A sort of 210 Po generator and its application
Through the decay chain and solid phase chromatography separation technology of 210Pb-210Bi-210Po, the problem of difficulty in obtaining and preserving 210Po is solved, and long-term and stable acquisition of high-core purity 210Po standard solution is achieved, improving the use cycle and safety of radioactive standard solution.
Patent Information
- Application Number
- CN202411949764.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-04-01
AI Technical Summary
The prior art is difficult to achieve convenient and low-cost acquisition of 210Po nuclides, and due to its short half-life, it is difficult to maintain and supply stably for a long time.
The decay chain of 210Pb-210Bi-210Po was used to load the 210Pb solution by loading the chromatographic column loaded with solid-phase adsorption material. The 210Po sub-body was separated and recovered by solid-phase chromatography separation technology. Combined with the principle of decay balance, the 210Po standard solution with high nuclear purity was achieved in a long-term and stable manner.
It has achieved long-term, stable and convenient acquisition of 210Po standard solution with high nuclear purity, overcomes the storage and supply difficulties caused by short half-life, and improves the use cycle and safety of radioactive standard solutions.
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Figure CN119733375A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of isotope separation and specifically relates to a 210 Po generator and its applications. Background Art
[0002] A radionuclide generator is a device that separates short half-life nuclides (called daughter nuclides) from long half-life nuclides (called parent nuclides). During its effective life, a radionuclide generator can separate daughter nuclides from the parent nuclides once at appropriate time intervals, just like milking a cow, so a radionuclide generator is also called a "cow."
[0003] CN114999701A discloses a strontium [ 90 Sr]-yttrium[ 90 Y] generator and separation method, [ 90 Sr]-yttrium[ 90 The generator comprises a first chromatographic column, a liquid storage tank and a second chromatographic column. 90 Sr]-yttrium[ 90 Y] Separation methods include: 90 Sr stock solution was pretreated to obtain strontium nitrate [ 90 Sr] solution; strontium nitrate [ 90 Sr] solution is loaded into the first chromatographic column; hydrochloric acid is used as eluent and eluent to elute and wash the first chromatographic column, and the primary eluent enters the reservoir; counter-carrier solution is mixed: the counter-carrier solution is added to the reservoir and mixed with the primary eluent as a mixed eluent; the mixed eluent flows through the unloaded strontium nitrate [ 90 Sr] solution, prepared to obtain 90 The present invention is simple and fast to operate, has high separation efficiency, and can produce high nuclear purity medical 90 Y nuclide.
[0004] Commonly used generators in medicine include: Mo-Tc generator, W-Re generator, Sr-Rb generator, Rb-Kr generator, etc. However, there is no convenient and low-cost 210 How to obtain Po.
[0005] 210 As a pure α nuclide, Po has very wide and important applications in radiometric measurement, environmental radioactivity monitoring, research and development and calibration of α spectrometers and low-background αβ detectors. 210 The half-life of Po is only 138.376 days. The radioactive standard solution of this nuclide and the radioactive reference source prepared by using the standard solution have a short service life and are difficult to preserve. 210The cow generator of Po solution is a technical problem that needs to be solved urgently. Summary of the invention
[0006] In view of the shortcomings of the prior art, the present invention aims to provide a 210 Po generator and its application. 210 The separation method of Po can achieve a long-term, stable and convenient acquisition 210 Po standard solution overcomes the problem that it cannot be used and supplied stably in the laboratory for a long time due to its short half-life and difficulty in preservation.
[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:
[0008] In a first aspect, the present invention provides a 210 Po generator, the generator adopts 210 Pb- 210 Bi- 210 The decay chain of Po is 210 Pb is produced by the mother nucleus 210 Po solution;
[0009] The generator comprises: a chromatographic column loaded with a solid phase adsorption material; 210 Pb solution, the 210 The Pb solution contains the precursor 210 Pb, and 210 Bihe 210 Po two daughters;
[0010] The solid phase adsorption material is a resin with a macroporous silica substrate as a skeleton, the porosity of the macroporous silica substrate is ≥0.8mL / g, the pore size is ≥500nm, and the particle size of the resin particles is 50-130μm; the solid phase adsorption material is selected from: any one of cation exchange resin, anion exchange resin or crown ether solid phase extraction resin or a combination of at least two of them.
[0011] One of the characteristics of the present invention is that 210 Pb is adsorbed from the solution into the chromatographic column, thus avoiding the need to store the solution. Solid phase storage is relatively safer and more convenient to use. 210 The Pb parent core solution can be subjected to the complete chromatographic separation process again after decay equilibrium, which is cumbersome to operate and requires higher safety.
[0012] The second feature of the present invention is that it is necessary to realize 210 Pb, 210 Bi, 210 Based on the separation of Po, only the elution210 Po and at the same time can better retain 210 Pb and 210 Bi is in the chromatographic column; if it is only for separation, there are many methods, such as using anion exchange resin, which can be eluted first 210 Pb and 210 Bi, recovered by post-elution 210 Po, but cannot 210 Pb, 210 Bi is retained in the chromatographic column to wait for a new decay equilibrium before separation 210 The purpose of Po. In other words, the order of elution in the separation process should be ensured to be 210 Po and then 210 Pb and 210 Bi.
[0013] The present invention adopts solid phase chromatography separation technology, selects suitable solid phase adsorption materials to be loaded into the chromatographic column, and uses the daughter body balance 210 Pb solution is used as the matrix. 210 Po daughter, get high nuclear purity 210 Po standard solution; at the same time, the parent nuclide 210 Pb and daughter 210 Bi will remain in the column. Seal the column for about 3-4 210 After the half-life of Po, 210 Pb and 210 Bi nuclides will reach decay equilibrium again, thus enriching the target nuclides. 210 Po. Once again 210 Po is eluted to obtain a high purity nuclear 210 Po standard solution. Packed by time segment 210 Pb in column and batch elution 210 Po standard solution can be obtained long-term, stable, conveniently and on-demand. 210 Po nuclide standard solution.
[0014] In the present invention 210 The Pb decay chain is shown below, consisting of 210 Bihe 210 Po two daughter bodies.
[0015]
[0016] In the present invention, the solid phase adsorption material selected is 210 Pb, 210 Po has good adsorption and separation performance.
[0017] Preferably, the matrix210 Pb and daughter 210 Bi, 210 The solution in which Po reaches decay equilibrium is used as the generator solution; at equilibrium, the parent 210 Pb and daughter 210 Bi, 210 The radioactivity values of Po are equal.
[0018] In the present invention, the 210 Pb- 210 Bi- 210 Po is used as a decay chain, and the matrix is stored for a certain period of time. 210 Pb and daughter 210 Bi, 210 The solution in which Po reaches decay equilibrium is used as the solution used by the generator. 210 Pb solution matrix 210 The amount of Pb can range from 1 kBq to Curie (Ci) activity level. 210 Pb. 210 The Pb solution is stored until the daughter phase is in equilibrium before being used for separation production 210 Po, and in equilibrium the solution 210 Pb and daughter 210 Bi, 210 The radioactivity values of Po are equal.
[0019] Preferably, the cation exchange resin is selected from: sulfonic acid type, carboxylic acid type or organic-inorganic composite resin.
[0020] Preferably, the anion exchange resin is selected from any one of a linear quaternary ammonium salt type strongly basic anion exchange resin, a tertiary ammonium type weakly basic anion exchange resin, a strongly basic silicon-based pyridine anion exchange resin or an organic-inorganic composite anion exchange resin.
[0021] In the present invention, the anion exchange resin is a strongly alkaline silicon-based pyridine anion exchange resin, a macroporous silica skeleton, and a pyridine quaternary ammonium salt as a functional group. The particle size of the resin particles is 50-130 μm, for example, it can be 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, 110 μm, 120 μm or 130 μm, etc., the porosity is ≥0.8 mL / g, for example, it can be 0.8 mL / g, 0.9 mL / g or 1 mL / g, etc., and the pore size is ≥500 nm, for example, it can be 500 nm, 550 nm or 600 nm, etc.
[0022] Preferably, the crown ether solid phase extraction resin is selected from: Silica-P-18-crown ether-6 solid phase extraction resin or organic / inorganic skeleton-18-crown ether-6 composite solid phase extraction resin.
[0023] Among them, 18-crown ether-6 is an organic compound with the chemical formula C 12 H 24 O6.
[0024] In the present invention, the organic / inorganic framework-18-crown ether-6 composite solid phase extraction resin can use zeolite as a crown ether-supported substrate. The optional commercial resins in the present invention also include Sr resin and Pb resin.
[0025] Preferably, the chromatographic column is a chromatographic column of φ5-12mm*40-600mm.
[0026] Among them, 5-12mm can be, for example, 5mm, 8mm, 10mm or 12mm, etc.; 40-600mm can be, for example, 40mm, 100mm, 200mm, 300mm, 400mm, 500mm or 600mm, etc.
[0027] As a specific implementation of the present invention, a chromatographic column of φ8mm*50mm is used; on this basis, the chromatographic column can be lengthened to be more beneficial to the separation and elution effect; theoretically, the longer and thinner the chromatographic column is, the better the separation effect will be, and the above range can be appropriately set accordingly.
[0028] Preferably, the 210 The solvent of the Pb solution is selected from any one of a hydrochloric acid solution, a nitric acid solution or a sulfuric acid solution.
[0029] Preferably, the solvent also contains an organic phase.
[0030] Preferably, the organic phase is ethanol.
[0031] In the present invention, the solvent may also be nitric acid, sulfuric acid or a mixed system with an organic phase such as ethanol added. When different solvents are used, different optimal separation and recovery schemes for the parent nucleus and daughter bodies are obtained.
[0032] In a second aspect, the present invention provides a 210 A method for separating Po, the separation method comprising the following steps:
[0033] Will 210 The Pb solution was loaded into the chromatographic column loaded with solid phase adsorption material, and nitric acid solution was used as the eluent. 210 Po is eluted from the column;
[0034] Seal the column for 3-4 210 The half-life of Po in the column 210 Pb and 210 Bi nuclides will reach decay equilibrium again, thus enriching the target nuclides. 210 Po; then use nitric acid solution as eluent210 Po is eluted from the column; repeated sealing and elution steps can continuously obtain 210 Po nuclide standard solution.
[0035] Preferably, the 210 The Pb solution contains the precursor 210 Pb, and 210 Bihe 210 Po two daughter bodies; the mother body 210 Pb and daughter 210 Bi, 210 The solution in which Po reaches decay equilibrium is used as the generator solution; at equilibrium, the parent 210 Pb and daughter 210 Bi, 210 The radioactivity values of Po are equal.
[0036] Preferably, the 210 The loading amount of the Pb solution is 0.01-1 column volume, for example, it can be 0.01, 0.1, 0.2, 0.4, 0.6, 0.8 or 1, etc.
[0037] In the present invention, the 210 The concentration of the Pb solution is between 200 kBq and 1 MBq. 210 The less the amount of Pb mother liquor, the better. 210 The more concentrated the Pb concentration is, the better, and it generally does not exceed 1 column volume. For elution separation, the smaller the sample volume, the better the subsequent elution effect; when 210 When the concentration of the Pb mother solution is relatively high, the amount of the mother solution loaded will be very small. For example, for a 10mL column, the loading amount is 1mL or 2mL.
[0038] Preferably, the loading temperature is 25-45°C, for example, 25°C, 30°C, 35°C, 40°C or 45°C.
[0039] In the present invention, the sample loading temperature is controlled to be 25-45°C, which is more conducive to the process rate of ion exchange. Too low a temperature will slow down the ion exchange process and affect the adsorption capacity at the ion exchange equilibrium, which is not conducive to the process. 210 Pb, 210 Bi, 210 For the separation of Po, too high temperature will affect the adsorption capacity at ion exchange equilibrium and increase the column pressure.
[0040] Preferably, the sample loading flow rate is 0.5-2 mL / min, for example, 0.5 mL / min, 1 mL / min, 1.5 mL / min or 2 mL / min.
[0041] Preferably, the concentration of the nitric acid solution is 0.15-3 mol / L, for example, it can be 0.15 mol / L, 1 mol / L, 2 mol / L or 3 mol / L.
[0042] In the present invention, for the cation exchange resin, the nitric acid concentration is preferably 0.15-0.2 mol / L, for example, 0.15 mol / L, 0.18 mol / L or 0.2 mol / L.
[0043] In the present invention, for the anion resin, the nitric acid concentration is preferably 0.5-2 mol / L, for example, 0.5 mol / L, 1 mol / L or 2 mol / L.
[0044] In the present invention, for the crown ether resin, the nitric acid concentration is preferably 2-3 mol / L, for example, 2 mol / L, 2.5 mol / L or 3 mol / L.
[0045] In the present invention, the flow rate will vary according to the size of the chromatographic column. Secondly, in theory, a slow flow rate will be conducive to the realization of separation, but the efficiency is low; a fast flow rate is conducive to improving the separation efficiency, but the separation effect will deteriorate; comprehensive consideration is required.
[0046] In the present invention, the amount of the eluent used is about 10 mL of solution under the best experimental conditions using a cation exchange resin. 210 The recycling of Po will 210 Pb and 210 Bi is better retained in the chromatographic column.
[0047] Preferably, the elution temperature is 32-37°C, for example, 32°C, 35°C or 37°C.
[0048] Preferably, the flow rate of the elution is 0.1-2 mL / min, for example, 0.1 mL / min, 0.5 mL / min, 1 mL / min or 2 mL / min.
[0049] In the present invention, the flow rate of the cation exchange resin is 0.1-2 mL / min, for example, it can be 0.1 mL / min, 0.5 mL / min, 1 mL / min or 2 mL / min.
[0050] In the present invention, the flow rate of the anion exchange resin is 0.1-2 mL / min, for example, it can be 0.1 mL / min, 0.5 mL / min, 1 mL / min or 2 mL / min.
[0051] In the present invention, the flow rate of the crown ether solid phase extraction resin is 0.1-0.5 mL / min, for example, it can be 0.1 mL / min, 0.2 mL / min, 0.3 mL / min, 0.4 mL / min or 0.5 mL / min.
[0052] In the present invention, the efficiency and separation effect are taken into consideration by controlling the flow rate of elution. In theory, a slow flow rate is conducive to the separation, but the efficiency is low; a fast flow rate will deteriorate the separation effect.
[0053] In a third aspect, the present invention provides the 210 Po generator and / or the second aspect 210 The separation method of Po is used in the preparation 210 Application of Po nuclide.
[0054] The numerical range described in the present invention not only includes the point values listed above, but also includes any point values between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values included in the range.
[0055] Compared with the prior art, the present invention has the following beneficial effects:
[0056] The method of the present invention can achieve long-term, stable, convenient and on-demand acquisition of 210 Po nuclide standard solution.
[0057] (1) 210 The Pb parent nucleus is solidified from the solution into the inside of the adsorption chromatographic column and preserved in the form of a solid phase, which improves safety from the perspective of radioactive safety management.
[0058] (2) 210 Pb, 210 Bi, 210 There are many technical means to separate Po, but first elution 210 Po, and you can 210 Pb and 210 Bi is completely retained in the chromatographic column, so that the cow generating device designed in the present invention can be realized. Therefore, specific requirements are put forward for the adsorbent, elution sequence, elution rate and efficiency.
[0059] (3) When the parent core is retained in the chromatographic column 210 Pb and its daughter 210 Bihe 210 After Po reaches decay equilibrium again, it can be 210 Po is washed again to achieve 210 Po solution is long-term, stable and convenient to use, fundamentally improving the short half-life 210The objective situation that Po solution is not easy to store and use.
[0060] (4) The washing method of the present invention 210 The Po solution core is extremely pure and has no 210 Bihe 210 The leakage of Pb is 210 Po provides very important guarantees for the quality and technical parameters of the standard solutions and radioactive reference sources prepared subsequently. BRIEF DESCRIPTION OF THE DRAWINGS
[0061] Figure 1 yes 210 Schematic diagram of the Po solution cow generator principle.
[0062] Figure 2 yes 210 The first elution curve of Pb mother liquor.
[0063] Figure 3 yes 210 Po secondary elution curve. DETAILED DESCRIPTION
[0064] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.
[0065] If no specific techniques or conditions are specified in the examples, the techniques or conditions described in the literature in the field or the product instructions are used. If no manufacturer is specified for the reagents or instruments used, they are all conventional products that can be purchased through regular channels.
[0066] Example 1
[0067] This embodiment provides a 210 A method for separating Po, the method comprising:
[0068] (1) A double-layer glass chromatographic column of φ8 mm × 50 mm was used, the temperature was controlled at 30° C., and the chromatographic column was fully loaded with a sulfonic acid type macroporous cation exchange resin, wherein the resin had a macroporous silica substrate as a skeleton, the porosity of the macroporous silica substrate was 1 mL / g, the pore size was 600 nm, and the average particle size of the resin particles was 75 μm.
[0069] (2) Use 0.2 mol / L nitric acid solution to rinse the chromatographic column from top to bottom at a flow rate of 2 mL / min.
[0070] (3) Take 5 mL of 210Pb mother solution, in which Pb and its daughters reach decay equilibrium, the radioactivity values of Pb, Bi and Po are all 500kBq, and the acid concentration of the solution is adjusted by dilution with 0.2mol / L nitric acid solution.
[0071] (4) At a flow rate of 2 mL / min, 210 The Pb mother liquor passes through the chromatographic column.
[0072] (5) Following step (4), a total of 30 mL of 0.2 mol / L nitric acid solution was used to elute the chromatographic column from top to bottom at a rate of 2 mL / min. After elution, the chromatographic column was sealed; the obtained eluent was tested and confirmed to contain only high specific activity 210 Po, not seen 210 Pb, 210 Bi and other nuclides have been successfully obtained with high nuclear purity 210 Po solution.
[0073] (6) After the chromatographic column was sealed for about 2 years, the Pb and its daughter Bi and Po in the chromatographic column basically reached radioactive decay equilibrium again; a total of 30 mL of 0.2 mol / L nitric acid solution was used to elute the chromatographic column from top to bottom at a flow rate of 2 mL / min. After elution, the chromatographic column was sealed; the obtained eluent was tested and confirmed to contain only high specific activity 210 Po, not seen 210 Pb, 210 Bi and other nuclides have been successfully obtained with high nuclear purity 210 Po solution.
[0074] (7) After the column is sealed again for 2 years, it can be rinsed and used again. 210 Po nuclide.
[0075] (8) According to steps (1)-(4), prepare 8-10 adsorbed 210 The chromatographic column of the Pb mother liquor can be sequentially eluted at intervals of about 100 days to obtain the 210 Po nuclide, thus stably and continuously obtaining high-quality 210 Po nuclide.
[0076] Example 2
[0077] This embodiment provides a 210 The method for separating Po is different from that in Example 1 in that a 0.1 mol / L nitric acid solution is used as an eluent. 210 Po is eluted from the column.
[0078] The same elution sequence and solution volume, 210The elution efficiency of Po is poor. Using a 0.2 mol / L solution, high specific activity ions can be concentrated in a volume of 5-15 mL of eluent. 210 Po solution. However, when 0.1mol / L elution is used, until the 30mL volume of eluent has completely passed through the chromatographic column, 210 The recovery of Po was about 45% of the expected activity.
[0079] Example 3
[0080] This embodiment provides a 210 The method for separating Po is different from that in Example 1 in that a 0.3 mol / L nitric acid solution is used as an eluent. 210 Po is eluted from the column.
[0081] Using 0.3 mol / L nitric acid for elution, high specific activity can be recovered in 5-10 mL volume of eluent. 210 Po solution, but in the eluent after 10mL volume, there will be 210 Pb, 210 Bi leaks out of the column.
[0082] Example 4
[0083] This embodiment provides a 210 The separation method of Po is different from that of Example 1 in that the elution temperature is 32° C. The elution result is not significantly different from that of Example 1.
[0084] Example 5
[0085] This embodiment provides a 210 The separation method of Po is different from that of Example 1 in that the elution temperature is 37° C. The column pressure is increased from <0.01 MPa to about 0.025 MPa, and the other experimental phenomena are not significantly different from those of Example 1.
[0086] Example 6
[0087] This embodiment provides a 210 A method for separating Po, wherein the method is different from that in Example 1 in that the elution temperature is 10°C.
[0088] Appears in 0-10mL eluent volume 210 The elution of Po indicates that the ion exchange rate and adsorption capacity decrease after the temperature decreases. 210 Po will be more difficult to be adsorbed by the column and more easily eluted. At the same time, a small amount of Po will appear in the eluent with a volume of about 25-30 mL. 210The phenomenon of Bi being eluted is also caused by the fact that the adsorption capacity and efficiency of the adsorbent decrease as the temperature decreases.
[0089] Example 7
[0090] This embodiment provides a 210 A method for separating Po, wherein the method is different from that in Example 1 in that the elution temperature is 45°C.
[0091] As the temperature rises, the ion exchange rate increases, and the metal ions are adsorbed faster and closer to the column inlet, resulting in a decrease in the elution rate. 210 Po was eluted out of the chromatographic column, and the overall recovery was slightly lower than the theoretical activity value, which was worse than that in Example 1, about 95%, and the volume of the eluent used was doubled.
[0092] Example 8
[0093] This embodiment provides a 210 The separation method of Po is different from that of Example 1 in that the flow rate of elution is 1 mL / min.
[0094] There was no significant change in the experimental phenomenon. In the eluent volume of 10-20mL 210 Po was eluted out in a concentrated manner, and the total elution time required for the same volume of eluent doubled. The efficiency of elution separation and recovery was slightly reduced, but still within an acceptable range.
[0095] Example 9
[0096] This embodiment provides a 210 The separation method of Po is different from that of Example 1 in that the flow rate of elution is 3 mL / min.
[0097] In 0-10mL volume of eluent 210 Po was concentrated and eluted, but the column pressure increased slightly, and a small amount of 210 Bi leakage, although not related to 210 Po is mixed, but reduced 210 The risk of Po core purity and the leakage of the mother core will affect the subsequent secondary elution. 210 Po's yield is unfavorable.
[0098] Example 10
[0099] This embodiment provides a 210 The separation method of Po is different from that of Example 1 in that the flow rate of elution is 0.05 mL / min.
[0100] In a volume of 20-30 mL of eluent 210 Po is concentrated and washed out. 210 The specific activity of Po decreases, and the elution efficiency decreases. In addition, the same volume of eluent takes too long to pass through the chromatographic column, and the overall solution processing efficiency is too low, which is not conducive to large-scale application and promotion.
[0101] Embodiment 11
[0102] This embodiment provides a 210 The separation method of Po is different from that of Example 1 in that the flow rate of elution is 5 mL / min.
[0103] The column pressure increased significantly to about 0.035MPa; the eluent volume of 0-15mL 210 Po was concentrated and eluted, but appeared in the 20-25 mL volume of eluent. 210 Bi leakage, also occurs in 25-30mL eluent volume 210 Pb leakage. Too fast elution flow rate is very detrimental to separation.
[0104] Example 12
[0105] This embodiment provides a 210 Po generator, the generator adopts 210 Pb- 210 Bi- 210 The decay chain of Po is 210 Pb is produced by the mother nucleus 210 Po solution; the generator comprises: a chromatographic column loaded with a solid phase adsorption material; the chromatographic column is loaded with 210 Pb solution, the 210 The Pb solution contains the precursor 210 Pb, and 210 Bihe 210 Po two daughter bodies; the solid phase adsorption material is a macroporous silicon-based composite sulfonic acid type cation exchange resin, specifically, the resin particles are about 75μm, the porosity is as high as 1mL / g, and the pore size is 600nm.
[0106] The mother 210 Pb and daughter 210 Bi, 210 The solution in which Po reaches decay equilibrium is used as the generator solution; at equilibrium, the parent 210 Pb and daughter 210 Bi, 210 The radioactivity values of Po are equal. The chromatographic column is a chromatographic column of φ8mm*50mm.
[0107] Comparative Example 1
[0108] This comparative example provides a 210 The Po generator is different from Example 12 in that the solid phase adsorption material is a common commercial macroporous sulfonic acid type cation exchange resin, specifically AG50W, with a porosity of 0.1 mL / g and a pore size of 30-40 nm.
[0109] A lower flow rate of about 0.1 mL / min is required for elution, otherwise it cannot be achieved. 210 Po, 210 Bihe 210 Successful separation of Pb; very low efficiency and easy to appear in the secondary elution 210 Bihe 210 Pb leakage can no longer be carried out for secondary and subsequent 210 Separation and recovery of Po.
[0110] Embodiment 13
[0111] This embodiment provides a 210 The Po generator is different from Example 12 in that the solid phase adsorption material is an anion exchange resin, which is a strongly alkaline silicon-based pyridine anion exchange resin with a macroporous silica skeleton and pyridine quaternary ammonium salt as a functional group. The resin particles are 75 μm, the porosity is as high as 1 mL / g, and the pore size is 600 nm.
[0112] The elution flow rate was 2 mL / min, and 0.5 mol / L nitric acid was used for elution. 210 Po, followed by a period of sealing and secondary elution, can achieve high efficiency separation and recovery 210 Po.
[0113] Comparative Example 2
[0114] This comparative example provides a 210 The Po generator is different from Example 12 in that the solid phase adsorption material is an anion exchange resin, specifically Amberlite IRA900.
[0115] To achieve 210 Po, 210 Bi, 210 For the separation of Pb, a lower flow rate of about 0.2 mol / L is required. The main reason is that commercial resins such as Amberlite IRA900 have low porosity and small pore size (porosity is generally 0.05-0.15 mL / g, pore size is generally 20-50 nm), which leads to a decrease in ion exchange rate, thus putting forward higher requirements on the flow rate. Otherwise, it will cause 210 Bi or210 Pb leakage affects the separation effect and subsequent multiple elutions 210 Po has an impact.
[0116] Embodiment 14
[0117] This embodiment provides a 210 Po generator, which differs from Example 12 in that the solid phase adsorption material is a crown ether solid phase extraction resin, specifically a macroporous Silica-P-crown ether adsorption resin (using silica particles with a particle size of 75 μm and a pore size of 600 nm as a substrate, using styrene and divinylbenzene to form a copolymer in the gap and then loading 18-crown ether-6).
[0118] Use 2 mol / L nitric acid for elution 210 Po, if necessary, a higher concentration of nitric acid can be used for elution 210 Po, but it is not recommended to use nitric acid above 4 mol / L, otherwise it will easily cause 210 Bihe 210 Pb leakage. Eluent at a flow rate of 2-3 mL / min can achieve 210 Po and 210 Bi, 210 Highly efficient separation of Pb 210 The recovery rate of Po is >95%.
[0119] Comparative Example 3
[0120] This comparative example provides a 210 The Po generator is different from Example 12 in that the solid phase adsorption material is a crown ether solid phase extraction resin, specifically a polystyrene-divinylbenzene microsphere-supported crown ether solid phase extraction resin. This type of crown ether resin has a low porosity and pore size (porosity of about 0.1 mL / g and pore size of about 30 nm) because the substrate is polystyrene-divinylbenzene microspheres, which leads to a low adsorption rate during adsorption and elution. Therefore, the flow rate during the elution process needs to be strictly controlled and is generally not greater than 0.2 mL / min. 2 mol / L nitric acid is used for elution recovery 210 Po, generally concentrated in 10-25mL eluent volume 210 Po, the specific activity is lower than that of Example 14, and the overall elution efficiency is also significantly lower than that of the ion exchange method. The elution efficiency is lower than that of the generator of cation exchange resin. Compared with the use of polystyrene-divinylbenzene microspheres, the effect of crown ether resin using Silica-P substrate is better.
[0121] The applicant declares that the above is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention shall fall within the protection scope and disclosure scope of the present invention.
Claims
1. A 210 The Po generator is characterized in that The generator uses 210 Pb- 210 Bi- 210 The decay chain of Po is 210 Pb is produced by the mother nucleus 210 Po solution; The generator comprises: a chromatographic column loaded with a solid phase adsorption material; 210 Pb solution, the 210 The Pb solution contains the precursor 210 Pb, and 210 Bihe 210 Po two daughters; The solid phase adsorption material is a resin with a macroporous silica substrate as a skeleton, the porosity of the macroporous silica substrate is ≥0.8mL / g, the pore size is ≥500nm, and the particle size of the resin particles is 50-130μm; the solid phase adsorption material is selected from: any one of cation exchange resin, anion exchange resin or crown ether solid phase extraction resin or a combination of at least two of them.
2. according to claim 1 210 The Po generator is characterized in that The mother 210 Pb and daughter 210 Bi, 210 The solution in which Po reaches decay equilibrium is used as the generator solution; at equilibrium, the parent 210 Pb and daughter 210 Bi, 210 The radioactivity values of Po are equal.
3. The method according to claim 1 or 2 210 The Po generator is characterized in that The cation exchange resin is selected from: sulfonic acid type, carboxylic acid type, organic-inorganic composite resin; Preferably, the anion exchange resin is selected from any one of a linear quaternary ammonium salt type strongly basic anion exchange resin, a tertiary ammonium type weakly basic anion exchange resin, a strongly basic silicon-based pyridine type anion exchange resin or an organic-inorganic composite anion exchange resin; Preferably, the crown ether solid phase extraction resin is selected from: Silica-P-18-crown ether-6 solid phase extraction resin, organic / inorganic skeleton-18-crown ether-6 composite solid phase extraction resin.
4. According to any one of claims 1-3 210 The Po generator is characterized in that The chromatographic column is a chromatographic column of φ5-12mm*40-600mm.
5. According to any one of claims 1-4 210 The Po generator is characterized in that Said 210 The solvent of the Pb solution is selected from any one of a hydrochloric acid solution, a nitric acid solution or a sulfuric acid solution; Preferably, the solvent further contains an organic phase; Preferably, the organic phase is ethanol.
6. A 210 A method for separating Po, characterized in that: The separation method comprises the following steps: Will 210 The Pb solution was loaded into the chromatographic column loaded with solid phase adsorption material, and nitric acid solution was used as the eluent. 210 Po is eluted from the column; Seal the column for 3-4 210 The half-life of Po in the column 210 Pb and 210 Bi nuclides will reach decay equilibrium again, thus enriching the target nuclides. 210 Po; then use nitric acid solution as eluent 210 Po is eluted from the column; repeated sealing and elution steps can continuously obtain 210 Po nuclide standard solution.
7. According to claim 6 210 A method for separating Po, characterized in that: Said 210 The Pb solution contains the precursor 210 Pb, and 210 Bihe 210 Po two daughter bodies; the mother body 210 Pb and daughter 210 Bi, 210 The solution in which Po reaches decay equilibrium is used as the generator solution; at equilibrium, the parent 210 Pb and daughter 210 Bi, 210 The radioactivity values of Po are equal.
8. The method according to claim 6 or 7 210 A method for separating Po, characterized in that: Said 210 The loading amount of Pb solution was 0.01-1 column volume; Preferably, the loading temperature is 25-45°C; Preferably, the flow rate of the loading is 0.5-2 mL / min.
9. The method according to any one of claims 6 to 8 210 A method for separating Po, characterized in that: The concentration of the nitric acid solution is 0.15-3 mol / L; Preferably, the elution temperature is 32-37°C; Preferably, the flow rate of the elution is 0.1-2 mL / min.
10. The method according to any one of claims 1 to 5 210 Po generator and / or any one of claims 6-9 210 The separation method of Po is used in the preparation 210 Application of Po nuclide.