CN117907407A - Sulfur titration cell for instant supplementing electrolyte - Google Patents

Sulfur titration cell for instant supplementing electrolyte Download PDF

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Publication number
CN117907407A
CN117907407A CN202211250225.3A CN202211250225A CN117907407A CN 117907407 A CN117907407 A CN 117907407A CN 202211250225 A CN202211250225 A CN 202211250225A CN 117907407 A CN117907407 A CN 117907407A
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CN
China
Prior art keywords
electrolyte
bottle body
bottle
connecting pipe
sulfur
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Pending
Application number
CN202211250225.3A
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Chinese (zh)
Inventor
单石文
李景娆
魏海波
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China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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Application filed by China Petroleum and Chemical Corp filed Critical China Petroleum and Chemical Corp
Priority to CN202211250225.3A priority Critical patent/CN117907407A/en
Publication of CN117907407A publication Critical patent/CN117907407A/en
Pending legal-status Critical Current

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Abstract

The invention relates to the technical field of measuring equipment, in particular to a sulfur titration cell for instant electrolyte replenishment, which comprises a first bottle body component, a second bottle body component and a connecting pipe, wherein the first bottle body component comprises a first bottle body and an air inlet pipe, the second bottle body component comprises a second bottle body, the bottom of the second bottle body is connected with the bottom of the first bottle body through the connecting pipe, and the connecting pipe and the air inlet pipe are respectively connected to two opposite sides of the first bottle body. The gas is input into the electrolyte from the gas inlet pipe for reaction and then is discharged from the first opening part, the solution taken away by the gas flow is instantaneously replenished under the action of the connecting pipe, the solution taken away by the gas flow in unit time is very small, the liquid level fluctuation and the potential fluctuation caused by the replenishing are very small, and the whole system tends to be in a stable state. In addition, the air flow flows at one side far away from the connecting pipe, so that the influence on the electrolyte at one side of the connecting pipe is small, the ion flow efficiency and experimental errors caused by fluid infusion during fluid infusion are reduced, the analysis of a sample is not influenced by the fluid infusion, and the working efficiency is improved.

Description

Sulfur titration cell for instant supplementing electrolyte
Technical Field
The invention relates to the technical field of measuring equipment, in particular to a sulfur titration cell for instant electrolyte replenishment.
Background
The microcoulomb instrument sulfur titrator is an instrument designed by adopting dynamic microcoulomb method principle, and adopts oxidation method to introduce sample into cracking tube for reaction, the measured material is converted into titratable sulfur dioxide, and the carrier gas is introduced into sulfur titration cell for titration, the sulfur dioxide reacts with measured ion in electrolyte to consume measured ion, and the measured ion concentration is reduced, the indication electrode pair indicates the change of this signal, and the changed signal is inputted into coulomb amplifier, then the coulomb amplifier outputs a correspondent current to electrolytic electrode, and at the same time the consumed measured ion is supplemented by electrolysis, according to Faraday law, the total content of measured ion of sample can be calculated by means of output current condition. The microcoulomb instrument sulfur titration cell is the core part of the microcoulomb instrument sulfur titration instrument, and after the to-be-detected object burns to generate gas, the gas reacts with ions in the electrolyte of the sulfur titration cell. And electrolyte in the microcoulomb instrument sulfur titration cell can be reduced under the action of air flow, so that the microcoulomb instrument sulfur titration cell needs to be supplemented with electrolyte in order to ensure the accuracy of experiments.
The existing microcoulomb instrument sulfur titration cell can not automatically and immediately supplement electrolyte, the condition that the liquid level of the electrolyte is lower than the normal range often occurs in the experimental process, and the sensitivity and the conversion rate of the instrument are reduced due to the fact that excessive electrolyte is added at one time, so that the electrolyte is needed to be manually supplemented by a syringe in the sample analysis process, the vibration of the switch titration Chi Xiangmen and the mutation of the liquid level in the titration cell easily cause the fluctuation of the baseline of the instrument in the liquid supplementing process, the interference is generated on the analysis sample of the instrument, the potential of the instrument is changed after the liquid supplementing, and the instrument must be readjusted after the baseline of the instrument is stabilized after the liquid supplementing, so that the time is wasted.
Disclosure of Invention
Based on the above, the invention provides a sulfur titration cell capable of stably completing instant electrolyte replenishing.
The utility model provides a sulphur titration cell of instant replenishment electrolyte, includes first bottle subassembly, second bottle subassembly and connecting pipe, first bottle subassembly includes first body, intake pipe, measuring electrode, reference electrode, positive pole, negative pole and stirring, first opening has been seted up at the top that first body is close to one side of intake pipe, measuring electrode with the positive pole is inserted and is located in the first body, reference electrode with the negative pole with the outside of first body is connected. The second bottle body assembly comprises a second bottle body, the bottom of the second bottle body is connected with the bottom of the first bottle body through the connecting pipe, the connecting pipe and the air inlet pipe are respectively connected to two opposite sides of the first bottle body, and a second opening part used for communicating with the atmosphere is formed in the second bottle body.
Optionally, the inner diameter of the connecting tube is 1-3mm.
Optionally, the horizontal plane of the joint of the air inlet pipe and the first bottle body is the same as the horizontal plane of the joint of the connecting pipe and the second bottle body.
Optionally, the second bottle body component comprises a bottle stopper, a plurality of first through holes are formed in the bottle stopper, the bottle stopper is inserted into the second opening part, and the diameter of the first through holes is smaller than or equal to 3mm.
Optionally, the number of the first through holes is at least two.
Optionally, the first bottle subassembly still includes two at least platinum pieces, two the platinum piece is located respectively measuring electrode with the one end of positive pole, and insert and locate in the electrolyte of first bottle, the second bottle is equipped with first scale mark and second scale mark, first scale mark is located the below of second scale mark, just the minimum horizontal plane of first scale mark is higher than measuring electrode and positive pole the upper edge of platinum piece, the second scale mark is less than the highest horizontal plane of intake pipe, prevents that electrolyte from flowing backwards to the quartz capsule, leads to the quartz capsule to break.
Optionally, the bottle further comprises a supporting rod, wherein two ends of the supporting rod are respectively connected with the outer surface side of the first bottle body and the outer surface side of the second bottle body.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
according to the sulfur titration cell for immediately supplementing the electrolyte, the electrolyte with iodine ions is injected into the second bottle body, the electrolyte with the same liquid level height is arranged in the first bottle body and the second bottle body under the action of the connecting pipe, and the electrolyte is detected after being stabilized. The gas to be detected is input into the electrolyte from the gas inlet pipe for reaction, the reacted gas is discharged from the first opening, a small amount of solution in the first bottle body taken away by the gas flow is instantaneously replenished under the action of the connecting pipe, the solution taken away by the gas flow in unit time is very small, the liquid level fluctuation and potential fluctuation caused by the replenishing are very small, and the whole system tends to be in a stable state. In addition, during measurement, trivalent iodide ions of a reference electrode connected with the first bottle body are diffused into electrolyte of the first bottle body, the trivalent iodide ions and the iodide ions reach balance under the electrolytic action of an instrument, when sulfur dioxide in gas enters the electrolyte of the first bottle body through an air inlet pipe, the trivalent iodide ions in the electrolyte react with the sulfur dioxide to form the iodide ions, the concentration of the trivalent iodide ions is reduced, the concentration of the iodide ions is increased, the iodide ions form the trivalent iodide ions under the action of current to supplement, and the concentration of the trivalent iodide ions and the concentration of the iodide ions in the electrolyte tend to be dynamically balanced. The air current flows in the one side of keeping away from the connecting pipe, and the stirring of stirring piece is in the one side of keeping away from the connecting pipe, and is less to the electrolyte influence of connecting pipe one side to the trivalent iodide ion from first body to the efficiency of second body diffusion when having reduced the fluid infusion has also reduced the iodide ion from the second body to the possibility of first body emergence diffusion, has further avoided the experimental error that the fluid infusion caused. The air current is discharged from the first opening part of first body, take away a small amount of solution, liquid level and pressure in the titration cell decline, the liquid level and the pressure of second body are higher than first body, the electrolyte in the second body is in succession in time through the connecting pipe to first body supplements the electrolyte, delay the speed that first body liquid level descends, make the electrolyte in the first body keep in normal within range for a long time, do not need the manual work to use the syringe to mend liquid, save the time of manual work benefit liquid and readjustment instrument, and do not influence the timing of instrument and the analysis of sample in the benefit liquid in-process, improve work efficiency.
Drawings
FIG. 1 is a schematic diagram of a sulfur titration cell for instant replenishment of electrolyte in accordance with an embodiment of the present invention.
Reference numerals illustrate:
100. a sulfur titration cell for instant replenishing electrolyte,
1. The first bottle assembly, 11, the first bottle, 111, the first opening, 12, the air inlet pipe, 13, the measuring electrode, 14, the reference electrode, 15, the anode, 16, the cathode, 17, the stirrer, 18 and the platinum sheet.
2. A second bottle body assembly 21, a second bottle body 211, a second opening 212, a first scale mark 213, a second scale mark 22, a bottle stopper 221, a first through hole,
3. A connecting pipe is connected with the connecting pipe,
4. And (5) supporting the rod.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, merely to facilitate description of the present invention and simplify the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like are used herein to describe various information, but such information should not be limited to these terms, which are merely used to distinguish one type of information from another. For example, a "first" message may also be referred to as a "second" message, and similarly, a "second" message may also be referred to as a "first" message, without departing from the scope of the invention.
Referring to fig. 1, this embodiment provides a sulfur titration cell for instant replenishment of electrolyte, including first bottle subassembly 1, second bottle subassembly 2 and connecting pipe 3, first bottle subassembly 1 includes first body 11 and intake pipe 12, second bottle subassembly 2 includes second body 21, the bottom of second body 21 is connected through connecting pipe 3 with the bottom of first body 11, connecting pipe 3 and intake pipe 12 are connected in the both sides that first body 11 is relative respectively, first opening 111 has been seted up at the top of one side that first body 11 is close to intake pipe 12, second opening 211 that is used for with the atmosphere intercommunication has been seted up to second body 21. Electrolyte with iodide ions is injected into the second bottle body 21, the electrolyte with the same liquid level height in the first bottle body 11 and the second bottle body 21 is detected under the action of the connecting pipe 3 after the electrolyte is stabilized under the stirring of the stirrer 17. The gas to be detected is input into the electrolyte from the gas inlet pipe 12 for reaction, the reacted gas is discharged from the first opening 111, a small amount of solution in the first bottle body 11 taken away by the gas flow is instantaneously replenished under the action of the connecting pipe 3, the solution taken away by the gas flow in unit time is very small, the liquid level fluctuation and potential fluctuation caused by the replenishing are very small, and the whole system tends to be in a stable state. In addition, during measurement, trivalent iodide ions in the reference electrode 14 connected with the first bottle body 11 diffuse into electrolyte of the first bottle body 11, the trivalent iodide ions and the iodide ions reach balance under the electrolytic action of an instrument, when sulfur dioxide in gas enters the electrolyte of the first bottle body 11 through the air inlet pipe, the trivalent iodide ions in the electrolyte react with the sulfur dioxide to form the iodide ions, the concentration of the trivalent iodide ions is reduced, the concentration of the iodide ions is increased, the iodide ions form the trivalent iodide ions under the action of current to supplement, and the concentration of the trivalent iodide ions in the electrolyte and the concentration of the iodide ions tend to be dynamically balanced. The air current flows in the one side of keeping away from connecting pipe 3, and the stirring of stirring in the one side of keeping away from connecting pipe 3, and is less to the electrolyte influence of connecting pipe 3 one side to the efficiency of trivalent iodide ion diffusion from first body 11 to second body 21 when having reduced the fluid infusion has also reduced the possibility that iodide ion takes place the diffusion from second body 21 to first body 11, has further avoided the experimental error that the fluid infusion caused. The air current is discharged from the first opening 111 of first body 11, take away a small amount of solution, liquid level and pressure in the first body 11 drop, liquid level and pressure of second body 21 are higher than first body 11, the electrolyte in the second body 21 is in real time continuous automatic to supply electrolyte in first body 11 through connecting pipe 3, delay the speed that first body 11 liquid level descends, make the electrolyte in first body 11 keep in normal range for a long time, do not need the manual work to mend liquid with the syringe, save the time of manual work benefit liquid and readjustment instrument, and do not influence the timing of instrument and analysis of sample in the benefit liquid in-process, improve work efficiency.
Preferably, referring to fig. 1, in the present embodiment, the inner diameter of the connection pipe 3 is 1-3mm. After the reaction between the first bottle body 11 and the gas, the concentration of the electrolyte in the first bottle body 11 is lower than that of the electrolyte in the second bottle body 21, when the inner diameter of the connecting pipe 3 is larger, the exchange efficiency of the electrolyte in the second bottle body 21 and the electrolyte in the first bottle body 11 is overlarge, ions in the second bottle body 21 quickly flow to the first bottle body 11, in-process of dynamic balance is easy to cause, trivalent iodine ions flow from the first bottle body 11 to the second bottle body 21, and iodine ions diffuse from the second bottle body 21 to the first bottle body 11, so that experimental results are affected.
Preferably, referring to fig. 1, in the present embodiment, the horizontal plane where the air inlet pipe 12 is connected to the first body 11 is the same horizontal plane as the horizontal plane where the connecting pipe 3 is connected to the second body 21. When the device is used, detected gas is input from the connecting pipe 3 and flows to the first opening 111 at the top of the first bottle body 11, the gas flow does not enter the connecting pipe 3, the influence of the gas flow on electrolyte near the connecting pipe 3 can be reduced, the stirring of the liquid near the connecting pipe 3 caused by the gas flow is avoided, and the exchange rate of the electrolyte between the connecting pipe 3 and the first bottle body 11 is influenced, so that the accuracy of a test result is ensured.
Preferably, referring to fig. 1, in the present embodiment, the first bottle assembly 1 includes a measuring electrode 13, a reference electrode 14, an anode 15 and a cathode 16, the measuring electrode 13 and the anode 15 are inserted into the first bottle 11, the reference electrode 14 and the cathode 16 are connected to the outside of the first bottle 11, a stirrer 17 is placed at the bottom of the first bottle 11, and a platinum sheet 18 connected to the measuring electrode 13 and the anode 15 is inserted into an electrolyte of the first bottle 11, and the electrolyte fully submerges the platinum sheet 18. The measuring electrode 13, the reference electrode 14, the anode 15 and the cathode 16 are connected with the device, the iodine ions can be reacted to form trivalent iodine ions through the anode 15 and the cathode 16, and the change of the potential during the experiment can be measured through the measuring electrode 13 and the reference electrode 14, so that the total sulfur content in the sample can be measured.
Preferably, referring to fig. 1, in the present embodiment, the second bottle assembly 2 includes a bottle stopper 22, the bottle stopper 22 is provided with a plurality of first through holes 221, and the bottle stopper 22 is inserted into the second opening 211, and the diameter of the first through holes 221 is less than or equal to 3mm. When the first through hole 221 is excessively large, foreign matter is easily caused to fall into the second body 21.
Preferably, referring to fig. 1, in the present embodiment, the number of the first through holes 221 is at least two. Specifically, in this embodiment, one end of the fluid infusion tube is connected to the reagent bottle, the other end is inserted into one first through hole 221, the other first through hole 221 is communicated with the atmosphere, and the electrolyte can be secondarily replenished into the second bottle body 21 under the action of the siphon principle, so that the liquid level of the electrolyte in the first bottle body 11 can be maintained within a normal range for a longer time, and the instrument is more stable.
Preferably, referring to fig. 1, in the present embodiment, the first bottle assembly 1 further includes at least two platinum sheets 18, and the two platinum sheets 18 are respectively disposed at one ends of the measuring electrode and the anode, and are inserted into the electrolyte of the first bottle. The second bottle body 21 is provided with a first scale line 212 and a second scale line 213, the first scale line 212 is arranged below the second scale line 213, and the lowest level of the first scale line 212 is higher than the upper edges of the platinum sheet 18 of the measuring electrode 13 and the anode 15. And the lowest level of the first score line 212 is above the upper edge of the platinum sheet 18 of the anode 15 and the measuring electrode 13. The second graduation marks are lower than the highest horizontal surface of the air inlet pipe 12.
When the height of the electrolyte in the second bottle body 21 is lower than the first scale line 212, the operator is reminded to supplement the electrolyte into the second bottle body 21,
Preferably, referring to fig. 1, in the present embodiment, the sulfur titration cell 100 for instant replenishment of electrolyte further includes a support bar 4, and both ends of the support bar 4 are respectively connected to the outer surface side of the first bottle body 11 and the outer surface side of the second bottle body 21. Make first body 11 and second body 21 constitute a whole under the effect of bracing piece 4, avoid taking place to rock or damage at the in-process of electrolyte from second body 21 flow to first body 11, first body 11 influences the accuracy of experimental result.
In the sulfur titration cell 100 for instant electrolyte replenishment provided in this embodiment, before use, electrolyte with iodide ions is injected into the second bottle body 21, and under the action of the connecting pipe 3, the electrolyte with the same liquid level in the first bottle body 11 and the second bottle body 21 is detected after the electrolyte is stabilized under the stirring of the stirrer 17. The gas to be detected is input into the electrolyte from the gas inlet pipe 12 for reaction, the reacted gas is discharged from the first opening 111, a small amount of solution in the first bottle body 11 taken away by the gas flow is instantaneously replenished under the action of the connecting pipe 3, the solution taken away by the gas flow in unit time is very small, the liquid level fluctuation and the potential fluctuation caused by the liquid replenishing are very small, and the whole system tends to be in a stable state, so that the liquid replenishing is stably completed. Through multiple experiments, the relative standard deviation of the experimental measurement result of the sulfur titration cell 100 using the instant electrolyte replenishing in the embodiment is within 2%, so that the stability of the experimental requirement is met, and the requirement of automatic electrolyte replenishing can be met.
The sulfur titration cell 100 for instant electrolyte replenishment of the present embodiment has the following advantageous effects:
1. Electrolyte with iodide ions is injected into the second bottle body 21, the electrolyte with the same liquid level height in the first bottle body 11 and the second bottle body 21 is detected under the action of the connecting pipe 3 after the electrolyte is stabilized under the stirring of the stirrer 17. The gas to be detected is input into the electrolyte from the gas inlet pipe 12 for reaction, the reacted gas is discharged from the first opening 111, a small amount of solution in the first bottle body 11 taken away by the gas flow is instantaneously replenished under the action of the connecting pipe 3, the solution taken away by the gas flow in unit time is very small, the liquid level fluctuation and potential fluctuation caused by the liquid replenishing are very small, the whole system tends to be in a stable state, the stability of a base line, the adjustment of an instrument and the analysis of a sample are not influenced in the liquid replenishing process, and the accuracy of an analysis result is not influenced.
2. During measurement, the trivalent iodide ions react with sulfur dioxide to form iodide ions, and the iodide ions form trivalent iodide ions to supplement under the action of current, so that the concentration of the trivalent iodide ions in the electrolyte tends to be dynamically balanced. The air current flows in the one side of keeping away from connecting pipe 3, and the stirring of stirring in the bottom of the first body 11 of one side of keeping away from connecting pipe 3, and is less to the electrolyte influence of connecting pipe 3 one side to the efficiency that trivalent iodide ion flows from first body 11 to second body 21 when having reduced the fluid infusion has also reduced the possibility that iodide ion takes place the diffusion phenomenon from second body 21 to first body 11, further avoids the experimental error that the fluid infusion caused.
3. When the device is used, detected gas is input from the connecting pipe 3 and flows to the first opening 111 at the top of the first bottle body 11, the gas flow does not enter the connecting pipe 3, the influence of the gas flow on electrolyte near the connecting pipe 3 can be reduced, the stirring of the liquid near the connecting pipe 3 caused by the gas flow is avoided, the success and failure of the connecting pipe 3 for supplementing the electrolyte to the first bottle body 11 is influenced, and the accuracy of a test result is ensured. The principle of siphon is utilized to directly supplement liquid into the first bottle body 11 through the reagent bottle containing the electrolyte and the siphon, because bubbles enter the siphon from the bottom in the first bottle body 11 under the stirring of the stirrer 17, and the liquid supplementing is failed. The liquid is supplied from the second body 21 to the first body 11 through the connecting pipe, and the liquid is supplied successfully because no air bubbles enter the connecting pipe 3.
While the foregoing is directed to the preferred embodiments of the present invention, it should be noted that modifications and variations could be made by those skilled in the art without departing from the principles of the present invention, and such modifications and variations are to be regarded as being within the scope of the invention.

Claims (7)

1. The utility model provides a sulphur titration cell of instant replenishment electrolyte, includes first bottle subassembly, second bottle subassembly and connecting pipe, first bottle subassembly includes first body, intake pipe, measuring electrode, reference electrode, positive pole, negative pole and stirring, first opening has been seted up at the top of the one side of first body near the intake pipe, measuring electrode with the positive pole inserts and locates in the first body, reference electrode with the negative pole is connected with the outside of first body;
the novel bottle is characterized in that the second bottle body assembly comprises a second bottle body, the bottom of the second bottle body is connected with the bottom of the first bottle body through the connecting pipe, the connecting pipe and the air inlet pipe are respectively connected to two opposite sides of the first bottle body, and the second bottle body is provided with a second opening part which is communicated with the atmosphere.
2. The sulphur titration cell for immediate replenishment of an electrolyte solution according to claim 1, wherein the inner diameter of the connecting tube is 1-3mm.
3. The sulfur titration cell for instant replenishment of electrolyte as recited in claim 1, wherein the level at which the air inlet tube is connected to the first body is the same level as the level at which the connecting tube is connected to the second body.
4. The sulfur titration cell for instant electrolyte replenishment according to claim 1, wherein the second bottle body assembly comprises a bottle stopper, a plurality of first through holes are formed in the bottle stopper, the bottle stopper is inserted into the second opening, and the diameter of the first through holes is 3mm or less.
5. The sulfur titration cell of claim 4, wherein the number of first through holes is at least two.
6. The sulfur titration cell for instant electrolyte replenishment according to claim 1, wherein the first bottle assembly further comprises at least two platinum sheets, the two platinum sheets are respectively arranged at one ends of the measuring electrode and the anode and are inserted into the electrolyte of the first bottle body, the second bottle body is provided with a first scale line and a second scale line, the first scale line is arranged below the second scale line, the lowest level of the first scale line is higher than the upper edges of the platinum sheets of the measuring electrode and the anode, and the second scale line is lower than the highest level of the air inlet pipe, so that the electrolyte is prevented from flowing backwards to the quartz tube, and the quartz tube is prevented from being broken.
7. The sulfur titration cell for instant replenishment of electrolyte as recited in claim 1, further comprising a support bar, wherein two ends of the support bar are connected to the exterior side of the first body and the exterior side of the second body, respectively.
CN202211250225.3A 2022-10-12 2022-10-12 Sulfur titration cell for instant supplementing electrolyte Pending CN117907407A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211250225.3A CN117907407A (en) 2022-10-12 2022-10-12 Sulfur titration cell for instant supplementing electrolyte

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211250225.3A CN117907407A (en) 2022-10-12 2022-10-12 Sulfur titration cell for instant supplementing electrolyte

Publications (1)

Publication Number Publication Date
CN117907407A true CN117907407A (en) 2024-04-19

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Application Number Title Priority Date Filing Date
CN202211250225.3A Pending CN117907407A (en) 2022-10-12 2022-10-12 Sulfur titration cell for instant supplementing electrolyte

Country Status (1)

Country Link
CN (1) CN117907407A (en)

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