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

Abstract

The invention provides a strontium-89 and strontium-90 separation device, and relates to the technical field of radioactive substance measurement. The separation device comprises a concentration unit, a liquid storage unit, an enrichment unit, a separation and purification unit and a sample preparation unit, wherein the concentration unit is used for concentrating metal ions in the liquid effluent of the nuclear power plant in the container to prepare a concentrated solution; the liquid storage unit is used for storing treatment liquid; the enrichment unit is respectively communicated with the concentration unit and the liquid storage unit so as to respectively obtain a concentrated solution and a treatment solution and desorb after enriching metal ions in the concentrated solution to form an enriched solution; the separation and purification unit is respectively communicated with the enrichment unit and the liquid storage unit and is used for separating and purifying the enriched liquid and removing interference ions to obtain purified liquid; the sample preparation unit is communicated with the separation and purification unit, and is used for obtaining the purified liquid and preparing the purified liquid into a to-be-measured sample. According to the separation device, the enrichment time of metal ions can be greatly shortened through the concentration unit, the working efficiency is remarkably improved, and a large amount of manpower and resource consumption are saved.

Description

Technical Field

[0001] The present invention relates to the technical field of radioactive material measurement, and in particular to a separation device and a separation and analysis method for strontium-89 and strontium-90. Background Art

[0002] Rapid and accurate analysis of radioactive materials is the basis and key to environmental radiation monitoring and nuclear emergency monitoring. 89 Sr and 90 Sr is a fission product with high radiation toxicity. 89 The half-life of Sr is 50.563 days, and it decays into stable nuclides through β decay. 89 Y. 90 Sr is an unstable long-lived radionuclide that can produce radionuclides through β decay 90 Y, 90 Y can decay into a stable element 90 Zr. 89 Sr (Eβmax=1499.3keV), 90 Sr (Eβmax=545.9keV) and its daughter 90 Y (Eβmax=2278.5keV) only emits β rays, and non-destructive measurement methods such as γ spectrum cannot measure them. β rays are continuous spectrum, and will be interfered by β rays of other radioactive nuclides during measurement. 89 Sr. 90 Sr and its daughter 90 Before measuring Y radioactivity, the sample needs to be radiochemically separated to remove other radionuclides in the sample.

[0003] Traditional radiochemical separation methods include precipitation, ion exchange, liquid-liquid extraction, etc. These conventional methods have complex processes and long sample analysis times. The current resource allocation of my country's nuclear power plants is difficult to adapt to this inefficient method and needs to be improved. Summary of the invention

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

[0005] To achieve the above-mentioned purpose and other related purposes, the first aspect of the present invention provides a strontium-89 and strontium-90 separation device for separating strontium-89 and strontium-90 from liquid effluent of a nuclear power plant in a container, the separation device comprising a concentration unit, a liquid storage unit, an enrichment unit, a separation and purification unit and a sample preparation unit, the concentration unit being used to concentrate the metal ions in the liquid effluent of the nuclear power plant to form a concentrated solution; the liquid storage unit being used to store the treatment solution; the enrichment unit being connected to the concentration unit and the liquid storage unit respectively to obtain the concentrated solution and the treatment solution respectively and to enrich the metal ions in the concentrated solution and then to desorb them to form an enriched solution; the separation and purification unit being connected to the enrichment unit and the liquid storage unit respectively and to separate and purify the enriched solution, remove interfering ions and obtain a purified solution; the sample preparation unit being connected to the separation and purification unit to obtain the purified solution and prepare the purified solution into a sample to be measured.

[0006] In one embodiment of the present invention, the concentration unit includes a concentration device and a first injection pump, the concentration device is provided with a first water inlet and a first water outlet, the first injection pump is provided with a first water pumping port and a first water discharge port, the first water inlet is connected to the water outlet of the container, the first water outlet is connected to the first water pumping port, and the first water discharge port is connected to the enrichment unit.

[0007] In one embodiment of the present invention, the enrichment unit includes a water sample storage box and an enrichment resin column, the water sample storage box is provided with a second water inlet, a third water inlet and a second water outlet, the second water inlet is connected to the first drain, the third water inlet is connected to the liquid storage unit, a second injection pump is provided on the pipeline between the water sample storage box and the liquid storage unit, the second injection pump is provided with a second water pumping port and a second drain, the second water pumping port is connected to the liquid storage unit, and the second drain is connected to the third water inlet; the enrichment resin column is provided with a first inlet and a first outlet, the first inlet is connected to the second water outlet or the liquid storage unit, and the first outlet is connected to the separation and purification unit; a third injection pump is provided on the pipeline between the water sample storage box and the enrichment resin column, the third injection pump is provided with a third water pumping port and a third drain, the third water pumping port is connected to the second water outlet, and the second drain is connected to the first inlet.

[0008] In one embodiment of the present invention, a fourth injection pump is provided on the pipeline between the separation and purification unit and the liquid storage unit, and a fourth water pumping port and a fourth water discharge port are provided on the fourth injection pump, the fourth water pumping 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, 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, the strontium-specific resin column is provided with a fourth inlet and a fourth outlet, 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, the fourth outlet is communicated with a waste liquid collection device, or the second inlet, the third inlet and the fourth inlet are respectively communicated with the liquid storage unit.

[0009] In one embodiment of the present invention, the sample preparation unit includes a first sample bottle for storing yttrium solution and a second sample bottle for storing strontium solution, the first sample bottle is connected to the third outflow port, and the second sample bottle is connected to the fourth outflow port.

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

[0011] Concentrating metal ions in liquid effluent from nuclear power plants to form concentrated liquid;

[0012] Pre-treating the concentrated solution to obtain a pre-treated solution, and desorbing the metal ions in the pre-treated solution after enrichment to form an enriched solution;

[0013] The enriched solution is separated and purified to remove interfering ions and obtain a purified solution;

[0014] preparing the purified solution into a sample to be measured;

[0015] The sample to be measured is sent to a liquid scintillation spectrometer for testing.

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

[0017]

[0018] Wherein: R is the recovery rate, %; Q is the concentration of metal ions in the sample to be measured, mg / L; Q0 is the concentration of metal ions in the pretreatment solution, mg / L.

[0019] In one embodiment of the present invention, when the liquid scintillation spectrometer is used for testing, 89 Sr / 90 The calculation formula of the detection efficiency of Y is as follows:

[0020]

[0021] Where: E: instrument pair 89 Sr / 90 Detection efficiency of Y, %; n s : Total sample count rate, cpm; n b : Background count rate, cpm; c0: 89 Sr / 90 Activity concentration of Y standard solution, Bq / mL; V0: 89 Sr / 90 Y: volume of standard solution, mL; λ: decay constant, 89 The decay constant of Sr is 9.52E-6min -1 , 90 The decay constant of Y is 4.56E-8min -1 ; t1: 89 Sr / 90 Y measures the intermediate moments and 89 Sr / 90 Y is the difference in the preparation time of the standard substance.

[0022] In one embodiment of the present invention, when the liquid scintillation spectrometer is used for testing, 89 The calculation formula of Sr activity concentration is as follows:

[0023]

[0024] Where: In liquid outflow 89 Activity concentration of Sr, Bq / L; E Sr :Instrument pair 89 Detection efficiency of Sr, %; n Sr : Total sample count rate, cpm; n Srb : Background count rate, cpm; R Sr : recovery rate of strontium ions; V: liquid effluent sample volume, L; 0.8: sample source volume conversion coefficient.

[0025] In one embodiment of the present invention, when the liquid scintillation spectrometer is used for testing, 90 The calculation formula of Sr activity concentration is as follows:

[0026]

[0027] Where: In liquid outflow 90 Activity concentration of Y, Bq / L; E Y :Instrument pair 90 Detection efficiency of Y, %; n Y : Total sample count rate, cpm; n Yb : Background count rate, cpm; R Y : recovery rate of yttrium ions; V: liquid effluent sample volume, L; 0.8: sample source volume conversion factor, t2: 90 Y measures the difference between the midpoint and half the total time required to complete effluent collection.

[0028] The strontium-89 and strontium-90 separation device of the present invention integrates a concentration unit, a liquid storage unit, an enrichment unit, a separation and purification unit and a sample preparation unit, which can simplify the operation process and improve the process continuity. The metal ions are concentrated by the concentration unit, which greatly reduces the time consumed for metal ion enrichment and significantly improves the work efficiency. The product obtained by the separation device can be directly used for subsequent analysis and testing, saving a lot of manpower and resource consumption. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For ordinary technicians in this field, other embodiments can be obtained based on these drawings without paying creative work.

[0030] Figure 1 FIG. 1 is a schematic diagram of a strontium-89 and strontium-90 separation device according to an embodiment of the present invention;

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

[0032] Component number description:

[0033] 10. container; 100. concentration unit; 110. concentration device; 111. first water inlet; 112. first water outlet; 120. first injection pump; 121. first water extraction port; 122. first drainage 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 box; 311, second water inlet; 312, third water inlet; 313, second water outlet; 320, enrichment resin column; 321, first inlet; 322, first outlet; 330, second injection pump; 331, second water extraction port; 332, second drain port; 340, first three-way valve; 350, third injection pump; 351, third water extraction port; 352, third drain port; 360, first switching valve; 3 70, first flow meter; 380, second flow meter; 390, third flow meter; 400, separation and purification unit; 410, fourth injection pump; 411, fourth water inlet; 412, fourth water outlet; 420, anion resin column; 421, second inlet; 422, second outlet; 430, yttrium special effect resin column; 431, third inlet; 432, third outlet; 440, strontium special effect resin column; 441, fourth inlet port; 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] The following is an explanation of the embodiments of the present invention by specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention. It should be noted that the features in the following embodiments and the embodiments can be combined with each other without conflict. It should also be understood that the terms used in the embodiments of the present invention are intended to describe specific embodiments, rather than to limit the scope of protection of the present invention. The test methods for which specific conditions are not indicated in the following examples are usually carried out under conventional conditions or according to the conditions recommended by the manufacturers.

[0035] When numerical ranges are given in the embodiments, it should be understood that unless otherwise specified in the present invention, both endpoints of each numerical range and any value between the two endpoints can be selected. Unless otherwise defined, all technical and scientific terms used in the present invention are familiar to those skilled in the art and the description of the present invention, and any method, device and material of the prior art similar or equivalent to the method, device and material in the embodiments of the present invention can also be used to implement the present invention.

[0036] It should be noted that the terms such as "upper", "lower", "left", "right", "middle" and "one" etc. used in this specification are only for the convenience of description and are not intended to limit the scope of implementation of the present invention. Changes or adjustments to their relative relationships, without substantially changing the technical content, should also be regarded as the scope of implementation of the present invention.

[0037] See also Figure 1 The present invention provides a strontium-89 and strontium-90 separation device, which is used to separate strontium-89 and strontium-90 from the liquid effluent of a nuclear power plant in a container 10. The separation device includes a concentration unit 100, a liquid 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 to concentrate the metal ions in the liquid effluent to form a concentrated solution; the liquid storage unit 200 is used to store the treatment solution; the enrichment unit 300 is connected to the concentration unit 100 and the liquid storage unit 200 respectively, so as to obtain the concentrated solution and the treatment solution respectively, and enrich the metal ions in the concentrated solution and then desorb them to form an enriched solution; the separation and purification unit 400 is connected to the enrichment unit 300 and the liquid storage unit 200 respectively, and is used to separate and purify the enriched solution, remove interfering ions, and obtain a purified solution; the sample preparation unit 500 is connected to the separation and purification unit 400, obtains the purified solution and prepares the purified solution into a sample to be measured. The separation device of the present application can greatly reduce the enrichment time of metal ions through the concentration unit 100, significantly improve work efficiency, and save a lot of manpower and resource consumption.

[0038] See also Figure 1In one embodiment, the concentration unit 100 includes a concentration device 110 and a first injection pump 120. The first injection pump 120 is used to transfer the liquid effluent in the container 10 to the concentration device 110 for concentration. The first injection pump 120 can be arranged on the side of the concentration device 110 close to the container 10, or on the side of the concentration device 110 close to the enrichment unit 300. In this embodiment, the first injection pump 120 is arranged on the 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 injection pump 120 is provided with a first water pumping port 121 and a first water outlet 122. The first water inlet 111 is connected to the water outlet of the container 10, the first water outlet 112 is connected to the first water pumping port 121, and the first water outlet 122 is connected to the enrichment unit 300. The type of the concentration device 110 is not limited here, as long as it can meet the concentration of metal ions in wastewater. In this embodiment, the concentration device 110 uses an electrodialyzer, which can selectively migrate ions in the wastewater under the action of an electric field. In other embodiments, the concentration unit 100 also includes a detection device for monitoring the ion concentration in the wastewater, and the detection device is arranged between the driving device and the enrichment unit 300. Exemplarily, the detection device can be a separate detection device, or it can be integrated with the first injection pump 120.

[0039] See also Figure 1In one embodiment, the liquid storage unit 200 includes a plurality of liquid storage bottles, each of which contains a different treatment liquid for participating in the metal ion enrichment of the concentrate by the enrichment unit 300 and the separation and purification of the enriched liquid by the separation and purification unit 400. Here, there is no restriction on the number of liquid storage bottles, which can be adjusted according to actual needs. In this embodiment, the liquid storage unit 200 includes five liquid storage bottles, which are respectively recorded as 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, and 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 also includes a waste liquid barrel 260 for collecting waste liquid, and the waste liquid barrel 260 is connected in parallel with a plurality of liquid storage bottles. There is no restriction on the type of treatment liquid here, which can be adjusted according to actual needs. Exemplarily, the treatment liquid in the first liquid storage bottle 210 is a 0.05mol / L to 0.1mol / L nitric acid solution, the treatment liquid in the second liquid storage bottle 220 is a 6mol / L to 8mol / L nitric acid / hydrochloric acid mixed solution, the treatment liquid in the third liquid storage bottle 230 is a 6mol / L to 8mol / L nitric acid solution, the treatment liquid in the fourth liquid storage bottle 240 is a 0.05mol / L to 0.1mol / L nitric acid solution, and the treatment liquid in the fifth liquid storage bottle 250 is a 0.05mol / L to 0.1mol / L hydrochloric acid solution. A valve for controlling the outflow of the treatment liquid is provided at the mouth of each liquid storage bottle. There is no restriction on the type of valve here. For example, the valve can be a manual valve or an electric valve, as long as it can control the outflow of the treatment liquid in the liquid storage bottle.

[0040] See also Figure 1In one embodiment, the enrichment unit 300 includes a water sample storage box 310 and an enrichment resin column 320. Here, the type of the enrichment resin column 320 is not limited. It is adaptively adjusted according to the type of ions in the wastewater to meet the enrichment and desorption of interfering ions in the concentrate, so as to facilitate subsequent separation and purification. In this embodiment, the enrichment resin column 320 is a cationic resin column. The water sample storage box 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 connected to the first drain port 122, and the third water inlet 312 is connected to the liquid storage unit 200. A second injection pump 330 is provided on the pipeline between the water sample storage box 310 and the liquid storage unit 200. The second injection pump 330 is provided with a second water pumping port 331 and a second drain port 332. The second water pumping port 331 is connected to the liquid storage unit 200, and the second drain port 332 is connected to the third water inlet 312. The enrichment resin column 320 is provided with a first inlet 321 and a first outlet 322. The first inlet 321 is connected to the second water outlet 313 or the liquid storage unit 200, and the first outlet 322 is connected to the separation and purification unit 400 or the first outlet 322 is connected to the waste liquid bucket 260. In this embodiment, a first three-way valve 340 is provided on the pipeline between the water sample storage box 310 and the second injection pump 330. By adjusting the first three-way valve 340, the liquid storage unit 200 can be connected to the water sample storage box 310 or the liquid storage unit 200 can be connected to the enrichment resin column 320. A third injection pump 350 is provided on the pipeline between the water sample storage box 310 and the enrichment resin column 320 to provide power for the flow of the concentrate, and by adjusting the third injection pump 350, the flow rate of the concentrate in the enrichment resin column 320 can be controlled to adjust the enrichment rate of the metal ions. The third injection pump 350 is provided with a third water pumping port 351 and a third water discharge port 352, the third water pumping port 351 is connected to the second water outlet 313, and the second water discharge port 332 is connected to the first inlet 321. The first outlet 322 can be connected to the waste liquid barrel 260 through a separate pipeline, or it can be integrated with other pipelines. In this embodiment, the first outlet 322 is connected to the pipeline between the liquid storage unit 200 and the separation and purification unit 400, and the first switching valve 360 ​​is provided on the pipeline between the first 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 to achieve the waste liquid flowing out of the enriched resin column 320 to flow to the waste liquid barrel 260 or the enriched liquid flowing out of the enriched resin column 320 to flow to the separation and purification unit 400 for further processing.

[0041] Furthermore, a first flow meter 370 is provided between the third injection pump 350 and the enrichment resin column 320. The volume of the concentrate flowing to the enrichment resin column 320 can be monitored by the first flow meter 370 to achieve quantitative collection of the concentrate. A second flow meter 380 is provided between the first three-way valve 340 and the second injection pump 330 to quantitatively collect the treated liquid of the liquid storage unit 200. Here, there is no restriction on the types of the first flow meter 370 and the second flow meter 380. For example, the first flow meter 370 and the second flow meter 380 can be mass flow meters or volume flow meters. In this embodiment, the first flow meter 370 and the second flow meter 380 are selected as mass flow meters.

[0042] In this embodiment, the enrichment process of the interfering ions in the concentrated solution 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, and the treatment liquid in the first liquid storage bottle 210 is transported to the enrichment resin column 320 to pre-treat the enrichment resin column 320, and the waste liquid generated by the pre-treatment is discharged into the waste liquid barrel 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 box 310 communicate with the liquid storage unit 200, the valve on the second liquid storage bottle 220 is opened, and the treatment liquid in the second liquid storage bottle 220 is transported to the water sample storage box 310 by the second injection pump 330 to pre-treat the concentrated solution to obtain the pre-treated solution. The valve on the second liquid storage bottle 220 is closed, the second injection pump 330 is closed, the third injection pump 350 is started, the pre-treated liquid in the water sample storage box 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 barrel 260. The third injection pump 350 is closed, 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, and the treated liquid in the second liquid storage bottle 220 is transported to the enrichment resin column 320 through the second injection pump 330 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 this embodiment, the treated liquid in the second liquid storage bottle 220 can adjust the pH of the concentrated liquid in the water sample storage box 310, which is conducive to better enrichment of the interfering metal ions in the concentrated liquid on the enrichment resin column 320. Exemplarily, the pH of the concentrated solution is adjusted to 1 to 2 using the treatment solution in the second liquid storage bottle 220. Exemplarily, the treatment solution in the first liquid storage bottle 210 is a 0.1 mol / L nitric acid solution, and the treatment solution in the second liquid storage bottle 220 is an 8 mol / L nitric acid solution.

[0043] See also Figure 1Since strontium-90 easily decays into yttrium-90, the content of strontium-90 is characterized by the content of yttrium-90. In one embodiment, a fourth injection pump 410 is provided on the pipeline between the separation and purification unit 400 and the liquid storage unit 200, and a fourth water pumping port 411 and a fourth water discharge port 412 are provided on the fourth injection pump 410. The fourth water pumping port 411 is connected to the liquid storage unit 200, and the fourth water discharge port 412 is connected to 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 special effect resin column 430 for adsorbing yttrium ions, and a strontium special effect resin column 440 for adsorbing strontium ions. The anion resin column 420 is provided with a second inlet 421 and a second outlet 422, the yttrium special effect resin column 430 is provided with a third inlet 431 and a third outlet 432, and the strontium special effect resin column 440 is provided with a fourth inlet 441 and a fourth outlet 442. In this embodiment, the second inlet 421 is connected to the first outlet 322, the third inlet 431 is connected to the second outlet 422, the fourth inlet 441 is connected to the third outlet 432, and the fourth outlet 442 is connected to the waste liquid barrel 260, or the second inlet 421, the third inlet 431 and the fourth inlet 441 are respectively connected to 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. By adjusting the second three-way valve 450, the liquid storage unit 200 can be connected with the anion resin column 420 or the liquid storage unit 200 can be connected 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 controlled to be connected with the third flow inlet 431 or the second flow outlet 422 can be controlled to be connected with the waste liquid barrel 260. By adjusting the fourth three-way valve 470, the third flow outlet 432 can be controlled to be connected with the fourth flow inlet 441 or the third flow outlet 432 can be controlled to be connected with the waste liquid barrel 260. By adjusting the fifth three-way valve 480, the fourth flow outlet 442 can be controlled to be connected with the waste liquid barrel 260 or the fourth flow outlet 442 can be controlled to be connected with the sample preparation unit 500. In order to simplify the pipeline, in this embodiment, the pipelines connecting the yttrium special effect resin column 430 and the strontium special effect resin column 440 with the sample preparation unit 500 and the pipelines connecting the yttrium special effect resin column 430 and the strontium special effect resin column 440 with the waste liquid barrel 260 are integrated, and a second switching valve 490 is provided on the integrated pipeline, and the flow direction of the liquid in the pipeline is adjusted by the second switching valve 490 to achieve the liquid flowing out of the resin column to flow into the sample preparation unit 500 or the waste liquid barrel 260. In this embodiment, the fourth injection pump 410 is provided on a side close to the liquid storage unit 200, and a third flow meter 390 is also provided between the fourth injection pump 410 and the first switching 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 here, 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, pre-treat the anion resin column 420, the yttrium special effect resin column 430, and the strontium special effect resin column 440. The specific operation is as follows: start the fourth injection pump 410, adjust the second three-way valve 450 so that the second inlet 421 is connected to the liquid storage unit 200, adjust the third three-way valve 460 so that the second outlet 422 is connected to the waste liquid bucket 260, open the valve on the third liquid storage bottle 230, use the treatment liquid in the third liquid storage bottle 230 to pre-treat 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 inlet 431 and the fourth three-way valve 460 are connected. The inlet 441 is connected to the liquid storage unit 200, the fourth three-way valve 470 is adjusted to make the third outflow port 432 connected to the waste liquid barrel 260, the fifth three-way valve 480 is adjusted to make the fourth outflow port 442 connected to the waste liquid barrel 260, the valve on the second liquid storage bottle 220 is opened, and the yttrium special effect resin column 430 and the strontium special effect resin column 440 are pretreated with the treatment liquid in the second liquid storage bottle 220. After the pretreatment is completed, the valve on the third liquid storage bottle 230 is closed, and the operation of the fourth injection pump 410 is stopped. The third three-way valve 460, the fourth three-way valve 470 and the fifth three-way valve 480 are adjusted so that the second flow outlet 422 is connected to the third flow inlet 431, the third flow outlet 432 is connected to the fourth flow inlet 441, and the fourth flow outlet 442 is connected to the waste liquid barrel 260, and the third injection pump 350 is started. Driven by the third injection pump 350, the enriched liquid flows through the anion resin column 420, the yttrium special effect resin column 430 and the strontium special effect resin column 440 in sequence, the anion resin column 420 adsorbs interfering ions in the enriched liquid, the yttrium special effect resin column 430 adsorbs yttrium ions in the enriched liquid, and the strontium special effect resin column 440 adsorbs strontium ions in the enriched liquid, so as to achieve ion separation and purification in the enriched liquid. After the adsorption is completed, the third injection pump 350 is closed, the fourth injection pump 410 is started, and 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 special effect resin column 430 to desorb the yttrium ions adsorbed on the yttrium special effect resin column 430, and the desorbed solution is transported to the sample preparation unit 500 to be prepared as a sample to be tested; the valve on the fifth liquid storage bottle 250 is closed, and 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 special effect resin column 440 to desorb the strontium ions on the strontium special effect resin column 440, and the desorbed solution is transported to the sample preparation unit 500 to be prepared as a sample to be tested. Exemplarily, the interfering ions in the enriched solution are iron ions, the treatment solution in the fourth liquid storage bottle 240 is a 0.05 mol / L nitric acid solution, and the treatment solution in the fifth liquid storage bottle 250 is a 0.05 mol / L hydrochloric acid solution.

[0045] See also 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 connected to the third flow outlet 432, and the second sample bottle 520 is connected to the fourth flow outlet 442. Further, the sample preparation unit 500 is used for a third sample bottle 530 for retaining a sample of the yttrium desorption solution and a fourth sample bottle 540 for retaining a sample of the strontium desorption solution. A sixth three-way valve 550 is provided on the pipeline connecting the first sample bottle 510 and the yttrium special effect resin column 430. The sixth three-way valve 550 is respectively connected to the third flow outlet 432, the first sample bottle 510 and the third sample bottle 530. Through the sixth three-way valve 550, a part of the desorption solution containing yttrium can be flowed to the first sample bottle 510 to prepare a sample to be measured, and the rest of the desorption solution containing yttrium can be flowed to the third sample bottle 530 for laboratory analysis when the monitoring result is abnormal. A seventh three-way valve 560 is provided on the pipeline connecting the second sample bottle 520 and the strontium special effect resin column 440. The seventh three-way valve 560 is connected to the fourth flow outlet 442, the second sample bottle 520 and the fourth sample bottle 540 respectively. By adjusting the seventh three-way valve 560, a part of the strontium desorption liquid flows to the second sample bottle 520 to be prepared into the sample to be measured, and the remaining strontium desorption liquid flows to the fourth sample bottle 540 for laboratory analysis when the monitoring results are abnormal.

[0046] See also Figure 1 In one embodiment, the samples to be measured in the first sample bottle 510 and the third sample bottle 530 need to be further processed. A pipeline can be set separately to connect the sample preparation unit 500 with the liquid storage unit 200, or a branch can be set 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 set on the pipeline between the separation and purification unit 400 and the liquid storage unit 200, and the liquid storage unit 200 is connected to the separation and purification unit 400 or the liquid storage unit 200 is connected to the sample preparation unit 500 by adjusting the eighth three-way valve 570.

[0047] When further processing the sample to be tested, the eighth three-way valve 570 is adjusted to connect the liquid storage unit 200 with the sample preparation unit 500, and the valve on the corresponding liquid storage bottle is opened to process the sample to be tested with the treatment liquid. In this embodiment, a ninth three-way valve 580 is provided at one end of the branch connected to the sample preparation unit 500, and the ninth three-way valve 580 can be adjusted to connect the branch with the sixth three-way valve 550 and / or the seventh three-way valve 560. For example, if the same processing liquid is used to process the sample to be detected, the first sample bottle 510 and the second sample bottle 520 can be connected to the liquid 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. If different processing liquids are used to process the sample to be detected, one of the first sample bottle 510 and the second sample bottle 520 can be connected to the liquid storage bottle by adjusting the sixth three-way valve 550, the seventh three-way valve 560 and the ninth three-way valve 580. After the processing is completed, the other of the first sample bottle 510 and the second sample bottle 520 can be connected to the liquid storage bottle by adjusting the sixth three-way valve 550, the seventh three-way valve 560 and the ninth three-way valve 580.

[0048] See also Figure 2 The present invention also provides a method for separating and analyzing strontium-89 and strontium-90 using the above separation device, comprising the following steps:

[0049] S1. Concentrating metal ions in liquid effluent from a nuclear power plant to form a concentrated solution;

[0050] S2, pre-treating the concentrated solution to obtain a pre-treated solution, enriching and desorbing the metal ions in the pre-treated solution to form an enriched solution;

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

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

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

[0054] In one embodiment, the above analysis method further comprises calculating the recovery rate of the metal ions after preparing the purified solution into the sample to be measured. The calculation formula of the recovery rate is as follows:

[0055]

[0056] Wherein: R is the recovery rate, %; Q is the concentration of metal ions in the sample to be measured, mg / L; Q0 is the concentration of metal ions in the pretreatment solution, mg / L.

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

[0058]

[0059] Where: E: instrument pair 89 Sr / 90 Detection efficiency of Y, %; n s : Total sample count rate, cpm; n b : Background count rate, cpm; c0: 89 Sr / 90 Activity concentration of Y standard solution, Bq / mL; V0: 89 Sr / 90 Y: volume of standard solution, mL; λ: decay constant, 89 The decay constant of Sr is 9.52E-6min -1 , 90 The decay constant of Y is 4.56E-8min -1 ; t1: 89 Sr / 90 Y measures the intermediate moments and 89 Sr / 90 Y is the difference in the preparation time of the standard substance.

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

[0061]

[0062] Where: In liquid outflow 89 Activity concentration of Sr, Bq / L; E Sr :Instrument pair 89 Detection efficiency of Sr, %; n Sr : Total sample count rate, cpm; n Srb : Background count rate, cpm; R Sr : recovery rate of strontium ions; V: liquid effluent sample volume, L; 0.8: sample source volume conversion coefficient.

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

[0064]

[0065] Where: In liquid outflow 90 Activity concentration of Y, Bq / L; E Y :Instrument pair 90 Detection efficiency of Y, %; n Y: Total sample count rate, cpm; n Yb : Background count rate, cpm; R Y : recovery rate of yttrium ions; V: liquid effluent sample volume, L; 0.8: sample source volume conversion factor, t2: 90 Y measures the difference between the midpoint and half the total time required to complete effluent collection.

[0066] The separation device of strontium-89 and strontium-90 of the present invention integrates a concentration unit, a liquid storage unit, an enrichment unit, a separation and purification unit and a sample preparation unit, which can simplify the operation process, improve the process continuity, and concentrate the metal ions through the concentration unit, greatly reducing the time consumed by the metal ion enrichment, significantly improving the work efficiency, and the product obtained by the separation device can be directly subjected to subsequent analysis and testing, saving a lot of manpower and resource consumption. Therefore, the present invention effectively overcomes some practical problems in the prior art and has high utilization value and use significance.

[0067] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.

Claims

1. A strontium-89 and strontium-90 separation device for separating strontium-89 and strontium-90 from liquid effluent of a nuclear power plant in a container (10), characterized in that: include: A concentration unit (100), the concentration unit (100) is used to concentrate metal ions in the liquid effluent of the nuclear power plant to form a concentrated liquid; A liquid storage unit (200), used for storing a treatment liquid; An enrichment unit (300) is connected to the concentration unit (100) and the liquid storage unit (200) respectively, so as to obtain the concentrated solution and the treated solution respectively and enrich the metal ions in the concentrated solution and then desorb them to form an enriched solution; A separation and purification unit (400) is connected to the enrichment unit (300) and the liquid storage unit (200) respectively, and is used to separate and purify the enriched liquid, remove interfering ions, and obtain a purified liquid; The sample preparation unit (500) is connected to the separation and purification unit (400), obtains the purified liquid and prepares the purified liquid into a sample to be measured.

2. The device for separating strontium-89 and strontium-90 according to claim 1, characterized in that: The concentration unit (100) comprises a concentration device (110) and a first injection pump (120); 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 pumping port (121) and a first water discharge port (122); the first water inlet (111) is connected to the water outlet of the container (10); the first water outlet (112) is connected to the first water pumping port (121); and the first water discharge port (122) is connected to the enrichment unit (300).

3. The device for separating strontium-89 and strontium-90 according to claim 2, characterized in that: The enrichment unit (300) comprises a water sample storage box (310) and an enrichment resin column (320); the water sample storage box (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 injection pump (330) is provided on the pipeline between the water sample storage box (310) and the liquid storage unit (200); the second injection pump (330) is provided with a second water pumping port (331) and a second water outlet (332); the second water pumping port (331) is communicated with the liquid storage unit (200); the second water outlet (332) is communicated with the second water outlet (331); The enriched resin column (320) is provided with a first inlet (321) and a first outlet (322), the first inlet (321) is connected to the second water outlet (313) or the liquid storage unit (200), and the first outlet (322) is connected to the separation and purification unit (400); a third injection pump (350) is provided on the pipeline between the water sample storage box (310) and the enriched resin column (320), and the third injection pump (350) is provided with a third water pumping port (351) and a third water discharge port (352), the third water pumping port (351) is connected to the second water outlet (313), and the second water discharge port (332) is connected to the first inlet (321).

4. The device for separating strontium-89 and strontium-90 according to claim 3, characterized in that: A fourth injection pump (410) is arranged on the pipeline between the separation and purification unit (400) and the liquid storage unit (200); the fourth injection pump (410) is provided with a fourth water pumping port (411) and a fourth water discharge port (412); the fourth water pumping port (411) is communicated with the liquid storage unit (200); the fourth water discharge port (412) is communicated with the separation and purification unit (400); the separation and purification unit (400) comprises an anion resin column (420) for adsorbing interfering ions, a yttrium special effect resin column (430) for adsorbing yttrium ions, and a strontium special effect resin column (440) for adsorbing strontium ions; the anion resin column (420) is provided with a second inlet (421) and a second outlet (422). The yttrium special effect resin column (430) is provided with a third inlet (431) and a third outlet (432), the strontium special effect resin column (440) is provided with a fourth inlet (441) and a fourth outlet (442), the second inlet (421) is connected to the first outlet (322), the third inlet (431) is connected to the second outlet (422), the fourth inlet (441) is connected to the third outlet (432), the fourth outlet (442) is connected to a waste liquid collection device, or the second inlet (421), the third inlet (431) and the fourth inlet (441) are respectively connected to a liquid storage unit (200).

5. The device for separating strontium-89 and strontium-90 according to claim 4, characterized in that: The sample preparation unit (500) comprises a first sample bottle (510) for storing yttrium solution and a second sample bottle (520) for storing strontium solution, wherein the first sample bottle (510) is connected to the third flow outlet (432), and the second sample bottle (520) is connected to 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 in that: The steps include: Concentrating metal ions in liquid effluent from nuclear power plants to form concentrated liquid; Pre-treating the concentrated solution to obtain a pre-treated solution, and enriching the metal ions in the pre-treated solution and then desorbing the enriched solution to form an enriched solution; The enriched solution is separated and purified to remove interfering ions and obtain a purified solution; preparing the purified solution into a sample to be measured; The sample to be measured is sent to a liquid scintillation spectrometer for testing.

7. The separation and analysis method according to claim 6, characterized in that: The method further includes calculating the recovery rate of the metal ions after preparing the purified solution into a sample to be measured, wherein the recovery rate is calculated as follows: Wherein: R is the recovery rate, %; Q is the concentration of metal ions in the sample to be measured, mg / L; Q0 is the concentration of metal ions in the pretreatment solution, mg / L.

8. The separation and analysis method according to claim 6, characterized in that: When the liquid scintillation spectrometer is used for testing, 89 Sr / 90 The calculation formula of the detection efficiency of Y is as follows: Where: E: instrument pair 89 Sr / 90 Detection efficiency of Y, %; n s : Total sample count rate, cpm; n b : Background count rate, cpm; c0: 89 Sr / 90 Activity concentration of Y standard solution, Bq / mL; V0: 89 Sr / 90 Y standard solution volume, mL; λ: decay constant, 89 The decay constant of Sr is 9.52E-6min -1 , 90 The decay constant of Y is 4.56E-8min -1 ; t1: 89 Sr / 90 Y measures the intermediate moments and 89 Sr / 90 Y is the difference in the preparation time of the standard substance.

9. The separation and analysis method according to claim 7, characterized in that: When the liquid scintillation spectrometer is used for testing, 89 The calculation formula of Sr activity concentration is as follows: Where: A 89Sr :In liquid effluent 89 Activity concentration of Sr, Bq / L; E Sr :Instrument pair 89 Detection efficiency of Sr, %; n Sr : Total sample count rate, cpm; n Srb : Background count rate, cpm; R Sr : Recovery rate of strontium ions; V: liquid effluent sample volume, L; 0.8: sample source volume conversion factor.

10. The separation and analysis method according to claim 7, characterized in that: When the liquid scintillation spectrometer is used for testing, 90 The calculation formula of Sr activity concentration is as follows: Where: In liquid outflow 90 Activity concentration of Y, Bq / L; E Y :Instrument pair 90 Detection efficiency of Y, %; n Y : Total sample count rate, cpm; n Yb : Background count rate, cpm; R Y : Recovery rate of yttrium ions; V: liquid effluent sample volume, L; 0.8: sample source volume conversion factor, t2: 90 Y measures the difference between the midpoint and half the total time required to complete effluent collection.

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