CN113311465B - Combined analysis method for content of Pu isotope and Np-237 in sample - Google Patents
Combined analysis method for content of Pu isotope and Np-237 in sample Download PDFInfo
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Abstract
The invention belongs to the technical field of radioactive substance analysis, and relates to a combined analysis method for the contents of Pu isotopes and Np-237 in a sample. The joint analysis method comprises the following steps: (1) with HNO3‑NaNO2Pretreating a resin column based on tri-n-octylphosphine oxide by using a solution system; (2) adding Pu-236 or Pu-242 as tracer for simultaneous measurement of Pu and Np-237 in sample, and using HNO3Adjusting the acidity of the sample with the solution, and adding NaNO2The valence state of Pu isotope in the solution adjusting sample is positive quadrivalence and the valence state of Np-237 is positive hexavalent; (3) passing the treated sample solution obtained in the step (2) through the resin column treated in the step (1) and then using HNO3‑NaNO2Solution system, HCl-NH2After the resin column is washed by an OH & HCl solution system, HCl-HF-NH is used2Eluting the resin column by an OH & HCl solution system; (4) the eluate was analyzed for Pu isotope and Np-237 content. By utilizing the method, the contents of Pu isotopes and Np-237 in the sample can be successfully, reliably, stably and synchronously analyzed.
Description
Technical Field
The invention belongs to the technical field of radioactive substance analysis, and relates to a combined analysis method for the contents of Pu isotopes and Np-237 in a sample.
Background
In a radiochemical analysis process, in order to ensure the accuracy of the analysis result of a nuclide to be detected, it is usually necessary to add a suitable isotope as a chemical recovery rate tracer before the chemical treatment of a sample so as to perform recovery rate correction on the analysis measurement result.
Although there are 22 isotopes, the majority of Np are short-lived nuclides with extremely short half-lives (< 1d), which are not easily accessible and storable and are less applicable.
Np-237(T1/2＝2.144×106Yearly) long-lived alpha-decay nuclides, which are compounds of the species Pu: (A), (B), and (C)238～242Pu), long life, high chemical and radiotoxicity, and has been a major concern for environmental monitoring and environmental radionuclide hazard assessment.
Many radiologic procedures use isotopes of Pu (including Pu's) based on their first ionization energies and similar chemical behavior characteristics, in the absence of suitable Np isotope chemical recovery tracers, that are close to Np (6.27eV) and Pu (6.03eV)242Pu(T1/2＝3.75×105y)、236Pu(T1/22.86y) and244Pu(T1/2＝8.00×107y)) as237Np chemical pretreatment and measurement of non-isotopic tracers. If non-isotopic elements are used242Pu or236Pu as a yield tracer, Pu/Np fractionation which may occur in the radiochemical separation process cannot ensure the accuracy of the correction of Np-237 data by using the Pu isotope yield tracer (although no obvious chemical fractionation between Np and Pu (Np/Pu is between 0.93 and 1.07) is observed in the combined analysis method of the content of Pu-236 and Np-237 in most reported samples, the chemical recovery rate of Pu is often found to be high and stable in practical analysis application, and the Np sometimes has large fluctuation, which undoubtedly increases the uncertainty of the analysis result of Np-237).
In addition, the production process of the medium-long life Np-235 and Np-236 inevitably generates Np-237, which seriously affects the accuracy of the analysis result of the low-background Np-237 in the sample and can not be used as an isotope tracer for measuring the low-level Np-237.
Disclosure of Invention
The invention aims to provide a combined analysis method for the content of Pu isotopes and Np-237 in a sample, so as to successfully, reliably, stably and synchronously analyze the content of the Pu isotopes and the Np-237 in the sample, and particularly obviously reduce the uncertainty of the analysis result of the content of the Np-237.
To achieve this object, in a basic embodiment, the present invention provides a method for the combined analysis of the Pu isotope and Np-237 content of a sample, said method comprising the steps of:
(1) with HNO3-NaNO2Pretreating a resin column based on tri-n-octylphosphine oxide by using a solution system;
(2) adding Pu-236 or Pu-242 as tracer for simultaneous measurement of Pu and Np-237 in sample, and using HNO3Adjusting the acidity of the sample with the solution, and adding NaNO2The valence state of Pu isotope in the solution adjusting sample is positive quadrivalence and the valence state of Np-237 is positive hexavalent;
(3) passing the treated sample solution obtained in the step (2) through the resin column treated in the step (1) and then using HNO3-NaNO2Solution system, HCl-NH2After the resin column is washed by an OH & HCl solution system, HCl-HF-NH is used2Eluting the resin column by an OH & HCl solution system;
(4) the eluate was analyzed for Pu isotope and Np-237 content.
Sample acidity, NaNO in the above-described combined assay method2The method and results of the study on the effects of concentration and valorization time on the fractionation of Pu isotope and Np-237 are as follows:
1. effect of sample acidity on Pu and Np fractionation
In 5mL of 3-12mol/L HNO3Adding 0.02mol/L NaNO2And tracer of Pu-236 and Np-237, shaking up, and standing for 30 minutes. Pu and Np were simultaneously isolated and purified using TK200 resin, and the results are shown in FIG. 1. The results show that: at 6-12mol/L HNO3Under the matrix, the recovery rate of Pu and Np is more than 98.48 +/-367% and a fractional distillation coefficient of 1.00 ± 0.07, indicating a synchronous, efficient separation efficiency of Pu and Np under this regulation.
2、NaNO2Effect of concentration on Pu and Np fractionation
At 5mL of 8mol/L HNO3Adding 0-0.12mol/L NaNO2And tracer of Pu-236 and Np-237, shaking up, and standing for 30 minutes. Pu and Np were simultaneously isolated and purified using TEVA resin, the results are shown in figure 2. The results show that: at 0.001-0.12mol/L NaNO2Under the matrix, the recovery rate of Pu and Np is more than 91.27 +/-4.11%, and the fractionation coefficient is 0.97 +/-0.09, which shows that under the regulation, Pu and Np have synchronous and efficient separation efficiency.
3. Effect of valorization time on Pu and Np fractionation
In the actual analysis process, the analysis time may be long, and NaNO is added2The redox property of NaNO changes after long-term exposure to air, and thus, the research on NaNO2The effect of the pacing time on the Pu/Np sync separation is shown in fig. 3. The results show that: in 24 hours, NaNO2The method can continuously, stably and reliably synchronously adjust the valence state of Pu to be positive quadrivalent and the valence state of Np to be positive hexavalent.
In a preferred embodiment, the present invention provides a method for the combined analysis of the Pu isotope and the Np-237 content of a sample, wherein in step (1) and step (3), said HNO is present3-NaNO2HNO in solution system3The concentration of (A) is 6-12mol/L, NaNO2The concentration of (B) is 0.001-0.12 mol/L.
In a preferred embodiment, the present invention provides a method for the combined analysis of the Pu isotope and Np-237 content of a sample, wherein in step (1), the tri-n-octylphosphine oxide-based resin column is a TK200 resin column.
In a preferred embodiment, the present invention provides a method for the combined analysis of the Pu isotope and the Np-237 content of a sample, wherein in step (2), said HNO is3The concentration of the solution is 6-12mol/L, and the NaNO is2The concentration of the solution is 0.001-0.12 mol/L.
In a preferred embodiment, the present invention providesA method for the combined analysis of the Pu isotope and the Np-237 content in a sample, wherein in step (2), NaNO is added2The solution adjusts the time for the Pu isotope in the sample to be in a positive quadrivalent state and the Np-237 in a positive hexavalent state to be in a range of 1-24 hours.
In a preferred embodiment, the present invention provides a method for the combined analysis of the Pu isotope and the Np-237 content of a sample, wherein in step (3), said HCl-NH is present2The concentration of HCl in an OH & HCl solution system is 12mol/L, NH2The concentration of OH & HCl is 0.03-0.1 mol/L.
In a preferred embodiment, the present invention provides a method for the combined analysis of the Pu isotope and the Np-237 content of a sample, wherein in step (3), said HCl-HF-NH is present2The concentration of HCl in the OH & HCl solution system is 0.05-0.2mol/L, the concentration of HF is 0.01-0.1mol/L, and NH2The concentration of OH & HCl is 0.05-0.3 mol/L.
In a preferred embodiment, the invention provides a method for the combined analysis of the Pu isotope and Np-237 content of a sample, wherein in step (4), the analysis method is inductively coupled plasma mass spectrometry (ICP-MS) analysis or α spectrometer analysis.
In a preferred embodiment, the present invention provides a method for the combined analysis of the Pu isotope and Np-237 content of a sample, wherein said sample is a water sample, a soil sample, a biological sample or a liquid effluent.
In a more preferred embodiment, the present invention provides a method for the combined analysis of the Pu isotope and the Np-237 content of a sample containing237Np is 3 × 10-4-5×102Bq is between.
The method has the advantages that the combined analysis method for the contents of the Pu isotope and the Np-237 in the sample can successfully, reliably, stably and synchronously analyze the contents of the Pu isotope and the Np-237 in the sample, and particularly obviously reduces the uncertainty of the analysis result of the content of the Np-237.
Drawings
FIG. 1 is a graph showing the effect of acidity on simultaneous purification of Pu-236 and Np-237 of TK 200.
FIG. 2 shows NaNO2Graph of the effect of concentration on the simultaneous purification of Pu-236 and Np-237 of TK 200.
FIG. 3 shows NaNO2Graph of the impact of the pacing time on the synchronized separation of Pu-236 and Np-237.
Detailed Description
Example 1:
the flow of an exemplary method for the combined analysis of Pu isotope and Np-237 content in a sample is as follows:
(1) prepared to the size of
Tri-n-octylphosphine oxide (TOPO) -based TK200 resin column (tribkem, france);
(2) 20mL of 8mol/L HNO was used3-0.02mol/L NaNO2Pretreating a resin column by a system;
(3) adjusting the water sample matrix to 6-12mol/L HNO3A system;
(4) adding 0.02mol/L NaNO into the sample solution2Shaking the solution evenly, standing for 30 minutes, and adjusting the valence state of Pu isotope to be positive quadrivalent and the valence state of Np to be positive hexavalent (60 minutes);
(5) passing the feed liquid with the adjusted valence state through a resin column at the flow rate of 1 mL/min;
(6) using 20mL of 8mol/L HNO3-0.02mol/L NaNO2Washing the resin to remove the sample matrix;
(7) using 20mL of 12mol/L HCl-0.05mol/L NH2Removing Th by OH & HCl washing;
(8) 15mL of 0.1mol/L HCl-0.01mol/L HF-0.1mol/L NH was used2OH & HCl elutes the resin column.
(9) The eluate was analysed for Pu isotope and Np-237 content (measured using an alpha spectrometer).
In order to verify the accuracy of the analysis result, 0.25mBq Pu-236 and 0.25mBq Np-237 are added into each same sample to be detected, and the conditions that the Pu and the Np are 6-9mol/L mol/LHNO are monitored simultaneously3、0.015-0.03mol/L NaNO2Under the system, the TK200 has the efficiency (recovery rate) and the fractional distillation coefficient for synchronously separating and purifying Pu and NpThe results are shown in table 1 below. A large number of analysis experiment results show that: the recovery rates of Pu-236 and Np-237 are both more than 93%, and the fractionation coefficient is between 0.95 and 1.05. This shows that the analysis method of the present invention can successfully, reliably, stably and synchronously analyze the content of Pu-236 and Np-237 in the sample.
TABLE 1 recovery and fractionation coefficients for simultaneous Pu-236 and Np-237 separations
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (10)
1. A combined analysis method for the content of Pu isotopes and Np-237 in a sample, which is characterized by comprising the following steps:
(1) with HNO3-NaNO2Pretreating a resin column based on tri-n-octylphosphine oxide by using a solution system;
(2) adding Pu-236 or Pu-242 as tracer for simultaneous measurement of Pu and Np-237 in sample, and using HNO3Adjusting the acidity of the sample with the solution, and adding NaNO2The valence state of Pu isotope in the solution adjusting sample is positive quadrivalence and the valence state of Np-237 is positive hexavalent;
(3) passing the treated sample solution obtained in the step (2) through the resin treated in the step (1)Column, in sequence with HNO3-NaNO2Solution system, HCl-NH2After the resin column is washed by an OH & HCl solution system, HCl-HF-NH is used2Eluting the resin column by an OH & HCl solution system;
(4) the eluate was analyzed for Pu isotope and Np-237 content.
2. The joint analysis method according to claim 1, characterized in that: in the step (1) and the step (3), the HNO3-NaNO2HNO in solution system3The concentration of (A) is 6-12mol/L, NaNO2The concentration of (B) is 0.001-0.12 mol/L.
3. The joint analysis method according to claim 1, characterized in that: in the step (1), the resin column based on the tri-n-octylphosphine oxide is a TK200 resin column.
4. The joint analysis method according to claim 1, characterized in that: in the step (2), the HNO3The concentration of the solution is 6-12mol/L, and the NaNO is2The concentration of the solution is 0.001-0.12 mol/L.
5. The joint analysis method according to claim 1, characterized in that: in the step (2), NaNO is added2The solution adjusts the time for the Pu isotope in the sample to be in a positive quadrivalent state and the Np-237 in a positive hexavalent state to be in a range of 1-24 hours.
6. The joint analysis method according to claim 1, characterized in that: in the step (3), the HCl-NH2The concentration of HCl in an OH & HCl solution system is 12mol/L, NH2The concentration of OH & HCl is 0.03-0.1 mol/L.
7. The joint analysis method according to claim 1, characterized in that: in the step (3), the HCl-HF-NH2The concentration of HCl in the OH & HCl solution system is 0.05-0.2mol/L, the concentration of HF is 0.01-0.1mol/L, and NH2The concentration of OH & HCl is 0.05-0.3 mol/L.
8. The joint analysis method according to claim 1, characterized in that: in the step (4), the analysis method is inductively coupled plasma mass spectrometry or alpha spectrometer analysis.
9. The joint analysis method according to one of claims 1 to 8, characterized in that: the sample is a water sample, a soil sample, a biological sample or liquid effluent.
10. The joint analysis method according to claim 9, wherein: the sample contains237Np is 3 × 10-4-5×102Bq is between.
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| CN114235973A (en) * | 2021-11-05 | 2022-03-25 | 中国原子能科学研究院 | Method for determining content of Np-237 in urine sample |
| CN114624363B (en) * | 2022-03-21 | 2024-02-13 | 中国工程物理研究院核物理与化学研究所 | Rapid separation and measurement method for plutonium in water body |
| CN116594054B (en) * | 2023-07-18 | 2023-09-26 | 清华大学 | The method comprises the following steps of 233 Pa standard gamma source and preparation method and application thereof |
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