CN108051283A - The extraction of trace neptunium element and separation method in a kind of fluid sample - Google Patents
The extraction of trace neptunium element and separation method in a kind of fluid sample Download PDFInfo
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- CN108051283A CN108051283A CN201711057694.2A CN201711057694A CN108051283A CN 108051283 A CN108051283 A CN 108051283A CN 201711057694 A CN201711057694 A CN 201711057694A CN 108051283 A CN108051283 A CN 108051283A
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- G—PHYSICS
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The present invention relates to the extraction of trace neptunium element and separation methods in a kind of fluid sample, belong to trace analysis Sample Pretreatment Technique Used field.Method of the present invention mainly using trioctylamine as extract packing material, the concentration of stringent Non-leaching salpeter solution, in the case where ensureing that there is higher distribution coefficient and stronger adsorption capacity to neptunium element, the interference of high abundance uranium element is removed, so as to reach preferable extract and separate effect；The oxalic acid of reusable heat and the mixed acid solution of nitric acid strictly control the concentration of the mixed acid solution of oxalic acid and nitric acid as eluant, eluent, neptunium element are made to have the higher rate of recovery, so as to reach preferable concentrated effect.Extraction of the present invention and separation method can simply and quickly realize the separation and concentration to trace neptunium element in fluid sample, and improve the sensitivity under uranium Matrix effects to trace neptunium elemental analysis, and the method analysis neptunium element result is reliable and stable and favorable reproducibility.
Description
Technical field
The present invention relates to a kind of extraction separating method, trace neptunium in more particularly to a kind of fluid sample (237Np) the extraction of element
It takes and separation method, belongs to trace analysis Sample Pretreatment Technique Used field.
Background technology
Do not have on the earth natural237Np, in environment237Np is post-processed from nuclear weapon test and nuclear fuel, content
Very low, when analysis, can also be subject to the Matrix effects of uranium.Therefore,237The difficult point of Np elemental analyses is that the separation of uranium matrix
With237The concentration of Np.Chromes are widely used a kind of separation methods in transuranic element separation, have and divide well
From effect, can separation and concentration is micro and trace element, while have many advantages, such as again it is easy to operate, be easily achieved.At present, use
Chromes are to micro237During the analysis of Np elements, the more extensive method of application is using tributyl phosphate (TBP) extraction leaching
Resin and 7402 quaternary ammonium salt extration resins are extracted as extraction packing material.However, TBP extracting chromatographic columns only adsorb four,
Hexad, then pentavalent237Np elements are not adsorbed, and cause pentavalent237Np elements are lost in from column.In order to avoid pentavalent237Np members
Element is lost in from column, first will237Np is adjusted to pentavalent, and fluid sample is made to first pass through TBP extracting chromatographic columns, and uranium interference element quilt
Adsorption afterwards will237Np is reduced to tetravalence, then adsorbs tetravalence with 7402 QUATERNARY AMMONIUM SALT chromatograph columns237Np elements, but should
Process needs two step extracting operations, and process is complicated, laborious, and 7402 QUATERNARY AMMONIUM SALT chromatograph columns are in desorption, addition
Compounding agent also has an impact follow-up icp ms (ICP-MS) detection.
The content of the invention
For the prior art for the trace in analysis fluid sample237Insufficient existing for Np elements, the purpose of the present invention exists
The trace in a kind of fluid sample of offer237The extraction of Np elements and separation method are filled by the use of trioctylamine (TOA) as extraction
Material, stringent Non-leaching HNO3The concentration of solution, and by the use of the oxalic acid of heat and the mixed acid solution of nitric acid as eluant, eluent, protecting
Card pair237In the case of Np has higher distribution coefficient and stronger adsorption capacity, the interference of high abundance uranium element is removed, so as to
Reach preferable extract and separate effect, there is the higher rate of recovery in ICP-MS measure.
The mesh of the present invention is achieved through the following technical solutions：
The extraction of trace neptunium element and separation method, the method are as follows in a kind of fluid sample：
(1) mixed solvent of TOA and dimethylbenzene is added in polytetrafluoroethylene powder, then stirs to dimethylbenzene and be evaporated completely
Entirely, then HNO is used3After aqueous solution I is adjusted to pulpous state, the both ends of wet method dress post and chromatograph column are filled with polytetrafluoroethylene (PTFE) silk, use purity
Not less than the chromatograph column that the water wash of deionized water is equipped with, then use HNO3Aqueous solution II balances chromatograph column；
(2) ferrous sulfamate is added in the fluid sample containing trace neptunium element and carries out reduction reaction, after reduction
Fluid sample upper prop, then with aqueous solution of nitric acid III elute chromatograph column, finally with 90 DEG C or more of oxalic acid and the mixed acid of nitric acid
Solution elutes chromatograph column, and collects eluent, that is, completes the separation to trace neptunium element in fluid sample.
The volume ratio of the in the mixed solvent of TOA and dimethylbenzene, TOA and dimethylbenzene preferably 1:4；In every gram of polytetrafluoroethylene powder
Add in the mixed solvent of 2mL TOA and dimethylbenzene.
HNO3The concentration of aqueous solution I is 0.1mol/L~0.3mol/L, and 0.5mL HNO are added in every gram of polytetrafluoroethylene powder3
Aqueous solution I.
HNO3The concentration of aqueous solution II is 1.5mol/L~2.5mol/L, HNO3The volume of aqueous solution II and the body of chromatograph column
Product ratio preferably 3.5~6:1, the preferred 1mL/min~2mL/min of flow velocity.
It when the content of neptunium element is less than 1 μ g in fluid sample, adds in and is no less than 0.8mmol ferrous sulfamates, reduction is anti-
No less than 10min between seasonable.
To ensure effect of extracting, the preferred 0.8mL/min~1.5mL/min of flow velocity of fluid sample upper prop.
The concentration of aqueous solution of nitric acid III is 2mol/L~6mol/L, the volume of aqueous solution of nitric acid III and the volume ratio of chromatograph column
It is preferred that 4~6:1, the preferred 1.5mL/min~2.5mL/min of flow velocity of aqueous solution of nitric acid III.
In the mixed acid solution of oxalic acid and nitric acid, the concentration of oxalic acid is 0.02mol/L~0.06mol/L, the concentration of nitric acid
For 0.1mol/L~0.2mol/L, the volume of the mixed acid solution of oxalic acid and nitric acid and the volume ratio preferably 6~10 of chromatograph column:1；
When eluting chromatograph column using the mixed acid solution of oxalic acid and nitric acid, the preferred 1mL/ of flow velocity of the mixed acid solution of oxalic acid and nitric acid
Min~2mL/min.
Advantageous effect：
With using the chromes phase of TBP extration resins and 7402 quaternary ammonium salt extration resins as extraction packing material
Than being made in the present invention using TOA as extraction packing material237The extraction separation process of Np simplifies, while right238The decontamination energy of U
Power can reach 104More than, extract and separate is better；By the mixed acid for strictly controlling the oxalic acid and nitric acid of being used as eluant, eluent
The concentration of solution, makes237Np elements have the higher rate of recovery, so as to reach preferable concentrated effect.Extraction of the present invention
It can simply and quickly be realized in fluid sample with separation method237The separation and concentration of Np elements, while realization pair238Point of U
From can realize to nanogram magnitude in fluid sample237The extract and separate of Np；The method of the invention can be improved to trace
Amount237The extraction efficiency of Np elements, and then improve under uranium Matrix effects to trace237The sensitivity of Np elemental analyses, and this side
Method is analyzed237The result of Np elements is reliable and stable and favorable reproducibility.
Specific embodiment
The present invention will be further described With reference to embodiment.
In following embodiment：
Polytetrafluoroethylene powder：The mesh of 30 mesh~60, Chinese medicines group chemical reagents corporation；
Icp ms (ICP-MS)：Model Mars-9000, the limited public affairs of optically focused science and technology (Hangzhou) share
Department；It is tested using common sensitivity mode237Np and238U isotopes.
Embodiment 1
(1) by 60mL TOA and the mixed solvent (V of dimethylbenzeneTOA:VDimethylbenzene=1:4) it is added to and fills 30g polytetrafluoroethylene (PTFE)
It in the beaker of powder, is subsequently placed in draught cupboard and with magnetic stirrer 1h, makes dimethylbenzene volatilization complete；15mL concentration is used again
For the HNO of 0.2mol/L3After aqueous solution I is adjusted to pulpous state, wet method dress post is carried out, the color being first equipped with the elution of 50mL deionized waters
Layer column, then the aqueous solution of nitric acid II for being 2.0mol/L with 15mL concentration balance chromatograph column, and control the flow velocity of aqueous solution of nitric acid II
For 1.5mL/min；
Wherein, the material of chromatograph column used is glass, internal diameter 10mm, height of bed 50mm, and the both ends of chromatograph column are with poly- four
Vinyl fluoride silk is filled；
(2) by 5 μ g uranium and 5ng237Np is added in the aqueous solution of nitric acid that 10mL concentration is 2.0mol/L, is configured to liquid
Sample；
(3) the ferrous sulfamate aqueous solution that 0.4mL concentration is 2.0mol/L, reduction reaction are added in into fluid sample
After 10min, the fluid sample after reduction is subjected to upper prop with the flow velocity of 1.0mL/min, the beaker of washing holding liquid sample simultaneously will
Cleaning solution upper prop together；Then, the aqueous solution of nitric acid III for being 2.0mol/L with 20mL concentration elutes chromatograph column, and controls nitric acid aqueous solution
The flow velocity of solution III is 2.0mL/min；Again with the oxalic acid and the mixed acid solution of nitric acid that 30mL temperature is 95 DEG CChromatograph column is eluted, and controls the mixed acid of oxalic acid and nitric acid molten
Flow velocity is 1.5mL/min, and collects eluent, in eluent237Np is what is separated from fluid sample237Np,
So as to complete in fluid sample237The separation of Np.
The eluent of collection is analyzed using ICP-MS,237The detected level of Np is 4.53ng, and sample recovery rate is
90.6%.
Embodiment 2
(1) by 60mL TOA and the mixed solvent (V of dimethylbenzeneTOA:VDimethylbenzene=1:4) it is added to and fills 30g polytetrafluoroethylene (PTFE)
It in the beaker of powder, is subsequently placed in draught cupboard and with magnetic stirrer 1h, makes dimethylbenzene volatilization complete；15mL concentration is used again
For the HNO of 0.2mol/L3After aqueous solution I is adjusted to pulpous state, wet method dress post is carried out, first with the good color of 50mL deionized waters wash equipment
Layer column, then the aqueous solution of nitric acid II for being 2.0mol/L with 15mL concentration balance chromatograph column, and control the flow velocity of aqueous solution of nitric acid II
For 1.5mL/min；
Wherein, the material of chromatograph column used is glass, internal diameter 10mm, height of bed 50mm, and the both ends of chromatograph column are with poly- four
Vinyl fluoride silk is filled；
(2) by 5 μ g uranium and 5ng237Np is added in the aqueous solution of nitric acid that 10mL concentration is 2.0mol/L, is configured to liquid
Sample；
(3) the ferrous sulfamate aqueous solution that 0.4mL concentration is 2.0mol/L, reduction reaction are added in into fluid sample
After 10min, the fluid sample after reduction is subjected to upper prop with the flow velocity of 1.0mL/min, the beaker of washing holding liquid sample simultaneously will
Cleaning solution upper prop together；Then, the aqueous solution of nitric acid III for being 3.0mol/L with 20mL concentration elutes chromatograph column, and controls nitric acid aqueous solution
The flow velocity of solution III is 2.0mL/min；Again with the oxalic acid and the mixed acid solution of nitric acid that 30mL temperature is 95 DEG CChromatograph column is eluted, and controls the mixed acid of oxalic acid and nitric acid molten
Flow velocity is 1.5mL/min, and collects eluent, in eluent237Np is what is separated from fluid sample237Np,
So as to complete in fluid sample237The separation of Np.
The eluent of collection is analyzed using ICP-MS,237The detected level of Np is 4.71ng, and sample recovery rate is
94.2%.
Embodiment 3
(1) by 60mL TOA and the mixed solvent (V of dimethylbenzeneTOA:VDimethylbenzene=1:4) it is added to and fills 30g polytetrafluoroethylene (PTFE)
It in the beaker of powder, is subsequently placed in draught cupboard and with magnetic stirrer 1h, makes dimethylbenzene volatilization complete；15mL concentration is used again
For the HNO of 0.2mol/L3After aqueous solution I is adjusted to pulpous state, wet method dress post is carried out, first with the good color of 50mL deionized waters wash equipment
Layer column, then the aqueous solution of nitric acid II for being 2.0mol/L with 15mL concentration balance chromatograph column, and control the flow velocity of aqueous solution of nitric acid II
For 1.5mL/min；
Wherein, the material of chromatograph column used is glass, internal diameter 10mm, height of bed 50mm, and the both ends of chromatograph column are with poly- four
Vinyl fluoride silk is filled；
(2) by 5 μ g uranium and 5ng237Np is added in the aqueous solution of nitric acid that 10mL concentration is 2.0mol/L, is configured to liquid
Sample；
(3) the ferrous sulfamate aqueous solution that 0.4mL concentration is 2.0mol/L, reduction reaction are added in into fluid sample
After 10min, the fluid sample after reduction is subjected to upper prop with the flow velocity of 1.5mL/min, the beaker of washing holding liquid sample simultaneously will
Cleaning solution upper prop together；Then, the aqueous solution of nitric acid III for being 4.0mol/L with 20mL concentration elutes chromatograph column, and controls nitric acid aqueous solution
The flow velocity of solution III is 2.0mL/min；Again with 30mL oxalic acid at a temperature of 90 °C and the mixed acid solution of nitric acidChromatograph column is eluted, and controls the mixed acid of oxalic acid and nitric acid molten
Flow velocity is 1.5mL/min, and collects eluent, in eluent237Np is what is separated from fluid sample237Np,
So as to complete in fluid sample237The separation of Np.
The eluent of collection is analyzed using ICP-MS,237The detected level of Np is 4.68ng, and sample recovery rate is
93.6%.
Embodiment 4
(1) by 60mL TOA and the mixed solvent (V of dimethylbenzeneTOA:VDimethylbenzene=1:4) it is added to and fills 30g polytetrafluoroethylene (PTFE)
It in the beaker of powder, is subsequently placed in draught cupboard and with magnetic stirrer 1h, makes dimethylbenzene volatilization complete；15mL concentration is used again
For the HNO of 0.2mol/L3After aqueous solution I is adjusted to pulpous state, wet method dress post is carried out, first with the good color of 50mL deionized waters wash equipment
Layer column, then the aqueous solution of nitric acid II for being 2.0mol/L with 15mL concentration balance chromatograph column, and control the flow velocity of aqueous solution of nitric acid II
For 1.5mL/min；
Wherein, the material of chromatograph column used is glass, internal diameter 10mm, height of bed 50mm, and the both ends of chromatograph column are with poly- four
Vinyl fluoride silk is filled；
(2) by 5 μ g uranium and 5ng237Np is added in the aqueous solution of nitric acid that 10mL concentration is 2.0mol/L, is configured to liquid
Sample；
(3) the ferrous sulfamate aqueous solution that 0.4mL concentration is 2.0mol/L, reduction reaction are added in into fluid sample
After 10min, the fluid sample after reduction is subjected to upper prop with the flow velocity of 1.0mL/min, the beaker of washing holding liquid sample simultaneously will
Cleaning solution upper prop together；Then, the aqueous solution of nitric acid III for being 5.0mol/L with 20mL concentration elutes chromatograph column, and controls nitric acid aqueous solution
The flow velocity of solution III is 2.0mL/min；Again with the oxalic acid and the mixed acid solution of nitric acid that 30mL temperature is 95 DEG CChromatograph column is eluted, and controls the mixed acid of oxalic acid and nitric acid molten
Flow velocity is 1.5mL/min, and collects eluent, in eluent237Np is what is separated from fluid sample237Np,
So as to complete in fluid sample237The separation of Np,.
The eluent of collection is analyzed using ICP-MS,237The detected level of Np is 4.45ng, and sample recovery rate is
89.0%.
In conclusion the foregoing is merely a prefered embodiment of the invention, it is not intended to limit the scope of the present invention.
Within the spirit and principles of the invention, any modifications, equivalent replacements and improvements are made should be included in the present invention's
Within protection domain.
Claims (8)
1. the extraction of trace neptunium element and separation method in a kind of fluid sample, it is characterised in that：The specific steps of the method
It is as follows：
(1) mixed solvent of TOA and dimethylbenzene is added in polytetrafluoroethylene powder, then stirred to dimethylbenzene volatilization completely,
HNO is used again3After aqueous solution I is adjusted to pulpous state, the both ends of wet method dress post and chromatograph column are filled with polytetrafluoroethylene (PTFE) silk, not small with purity
In the chromatograph column that the water wash of deionized water is equipped with, then use HNO3Aqueous solution II balances chromatograph column；
(2) ferrous sulfamate is added in the fluid sample containing trace neptunium element and carries out reduction reaction, by the liquid after reduction
Body sample upper prop, then chromatograph column is eluted with aqueous solution of nitric acid III, finally with 90 DEG C or more of oxalic acid and the mixed acid solution of nitric acid
Chromatograph column is eluted, and collects eluent, that is, completes the separation to trace neptunium element in fluid sample；
Wherein, HNO3The concentration of aqueous solution I is 0.1mol/L~0.3mol/L, HNO3The concentration of aqueous solution II for 1.5mol/L~
2.5mol/L, the concentration of aqueous solution of nitric acid III is 2mol/L~6mol/L；In the mixed acid solution of oxalic acid and nitric acid, oxalic acid it is dense
It spends for 0.02mol/L~0.06mol/L, the concentration of nitric acid is 0.1mol/L~0.2mol/L.
2. the extraction of trace neptunium element and separation method in a kind of fluid sample according to claim 1, it is characterised in that：
The in the mixed solvent of TOA and dimethylbenzene, the volume of TOA and the volume ratio of dimethylbenzene are 1:4；Every gram of polytetrafluoroethylene powder adds in
The mixed solvent of 2mL TOA and dimethylbenzene.
3. the extraction of trace neptunium element and separation method in a kind of fluid sample according to claim 1, it is characterised in that：
Every gram of polytetrafluoroethylene powder adds in 0.5mL HNO3Aqueous solution I.
4. the extraction of trace neptunium element and separation method in a kind of fluid sample according to claim 1, it is characterised in that：
HNO3The flow velocity of aqueous solution II is 1mL/min~2mL/min；HNO3The volume of aqueous solution II and the volume ratio of chromatograph column for 3.5~
6:1。
5. the extraction of trace neptunium element and separation method in a kind of fluid sample according to claim 1, it is characterised in that：
When the content of neptunium element is less than 1 μ g in fluid sample, adds in and be no less than 0.8mmol ferrous sulfamates, the reduction reaction time is not
Less than 10min.
6. the extraction of trace neptunium element and separation method in a kind of fluid sample according to claim 1, it is characterised in that：
The flow velocity of fluid sample upper prop is 0.8mL/min~1.5mL/min.
7. the extraction of trace neptunium element and separation method in a kind of fluid sample according to claim 1, it is characterised in that：
The flow velocity of aqueous solution of nitric acid III is 1.5mL/min~2.5mL/min, and the volume and the volume ratio of chromatograph column of aqueous solution of nitric acid III are
4~6:1.
8. the extraction of trace neptunium element and separation method in a kind of fluid sample according to claim 1, it is characterised in that：
The volume of the mixed acid solution of oxalic acid and nitric acid is 6~10 with the volume ratio of chromatograph column:1, the mixed acid solution of oxalic acid and nitric acid
Flow velocity be 1mL/min~2mL/min.
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Cited By (2)
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| CN111380943A (en) * | 2020-03-13 | 2020-07-07 | 中国原子能科学研究院 | Method for analyzing content of trace neptunium in large amount of uranium in nuclear fuel post-processing flow |
| 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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| CN111380943A (en) * | 2020-03-13 | 2020-07-07 | 中国原子能科学研究院 | Method for analyzing content of trace neptunium in large amount of uranium in nuclear fuel post-processing flow |
| 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 |
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