CN103337270A - Method for preparing radionuclide <95m,97m>TC - Google Patents
Method for preparing radionuclide <95m,97m>TC Download PDFInfo
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- CN103337270A CN103337270A CN 201310286362 CN201310286362A CN103337270A CN 103337270 A CN103337270 A CN 103337270A CN 201310286362 CN201310286362 CN 201310286362 CN 201310286362 A CN201310286362 A CN 201310286362A CN 103337270 A CN103337270 A CN 103337270A
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Abstract
The invention discloses a new method for preparing radionuclide <95m,97m>TC. The method is mainly characterized by comprising the steps of dissolving a natural Mo target irradiated by deuteron (d,<2>H) with market H2O2, converting dissolved Mo and TC into Na2MoO4 and Na2TCO4 with NaOH, keeping alkalinity of a solution at 10% approximately, coating a Dowex-1 anion exchange resin column with a Na2MoO4 solution containing <95m,97m>TC, leaching with NaOH at a weight concentration of 9.5-10.5% to remove Mo from the solution firstly, leaching with HC1 of 1.5-2.5mol/L and HNO3 of 2-3mol/L respectively to remove other impurities, and leaching with HNO3 with volume of 5.0-8.0 times of that of the exchange column and the concentration of 7.0-8.0mol/L at last. According to <95m, 97m>TC prepared by the method, the content of Mo detected by a spectrophotometric method is zero; the radionuclide purity of Tc is greater than 99.9%; the radiochemical purity of <95m, 97m>TC is greater than 99.0; the preparation method is simple in operational procedure; an organic extractant is not used; and no secondary pollution is caused to the environment.
Description
Technical field
The present invention relates to the isotope technology field, more specifically, relate to a kind of by deuteron (d,
2H) the natural Mo target of irradiation is produced radioactive nuclide
95m, 97mThe method of Tc.
Background technology
You Yu Technetium does not have stable nuclide and exists, study the geochemistry of technetium, the nuclein migration of technetium (as the long half-lift isotope
99The tracer nuclide) Yi of Tc is Ji the behavior of Technetium in plant and animal, the just necessary radioactive isotope that adopts moderate technetium of half life period.The radioactive isotope of technetium mainly contains
93Tc(T
1/2=43.5m),
95mTc(T
1/2=61d),
96Tc(T
1/2=51.5m),
97mTc(T
1/2=91d),
99mTc(T
1/2=6.02h) etc., wherein,
93Tc,
96Tc and
99mThe half life period of Tc is shorter relatively, has only dozens of minutes to arrive several hours, is not suitable for the geochemistry of technetium, the researching nuclein migration of technetium etc.; And
95mTc and
97mThe half life period of Tc is longer relatively, is respectively 61d and 91d, is suitable for the geochemistry of technetium, the researching nuclein migration of technetium etc.
95m, 97mTc generally produces by accelerator, and bibliographical information mainly contains following 2 kinds of methods: a kind of method be a particle (
4He) bombardment nickel target
93Nb (a, 2n)
95mTc makes
95mTc, this method need adopt enrichment
93Nb, target material cost height, and only the acid mixture of nickel target with concentrated hydrochloric acid and red fuming nitric acid (RFNA) is dissolved in the document, do not carry out the radiochemistry of Tc, Nb and separate.Another kind method be with the 20-22MeV proton (
1H) bombardment Mo target
NatMo (p, xn)
95mTc, radiochemistry is separated the HDEHP extraction of filtration, Mo and impurity of the dissolving comprise the Mo target, molybdic acid and the removal of extractant etc.; Though this method carried out putting divide from, detachment process comparatively complicated, and used organic extractant HDEHP(di-(2-ethylhexyl)phosphoric acid), easily environment is caused secondary pollution.
Produce with accelerator
95m, 97mTc relates to the dissolving of irradiation, irradiation Mo target of preparation, the Mo target of Mo target and Mo and technology such as separates with the radiochemistry of Tc.The wherein preparation of Mo target adopts that generally electrochemical plating, vacuum sputtering, Mo sheet mounting method, Mo plate are directly processed etc.The dissolving of irradiation Mo target mainly contains chloroazotic acid (potpourri of concentrated hydrochloric acid and red fuming nitric acid (RFNA)) dissolution method, red fuming nitric acid (RFNA) or the concentrated sulphuric acid, 10% NaOH(or 1mol/L NaOH) and 30% H
2O
2Solution heating for dissolving method, ammoniacal liquor and 30% H
2O
2Mixed solution dissolution method etc.The concentrated acid dissolution method is operated more loaded down with trivial details owing to need to add a large amount of alkali neutralizing acids; Ammoniacal liquor and 30% H
2O
2The mixed solution dissolution method because dissolving back alkalescence is on the low side, need adds alkali and make solution become strong basicity, operates also more loaded down with trivial details.10% NaOH(or 1mol/L NaOH) and 30% H
2O
2Solution heating for dissolving method, course of dissolution not only need heating, and dissolution velocity inadequately fast, effect is also general.The radiochemistry separation method of Mo is many, and Al is arranged
2O
3Chromatography, anion exchange resins exchange process, Zeo-karb exchange process, Fe (OH)
3Coprecipitation, solvent extraction or several method are used in combination etc.To from a few gram Mo, isolate trace (~ μ g level)
95m, 97mTc, it is very difficult adopting conventional method, does not also reach the requirement of separation and purification.Co-precipitation and solvent extraction complex operation, the recovery of Tc is not high, and easily causes secondary pollution; Al
2O
3The chromatography operation is also more loaded down with trivial details, Al
2O
3Also difficulty of processing, and cause that easily the leakage of Mo is worn etc.Bibliographical information passes through
NatMo (p, xn)
95mTc reacts production
95mTc, its Mo with
95mThe radiochemistry of Tc is separated and has only been listed roughly step, comprises the HDEHP extraction of filtration, Mo and impurity of dissolving, molybdic acid of Mo and the removal of extractant etc., and concrete steps are not described in detail in detail; In addition, though this method carried out putting divide from, detachment process comparatively complicated, and used organic extractant HDEHP(di-(2-ethylhexyl)phosphoric acid) easily environment is caused secondary pollution.Other have bibliographical information with a particle (
4He) bombardment nickel target
93Nb (a, 2n)
95mTc makes
95mTc, this method need adopt enrichment
93Nb, target material cost height, and only the acid mixture of nickel target with concentrated hydrochloric acid and red fuming nitric acid (RFNA) is dissolved in the document, do not carry out the radiochemistry of Tc, Nb and separate.
Summary of the invention
Produce radioactive nuclide at prior art
95m, 97mThe present situation of Tc, purpose of the present invention aim to provide a kind of deuteron (d,
2H) irradiation bombard radionuclide purity that natural Mo target produces Tc greater than 99.9% and
95m, 97mThe radiochemical purity of Tc is greater than 99.0%
95m, 97mThe Tc new method, the lock out operation complexity, the use organic extractant that overcome prior art for preparing cost height, Mo and Tc simultaneously easily cause secondary pollution problems to environment.
At purpose of the present invention, basic skills of the present invention is after first NaOH with q.s gets off Mo drip washing, then to use HCl, HNO again
3The non-materials and a spot of of putting such as the Mo of the trace that drip washing is not got off and Mg, the Mn of trace, Cr, Fe, Si
95Zr,
95,96Nb,
94,95,97,103Radioimpurity radioactive impurity drip washing such as Ru are got off, and needed
95m, 97mTc still stays on the Dowex-1 anion exchange resins, at last with the HNO of the about 7.5mol/L of weight concentration
3Drip washing Na
2 95m, 97mTcO
4Thereby, the HNO of assurance high concentration
3Do not contain other metallic ion and radioimpurity radioactive impurity in the leacheate, the content spectrophotometric method that obtains Mo detect be zero, the radionuclide purity of Tc greater than 99.9%,
95m, 97mThe radiochemical purity of Tc is greater than 99.0% high-purity
95m, 97mTc.
The radioactive nuclide of producing provided by the invention
95m, 97mThe method of Tc mainly may further comprise the steps:
(1) natural Mo target preparation: with the dimensioned Mo target sheet of natural Mo plate according to the accelerator target holder;
(2) Mo target irradiation: with intensity be 150 ~ 155 μ A deuteron (d,
2H) bundle irradiation bombardment Mo target is 28 ~ 33 hours, places behind the irradiation to be no less than 43 days and to enter dissolution process;
(3) irradiation Mo target dissolving: use commercially available H
2O
2Dissolving irradiation Mo target, H
2O
2Consumption by 2.5 ~ 5.0mL/g Mo, fully the dissolving back adds the NaOH of weight concentration 9.5 ~ 10.5 %, with Mo, the T after the dissolving
CConvert Na to
2MoO
4And Na
2T
CO
4, the consumption of NaOH is by 5.0 ~ 8.0mL/g Mo, and the basicity of solution maintains 9.5 ~ 10.5 %;
(4) Mo with
95m, 97mTc separates: contain
95m, 97mT
CNa
2MoO
4Dowex-1 anion-exchange resin column on the solution, detecting to the Mo content spectrophotometric method in the leacheate with the NaOH drip washing of weight concentration 9.5 ~ 10.5 % is zero, removes NaOH with distilled water drip washing; Using 10.0 ~ 12.5 times of exchange column volumes, concentration afterwards respectively is the HCl drip washing of 1.5 ~ 2.5mol/L, and 8.0 ~ 10.0 times of exchange column volumes, concentration are the HNO of 2 ~ 3mol/L
3The non-material and a spot of of putting of Mo, Mg, Mn, Cr, Fe, Si of trace is removed in drip washing
95Zr,
95,96Nb,
94,95,97,103The Ru radioimpurity radioactive impurity; The HNO that to use 5.0 ~ 8.0 times of concentration of exchange column volume at last be 7.0 ~ 8.0mol/L
3Drip washing is contained
95m, 97mThe Na of Tc
2TcO
4Solution;
(5) conversion processing: the resulting solution heating evaporation of step (4) is removed HNO
3, remove remaining HNO with HCl more afterwards
3, the radionuclide purity that obtains Tc at last greater than 99.9%,
95m, 97mThe radiochemical purity of Tc is greater than 99.0% Na
2 95m, 97mTcO
4Solution.
The present invention adopts natural Mo target preparation
95m, 97mTc.Natural Mo target mainly contains
92Mo(14.84%),
94Mo(9.25%),
95Mo(15.92%),
96Mo(16.68%),
97Mo(9.55%),
98Mo(24.13%) and
100Mo(9.63%) etc. isotope also contains elements such as micro Mg, Mn, Cr, Fe, Si in addition, with deuteron (d,
2H) the natural Mo target of irradiation mainly take place (d, 2n), (d n) waits nuclear reaction, and the main coordination that produces Tc have:
93Tc：
?92Mo（d，n）
93Tc，T
1/2=43.5m；
95mTc：
94Mo（d，n）
95mTc，T
1/2=61d；
95Mo（d，2n）
95mTc，T
1/2=61d；
96Tc：
95Mo（d，n）
96Tc，T
1/2=4.28d；
97mTc：
96Mo（d，n）
97mTc，T
1/2=91.4d；
97Mo（d，2n）
97mTc，T
1/2=91.4d
93The half life period of Tc is 43.5m, places behind the irradiation and just decays in 1 day, can not consider its influence;
96The half life period of Tc is 4.28d, places behind the same irradiation and can not consider its influence (radioactive nuclide generally place just think after 10 half life period stable) in 43 days.With deuteron (d,
2H) the natural Mo target of irradiation, after irradiation Mo target was placed 43 days, the isotope of Tc just only needed to pay close attention to target product
95mTc and
97mTc, ensuing problem solve exactly Mo with
95m, 97mThe radiochemistry of Tc is separated.
How the natural Mo target of irradiation is separated through radiochemistry and removes a large amount of Mo(gram magnitudes) and non-material and trace put such as Mg, Mn, Cr, Fe, Si on a small quantity
95Zr,
95,96Nb,
94,95,97,103Radioimpurity radioactive impurities such as Ru, the radionuclide purity that obtains Tc greater than 99.9% and
95m, 97mThe radiochemical purity of Tc is greater than 99.0%
95m, 97mTc is to adopt natural Mo target preparation
95m, 97mThe technological difficulties of Tc.Technique scheme of the present invention has solved this technical matters well, and the preparation method running program is simple, does not use organic extractant, can not cause secondary pollution to environment.
At the above-mentioned radioactive nuclide of producing
95m, 97mT
CScheme in, described Dowex-1 anion exchange resins preferably adopts the Dowex-1 anion exchange resins after handling transition.Described transition Dowex-1 anion exchange resins, refer to Dowex-1 anion exchange resins upper prop after, use distilled water, HCl, distilled water, HNO successively
3, distilled water drip washing, use the NaOH drip washing of weight concentration 9.5 ~ 10.5 % afterwards again, handle through drip washing repeatedly, resin basicity maintains 9.5 ~ 10.5% Dowex-1 anion exchange resins.In Dowex-1 anion exchange resins processing procedure transition, preferably use HCl, distilled water, HNO successively
3, distilled water carries out cycling elution, cycle index is no less than 3 times, it is neutral that drip washing to leacheate is.In the cycling elution process, the rate of flow in rinse of each link is preferably controlled in 0.4 ~ 0.6 mL/min scope.The Dowex-1 resin was preferably handled through cleaning, oven dry, grinding and screening, and is selected for use particle diameter at the Dowex-1 resin of 80 ~ 120 order scopes before last anion-exchange column.
At the above-mentioned radioactive nuclide of producing
95m, 97mT
CScheme in, use commercially available H
2O
2Dissolving irradiation Mo target preferably adopts on a small quantity repeatedly dissolution mechanism, uses commercially available H at least
2O
2Dissolving irradiation Mo target 2 times, H
2O
2The each dissolving of consumption should be in 0.5 ~ 1.0mL/g Mo scope, and total consumption is 2.5 ~ 5.0mL/g Mo; On the irradiation Mo target solution behind the Dowex-1 anion-exchange resin column NaOH of operating weight concentration 9.5 ~ 10.5% carry out drip washing, rate of flow in rinse should be controlled in 0.4 ~ 0.6 mL/min scope.
Highly purified in order to prepare
95m, 97mTc, inventor have improved the dissolving method of Mo.Prepare highly purified
95m, 97mTc, irradiation, the dissolving of irradiation Mo target that relates to preparation, the Mo target of Mo target separates with the radiochemistry of irradiation Mo target etc.In the preparation of Mo target, consider factors such as complexity and cost, compared the quality of several method, the present invention adopts highly purified Mo plate (99.99%) directly to process irradiation Mo target.The dissolving of irradiation Mo target, the inventor finds in experimentation, uses commercially available H separately
2O
2(about 30% H of weight concentration
2O
2) dissolving Mo is than with 10% NaOH(or 1mol/L NaOH) and commercially available H
2O
2The mixed solution dissolution velocity is fast, effective and need not heat, so the present invention has adopted the first commercially available H that uses
2O
2Dissolving Mo, Mo, Tc after back NaOH with weight concentration about 10% will dissolve convert to and separate needed Na
2MoO
4And Na
2TcO
4Pattern.The radiochemistry of irradiation Mo target is separated, in high-purity
95m, 97mBe most important link in the preparation process of Tc, the inventor in the separation method of Mo and Tc, has only adopted Dowex-1 anion exchange resins, and only used NaOH, HCl, HNO in detachment process according to the actual conditions of analysis, simulated experiment
3Deng inorganic reagent drip washing, do not use organic extractant, can not cause secondary pollution to environment, obtain needed microgram magnitude through separation and purification
95m, 97mTc, the content spectrophotometric method of its Mo detect be zero, the radionuclide purity of Tc greater than 99.9%,
95m, 97mThe radiochemical purity of Tc is greater than 99.0%.
Description of drawings
Accompanying drawing 1 is that horizontal ordinate is the sample gamma spectrum figure of number.
Accompanying drawing 2 is sample gamma spectrum figure.
From the gamma spectrum of accompanying drawing 1 and accompanying drawing 2 as can be seen, energy spectrum region has only the feature power spectrum of Tc, does not have the power spectrum of other nucleic, and its radionuclide purity is greater than 99.9%.Wherein, 204keV, 582 keV, 616 keV, 765 keV, 786 keV, 820 keV, 835 keV, 947 keV, 1039 keV, 1073 keV belong to
95mTc; 96.5 keV belongs to
97mTc; 252 keV belong to
105Tc; Illustrate and obtained highly purified containing
95m, 97mThe Na of Tc
2TcO
4Solution.
Embodiment:
1. the preparation of natural Mo target
The highly purified natural Mo plate of buying (99.99%) is processed into the target sheet that meets dimensional requirement according to the requirement of accelerator target holder.Processed 4 natural Mo targets altogether, 1 is used for making simulation test, and 1 is used for
99Tc
mRecovery test, other 2 are used for the irradiation target.
2. the irradiation of Mo target
Employing d nuclear (
2H) irradiation bombards natural Mo target, and " cooling " (namely placed 45 days, in order to allow short-decayed isotope after 45 days
93Tc and
96Decays such as Tc) radiochemistry of carrying out the irradiation target is separated.
Situation such as the table 1 of 2 Mo target sheet irradiation.
The irradiation situation of table 1 Mo target
3. the separation of simulation Mo target
Because irradiation Mo target contains and has hot, should not directly carry out the experiments such as dissolving, separation of irradiation Mo target, so need carry out earlier " cold test " before irradiation Mo target separates carrying out, dissolving, the simulation Mo target of namely simulating the Mo target earlier separate and
99Tc
mRecovery tests etc. are in order to find out method and condition for experiments such as the dissolving of irradiation Mo target, separation.
1) improved dissolving method is adopted in the dissolving of the dissolving Mo of simulation Mo target, namely directly uses 30% H
2O
2Dissolving Mo need not heat in the course of dissolution.
(1) dissolving of Mo sheet
The thick Mo sheet of the heavy 1-5mm of 3g is cut into small pieces (3mm * 3mm), add weight concentration 30% H 5 times by each 0.5mL/g Mo score
2O
2The Mo sheet is dissolved, and course of dissolution does not need heating.Add the NaOH of weight concentration 10% after the dissolving again with the MoO of dissolving
3Convert Na to
2MoO
4, the NaOH use amount, needed whole Na before last Dowex-1 anion-exchange resin column by 8.0mL/g Mo
2MoO
4The basicity of solution maintains about 10%.
(2) dissolving of simulation Mo target
To simulate Mo target sheet and be fixed in the dissolving tank, adopt the method for above-mentioned (1), add weight concentration 30% H 5 times by each 0.5mL/g Mo score
2O
2Simulation Mo target sheet is dissolved, add the NaOH of weight concentration 10% after the dissolving again with the MoO of dissolving
3Convert Na to
2MoO
4, the NaOH use amount is by 8.0mL/g Mo, Na
2MoO
4The basicity of solution maintains about 10%, and the meltage control of Mo is about 6g.
2) Mo separates
As previously mentioned, (100 ± 20 orders, ф 1.0 * 20.0cm) carry out separating of Tc and Mo etc. to adopt Dowex-1 anion exchange resins.
(1) processing of Dowex-1 resin
After the cleaning of Dowex-1 resin, oven dry is ground with muller, uses the molecular sieve sub-sieve again, and it is standby to get 100 ± 20 purpose Dowex-1 resins.
With anion-exchange column on above-mentioned 100 ± 20 purpose Dowex-1 resins.Elder generation is cleaned with distilled water, uses the HCl drip washing 100-150mL of 6mol/L then, and is with distilled water that the HCl flush away is extremely neutral, uses the HNO of 3mol/L again
3Drip washing 100-150mL, with distilled water with HNO
3Flush away is to neutral.Repeat above-mentioned steps 3 times, flow velocity is controlled about 0.5 mL/min.
(2) transition of Dowex-1 resin
With 10% NaOH drip washing, about 500 mL of elution volume maintain about 10% the basicity of Dowex-1 resin with above-mentioned treated Dowex-1 resin.
(3) separation of Mo
The Na that will contain 5.9532g Mo
2MoO
4The Dowex-1 anion-exchange resin column of solution (its basicity is about 10%) after transition used 10% NaOH drip washing then, and flow velocity is controlled about 0.5 mL/min, its elution volume and content such as table 2.The content metric measurement of Mo.
Metric measurement Mo: sample thief is diluted with water to 25mL in 50 mL volumetric flasks, adds 2.5mL HNO
3(HNO
3Drip 0.5% KMnO before using
4Solution is to showing stable light red); The KSCN solution and 2.5mL 10% SnCl that add 5mL 25% again
2Solution shakes up, and is diluted with water to 50mL, places 15min, surveys absorbance in the 430nm place with the 1cm cuvette.
Table 2 10% NaOH elution volume and Mo content
Last table accumulative total Mo total content is 5.8031g, and the recovery is 97.5%.In order to guarantee that as far as possible Dowex-1 anion exchange resins does not contain Mo, at drip washing 1000 mL, absorbance is under 0 the situation, again drip washing 200mL 10% NaOH solution.
After 10% NaOH drip washing is intact, make Dowex-1 anion exchange resins to neutral the NaOH flush away with distilled water, its leacheate absorbance is 0; Use the HCl drip washing 120-150mL of 2mol/L then, its leacheate absorbance is 0; Use the HNO of 3mol/L again
3Drip washing 100-120mL, its leacheate absorbance also is 0; At last with distilled water with HNO
3Flush away to leacheate is neutral, and its leacheate absorbance is 0.HCl leacheate, HNO
3The absorbance of leacheate and distilled water leacheate is 0 all, illustrates that their leacheate does not contain Mo.In addition, HNO
3Leacheate carries out the ICP(inductively coupled plasma after treatment) analyze (detectability ppm level), its content consistent with blank sample (＜0.1ppm), this shows HNO
3It is few that leacheate does not contain the content of Mo or Mo.
Above-mentioned experimental result shows that 10% NaOH solution can be with Na
2MoO
4Fully drip washing is got off, thereby guarantee in drip washing thereafter
95m, 97mDo not contain Na in the Tc sample
2MoO
4By the HCl of 2mol/L and the HNO of 3mol/L
3Drip washing further guarantees not contain Mo and other impurity in the Tc of drip washing thereafter sample.
3)
99Tc
mRecovery test
99Tc
mRecovery test and simulation Mo target in the separation test of Mo identical, unique different be at Na
2MoO
4The Na that adds 7.5mCi on the solution before the anion-exchange column
2 99Tc
mO
4Upper prop again behind the solution.
In the detachment process of simulation Mo target, the HNO of the NaOH through 10%, the HCl of 2mol/L and 3mol/L
3After the drip washing, leacheate does not detect radioactivity, this explanation:
(1) 10% NaOH can not be with Na
2 99Tc
mO
4Drip washing is got off;
(2) HCl of 2mol/L can not be with Na
2 99Tc
mO
4Drip washing is got off;
(3) HNO of 3mol/L
3Can not be with Na
2 99Tc
mO
4Drip washing is got off.
Need to prove the HNO of 3mol/L especially
3Generally most metal ions drip washing from the anion-exchange column can be got off, here earlier with the HNO of low concentration
3The HNO of high concentration is used in (3mol/L) drip washing again
3(7.5mol/L) drip washing Na
2 99Tc
mO
4Thereby, the HNO of assurance high concentration
3Do not contain other metallic ion in the leacheate, obtain highly purified Tc.
At the HNO with 3mol/L
3After drip washing is intact, use the HNO of 7.5mol/L instead
3Drip washing 60-100mL is until Na
2 99Tc
mO
4Drip washing is got off fully.Use the Na of 7.5mCi simultaneously
2 99Tc
mO
4Make object of reference, calculate
99Tc
mThe recovery, its recovery〉99%, detect through ICP, its content consistent with blank sample (＜0.1ppm), the HNO of 7.5mol/L is described
3It is few that leacheate does not contain the content of Mo or Mo, thereby guarantee to obtain highly purified Tc.
4. the separation of irradiation Mo target
The dissolving of irradiation Mo target with separate fully with to simulate the Mo target the same.
1) dissolving of irradiation Mo target
Heavy 120.5g before No. 1 target dissolving, the heavy 117.4g in dissolving back, meltage is 3.1 g; Heavy 122.4g before No. 2 target dissolvings, the heavy 119.4g in dissolving back, meltage is 3.0 g, merges lysate, contains Mo 6.1 g, the about 40mL of volume, control solution basicity is about 10%.
2) separation of irradiation Mo target
With the Dowex-1 anion-exchange resin column after transition on the above-mentioned merging lysate, use 10% NaOH drip washing then, flow velocity is controlled about 0.5 mL/min, and the NaOH elution volume is 1200 mL; Use about 100 mL distilled water drip washing then; Use the HCl drip washing of 150 mL 2mol/L again; Then use the HNO of 120 mL 3mol/L again
3Drip washing; Use the HNO of 7.5mol/L at last
3Drip washing 100mL is contained
95m, 97mThe Na of Tc
2TcO
4Solution.
Contain
95m, 97mThe Na of Tc
2TcO
4HNO is removed in the solution evaporation
3After, add 2 ~ 3 HCl again and remove remaining HNO
3, add 2 mL dissolved in distilled water at last, contained
95m, 97mThe Na of Tc
2TcO
4Solution.The solution that takes a morsel analyses with ply of paper that (developping agent is acetonitrile: water=8:2) carry out
95m, 97mThe radiochemicsl purity of Tc is measured, and its radiochemicsl purity is 99.0%.In addition, the solution that takes a morsel is made the source, surveys gamma spectrum; Its gamma spectrum as depicted in figs. 1 and 2.As can be seen from the figure, energy spectrum region has only the feature power spectrum of Tc, does not have the power spectrum of other nucleic, and its radionuclide purity is greater than 99.9%.Wherein, 204keV, 582 keV, 616 keV, 765 keV, 786 keV, 820 keV, 835 keV, 947 keV, 1039 keV, 1073 keV belong to
95mTc; 96.5 keV belongs to
97mTc; 252 keV belong to
105Tc; Illustrate and obtained highly purified containing
95m, 97mThe Na of Tc
2TcO
4Solution.
Claims (8)
1. produce radioactive nuclide for one kind
95m, 97mT
CMethod, it is characterized in that mainly comprising following process:
(1) natural Mo target preparation: with the dimensioned Mo target sheet of natural Mo plate according to the accelerator target holder;
(2) Mo target irradiation: with intensity be 150 ~ 155 μ A deuteron (d,
2H) bundle irradiation bombardment Mo target is 28 ~ 33 hours, places behind the irradiation to be no less than 43 days and to enter dissolution process;
(3) irradiation Mo target dissolving: use commercially available H
2O
2Dissolving irradiation Mo target, H
2O
2Consumption by 2.5 ~ 5.0mL/g Mo, fully the dissolving back adds the NaOH of weight concentration 9.5 ~ 10.5 %, with Mo, the T after the dissolving
CConvert Na to
2MoO
4And Na
2T
CO
4, the consumption of NaOH is by 5.0 ~ 8.0mL/g Mo, and the basicity of solution maintains 9.5 ~ 10.5 %;
(4) Mo with
95m, 97mTc separates: contain
95m, 97mT
CNa
2MoO
4Dowex-1 anion-exchange resin column on the solution, detecting to the Mo content spectrophotometric method in the leacheate with the NaOH drip washing of weight concentration 9.5 ~ 10.5 % is zero, removes NaOH with distilled water drip washing; Using 10.0 ~ 12.5 times of exchange column volumes, concentration afterwards respectively is the HCl drip washing of 1.5 ~ 2.5mol/L, and 8.0 ~ 10.0 times of exchange column volumes, concentration are the HNO of 2 ~ 3mol/L
3The non-material and a spot of of putting of Mo, Mg, Mn, Cr, Fe, Si of trace is removed in drip washing
95Zr,
95,96Nb,
94,95,97,103The Ru radioimpurity radioactive impurity; The HNO that to use 5.0 ~ 8.0 times of concentration of exchange column volume at last be 7.0 ~ 8.0mol/L
3Drip washing is contained
95m, 97mThe Na of Tc
2TcO
4Solution;
(5) conversion processing: the resulting solution heating evaporation of step (4) is removed HNO
3, remove remaining HNO with HCl more afterwards
3, the radionuclide purity that obtains Tc at last greater than 99.9%,
95m, 97mThe radiochemical purity of Tc is greater than 99.0% Na
2 95m, 97mTcO
4Solution.
2. the radioactive nuclide of producing according to claim 1
95m, 97mT
CMethod, it is characterized in that described Dowex-1 anion-exchange resin column is the Dowex-1 anion-exchange resin column after handling through transition, handle described transition is behind anion-exchange column on the Dowex-1 resin, uses distilled water, HCl, distilled water, HNO successively
3, distilled water drip washing, use the NaOH drip washing of weight concentration 9.5 ~ 10.5 % afterwards again, make the basicity of resin maintain 9.5 ~ 10.5%.
3. the radioactive nuclide of producing according to claim 2
95m, 97mT
CMethod, it is characterized in that the Dowex-1 resin is for through cleaning, oven dry, grinding and screening is handled particle diameter at 80 ~ 120 purpose Dowex-1 resins.
4. the radioactive nuclide of producing according to claim 2
95m, 97mT
CMethod, it is characterized in that on the Dowex-1 resin using HCl, distilled water, HNO successively behind the anion-exchange column
3, the distilled water cycling elution, cycle index is no less than 3 times, and distilled water drip washing to the leacheate in the cycling elution is neutral.
5. the radioactive nuclide of producing according to claim 4
95m, 97mT
CMethod, it is characterized in that using successively HCl, distilled water, HNO
3, distilled water carries out cycling elution, rate of flow in rinse is controlled at 0.4 ~ 0.6 mL/min.
6. according to the described radioactive nuclide of producing of one of claim 1 to 5
95m, 97mT
CMethod, it is characterized in that the commercially available H of irradiation Mo target
2O
2At least dissolve H 2 times
2O
2Each consumption is 0.5 ~ 1.0mL/g Mo, and total consumption is 2.5 ~ 5.0mL/g Mo.
7. according to the described radioactive nuclide of producing of one of claim 1 to 5
95m, 97mT
CMethod, it is characterized in that Dowex-1 anion-exchange resin column on the irradiation Mo target solution with the NaOH drip washing of weight concentration 9.5 ~ 10.5 %, its rate of flow in rinse control is at 0.4 ~ 0.6 mL/min.
8. the radioactive nuclide of producing according to claim 6
95m, 97mT
CMethod, it is characterized in that Dowex-1 anion-exchange resin column on the irradiation Mo target solution with the NaOH drip washing of weight concentration 9.5 ~ 10.5 %, its rate of flow in rinse control is at 0.4 ~ 0.6 mL/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108977859A (en) * | 2018-08-03 | 2018-12-11 | 中国核动力研究设计院 | A method of preparing -63 radioactive source of nickel |
| CN110335697A (en) * | 2019-07-11 | 2019-10-15 | 四川大学 | A kind of high abundance98The preparation method of Tc |
| CN111621645A (en) * | 2020-06-09 | 2020-09-04 | 西安迈斯拓扑科技有限公司 | Irradiation from accelerator100Mo production99mRecovery from Tc process effluent100Method for Mo |
| CN111733339A (en) * | 2020-06-29 | 2020-10-02 | 中国科学院近代物理研究所 | Irradiation enrichment by accelerator100Mo production99mTc method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108977859A (en) * | 2018-08-03 | 2018-12-11 | 中国核动力研究设计院 | A method of preparing -63 radioactive source of nickel |
| CN110335697A (en) * | 2019-07-11 | 2019-10-15 | 四川大学 | A kind of high abundance98The preparation method of Tc |
| CN110335697B (en) * | 2019-07-11 | 2020-09-29 | 四川大学 | High abundance98Tc preparation method |
| CN112885495A (en) * | 2019-11-29 | 2021-06-01 | 艾尔贝姆应用公司 | Method for producing Ac-225 from Ra-226 |
| CN111621645A (en) * | 2020-06-09 | 2020-09-04 | 西安迈斯拓扑科技有限公司 | Irradiation from accelerator100Mo production99mRecovery from Tc process effluent100Method for Mo |
| CN111733339A (en) * | 2020-06-29 | 2020-10-02 | 中国科学院近代物理研究所 | Irradiation enrichment by accelerator100Mo production99mTc method |
| CN111733339B (en) * | 2020-06-29 | 2022-05-17 | 中国科学院近代物理研究所 | Irradiation enrichment by accelerator100Mo production99mTc method |
| CN114121330A (en) * | 2021-11-11 | 2022-03-01 | 中国核动力研究设计院 | Molybdenum-technetium generator, preparation method and device |
| CN114121330B (en) * | 2021-11-11 | 2024-05-14 | 中国核动力研究设计院 | Molybdenum technetium generator, preparation method and device |
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