CN212622385U - Automatic replenish titration cell of electrolyte - Google Patents
Automatic replenish titration cell of electrolyte Download PDFInfo
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- CN212622385U CN212622385U CN202021123403.2U CN202021123403U CN212622385U CN 212622385 U CN212622385 U CN 212622385U CN 202021123403 U CN202021123403 U CN 202021123403U CN 212622385 U CN212622385 U CN 212622385U
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- titration cell
- storage tank
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Abstract
The utility model relates to an automatic replenishing electrolyte's titration cell is applicable to chlorine content analysis among the petrochemical, and it discloses that the titration cell is provided with the liquid storage tank, and liquid storage tank lower extreme and titration cell lower extreme have the communicating pipe that is linked together. The liquid storage tank is provided with a lowest liquid level line and a highest liquid level line which are the same as the scale height of the titration cell, the top of the liquid storage tank is provided with a ground plug, and the top of the ground plug is provided with 2 exhaust holes communicated with the atmosphere. The middle upper part of the liquid storage tank is provided with a support rod connected with the titration cell, so that the liquid storage tank and the titration cell are connected into a whole. The utility model discloses can automatic replenishment electrolyte in succession, do not need manual operation, and very little to instrument interference during the fluid infusion, instrument baseline and rate of recovery are stable. The titration cell does not influence the adjustment and calibration of instruments and the analysis of samples in the automatic liquid supplementing process, and the working efficiency is improved.
Description
Technical Field
The utility model relates to a microcoulomb analyzer in the analysis of petrochemical products, in particular to a titration cell of a microcoulomb chlorine analyzer.
Background
The trace chlorine content in the petrochemical product can poison the catalyst of a downstream processing device, most of the trace chlorine content is less than 1mg/kg, and the accurate determination of the trace chlorine content has important significance. At present, the content is mainly determined by a microcoulomb method, and an adopted analytical instrument is mainly a microcoulomb instrument and comprises a titration cell, an amplifier and a temperature and flow controller. The titration cell is a heart component of a microcoulometer and consists of 4 electrodes, a cell cup and a sample gas inlet pipe, and the cell cup, the reference arm and the cathode arm are filled with electrolyte. The working principle is as follows: the sample is combusted in the combustion tube, organic chlorine is converted into hydrogen chloride, the hydrogen chloride enters the titration cell along with carrier gas and oxygen and reacts with Ag & lt + & gt in the electrolyte of the titration cell, consumed silver ions are supplemented by electrolysis of the microcoulometer, and the chlorine content in the sample is calculated according to the Faraday's law of electrolysis. The electrolyte in the titration cell is taken away by the carrier gas and the oxygen which enter the titration cell and flows into the atmosphere from the outlet of the cell cover, so that the electrolyte in the titration cell volatilizes and is lost, and the liquid level gradually decreases. When the liquid level reaches the lowest scribed line, the baseline fluctuates and burrs occur, the recovery rate changes, the measurement result is inaccurate, the manual injector is needed to supplement the electrolyte into the titration cell in time, the instrument is readjusted, and the recovery rate of the instrument is measured again, so that time and labor are wasted. Because most of the petrochemical products have low chlorine content, the sensitivity of the domestic microcoulometer is not high, the performance is unstable, the failure rate is high, and the repeatability of an analysis result is poor, the adjustment time of the instrument and the analysis time of a sample are long, the instrument is not debugged or the sample is not analyzed completely, the liquid level of the electrolyte in a titration cell is lower than a normal range, and the electrolyte needs to be supplemented manually. In the process of liquid replenishment, vibration of a box door of the titration tank is switched on or off, and sudden change of liquid level in the titration tank interferes the instrument, and the potential of the instrument is changed after liquid replenishment, so that the baseline of the instrument fluctuates violently, the recovery rate changes, and the instrument can be continuously adjusted and calibrated after the baseline of the instrument is stable, and the recovery rate of the instrument is measured. Sometimes, a lot of samples to be tested exist, the analysis time is long, and electrolyte is supplemented regularly in the analysis process. The general instrument needs to be supplemented with electrolyte for 2-3 hours, the instrument needs to be debugged again after the electrolyte is supplemented, a large amount of time and labor are consumed, and the sample analysis result cannot be reported in time.
The sample injection amount of the traditional microcoulomb method is 8.4 microliters, and the measurement of the chlorine content of less than 1mg/kg in a sample has great difficulty due to the fact that the sample injection amount is too small. The Guangdian petrochemical inspection center improves the structure of the microcoulomb method quartz tube, improves the furnace temperature and the flow rate of oxygen, simultaneously improves the sample volume from 8.4 microliter to more than 20 microliter, and improves the sensitivity and the accuracy of analysis. However, after the method is improved, the electrolyte in the titration cell is taken away by oxygen with higher temperature and higher flow rate, the volatilization loss is faster, the electrolyte needs to be supplemented for 1 time when the instrument works for 2 hours, and the liquid supplementation and the instrument adjustment are more frequent, so that the instrument adjustment time is long, the working efficiency is low, the sample analysis is delayed, and the device production is influenced.
The liquid level of the electrolyte of the conventional titration cell has an upper scale mark and a lower scale mark, namely a highest liquid level scale mark and a lowest liquid level scale mark, and the liquid level of the titration cell cannot exceed the upper scale mark, otherwise, the detection sensitivity of an instrument is reduced. The liquid level of the electrolyte cannot be lower than the lowest scale mark of the instrument, otherwise, the baseline fluctuates and burrs occur, the recovery rate changes, and the accuracy of the measurement result is influenced. In order to ensure that the electrolyte of the titration cell remains stable for a long time during instrument commissioning and sample analysis, improvements in the structure and solution filling methods of conventional titration cells are needed.
The existing titration cell can not continuously and automatically supplement electrolyte, only can supplement the electrolyte through manual interruption, and the quantity of the electrolyte supplemented every time is large, so that the liquid level of the titration cell is suddenly changed, the potential of the electrolyte and the baseline of an instrument are influenced, and the adjustment of the instrument and the analysis of a sample are influenced. The general instrument works for 2-3 hours and needs to be supplemented with electrolyte, the sample in the morning is not finished sometimes, the electrolyte can fall below the minimum scribed line when the sample is analyzed in the afternoon, the analysis of the sample can be continued only after the electrolyte needs to be supplemented and the instrument needs to be recalibrated again, a large amount of time and manpower are wasted, the sample analysis result cannot be reported in time, and the production of the device is influenced.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing an automatic replenish titration cell of electrolyte, it can make the titration cell in the twinkling of an eye fluid infusion immediately, accomplishes in the titration cell electrolyte in case the volatilization loss, automatic replenish electrolyte at once, and interference to the instrument influences fewly, and is undulant and the rate of recovery influence very little to the instrument base line, does not influence the timing of instrument and the analysis of sample, and can delay the falling speed of titration cell liquid level.
The technical solution of the utility model is that: the structure of the titration cell cup is improved on the basis of the titration cell cup, the gas-guide tube, the stirrer, the anode, the cathode, the measuring electrode and the reference electrode in the prior art. The utility model discloses there is the liquid storage tank, and there is the communicating pipe that is linked together liquid storage tank lower extreme and titration cell lower extreme, and the internal diameter of communicating pipe is 1 ~ 3 millimeters. The top of the liquid storage tank is provided with a ground plug, the top of the ground plug is provided with 2 exhaust holes communicated with the atmosphere, and the middle upper part of the liquid storage tank is provided with a support rod connected with the titration cell cup, so that the liquid storage tank and the titration cell cup are connected into a whole. The liquid storage tank is provided with a lowest liquid level scale mark and a highest liquid level scale mark which have the same height with the titration cell cup.
The working principle is as follows: the sample is combusted in a combustion tube of a quartz tube, organic chlorine is converted into hydrogen chloride, enters a titration cell along with carrier gas and oxygen, silver ions consumed by reaction with Ag & lt + & gt in electrolyte of the titration cell are supplemented by electrolysis of a microcoulometer, and the chlorine content in the sample is calculated according to a Faraday's law of electrolysis. The electrolyte in the titration cell is taken away by the carrier gas and the oxygen which enter the titration cell from the bottom and flows into the atmosphere from the outlet of the titration cell cover, so that the volatilization loss of the electrolyte in the titration cell is caused, and the liquid level gradually decreases. At this time, the electrolyte in the liquid storage tank is instantly and instantly replenished into the titration cell from the communicating pipe under the action of atmospheric pressure, the amount of replenished liquid is little each time, the influence on the liquid level and the potential of the titration cell is little, the influence on the interference of an instrument is little, and the fluctuation of the baseline of the instrument and the change of the recovery rate are little in the process of replenishing the liquid, so that the adjustment of the instrument and the sample analysis are not influenced in the continuous automatic replenishing process of the titration cell.
The bottom that traditional titration cell pond cup got into from titration cell pond cup because of having carrier gas and oxygen, and the electrolyte of titration cell pond cup produces a large amount of bubbles under the stirring of stirring, and the bubble emerges from the export of titration cell pond lid, if utilize the principle of siphon, inserts the siphon toward titration cell pond cup, directly supplements electrolyte in to traditional titration cell, and the bubble can get into in the siphon, leads to supplementing electrolyte failure. Therefore, automatic fluid infusion is difficult to realize without improving the structure of the traditional titration cell.
The utility model has the advantages that the titration cell can automatic replenishment electrolyte in succession, does not need manual operation, and disturbs very little to the instrument during the fluid infusion, and the baseline is stable with the rate of recovery. In the automatic liquid supplementing process of the titration cell, instrument adjustment and sample analysis are not affected, and the working efficiency is improved.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Detailed Description
According to the figure 1, the utility model discloses on the basis of prior art's titration cell pond cup 1, air duct 3, stirring bar 7, positive pole 11, negative pole 12, reference electrode 9, measuring electrode 10, quartz capsule 14, improve the structure and the fluid infusion method of titration cell. The utility model discloses especially there is liquid storage tank 2, and liquid storage tank 2 lower extreme and titration cell lower extreme have communicating pipe 13 that is linked together, and communicating pipe 13's internal diameter is 1 ~ 3 millimeters. The liquid storage tank 2 and the titration cell 1 are both provided with a lowest scale mark 4 and a highest scale mark 5 which have the same height, the top of the liquid storage tank is provided with a ground plug 8, the top of the ground plug 8 is provided with 2 holes communicated with the atmosphere, and the middle upper part of the liquid storage tank 2 is provided with a support rod 6 connected with a cell cup of the titration cell, so that the liquid storage tank and the titration cell are connected into a whole. The liquid storage tank is provided with a lowest liquid level scale mark 4 and a highest liquid level scale mark 5 which have the same height with the titration cell cup.
Claims (1)
1. The utility model provides an automatic replenishing electrolyte's titration cell, includes titration cell cup, air duct, stirring, positive pole, negative pole, reference electrode, measuring electrode, characterized by:
(1) the device is provided with a liquid storage tank, the lower end of the liquid storage tank is communicated with the lower end of a titration cell cup, and the inner diameter of the communicating pipe is 1-3 mm;
(2) the top of the liquid storage tank is provided with a ground plug, the top of the ground plug is provided with 2 exhaust holes communicated with the atmosphere, and the middle upper part of the liquid storage tank is provided with a support rod connected with the titration cell cup, so that the liquid storage tank and the titration cell cup are connected into a whole;
(3) the liquid storage tank is provided with a lowest liquid level scale mark and a highest liquid level scale mark which have the same height with the titration cell cup.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021123403.2U CN212622385U (en) | 2020-06-17 | 2020-06-17 | Automatic replenish titration cell of electrolyte |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021123403.2U CN212622385U (en) | 2020-06-17 | 2020-06-17 | Automatic replenish titration cell of electrolyte |
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| CN212622385U true CN212622385U (en) | 2021-02-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113804742A (en) * | 2020-06-17 | 2021-12-17 | 中国石油化工股份有限公司 | Titration cell capable of continuously and automatically replenishing electrolyte twice |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113804742A (en) * | 2020-06-17 | 2021-12-17 | 中国石油化工股份有限公司 | Titration cell capable of continuously and automatically replenishing electrolyte twice |
| CN113804742B (en) * | 2020-06-17 | 2024-06-18 | 中国石油化工股份有限公司 | Titration cell for continuously and automatically supplementing electrolyte twice |
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