A pretreatment device suitable for separating strontium-90 by ion exchange method
By designing an automated device for strontium-90 pretreatment, the problems of inefficient manual operation, safety risks and unstable analysis results in the prior art are solved, automatic processing of sample solutions and accurate quantity addition of reagents are realized, and the accuracy and stability of analysis results are improved.
Patent Information
- Application Number
- CN202111532933.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-12-15
- Publication Date
- 2025-04-11
- Estimated Expiration
- 2041-12-15
AI Technical Summary
In the pre-extraction process of strontium-90 in the prior art, the inefficiency, personal injury, unstable analysis results and inaccurate reagent quantification caused by pure manual operation.
A pretreatment device including a liquid mixing tank, a sample injection tube, an online pH measuring instrument, an additive pump, a combination pump, a regeneration pump, an ion exchange resin column and a controller is designed to realize the automatic addition of sample solution, pH adjustment, and automatic transition and regeneration of ion exchange resin.
Through automated operations, manual operation time is reduced, the stability and accuracy of analysis results are improved, the radiation dose and injury risk of operators are reduced, and the precise amount of reagents is achieved.
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Figure CN114325802B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of radiochemical analysis and monitoring, and in particular to a pre-treatment device suitable for separating strontium-90 by an ion exchange method. Background Art
[0002] Strontium (Sr) is an alkaline earth metal with chemical properties similar to calcium, and is easily deposited on biological bones. Among them, strontium-90 has a long half-life (28.79a) and is a radioactive metal element that is more harmful to the human body. The liquid effluent of nuclear power plants contains trace amounts of strontium-90 nuclides, so the specific activity of strontium-90 in the liquid effluent of nuclear power plants and the water samples around nuclear power plants needs to be monitored regularly.
[0003] When the ion exchange method in "HJ 815-2016 Radiochemical Analysis Method of Strontium-90 in Ash of Water and Biological Samples" is used to analyze the specific activity of strontium-90 in liquid samples, the amount of samples required for collection and transportation is large, the analysis process is time-consuming, and the steps of sampling, desorption, and resin regeneration in the pre-treatment process are usually manually operated. Manual operation causes operators to be in close contact with nuclear pollutants for a long time, increasing the radiation dose, and the use of a variety of acid and alkali reagents in the whole process increases the risk of injury to operators. When the same work is repeated for a long time, it is easy for operators to become careless and lazy, resulting in reduced work efficiency and errors in the analysis results. Looking back at the entire ion exchange process, the steps of sampling, sampling, desorption, and resin regeneration are simple and repetitive tasks, so a processing device can be designed to handle them to reduce the burden on operators, reduce the time operators are exposed to nuclear pollutants, reduce the risk of operators being injured by acid and alkali reagents, and improve the stability of the analysis results. Summary of the invention
[0004] The purpose of the present invention is to provide a pretreatment device suitable for separating strontium-90 by ion exchange method, so as to solve the problem of low efficiency caused by pure manual operation in the pre-extraction process of strontium-90 in the prior art, solve the problem of personal injury, solve the problem of unstable analysis results, and solve the problem of how to accurately quantify reagents in the process of converting manual operation to automated operation.
[0005] The technical solution of the present invention is achieved in this way:
[0006] A pretreatment device suitable for separating strontium-90 by an ion exchange method, comprising a mixing box, a sample injection tube, an online pH value measuring instrument, an addition pump, a combination pump, a regeneration pump, an ion exchange resin column, a controller, a strontium concentrate reagent bottle, a high-purity water bottle, a sodium chloride solution reagent bottle, a strontium desorption solution reagent bottle, a sodium hydroxide solution reagent bottle, a hydrochloric acid solution reagent bottle, an acetic acid-ammonium acetate solution reagent bottle, a strontium carrier solution reagent bottle and a waste liquid pool;
[0007] One end of the sample inlet tube is connected to the mixing liquid box, and the other end is placed in the air;
[0008] The adding pump connects the strontium carrier solution reagent bottle, the sodium hydroxide solution reagent bottle, the hydrochloric acid solution reagent bottle and the acetic acid-ammonium acetate solution reagent bottle to the mixing tank through a pipeline;
[0009] The online pH value measuring instrument is connected to the mixing liquid tank through a combined pump and a pipeline to form a circulation loop;
[0010] The mixing tank is connected to the ion exchange resin column through a combination pump and a pipeline;
[0011] The strontium desorption liquid reagent bottle is connected to the ion exchange resin column through a combination pump and a pipeline;
[0012] The regeneration pump connects the hydrochloric acid solution reagent bottle, the high-purity water bottle and the sodium chloride solution reagent bottle to the ion exchange resin column through a pipeline;
[0013] The ion exchange resin column is connected to the strontium concentrate reagent bottle and the waste liquid pool through a pipeline;
[0014] The mixing liquid box, the online pH value measuring instrument, the adding pump, the combined pump and the regeneration pump are electrically connected to the controller respectively.
[0015] A further technical solution is that the mixing box also includes a stirring motor, an agitator, a water level detector, a liquid inlet and a liquid outlet. The agitator and the water level detector are arranged in the mixing box, and a stirring motor is arranged outside the mixing box. The stirring motor is fixedly connected to the agitator, the liquid inlet is opened at the top of the mixing box, and the liquid outlet is opened at the bottom of the mixing box. The stirring motor and the water level detector are electrically connected to the controller respectively.
[0016] A further technical solution is that the sampling tube also includes a filter, a first solenoid valve and a stop valve. One end of the sampling tube is connected to the liquid inlet of the mixing box. The stop valve, the first solenoid valve and the filter are connected in series in sequence from the liquid inlet to the air. The first solenoid valve is electrically connected to the controller.
[0017] A further technical solution is that the online pH meter includes a solution circulation pool and a measuring meter, the measuring meter is arranged in the solution circulation pool, the solution circulation pool is connected to the liquid inlet and the combination pump of the mixing box through pipelines, and the measuring meter is electrically connected to the controller.
[0018] A further technical solution is that it also includes a multi-position multi-way selection valve, a fifth solenoid valve and a sixth solenoid valve. The ion exchange resin column is provided with an inlet and an outlet. The multi-position multi-way selection valve is connected to the inlet through a pipeline, and the outlet is respectively connected to the strontium concentrate reagent bottle and the waste liquid pool through pipelines. The fifth solenoid valve is connected in series to the pipeline connecting the outlet to the strontium concentrate reagent bottle, and the sixth solenoid valve is connected in series to the pipeline between the outlet and the waste liquid pool. The multi-position multi-way selection valve, the fifth solenoid valve and the sixth solenoid valve are electrically connected to the controller.
[0019] A further technical solution is that it also includes a No. 1 three-way connector, a No. 2 three-way connector, a first plunger pump, a second plunger pump and a second solenoid valve.
[0020] The addition pump is a multi-channel peristaltic pump, which comprises at least four independent channels of strontium carrier solution, acetic acid-ammonium acetate solution, hydrochloric acid solution and sodium hydroxide solution. The inlets of the corresponding independent channels of the addition pump are connected to the strontium carrier solution reagent bottle, the acetic acid-ammonium acetate solution reagent bottle, the hydrochloric acid solution reagent bottle and the sodium hydroxide solution reagent bottle respectively by name through pipelines.
[0021] The strontium carrier solution channel of the addition pump is connected to the first plunger pump and the waste liquid pool through a No. 1 three-way joint and a pipeline, a second solenoid valve is connected in series to the channel between the No. 1 three-way joint and the waste liquid pool, and the first plunger pump is connected to the liquid inlet through a pipeline.
[0022] The acetic acid-ammonium acetate solution channel of the adding pump is connected to the second plunger pump and the second solenoid valve through a No. 2 three-way joint and a pipeline, and the second plunger pump is connected to the liquid inlet through a pipeline.
[0023] The hydrochloric acid solution channel and the sodium hydroxide solution channel of the addition pump are connected to the liquid inlet through pipelines respectively.
[0024] The first plunger pump, the second plunger pump and the second solenoid valve are electrically connected to the controller.
[0025] A further technical solution is to further include a third three-way connector, a third solenoid valve and a fourth solenoid valve.
[0026] The combined pump is a multi-channel peristaltic pump, which contains at least two independent channels for sample solution and strontium desorption solution. The inlet of the sample solution channel is connected to the liquid outlet of the mixing box through a pipeline, and the inlet of the strontium desorption solution channel is connected to the strontium desorption solution reagent bottle through a pipeline.
[0027] The sample solution channel outlet of the combination pump is connected to the solution circulation pool and the multi-position multi-way selection valve respectively through a No. 3 three-way joint and a pipeline, a third solenoid valve is connected in series to the pipeline between the No. 3 three-way joint and the solution circulation pool, and a fourth solenoid valve is connected in series to the pipeline between the No. 3 three-way joint and the multi-position multi-way selection valve.
[0028] The third solenoid valve and the fourth solenoid valve are electrically connected to the controller.
[0029] A further technical solution is that the regeneration pump is a multi-channel peristaltic pump, comprising at least three independent channels of hydrochloric acid solution, high-purity water, and sodium chloride solution. The inlets of the corresponding independent channels of the regeneration pump are connected to the hydrochloric acid solution reagent bottle, the sodium chloride solution reagent bottle, and the high-purity water bottle respectively by name through pipelines.
[0030] A further technical solution is that the multi-position multi-way selection valve includes a sample solution channel, a strontium desorption solution channel, a hydrochloric acid solution channel, a sodium chloride solution channel and a high-purity water channel.
[0031] The sample solution channel inlet of the multi-position multi-way selection valve is connected to the sample solution channel outlet of the combination pump through a pipeline.
[0032] The inlet of the strontium desorption liquid channel of the multi-position multi-way selection valve is connected with the outlet of the strontium desorption liquid channel of the combination pump through a pipeline.
[0033] The hydrochloric acid solution channel inlet of the multi-position multi-way selector valve is connected to the hydrochloric acid solution channel outlet of the regeneration pump through a pipeline.
[0034] The sodium chloride solution channel inlet of the multi-position multi-way selector valve is connected to the sodium chloride solution channel outlet of the regeneration pump through a pipeline.
[0035] The high-purity water channel inlet of the multi-position multi-way selector valve is connected to the high-purity water channel outlet of the regeneration pump through a pipeline.
[0036] The outlets of each channel of the multi-position multi-way selection valve are communicated with the inlet of the ion exchange resin column through a pipeline.
[0037] The beneficial effects of the present invention are:
[0038] 1. When the ion exchange method in "HJ 815-2016 Radiochemical Analysis Method of Strontium-90 in Water and Biological Sample Ash" is used to analyze the specific activity of strontium-90 in liquid samples, the present invention can be connected to the liquid effluent sampling system of a nuclear power plant to achieve automatic sampling and avoid the sampling and transportation of large-volume samples.
[0039] 2. It can automatically add chemical reagents to the sample solution and adjust the pH value of the solution.
[0040] 3. Automatically pass the sample solution through the ion exchange resin column and automatically desorb the strontium-90 nuclide in the resin column.
[0041] 4. Realize automatic on-site regeneration of ion exchange resin.
[0042] 5. The device of the present invention automates the time-consuming steps in the analysis method that require manual operation, such as sample injection, desorption, resin regeneration, etc., which affect the accuracy of the analysis results, thereby improving the stability and accuracy of the analysis results.
[0043] 6. The technical problem of how to accurately quantify each reagent in the process of manual to automatic conversion has been solved. BRIEF DESCRIPTION OF THE DRAWINGS
[0044] Figure 1 This is a layout diagram of the present invention.
[0045] In the figure, 1 is a filter, 2 is a first solenoid valve, 3 is a stop valve, 4 is a mixing tank, 5 is a first waste liquid tank, 6 is an agitator, 7 is a first liquid inlet, 8 is a water level detector, 9 is a stirring motor, 10 is a second liquid inlet, 11 is a liquid outlet, 12 is a second solenoid valve, 13 is a first plunger pump, 14 is a second plunger pump, 15 is an addition pump, 16 is a controller, 17 is a solution circulation tank, 18 is a measuring meter, 19 is a combination pump, 20 is a third solenoid valve, 21 is a fourth solenoid valve, 22 is a regeneration pump, 23 is a multi-position multi-way Selection valve, 24 ion exchange resin column, 25 fifth solenoid valve, 26 sixth solenoid valve, 27 second waste liquid pool, 28 strontium concentrate reagent bottle, 29 high-purity water bottle, 30 sodium chloride solution reagent bottle, 31 strontium desorption solution reagent bottle, 32 strontium carrier solution reagent bottle, 33 hydrochloric acid solution reagent bottle, 34 acetic acid-ammonium acetate solution reagent bottle, 35 sodium hydroxide solution reagent bottle, 36 No. 1 three-way connector, 37 No. 2 three-way connector, 38 No. 3 three-way connector, 39 injection tube. DETAILED DESCRIPTION
[0046] In order to better understand the technical content of the present invention, specific embodiments are provided below, and the present invention is further described in conjunction with the accompanying drawings.
[0047] See also Figure 1A pretreatment device suitable for separating strontium-90 by ion exchange method, comprising a mixing box 4, a sampling tube 39, an online pH value measuring instrument, an addition pump 15, a combination pump 19, a regeneration pump 22, an ion exchange resin column 24, a controller 16, a strontium concentrate reagent bottle 28, a high-purity water bottle 29, a sodium chloride solution reagent bottle 30, a strontium desorption solution reagent bottle 31, a sodium hydroxide solution reagent bottle 35, a hydrochloric acid solution reagent bottle 33, an acetic acid-ammonium acetate solution reagent bottle 34, a strontium carrier solution reagent bottle 32 and a waste liquid pool, one end of the sampling tube 39 is connected to the mixing box 4, and the other end is placed in the air. The addition pump 15 connects the strontium carrier solution reagent bottle 32, the sodium hydroxide solution reagent bottle 35, the hydrochloric acid solution reagent bottle 33 and the acetic acid-ammonium acetate solution reagent bottle 34 to the mixing box 4 through a pipeline. The online pH value measuring instrument is connected to the mixing box 4 through the combination pump 19 and the pipeline to form a circulation loop. The mixing tank 4 is connected to the ion exchange resin column 24 through the combination pump 19 and the pipeline. The strontium desorption liquid reagent bottle 31 is connected to the ion exchange resin column 24 through the combination pump 19 and the pipeline. The regeneration pump 22 connects the hydrochloric acid solution reagent bottle 33, the high-purity water bottle 29 and the sodium chloride solution reagent bottle 30 to the ion exchange resin column 24 through the pipeline. The ion exchange resin column 24 is connected to the strontium concentrate reagent bottle 28 and the waste liquid tank through the pipeline. The mixing tank 4, the online pH value measuring instrument, the addition pump 15, the combination pump 19, and the regeneration pump 22 are each electrically connected to the controller 16.
[0048] After the water sample to be tested enters the mixing tank 4 from the sampling tube 39, the addition pump 15 then transports the corresponding chemical reagent to the mixing tank 4. After adjusting to a suitable pH value, the combination pump 19 transports the sample solution to be tested to the ion exchange resin column 24 for adsorption. The adsorbed sample solution waste liquid will be discharged into the second waste liquid pool 27. Then the combination pump 19 transports the desorption liquid to the ion exchange resin column 24 to complete elution and desorption. The desorbed strontium-90 concentrate is discharged into the strontium concentrate reagent bottle 28 for collection. Finally, the regeneration pump transports the regeneration reagent to the ion exchange resin column 24 for regeneration of the ion exchange resin column 24, and the regenerated waste liquid is discharged into the second waste liquid pool 27.
[0049] Specifically, a stirrer 6 and a water level detector 8 are provided in the mixing box 4, and a stirring motor 9 is provided outside the mixing box 4, wherein the stirring motor 9 is used to drive the stirrer 6 to stir the liquid in the mixing box 4, and the water level detector 8 is used to monitor the water level height and transmit the triggered signal to the controller 16. The mixing box 4 is provided with a first liquid inlet 7, a second liquid inlet 10 and a liquid outlet 11, and the first liquid inlet 7 is connected to a sampling pipeline for obtaining a water sample to be tested through a sampling tube 39, and a stop valve 3, a first solenoid valve 2 and a filter 1 are connected in series in sequence from the first liquid inlet 7 to the sampling pipeline. Preferably, the first solenoid valve 2, the stirring motor 9 and the water level detector 8 are electrically connected to the controller 16.
[0050] Specifically, the online pH meter is used to measure the pH value of the liquid in the mixing box 4, and includes an organic glass solution circulation pool 17 and a measuring meter 18. The organic glass solution circulation pool 17 is used to temporarily store the sample solution, and the measuring meter 18 is used to measure the pH value of the sample entering the pool. The solution circulation pool 17 is connected to the second liquid inlet 10 of the mixing box 4 through a plastic hose. Preferably, the measuring meter 18 is electrically connected to the controller 16.
[0051] Specifically, the external material of the ion exchange resin column 24 is tubular organic transparent glass, with a volume of 50mL, and the inlet and outlet ends are disassembled, and the internal material is a styrene type strong acid cation exchange resin, and the resin is replaceable. The multi-position multi-way selector valve 23 is arranged at the inlet and is communicated with the inlet through a plastic hose. The fifth solenoid valve 25 and the sixth solenoid valve 26 are arranged at the outlet, and the outlet is connected to the strontium concentrate reagent bottle 28 and the second waste liquid pool 27 respectively through a three-way joint and a plastic hose, and the hose between the three-way joint and the strontium concentrate reagent bottle 28 is provided with the fifth solenoid valve 25, and the hose between the three-way joint and the second waste liquid pool 27 is provided with the sixth solenoid valve 26. Preferably, the multi-position multi-way selector valve 23, the fifth solenoid valve 25 and the sixth solenoid valve 26 are electrically connected to the controller 16.
[0052] Specifically, the addition pump 15 is a multi-channel peristaltic pump, the flow rate and flow velocity of the peristaltic pump can be set by the controller 16, and it includes at least four independent channels of strontium carrier solution, acetic acid-ammonium acetate solution, hydrochloric acid solution, and sodium hydroxide solution. The inlets of each independent channel of the corresponding chemical reagent addition pump 15 are connected to the strontium carrier solution reagent bottle 32, the acetic acid-ammonium acetate solution reagent bottle, the hydrochloric acid solution reagent bottle 33, and the sodium hydroxide solution reagent bottle 35 through plastic hoses.
[0053] Among them, the strontium carrier solution channel of the addition pump 15 is connected to the first plunger pump 13 and the first waste liquid pool 5 through a No. 1 three-way connector 36 and a plastic hose. A second solenoid valve 12 is provided on the plastic hose between the No. 1 three-way connector 36 and the first waste liquid pool 5. The first plunger pump 13 can directly inject the strontium carrier solution into the second liquid inlet 10.
[0054] The acetic acid-ammonium acetate solution channel of the adding pump 15 is connected to the second plunger pump 14 and the second solenoid valve 12 through a No. 2 tee and a plastic hose, and the second plunger pump 14 can directly inject the acetic acid-ammonium acetate solution into the second liquid inlet 10 .
[0055] The hydrochloric acid solution channel and the sodium hydroxide solution channel of the addition pump 15 are connected to the second liquid inlet 10 through plastic hoses respectively.
[0056] Preferably, the adding pump 15 , the first plunger pump 13 , the second plunger pump 14 and the second solenoid valve 12 are electrically connected to the controller 16 .
[0057] Specifically, the combined pump 19 is a multi-channel peristaltic pump, the flow rate and flow velocity of which can be set by the controller 16, and at least two independent channels of the sample solution and the strontium desorption solution are included. The inlet of the sample solution channel is connected to the liquid outlet 11 of the mixing box 4 through a plastic hose, and the inlet of the strontium desorption solution channel is connected to the strontium desorption solution reagent bottle 31 through a plastic hose.
[0058] Among them, the sample solution channel outlet of the combination pump 19 is connected to the online pH meter and the multi-position multi-way selection valve 23 respectively through a No. 3 three-way connector 38 and a plastic hose. A third solenoid valve 20 is provided on the hose between the No. 3 three-way connector 38 and the online pH meter, and a fourth solenoid valve 21 is provided on the hose between the No. 3 three-way connector 38 and the multi-position multi-way selection valve 23.
[0059] Preferably, the combination pump 19 , the third solenoid valve 20 and the fourth solenoid valve 21 are electrically connected to the controller 16 .
[0060] Specifically, the regeneration pump 22 is a multi-channel peristaltic pump, the flow rate and flow velocity of which can be set by the controller 16, and at least includes three independent channels of hydrochloric acid solution, high-purity water, and sodium chloride solution, and the inlets of the corresponding independent channels of the regeneration pump 22 are respectively connected to the hydrochloric acid solution reagent bottle 33, the sodium chloride solution reagent bottle 30, and the high-purity water bottle 29 through plastic hoses. Preferably, the regeneration pump 22 is electrically connected to the controller 16.
[0061] Specifically, the multi-position multi-way selector valve 23 includes at least five liquid inlet channels, and the five liquid inlet channels are respectively used to introduce sample solution, strontium desorption solution, hydrochloric acid solution, sodium chloride solution, and high-purity water. The channel switch switching can be controlled by the controller 16. The inlet of its sample solution channel is connected to the sample solution channel outlet of the combination pump 19, the inlet of its strontium desorption solution channel is connected to the strontium desorption solution channel outlet of the combination pump 19 through a plastic hose, the inlet of its hydrochloric acid solution channel is connected to the outlet of the hydrochloric acid solution channel of the regeneration pump 22 through a plastic hose, the inlet of its sodium chloride solution channel is connected to the outlet of the sodium chloride solution channel of the regeneration pump 22 through a plastic hose, the inlet of its high-purity water channel is connected to the outlet of the high-purity water channel of the regeneration pump 22 through a plastic hose, and the liquid outlet 11 of each channel is connected to the inlet of the ion exchange resin column 24 through a plastic hose.
[0062] Specifically, the multi-channel peristaltic pump can choose the Lange BT100-1L peristaltic pump model, which has flow detection function, quantitative and constant speed setting function, and analog communication function.
[0063] Specifically, the plunger pump can be selected from an automatic potentiometric titrator of model METTLER TOLEDO T90.
[0064] Working principle of the present invention:
[0065] The liquid effluent of the nuclear power plant is stored in cans, and the pre-treatment device of strontium-90 is connected to the sampling pipelines of each liquid storage tank through a plastic hose. When working, the manual stop valve 3 of the device is in the open state, and the controller 16 is set to open the first solenoid valve 2 at regular intervals to fill the sample solution into the mixing tank 4, and the sample solution passes through the filter 1 to filter out particulate impurities. When the water level detector 8 detects that the sample solution in the mixing tank 4 reaches the set liquid level, the water level detector 8 inputs a signal to the controller 16, and the controller 16 closes the first solenoid valve 2, stops the liquid from entering, and starts the stirring motor 9 to drive the stirrer 6 to stir.
[0066] Then the controller 16 sends a signal to open the second solenoid valve 12, open the corresponding channel of the strontium carrier solution in the addition pump 15, and discharge the strontium carrier solution into the first waste liquid pool 5, so as to eliminate the bubbles in the pipeline. The amount of liquid discharge can be set in the controller 16 according to the length of the pipeline. After the exhaust is completed, the second solenoid valve 12 is closed, the first plunger pump 13 is opened, and the strontium carrier solution is added to the mixing tank 4. The amount of strontium carrier solution added can be set in the controller 16. After the strontium carrier solution is added, the first plunger pump 13 is closed, and the strontium carrier solution channel in the addition pump 15 is closed. Preferably, the amount of strontium carrier solution added is 2.00mL. Through the characteristics of the first plunger pump 13, accurate addition can be performed.
[0067] Then the controller 16 opens the second solenoid valve 12, opens the corresponding channel of the acetic acid-ammonium acetate solution in the addition pump 15, discharges the acetic acid-ammonium acetate solution into the first waste liquid pool 5, removes the bubbles in the pipeline, and the discharge volume can be set in the controller 16 according to the length of the pipeline. After the exhaust is completed, the second solenoid valve 12 is closed, the second plunger pump 14 is opened, and the acetic acid-ammonium acetate solution is added to the mixing tank 4. The amount of acetic acid-ammonium acetate added can be set in the controller 16. After the addition of acetic acid-ammonium acetate is completed, the second plunger pump 14 is closed, and the acetic acid-ammonium acetate solution channel in the addition pump 15 is closed. Preferably, the amount of acetic acid-ammonium acetate solution added is 20.00mL. Through the characteristics of the second plunger pump 14, accurate addition can be performed.
[0068] Then the controller 16 controls to open the third solenoid valve 20, close the fourth solenoid valve 21, open the online pH meter, open the sample solution channel of the combination pump 19, transport the sample solution in the mixing box 4 to the organic glass solution circulation pool 17 of the online pH meter, and measure the pH value of the solution in the mixing box 4. The pH target value of the solution in the mixing box 4 set in the controller 16 is 4.5-5.0. When the online pH meter measures that the solution in the mixing box 4 deviates from this interval, the corresponding hydrochloric acid solution or sodium hydroxide solution channel in the addition pump 15 channel is opened, and hydrochloric acid solution or sodium hydroxide solution is added to adjust the solution in the mixing box 4 to the target pH interval value. After the pH value is adjusted, the controller 16 sequentially closes the addition pump 15, closes the combination pump 19, closes the third solenoid valve 20, and closes the online pH meter.
[0069] Then the controller 16 controls to open the sixth solenoid valve 26 in sequence, close the fifth solenoid valve 25, open the sample solution channel in the multi-position multi-way selection valve 23, open the fourth solenoid valve 21, open the sample solution channel of the combination pump 19, and allow the sample solution to flow into the second waste liquid pool 27 after passing through the ion exchange resin column 24. The total injection volume and injection speed of the solution can be set in the controller 16, and the optimal value is 20mL / min. After the sample solution in the mixing tank 4 is completely evacuated, the controller 16 controls to close the sample solution channel of the combination pump 19 in sequence and closes the sixth solenoid valve 26.
[0070] Then the controller 16 controls to open the fifth solenoid valve 25, opens the strontium desorption liquid injection channel in the multi-position multi-way selection valve 23, opens the strontium desorption liquid injection channel of the combination pump 19, and allows the strontium desorption liquid to pass through the ion exchange resin column 24. The total injection volume and injection speed of the strontium desorption liquid can be set in the controller 16, and the optimal value is the injection speed of 4 to 5 mL / min and the total injection volume of 200 mL. After the strontium desorption liquid reaches the set total injection volume, the controller 16 controls to sequentially close the strontium desorption liquid injection channel of the combination pump 19, close the fourth solenoid valve 21, close the desorption liquid injection channel in the multi-position multi-way selection valve 23, and close the fifth solenoid valve 25.
[0071] At this point, the separation of strontium-90 in the sample solution is complete.
[0072] Regeneration of ion exchange resin column 24:
[0073] The controller 16 controls the opening of the sixth solenoid valve 26, opens the high-purity water injection channel in the multi-position multi-way selection valve 23, and opens the high-purity water channel of the regeneration pump 22. The total injection volume and injection speed of high-purity water can be set in the controller 16. The optimal value is the injection speed of 3mL / min and the total injection volume of 100mL.
[0074] After the high-purity water reaches the set total amount, the controller 16 controls in sequence to close the high-purity water injection channel in the multi-position multi-way selection valve 23, close the high-purity water channel of the regeneration pump 22, open the hydrochloric acid solution injection channel in the multi-position multi-way selection valve 23, and open the hydrochloric acid solution channel of the regeneration pump 22. The total injection volume and injection speed of the hydrochloric acid solution can be set in the controller 16. The optimal value is an injection speed of 3mL / min and a total injection volume of 200mL.
[0075] After the injection volume of the hydrochloric acid solution reaches the set total amount, the controller 16 sequentially controls the closing of the hydrochloric acid solution injection channel in the multi-position multi-way selection valve 23, the closing of the hydrochloric acid solution channel of the regeneration pump 22, the opening of the high-purity water injection channel in the multi-position multi-way selection valve 23, and the opening of the high-purity water channel of the regeneration pump 22. The total injection volume and injection speed of the high-purity water can be set in the controller 16, and the optimal value is the injection speed of 3mL / min and the total injection volume of 200mL.
[0076] After the high-purity water injection volume reaches the set total amount, the controller 16 sequentially controls to close the high-purity water injection channel in the multi-position multi-way selection valve 23, closes the high-purity water channel of the regeneration pump 22, opens the sodium chloride injection channel in the multi-position multi-way selection valve 23, and opens the sodium chloride channel of the regeneration pump 22. The total injection volume and injection speed of sodium chloride can be set in the controller 16. The optimal value is an injection speed of 3mL / min and a total injection volume of 200mL.
[0077] After the sodium chloride injection volume reaches the set total amount, the controller 16 sequentially controls to close the sodium chloride injection channel in the multi-position multi-way selection valve 23, closes the sodium chloride channel of the regeneration pump 22, opens the high-purity water injection channel in the multi-position multi-way selection valve 23, and opens the high-purity water channel of the regeneration pump 22. The total injection volume and injection speed of high-purity water can be set in the controller 16. The optimal value is an injection speed of 3mL / min and a total injection volume of 200mL.
[0078] When the high-purity water injection volume reaches the set total amount, the controller 16 sequentially controls the closing of the high-purity water injection channel in the multi-position multi-way selector valve 23, the high-purity water channel of the regeneration pump 22, and the sixth solenoid valve 26. Thus, the regeneration of the ion exchange resin column 24 is completed.
[0079] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A pretreatment device suitable for separating strontium-90 by ion exchange method, comprising a mixing box (4), a sample injection tube (39), an online pH value measuring instrument, an addition pump (15), a combination pump (19), a regeneration pump (22), an ion exchange resin column (24), a controller (16), a strontium concentrate reagent bottle (28), a high-purity water bottle (29), a sodium chloride solution reagent bottle (30), a strontium desorption solution reagent bottle (31), a sodium hydroxide solution reagent bottle (35), a hydrochloric acid solution reagent bottle (33), an acetic acid-ammonium acetate solution reagent bottle (34), a strontium carrier solution reagent bottle (32) and a waste liquid tank, characterized in that: One end of the sample inlet tube (39) is connected to the mixing liquid box (4), and the other end is placed in the air; The adding pump (15) connects the strontium carrier solution reagent bottle (32), the sodium hydroxide solution reagent bottle (35), the hydrochloric acid solution reagent bottle (33) and the acetic acid-ammonium acetate solution reagent bottle (34) to the mixing tank (4) through a pipeline; The online pH value measuring instrument is connected to the mixing tank (4) through a combined pump (19) and a pipeline to form a circulation loop; The liquid mixing box (4) is connected to the ion exchange resin column (24) through a combined pump (19) and a pipeline; The strontium desorption liquid reagent bottle (31) is connected to the ion exchange resin column (24) via a combined pump (19) and a pipeline; The regeneration pump (22) connects the hydrochloric acid solution reagent bottle (33), the high-purity water bottle (29) and the sodium chloride solution reagent bottle (30) to the ion exchange resin column (24) through a pipeline; The ion exchange resin column (24) is connected to a strontium concentrate reagent bottle (28) and a waste liquid pool through a pipeline; The liquid mixing tank (4), the online pH value measuring instrument, the adding pump (15), the combined pump (19), and the regeneration pump (22) are each electrically connected to the controller (16).
2. A pretreatment device suitable for separating strontium-90 by ion exchange method according to claim 1, characterized in that: The liquid mixing box (4) further comprises a stirring motor (9), a stirrer (6), a water level detector (8), a liquid inlet and a liquid outlet (11); the stirrer (6) and the water level detector (8) are arranged in the liquid mixing box (4); a stirring motor (9) is arranged outside the liquid mixing box (4); the stirring motor (9) is fixedly connected to the stirrer (6); the liquid inlet is arranged at the top of the liquid mixing box (4); the liquid outlet (11) is arranged at the bottom of the liquid mixing box (4); the stirring motor (9) and the water level detector (8) are electrically connected to the controller (16) respectively.
3. A pretreatment device suitable for separating strontium-90 by ion exchange method according to claim 2, characterized in that: The sample injection tube (39) further comprises a filter (1), a first solenoid valve (2) and a stop valve (3); one end of the sample injection tube (39) is connected to a liquid inlet of a liquid mixing box (4); the stop valve (3), the first solenoid valve (2) and the filter (1) are sequentially connected in series in a direction from the liquid inlet to the air; the first solenoid valve (2) is electrically connected to a controller (16).
4. A pre-treatment device suitable for separating strontium-90 by ion exchange method according to claim 3, characterized in that: The online pH value measuring instrument comprises a solution circulation pool (17) and a measuring meter (18), wherein the measuring meter (18) is arranged in the solution circulation pool (17), the solution circulation pool (17) is respectively connected to the liquid inlet of the mixing tank (4) and the combined pump (19) through pipelines, and the measuring meter (18) is electrically connected to the controller (16).
5. A pre-treatment device suitable for separating strontium-90 by ion exchange method according to claim 4, characterized in that: The invention also comprises a multi-position multi-way selector valve (23), a fifth solenoid valve (25) and a sixth solenoid valve (26); an inlet and an outlet are provided on the ion exchange resin column (24); the multi-position multi-way selector valve (23) is connected to the inlet through a pipeline; the outlet is connected to a strontium concentrate reagent bottle (28) and a waste liquid pool through pipelines; the fifth solenoid valve (25) is connected in series to the pipeline connecting the outlet to the strontium concentrate reagent bottle (28); the sixth solenoid valve (26) is connected in series to the pipeline between the outlet and the waste liquid pool; the multi-position multi-way selector valve (23), the fifth solenoid valve (25) and the sixth solenoid valve (26) are electrically connected to a controller (16).
6. A pre-treatment device suitable for separating strontium-90 by ion exchange method according to claim 5, characterized in that: It also includes a No. 1 three-way connector (36), a No. 2 three-way connector (37), a first plunger pump (13), a second plunger pump (14) and a second solenoid valve (12); The addition pump (15) is a multi-channel peristaltic pump, comprising at least four independent channels for a strontium carrier solution, an acetic acid-ammonium acetate solution, a hydrochloric acid solution, and a sodium hydroxide solution. The inlets of the corresponding independent channels of the addition pump (15) are connected to the strontium carrier solution reagent bottle (32), the acetic acid-ammonium acetate solution reagent bottle, the hydrochloric acid solution reagent bottle (33), and the sodium hydroxide solution reagent bottle (35) through pipelines. The strontium carrier solution channel of the addition pump (15) is connected to the first plunger pump (13) and the waste liquid pool via a No. 1 three-way connector (36) and a pipeline, a second solenoid valve (12) is connected in series to the channel between the No. 1 three-way connector (36) and the waste liquid pool, and the first plunger pump (13) is connected to the liquid inlet via a pipeline; The acetic acid-ammonium acetate solution channel of the addition pump (15) is connected to the second plunger pump (14) and the second solenoid valve (12) through a No. 2 three-way connector (37) and a pipeline, and the second plunger pump (14) is connected to the liquid inlet through a pipeline; The hydrochloric acid solution channel and the sodium hydroxide solution channel of the addition pump (15) are connected to the liquid inlet through pipelines respectively; The first plunger pump (13), the second plunger pump (14) and the second solenoid valve (12) are electrically connected to a controller (16).
7. A pre-treatment device suitable for separating strontium-90 by ion exchange method according to claim 6, characterized in that: It also includes a No. 3 three-way connector (38), a third solenoid valve (20) and a fourth solenoid valve (21); The combined pump (19) is a multi-channel peristaltic pump, comprising at least two independent channels for a sample solution and a strontium desorption solution, wherein the inlet of the sample solution channel is connected to a liquid outlet (11) of a mixing box (4) through a pipeline, and the inlet of the strontium desorption solution channel is connected to a strontium desorption solution reagent bottle (31) through a pipeline; The sample solution channel outlet of the combination pump (19) is connected to the solution circulation pool (17) and the multi-position multi-way selection valve (23) respectively through a No. 3 three-way connector (38) and a pipeline, a third solenoid valve (20) is connected in series to the pipeline between the No. 3 three-way connector (38) and the solution circulation pool (17), and a fourth solenoid valve (21) is connected in series to the pipeline between the No. 3 three-way connector (38) and the multi-position multi-way selection valve (23); The third solenoid valve (20) and the fourth solenoid valve (21) are electrically connected to the controller (16).
8. A pre-treatment device suitable for separating strontium-90 by ion exchange method according to claim 7, characterized in that: The regeneration pump (22) is a multi-channel peristaltic pump, comprising at least three independent channels for hydrochloric acid solution, high-purity water, and sodium chloride solution. The inlets of the independent channels of the corresponding regeneration pump (22) are connected to the hydrochloric acid solution reagent bottle (33), the sodium chloride solution reagent bottle (30), and the high-purity water bottle (29) through pipelines.
9. A pre-treatment device suitable for separating strontium-90 by ion exchange method according to claim 8, characterized in that: The multi-position multi-way selection valve (23) comprises a sample solution channel, a strontium desorption solution channel, a hydrochloric acid solution channel, a sodium chloride solution channel and a high-purity water channel; The sample solution channel inlet of the multi-position multi-way selection valve (23) is connected to the sample solution channel outlet of the combination pump (19) through a pipeline; The strontium desorption liquid channel inlet of the multi-position multi-way selection valve (23) is connected to the strontium desorption liquid channel outlet of the combination pump (19) through a pipeline; The hydrochloric acid solution channel inlet of the multi-position multi-way selector valve (23) is connected to the hydrochloric acid solution channel outlet of the regeneration pump (22) through a pipeline; The sodium chloride solution channel inlet of the multi-position multi-way selector valve (23) is connected to the sodium chloride solution channel outlet of the regeneration pump (22) through a pipeline; The high-purity water channel inlet of the multi-position multi-way selector valve (23) is connected to the high-purity water channel outlet of the regeneration pump (22) through a pipeline; The outlets of the various channels of the multi-position multi-way selector valve (23) are connected to the inlet of the ion exchange resin column (24) through a pipeline.
Citation Information
Patent Citations
Pretreatment device suitable for separating strontium-90 by ion exchange method
CN216526311U