Method and apparatus for measuring an organic phase sample
By plotting the X-ray absorption spectra of uranium and plutonium series working standard solutions, calculating the natural logarithm value, and drawing working curves, the problem of cumbersome preparation of organic phase standard solutions in existing technologies has been solved, enabling rapid and accurate measurement of organic samples and reducing nuclear material waste and personnel exposure risks.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- THE 404 COMPANY LIMITED CHINA NAT NUCLEAR
- Filing Date
- 2023-09-12
- Publication Date
- 2026-05-29
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Figure CN117030978B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of post-processing analysis technology, specifically to a method and apparatus for measuring organic phase samples. Background Technology
[0002] In the post-processing analysis, the L-side density meter is used to measure the mass concentration of high-concentration uranium-neptunium-plutonium samples. There are two sample states: an aqueous nitric acid system and an organic 30% TBP kerosene system. The instrument must first generate a working curve before measuring the sample, and it requires periodic calibration. Traditional methods for generating working curves involve preparing a series of standard solutions for both the aqueous and organic phases, measuring them with the L-side density meter, and then generating separate working curves.
[0003] Currently, the method for plotting the working curve of the L-side density meter has the following problems: 1. The amount of standard used to prepare both aqueous and organic phase standards is large, resulting in waste of nuclear materials; 2. Organic phase standards are generally obtained by first preparing a high-concentration aqueous phase standard and then extracting it with 30% TBP kerosene, which is cumbersome and there is no effective and accurate method for determining the value of organic phase standards. Summary of the Invention
[0004] The technical problem to be solved by this invention is to provide a method for measuring organic phase samples. This method eliminates the need to prepare organic phase standard solutions, thereby reducing standard consumption and workload, improving calibration efficiency and saving production costs. Simultaneously, it reduces contact time with radioactive materials, lowering the dose rate for operators.
[0005] To address the aforementioned technical problems, embodiments of the present invention provide the following solutions:
[0006] The present invention provides a method for measuring organic phase samples, comprising:
[0007] Determine the working standard solutions for the uranium series and the plutonium series;
[0008] Based on the uranium series working standard solution and the plutonium series working standard solution, the uranium standard X-ray absorption spectrum and the plutonium standard X-ray absorption spectrum were measured and obtained respectively.
[0009] The standard natural logarithm value of uranium is calculated based on the standard X-ray absorption spectrum of uranium, and the standard natural logarithm value of plutonium is calculated based on the standard X-ray absorption spectrum of plutonium.
[0010] The uranium working curve is obtained based on the natural logarithm of the uranium standard and the uranium concentration of the uranium series working standard solution; the plutonium working curve is obtained based on the natural logarithm of the plutonium standard and the plutonium concentration of the plutonium series working standard solution.
[0011] The organic phase sample was measured based on the uranium and plutonium working curves.
[0012] Preferably, uranium series working standard solutions and plutonium series working standard solutions are selected, including:
[0013] Uranium series working standard solutions were prepared by mixing uranium standard stock solution and 1 mol / L nitric acid solution.
[0014] A series of working standard solutions of plutonium were prepared by mixing plutonium standard stock solution and 1 mol / L nitric acid solution.
[0015] Preferably, the above-mentioned method for measuring organic phase samples further includes:
[0016] 1.0 mL of deionized water was obtained, and the aqueous phase uranium blank results and aqueous phase plutonium blank results were measured.
[0017] The instrument background was determined based on the aqueous uranium blank results and the aqueous plutonium blank results.
[0018] Preferably, based on the uranium series working standard solution and the plutonium series working standard solution, the uranium standard X-ray absorption spectrum and the plutonium standard X-ray absorption spectrum are measured and obtained respectively, including:
[0019] A certain volume of uranium series working standard solution was obtained, added to an L-sided measuring cell, and the X-ray absorption spectrum of the uranium standard was obtained by measuring on an L-sided density meter;
[0020] A certain volume of plutonium series working standard solution was obtained, added to an L-sided measuring cell, and the plutonium standard X-ray absorption spectrum was obtained by measuring on an L-sided densitometer.
[0021] Preferably, the natural logarithm value of uranium is calculated based on the uranium standard X-ray absorption spectrum, and the natural logarithm value of plutonium is calculated based on the plutonium standard X-ray absorption spectrum, including:
[0022] Based on the L absorption boundary of the uranium standard X-ray absorption spectrum, E1 and E2 fitting intervals are selected on both sides, and the ratio is calculated based on the integral area given in the spectrum to obtain the natural logarithm value of the uranium standard.
[0023] Based on the L absorption boundary of the plutonium standard X-ray absorption spectrum, E1 and E2 fitting intervals are selected on both sides, and the ratio is calculated based on the integral area given in the spectrum to obtain the natural logarithm value of the plutonium standard.
[0024] Preferably, the uranium working curve is obtained based on the natural logarithm of the uranium standard and the uranium concentration of the uranium series working standard solutions, and the plutonium working curve is obtained based on the natural logarithm of the plutonium standard and the plutonium concentration of the plutonium series working standard solutions, including:
[0025] The uranium working curve is obtained by linearly fitting the natural logarithmic value of the uranium standard with the uranium concentration of the uranium series working standard solution.
[0026] The plutonium working curve is obtained by linearly fitting the natural logarithm value of the plutonium standard with the plutonium concentration of the plutonium series working standard solutions.
[0027] Preferably, the above-mentioned method for measuring organic phase samples further includes:
[0028] A reference spectrum of the aqueous phase was obtained based on a 1 mol / L nitric acid solution;
[0029] The organic phase reference spectrum was obtained based on 30% TBP-kerosene.
[0030] Embodiments of the present invention also provide a measuring device for organic phase samples, comprising:
[0031] The determination module is used to determine the working standard solutions for the uranium series and the plutonium series;
[0032] The measurement module is used to measure and obtain uranium standard X-ray absorption spectra and plutonium standard X-ray absorption spectra respectively based on the uranium series working standard solutions and the plutonium series working standard solutions; to calculate the natural logarithm of uranium standard X-ray absorption spectra and the natural logarithm of plutonium standard X-ray absorption spectra; to obtain uranium working curves based on the natural logarithm of uranium standard X-ray absorption spectra and the uranium concentration of the uranium series working standard solutions, and to obtain plutonium working curves based on the natural logarithm of plutonium standard X-ray absorption spectra and the plutonium concentration of the plutonium series working standard solutions; and to measure organic phase samples based on the uranium working curves and the plutonium working curves.
[0033] Preferably, the determining module is specifically used to: prepare a uranium series working standard solution by using uranium standard reserve solution and 1 mol / L nitric acid solution; and prepare a plutonium series working standard solution by using plutonium standard reserve solution and 1 mol / L nitric acid solution.
[0034] Preferably, the measuring device for the above-mentioned organic phase sample further includes:
[0035] The determination module is used to obtain 1.0 mL of deionized water, measure the aqueous phase uranium blank result and the aqueous phase plutonium blank result; and determine the instrument background based on the aqueous phase uranium blank result and the aqueous phase plutonium blank result.
[0036] The above-described solution of the present invention has at least the following beneficial effects:
[0037] The above-described solution of the present invention involves: determining uranium series working standard solutions and plutonium series working standard solutions; measuring and obtaining uranium standard X-ray absorption spectra and plutonium standard X-ray absorption spectra respectively based on the uranium series working standard solutions and the plutonium series working standard solutions; calculating the natural logarithm value of the uranium standard based on the uranium standard X-ray absorption spectra, and calculating the natural logarithm value of the plutonium standard based on the plutonium standard X-ray absorption spectra; obtaining a uranium working curve based on the natural logarithm value of the uranium standard and the uranium concentration of the uranium series working standard solutions, and obtaining a plutonium working curve based on the natural logarithm value of the plutonium standard and the plutonium concentration of the plutonium series working standard solutions; and measuring organic phase samples based on the uranium working curves and the plutonium working curves. This allows for the measurement of organic samples without the need for preparing organic phase standard solutions, reducing standard consumption and personnel workload, improving calibration timeliness and saving production costs, while also reducing contact time with radioactive materials and lowering the dose rate level for operators. Attached Figure Description
[0038] Figure 1 This is a schematic flowchart of the method for measuring organic phase samples according to the present invention;
[0039] Figure 2 This is a schematic diagram of the module of the organic phase sample measuring device of the present invention. Detailed Implementation
[0040] Exemplary embodiments of the present disclosure will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
[0041] like Figure 1 As shown, the present invention provides a method for measuring organic phase samples, comprising:
[0042] Step 11: Determine the uranium series working standard solutions and the plutonium series working standard solutions;
[0043] Step 12: Measure and obtain the uranium standard X-ray absorption spectrum and the plutonium standard X-ray absorption spectrum respectively based on the uranium series working standard solution and the plutonium series working standard solution;
[0044] Step 13: Calculate the natural logarithm value of uranium standard based on the uranium standard X-ray absorption spectrum, and calculate the natural logarithm value of plutonium standard based on the plutonium standard X-ray absorption spectrum;
[0045] Step 14: Obtain the uranium working curve based on the natural logarithm of the uranium standard and the uranium concentration of the uranium series working standard solution; obtain the plutonium working curve based on the natural logarithm of the plutonium standard and the plutonium concentration of the plutonium series working standard solution.
[0046] Step 15: Measure the organic phase sample according to the uranium working curve and the plutonium working curve.
[0047] In this embodiment, uranium and plutonium working standard solutions are determined; based on the uranium and plutonium working standard solutions, uranium and plutonium standard X-ray absorption spectra are measured and obtained respectively; the natural logarithm of the uranium standard is calculated based on the uranium standard X-ray absorption spectrum, and the natural logarithm of the plutonium standard is calculated based on the plutonium standard X-ray absorption spectrum; a uranium working curve is obtained based on the natural logarithm of the uranium standard and the uranium concentration of the uranium working standard solution, and a plutonium working curve is obtained based on the natural logarithm of the plutonium standard and the plutonium concentration of the plutonium working standard solution; and an organic phase sample is measured based on the uranium and plutonium working curves. Measuring organic samples using the obtained uranium and plutonium working curves eliminates the need to prepare organic phase standard solutions, significantly reducing standard consumption and personnel workload, effectively improving calibration timeliness and saving production costs, while also reducing contact time with radioactive materials and lowering the dose rate level for operators. It enables rapid and accurate analysis of the concentration of constant uranium and plutonium in radioactive process feed solutions, and the measurement results can be obtained in real time. It is fast, accurate and safe.
[0048] In an optional embodiment of the present invention, step 11 includes:
[0049] Step 111: Prepare a series of working standard solutions for uranium by mixing uranium standard stock solution and 1 mol / L nitric acid solution;
[0050] Step 112: Prepare a series of working standard solutions of plutonium by mixing plutonium standard stock solution and 1 mol / L nitric acid solution.
[0051] In this embodiment, uranium standard solutions with uranium concentrations of 2.00 g / L, 40.00 g / L, 80.00 g / L, 120.0 g / L, 160.0 g / L, and 200.0 g / L were prepared using uranium standard stock solution and 1 mol / L nitric acid solution, respectively.
[0052] A series of working standard solutions of plutonium with concentrations of 2.00 g / L, 10.00 g / L, 20.00 g / L, 30.00 g / L, 40.00 g / L, and 50.00 g / L were prepared using plutonium standard stock solution and 1 mol / L nitric acid solution.
[0053] In an optional embodiment of the present invention, the method further includes:
[0054] 1.0 mL of deionized water was obtained, and the aqueous phase uranium blank results and aqueous phase plutonium blank results were measured.
[0055] The instrument background was determined based on the aqueous uranium blank results and the aqueous plutonium blank results.
[0056] In this embodiment, 1.0 mL of deionized water is added to the L-side measurement cell and placed in the L-side density meter measurement chamber. First, the aqueous phase uranium measurement mode is selected to obtain the aqueous phase uranium blank result; then, the aqueous phase plutonium measurement mode is selected to read back the measurement spectrum to obtain the aqueous phase plutonium blank result.
[0057] The instrument background is acceptable when all uranium and plutonium blank results are less than 0.1 g / L. Otherwise, the sample holder needs to be cleaned or replaced to ensure that the background value meets the requirements before starting the sample measurement.
[0058] In an optional embodiment of the present invention, step 12 includes:
[0059] Step 121: Obtain a certain volume of uranium series working standard solution, add it to the L-side measurement cell, and measure the uranium standard X-ray absorption spectrum on the L-side density meter;
[0060] Step 122: Obtain a certain volume of plutonium series working standard solution, add it to the L-side measuring cell, and measure the plutonium standard X-ray absorption spectrum on the L-side densitometer.
[0061] In this embodiment, a certain volume of uniformly mixed uranium series working standard solution and plutonium series working standard solution are quickly and accurately transferred using a pipette and sequentially added to the L-side measuring cell. The corresponding uranium standard X-ray absorption spectrum and plutonium standard X-ray absorption spectrum are obtained on the L-side densitometer for subsequent calculations. For steps 111 and 112, uranium series working standard solutions and plutonium series working standard solutions of different concentrations are measured sequentially to obtain uranium standard X-ray absorption spectra and plutonium standard X-ray absorption spectra corresponding to different concentrations of working standard solutions.
[0062] In an optional embodiment of the present invention, step 13 includes:
[0063] Step 131: Select the E1 and E2 fitting intervals on both sides of the L absorption boundary of the uranium standard X-ray absorption spectrum, calculate the ratio based on the integral area given in the spectrum, and obtain the natural logarithm value of the uranium standard.
[0064] Step 132: Select the E1 and E2 fitting intervals on both sides of the L absorption boundary of the plutonium standard X-ray absorption spectrum, calculate the ratio based on the integral area given in the spectrum, and obtain the natural logarithm value of the plutonium standard.
[0065] In this embodiment, E1 and E2 fitting intervals are selected on both sides of the L absorption boundary of the uranium standard X-ray absorption spectrum, and the natural logarithm of their ratio is calculated based on the integral area given in the spectrum to obtain the natural logarithm of the uranium standard.
[0066] The E1 and E2 fitting intervals are selected on both sides of the L absorption boundary of the plutonium standard X-ray absorption spectrum. The natural logarithm of their ratio is calculated based on the integral area given in the spectrum to obtain the natural logarithm of the plutonium standard.
[0067] For the uranium standard X-ray absorption spectra and plutonium standard X-ray absorption spectra corresponding to the working standard solutions of different concentrations obtained in steps 121 and 122, the natural logarithm values of the uranium standard and plutonium standard corresponding to the working standard solutions of different concentrations are obtained by the above calculation method.
[0068] In an optional embodiment of the present invention, step 14 includes:
[0069] Step 141: Perform linear fitting between the natural logarithmic value of the uranium standard and the uranium concentration of the uranium series working standard solution to obtain the uranium working curve;
[0070] Step 142: Perform linear fitting between the natural logarithm value of the plutonium standard and the plutonium concentration of the plutonium series working standard solutions to obtain the plutonium working curve.
[0071] In this embodiment, the natural logarithm values of uranium standards corresponding to different concentrations of uranium series working standard solutions obtained in step 131 are linearly fitted with the uranium concentration values of different concentrations of uranium series working standard solutions to obtain uranium working curves.
[0072] The natural logarithm values of plutonium standard corresponding to different concentrations of plutonium series working standard solutions obtained in step 132 are linearly fitted with the plutonium concentration values of different concentrations of plutonium series working standard solutions to obtain the plutonium working curve.
[0073] In an optional embodiment of the present invention, the method further includes:
[0074] A 1 mol / L nitric acid solution was prepared, and measurements were taken within the different E1 and E2 absorption boundaries of different uranium and plutonium to obtain an aqueous phase reference spectrum.
[0075] Organic phase reference spectra were obtained by measuring different E1 and E2 absorption boundaries of 30% TBP-kerosene within different uranium and plutonium.
[0076] In this embodiment, approximately 1.6 mL of 1 mol / L nitric acid solution and 1.6 mL of 30% TBP-kerosene were added to the L-side measuring cell. The L-side measuring cell was placed in the L-side density meter measuring chamber for measurement to obtain aqueous phase reference spectrum and organic phase reference spectrum. The obtained uranium and plutonium working curves were compared with the aqueous phase reference spectrum and organic phase reference spectrum. The values of the aqueous phase reference spectrum and organic phase reference spectrum under different E1 and E2 absorption boundaries were calculated for reference correction optimization to further improve the accuracy of uranium and plutonium working curves.
[0077] The accuracy and precision of organic phase samples measured by the above method were compared experimentally:
[0078] The actual concentration ρ of uranium or plutonium in the sample is calculated using the following formula:
[0079] ρ=ρ i ×n
[0080] In the formula:
[0081] ρ — The actual concentration of uranium or plutonium in the sample, expressed in grams per liter (g / L);
[0082] ρi — the concentration of uranium or plutonium given by the measurement software, in grams per liter (g / L);
[0083] n — Sample dilution factor.
[0084] For organic phase samples measured using the above method, the accuracy and precision are calculated based on the measurement results.
[0085] By preparing the organic phase standard solution, an organic phase uranium standard curve was obtained. The organic phase sample was measured, and the accuracy and precision were calculated based on the measurement results. The accuracy and precision of the measurement results from the two methods were compared, as shown in Tables 1 and 2 below:
[0086] Table 1. Uranium Measurement Results of Organic Phase Uranium Standard Curve and Optimized Aqueous Phase Uranium Standard Curve
[0087]
[0088]
[0089] Table 2. Plutonium measurement data results of the organic phase plutonium standard curve and the optimized aqueous phase plutonium standard curve.
[0090]
[0091] By comparison, the precision of the measurement results obtained using the measurement method of this invention is close to that obtained by preparing an organic phase uranium standard curve using an organic phase standard solution. The measurement method of this invention, while ensuring the precision of the measurement results, eliminates the need to prepare an organic phase standard solution, significantly reducing standard consumption and personnel workload. It effectively improves calibration efficiency and saves production costs, while also reducing contact time with radioactive materials and lowering the dose rate level for operators. It enables rapid and accurate analysis of constant uranium and plutonium concentrations in radioactive process feed solutions, with real-time measurement results, and is characterized by speed, accuracy, and safety.
[0092] like Figure 2 As shown, the present invention also provides a measuring device 20 for organic phase samples, comprising:
[0093] Module 21 is used to determine the uranium series working standard solutions and the plutonium series working standard solutions;
[0094] Measurement module 22 is used to measure and obtain uranium standard X-ray absorption spectra and plutonium standard X-ray absorption spectra respectively based on the uranium series working standard solutions and the plutonium series working standard solutions; calculate the natural logarithm value of uranium standard X-ray absorption spectra and the natural logarithm value of plutonium standard X-ray absorption spectra; obtain uranium working curves based on the natural logarithm value of uranium standard X-ray absorption spectra and the uranium concentration of the uranium series working standard solutions, and obtain plutonium working curves based on the natural logarithm value of plutonium standard X-ray absorption spectra and the plutonium concentration of the plutonium series working standard solutions; and measure organic phase samples based on the uranium working curves and plutonium working curves.
[0095] Preferably, the determining module 21 is specifically used to: prepare a uranium series working standard solution by using uranium standard reserve solution and 1 mol / L nitric acid solution; and prepare a plutonium series working standard solution by using plutonium standard reserve solution and 1 mol / L nitric acid solution.
[0096] Preferably, the measuring device 20 for the organic phase sample further includes:
[0097] The determination module 23 is used to obtain 1.0 mL of deionized water, measure the aqueous phase uranium blank result and the aqueous phase plutonium blank result, and determine the instrument background based on the aqueous phase uranium blank result and the aqueous phase plutonium blank result.
[0098] Preferably, uranium series working standard solutions and plutonium series working standard solutions are selected, including:
[0099] Uranium series working standard solutions were prepared by mixing uranium standard stock solution and 1 mol / L nitric acid solution.
[0100] A series of working standard solutions of plutonium were prepared by mixing plutonium standard stock solution and 1 mol / L nitric acid solution.
[0101] Preferably, the above-mentioned device further includes:
[0102] 1.0 mL of deionized water was obtained, and the aqueous phase uranium blank results and aqueous phase plutonium blank results were measured.
[0103] The instrument background was determined based on the aqueous uranium blank results and the aqueous plutonium blank results.
[0104] Preferably, based on the uranium series working standard solution and the plutonium series working standard solution, the uranium standard X-ray absorption spectrum and the plutonium standard X-ray absorption spectrum are measured and obtained respectively, including:
[0105] A certain volume of uranium series working standard solution was obtained, added to an L-sided measuring cell, and the X-ray absorption spectrum of the uranium standard was obtained by measuring on an L-sided density meter;
[0106] A certain volume of plutonium series working standard solution was obtained, added to an L-sided measuring cell, and the plutonium standard X-ray absorption spectrum was obtained by measuring on an L-sided densitometer.
[0107] Preferably, the natural logarithm value of uranium is calculated based on the uranium standard X-ray absorption spectrum, and the natural logarithm value of plutonium is calculated based on the plutonium standard X-ray absorption spectrum, including:
[0108] Based on the L absorption boundary of the uranium standard X-ray absorption spectrum, E1 and E2 fitting intervals are selected on both sides, and the ratio is calculated based on the integral area given in the spectrum to obtain the natural logarithm value of the uranium standard.
[0109] Based on the L absorption boundary of the plutonium standard X-ray absorption spectrum, E1 and E2 fitting intervals are selected on both sides, and the ratio is calculated based on the integral area given in the spectrum to obtain the natural logarithm value of the plutonium standard.
[0110] Preferably, the uranium working curve is obtained based on the natural logarithm of the uranium standard and the uranium concentration of the uranium series working standard solutions, and the plutonium working curve is obtained based on the natural logarithm of the plutonium standard and the plutonium concentration of the plutonium series working standard solutions, including:
[0111] The uranium working curve is obtained by linearly fitting the natural logarithmic value of the uranium standard with the uranium concentration of the uranium series working standard solution.
[0112] The plutonium working curve is obtained by linearly fitting the natural logarithm value of the plutonium standard with the plutonium concentration of the plutonium series working standard solutions.
[0113] Preferably, the above-mentioned device further includes:
[0114] A reference spectrum of the aqueous phase was obtained based on a 1 mol / L nitric acid solution;
[0115] The organic phase reference spectrum was obtained based on 30% TBP-kerosene.
[0116] It should be noted that this device is the same as the method described above. All implementations in the above method embodiments are applicable to the embodiments of this device and can achieve the same technical effect.
[0117] The above description represents the preferred embodiments of the present invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A method for measuring organic phase samples, characterized in that, include: Determine the working standard solutions for the uranium series and the plutonium series; Based on the uranium series working standard solution and the plutonium series working standard solution, the uranium standard X-ray absorption spectrum and the plutonium standard X-ray absorption spectrum were measured and obtained respectively. The standard natural logarithm value of uranium is calculated based on the standard X-ray absorption spectrum of uranium, and the standard natural logarithm value of plutonium is calculated based on the standard X-ray absorption spectrum of plutonium. The uranium working curve is obtained based on the natural logarithm of the uranium standard and the uranium concentration of the uranium series working standard solution; the plutonium working curve is obtained based on the natural logarithm of the plutonium standard and the plutonium concentration of the plutonium series working standard solution. The organic phase sample was measured based on the uranium and plutonium working curves.
2. The method for measuring organic phase samples according to claim 1, characterized in that, Determining the working standard solutions for the uranium series and plutonium series includes: Uranium series working standard solutions were prepared by mixing uranium standard stock solution and 1 mol / L nitric acid solution. A series of working standard solutions for plutonium were prepared by mixing plutonium standard stock solution and 1 mol / L nitric acid solution.
3. The method for measuring organic phase samples according to claim 2, characterized in that, Also includes: 1.0 mL of deionized water was obtained, and the aqueous phase uranium blank results and aqueous phase plutonium blank results were measured. The instrument background was determined based on the aqueous uranium blank results and the aqueous plutonium blank results.
4. The method for measuring organic phase samples according to claim 2, characterized in that, Based on the uranium series working standard solutions and the plutonium series working standard solutions, the uranium standard X-ray absorption spectra and plutonium standard X-ray absorption spectra were measured and obtained, respectively, including: A certain volume of uranium series working standard solution was obtained, added to an L-sided measuring cell, and the X-ray absorption spectrum of the uranium standard was obtained by measuring on an L-sided density meter; A certain volume of plutonium series working standard solution was obtained, added to an L-sided measuring cell, and the plutonium standard X-ray absorption spectrum was obtained by measuring on an L-sided densitometer.
5. The method for measuring organic phase samples according to claim 4, characterized in that, The natural logarithm value of uranium is calculated based on the uranium standard X-ray absorption spectrum, and the natural logarithm value of plutonium is calculated based on the plutonium standard X-ray absorption spectrum, including: Based on the L absorption boundary of the uranium standard X-ray absorption spectrum, E1 and E2 fitting intervals are selected on both sides, and the ratio is calculated based on the integral area given in the spectrum to obtain the natural logarithm value of the uranium standard. Based on the L absorption boundary of the plutonium standard X-ray absorption spectrum, E1 and E2 fitting intervals are selected on both sides, and the ratio is calculated based on the integral area given in the spectrum to obtain the natural logarithm value of the plutonium standard.
6. The method for measuring organic phase samples according to claim 5, characterized in that, The uranium working curve is obtained based on the natural logarithm of the uranium standard and the uranium concentration of the uranium series working standard solutions. The plutonium working curve is obtained based on the natural logarithm of the plutonium standard and the plutonium concentration of the plutonium series working standard solutions, including: The uranium working curve is obtained by linearly fitting the natural logarithmic value of the uranium standard with the uranium concentration of the uranium series working standard solution. The plutonium working curve is obtained by linearly fitting the natural logarithm value of the plutonium standard with the plutonium concentration of the plutonium series working standard solutions.
7. The method for measuring organic phase samples according to claim 2, characterized in that, Also includes: A reference spectrum of the aqueous phase was obtained based on a 1 mol / L nitric acid solution; Organic phase reference spectra were obtained based on 30% TBP-kerosene.
8. A measuring device for organic phase samples, characterized in that, The determination module is used to determine the working standard solutions for the uranium series and the plutonium series; The measurement module is used to measure and obtain uranium standard X-ray absorption spectra and plutonium standard X-ray absorption spectra respectively based on the uranium series working standard solutions and the plutonium series working standard solutions; to calculate the natural logarithm of uranium standard X-ray absorption spectra and the natural logarithm of plutonium standard X-ray absorption spectra; to obtain uranium working curves based on the natural logarithm of uranium standard X-ray absorption spectra and the uranium concentration of the uranium series working standard solutions, and to obtain plutonium working curves based on the natural logarithm of plutonium standard X-ray absorption spectra and the plutonium concentration of the plutonium series working standard solutions; and to measure organic phase samples based on the uranium working curves and the plutonium working curves.
9. The measuring device for organic phase samples according to claim 8, characterized in that, The determining module is specifically used for: preparing uranium series working standard solutions by using uranium standard reserve solution and 1 mol / L nitric acid solution; and preparing plutonium series working standard solutions by using plutonium standard reserve solution and 1 mol / L nitric acid solution.
10. The measuring device for organic phase samples according to claim 8, characterized in that, Also includes: The determination module is used to obtain 1.0 mL of deionized water, measure the aqueous phase uranium blank result and the aqueous phase plutonium blank result; and determine the instrument background based on the aqueous phase uranium blank result and the aqueous phase plutonium blank result.
Citation Information
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