A method for preparing a gallium phosphate target material and 68 A method for preparing Ge

Abstract

The application relates to the technical field of medical treatment, and particularly discloses a preparation method of a gallium phosphate target material and a gallium phosphate target material prepared by using the same 68 The application relates to a preparation method of a gallium phosphate target material. 68 The application relates to a preparation method of a gallium phosphate target material. 68 The application relates to a preparation method of a gallium phosphate target material. The preparation method of the gallium phosphate target material comprises the following steps: S1, placing gallium phosphate powder into a target material mold and sintering, so that the gallium phosphate powder forms a gallium phosphate crystal; and S2, placing the gallium phosphate crystal into a metal tank for packaging, so as to obtain the gallium phosphate target material. In the application, the gallium phosphate is used as an irradiation target material, so that the target material has a high melting point and high thermal stability, can be applied to a high-beam accelerator, is more suitable for commercial scale production, can avoid using copper / silver as a target material base, avoids introducing copper / silver impurities in the target dissolving process, and can reduce the introduction of radioactive impurity ions in the irradiation process of the target material, so that the separation difficulty is reduced.

Description

Technical Field

[0001] This invention relates to the field of medical technology, specifically providing a method for preparing a gallium phosphate target and... 68 Preparation method of Ge. Background Technology

[0002] Positron emission tomography (PET) is an excellent molecular imaging technique in the field of nuclear medicine, and it has been widely used in the diagnosis and evaluation of various diseases such as brain diseases, mental illnesses, neuroendocrine tumors, prostate cancer, and infections.

[0003] Radionuclides 68 Ga, as a PET radiotracer with a half-life of 67.63 minutes, is becoming increasingly important in the detection and diagnosis of various cancers, as well as in the planning and monitoring of radiotherapy. 68 Ge as a production 68 The parent nuclide of Ga, for 68 The demand for Ge production is also increasing.

[0004] at present 68 Ge is primarily produced by bombarding gallium targets with medical particle accelerators. 69 Ga(p, 2n) 68 Ge reaction is used for production. Irradiation targets can be made of zinc, gallium alloys, Ga4Ni, Ga oxides (Ga2O3, Ga2O), NatGa, etc. However, zinc targets produce more radioactive impurities during irradiation, making separation difficult. Ga2O3 transforms from hexagonal α-type to monoclinic β-type at about 600℃, resulting in increased volume. If the beam intensity exceeds the critical limit, it can cause the target capsule to rupture. Therefore, this type of target can only be used for medium-intensity beams, but not for the high-intensity beams required for commercial production. Ga2O targets are complex to prepare and require a long preparation time, leading to… 68 Ge has low preparation efficiency; NatGa is packaged in a niobium can as a target material, which requires a separate beam system and its preparation is complicated; gallium-nickel alloy targets have good thermal conductivity and high melting point, and Ni is easy to separate, but gallium-nickel alloy targets generally use copper as the target material substrate, which introduces copper impurities during the target dissolution process, increasing the complexity of the process.

[0005] In the prior art, used for production 68 Ge's target materials suffer from difficulties in preparation, introduce numerous impurities, and have high requirements for the beam, leading to... 68 Ge's production efficiency is not high. Summary of the Invention

[0006] The present invention aims to at least partially solve the above-mentioned technical problems, that is, to at least partially solve the existing problems used in production 68Ge's target materials suffer from problems such as difficulty in target preparation, high impurity content, and high requirements for beam quality. 68 The problem of low production efficiency of Ge.

[0007] In a first aspect, the present invention provides a method for preparing a gallium phosphate target, the method comprising the following steps: S1: placing gallium phosphate powder into a target mold and sintering it to obtain a gallium phosphate crystal; S2: placing the gallium phosphate crystal into a metal can for encapsulation to obtain a gallium phosphate target.

[0008] In the preferred embodiment of the above-mentioned method for preparing gallium phosphate target, the purity of the gallium phosphate powder is not less than 98%.

[0009] In the preferred embodiment of the above-mentioned method for preparing gallium phosphate target, the gallium phosphate powder is prepared by hydrothermal synthesis reaction of gallium trioxide and phosphoric acid, wherein the reaction temperature is 100-180℃ and the reaction pressure is 3-6 MPa during the hydrothermal synthesis reaction.

[0010] In the preferred embodiment of the above-mentioned method for preparing gallium phosphate target, the reaction temperature is 120°C and the reaction pressure is 4 MPa.

[0011] In the preferred embodiment of the above-mentioned method for preparing gallium phosphate target, the molar ratio of gallium trioxide to phosphoric acid is 1:3.

[0012] In a second aspect, the present invention provides 68 The preparation method of Ge, 68 Ge is prepared using the gallium phosphate target described above. The preparation method includes the following steps: T1: placing the gallium phosphate target in a particle accelerator and irradiating it; T2: dissolving the irradiated gallium phosphate target to obtain a solution containing metal ion impurities. 68 Ge solution; T3: The solution containing metal ion impurities... 68 The Ge solution was separated and purified to obtain a solution containing... 68 Ge concentrate.

[0013] In the above 68 In a preferred embodiment of the method for preparing Ge, the irradiation conditions for irradiating the gallium phosphate target are: the irradiation energy range is 19–28 MeV; and / or the beam current intensity range is 100–300 μA.

[0014] In the above 68 In a preferred embodiment of the method for preparing Ge, the irradiation conditions for irradiating the gallium phosphate target are: the irradiation energy is 28 MeV; and / or the beam current intensity is 300 μA.

[0015] In the above 68 In a preferred embodiment of the method for preparing Ge, "the irradiated gallium phosphate target is dissolved to obtain a product containing metal ion impurities." 68 The steps for obtaining the "Ge solution" specifically include: T21: removing the irradiated gallium phosphate target from the metal container and dissolving it in concentrated sulfuric acid to obtain a solution; T22: adjusting the pH of the solution to an HCl concentration of 1.3–1.6 M to obtain a solution containing metal ion impurities. 68 Ge solution.

[0016] In the above 68 In a preferred embodiment of the method for preparing Ge, "the metal ion impurity-containing... 68 The Ge solution was separated and purified to obtain a solution containing... 68 The specific steps of the "Ge concentrate" include: T31: [The text abruptly ends here, likely due to an incomplete sentence or a formatting error.] 68 A Ge solution is added to the first separation column to remove zinc impurities, and the effluent is collected; T32: Sodium citrate and alkaline solution are added to the effluent, and the pH of the effluent is adjusted to 11.5-13, then added to the second separation column; T33: The second separation column is washed sequentially with sodium citrate (pH 11.5-13), alkaline solution (pH 11.5-13), and water; T34: The second separation column is eluted with an eluent to obtain a solution containing... 68 A concentrate of Ge; wherein the first separation column comprises at least AG1-X8 resin and the second separation column comprises at least Sephadex G25 resin.

[0017] When the above-mentioned preferred technical solution is adopted, that is, the present invention uses gallium phosphate as the irradiation target, which gives the target a higher melting point and higher thermal stability. Its performance is superior to that of gallium oxide targets, and it can be used in the production of cyclotron accelerators. 68 Compared to NatGa targets, Ge targets are suitable for high-current accelerators and are more suitable for commercial-scale production. Compared to alloy targets, Ge targets avoid the use of copper / silver as the substrate, thus avoiding the introduction of copper / silver impurities during the dissolution process. This solves the problem of introducing copper or silver impurities during the dissolution process of copper / silver-based alloy targets and reduces the introduction of radioactive impurity ions during irradiation, thereby reducing the difficulty of separation.

[0018] Furthermore, by ensuring that the purity of the gallium phosphate powder is not less than 98%, a high purity of the gallium phosphate powder can be guaranteed, resulting in a high purity gallium phosphate crystal and reducing impurities in the gallium phosphate target. On the one hand, this avoids the introduction of other derivative impurities during irradiation due to impurities mixed in the gallium phosphate powder; on the other hand, it also avoids the influence of impurities mixed in the gallium phosphate powder on... 68Separation and purification of Ge, and then the prepared 68 Ge has higher purity.

[0019] Further, by setting the molar ratio of gallium sesquioxide and phosphoric acid to 1:3, the gallium sesquioxide and the phosphoric acid can be ensured to be excessive when performing the hydrothermal synthesis reaction, so that the gallium sesquioxide solid can fully react with the phosphoric acid, avoiding the residual gallium sesquioxide affecting the purity of the gallium phosphate powder, and further helping to improve the purity of the prepared gallium phosphate powder.

[0020] Further, by using the gallium phosphate target as an irradiation target for preparing 68 Ge, the use of copper / silver as a target substrate can be avoided, and further the introduction of copper / silver impurities in the target dissolution process can be avoided, solving the problem of the introduction of copper or silver impurities in the dissolution process of the alloy target with copper / silver as the substrate, and reducing the separation difficulty; since the gallium phosphate target has a high melting point and high thermal stability, its performance is better than that of the gallium oxide target, and it can be applied to the production of 68 Ge by the cyclotron; compared with the NatGa target, the gallium phosphate target is suitable for high-beam accelerators and is more suitable for commercial-scale production.

[0021] Further, by irradiating the gallium phosphate target at a higher irradiation energy and a stronger beam intensity, the yield of 68 Ge can be improved, the irradiation time can be reduced, and the production efficiency of 68 Ge can be improved.

[0022] Further, by taking out the gallium phosphate target after irradiation from the metal can and adding concentrated sulfuric acid for dissolution, the dissolution of the substrate material in the target dissolution process is avoided, the introduction of impurity ions is reduced, and the separation difficulty is reduced.

[0023] Further, by designing the separation system of the first separation column and the second separation column, after dissolving the gallium phosphate target after irradiation, the AG1-X8 resin can be used to efficiently remove the Zn impurity ions produced after irradiation, and the Sephedex G25 resin can be used to efficiently remove the Ga, Co and other impurity ions and 68 Ge, so that the obtained 68 Ge product has high purity and high recovery rate. BRIEF DESCRIPTION OF DRAWINGS

[0024] The preferred embodiments of the present application will be described below with reference to the accompanying drawings, in which:

[0025] Figure 1 is a flowchart of the preparation method of the gallium phosphate target of the present application;

[0026] Figure 2 is a flowchart of the preparation method of the gallium phosphate target of the present application;68 Flow chart of main steps of the preparation method of Ge;

[0027] Figure 3 is the preparation method of the gallium phosphate target of the present application 68 Flow chart of specific embodiments of the preparation method of Ge. DETAILED DESCRIPTION

[0028] The preferred embodiments of the present application are described below with reference to the accompanying drawings. Those skilled in the art will understand that these embodiments are only used to explain the technical principles of the present application, and are not intended to limit the protection scope of the present application.

[0029] The test methods in the following examples are all conventional methods unless otherwise specified; the raw materials, reagents and materials used in the following examples are all commercially available products unless otherwise specified.

[0030] Based on the existing 68 The target material used for the preparation of Ge has problems such as difficult preparation of the target material, more radioactive impurities generated during irradiation, higher requirements for the light beam, etc., which leads to 68 low efficiency of Ge preparation, the present application provides a preparation method of a gallium phosphate target for producing 68 Ge.

[0031] Specifically, please refer to Figure 1 , Figure 1 is the flow chart of the preparation method of the gallium phosphate target of the present application.

[0032] As shown in Figure 1 , the preparation method of the gallium phosphate target of the present application comprises the following steps:

[0033] S1: Put the gallium phosphate powder into the target material mold, sinter, and obtain the gallium phosphate crystal;

[0034] S2: Put the gallium phosphate crystal into a metal can for packaging, and obtain the gallium phosphate target.

[0035] By using gallium phosphate as the irradiation target material, the target material has a high melting point and high thermal stability, and its performance is better than that of the gallium oxide target material, and can be applied to the production of 68 Ge by the cyclotron; compared with the NatGa target material, it can be applied to the high-beam accelerator, and is more suitable for commercial scale production; compared with the alloy target material, it can avoid using copper / silver as the target material substrate, thereby avoiding the introduction of copper / silver impurities in the target dissolution process, solving the problem of the introduction of copper or silver impurities in the dissolution process of the alloy target material with copper / silver as the substrate, and reducing the difficulty of separation.

[0036] It should be noted that gallium phosphate powder can form gallium phosphate crystals after sintering. By placing gallium phosphate powder into a target mold and sintering it, the desired gallium phosphate crystals can be obtained. The gallium phosphate crystals are then placed into a metal can for encapsulation, thus producing gallium phosphate targets.

[0037] It should also be noted that since gallium phosphate crystals are formed by sintering gallium phosphate powder, the purity of the gallium phosphate powder has a significant impact on the purity of the gallium phosphate crystals. Therefore, the quality of the prepared gallium phosphate target can be controlled by controlling the purity of the gallium phosphate powder.

[0038] Preferably, the purity of the gallium phosphate powder is not less than 98%.

[0039] This setup ensures high purity of the gallium phosphate powder, resulting in high purity gallium phosphate crystals and reduced impurities in the gallium phosphate target. On one hand, it prevents impurities in the gallium phosphate powder from introducing other derivative impurities during irradiation; on the other hand, it also avoids the influence of impurities in the gallium phosphate powder on... 68 The separation and purification of Ge reduces the difficulty of separation, making the prepared... 68 Ge has a higher recovery rate.

[0040] It should be noted that this invention does not impose any restrictions on the specific preparation method of gallium phosphate powder, as long as gallium phosphate powder with the required purity can be obtained.

[0041] Preferably, the gallium phosphate powder is prepared by a hydrothermal synthesis reaction of gallium trioxide and phosphoric acid.

[0042] Specifically, the reaction mechanism for preparing gallium phosphate powder from gallium trioxide and phosphoric acid via a hydrothermal synthesis reaction is as follows:

[0043] Ga₂O₃ + 2H₃PO₄ = 2GaPO₄ + 3H₂O

[0044] The reaction temperature is 100–180℃, the reaction pressure is 3–6 MPa, and the molar ratio of gallium trioxide to phosphoric acid is 1:(2–4).

[0045] Preferably, the temperature of the hydrothermal synthesis reaction is 120°C.

[0046] This setup avoids two problems: firstly, gallium trioxide failing to fully react with phosphoric acid to form gallium phosphate due to excessively low temperatures; and secondly, it prevents energy waste caused by excessively high temperatures.

[0047] Preferably, the reaction pressure of the hydrothermal synthesis reaction is 4 MPa.

[0048] Through the arrangement, on the one hand, the insufficient reaction of gallium sesquioxide and phosphoric acid to generate gallium phosphate due to the excessively low pressure can be avoided, and on the other hand, the excessively high pressure to increase the pressure bearing requirement of the reaction equipment can be avoided.

[0049] Preferably, the molar ratio of gallium sesquioxide and phosphoric acid is 1:3.

[0050] Through the arrangement, the excess of phosphoric acid can be ensured when the gallium sesquioxide and the phosphoric acid are subjected to the hydrothermal synthesis reaction, so that the gallium sesquioxide solid is fully reacted with the phosphoric acid, the residual gallium sesquioxide is avoided to affect the purity of the gallium phosphate powder, and the purity of the prepared gallium phosphate powder is further improved.

[0051] It should be noted that, in actual application, the gallium phosphate powder can be placed into a muffle furnace for sintering to form gallium phosphate crystals, or the gallium phosphate powder can be placed into a sintering furnace for sintering to form gallium phosphate crystals, or the gallium phosphate powder can be placed into any other possible container for sintering to form gallium phosphate crystals, and the like, and the adjustment and change of the sintering mode of the gallium phosphate powder do not deviate from the principles and scope of the present application, and should be included in the protection scope of the present application.

[0052] Preferably, the gallium phosphate powder is placed into a muffle furnace for sintering to form gallium phosphate crystals.

[0053] It should be noted that, in actual application, the present application does not make any limitation on the sintering temperature, as long as the gallium phosphate powder can form gallium phosphate crystals, and the like, and the adjustment and change of the sintering temperature do not deviate from the principles and scope of the present application, and should be included in the protection scope of the present application.

[0054] Preferably, the sintering temperature is 500-550℃.

[0055] Further preferably, the sintering temperature is 540℃.

[0056] Through the arrangement, the gallium phosphate powder can be more fully converted into gallium phosphate crystals, the yield of the gallium phosphate crystals is higher, and the preparation cost of the gallium phosphate target is further reduced.

[0057] It should be noted that, in actual application, the gallium phosphate crystals can be placed into an aluminum can for packaging to obtain a gallium phosphate target, or the gallium phosphate crystals can be placed into a niobium can for packaging to obtain a gallium phosphate target, and the like, and the adjustment and change of the specific arrangement type of the packaging material of the target do not deviate from the principles and scope of the present application, and should be included in the protection scope of the present application.

[0058] Preferably, gallium phosphate crystals are encapsulated in an aluminum can to obtain a gallium phosphate target.

[0059] Because target materials encapsulated in niobium containers require a separate beam system during irradiation, this increases irradiation costs. Compared to encapsulating gallium phosphate crystals in niobium containers, encapsulating gallium phosphate crystals in aluminum containers reduces costs during the irradiation preparation of gallium phosphate targets. 68 At Ge time, no separate beam system is required, reducing the beam current requirements during the irradiation process and thus reducing [the risk of contamination]. 68 The production cost of Ge.

[0060] Furthermore, the present invention also provides 68 Preparation method of Ge 68 Ge is prepared using the gallium phosphate target material described above.

[0061] Specifically, please refer to Figure 2 , Figure 2 This is the invention 68 A flowchart of the main steps in the preparation method of Ge.

[0062] like Figure 2 As shown, 68 The preparation method of Ge includes the following steps:

[0063] T1: Place the gallium phosphate target into the particle accelerator and irradiate the gallium phosphate target.

[0064] T2: Dissolve the irradiated gallium phosphate target to obtain a solution containing metal ion impurities. 68 Ge solution;

[0065] T3: Contains metal ion impurities. 68 The Ge solution was separated and purified to obtain a solution containing... 68 Ge concentrate.

[0066] This setup utilizes gallium phosphate targets with high melting points and high thermal stability to prepare... 68 Ge can be used for irradiation at higher irradiation energies and stronger beam intensities, thereby improving irradiation efficiency and increasing... 68 Ge's yield, thereby increasing 68 The production efficiency of Ge is improved, and the introduction of impurities during the irradiation process is reduced. By avoiding the use of copper / silver as the target substrate, the dissolution of the substrate material during target dissolution is avoided, further reducing the introduction of impurity ions. 68 The separation and purification of Ge is simpler. 68 Ge has a higher recovery rate.

[0067] It should be noted that in practical applications, gallium phosphate targets can be placed in cyclotrons and irradiated, or gallium phosphate targets can be placed in any other possible particle acceleration equipment and irradiated, etc. Such adjustments and changes to the specific irradiation method of gallium phosphate targets do not deviate from the principles and scope of the present invention and should be included within the protection scope of the present invention.

[0068] Preferably, the gallium phosphate target is placed in a cyclotron and irradiated.

[0069] In a preferred embodiment of the present invention, the irradiation conditions for irradiating the gallium phosphate target are as follows:

[0070] The irradiation energy ranges from 19 to 28 MeV, the beam current ranges from 100 to 300 μA, and the irradiation time ranges from 9 to 11 hours.

[0071] More preferably, the irradiation energy is 28 MeV, the beam current intensity is 300 μA, and the irradiation time is 10 h.

[0072] By irradiating gallium phosphate targets under high irradiation and strong beam intensity, it is possible not only to improve... 68 Ge's yield can also increase 68 Ge production efficiency.

[0073] See next Figure 3 , Figure 3 This is the invention 68 Flowcharts of specific embodiments of the method for preparing Ge.

[0074] Preferably, such as Figure 3 As shown, "Dissolving the irradiated gallium phosphate target yields a product containing metal ion impurities." 68 The specific steps involved in preparing the "Ge solution" include:

[0075] T21: Remove the irradiated gallium phosphate target from the metal container and dissolve it in concentrated sulfuric acid to obtain a solution.

[0076] Specifically, after the irradiated gallium phosphate target is transferred to a hot chamber for cooling, the aluminum can is cut open, the gallium phosphate target is taken out, the gallium phosphate target is placed in a dissolution pool, concentrated sulfuric acid is added to the dissolution pool to dissolve the gallium phosphate target, and a solution is obtained.

[0077] The reaction mechanism of the dissolution process of gallium phosphate target is as follows:

[0078] 2GaPO4 + 2H2SO4 = 2Ga 3+ +2HPO4 - +2SO4 2- +H2

[0079] Through such arrangement, by taking out the gallium phosphate target after irradiation from the metal canister and adding concentrated sulfuric acid for dissolution, the dissolution of the base material during target dissolution is avoided, the introduction of impurity ions is reduced, and the separation difficulty is reduced.

[0080] T22: adjust the PH of the dissolving solution to 1.3-1.6M HCl concentration to obtain a 68 Ge solution containing metal ion impurities.

[0081] It should be noted that in step T22, when adjusting the PH of the dissolving solution, an acidic solution and a basic solution are used to adjust the PH of the dissolving solution, for example, one or more of hydrochloric acid, dilute sulfuric acid, nitric acid can be used as the acidic solution, and one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate can be used as the basic solution, etc. The adjustment and change of the specific type of the acidic solution and the basic solution used in the PH adjustment process of the dissolving solution do not deviate from the principles and scope of the present application, and should be included in the protection scope of the present application.

[0082] Preferably, hydrochloric acid is used as the acidic solution, and sodium hydroxide is used as the basic solution to adjust the PH of the dissolving solution to 1.3-1.6M HCl concentration.

[0083] Further preferably, the PH of the dissolving solution is adjusted to 1.5M HCl concentration.

[0084] Preferably, as shown in Figure 3 , the step of "separating and purifying the 68 Ge solution containing metal ion impurities to obtain a concentrated solution containing 68 Ge" specifically includes:

[0085] T31: adding the 68 Ge solution containing metal ion impurities to a first separation column to remove zinc impurities and collect the effluent, wherein the first separation column at least includes AG1-X8 resin.

[0086] It should be noted that since the AG1-X8 resin can complex with zinc ions in an acidic system of 1.3-1.6M HCl, and also adsorb a large amount of cobalt ions, most of the zinc ions and cobalt ions are left in the first separation column, and the effluent containing gallium ions, 68 Ge ions and a small amount of impurity ions (zinc ions, cobalt ions) is obtained.

[0087] T32: Add sodium citrate and alkaline solution to the effluent and adjust the pH of the effluent to 11.5-13, then add it to the second separation column, wherein the second separation column includes at least Sephadex G25 resin.

[0088] It should be noted that the hydroxyl groups in Sephadex G25 resin can selectively adsorb under weakly alkaline conditions (pH 11.5–13). 68 Ge ions are reacted with sodium citrate to form a complex (gallium citrate), preventing gallium ions from precipitating as Ga(OH)3 under alkaline conditions. Sodium citrate also forms a cobalt citrate complex with cobalt ions in the effluent. Both gallium citrate and cobalt citrate complexes are water-soluble, thus preventing gallium and cobalt ions from remaining in the Sephadex G25 resin. Therefore, adding sodium citrate and alkaline solution to the effluent and adjusting its pH to 11.5–13 can achieve… 68 Separation of Ge.

[0089] T33: The second separation column is washed sequentially with sodium citrate solution with pH 11.5–13, alkaline solution with pH 11.5–13, and water.

[0090] The Sephadex G25 resin was washed sequentially with sodium citrate and water to further remove gallium, cobalt, and zinc ion impurities, thereby further improving its performance. 68 Separation efficiency of Ge.

[0091] T34: Elution was performed using an eluent to obtain a product containing... 68 Ge concentrate;

[0092] Sephadex G25 resin was eluted with eluent to obtain a solution containing... 68 Ge's concentrated solution, to achieve 68 Purification of Ge.

[0093] It should be noted that in practical applications, no restrictions are placed on the specific type of alkaline solution. For example, the alkaline solution can be set as one or more of sodium hydroxide, potassium hydroxide, and lithium hydroxide, etc. Such adjustments and changes to the specific type of alkaline solution do not deviate from the principles and scope of the present invention and should be included within the protection scope of the present invention.

[0094] Preferably, the alkaline solution is sodium hydroxide, and sodium citrate and sodium hydroxide are added to the effluent to adjust the pH of the effluent to 11.5-13.

[0095] It should be noted that, when washing the second separation column, the present application does not limit the concentration of sodium citrate and the number of washing times. For example, sodium citrate can be used only once, or sodium citrate of the same concentration can be used multiple times, or sodium citrate of different concentrations can be used multiple times, and the like. Such flexible adjustment and change do not deviate from the principles and scope of the present application and should be included in the protection scope of the present application.

[0096] In the step T33, when washing the second separation column, 5 bed volumes of 1M sodium citrate are used to wash the second separation column, and then 5 bed volumes of 0.001M sodium citrate are used to wash the second separation column.

[0097] Through such a setting, the use of 5 bed volumes of 1M sodium citrate to wash the second separation column can form citric acid complexes of the residual gallium ions and cobalt ions in the second separation column, and the use of 5 bed volumes of 0.001M sodium citrate to wash the second separation column can further form citric acid complexes of the residual gallium ions and cobalt ions in the second separation column. Since the residual gallium ions and cobalt ions are less, when washing the second time, the use of low-concentration sodium citrate can make the residual gallium ions and cobalt ions in the second separation column form soluble citric acid complexes.

[0098] It should be noted that 1 bed volume is the volume of the filler of the second separation column.

[0099] For example, the volume of the filler of the second separation column is set to V,

[0100] Then, 1 bed volume = 1 × V;

[0101] 3 bed volumes = 3 × V;

[0102] 5 bed volumes = 5 × V;

[0103] 10 bed volumes = 10 × V.

[0104] It should be further noted that the pH of 5 bed volumes of 1M sodium citrate and 5 bed volumes of 0.001M sodium citrate is 11.5-13, that is, after measuring the sodium citrate, an alkali solution (such as sodium hydroxide) is used to adjust the pH to 11.5-13.

[0105] Specifically, 10 bed volumes of 0.03M alkali solution are used to wash the second separation column.

[0106] By using an alkali solution to wash the second separation column, part of the residual Ga, Co, Zn, and the like can be eluted, further reducing the retention of impurity ions on the second separation column.

[0107] In step T33 above, when washing the second separation column with water, the present invention does not impose any restrictions on the amount of water used for washing. For example, the second separation column can be washed with one bed volume of water, or two bed volumes of water, etc. Such adjustments and changes in the amount of water used for washing the second separation column do not deviate from the principles and scope of the present invention and should be included within the protection scope of the present invention.

[0108] Preferably, the second separation column is washed with one bed volume of water.

[0109] By using water to wash the second separation column, this setup can further remove impurity ions from the column and improve its performance. 68 On the one hand, it improves the purity of Ge separation, and on the other hand, it can reduce the alkalinity of the second separation column, which facilitates subsequent elution steps.

[0110] In step T34 above, when eluting the second separation column, one or more of hydrochloric acid, sulfuric acid, and nitric acid can be used as the eluent, etc. Such adjustments and changes to the specific type of eluent do not deviate from the principle and scope of the present invention and should be included within the protection scope of the present invention.

[0111] In a preferred embodiment of the present invention, a 3-bed volume of 0.1M hydrochloric acid is used as the eluent to elute the second separation column, thereby removing the adsorbed material from the second separation column. 68 Ge was washed off, and the product contained... 68 Ge concentrate.

[0112] It should be noted that for the first separation column, 0.01M HCl is used for elution to recover the Zn impurity ions adsorbed on the first separation column. The first separation column can be reused, reducing costs. 68 The cost of separating and purifying Ge, thereby reducing 68 The production cost of Ge.

[0113] It should also be noted that the second separation column, being cross-linked from glucose and glycerol groups, is stable under both weakly acidic and weakly alkaline conditions. Therefore, it can be reused for separation after only a simple activation treatment, thus enabling its repeated use and reducing costs. 68 The cost of separating and purifying Ge.

[0114] The present invention will be described in detail below through specific embodiments. 68 Preparation method of Ge.

[0115] Example 1

[0116] The embodiment of the present application 68 The preparation step of Ge is as follows:

[0117] S11: Phosphoric acid is added to di-gallium trioxide to prepare gallium phosphate powder through a hydrothermal synthesis reaction, wherein the molar ratio of di-gallium trioxide to phosphoric acid is 1:3, the reaction temperature of the hydrothermal synthesis reaction is 120°C, the reaction pressure is 4Mpa, and the purity of the prepared gallium phosphate powder is 98%.

[0118] S12: The gallium phosphate powder is placed into a target mold to perform sintering, thereby obtaining a gallium phosphate crystal, wherein the sintering temperature is 540°C.

[0119] S2: The gallium phosphate crystal is placed into an aluminum tank to perform packaging, thereby obtaining a gallium phosphate target;

[0120] S3: The gallium phosphate target is placed into a cyclotron, and the gallium phosphate target is irradiated, wherein the irradiation energy is 28MeV, the beam intensity is 300μA, and the irradiation time is 10h.

[0121] S41: The gallium phosphate target after irradiation is taken out from the aluminum tank, and concentrated sulfuric acid is added to dissolve, thereby obtaining a dissolving solution.

[0122] S42: Sodium hydroxide and hydrochloric acid are added to the dissolving solution, the PH of the dissolving solution is adjusted to 1.5M of HCl concentration, thereby obtaining a 68 Ge solution containing metal ion impurities.

[0123] S51: The 68 Ge solution containing metal ion impurities is added into a first separation column (AG1-X8 resin) to remove zinc impurities, and the effluent is collected.

[0124] S52: Sodium citrate and sodium hydroxide are added to the effluent, and the PH of the effluent is adjusted to 12.5.

[0125] S53: The second separation column (Sephadex G25 resin) is sequentially washed with 1M sodium citrate with PH of 12.5, 0.001M sodium citrate with PH of 12.5, 0.03M sodium hydroxide with PH of 12.5, and water.

[0126] S53: The second separation column is eluted with 0.1M HCl, thereby obtaining a concentrated solution containing 68 Ge.

[0127] Example 2

[0128] The embodiment of the present application 68The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the irradiation energy of the gallium phosphate target. In this example, the irradiation energy of the gallium phosphate target is 16MeV.

[0129] Example 3

[0130] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the irradiation energy of the gallium phosphate target. In this example, the irradiation energy of the gallium phosphate target is 19 MeV.

[0131] Example 4

[0132] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the irradiation energy of the gallium phosphate target. In this example, the irradiation energy of the gallium phosphate target is 25 MeV.

[0133] Example 5

[0134] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the irradiation energy of the gallium phosphate target. In this example, the irradiation energy of the gallium phosphate target is 34 MeV.

[0135] Example 6

[0136] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the beam intensity of the gallium phosphate target irradiation. In this example, the beam intensity of the gallium phosphate target is 80 μA.

[0137] Example 7

[0138] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the beam intensity of the gallium phosphate target irradiation. In this example, the beam intensity of the gallium phosphate target is 100 μA.

[0139] Example 8

[0140] This embodiment 68The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the beam intensity of the gallium phosphate target irradiation. In this example, the beam intensity of the gallium phosphate target is 200 μA.

[0141] Example 9

[0142] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the beam intensity of the gallium phosphate target irradiation. In this example, the beam intensity of the gallium phosphate target is 400 μA.

[0143] Example 10

[0144] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the reaction temperature of preparing gallium phosphate powder by hydrothermal synthesis and the purity of the obtained gallium phosphate powder. In this example, the reaction temperature of preparing gallium phosphate powder by hydrothermal synthesis is 100°C, and the purity of the obtained gallium phosphate powder is 96.5%.

[0145] Example 11

[0146] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the reaction temperature of preparing gallium phosphate powder by hydrothermal synthesis and the purity of the obtained gallium phosphate powder. In this example, the reaction temperature of preparing gallium phosphate powder by hydrothermal synthesis is 180°C, and the purity of the obtained gallium phosphate powder is 98.2%.

[0147] Example 12

[0148] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the reaction pressure and the purity of the gallium phosphate powder obtained by the hydrothermal synthesis reaction. In this example, the reaction pressure of the gallium phosphate powder obtained by the hydrothermal synthesis reaction is 3 MPa, and the purity of the gallium phosphate powder obtained is 96.6%.

[0149] Example 13

[0150] This embodiment 68The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the reaction pressure and the purity of the gallium phosphate powder obtained by the hydrothermal synthesis reaction. In this example, the reaction pressure of the gallium phosphate powder obtained by the hydrothermal synthesis reaction is 6 MPa, and the purity of the gallium phosphate powder obtained is 98.2%.

[0151] Example 14

[0152] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the molar ratio of gallium trioxide to phosphoric acid when preparing gallium phosphate powder by hydrothermal synthesis reaction and the purity of the obtained gallium phosphate powder. In this example, the molar ratio of gallium trioxide to phosphoric acid is 1:2, and the purity of the obtained gallium phosphate powder is 95%.

[0153] Example 15

[0154] This embodiment 68 The preparation steps of Ge are the same as in Example 1. The only difference between this example and Example 1 is the molar ratio of gallium trioxide to phosphoric acid when preparing gallium phosphate powder by hydrothermal synthesis reaction and the purity of the obtained gallium phosphate powder. In this example, the molar ratio of gallium trioxide to phosphoric acid is 1:4, and the purity of the obtained gallium phosphate powder is 98%.

[0155] Comparative Example 1 :

[0156] This comparative example preparation 68 The target material used in Ge is a gallium-nickel alloy target.

[0157] This comparative example 68 The preparation steps of Ge are as follows:

[0158] T1: The gallium-nickel alloy target is placed in a cyclotron and irradiated. The irradiation energy is 20 MeV, the beam current is 300 μA, and the irradiation time is 10 h.

[0159] T2: Dissolving the irradiated gallium-nickel alloy target yields a product containing metal ion impurities. 68 Ge solution.

[0160] T3: Contains metal ion impurities. 68 The Ge solution was separated and purified to obtain a solution containing... 68 Ge concentrate.

[0161] Specifically, after the target material is dissolved, it is separated and purified using two resins: Chelex 100 and Sephadex G25.

[0162] Comparative Example 2

[0163] The comparative example was prepared 68 The target material used for Ge was a NatGa target material.

[0164] The preparation steps of Ge in the comparative example were as follows: 68 The preparation steps of Ge in the comparative example were as follows:

[0165] T1: The NatGa target material was placed into a cyclotron and irradiated, wherein the irradiation energy was 45 MeV, the beam intensity was 50 μA, and the irradiation time was 21 days.

[0166] T2: The NatGa target material after irradiation was dissolved to obtain a Ge solution containing metal ion impurities. 68 The Ge solution.

[0167] T3: The Ge solution containing metal ion impurities was separated and purified to obtain a concentrated solution containing Ge. 68 The Ge solution. 68 The Ge solution.

[0168] Specifically, after the target material was dissolved, AG1-X8, Chelex 100 and Sephadex G25 resins were used for separation and purification.

[0169] Comparative Example 3

[0170] The comparative example was prepared 68 The target material used for Ge was a Ga2O target material.

[0171] The preparation steps of Ge in the comparative example were as follows: 68 The preparation steps of Ge in the comparative example were as follows:

[0172] T1: The Ga2O target material was placed into a cyclotron and irradiated, wherein the irradiation energy was 34 MeV, the beam intensity was 80 μA, and the irradiation time was 15 days.

[0173] T2: The Ga2O target material after irradiation was dissolved to obtain a Ge solution containing metal ion impurities. 68 The Ge solution.

[0174] T3: The Ge solution containing metal ion impurities was separated and purified to obtain a concentrated solution containing Ge. 68 The Ge solution. 68 The Ge solution.

[0175] Specifically, after the target material was dissolved, an extraction method was used for separation and purification.

[0176] Test Example 1

[0177] The steps of the above embodiments and comparative examples were performed respectively. 68 Preparation of Ge, and obtaining a product containing 68 Ge concentrate was tested to obtain the contents of... 68 Ge's concentrate 68 The radiochemical concentration of Ge 68 Ge's nuclear purity, 68 The radiochemical purity of Ge is used to determine the obtained 68 Does Ge conform to the DOE specification?

[0178] The specific testing methods are as follows:

[0179] The above were detected using an activity meter. 68 A concentrated solution of Ge was obtained. 68 Radiochemical concentration of Ge;

[0180] The above-mentioned detectors were used to detect the high-purity germanium detector. 68 A concentrated solution of Ge was obtained. 68 Ge's nuclear purity;

[0181] The above were detected using thin-layer chromatography. 68 A concentrated solution of Ge was obtained. 68 Radiochemical purity of Ge.

[0182] After testing, the results obtained from the examples and comparative examples... 68 The radiochemical concentrations of Ge were all greater than 10 mCi / ml, as obtained in the examples and comparative examples. 68 The purity of Ge was greater than 99% in all examples and comparative examples. 68 The radiochemical purity of Ge is greater than 99%, that is, the preparation methods according to the examples and comparative examples yielded [Ge]. 68 All Ge conforms to the DOE specifications.

[0183] Test Example 2

[0184] The preparations were carried out using the steps of the above-described embodiments and comparative examples, respectively, and the products containing [the ingredients] were obtained. 68 Ge concentrate, testing 68 The yield R of Ge concentrate and 68 The recovery rate K of Ge is shown in Table 1.

[0185] 68 The specific method for detecting the yield of Ge is as follows:

[0186] The above were determined using an activity meter. 68 The radiochemical activity B of the concentrated Ge solution is calculated according to the following formula. 68The yield R of Ge (unit: μCi / (μA.h));

[0187] R = B ÷ I ÷ t.

[0188] Wherein, I is the beam intensity (unit: μA) during irradiation, and t is the irradiation time (unit: h) during irradiation.

[0189] It should be noted that, 68 The yield of Ge is expressed as: the yield of Ge produced by unit beam intensity irradiation per hour 68 The activity of the Ge radioactive source.

[0190] 68 The detection method of the recovery rate K of Ge is specifically:

[0191] During the preparation process, the ICP-MS is used to detect the dissolved solution before separation and purification, analyze and obtain 68 The concentration C1 (mg / L) of Ge, the ICP-MS is used to detect the concentrated solution of Ge prepared, analyze and obtain 68 The concentration C2 (mg / L) of Ge, 68

[0192] The recovery rate K of Ge is calculated according to the following formula, 68

[0193] K = (C1 ÷ C2) × 100%.

[0194] Table 1: Test data of examples and comparative examples

[0195]

[0196]

[0197] From the test data in Table 1, it can be seen that:

[0198] 1. Comparative Examples 1 to 3 and Examples 1 to 14 are compared, the yield of Ge of Comparative Examples 1 to 3 is obviously lower than that of Examples 1 to 14, and the irradiation time of Comparative Examples 2 and 3 is obviously longer than that of Examples 1 to 14, that is, the production of required Ge is required. 68 2. The yield of Ge of Comparative Examples 2 and 3 is obviously lower than that of Examples 1 to 14, and the irradiation time of Comparative Examples 2 and 3 is obviously longer than that of Examples 1 to 14, that is, the production of required Ge is required. 68 3. The yield of Ge produced by using the gallium phosphate target material is obviously higher than that of other types of target materials, and the irradiation time required for producing Ge by using the gallium phosphate target material is obviously shorter than that of NatGa target material and Ga2O target material, and the production efficiency is higher. 68 4. The yield of Ge produced by using the gallium phosphate target material is obviously higher than that of other types of target materials, and the irradiation time required for producing Ge by using the gallium phosphate target material is obviously shorter than that of NatGa target material and Ga2O target material, and the production efficiency is higher. 68

[0199] ​​​2. Compare Examples 1 to 5. Examples 1, 3, 4, and 5 are... 68 The yield of Ge was significantly higher than that in Examples 2 and 5, indicating that when the irradiation energy is 19–28 MeV, the yield obtained is higher. 68 Ge has a relatively high yield.

[0200] Due to irradiation energy and 69 The reaction rate of Ga is related to nuclear reactions. As the irradiation energy increases, the reaction rate gradually increases. When the irradiation energy reaches a certain level, the reaction rate reaches its optimal state. When the irradiation energy increases further, the reaction rate will decrease again.

[0201] Since the target material has a certain thickness, the energy will attenuate after passing through the surface of the target material and irradiating the interior of the target material. If the irradiation energy is low, although the surface of the target material can receive sufficient irradiation energy, the energy attenuates when it passes through the target material and reaches the interior of the target material, which is insufficient to achieve a good reaction state inside the target material. If the energy is too high, although it can also ensure a high energy when irradiating the interior of the target material, so that the interior of the target material can achieve a good reaction state, the high irradiation energy will cause the reaction rate on the surface of the target material to decrease. In order to ensure a good reaction state on both the surface and inside of the target material, the preferred irradiation energy is 19 to 28 MeV.

[0202] 3. Comparing Example 1 with Examples 6 to 9, the yields of Examples 1, 7, and 8 were significantly higher than that of Example 6. As the beam intensity increased, 68 The yield of Ge also increases accordingly. When the beam intensity increases to a certain level, the yield reaches saturation. However, when the beam intensity increases further, excessively high beam intensity will damage the target structure, which will lead to… 68 The yield of Ge further decreased, indicating that the irradiation conditions are suitable when the beam current intensity is 100–300 μA, resulting in relatively high production efficiency without damaging the target structure, and the prepared Ge yield is optimal. 68 Ge yield is at a high level.

[0203] 4. Compare Example 1 with Examples 10 to 14. Examples 1, 11, and 13... 68 Ge recovery rate and 68 The yields of Ge were significantly higher than those in Examples 10, 12, and 14, indicating that when the purity of gallium phosphate powder is greater than 98%, the prepared Ge yield can be significantly increased. 68 Ge recovery rate and 68 Ge yields are at a good level.

[0204] Although in Example 168 Ge recovery rate and 68 The yield of Ge was lower than that in Examples 11 and 13, but with the increase in the purity of gallium phosphate powder, 68 Ge recovery rate and 68 The yield of Ge did not improve significantly, while further improvement in the purity of gallium phosphate powder would increase the difficulty of preparing gallium phosphate powder, leading to a further increase in production costs.

[0205] Therefore, it can be seen that when the purity of gallium phosphate powder is 98%, the prepared... 68 Ge recovery rate and 68 The yield of Ge is at a good level, and the preparation difficulty of gallium phosphate powder will not increase significantly.

[0206] It should be noted that the recovery rate represents the product after purification. 68 Ge and before purification 68 The concentration ratio of Ge, that is, the impurity content in the solution, determines the recovery rate. The purity of the gallium phosphate target determines the impurity content in the solution, and the purity of the gallium phosphate powder, in turn, affects the purity of the gallium phosphate target. Therefore... 68 The recovery rate of Ge is closely related to the purity of gallium phosphate powder. That is, under the same separation and purification process conditions, the higher the purity of gallium phosphate powder, the better. 68 The higher the recovery rate of Ge, the lower the purity of the gallium phosphate powder. 68 The lower the recovery rate of Ge.

[0207] Impurities in the gallium phosphate target can affect the irradiation effect during the irradiation process; therefore, the purity of the gallium phosphate powder also affects the irradiation effect. 68 The higher the purity of gallium phosphate powder, the better the yield of Ge. 68 Ge's yield is also relatively high.

[0208] 5. Comparing Example 1 with Examples 10 and 11, the purity of gallium phosphate powder in Example 1 is significantly higher than that in Example 10. Although the purity of gallium phosphate powder in Example 11 is higher than that in Example 1, the purity of the prepared gallium phosphate powder does not increase significantly with the increase of the hydrothermal synthesis reaction temperature. Moreover, considering that the increase of the hydrothermal synthesis reaction temperature will lead to the increase of energy consumption, it can be concluded that the preferred temperature for the hydrothermal synthesis reaction is 120°C.

[0209] 6. Comparing Example 1 with Examples 12 and 13, the purity of the gallium phosphate powder prepared in Example 1 is significantly higher than that in Example 12. Although the purity of the gallium phosphate powder prepared in Example 13 is higher than that in Example 1, the purity of the prepared gallium phosphate powder does not increase significantly with the increase of the reaction pressure of the hydrothermal synthesis reaction. Moreover, considering that the increase of the temperature of the hydrothermal synthesis reaction will lead to higher requirements for equipment and higher difficulty in preparing gallium phosphate powder, it can be concluded that the preferred reaction pressure of the hydrothermal synthesis reaction is 4 MPa.

[0210] 7. Comparing Example 1 with Examples 14 and 15, the purity of the gallium phosphate powder prepared in Example 1 is significantly higher than that in Example 14. The purity of the gallium phosphate powder prepared in Example 1 is equal to that of the gallium phosphate powder prepared in Example 15. That is, as the molar ratio of gallium trioxide to phosphoric acid decreases, the purity of the gallium phosphate powder first increases and then remains unchanged. Therefore, it can be seen that the preferred molar ratio of gallium trioxide to phosphoric acid in the hydrothermal synthesis reaction is 1:3.

[0211] The technical solution of the present invention has been described above with reference to the preferred embodiments shown in the accompanying drawings. However, it will be readily understood by those skilled in the art that the scope of protection of the present invention is obviously not limited to these specific embodiments. Without departing from the principles of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after such changes or substitutions will all fall within the scope of protection of the present invention.

Claims

1. A method for preparing a gallium phosphate target, characterized in that, The method for preparing the gallium phosphate target includes the following steps: S1: Gallium phosphate powder is placed into a target mold and sintered to obtain gallium phosphate crystal; S2: The gallium phosphate crystal is placed in a metal can for encapsulation to obtain a gallium phosphate target.

2. The method for preparing gallium phosphate target according to claim 1, characterized in that, The purity of the gallium phosphate powder is not less than 98%.

3. The method for preparing gallium phosphate target according to claim 1, characterized in that, The gallium phosphate powder is prepared by a hydrothermal synthesis reaction of gallium trioxide and phosphoric acid. In the hydrothermal synthesis process, the reaction temperature is 100~180℃ and the reaction pressure is 3~6Mpa.

4. The method for preparing gallium phosphate target according to claim 3, characterized in that, The reaction temperature is 120°C and the reaction pressure is 4 MPa.

5. The method for preparing gallium phosphate target according to claim 3, characterized in that, The molar ratio of gallium trioxide to phosphoric acid is 1:

3.

6. A kind 68 The method for preparing Ge is characterized by, The 68 Ge is prepared using a gallium phosphate target material prepared by any one of claims 1 to 5, wherein the preparation method includes the following steps: T1: The gallium phosphate target is placed in a particle accelerator and irradiated. T2: Dissolve the irradiated gallium phosphate target to obtain a solution containing metal ion impurities. 68 Ge solution; T3: The substance containing metal ion impurities 68 The Ge solution was separated and purified to obtain a solution containing... 68 Ge concentrate.

7. The method according to claim 6 68 The method for preparing Ge is characterized by, The irradiation conditions for irradiating the gallium phosphate target are as follows: The irradiation energy range is 19~28 MeV; And / or, the beam current intensity ranges from 100 to 300 μA.

8. The method according to claim 7 68 The method for preparing Ge is characterized by, The irradiation conditions for irradiating the gallium phosphate target are as follows: The irradiation energy is 28 MeV; And / or, the beam current intensity is 300 μA.

9. The method according to claim 6 68 The method for preparing Ge is characterized by, "Dissolving the irradiated gallium phosphate target yields a solution containing metal ion impurities." 68 The specific steps involved in preparing the "Ge solution" include: T21: Remove the irradiated gallium phosphate target from the metal container and dissolve it in concentrated sulfuric acid to obtain a solution; T22: Adjust the pH of the solution to an HCl concentration of 1.3~1.6M to obtain a solution containing metal ion impurities. 68 Ge solution.

10. The claim 6 68 The method for preparing Ge is characterized by, "The impurities containing metal ions" 68 The Ge solution was separated and purified to obtain a solution containing... 68 The specific steps involved in producing "Ge concentrate" include: T31: The substance containing metal ion impurities 68 The Ge solution is added to the first separation column to remove zinc impurities and collect the effluent; T32: Add sodium citrate and alkaline solution to the effluent, adjust the pH of the effluent to 11.5~13, and then add it to the second separation column; T33: The second separation column is washed sequentially with sodium citrate solution with pH 11.5-13, alkaline solution with pH 11.5-13, and water; T34: The second separation column is eluted with eluent to obtain a solution containing... 68 Ge concentrate; The first separation column comprises at least AG1-X8 resin, and the second separation column comprises at least Sephadex G25 resin.

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