Separation device and separation analysis method for strontium-89 and strontium-90

Abstract

The application provides a separation device for strontium-89 and strontium-90, and relates to the technical field of radioactive substance measurement. The separation device comprises a concentration unit, a storage unit, an enrichment unit, a separation and purification unit and a sample preparation unit. The concentration unit is used for concentrating and preparing metal ions in nuclear power plant liquid effluent in a container to form concentrated liquid. The storage unit is used for storing treatment liquid. The enrichment unit is communicated with the concentration unit and the storage unit respectively to obtain the concentrated liquid and the treatment liquid respectively, and desorb the metal ions in the concentrated liquid after enrichment to form enriched liquid. The separation and purification unit is communicated with the enrichment unit and the storage unit respectively, and is used for separating and purifying the enriched liquid, removing interfering ions and obtaining purified liquid. The sample preparation unit is communicated with the separation and purification unit, obtains the purified liquid and prepares the purified liquid into a sample to be measured. The separation device can greatly reduce the enrichment time of metal ions, significantly improve the work efficiency and save a large amount of manpower and resource consumption through the concentration unit.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of radioactive substance measurement, and particularly relates to a strontium-89 and strontium-90 separation device and separation analysis method. BACKGROUND

[0002] Quick and accurate analysis of radioactive substances is the basis and key of environmental radiation monitoring and nuclear emergency monitoring. 89 Sr and 90 Sr are both high-radiation-toxicity fission products. 89 The half-life of Sr is 50.563 days, and it generates stable nuclide 89 Y through beta decay. 90 Sr is an unstable long-lived radioactive nuclide, which can produce radioactive nuclide 90 Y through beta decay. 90 Y can decay into stable element 90 Zr. 89 Sr (Eβmax=1499.3keV), 90 Sr (Eβmax=545.9keV) and its daughter 90 Y (Eβmax=2278.5keV) all only emit beta rays, and non-destructive measurement methods such as gamma-ray spectroscopy cannot realize measurement of them. The beta rays are continuous spectrum, and will be interfered by beta rays of other radioactive nuclides during measurement. Therefore, before the radioactive measurement of 89 Sr, 90 Sr and its daughter 90 Y, the sample needs to be subjected to radiochemical separation to remove other radioactive nuclides in the sample.

[0003] Traditional radiochemical separation methods include precipitation method, ion exchange method, liquid-liquid extraction method and the like. These conventional methods have complex processes and long sample analysis time. The existing resource configuration of nuclear power plants in China is difficult to adapt to such low-efficiency methods, and needs to be improved. SUMMARY

[0004] In view of the problems in the prior art, the present application provides a strontium-89 and strontium-90 separation device and separation analysis method to improve the problems of complex radiochemical separation process and long analysis time of the existing method.

[0005] To achieve the above object and other related objects, the present application provides a strontium-89 and strontium-90 separation device for separating strontium-89 and strontium-90 in liquid effluent of a nuclear power plant, comprising a concentration unit, a storage unit, an enrichment unit, a separation and purification unit and a sample preparation unit, wherein the concentration unit is used to concentrate metal ions in the liquid effluent of the nuclear power plant to form a concentrated solution; the storage unit is used to store a treatment solution; the enrichment unit is in communication with the concentration unit and the storage unit respectively to obtain the concentrated solution and the treatment solution respectively, and to enrich metal ions in the concentrated solution and then desorb to form an enriched solution; the separation and purification unit is in communication with the enrichment unit and the storage unit respectively, and is used to separate and purify the enriched solution to remove interfering ions to obtain a purified solution; and the sample preparation unit is in communication with the separation and purification unit to obtain the purified solution and prepare the purified solution into a sample to be measured.

[0006] In an embodiment of the present application, the concentration unit comprises a concentration device and a first syringe pump, the concentration device is provided with a first water inlet and a first water outlet, the first syringe pump is provided with a first water suction port and a first water discharge port, the first water inlet is in communication with a water outlet of a container, the first water outlet is in communication with the first water suction port, and the first water discharge port is in communication with the enrichment unit.

[0007] In an embodiment of the present application, the enrichment unit comprises a water sample storage tank and an enrichment resin column, the water sample storage tank is provided with a second water inlet, a third water inlet and a second water outlet, the second water inlet is in communication with the first water discharge port, the third water inlet is in communication with the storage unit, a second syringe pump is arranged on a pipeline between the water sample storage tank and the storage unit, the second syringe pump is provided with a second water suction port and a second water discharge port, the second water suction port is in communication with the storage unit, and the second water discharge port is in communication with the third water inlet; the enrichment resin column is provided with a first flow inlet and a first flow outlet, the first flow inlet is in communication with the second water outlet or the storage unit, and the first flow outlet is in communication with the separation and purification unit; a third syringe pump is arranged on a pipeline between the water sample storage tank and the enrichment resin column, the third syringe pump is provided with a third water suction port and a third water discharge port, the third water suction port is in communication with the second water outlet, and the second water discharge port is in communication with the first flow inlet.

[0008] In an embodiment of the present application, a fourth syringe pump is arranged on the pipeline between the separation and purification unit and the liquid storage unit, and the fourth syringe pump is provided with a fourth water suction port and a fourth water discharge port, wherein the fourth water suction port is communicated with the liquid storage unit, and the fourth water discharge port is communicated with the separation and purification unit; the separation and purification unit comprises an anion resin column for adsorbing interfering ions, a yttrium specific resin column for adsorbing yttrium ions, and a strontium specific resin column for adsorbing strontium ions, wherein the anion resin column is provided with a second inlet and a second outlet, the yttrium specific resin column is provided with a third inlet and a third outlet, and the strontium specific resin column is provided with a fourth inlet and a fourth outlet, and the second inlet is communicated with the first outlet, the third inlet is communicated with the second outlet, the fourth inlet is communicated with the third outlet, and the fourth outlet is communicated with a waste liquid collecting device, or the second inlet, the third inlet and the fourth inlet are respectively communicated with liquid storage units.

[0009] In an embodiment of the present application, the sample preparation unit comprises a first sample bottle for storing a yttrium solution and a second sample bottle for storing a strontium solution, wherein the first sample bottle is communicated with the third outlet, and the second sample bottle is communicated with the fourth outlet.

[0010] The second aspect of the present application provides a method for separating and analyzing strontium-89 and strontium-90 by using the separation device, comprising the following steps:

[0011] Concentrating metal ions in liquid effluent of a nuclear power plant to form a concentrated liquid;

[0012] Pretreating the concentrated liquid to obtain a pretreated liquid, and desorbing metal ions enriched in the pretreated liquid to form an enriched liquid;

[0013] Separating and purifying the enriched liquid to remove interfering ions and obtain a purified liquid;

[0014] Preparing the purified liquid into a sample to be measured;

[0015] Sending the sample to be measured into a liquid scintillation spectrometer for testing.

[0016] In an embodiment of the present application, the analysis method further comprises calculating the recovery rate of metal ions after the step of preparing the purified liquid into a sample to be measured, and the calculation formula of the recovery rate is as follows:

[0017]

[0018] In the formula, R represents the recovery rate, %, Q represents the concentration of metal ions in the sample to be measured, mg / L, and Q0 represents the concentration of metal ions in the pretreated liquid, mg / L.

[0019] In an embodiment of the present application, when testing with the liquid scintillation counter, 89 Sr 90 The calculation formula of the detection efficiency of Y is as follows:

[0020]

[0021] In the formula, E: the detection efficiency of the instrument to 89 Sr 90 Y, %; n s : the total count rate of the sample, cpm; n b : the background count rate, cpm; c0: 89 Sr 90 Y, Bq / mL; V0: 89 Sr 90 Y, mL; λ: the decay constant, 89 The decay constant of Sr is 9.52E-6 min -1 , 90 The decay constant of Y is 4.56E-8 min -1 ; t1: 89 Sr 90 The difference between the intermediate time of Y measurement and 89 Sr 90 The preparation time of Y standard substance.

[0022] In an embodiment of the present application, when testing with the liquid scintillation counter, 89 The calculation formula of the activity concentration of Sr is as follows:

[0023]

[0024] In the formula, The activity concentration of Sr in the liquid effluent, Bq / L; E 89 : the detection efficiency of the instrument to Sr Sr 89 : the detection efficiency of the instrument to Sr : the total count rate of the sample, cpm; n Srb : the background count rate, cpm; R Sr : the recovery rate of strontium ions; V: the volume of the liquid effluent sample, L; 0.8: the volume conversion coefficient of the sample source.

[0025] In an embodiment of the present application, when testing with the liquid scintillation counter, 90 The calculation formula of the activity concentration of Sr is as follows:

[0026]

[0027] In the formula, Liquid effluent 90 Activity concentration of Y, Bq / L; E Y Instrumental efficiency 90 Detection efficiency of Y, %; n Y Total sample count rate, cpm; n Yb Background count rate, cpm; R Y Recovery of yttrium ions; V: Liquid effluent sample volume, L; 0.8: Sample source volume conversion factor, t2: 90 Difference between the intermediate time of Y measurement and half of the total time required for the completion of effluent collection.

[0028] The strontium-89 and strontium-90 separation device of the present application integrates the concentration unit, the liquid storage unit, the enrichment unit, the separation and purification unit and the sample preparation unit, which can simplify the operation process, improve the process continuity, concentrate the metal ions through the concentration unit, greatly reduce the time consumed by the enrichment of metal ions, significantly improve the work efficiency, and the product obtained through the separation device can be directly subjected to subsequent analysis and testing, saving a lot of manpower and resource consumption. BRIEF DESCRIPTION OF DRAWINGS

[0029] In order to more clearly illustrate the technical solutions of the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present application, and those skilled in the art can obtain other embodiments according to these drawings without creative labor.

[0030] Figure 1 The schematic diagram of the strontium-89 and strontium-90 separation device in an embodiment of the present application;

[0031] Figure 2 The flow chart of the separation and analysis of strontium-89 and strontium-90.

[0032] Element number explanation:

[0033] 10, container; 100, concentration unit; 110, concentration device; 111, first water inlet; 112, first water outlet; 120, first syringe pump; 121, first water suction port; 122, first water discharge port; 200, liquid storage unit; 210, first liquid storage bottle; 220, second liquid storage bottle; 230, third liquid storage bottle; 240, fourth liquid storage bottle; 250, fifth liquid storage bottle; 260, waste liquid barrel; 300, enrichment unit; 310, water sample storage tank; 311, second water inlet; 312, third water inlet; 313, second water outlet; 320, enrichment resin column; 321, first flow inlet; 322, first flow outlet; 330, second syringe pump; 331, second water suction port; 332, second water discharge port; 340, first three-way valve; 350, third syringe pump; 351, third water suction port; 352, third water discharge port; 360, first switching valve; 370, first flow meter; 380, second flow meter; 390, third flow meter; 400, separation and purification unit; 410, fourth syringe pump; 411, fourth water suction port; 412, fourth water discharge port; 420, anion resin column; 421, second flow inlet; 422, second flow outlet; 430, yttrium specific resin column; 431, third flow inlet; 432, third flow outlet; 440, strontium specific resin column; 441, fourth flow inlet; 442, fourth flow outlet; 450, second three-way valve; 460, third three-way valve; 470, fourth three-way valve; 480, fifth three-way valve; 490, second switching valve; 500, sample preparation unit; 510, first sample bottle; 520, second sample bottle; 530, third sample bottle; 540, fourth sample bottle; 550, sixth three-way valve; 560, seventh three-way valve; 570, eighth three-way valve; 580, ninth three-way valve. DETAILED DESCRIPTION

[0034] Other advantages and embodiments of the present application will be disclosed in the following detailed description of the embodiments of the present application, and will be apparent from the drawings and the specification. The present application can be carried out or implemented by different embodiments, and the details of the specification can be modified based on different views and applications without departing from the spirit of the present application. It should be noted that the following examples and features in the examples can be combined with each other without conflict. It should also be understood that the terms used in the examples of the embodiments of the present application are used to describe specific embodiments, and are not intended to limit the scope of protection of the present application. The test methods in the following examples are not specified, and are generally carried out under conventional conditions, or under the conditions recommended by the manufacturers.

[0035] When the embodiments give numerical ranges, it should be understood that unless the application indicates otherwise, every numerical range's two endpoints, and any number between the two endpoints, can be selected. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art in the field of the application, and any method and material similar or equivalent in function, in result to those described herein, as the skilled artisan is aware, can be used to implement the present application.

[0036] It should be noted that the terms such as "upper", "lower", "left", "right", "middle", and "one" cited in the specification are only for the convenience of clear description, and are not intended to limit the scope of the application. Changes or adjustments of the relative relationship without substantial changes in technical content are also considered as the scope of the application.

[0037] Please refer to Figure 1 The application provides a separation device for strontium-89 and strontium-90, which is used for separating strontium-89 and strontium-90 in nuclear power plant liquid effluent in a container 10. The separation device comprises a concentration unit 100, a storage unit 200, an enrichment unit 300, a separation and purification unit 400 and a sample preparation unit 500. The concentration unit 100 is used for concentrating metal ions in the liquid effluent to form a concentrated liquid. The storage unit 200 is used for storing a treatment liquid. The enrichment unit 300 is in communication with the concentration unit 100 and the storage unit 200 respectively, so as to obtain the concentrated liquid and the treatment liquid respectively, and enriches the metal ions in the concentrated liquid and then desorbs to form an enriched liquid. The separation and purification unit 400 is in communication with the enrichment unit 300 and the storage unit 200 respectively, and is used for separating and purifying the enriched liquid, removing interfering ions, and obtaining a purified liquid. The sample preparation unit 500 is in communication with the separation and purification unit 400, obtains the purified liquid, and prepares the purified liquid into a sample to be measured. The separation device of the application can greatly reduce the enrichment time of the metal ions through the concentration unit 100, significantly improve the work efficiency, and save a large amount of manpower and resource consumption.

[0038] Please refer to Figure 1In an embodiment, the concentration unit 100 comprises a concentration device 110 and a first syringe pump 120 for transferring the liquid effluent in the container 10 to the concentration device 110 for concentration. The first syringe pump 120 can be disposed at a side of the concentration device 110 close to the container 10 or at a side of the concentration device 110 close to the enrichment unit 300. In the present embodiment, the first syringe pump 120 is disposed at a side of the concentration device 110 close to the enrichment unit 300. The concentration device 110 is provided with a first water inlet 111 and a first water outlet 112, and the first syringe pump 120 is provided with a first water suction inlet 121 and a first water discharge outlet 122. The first water inlet 111 is in communication with the water outlet of the container 10, the first water outlet 112 is in communication with the first water suction inlet 121, and the first water discharge outlet 122 is in communication with the enrichment unit 300. The type of the concentration device 110 is not limited herein as long as it can meet the requirement of concentrating the metal ions in the wastewater. In the present embodiment, the concentration device 110 is an electrodialyzer which can cause selective migration of ions in the wastewater under the action of an electric field. In other embodiments, the concentration unit 100 further comprises a detection device for monitoring the ion concentration in the wastewater, which is disposed between the driving device and the enrichment unit 300. The detection device can be a separate detection device or integrated with the first syringe pump 120.

[0039] Referring to Figure 1In an embodiment, the liquid storage unit 200 comprises a plurality of liquid storage bottles, each of which stores a different treatment liquid for use in the enrichment unit 300 for enriching metal ions in the concentrated liquid and the separation and purification unit 400 for separating and purifying the enriched liquid. The number of liquid storage bottles is not limited and can be adjusted according to actual needs. In this embodiment, the liquid storage unit 200 comprises five liquid storage bottles, which are referred to as a first liquid storage bottle 210, a second liquid storage bottle 220, a third liquid storage bottle 230, a fourth liquid storage bottle 240, and a fifth liquid storage bottle 250. The first liquid storage bottle 210, the second liquid storage bottle 220, the third liquid storage bottle 230, the fourth liquid storage bottle 240, and the fifth liquid storage bottle 250 are connected in parallel. In other embodiments, the liquid storage unit 200 further comprises a waste liquid tank 260 for collecting waste liquid, and the waste liquid tank 260 is connected in parallel with the plurality of liquid storage bottles. The types of treatment liquids are not limited and can be adjusted according to actual needs. For example, the treatment liquid in the first liquid storage bottle 210 is a 0.05 mol / L-0.1 mol / L nitric acid solution, the treatment liquid in the second liquid storage bottle 220 is a 6 mol / L-8 mol / L nitric acid / hydrochloric acid mixed solution, the treatment liquid in the third liquid storage bottle 230 is a 6 mol / L-8 mol / L nitric acid solution, the treatment liquid in the fourth liquid storage bottle 240 is a 0.05 mol / L-0.1 mol / L nitric acid solution, and the treatment liquid in the fifth liquid storage bottle 250 is a 0.05 mol / L-0.1 mol / L hydrochloric acid solution. A valve for controlling the flow of the treatment liquid is arranged at the bottle opening of each liquid storage bottle. The type of valve is not limited, for example, the valve can be a manual valve or an electric valve, as long as it can control the flow of the treatment liquid in the liquid storage bottle.

[0040] Please refer to Figure 1In an embodiment, the enrichment unit 300 comprises a water sample storage tank 310 and an enrichment resin column 320. The type of the enrichment resin column 320 is not limited here, and is adjusted according to the ion species in the wastewater, so that the enrichment and desorption of interfering ions in the concentrated liquid can be achieved, and subsequent separation and purification can be facilitated. In this embodiment, the enrichment resin column 320 is a cation resin column. The water sample storage tank 310 is provided with a second water inlet 311, a third water inlet 312, and a second water outlet 313. The second water inlet 311 is in communication with the first water outlet 122, and the third water inlet 312 is in communication with the liquid storage unit 200. A second syringe pump 330 is provided on the pipeline between the water sample storage tank 310 and the liquid storage unit 200. The second syringe pump 330 is provided with a second water inlet 331 and a second water outlet 332. The second water inlet 331 is in communication with the liquid storage unit 200, and the second water outlet 332 is in communication with the third water inlet 312. The enrichment resin column 320 is provided with a first flow inlet 321 and a first flow outlet 322. The first flow inlet 321 is in communication with the second water outlet 313 or the liquid storage unit 200, and the first flow outlet 322 is in communication with the separation and purification unit 400 or the first flow outlet 322 is in communication with the waste liquid tank 260. In this embodiment, a first three-way valve 340 is provided on the pipeline between the water sample storage tank 310 and the second syringe pump 330. By adjusting the first three-way valve 340, the liquid storage unit 200 can be in communication with the water sample storage tank 310 or the liquid storage unit 200 can be in communication with the enrichment resin column 320. A third syringe pump 350 is provided on the pipeline between the water sample storage tank 310 and the enrichment resin column 320, which is used to provide power for the flow of the concentrated liquid. By adjusting the third syringe pump 350, the flow rate of the concentrated liquid in the enrichment resin column 320 can be controlled, so as to adjust the enrichment rate of metal ions. The third syringe pump 350 is provided with a third water inlet 351 and a third water outlet 352. The third water inlet 351 is in communication with the second water outlet 313, and the second water outlet 332 is in communication with the first flow inlet 321. The first flow outlet 322 can be in communication with the waste liquid tank 260 through a separate pipeline, or can be integrated with other pipelines. In this embodiment, the first flow outlet 322 is connected to the pipeline between the liquid storage unit 200 and the separation and purification unit 400. A first switching valve 360 is provided on the pipeline between the first flow outlet 322 and the separation and purification unit 400. By controlling the first switching valve 360, the flow direction of the liquid in the pipeline can be adjusted, so that the waste liquid flowing out of the enrichment resin column 320 flows to the waste liquid tank 260 or the enriched liquid flowing out of the enrichment resin column 320 flows to the separation and purification unit 400 for further treatment.

[0041] Further, the third injection pump 350 and the enrichment resin column 320 are further provided with a first flow meter 370, through which the volume of the concentrated liquid flowing to the enrichment resin column 320 can be monitored, so as to realize quantitative collection of the concentrated liquid. The first three-way valve 340 and the second injection pump 330 are provided with a second flow meter 380, so as to realize quantitative collection of the treatment liquid of the liquid storage unit 200. Herein, the types of the first flow meter 370 and the second flow meter 380 are not limited, for example, the first flow meter 370 and the second flow meter 380 can be mass flow meters or volume flow meters. In the embodiment, the first flow meter 370 and the second flow meter 380 are mass flow meters.

[0042] In the embodiment, the enrichment process of the interference ions in the concentrated liquid by the enrichment unit 300 is as follows: the first three-way valve 340 is adjusted to make the enrichment resin column 320 communicate with the liquid storage unit 200, the valve on the first liquid storage bottle 210 is opened, the second injection pump 330 is started, the treatment liquid in the first liquid storage bottle 210 is transported to the enrichment resin column 320, so as to pretreat the enrichment resin column 320, and the waste liquid generated by the pretreatment is discharged into the waste liquid tank 260. The valve on the first liquid storage bottle 210 is closed, the first three-way valve 340 is adjusted to make the water sample storage tank 310 communicate with the liquid storage unit 200, the valve on the second liquid storage bottle 220 is opened, the treatment liquid in the second liquid storage bottle 220 is transported to the water sample storage tank 310 by the second injection pump 330, so as to pretreat the concentrated liquid, and the pretreated liquid is obtained. The valve on the second liquid storage bottle 220 is closed, the second injection pump 330 is stopped, the third injection pump 350 is started, the pretreated liquid in the water sample storage tank 310 is transferred to the enrichment resin column 320 for enrichment treatment, and the waste liquid generated by the enrichment treatment is discharged into the waste liquid tank 260. The third injection pump 350 is stopped, the second injection pump 330 is started, the first three-way valve 340 is adjusted to make the liquid storage unit 200 communicate with the enrichment resin column 320, the valve on the second liquid storage bottle 220 is opened, the treatment liquid in the second liquid storage bottle 220 is transported to the enrichment resin column 320 by the second injection pump 330, so as to desorb the metal ions enriched on the enrichment resin column 320 to form an enriched liquid, and the enriched liquid is transported to the separation and purification unit 400 for further treatment. In the embodiment, the treatment liquid in the second liquid storage bottle 220 can adjust the pH of the concentrated liquid in the water sample storage tank 310, which is beneficial to the enrichment of the interference metal ions in the concentrated liquid on the enrichment resin column 320. For example, the pH of the concentrated liquid is adjusted to 1-2 by the treatment liquid in the second liquid storage bottle 220. For example, the treatment liquid in the first liquid storage bottle 210 is a 0.1 mol / L nitric acid solution, and the treatment liquid in the second liquid storage bottle 220 is an 8 mol / L nitric acid solution.

[0043] Please refer to Figure 1Since strontium-90 is easy to decay into yttrium-90, the content of strontium-90 is characterized by the content of yttrium-90. In an embodiment, a fourth syringe pump 410 is arranged on the pipeline between the separation and purification unit 400 and the liquid storage unit 200, and the fourth syringe pump 410 is provided with a fourth water suction port 411 and a fourth water discharge port 412, the fourth water suction port 411 is in communication with the liquid storage unit 200, and the fourth water discharge port 412 is in communication with the separation and purification unit 400. In this embodiment, the separation and purification unit 400 includes an anion resin column 420 for adsorbing interfering ions, a yttrium specific resin column 430 for adsorbing yttrium ions, and a strontium specific resin column 440 for adsorbing strontium ions, the anion resin column 420 is provided with a second flow inlet 421 and a second flow outlet 422, the yttrium specific resin column 430 is provided with a third flow inlet 431 and a third flow outlet 432, and the strontium specific resin column 440 is provided with a fourth flow inlet 441 and a fourth flow outlet 442. In this embodiment, the second flow inlet 421 is in communication with the first flow outlet 322, the third flow inlet 431 is in communication with the second flow outlet 422, the fourth flow inlet 441 is in communication with the third flow outlet 432, and the fourth flow outlet 442 is in communication with the waste liquid tank 260, or the second flow inlet 421, the third flow inlet 431 and the fourth flow inlet 441 are respectively in communication with the liquid storage unit 200. In this embodiment, a second three-way valve 450 is arranged between the separation and purification unit 400 and the liquid storage unit 200, and by adjusting the second three-way valve 450, the liquid storage unit 200 can be in communication with the anion resin column 420 or the liquid storage unit 200 can be in communication with the yttrium specific resin column 430 and the strontium specific resin column 440. The second flow outlet 422 is provided with a third three-way valve 460, the third flow outlet 432 is provided with a fourth three-way valve 470, and the fourth flow outlet 442 is provided with a fifth three-way valve 480. By adjusting the third three-way valve 460, the second flow outlet 422 can be in communication with the third flow inlet 431 or the second flow outlet 422 can be in communication with the waste liquid tank 260. By adjusting the fourth three-way valve 470, the third flow outlet 432 can be in communication with the fourth flow inlet 441 or the third flow outlet 432 can be in communication with the waste liquid tank 260. By adjusting the fifth three-way valve 480, the fourth flow outlet 442 can be in communication with the waste liquid tank 260 or the fourth flow outlet 442 can be in communication with the sample preparation unit 500. In order to simplify the pipeline, in this embodiment, the pipelines in which the yttrium specific resin column 430 and the strontium specific resin column 440 are in communication with the sample preparation unit 500 and the pipelines in which the yttrium specific resin column 430 and the strontium specific resin column 440 are in communication with the waste liquid tank 260 are integrated, and a second switch valve 490 is arranged on the integrated pipeline. By adjusting the flow direction of the liquid in the pipeline through the second switch valve 490, the liquid flowing out of the resin column can flow into the sample preparation unit 500 or the waste liquid tank 260. In this embodiment, the fourth syringe pump 410 is arranged near one side of the liquid storage unit 200, and a third flow meter 390 is further arranged between the fourth syringe pump 410 and the first switch valve 360, for quantitatively collecting the treatment liquid in the liquid storage unit 200.The type of the third flow meter 390 is not limited, for example, the third flow meter 390 can be a mass flow meter or a volume flow meter. In this embodiment, the third flow meter 390 is a mass flow meter.

[0044] In this embodiment, the separation and purification unit 400 separates and purifies the enriched liquid as follows: first, the anion resin column 420, the yttrium specific resin column 430 and the strontium specific resin column 440 are pretreated. The specific operation is as follows: start the fourth injection pump 410, adjust the second three-way valve 450 so that the second flow inlet 421 communicates with the liquid storage unit 200, adjust the third three-way valve 460 so that the second flow outlet 422 communicates with the waste liquid barrel 260, open the valve on the third liquid storage bottle 230, and use the treatment liquid in the third liquid storage bottle 230 to pretreat the anion resin column 420, close the valve on the third liquid storage bottle 230, adjust the second three-way valve 450 so that the third flow inlet 431 and the fourth flow inlet 441 communicate with the liquid storage unit 200, adjust the fourth three-way valve 470 so that the third flow outlet 432 communicates with the waste liquid barrel 260, adjust the fifth three-way valve 480 so that the fourth flow outlet 442 communicates with the waste liquid barrel 260, open the valve on the second liquid storage bottle 220, and use the treatment liquid in the second liquid storage bottle 220 to pretreat the yttrium specific resin column 430 and the strontium specific resin column 440, after the pretreatment is completed, close the valve on the third liquid storage bottle 230, and stop the fourth injection pump 410. Adjust the third three-way valve 460, the fourth three-way valve 470 and the fifth three-way valve 480 so that the second flow outlet 422 communicates with the third flow inlet 431, the third flow outlet 432 communicates with the fourth flow inlet 441, and the fourth flow outlet 442 communicates with the waste liquid barrel 260, start the third injection pump 350, and under the drive of the third injection pump 350, the enriched liquid flows through the anion resin column 420, the yttrium specific resin column 430 and the strontium specific resin column 440 in sequence, the anion resin column 420 adsorbs the interfering ions in the enriched liquid, the yttrium specific resin column 430 adsorbs the yttrium ions in the enriched liquid, and the strontium specific resin column 440 adsorbs the strontium ions in the enriched liquid, so as to separate and purify the ions in the enriched liquid. After adsorption is completed, the third injection pump 350 is closed, the fourth injection pump 410 is started, the valve on the fifth liquid storage bottle 250 is opened, the fourth injection pump 410 injects the treatment liquid in the fifth liquid storage bottle 250 into the yttrium specific resin column 430 to desorb the yttrium ions adsorbed on the yttrium specific resin column 430, and the desorbed solution is delivered to the sample preparation unit 500 to prepare a to-be-tested sample; the valve on the fifth liquid storage bottle 250 is closed, the valve on the fourth liquid storage bottle 240 is opened, the fourth injection pump 410 injects the treatment liquid in the fifth liquid storage bottle 250 into the strontium specific resin column 440 to desorb the strontium ions on the strontium specific resin column 440, and the desorbed solution is delivered to the sample preparation unit 500 to prepare a to-be-tested sample. For example, the interfering ions in the enriched liquid are iron ions, the treatment liquid in the fourth liquid storage bottle 240 is a 0.05 mol / L nitric acid solution, and the treatment liquid in the fifth liquid storage bottle 250 is a 0.05 mol / L hydrochloric acid solution.

[0045] See Figure 1In one embodiment, the sample preparation unit 500 includes a first sample bottle 510 for storing yttrium solution and a second sample bottle 520 for storing strontium solution, the first sample bottle 510 is in communication with the third flow outlet 432, and the second sample bottle 520 is in communication with the fourth flow outlet 442. Further, the sample preparation unit 500 includes a third sample bottle 530 for sampling the yttrium elution solution and a fourth sample bottle 540 for sampling the strontium elution solution. A sixth three-way valve 550 is arranged on the pipeline connecting the first sample bottle 510 and the yttrium specific resin column 430, the sixth three-way valve 550 is in communication with the third flow outlet 432, the first sample bottle 510 and the third sample bottle 530 respectively, and through the sixth three-way valve 550, a part of the yttrium elution solution can flow into the first sample bottle 510 to prepare the sample to be measured, and the remaining yttrium elution solution can flow into the third sample bottle 530 for laboratory analysis when the result is abnormal. A seventh three-way valve 560 is arranged on the pipeline connecting the second sample bottle 520 and the strontium specific resin column 440, the seventh three-way valve 560 is in communication with the fourth flow outlet 442, the second sample bottle 520 and the fourth sample bottle 540 respectively, and by adjusting the seventh three-way valve 560, a part of the strontium elution solution can flow into the second sample bottle 520 to prepare the sample to be measured, and the remaining strontium elution solution can flow into the fourth sample bottle 540 for laboratory analysis when the result is abnormal.

[0046] Please refer to Figure 1 In one embodiment, the sample to be measured in the first sample bottle 510 and the third sample bottle 530 needs to be further processed. A separate pipeline can be arranged to connect the sample preparation unit 500 and the liquid storage unit 200, or a branch pipeline can be arranged on the pipeline between the separation and purification unit 400 and the liquid storage unit 200. In one embodiment, an eighth three-way valve 570 is arranged on the pipeline between the separation and purification unit 400 and the liquid storage unit 200, and by adjusting the eighth three-way valve 570, the liquid storage unit 200 is in communication with the separation and purification unit 400 or the liquid storage unit 200 is in communication with the sample preparation unit 500.

[0047] When the sample to be tested is further processed, the eighth three-way valve 570 is adjusted to connect the storage unit 200 with the sample preparation unit 500, and the valve on the corresponding storage bottle is opened, so that the sample to be tested is processed by the processing liquid. In the embodiment, the branch connected with the sample preparation unit 500 is provided with a ninth three-way valve 580, and the ninth three-way valve 580 is adjusted to realize the connection of the branch with the sixth three-way valve 550 and / or the seventh three-way valve 560. For example, if the processing liquid used when the sample to be tested is processed is the same, the first sample bottle 510 and the second sample bottle 520 can be connected with the storage bottle at the same time by adjusting the sixth three-way valve 550, the seventh three-way valve 560 and the ninth three-way valve 580, and if the processing liquid used when the sample to be tested is processed is different, one of the first sample bottle 510 and the second sample bottle 520 can be connected with the storage bottle by adjusting the sixth three-way valve 550, the seventh three-way valve 560 and the ninth three-way valve 580, and after the processing is completed, the other of the first sample bottle 510 and the second sample bottle 520 can be connected with the storage bottle by adjusting the sixth three-way valve 550, the seventh three-way valve 560 and the ninth three-way valve 580.

[0048] Referring to Figure 2 The application further provides a method for separating and analyzing strontium-89 and strontium-90 by using the separation device, comprising the following steps:

[0049] S1, concentrating metal ions in liquid effluent of a nuclear power plant to form a concentrated liquid;

[0050] S2, pretreating the concentrated liquid to obtain a pretreated liquid, desorbing and enriching metal ions in the pretreated liquid to form an enriched liquid;

[0051] S3, separating and purifying the enriched liquid to remove interfering ions to obtain a purified liquid;

[0052] S4, preparing the purified liquid into a sample to be measured;

[0053] S5, sending the sample to be measured into a liquid scintillation spectrometer for testing.

[0054] In an embodiment, the analysis method further comprises calculating the recovery rate of the metal ions after the step of preparing the purified liquid into the sample to be measured, and the calculation formula of the recovery rate is as follows:

[0055]

[0056] In the formula, R is the recovery rate, %, Q is the concentration of the metal ions in the sample to be measured, mg / L, and Q0 is the concentration of the metal ions in the pretreated liquid, mg / L.

[0057] In some embodiments, when the sample to be measured is detected by the liquid scintillation spectrometer, 89Sr 90 The calculation formula of the detection efficiency of Y is as follows:

[0058]

[0059] E: instrument efficiency, %; n 89 Sr 90 Y detection efficiency, %; n s : total count rate of sample, cpm; n b : background count rate, cpm; c0: 89 Sr 90 Y standard solution activity concentration, Bq / mL; V0: 89 Sr 90 Y standard solution volume, mL; λ: decay constant, 89 The decay constant of Sr is 9.52E-6 min -1 , 90 The decay constant of Y is 4.56E-8 min -1 ; t1: 89 Sr 90 The difference between the intermediate time of Y measurement and 89 Sr 90 The difference between the preparation time of Y standard substance and

[0060] 89 The calculation formula of the activity concentration of Sr is as follows:

[0061]

[0062] E: instrument efficiency, %; n The activity concentration of Sr in liquid effluent, Bq / L; E 89 : instrument efficiency, %; n Sr : instrument efficiency, %; n 89 Sr detection efficiency, %; n Sr : total count rate of sample, cpm; n Srb : background count rate, cpm; R Sr : recovery rate of strontium ion; V: liquid effluent sample volume, L; 0.8: sample source volume conversion coefficient.

[0063] 90 The calculation formula of the activity concentration of Sr is as follows:

[0064]

[0065] E: instrument efficiency, %; n The activity concentration of Y in liquid effluent, Bq / L; E 90 : instrument efficiency, %; n Y : instrument efficiency, %; n 90 Y detection efficiency, %; n Y: Total sample count rate, cpm; n Yb : Background count rate, cpm; R Y : Recovery of yttrium ions; V: Liquid effluent sample volume, L; 0.8: Sample source volume conversion factor, t2: 90 The difference between the intermediate time of Y measurement and half of the total time required for the completion of effluent collection.

[0066] The separation device for strontium-89 and strontium-90 of the present application integrates the concentration unit, the liquid storage unit, the enrichment unit, the separation and purification unit and the sample preparation unit, which can simplify the operation process, improve the process continuity, concentrate the metal ions through the concentration unit, greatly reduce the time consumed by the enrichment of metal ions, significantly improve the work efficiency, and directly perform subsequent analysis and testing on the product obtained through the separation device, thereby saving a large amount of manpower and resource consumption. Therefore, the present application effectively overcomes some practical problems in the prior art, thereby having high utilization value and use significance.

[0067] The above examples only exemplarily illustrate the principles and effects of the present application, and are not used to limit the present application. Any person skilled in the art can modify or change the above examples without departing from the spirit and scope of the present application. Therefore, all equivalent modifications or changes completed by those skilled in the art without departing from the spirit and technical thought disclosed by the present application should be covered by the claims of the present application.

Claims

1. A device for separating strontium-89 and strontium-90 from nuclear power plant liquid effluents in a container (10), characterized in that, The application relates to a nuclear power plant liquid effluent treatment device, which comprises the following units: a concentration unit (100) for concentrating metal ions in the nuclear power plant liquid effluent to prepare a concentrated liquid, the concentration unit (100) comprising a concentration device (110) and a first injection pump (120); a storage unit (200) for storing a treatment liquid; an enrichment unit (300) in communication with the concentration unit (100) and the storage unit (200) respectively, for obtaining the concentrated liquid and the treatment liquid respectively, enriching metal ions in the concentrated liquid and then desorbing to form an enriched liquid, the enrichment unit (300) comprising a water sample storage tank (310) and an enrichment resin column (320); a separation and purification unit (400) in communication with the enrichment unit (300) and the storage unit (200) respectively, and used for separating and purifying the enriched liquid to remove interfering ions and obtain a purified liquid, the separation and purification unit (400) comprising an anion resin column (420) for adsorbing interfering ions, a yttrium specific resin column (430) for adsorbing yttrium ions and a strontium specific resin column (440) for adsorbing strontium ions; a sample preparation unit (500) in communication with the separation and purification unit (400), for obtaining the purified liquid and preparing the purified liquid into a sample to be measured, the sample preparation unit (500) comprising a first sample bottle (510) for storing a yttrium solution and a second sample bottle (520) for storing a strontium solution.

2. The apparatus for separation of strontium-89 and strontium-90 according to claim 1, characterized in that, The concentration device (110) is provided with a first water inlet (111) and a first water outlet (112), the first injection pump (120) is provided with a first water suction port (121) and a first water discharge port (122), the first water inlet (111) is in communication with a water outlet of a container (10), the first water outlet (112) is in communication with the first water suction port (121), and the first water discharge port (122) is in communication with the enrichment unit (300).

3. The apparatus for separation of strontium-89 and strontium-90 according to claim 2, characterized in that, The water sample storage tank (310) is provided with a second water inlet (311), a third water inlet (312) and a second water outlet (313), the second water inlet (311) is communicated with the first water outlet (122), the third water inlet (312) is communicated with the liquid storage unit (200), a second syringe pump (330) is arranged on the pipeline of the water sample storage tank (310) and the liquid storage unit (200), the second syringe pump (330) is provided with a second water inlet (331) and a second water outlet (332), the second water inlet (331) is communicated with the liquid storage unit (200), and the second water outlet (332) is communicated with the third water inlet (312); The enrichment resin column (320) is provided with a first flow inlet (321) and a first flow outlet (322), the first flow inlet (321) is communicated with the second water outlet (313) or the liquid storage unit (200), and the first flow outlet (322) is communicated with the separation and purification unit (400); A third syringe pump (350) is arranged on the pipeline between the water sample storage tank (310) and the enrichment resin column (320), the third syringe pump (350) is provided with a third water inlet (351) and a third water outlet (352), the third water inlet (351) is communicated with the second water outlet (313), and the second water outlet (332) is communicated with the first flow inlet (321).

4. The apparatus for separation of strontium-89 and strontium-90 according to claim 3, characterized in that, A fourth syringe pump (410) is arranged on the pipeline between the separation and purification unit (400) and the liquid storage unit (200), the fourth syringe pump (410) is provided with a fourth water inlet (411) and a fourth water outlet (412), the fourth water inlet (411) is communicated with the liquid storage unit (200), and the fourth water outlet (412) is communicated with the separation and purification unit (400); The anion resin column (420) is provided with a second flow inlet (421) and a second flow outlet (422), the yttrium specific resin column (430) is provided with a third flow inlet (431) and a third flow outlet (432), the strontium specific resin column (440) is provided with a fourth flow inlet (441) and a fourth flow outlet (442), the second flow inlet (421) is communicated with the first flow outlet (322), the third flow inlet (431) is communicated with the second flow outlet (422), the fourth flow inlet (441) is communicated with the third flow outlet (432), and the fourth flow outlet (442) is communicated with a waste liquid collecting device, or the second flow inlet (421), the third flow inlet (431) and the fourth flow inlet (441) are respectively communicated with the liquid storage unit (200).

5. The apparatus for separation of strontium-89 and strontium-90 according to claim 4, characterized in that, The first sample bottle (510) is communicated with the third flow outlet (432), and the second sample bottle (520) is communicated with the fourth flow outlet (442).

6. A method for separating and analyzing strontium-89 and strontium-90 using the separation device according to any one of claims 1 to 5, characterized by, The method comprises the following steps: Concentrating metal ions in liquid effluent of a nuclear power plant to form a concentrated liquid; The concentrated liquid is pretreated to obtain a pretreated liquid, and the metal ions in the pretreated liquid are enriched and then desorbed to form an enriched liquid; The enriched liquid is separated and purified to remove interfering ions, and a purified liquid is obtained; The purified liquid is prepared into a sample to be measured; The sample to be measured is sent into a liquid scintillation spectrometer for testing.

7. The separation analysis method according to claim 6, wherein, After the step of preparing the purified liquid into a sample to be measured, the recovery rate of the metal ions is calculated, and the calculation formula of the recovery rate is as follows: In the formula, R is the recovery rate, %; Q is the concentration of the metal ions in the sample to be measured, mg / L; Q0 is the concentration of the metal ions in the pretreated liquid, mg / L.

8. The separation analysis method according to claim 6, wherein, When testing with the liquid scintillation spectrometer, 89 Sr 90 The formula for calculating the detection efficiency of Y is as follows: Where: E: instrument efficiency 89 Sr / 90 Y: detection efficiency of Y, %; n s : total count rate of sample, cpm; n b : background count rate, cpm; c0: 89 Sr / 90 Y: activity concentration of Y standard solution, Bq / mL; V0: 89 Sr / 90 Y: volume of Y standard solution, mL; λ: decay constant, 89 The decay constant for Sr is 9.52E-6 min -1 , 90 The decay constant for Y is 4.56E-8 min -1 ; t1: 89 Sr / 90 Y the difference between the measurement intermediate time and 89 Sr / 90 Y the time of the standard substance configuration.

9. The separation analysis method according to claim 7, wherein, When testing with the liquid scintillation spectrometer, 89 The formula for calculating the activity concentration of Sr is as follows: where: : Sr activity concentration in liquid effluent, Bq / L 89 Sr activity concentration, Bq / L; E Sr : instrument efficiency for 89 Sr detection efficiency, %; : total sample count rate, cpm; : background count rate, cpm; R Sr : strontium ion recovery; V: liquid effluent sample volume, L; 0.8: sample source volume conversion coefficient.

10. The separation analysis method according to claim 7, wherein, When testing with the liquid scintillation spectrometer, 90 The formula for calculating the activity concentration of Sr is as follows: wherein: : Recovery of Y in liquid effluent 90 Activity concentration of Y, Bq / L; E Y : Instrumental efficiency 90 Detection efficiency of Y, %; : Total sample count rate, cpm; : Background count rate, cpm; R Y : Recovery of Yttrium ions; V: volume of liquid effluent sample, L; 0.8: volume conversion factor from sample source, : 90 Y the difference between the intermediate time of the Y measurement and half of the total time required for the effluent collection to be completed.

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