CN103614577B - Quick preparation method of <239>Np tracer - Google Patents

Quick preparation method of <239>Np tracer Download PDF

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Publication number
CN103614577B
CN103614577B CN201310626323.7A CN201310626323A CN103614577B CN 103614577 B CN103614577 B CN 103614577B CN 201310626323 A CN201310626323 A CN 201310626323A CN 103614577 B CN103614577 B CN 103614577B
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nitric acid
preparation
tracer agent
chromatograph post
chromatograph
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CN103614577A (en
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施燕梅
伊小伟
张海涛
何小兵
李谋
白涛
张佳媚
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Northwest Institute of Nuclear Technology
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Northwest Institute of Nuclear Technology
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    • 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

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Abstract

The invention relates to a quick preparation method of a <239>Np tracer. The invention provides a method for separating <239>Np in <243>Am by using an HDEHP (Di-(2-ethylhexyl)phosphoric acid) extraction resin for the first time by using the characteristic that the HDEHP extraction resin adsorbs the Am (III) but does not adsorb Np (V). Compared with other methods, the method provided by the invention is simple and quick to operate, and does not need to introduce any redox agent in the operational process; the obtained solution system is simple; the preparation and recovery rate of the <239>Np is 90%, and the radiopurity is 99.98%; and the <243>Am can be recycled and reutilized.

Description

A kind of 239the fast preparation method of Np tracer agent
Technical field
The present invention relates in Application of Nuclear Technology field 239the preparation method of Np, is specifically related to require highly purified 239np technology of preparing.
Background technology
Long lived nuclides 237the analysis of Np seems very important in the various fields such as environmental monitoring, nuclear waste disposal.Mass spectrum or ɑ gamma spectrometry 237during Np, need to carry out separation and purification and select suitable tracer agent instruction 237np chemical recovery rate.
? 237in the isotropic substance of Np, be suitable as 237the coordination of Np tracer agent have 239np, 235np, 236np. 236np (T 1/2=1.2 × 10 5a) need to use deuteron bombardment 235u just can obtain, and purification preparation method is complicated; 235np (T 1/2=396d) not easily obtain and purity is not high, generally need use X-ray spectrometry; 239np (T 1/2=2.355d) there is obvious γ characteristic peak, be applicable to adopting gamma spectrometer measure and easily obtain, therefore 239np Chang Zuowei 237np chemical process rate of recovery instruction nucleic.? 237in the analysis of Np, need first to measure with gamma spectrometer 239the content of Np, obtains 237the rate of recovery of Np, then measure with ICP-MS or ɑ spectrometer 237np, finally obtains in sample 237the content of Np.
239the production of Np has two kinds of methods, 239np can be irradiated by pile neutron 238u produces:
In laboratory, parent can be passed through by approach below 243am isolates 239np:
239np is short-life beta emitter (T 1/2=2.355d), and 243am is long lifetime ɑ radiator (T 1/2=7370a).At 10 239after 23.6 days transformation period of Np, this reaches secular equilibrium to mother/daughter body.Adopt 243am produces 239np irradiates than using pile neutron 238u produces 239np is more easy, so laboratory often adopts 243am is separated preparation 239np.Current finding bibliographical information from 243be separated in Am 239np has liquid-liquid extraction, ion-exchange, chromes etc.Liquid-liquid extraction method adopt organic solvent from 243extract in Am 239np, back extraction enters aqueous phase (J.Radioanal.Nucl.Chem. again, Vol.254.No.3 (2002) 527-532), valence state due to Np is wayward in tetravalence, and extraction process is comparatively complicated in addition, so replaced by ion exchange method and chromes in recent years, wherein the most often use TEVA chromes (J.Radioanal.Nucl.Chem., Vol.266, No.1 (2005) 71.74), adopt TEVA resin to adsorb 243in Am 239np, thus realize Am/Np separation, the method also relates to the tetravalence control problem of Np, and because Np is reduced to tetravalence by needs reductive agent, flow process is more complicated, also likely introduces other impurity.
Summary of the invention
The technology of the present invention utilizes HDEHP extration resin Am (III) absorption or not to the characteristic of Np (V), proposes first and utilizes HDEHP extration resin to carry out 243in Am 239the method of the separation of Np, compared with additive method, easy and simple to handle, quick, operating process is without the need to introducing any redox agent, and the solution system of acquisition is simple, in method 239the preparation rate of recovery of Np is 90%, and radioactive purity is 99.98%, use 243the recyclable recycling of Am.
Technical solution of the present invention is:
A kind of 239the fast preparation method of Np tracer agent, draw together following steps:
1) preparation of chromatograph post: chromatograph column packed two-2-ethylhexyl phosphoric acid resin, with 0.1 ~ 0.3mol/L nitric acid dousing more than 24 hours;
2) get a certain amount of 243am, in small beaker, is adjusted to 5ml0.1 ~ 0.3mol/L nitric acid system;
3) by step 2) in nitric acid system solution transfer on chromatograph post, collect effluent liquid;
4) with 5ml0.1 ~ 0.3mol/L nitric acid drip washing chromatograph post, effluent liquid is collected;
5) by step 4) effluent liquid and step 3) effluent liquid merge, obtain 239np tracer agent.
Above-mentioned preparation method also comprises step 6):
With the nitric acid desorb chromatograph post of 20ml1 ~ 3mol/L, collect stripping liquid, recycling.
Above-mentioned two-2-ethylhexyl phosphoric acid resins are 150 ~ 200 orders, containing 50% 2-2-ethylhexyl phosphoric acid.
Above-mentioned chromatograph post is glass column, and chromatograph post specification is
Above-mentioned steps 1) in concentration of nitric acid be 0.1mol/L; Above-mentioned steps 2) in nitric acid pH value be 1, purity is that top grade is pure, and concentration is 0.1mol/L; Above-mentioned steps 4) in concentration of nitric acid be 0.1mol/L; Above-mentioned steps 6) in nitric acid purity be that top grade is pure, concentration is 1mol/L.
The envrionment temperature of above-mentioned preparation method is room temperature.
Advantage of the present invention is:
1, system of the present invention is simple, uses nitric acid system merely, does not introduce other impurity, preparation 239np purity is high.
2, the present invention 239it is fast that Np prepares speed, 243about need within 10 minutes, just can obtain after Am solution transfer upper prop 239np.
3, the present invention is simple to operate, preparation 239do not need to add redox agent during Np and carry out valence state adjustment.
Accompanying drawing explanation
Fig. 1 is 243be separated in Am 239np schema; In figure: (1) is 0.1mol/L nitric acid, (2) are 0.1mol/L nitric acid, and (3) are 1mol/L nitric acid;
Fig. 2 is 243am and 239γ spectrogram during Np secular equilibrium;
Fig. 3 is 239the γ spectrogram of Np solution;
Fig. 4 is 243the γ spectrogram of Am solution.
Embodiment
Separation process of the present invention is shown in Fig. 1, 239the preparation process of Np is as follows:
Get a certain amount of 243am, in small beaker, is adjusted to 5ml0.1mol/L nitric acid system, and solution is transferred on HDEHP extration resin post, collects effluent liquid, should only contain in this liquid 239np; With 5ml0.1mol/L nitric acid drip washing HDEHP extration resin post, collect effluent liquid, with above 239np merges; Use the nitric acid desorb of 20ml1mol/L again, collect stripping liquid, this liquid is 243am; After depositing 23.6d 243am with 239preparation can be continued after Np reaches secular equilibrium 239np tracer agent.
Specifically be divided into five main implementation steps:
1) preparation of chromatograph post: chromatograph column packed resin is HDEHP (two-2-ethylhexyl phosphoric acids) resin, soaks more than 24 hours with 0.1 ~ 0.3mol/L nitric acid (preferred 0.1mol/L nitric acid), for subsequent use.Chromatograph post is glass column, and chromatograph post specification is hDEHP resin is 150 ~ 200 orders, containing 50% 2-2-ethylhexyl phosphoric acid.
2) get a certain amount of 243am is in small beaker, and be adjusted to 5ml0.1 ~ 0.3mol/L nitric acid system (preferred 0.1mol/L nitric acid system), pH value is 1, and gamma spectrometer is measured 243am with 239np mixing solutions spectrogram is shown in Fig. 2.
3) above-mentioned solution is transferred on HDEHP extration resin post, collect effluent liquid, only contain in this liquid 239np, gamma spectrometer is measured 239np spectrogram is shown in Fig. 3.
4) with 5ml0.1 ~ 0.3mol/L nitric acid (preferred 0.1mol/L nitric acid) drip washing HDEHP extration resin post, effluent liquid is collected, with 3) in 239np merges.
5) use the nitric acid of the nitric acid of 20ml1 ~ 3mol/L (preferred 1mol/L) to resolve again, collect stripping liquid, this liquid contains 243am, gamma spectrometer is measured 243am spectrogram is shown in Fig. 4. 243am solution deposit after 23.6d with 239preparation can be continued after Np reaches secular equilibrium 239np tracer agent.
6) 239the radioactive purity method of inspection of Np.Preparation 239np Thin-film Sources, measures and adopts gamma spectrometer to measure, and measuring result is corrected to and is separated the moment 239the specific activity of Np solution, cooling 25d, extremely 239radioactive source totally, is placed on that gamma detector surface measurement do not separate by Np decay 243the activity of Am, due to 243the Am life-span is very long, and namely measuring result thinks what the separation moment introduced 243the amount of Am.Then 243am with 239the activity ratio that Np is being separated the moment is: A am/ A np=0.02%.The radioactive purity of Np is 99.98%.
Aforesaid operations environment is room temperature.

Claims (6)

1. one kind 239the fast preparation method of Np tracer agent, is characterized in that: comprise the following steps:
1) preparation of chromatograph post: chromatograph column packed two-2-ethylhexyl phosphoric acid resin, with 0.1 ~ 0.3mol/L nitric acid dousing more than 24 hours, for subsequent use;
2) get a certain amount of 243am, in small beaker, is adjusted to 5ml0.1 ~ 0.3mol/L nitric acid system;
3) by step 2) in nitric acid system solution transfer on chromatograph post, collect effluent liquid;
4) with 5ml0.1 ~ 0.3mol/L nitric acid drip washing chromatograph post, effluent liquid is collected;
5) by step 4) effluent liquid and step 3) effluent liquid merge, obtain 239np tracer agent.
2. according to claim 1 239the fast preparation method of Np tracer agent, is characterized in that: also comprise step 6):
With the nitric acid desorb chromatograph post of 20ml1 ~ 3mol/L, collect stripping liquid, recycling.
3. according to claim 1 or 2 239the fast preparation method of Np tracer agent, is characterized in that: described two-2-ethylhexyl phosphoric acid resins are 150 ~ 200 orders, containing 50% 2-2-ethylhexyl phosphoric acid.
4. according to claim 1 or 2 239the fast preparation method of Np tracer agent, is characterized in that: described chromatograph post is glass column, and chromatograph post specification is
5. according to claim 1 or 2 239the fast preparation method of Np tracer agent, is characterized in that: the concentration of nitric acid in described step 1) is 0.1mol/L; Described step 2) in nitric acid pH value be 1, purity is that top grade is pure, and concentration is 0.1mol/L; Concentration of nitric acid in described step 4) is 0.1mol/L; Nitric acid purity in described step 6) is that top grade is pure, and concentration is 1mol/L.
6. according to claim 1 or 2 239the fast preparation method of Np tracer agent, is characterized in that: the envrionment temperature of described preparation method is room temperature.
CN201310626323.7A 2013-11-27 2013-11-27 Quick preparation method of <239>Np tracer Expired - Fee Related CN103614577B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB801742A (en) * 1954-05-18 1958-09-17 Atomic Energy Authority Uk Solvent extraction of neptunium
US3687641A (en) * 1971-03-09 1972-08-29 Atomic Energy Commission Separation and recovery of americium from curium and other elements
CN85105352A (en) * 1985-07-13 1987-01-07 清华大学 The method of from radioactive liquid waste, separating actinide
CN1071964A (en) * 1992-12-24 1993-05-12 清华大学 Method without multistage fractionation extraction separation americium of complexing agent and rare earth element
CN201529491U (en) * 2009-03-12 2010-07-21 中国原子能科学研究院 La-142 fast separation system

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB801742A (en) * 1954-05-18 1958-09-17 Atomic Energy Authority Uk Solvent extraction of neptunium
US3687641A (en) * 1971-03-09 1972-08-29 Atomic Energy Commission Separation and recovery of americium from curium and other elements
CN85105352A (en) * 1985-07-13 1987-01-07 清华大学 The method of from radioactive liquid waste, separating actinide
CN1071964A (en) * 1992-12-24 1993-05-12 清华大学 Method without multistage fractionation extraction separation americium of complexing agent and rare earth element
CN201529491U (en) * 2009-03-12 2010-07-21 中国原子能科学研究院 La-142 fast separation system

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
用萃取色层法分离Np(IV),Np(V)和Np(VI);鲍梦熊等;《原子能科学技术》;19860630(第6期);全文 *
萃淋树脂色谱法分离辐照核燃料中的镅钕钐;陈佩贤等;《原子能科学技术》;19890531;第23卷(第3期);第45-49页 *
高放废液中微量Am的放化分析;陈耀中等;《原子能科学技术》;19920531;第26卷(第3期);全文 *

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