WO2010001728A1 - キレート交換樹脂を用いた放射性銅の分離方法 - Google Patents
キレート交換樹脂を用いた放射性銅の分離方法 Download PDFInfo
- Publication number
- WO2010001728A1 WO2010001728A1 PCT/JP2009/061020 JP2009061020W WO2010001728A1 WO 2010001728 A1 WO2010001728 A1 WO 2010001728A1 JP 2009061020 W JP2009061020 W JP 2009061020W WO 2010001728 A1 WO2010001728 A1 WO 2010001728A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- radioactive
- copper
- nickel
- cobalt
- exchange resin
- Prior art date
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Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21G—CONVERSION OF CHEMICAL ELEMENTS; RADIOACTIVE SOURCES
- G21G1/00—Arrangements for converting chemical elements by electromagnetic radiation, corpuscular radiation or particle bombardment, e.g. producing radioactive isotopes
- G21G1/001—Recovery of specific isotopes from irradiated targets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J45/00—Ion-exchange in which a complex or a chelate is formed; Use of material as complex or chelate forming ion-exchangers; Treatment of material for improving the complex or chelate forming ion-exchange properties
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0476—Separation of nickel from cobalt
- C22B23/0484—Separation of nickel from cobalt in acidic type solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1616—Leaching with acyclic or carbocyclic agents of a single type
- C22B3/165—Leaching with acyclic or carbocyclic agents of a single type with organic acids
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21G—CONVERSION OF CHEMICAL ELEMENTS; RADIOACTIVE SOURCES
- G21G1/00—Arrangements for converting chemical elements by electromagnetic radiation, corpuscular radiation or particle bombardment, e.g. producing radioactive isotopes
- G21G1/001—Recovery of specific isotopes from irradiated targets
- G21G2001/0094—Other isotopes not provided for in the groups listed above
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- the present invention relates to a method for separating radioactive copper using a chelate exchange resin.
- Non-Patent Document 1 reports a method of separating radioactive copper by dissolving an irradiated 64 Ni target in concentrated hydrochloric acid and passing the solution through an anion exchange resin.
- Non-Patent Document 2 a Cu-64 manufacturing apparatus using the method of Non-Patent Document 1 is proposed, and it is reported that Cu-64 can be manufactured within 3 hours.
- radioactive radionuclides such as Co-55, Co-56, Co-57, and Co-58 which are by-products are generated together with radioactive copper.
- radioactive cobalt such as Co-55, Co-56, Co-57, and Co-58 which are by-products are generated together with radioactive copper.
- the present invention has been made in view of the circumstances as described above, and an object of the present invention is to provide a method for separating radioactive copper using a chelate exchange resin capable of quickly separating radioactive copper.
- the method for separating radioactive copper using the chelate exchange resin of the present invention is characterized by the following in order to solve the above problems.
- a method for separating radioactive copper from nickel containing radioactive copper and radioactive cobalt wherein nickel containing radioactive copper and radioactive cobalt is dissolved in an acidic solution and passed through a chelate exchange resin packed column, nickel, After retaining radioactive copper and radioactive cobalt in the chelate exchange resin, an acidic solution is passed through the chelate exchange resin packed column to elute nickel and radioactive cobalt, and then to the chelate exchange resin packed column after elution of nickel and radioactive cobalt. Radioactive copper is eluted by passing an acidic solution having a concentration higher than that of the acidic solution.
- an acidic solution for dissolving nickel containing radioactive copper and radioactive cobalt and an acidic solution for eluting nickel and radioactive cobalt are 0.25 to 0.06 mol / L hydrochloric acid or nitric acid, or 0.12 to 0.03 mol / L sulfuric acid.
- the acidic solution for eluting radioactive copper after eluting nickel and radioactive cobalt is hydrochloric acid or nitric acid having a concentration of 0.5 mol / L or more, or sulfuric acid having a concentration of 0.25 mol / L or more.
- FIG. 1 is a flowchart showing a process of separating radioactive copper using a chelate exchange resin.
- FIG. 2 is a schematic view of a separation apparatus for radioactive copper using a chelate exchange resin.
- FIG. 3A is a perspective view of a heating container in the separation apparatus of FIG. 2, and
- FIG. 3B is a perspective view of the container.
- the present invention has the characteristics as described above.
- chelate exchange resins include concentration and recovery of trace metals contained in rivers and seawater, removal of trace metals contained in analytical solvents, and the like. Copper is often used for concentration, recovery, or removal from the sample because it is retained in the chelate exchange resin under any acidic, neutral, or basic conditions, but it is often used for transition metals such as cobalt and nickel.
- transition metals such as cobalt and nickel.
- Patent Document 1 and Non-Patent Document 1 a method of separating radioactive copper by dissolving irradiated 64 Ni target in concentrated hydrochloric acid and passing the solution through an anion exchange resin.
- radioactive cobalt is also generated in the irradiated 64 Ni target
- Non-Patent Document 3 reports that it is difficult to separate radioactive cobalt and radioactive copper.
- the present inventors have intensively studied for realizing separation of radioactive copper from nickel containing radioactive copper and radioactive cobalt, and have completed the present invention by paying attention to a chelate exchange resin. . The best mode for carrying out the present invention will be described below.
- FIG. 1 is a flowchart showing a process of separating radioactive copper using a chelate exchange resin.
- FIG. 1 is a flowchart showing a process of separating radioactive copper using a chelate exchange resin.
- step A in FIG. 1 in addition to an acidic solution, it dissolves in nickel containing radioactive cobalt and radioactive copper.
- radioactive cobalt is a radioisotope of cobalt such as Co-55, Co-56, Co-57, and Co-58
- radioactive copper is Cu-60, Cu-61, Cu-62, Cu It is a radioactive isotope of copper such as ⁇ 64 and Cu-67.
- Nickel containing radioactive cobalt and radioactive copper was produced by, for example, irradiating protons, deuterons, or alpha (helium) particles accelerated using a stable isotope of nickel as a target material to produce radioactive copper and radioactive cobalt.
- nickel chloride obtained by evaporating to dryness by dissolving the target material that produced this radioactive copper and radioactive cobalt in hydrochloric acid containing hydrogen peroxide, or nitric acid obtained by using nitric acid or sulfuric acid instead of hydrochloric acid examples include nickel and nickel sulfate.
- the target material Ni metal electrodeposited or NiO can be used.
- the acidic solution for dissolving nickel containing radioactive cobalt and radioactive copper is, for example, 0.25 to 0.06 mol / L, more preferably 0.2 to 0.08 mol / L, and particularly 0.15 to 0.1 mol / L.
- L hydrochloric acid or nitric acid, or 0.12 to 0.03 mol / L, more preferably 0.1 to 0.04 mol / L, particularly 0.07 to 0.05 mol / L sulfuric acid can be used.
- nickel, radioactive copper, and radioactive cobalt are retained in the chelate exchange resin in Step B described later, and in particular, radioactive copper can be preferentially retained.
- hydrochloric acid or nitric acid with a concentration higher than 0.25 mol / L is not preferable because copper may be eluted together with nickel and radioactive cobalt.
- nickel and radioactive cobalt may not elute while being held in the chelate exchange resin packed column described later.
- the concentration range of hydrochloric acid and nitric acid is preferably 0.25 to 0.06 mol / L.
- the sulfuric acid concentration range is preferably 0.12 to 0.03 mol / L.
- the combination of radioactive cobalt and nickel containing radioactive copper and an acidic solution for dissolving the same is not particularly limited, but in order to more effectively separate radioactive copper, the solubility of nickel containing radioactive cobalt and radioactive copper is high. It is preferable to dissolve in an acidic solution, and examples of preferable combinations include nickel chloride and hydrochloric acid, nickel nitrate and nitric acid, and nickel sulfate and sulfuric acid.
- nickel containing radioactive cobalt and radioactive copper is dissolved in a small amount of acidic solution, for example, 0.5 to 2 mL of acidic solution.
- step B the solution obtained by dissolving nickel containing radioactive cobalt and radioactive copper in step A in an acidic solution is contacted (charged) with a chelate exchange resin packed in a column.
- the lysate charged in the column in this step is a lysate using 0.5 to 2 mL of acidic solution as described above, and its volume is small so that it exists in the column.
- nickel, radioactive copper, and radioactive cobalt are effectively adsorbed and held by the chelate exchange resin.
- the chelate exchange resin may be any chelate resin that can adsorb nickel, radioactive copper, and radioactive cobalt.
- Such chelate exchange resins are used to concentrate and collect trace amounts of nickel, copper, and cobalt contained in environmental samples such as food digests, river water, and seawater. What has been used for the removal of cobalt can be used, and only copper can be selectively captured and eluted by changing the pH of the solution.
- Specific examples include coordination capable of forming chelates with nickel, radioactive copper and radioactive cobalt on styrene-based polymer resins (matrix) such as styrene-divinylbenzene copolymer and acrylic acid ester-based polymers such as methacrylate polymers. Examples thereof include resins and solid phase fillers in which aminocarboxylic acids such as iminodiacetic acid and ethylenediaminetriacetic acid are introduced as groups.
- step C an acidic solution is passed through a chelate exchange resin packed column in which nickel, radioactive copper and radioactive cobalt are retained. As a result, only nickel and radioactive cobalt are eluted.
- the acidic solution used here preferably has a low concentration.
- L sulfuric acid can be used.
- hydrochloric acid or nitric acid with a concentration higher than 0.25 mol / L is not preferable because copper may be eluted together with nickel and radioactive cobalt.
- nickel and radioactive cobalt may not elute while being held in the chelate exchange resin packed column described later.
- the concentration range of hydrochloric acid and nitric acid is preferably 0.25 to 0.06 mol / L.
- the sulfuric acid concentration range is preferably 0.12 to 0.03 mol / L.
- step D a highly concentrated acidic solution is passed through a chelate exchange resin packed column after elution of nickel and radioactive cobalt. As a result, the radioactive copper retained in the chelate exchange resin is eluted.
- the acidic solution used in step D uses an acidic solution having a higher concentration than the acidic solution used in step A and step C. For example, hydrochloric acid or nitric acid having a concentration of 0.5 mol / L or more, or sulfuric acid having a concentration of 0.25 mol / L or more can be used.
- hydrochloric acid or nitric acid having a concentration of less than 0.5 mol / L it is not preferable because radioactive copper is retained in the column and does not elute.
- sulfuric acid having a concentration of less than 0.25 mol / L it is not preferable to use sulfuric acid having a concentration of less than 0.25 mol / L.
- the upper limit value is not particularly limited, and may be any available value that does not affect the apparatus.
- FIG. 2 is a schematic diagram of a separation apparatus for radioactive copper using a chelate exchange resin.
- the heating container 3 is made of quartz.
- the heating device 1 has a cavity that matches the shape of the heating container 3 so that it can be heated efficiently.
- the lid 14 (cap portion) is a combination of a perforated cap 14a and a butyl septum 14b, and a liquid feeding tube 15 such as a syringe or PEEK tube can be directly inserted into the butyl septum 14b. Without opening the bottle, liquid feeding by pressure feeding and evaporation to dryness by decompression can be performed.
- the heating controller 2 controlled the heating temperature of the heating device 1 to heat the heating container 3 to 150 ° C. or higher, and the heating was continued until 64 NiO charged into the heating container 3 was completely dissolved. After 64 NiO was completely dissolved, the heating vessel 3 was heated to 200 ° C. or higher with the heating device 1 to evaporate the 64 NiO solution. The evaporated acid is trapped by the acid capturing unit 8 made of a basic substance such as soda lime so that the acid does not leak outside.
- the solid phase extraction column 6b is for removing a chelate site (organic compound) that is considered to be eluted under acidic conditions.
- the chelate site is concerned at acting as an inhibitor in the synthesis of radioactive copper-labeled drugs, and therefore needs to be removed at this stage.
- hydrochloric acid solution After passing the hydrochloric acid solution through the separation unit 6, 0.1 mol / L hydrochloric acid is pumped through the solvent storage tank 4 b through the three-way valves 9, 10 to elute nickel and radioactive cobalt. did. The eluate of nickel and radioactive cobalt is returned to the heating container 3 by pressure feeding via the three-way valves 12 and 11.
- the container 5 has the same configuration as the heating container 3 except that the bottom does not have a V shape.
- the high-purity radioactive copper can be separated in about 2 hours by the separation apparatus of FIG. It was also confirmed that a small-scale separation device can be used.
- Example 2 Adsorption and elution of nickel, radioactive cobalt, and radioactive copper on a chelate exchange resin packed column were examined using various concentrations of hydrochloric acid. The same chelate exchange resin packed column as in Example 1 was used.
- hydrochloric acid was prepared in six concentrations of 0.01 M, 0.03 M, 0.06 M, 0.1 M, 0.15 M, and 0.25 ⁇ ⁇ M containing nickel, radioactive cobalt, and radioactive copper.
- the elution rate (fraction radioactivity / total radioactivity x 100) and the residual rate on the column were calculated.
- the experimental results for each element are shown in Tables 1 and 2.
- the numerical value on the right side of the “column” column in the table is the residual ratio (%) of the element in the column.
- the concentration range of hydrochloric acid in which most of nickel and radioactive cobalt are eluted and hardly remains in the column that is, the concentration range of hydrochloric acid suitable for selective separation of nickel and radioactive cobalt is 0.06 to 0.25%. M was confirmed. However, at or near 0.25M, radioactive copper also elutes almost simultaneously with nickel and radioactive cobalt, which may reduce the separation efficiency of radioactive copper. Therefore, it was confirmed that the concentration of hydrochloric acid for eluting nickel and radioactive cobalt is preferably 0.06 to 0.15 M, and most preferably 0.1 M. It was confirmed that the concentration of hydrochloric acid for eluting radioactive copper was preferably 0.5 M or more.
- the preferred concentration conditions when nitric acid is used instead of hydrochloric acid are the same as the above-mentioned hydrochloric acid concentration conditions.
- the concentration for eluting nickel and radioactive cobalt is preferably 0.025 to 0.075 mm, most preferably 0.05 to elute radioactive copper.
- the concentration for this is preferably 0.25M or more.
- high-purity Cu-60, Cu-61, Cu-62, Cu-64, Cu-67, and other radioactive copper can be separated in about 2 hours. Become. Further, by utilizing the present invention, a small-scale separation device can be obtained, and the installation restriction in the cell for shielding radiation is further relaxed, which is effective in preventing exposure of workers engaged in the production of radioactive copper. is there.
- radioactive copper is a radioisotope that is widely used in the medical field such as diagnostic imaging and treatment, it is also useful as a plant research tracer, so it is expected to be used in medical settings and RI manufacturing facilities.
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Abstract
Description
図2は、キレート交換樹脂を用いた放射性銅の分離装置の模式図である。
<実施例2>
種々の濃度の塩酸を用いて、キレート交換樹脂充填カラムへのニッケル、放射性コバルト、放射性銅の吸着及び溶出について検討した。キレート交換樹脂充填カラムは、実施例1と同じものを使用した。
Claims (3)
- 放射性銅と放射性コバルトを含むニッケルから放射性銅を分離する方法であって、放射性銅と放射性コバルトを含むニッケルを酸性溶液に溶解してキレート交換樹脂充填カラムに通液してニッケル、放射性銅及び放射性コバルトをキレート交換樹脂に保持した後、このキレート交換樹脂充填カラムに酸性溶液を通液してニッケル及び放射性コバルトを溶出し、次いでニッケル及び放射性コバルト溶出後のキレート交換樹脂充填カラムに前記酸性溶液よりも高濃度の酸性溶液を通液して放射性銅を溶出することを特徴とするキレート交換樹脂を用いた放射性銅の分離方法。
- 放射性銅と放射性コバルトを含むニッケルを溶解する酸性溶液、及び、ニッケル及び放射性コバルトを溶出する酸性溶液は、0.25~0.06mol/Lの塩酸もしくは硝酸、又は0.12~0.03mol/Lの硫酸であることを特徴とする請求項1に記載のキレート交換樹脂を用いた放射性銅の分離方法。
- ニッケル及び放射性コバルトを溶出後に放射性銅を溶出する酸性溶液は、0.5mol/L以上の濃度の塩酸もしくは硝酸、又は0.25mol/L以上の濃度の硫酸であることを特徴とする請求項1に記載のキレート交換樹脂を用いた放射性銅の分離方法。
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2010518984A JP4877863B2 (ja) | 2008-06-30 | 2009-06-17 | キレート交換樹脂を用いた放射性銅の分離方法 |
US13/001,861 US8647595B2 (en) | 2008-06-30 | 2009-06-17 | Method for separating radioactive copper using chelating-ion exchange resin |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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JP2008-171032 | 2008-06-30 | ||
JP2008171032 | 2008-06-30 |
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WO2010001728A1 true WO2010001728A1 (ja) | 2010-01-07 |
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PCT/JP2009/061020 WO2010001728A1 (ja) | 2008-06-30 | 2009-06-17 | キレート交換樹脂を用いた放射性銅の分離方法 |
Country Status (3)
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US (1) | US8647595B2 (ja) |
JP (1) | JP4877863B2 (ja) |
WO (1) | WO2010001728A1 (ja) |
Cited By (1)
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JP2013530384A (ja) * | 2010-04-30 | 2013-07-25 | アルゲッタ エイエスエイ | 同位体の製造方法 |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US8802041B1 (en) * | 2014-01-24 | 2014-08-12 | Toxco, Inc. | Decontamination of radioactive metals |
EP4208625A1 (en) | 2020-09-03 | 2023-07-12 | Curium US LLC | Purification process for the preparation of non-carrier added copper-64 |
CN113413928B (zh) * | 2021-06-23 | 2023-04-21 | 中国核动力研究设计院 | 一种镍-63自动化分离装置及其分离工艺 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6065004A (ja) * | 1983-09-20 | 1985-04-13 | Hiroaki Egawa | キレ−ト樹脂及びその製造法 |
JPS61283605A (ja) * | 1985-06-10 | 1986-12-13 | Hiroaki Egawa | キレ−ト樹脂及びその製法 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS52106099A (en) | 1976-03-03 | 1977-09-06 | Hitachi Ltd | Treating method of radioactive resin waste |
JPH0247699A (ja) | 1988-08-09 | 1990-02-16 | Yuichi Murakami | 音声による文字入力装置 |
-
2009
- 2009-06-17 WO PCT/JP2009/061020 patent/WO2010001728A1/ja active Application Filing
- 2009-06-17 US US13/001,861 patent/US8647595B2/en not_active Expired - Fee Related
- 2009-06-17 JP JP2010518984A patent/JP4877863B2/ja not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6065004A (ja) * | 1983-09-20 | 1985-04-13 | Hiroaki Egawa | キレ−ト樹脂及びその製造法 |
JPS61283605A (ja) * | 1985-06-10 | 1986-12-13 | Hiroaki Egawa | キレ−ト樹脂及びその製法 |
Non-Patent Citations (1)
Title |
---|
XIAOLIN HOU ET AL.: "Separation of no-carrier- added Cu from a proton irradiated 64Ni enriched nickel target", APPLIED RADIATION AND ISOTOPES, vol. 57, 2002, pages 773 - 777 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2013530384A (ja) * | 2010-04-30 | 2013-07-25 | アルゲッタ エイエスエイ | 同位体の製造方法 |
Also Published As
Publication number | Publication date |
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JPWO2010001728A1 (ja) | 2011-12-15 |
US20110142735A1 (en) | 2011-06-16 |
JP4877863B2 (ja) | 2012-02-15 |
US8647595B2 (en) | 2014-02-11 |
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