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CN108152112A - Pu in a kind of low-activity sample,241Am and90The method of Sr separation determinations - Google Patents

Pu in a kind of low-activity sample,241Am and90The method of Sr separation determinations Download PDF

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Publication number
CN108152112A
CN108152112A CN201711363870.5A CN201711363870A CN108152112A CN 108152112 A CN108152112 A CN 108152112A CN 201711363870 A CN201711363870 A CN 201711363870A CN 108152112 A CN108152112 A CN 108152112A
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sample
columns
separation
low
teva
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靳小军
孔雪艳
韩雪梅
刘燕
夏峰林
乔淑霞
徐丽霞
陈静
陈文若
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404 Co Ltd China National Nuclear Corp
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404 Co Ltd China National Nuclear Corp
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/405Concentrating samples by adsorption or absorption
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01TMEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/36Measuring spectral distribution of X-rays or of nuclear radiation spectrometry
    • G01T1/363Measuring spectral distribution of X-rays or of nuclear radiation spectrometry with Cerenkov detectors

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  • High Energy & Nuclear Physics (AREA)
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Abstract

The present invention relates in a kind of low-activity sample238‑240Pu、241Am and90The method of Sr separation determinations, includes the following steps:1) sample pretreatment;2)238‑240Pu、241Am and90After Sr separation and concentrations add in ascorbic acid in the lysate obtained by step 1), the valence state of plutonium is adjusted to tetravalence by sodium nitrite, by TEVA, TRU and SR crosscurrent extraction chromatograph resin column, flow velocity 1mL~1.2mL/min is kept;At this point,238‑240Pu will be attracted on TEVA columns,241Am is attracted on TRU columns,90Sr is attracted on SR columns;With on the hydrochloric acid solution elution TEVA columns of 20mL~25mL 0.02mol/L238‑240Pu, on the hydrochloric acid solution elution TRU columns of 15mL~20mL 3.0mol/L241Am, on 15mL~20mL 0.01mol/L salpeter solutions elution SR columns90Sr;3)238‑240Pu、241Am and90Sr is measured,238‑240Pu、241Am leacheates prepare α sources using cerium fluoride microdeposit method, in being measured on alpha energy spectrum;90Sr leacheates are placed 14d and are treated90Sr‑90Cherenkov's counting method measures after Y balances.Using this analysis method, can complete Pu in sample,241Am and90The separation and concentration of Sr, shortening Pu,241Am and90The analytical cycle of Sr.

Description

Pu in a kind of low-activity sample,241Am and90The method of Sr separation determinations
Technical field
The invention belongs to the elimination of nuclear facilities and disposal of three wastes technical field of research, and in particular in a kind of low-activity sample Pu、241Am and90The method of Sr separation determinations.
Background technology
Analysis sample size is big in the elimination of nuclear facilities and disposal of three wastes project, and analysis project is more, and radioactive level height is not One, analytical cycle is tight, will face the problems such as processing sample size big, analytical cycle is long, personnel's radioactive dose height.
At present Pu,241Am、90Tri- analysis methods of Sr can only be with reference to environment grade sample analysis standard, and three analytical standards are each From independence, sample pretreatment, separation condition etc. are different so that analytical cycle is long, can not meet the elimination of nuclear facilities and the three wastes are controlled Manage a large amount of sample analysis demands.Using TEVA, TRU, SR crosscurrent extraction chromatograph column can realize Pu in sample,241Am and90The one of Sr Secondary separation and measure, this method have the characteristics that separation is simple, easily operated.
Invention content
It is an object of the invention to:Realize low-activity sample in Pu,241Am and90The method of the separation determination of Sr.
Technical scheme is as follows:
In a kind of low-activity sample238-240Pu、241Am and90The method of Sr separation determinations, includes the following steps:
1) sample pretreatment
Solid sample:25g~50g samples are weighed, 100mL~200mL salpeter solutions is added in, leaches at a certain temperature 4h;Leaching liquid is collected in centrifugation, and solid residue is washed with 50mL~100mL salpeter solutions, merges solution, and it is 2 to adjust pH, is obtained Solid sample sample;
Fluid sample:200mL~500mL waters sample solution is pipetted in 1000mL beakers, it is 2 or so to adjust pH, Heating is concentrated into 200mL on electric hot plate, obtains fluid sample sample;
In solid sample sample or fluid sample sample, 1mL 1.25mol/L Ca (NO are sequentially added3)2Solution, 2~3 Drip (the NH of phenolphthalein indicator, 5mL 3.2mol/L4)2HPO4, and stir evenly, it is slowly added dropwise into dense NH4OH makes solution become light Pink colour forms Ca at this time3(PO4)2Precipitation, centrifuges 10min under 2000r/min, discards clear liquid;Precipitation 20mL~25mL 3.0mol/L HNO3+0.1mol/L Al(NO3)3Dissolving obtains lysate;
2)238-240Pu、241Am and90Sr separation and concentrations
After the valence state of plutonium is adjusted to tetravalence by addition ascorbic acid, sodium nitrite in the lysate obtained by step 1), lead to TEVA, TRU and SR crosscurrent extraction chromatograph resin column are crossed, keeps flow velocity 1mL~1.2mL/min;At this point,238-240Pu will be adsorbed On TEVA columns,241Am is attracted on TRU columns,90Sr is attracted on SR columns;
With on the hydrochloric acid solution elution TEVA columns of 20mL~25mL 0.02mol/L238-240Pu, with 15mL~20mL On the hydrochloric acid solution elution TRU columns of 3.0mol/L241Am, on 15mL~20mL 0.01mol/L salpeter solutions elution SR columns 's90Sr;
3)238-240Pu、241Am and90Sr is measured
238-240Pu、241Am leacheates prepare α sources using cerium fluoride microdeposit method, in being measured on alpha energy spectrum;
90Sr leacheates are placed 14d and are treated90Sr-90Cherenkov's counting method measures after Y balances.
The detailed process that cerium fluoride microdeposit method described in step 3) prepares α sources is:238-240Pu and241The leacheate of Am In, it is separately added into 0.1mL 0.5mg/mL cerium carrier solutions (Ce3+), the dense HF of 1.0mL are uniformly mixed, and place more than 30min, in 0.1 μm of aperture, a diameter of 25mm polypropylene material filter paper on filtered, filter paper with solid gum is attached to α stainless steels after drying On shallow bid.
Alpha energy spectrum described in step 3) measures238-240Energy selection 5.11MeV~5.50MeV of Pu.
Alpha energy spectrum described in step 3) measures241Energy selection 5.38MeV~5.54MeV of Am.
The leaching temperature of solid sample described in step 1) is 75 DEG C~85 DEG C.
Volume 1 of the salpeter solution for concentrated nitric acid and water described in step 1):1 is formulated.
The remarkable result of the present invention is:Using this analysis method, it can be achieved that a upper prop, you can complete Pu in sample 、241Am and90The separation and concentration of Sr, shortening Pu,241Am and90The analytical cycle of Sr.With can batch processing, input personnel it is few, point Analyse the advantages such as the period is short.
The analysis method to Pu,241Am、90Sr methods high income, detection limit are low, can meet the elimination of nuclear facilities and administer work Pu in low in journey project, extremely low level radioactive pollution sample,241Am and90The analysis of Sr measures.
Description of the drawings
Fig. 1 be a kind of low-activity sample of the present invention in Pu,241Am and90The method flow diagram of Sr separation determinations.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment to Pu in a kind of low-activity sample of the present invention,241Am and90Sr The method of separation determination is described in further detail.
As shown in Figure 1, in a kind of low-activity sample238-240Pu、241Am and90The method of Sr separation determinations, including following Step:
1) sample pretreatment
Solid sample:25g~50g samples are weighed, 100mL~200mL salpeter solutions is added in, leaches at a certain temperature 4h;Leaching liquid is collected in centrifugation, and solid residue is washed with 50mL~100mL salpeter solutions, merges solution, and it is 2 to adjust pH, is obtained Solid sample sample;
Fluid sample:200mL~500mL waters sample solution is pipetted in 1000mL beakers, it is 2 or so to adjust pH, Heating is concentrated into 200mL on electric hot plate, obtains fluid sample sample;
In solid sample sample or fluid sample sample, 1mL 1.25mol/L Ca (NO are sequentially added3)2Solution, 2~3 Drip (the NH of phenolphthalein indicator, 5mL 3.2mol/L4)2HPO4, and stir evenly, it is slowly added dropwise into dense NH4OH makes solution become light Pink colour forms Ca at this time3(PO4)2Precipitation, centrifuges 10min under 2000r/min, discards clear liquid;Precipitation 20mL~25mL 3.0mol/L HNO3+0.1mol/L Al(NO3)3Dissolving obtains lysate;
2)238-240Pu、241Am and90Sr separation and concentrations
After the valence state of plutonium is adjusted to tetravalence by addition ascorbic acid, sodium nitrite in the lysate obtained by step 1), lead to TEVA, TRU and SR crosscurrent extraction chromatograph resin column are crossed, keeps flow velocity 1mL~1.2mL/min;At this point,238-240Pu will be adsorbed On TEVA columns,241Am is attracted on TRU columns,90Sr is attracted on SR columns;
With on the hydrochloric acid solution elution TEVA columns of 20mL~25mL 0.02mol/L238-240Pu, with 15mL~20mL On the hydrochloric acid solution elution TRU columns of 3.0mol/L241Am, on 15mL~20mL0.01mol/L salpeter solutions elution SR columns 's90Sr;
3)238-240Pu、241Am and90Sr is measured
238-240Pu、241Am leacheates prepare α sources using cerium fluoride microdeposit method, in being measured on alpha energy spectrum;
90Sr leacheates are placed 14d and are treated90Sr-90Cherenkov's counting method measures after Y balances.
The detailed process that cerium fluoride microdeposit method described in step 3) prepares α sources is:238-240Pu and241The leacheate of Am In, it is separately added into 0.1mL 0.5mg/mL cerium carrier solutions (Ce3+), the dense HF of 1.0mL are uniformly mixed, and place more than 30min, in 0.1 μm of aperture, a diameter of 25mm polypropylene material filter paper on filtered, filter paper with solid gum is attached to α stainless steels after drying On shallow bid.
Alpha energy spectrum described in step 3) measures238-240Energy selection 5.11MeV~5.50MeV of Pu.
Alpha energy spectrum described in step 3) measures241Energy selection 5.38MeV~5.54MeV of Am.
The leaching temperature of solid sample described in step 1) is 75 DEG C~85 DEG C.
Volume 1 of the salpeter solution for concentrated nitric acid and water described in step 1):1 is formulated.

Claims (6)

1. in a kind of low-activity sample238-240Pu、241Am and90The method of Sr separation determinations, which is characterized in that including following step Suddenly:
1) sample pretreatment
Solid sample:25g~50g samples are weighed, 100mL~200mL salpeter solutions is added in, leaches 4h at a certain temperature;From The heart collects leaching liquid, and solid residue is washed with 50mL~100mL salpeter solutions, merges solution, and it is 2 to adjust pH, obtains solid-like Product sample;
Fluid sample:200mL~500mL waters sample solution is pipetted in 1000mL beakers, it is 2 or so to adjust pH, in electric heating Heating is concentrated into 200mL on plate, obtains fluid sample sample;
In solid sample sample or fluid sample sample, 1mL 1.25mol/L Ca (NO are sequentially added3)2Solution, 2~3 drop phenol (the NH of phthalein indicator, 5mL 3.2mol/L4)2HPO4, and stir evenly, it is slowly added dropwise into dense NH4OH makes solution become light powder Color forms Ca at this time3(PO4)2Precipitation, centrifuges 10min under 2000r/min, discards clear liquid;Precipitation 20mL~25mL 3.0mol/L HNO3+0.1mol/L Al(NO3)3Dissolving obtains lysate;
2)238-240Pu、241Am and90Sr separation and concentrations
After the valence state of plutonium is adjusted to tetravalence by addition ascorbic acid, sodium nitrite in the lysate obtained by step 1), pass through TEVA, TRU and SR crosscurrent extraction chromatograph resin column keep flow velocity 1mL~1.2mL/min;At this point,238-240Pu will be attracted to On TEVA columns,241Am is attracted on TRU columns,90Sr is attracted on SR columns;
With on the hydrochloric acid solution elution TEVA columns of 20mL~25mL 0.02mol/L238-240Pu, with 15mL~20mL 3.0mol/ On the hydrochloric acid solution elution TRU columns of L241Am, on 15mL~20mL 0.01mol/L salpeter solutions elution SR columns90Sr;
3)238-240Pu、241Am and90Sr is measured
238-240Pu、241Am leacheates prepare α sources using cerium fluoride microdeposit method, in being measured on alpha energy spectrum;
90Sr leacheates are placed 14d and are treated90Sr-90Cherenkov's counting method measures after Y balances.
2. in a kind of low-activity sample as described in claim 1238-240Pu、241Am and90The method of Sr separation determinations, it is special Sign is:
The detailed process that cerium fluoride microdeposit method described in step 3) prepares α sources is:238-240Pu and241In the leacheate of Am, respectively Add in 0.1mL 0.5mg/mL cerium carrier solutions (Ce3+), the dense HF of 1.0mL are uniformly mixed, and more than 30min are placed, in 0.1 μ of aperture M, it is filtered on the polypropylene material filter paper of a diameter of 25mm, filter paper is attached to solid gum on α stainless steel shallow bids after drying.
3. in a kind of low-activity sample as described in claim 1238-240Pu、241Am and90The method of Sr separation determinations, it is special Sign is:Alpha energy spectrum described in step 3) measures238-240Energy selection 5.11MeV~5.50MeV of Pu.
4. in a kind of low-activity sample as described in claim 1238-240Pu、241Am and90The method of Sr separation determinations, it is special Sign is:Alpha energy spectrum described in step 3) measures241Energy selection 5.38MeV~5.54MeV of Am.
5. in a kind of low-activity sample as described in claim 1238-240Pu、241Am and90The method of Sr separation determinations, it is special Sign is:The leaching temperature of solid sample described in step 1) is 75 DEG C~85 DEG C.
6. in a kind of low-activity sample as described in claim 1238-240Pu、241Am and90The method of Sr separation determinations, it is special Sign is:Volume 1 of the salpeter solution for concentrated nitric acid and water described in step 1):1 is formulated.
CN201711363870.5A 2017-12-18 2017-12-18 Pu in a kind of low-activity sample,241Am and90The method of Sr separation determinations Pending CN108152112A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109239760A (en) * 2018-08-22 2019-01-18 北京航空航天大学 Radionuclide On-site sampling concentration detection device in a kind of seawater
CN109316777A (en) * 2018-08-30 2019-02-12 中国工程物理研究院核物理与化学研究所 A kind of cerium and rare earths separation method
CN109735711A (en) * 2018-12-27 2019-05-10 中核四0四有限公司 The leaching method of plutonium in a kind of concrete
CN112285226A (en) * 2020-10-16 2021-01-29 中国人民解放军63653部队 Rapid combined analysis method for Pu-239, Sr-90 and Cs-137 in waste liquid
CN112462410A (en) * 2020-11-09 2021-03-09 中核四0四有限公司 Method for analyzing plutonium in waste ion exchange resin sample
CN113359177A (en) * 2021-04-08 2021-09-07 中国辐射防护研究院 Combined analysis method for content of Pu, Am and Sr-90 in large-mass solid environment
CN113406114A (en) * 2021-04-28 2021-09-17 中国辐射防护研究院 Combined analysis method for content of Pu, Am and U in aerosol
CN114047539A (en) * 2021-11-04 2022-02-15 山东核电有限公司 Method for measuring activity of Fe and Ni in nuclear effluent
CN116594053A (en) * 2023-07-18 2023-08-15 清华大学 The radioactive solution contains transuranic alpha nuclide, 90 Sr and 137 cs separation system and device
CN116626742A (en) * 2023-07-18 2023-08-22 清华大学 A transuranic alpha nuclide in a radioactive solution, 90 Sr and 137 method for separating Cs fast group and application thereof

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109239760A (en) * 2018-08-22 2019-01-18 北京航空航天大学 Radionuclide On-site sampling concentration detection device in a kind of seawater
CN109316777A (en) * 2018-08-30 2019-02-12 中国工程物理研究院核物理与化学研究所 A kind of cerium and rare earths separation method
CN109316777B (en) * 2018-08-30 2021-04-06 中国工程物理研究院核物理与化学研究所 Method for separating cerium and rare earth elements
CN109735711A (en) * 2018-12-27 2019-05-10 中核四0四有限公司 The leaching method of plutonium in a kind of concrete
CN112285226A (en) * 2020-10-16 2021-01-29 中国人民解放军63653部队 Rapid combined analysis method for Pu-239, Sr-90 and Cs-137 in waste liquid
CN112462410A (en) * 2020-11-09 2021-03-09 中核四0四有限公司 Method for analyzing plutonium in waste ion exchange resin sample
CN113359177A (en) * 2021-04-08 2021-09-07 中国辐射防护研究院 Combined analysis method for content of Pu, Am and Sr-90 in large-mass solid environment
CN113406114A (en) * 2021-04-28 2021-09-17 中国辐射防护研究院 Combined analysis method for content of Pu, Am and U in aerosol
CN113406114B (en) * 2021-04-28 2022-10-21 中国辐射防护研究院 Combined analysis method for content of Pu, am and U in aerosol
CN114047539A (en) * 2021-11-04 2022-02-15 山东核电有限公司 Method for measuring activity of Fe and Ni in nuclear effluent
CN116594053A (en) * 2023-07-18 2023-08-15 清华大学 The radioactive solution contains transuranic alpha nuclide, 90 Sr and 137 cs separation system and device
CN116626742A (en) * 2023-07-18 2023-08-22 清华大学 A transuranic alpha nuclide in a radioactive solution, 90 Sr and 137 method for separating Cs fast group and application thereof
CN116626742B (en) * 2023-07-18 2023-11-07 清华大学 A transuranic alpha nuclide in a radioactive solution, 90 Sr and 137 method for separating Cs fast group and application thereof
CN116594053B (en) * 2023-07-18 2024-01-19 清华大学 The radioactive solution contains transuranic alpha nuclide, 90 Sr and 137 cs separation system and device

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