding hole A 231, with its bottom slidingly engaging with the inner end face of the sliding hole A 231. The moving block 22 is provided with a vertical working electrode mounting hole 221 for mounting a working electrode 3. This working electrode mounting hole 221 is located directly above the through hole A 232, allowing the working electrode 3 to be mounted from... The through hole A 232 enters the solution container 1; the moving block 22 is threadedly engaged with the adjusting screw 21 on one side of the working electrode mounting hole 221; the moving block 22 is restricted by the rotating adjusting screw 21 and the inner end face of the sliding hole A 231, and can only move laterally along the axis of the adjusting screw 21; the worktable 2 directly opposite the end of the through hole A 232 is provided with a vertical counter electrode mounting hole 24 for mounting the counter electrode 5; the lateral movement of the moving block 22 can just be converted into the working electrode 3 moving closer to or further away from the counter electrode 5; the worktable 2 on one side of the T-shaped groove A 23 is provided with a scale 25 set in the direction of the through hole A 232; the distance between the working electrode 3 and the counter electrode 5 can be directly reflected on the scale 25; the worktable 2 is also provided with a vertical reference electrode mounting hole 26 for mounting the reference electrode 4.

[0044] In this embodiment, the rotation of the operating end 211 can be precisely converted into the movement of the working electrode 3 relative to the counter electrode 5 through the threaded engagement of the adjusting screw 21 and the moving block 22. The amount of movement of the working electrode 3 can be reflected in the reading of the scale 25 on the worktable 2. That is, a certain fixed point of the moving block 22 points to the scale 25, and the movement of the moving block 22 changes the reading on the scale 25. The difference in the reading can quantify the distance of the moving block 22, i.e., the working electrode 3, from the counter electrode 5. In this way, the three-electrode testing device of this embodiment can quantify the distance change of the working electrode 3 and the counter electrode 5 during the test, and eliminate external interference as much as possible. The test repeatability is high, the single measurement accuracy is high, and it is trustworthy. The external interference includes, but is not limited to, the change in the posture of the working electrode 3 and the counter electrode 5 caused by the touch of a human hand.

[0045] The operating end 211 of the adjusting screw 21 is a hexagonal prism, which makes it easy to rotate by hand to drive the adjusting screw 21 to rotate.

[0046] The bottom of the workbench 2 is provided with a step 27 that is embedded in the port of the solution container 1; the step 27 forms a tight fit with the port of the solution container 1 to prevent the solution from splashing out from the edge of the solution container 1.

[0047] The working electrode 3 includes mounting rod A 313; the reference electrode 4 includes mounting rod B; and the counter electrode 5 includes mounting rod C 314. Mounting rods A 313, B, and C 314 respectively allow the working electrode 3, counter electrode 5, and reference electrode 4 to extend below the liquid surface in the solution container 1. Mounting rods A 313, B, and C 314 are all vertically hollow, with wires 315 extending from their upper ends to their lower ends, used to connect the test points of the working electrode 3, counter electrode 5, and reference electrode 4, respectively. The wires 315 are flexible. The electrode clip 311 of the electrochemical workstation is clipped onto the wire 315. If the workstation electrode clip 311 is directly clipped onto the electrode, the interaction force between the electrode clip 311 and the electrode will change the electrode position. The diameter of mounting rod A 313 matches the diameter of the working electrode mounting hole 221 and is used to lock mounting rod A 313. The diameter of mounting rod B matches the diameter of the reference electrode mounting hole 26 and is used to lock mounting rod B. The diameter of mounting rod C 314 matches the diameter of the electrode mounting hole 24 and is used to lock mounting rod C 314.

[0048] Rubber sleeves 316 are fitted at the same axial positions of mounting rods A, B, and C 314. The rubber sleeves 316 of mounting rods A, B, and C 314 respectively mate with the inner walls of the working electrode mounting hole 221, the reference electrode mounting hole 26, and the counter electrode mounting hole 24. The maximum outer diameter of the rubber sleeves 316 is larger than the corresponding electrode mounting holes. Because the rubber sleeves 316 have a certain radial shrinkage capacity and a certain friction on their outer surface, they can be inserted into the corresponding electrode mounting holes to form a stable connection. At the same time, the rubber sleeves 316 can also limit the depth to which the working electrode 3, the counter electrode 5, and the reference electrode 4 penetrate into the solution container 1.

[0049] The helix angle of the adjusting screw 21 is less than the friction angle of the adjusting screw 21, thereby realizing the self-locking function between the adjusting screw 21 and the moving block 22.

[0050] The working principle of Example 1: The working electrode 3 is installed in the working electrode mounting hole 221; the counter electrode 5 is installed in the counter electrode mounting hole 24; then the adjusting screw 21 is driven to rotate through the operating end 211; the rotation of the adjusting screw 21 can be accurately converted into the movement of the moving block 22 relative to the counter electrode 5 because of the threaded engagement between the adjusting screw 21 and the moving block 22; the amount of movement of the working electrode 3 can be reflected in the reading of the scale 25 on the worktable 2; the change in the reading can quantify the distance of the moving block 22, i.e., the working electrode 3, from the counter electrode 5.

[0051] Example 2: The working electrode 3 is a glassy carbon electrode; the glassy carbon segment 312 of the glassy carbon electrode is horizontally oriented towards the electrode mounting hole 24; when testing powder materials, the powder needs to be loaded on the glassy carbon electrode; the powder needs to be ground off after the glassy carbon electrode is used; as the number of times the glassy carbon electrode is used increases, the glassy carbon electrode is also forced to undergo a certain amount of grinding; the length of the glassy carbon segment 312 of the glassy carbon electrode becomes shorter, and the test results show errors; in order to solve the above problems, the technical solution of Example 2 is proposed.

[0052] See Figure 8-13Embodiment 2 is basically the same as Embodiment 1, and the similarities will not be repeated. The differences are as follows: the movable block 22 is provided with a mounting block 222, a hexagonal block 223, and an eccentric cylinder 224; the top surface of the movable block 22 is provided with a horizontally arranged T-shaped groove B 225; the T-shaped groove B 225 includes a horizontally arranged sliding hole B 2251 and a vertically arranged through hole B 2252 on the upper and lower surfaces of the movable block 22; the through hole B 2252 coincides with the through hole A 232; the mounting block 222 and the hexagonal block 223 are installed in the sliding hole B 2251; the working electrode mounting hole 221 is provided on the mounting block 222 for mounting a glassy carbon electrode; one side of the mounting block 222 is in contact with the side wall of the sliding hole B 2251; On the other side of mounting block 222, there is a hexagonal block 223; the bottom of mounting block 222 and the bottom of hexagonal block 223 both abut against the inner end of sliding hole B 2251; this allows for manual adjustment of mounting block 222 so that it carries the glassy carbon electrode along sliding hole B 2251, thereby adjusting the position of the glassy carbon electrode; the main body of eccentric cylinder 224 is cylindrical and is vertically fitted inside hexagonal block 223 at the eccentric position; the top of the main body of eccentric cylinder 224 has an insertion hole 2241; this insertion hole 2241 is used to insert a cylindrical object, which can drive the main body of eccentric cylinder 224 to rotate; in this embodiment, the insertion hole 2241 is a countersunk hexagonal socket; a corresponding hexagonal wrench is selected for inserting the cylindrical object. The disassembly tool is a commonly available tool; a threaded post 2242 extends downward from the bottom of the eccentric cylinder 224 body; the threaded post 2242 engages with the inner thread of the sliding hole 2251 and is offset from the axis of the eccentric cylinder 224; the hexagonal block 223 and the eccentric cylinder 224 constitute an eccentric clamping mechanism; within this eccentric clamping mechanism, the rotation of the eccentric cylinder 224 body can be controlled through the insertion hole 2241; the rotation of the eccentric cylinder 224 body can change the shape and position of the hexagonal block 223; the shape and position changes of the hexagonal block 223 achieve the clamping or loosening of the side of the hexagonal block 223 against the mounting block 222; because there are two eccentric settings within this eccentric clamping mechanism, that is, the eccentric cylinder 224 body relative to... The eccentricity of the hexagonal block 223 and the eccentricity of the threaded column 2242 relative to the eccentric cylinder 224 body mean that the reaction force of the mounting block 222 cannot directly act on the threaded column 2242, let alone drive the threaded column 2242 to rotate; therefore, the self-locking capability of this eccentric clamping mechanism is good. The moving block 22 has a downwardly extending calibration plate 226 on the side facing the electrode mounting hole 24; the calibration plate 226 passes downward through the through hole B 2252 and the through hole A 232; the bottom end of the calibration plate 226 penetrates the solution container 1 to a depth not exceeding the test depth of the glassy carbon electrode; the test depth of the glassy carbon electrode refers to the depth of the glassy carbon section 312 of the glassy carbon electrode penetrating into the solution container 1 when the glassy carbon electrode and the electrode 5 are tested.Periodically, the moving block 22 is moved to the position closest to the electrode mounting hole 24 by adjusting the screw. Then, the glassy carbon electrode is pulled up so that the glassy carbon segment 312 of the glassy carbon electrode is at the depth of the calibration plate 226, aligning the glassy carbon segment 312 of the glassy carbon electrode with the calibration plate 226. Next, the clamping state of the hexagonal block 223 on the mounting block 222 is released, and the position of the mounting block 222 in the sliding hole B is manually adjusted so that the end of the glassy carbon segment 312 of the glassy carbon electrode abuts against the end face of the calibration plate 226. Finally, the hexagonal block 223 is driven to clamp the mounting block 222, restoring the depth of the glassy carbon segment 312 of the glassy carbon electrode. This completes the calibration of the end of the glassy carbon segment 312 of the glassy carbon electrode. The interval between two adjacent calibration operations can also be the corresponding number of uses.

[0053] The impact of wear and shortening of the glassy carbon electrode on the accuracy of measurement results; in this embodiment, the working electrode 3 is mounted on a clampable mounting block 222; when the glassy carbon electrode wears and shortens, first adjust the moving block 22 to the position closest to the counter electrode 5; then pull the glassy carbon electrode up so that the glassy carbon segment 312 of the glassy carbon electrode is at a height equivalent to that of the calibration plate 226, and align the glassy carbon segment 312 with the calibration plate 226; next, use the eccentric clamping mechanism to release the clamping state of the mounting block 222, then manually adjust the position of the mounting block 222 so that the end of the glassy carbon electrode is in close contact with the end face of the calibration plate 226, then restore the clamping of the eccentric clamping mechanism on the mounting block 222, and then restore the depth of the glassy carbon segment 312 of the glassy carbon electrode; at this time, the glassy carbon electrode has completed the calibration work and can be used for three-electrode testing.

[0054] Example 3: A testing method using the three-electrode testing device described in Example 1, comprising the following steps:

[0055] ① Install working electrode 3, reference electrode 4, and counter electrode 5.

[0056] Locate the working electrode mounting hole 221, reference electrode mounting hole 26, and counter electrode mounting hole 24 on the worktable 2; insert the working electrode 3, reference electrode 4, and counter electrode 5 into the corresponding working electrode mounting hole 221, reference electrode mounting hole 26, and counter electrode mounting hole 24 from bottom to top to the appropriate extent;

[0057] ② Attach the workbench 2 to the port of the solution container 1; drive the adjusting screw 21 to rotate through the operating end 211; the adjusting screw 21 moves the moving block 22 and the working electrode 3 to the position closest to the counter electrode 5; release the clamping state of the hexagonal block 223 on the mounting block 222 through the eccentric cylinder 224; manually adjust the position of the mounting block 222 so that the end of the glassy carbon section 312 of the carbon electrode is in close contact with the calibration plate 226; then restore the clamping state of the hexagonal block 223 on the mounting block 222 through the eccentric cylinder 224.

[0058] ③ Connect the wire 315 of the working electrode 3, the wire 315 of the reference electrode 4, and the wire 315 of the counter electrode 5 to the electrochemical workstation.

[0059] ④ Perform three-electrode testing

[0060] The operating terminal 211 drives the adjusting screw 21 to rotate; the adjusting screw 21 drives the moving block 22 and the working electrode 3 to move closer to or away from the counter electrode 5; after the working electrode 3 moves to a suitable distance, the reading of the electrochemical workstation and the reading reflected on the scale 25 by the moving block 22 are recorded.

[0061] ⑤ Reproduce the three-electrode test

[0062] The working electrode 3 is moved back and forth by the operating terminal 211; when the reading reflected on the scale 25 by the moving block 22 is consistent with the reading in step ④, the reading of the electrochemical workstation is recorded for verification.

[0063] Example 4: A testing method using the three-electrode testing device described in Example 2, comprising the following steps:

[0064] ① Install working electrode 3, reference electrode 4, and counter electrode 5.

[0065] Locate the working electrode mounting hole 221, reference electrode mounting hole 26, and counter electrode mounting hole 24 on the worktable 2; insert the working electrode 3, reference electrode 4, and counter electrode 5 into the corresponding working electrode mounting hole 221, reference electrode mounting hole 26, and counter electrode mounting hole 24 from bottom to top to the appropriate extent;

[0066] ② Attach workbench 2 to the port of solution container 1;

[0067] ③ Connect the wire 315 of the working electrode 3, the wire 315 of the reference electrode 4, and the wire 315 of the counter electrode 5 to the electrochemical workstation.

[0068] ④ Perform three-electrode testing

[0069] The operating terminal 211 drives the adjusting screw 21 to rotate; the adjusting screw 21 drives the moving block 22 and the working electrode 3 to move closer to or away from the counter electrode 5; after the working electrode 3 moves to a suitable distance, the reading of the electrochemical workstation and the reading reflected on the scale 25 by the moving block 22 are recorded.

[0070] ⑤ Reproduce the three-electrode test

[0071] The working electrode 3 is moved back and forth by the operating terminal 211; when the reading reflected on the scale 25 by the moving block 22 is consistent with the reading in step ④, the reading of the electrochemical workstation is recorded for verification.

Claims

1. A three-electrode test device comprising a solution container, a workbench, a working electrode, a reference electrode, a counter electrode; the workbench is installed on the solution container; characterized in that, The workbench is provided with an adjusting screw and a moving block; the top surface of the workbench is provided with a transversely arranged T-shaped slot A; the T-shaped slot A includes a transversely arranged sliding hole A and a vertically arranged through hole A arranged above and below the workbench; the adjusting screw penetrates the sliding hole A in the direction of the through hole A; the end of the adjusting screw extends beyond the side surface of the workbench and is provided with an operating end; the moving block is embedded in the sliding hole A and is in sliding fit with the bottom of the moving block and the inner end surface of the sliding hole A; the moving block is provided with a vertically arranged working electrode mounting hole; the working electrode mounting hole is located directly above the through hole A; the moving block is in threaded fit with the adjusting screw at the side of the working electrode mounting hole; the workbench provided with the through hole A is provided with a vertically arranged counter electrode mounting hole opposite to the end of the through hole A; the workbench at the side of the T-shaped slot A is provided with a scale arranged in the direction of the through hole A; the workbench is further provided with a vertically arranged reference electrode mounting hole; The working electrode is a glassy carbon electrode; the glassy carbon section of the glassy carbon electrode is horizontally directed to the counter electrode mounting hole; the moving block is provided with a mounting block, a hexagonal block and an eccentric cylinder; the top surface of the moving block is provided with a transversely arranged T-shaped slot B; the T-shaped slot B includes a transversely arranged sliding hole B and a vertically arranged through hole B arranged above and below the moving block; the through hole B is coincided with the through hole A; the mounting block and the hexagonal block are mounted in the sliding hole B; the working electrode mounting hole is arranged on the mounting block; the side surface of one side of the mounting block is in fit with the side wall of the sliding hole B; the other side of the mounting block is provided with the hexagonal block; the bottom of the mounting block and the bottom of the hexagonal block are in abutment with the inner end of the sliding hole B; the main body of the eccentric cylinder is in vertically sleeved fit in the hexagonal block at the eccentric position of the hexagonal block; the main body of the eccentric cylinder is provided with an insertion hole at the top end; the main body of the eccentric cylinder is downwardly extended with a threaded column at the bottom end; the threaded column is in threaded fit with the inner end of the sliding hole B and is deviated from the axis of the eccentric cylinder; the side of the moving block directed to the counter electrode mounting hole is provided with a downwardly extended calibration plate; the calibration plate downwardly penetrates the through hole B and the through hole A; the bottom end of the calibration plate is not more than the testing depth of the glassy carbon electrode in depth when deeply inserted into the solution container.

2. The three-electrode test device of claim 1, wherein: The operating end of the adjusting screw is a hexagonal prism.

3. The three-electrode test device of claim 1, wherein: The bottom of the workbench is provided with a step embedded in the port of the solution container.

4. The three-electrode test device of claim 1, wherein: The working electrode includes a mounting rod A; the reference electrode includes a mounting rod B; the counter electrode includes a mounting rod C; the mounting rod A, the mounting rod B and the mounting rod C are all vertically hollow and the upper end of each is connected with a lead wire extended to the lower end; the diameter of the mounting rod A is matched with the diameter of the working electrode mounting hole; the diameter of the mounting rod B is matched with the diameter of the reference electrode mounting hole; the diameter of the mounting rod C is matched with the diameter of the counter electrode mounting hole.

5. The three-electrode test device of claim 4, wherein: The mounting rod A, the mounting rod B and the mounting rod C are all sleeved with rubber sleeves at the same axial position; the rubber sleeves of the mounting rod A, the mounting rod B and the mounting rod C are respectively matched with the inner wall of the working electrode mounting hole, the reference electrode mounting hole and the counter electrode mounting hole.

6. A test method using the three-electrode test device of claim 1, characterized by: The method comprises the following steps: ① installing the working electrode, the reference electrode and the counter electrode The working electrode mounting hole, the reference electrode mounting hole and the counter electrode mounting hole are found on the workbench; the working electrode, the reference electrode and the counter electrode are respectively inserted into the corresponding working electrode mounting hole, reference electrode mounting hole and counter electrode mounting hole from bottom to top to a suitable degree; ②Put the workbench on the solution container port; when the glassy carbon electrode is shortened due to wear, first adjust the moving block to the nearest position to the counter electrode; then pull up the glassy carbon electrode so that the glassy carbon segment of the glassy carbon electrode is at the same height as the calibration plate and faces the calibration plate; then, use the eccentric clamping mechanism to release the clamping of the mounting block, and then manually adjust the position of the mounting block so that the end of the glassy carbon electrode is in close contact with the end face of the calibration plate, and then restore the clamping of the mounting block by the eccentric clamping mechanism and the depth of the glassy carbon segment of the glassy carbon electrode; at this time, the glassy carbon electrode has completed the calibration work; ③Connect the wires of the working electrode, the wires of the reference electrode, and the wires of the counter electrode to the electrochemical workstation; ④Perform three-electrode test Drive the adjusting screw to rotate through the operation end; the adjusting screw drives the moving block and the working electrode to approach or move away from the counter electrode; after the working electrode is moved to the appropriate distance, record the reading of the electrochemical workstation and the reading reflected by the moving block on the scale; ⑤Repeat the three-electrode test Control the reciprocating movement of the working electrode through the operation end; when the reading reflected by the moving block on the scale is consistent with the reading in step ④, record the reading of the electrochemical workstation for review.

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