CN104597174A - Isotope dilution mass spectrometry method for determining content of uranium in uranium niobium alloy - Google Patents
Isotope dilution mass spectrometry method for determining content of uranium in uranium niobium alloy Download PDFInfo
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- CN104597174A CN104597174A CN201310535057.7A CN201310535057A CN104597174A CN 104597174 A CN104597174 A CN 104597174A CN 201310535057 A CN201310535057 A CN 201310535057A CN 104597174 A CN104597174 A CN 104597174A
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- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 53
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 15
- 238000004750 isotope dilution mass spectroscopy Methods 0.000 title claims abstract description 11
- GMVPEJUTFFCKDK-UHFFFAOYSA-N [Nb].[U] Chemical compound [Nb].[U] GMVPEJUTFFCKDK-UHFFFAOYSA-N 0.000 title abstract 9
- 239000000523 sample Substances 0.000 claims abstract description 27
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- 239000012488 sample solution Substances 0.000 claims abstract description 16
- 238000005259 measurement Methods 0.000 claims abstract description 8
- 238000004458 analytical method Methods 0.000 claims abstract description 5
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 5
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 18
- 150000002500 ions Chemical class 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 230000000155 isotopic effect Effects 0.000 claims description 12
- 125000005289 uranyl group Chemical group 0.000 claims description 7
- -1 Polytetrafluoroethylene Polymers 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000012749 thinning agent Substances 0.000 claims description 6
- 238000003556 assay Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- LGZXYFMMLRYXLK-UHFFFAOYSA-N mercury(2+);sulfide Chemical compound [S-2].[Hg+2] LGZXYFMMLRYXLK-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000000176 thermal ionisation mass spectrometry Methods 0.000 claims description 3
- 229910002007 uranyl nitrate Inorganic materials 0.000 claims description 3
- 230000004304 visual acuity Effects 0.000 claims description 3
- 239000013585 weight reducing agent Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000010955 niobium Substances 0.000 abstract description 6
- 229910052758 niobium Inorganic materials 0.000 abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 abstract description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract 2
- 239000003085 diluting agent Substances 0.000 abstract 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 abstract 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 abstract 1
- 238000001819 mass spectrum Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000005070 sampling Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000011824 nuclear material Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses an isotope dilution mass spectrometry method for determining the content of uranium in a uranium niobium alloy. A formula for calculating the content of uranium in the uranium niobium alloy is derived according to an isotope dilution mass spectrometry principle. A decomposition process of the uranium niobium alloy is researched, the sampling quantity and the amount of a diluent are optimized, and the influences of mass spectrum line interference and alloy element interference on a measurement result are discussed. The method comprises the following steps: adding nitric acid and hydrofluoric acid to quantitatively dissolve the uranium niobium alloy, adding a quantitative amount of a uranium isotope diluent to directly prepare a mixed sample solution, determining the mixed solution and the uranium isotope proportion in the uranium niobium alloy sample through mass spectrometry, and calculating the content of uranium in the uranium niobium alloy. Quantitative separation of uranium is not needed by the determined method. An XRF technique, an ICP-AES technique and an element analysis technique are used to measure the content of niobium and the total content of impurity elements in the uranium niobium alloy, and back stepping is carried out to obtain the corresponding uranium content order in order to verify the accuracy of the analytical result, and the obtained result is consistent with a result obtained through the experiment method. When the method disclosed in the invention is used to analyze the uranium niobium alloy sample, the relative standard uncertainty of determination results is 0.2% (6 determinations), and the expanded uncertainty is 0.5% (95% confidence level).
Description
Technical field
The invention belongs to casting technology field, be specifically related to a kind of isotope dilution mass spectrometry measuring uranium content in u-ni alloy.
Background technology
The chemical composition alloy performance of U-Nb alloy has a significant impact, and therefore its chemical composition of Accurate Determining is the requisite quality monitoring step of U-Nb alloying technology process.U-Nb alloy component comprises U, Nb and impurity content.Wherein Nb content generally applies emission spectrometry or x ray fluorescence spectrometry measures, and metallic impurity elements application emission spectrometry measures, but not metallic impurity elements application element analyser measures.In recent years, increasingly strict along with quality monitoring, and the requirement of nuclear material mass balance, in U-Nb alloy, the mensuration of matrix U content more and more comes into one's own.Common spectroscopy measurements technology, because the spectral line of uranium is easily disturbed, is not suitable for the measurement of uranium content in u-ni alloy, other chemical analysis technology, because the Quantitative Separation involving uranium and niobium and other impurity, chemical treating process is quite loaded down with trivial details.
Summary of the invention
In order to overcome the above-mentioned technical matters that prior art field exists, the object of the invention is to, provide a kind of isotope dilution mass spectrometry measuring uranium content in u-ni alloy, testing result is reliable.
The isotope dilution mass spectrometry of uranium content in mensuration u-ni alloy provided by the invention, comprises the following steps:
(1) key instrument and reagent: MI1201 type thermal ionization mass spectrometer (SELMI company of Ukraine); Analytical balance (resolving power 0.01mg); Be coated with sample heating arrangement (mass spectrograph is supporting special, and 0 ~ 3.0A heating current is adjustable); Electric hot plate (2000W, power adjustable); Uranium isotope thinning agent (uranyl nitrtate (UO2(NO3) 2) solution, the massfraction of uranium is 0.59065%, isotopic abundance: 234U:1.2367,235U:88.1540,236U:0.4346,238U:10.1747), laboratory is made by oneself; Nitric acid (AR); Hydrofluorite (AR); Hydrogen peroxide (AR).Quartz glass beaker (5mL); Polytetrafluoroethylene beaker (50mL); Micropipettor (1 μ L); Filament plug-in unit (Re is with, and mass spectrograph is special);
(2) assay method: the Uranium Isotope Ratio of u-ni alloy measures: take about appropriate u-ni alloy sample in quartz glass beaker, add appropriate 7mol/L nitric acid, then add 2 ~ 3 hydrogen peroxide, heating for dissolving is complete, steams near dry; Add a certain amount of 0.1mol/L nitric acid, be mixed with the uranyl nitrtate sample solution that uranium-bearing is about 5mg/mL; Be placed in by filament plug-in unit and be coated with on sample heating arrangement, pipette 1 μ L sample solution, drop on filament, heating makes its orange oxide being converted into Chinese red (UO3), proceeds to mass spectrograph ion gun by after the sabot of filament plug-in unit; Take out instrument system vacuum, treat that ion gun vacuum pressure is less than 1 × 10-4Pa, analysis conduit vacuum pressure is less than 1 × 10-5Pa, injects liquid nitrogen to mass spectrograph liquid nitrogen cold trap; Raise ionization belt current to about 5.5A, make 187Re+ ion current intensity be 0.3V ± 0.01V; Slowly raise evaporator strip electric current again to 2A ± 0.1A, make 238U+ ion current intensity be about 5V ± 0.1V, regulate mass spectrograph focusing parameter, make peak shape best, and make ion current signal intensity comparatively stable; Apply multiple Faraday cup receiver and receive measurement 234U+, 235U+, 236U+ and 238U+ ion current intensity simultaneously, automatically provided the Uranium Isotope Ratio value n(234U of u-ni alloy sample by instrument)/n(238U), n(235U)/n(238U), n(236U)/n(238U), then calculate corresponding isotopic abundance according to radiometer; The preparation of recombined sample solution and isotopic abundance ratio thereof measure: take about 100mg u-ni alloy sample (accurately true to 0.01mg) in polytetrafluoroethylene beaker, add a certain amount of 7mol/L nitric acid, be placed in heating for dissolving on electric hot plate complete, then add 2 ~ 3 hydrofluorite to dissolving completely; Use weight reduction to take appropriate uranium isotope thinning agent (being accurate to 0.01mg), add in sample solution; Add appropriate 7mol/L nitric acid again, be heated near dry, be prepared into recombined sample; Add a certain amount of 0.1mol/L nitric acid in recombined sample, recombined sample is mixed with the uranyl nitrate solution that uranium-bearing is about 5mg/mL; Equally, application Thermal Ionization Mass Spectrometry, in measuring by the Uranium Isotope Ratio of u-ni alloy, follow-up same mass spectrometry procedure measures the Uranium Isotope Ratio value n(235U of recombined sample solution)/n(238U);
(3) by formula:
draw uranium content in U-Nb alloy.
The isotope dilution mass spectrometry of uranium content in mensuration u-ni alloy provided by the invention, its beneficial effect is, the shortcoming that the spectral line overcoming existing spectroscopy measurements method uranium is easily disturbed, and the defect that in the Quantitative Separation process of uranium and niobium and other impurity, chemical treatment is quite loaded down with trivial details, achieve uranium content in fast and convenient mensuration u-ni alloy, and measurement result accurately and reliably, meets Production requirement; , the essence of isotopic dilution quantitative analysis to cause sample isotopic abundance ratio to change the combination carrying out mass spectroscopy after the precise of balance and isotopic dilution, is a kind of absolute measurement techniques of material amount.
Embodiment
Below in conjunction with an embodiment, the isotope dilution mass spectrometry of uranium content in mensuration u-ni alloy provided by the invention is described in detail.
Embodiment
The isotope dilution mass spectrometry of uranium content in the mensuration u-ni alloy of the present embodiment, comprises following content:
(1) key instrument and reagent: MI1201 type thermal ionization mass spectrometer (SELMI company of Ukraine); Analytical balance (resolving power 0.01mg).Be coated with sample heating arrangement (mass spectrograph is supporting special, and 0 ~ 3.0A heating current is adjustable); Electric hot plate (2000W, power adjustable); Uranium isotope thinning agent (uranyl nitrtate (UO
2(NO
3)
2) solution, the massfraction of uranium is 0.59065%, isotopic abundance:
234u:1.2367,
235u:88.1540,
236u:0.4346,
238u:10.1747), laboratory self-control; Nitric acid (AR); Hydrofluorite (AR); Hydrogen peroxide (AR).Quartz glass beaker (5mL); Polytetrafluoroethylene beaker (50mL); Micropipettor (1 μ L); Filament plug-in unit (Re is with, and mass spectrograph is special);
(2) assay method: the Uranium Isotope Ratio of u-ni alloy measures: take about 2mg u-ni alloy sample in quartz glass beaker, add 2mL 7mol/L nitric acid, then add 2 ~ 3 hydrogen peroxide, and heating for dissolving is complete, steams near dry; Add a certain amount of 0.1mol/L nitric acid, be mixed with the uranyl nitrtate sample solution that uranium-bearing is about 5mg/mL; Be placed in by filament plug-in unit and be coated with on sample heating arrangement, pipette 1 μ L sample solution, drop on filament, heating makes it be converted into the orange oxide (UO of Chinese red
3), proceed to mass spectrograph ion gun by after the sabot of filament plug-in unit; Take out instrument system vacuum, treat that ion gun vacuum pressure is less than 1 × 10
-4pa, analysis conduit vacuum pressure is less than 1 × 10
-5pa, injects liquid nitrogen to mass spectrograph liquid nitrogen cold trap; Raise ionization belt current to about 5.5A, make
187re
+ion current intensity is 0.3V; Slowly raise evaporator strip electric current again to about 2A, make
238u
+ion current intensity is about 5V, regulates mass spectrograph focusing parameter, makes peak shape best, and makes ion current signal intensity comparatively stable; Apply multiple Faraday cup receiver and receive measurement simultaneously
234u
+,
235u
+,
236u
+with
238u
+ion current intensity, is provided the Uranium Isotope Ratio value n(of u-ni alloy sample automatically by instrument
234u)/n(
238u), n(
235u)/n(
238u), n(
236u)/n(
238u), then according to radiometer calculate corresponding isotopic abundance; The preparation of recombined sample solution and isotopic abundance ratio thereof measure: take about 100mg u-ni alloy sample (being accurate to 0.01mg) in polytetrafluoroethylene beaker, add 10mL 7mol/L nitric acid, be placed in heating for dissolving on electric hot plate complete, then add 2 ~ 3 hydrofluorite to dissolving completely; Use weight reduction to take about 750mg uranium isotope thinning agent (being accurate to 0.01mg), add in sample solution; Add 5mL 7mol/L nitric acid again, be heated near dry, be prepared into recombined sample; Add a certain amount of 0.1mol/L nitric acid in recombined sample, recombined sample is mixed with the uranyl nitrate solution that uranium-bearing is about 5mg/mL; Equally, application Thermal Ionization Mass Spectrometry, in measuring by the Uranium Isotope Ratio of u-ni alloy, follow-up same mass spectrometry procedure measures the Uranium Isotope Ratio value n(of recombined sample solution
235u)/n(
238u);
(3) by formula:
draw uranium content in U-Nb alloy.
Claims (1)
1. measure an isotope dilution mass spectrometry for uranium content in u-ni alloy, it is characterized in that: said method comprising the steps of:
(1) key instrument and reagent: MI1201 type thermal ionization mass spectrometer (SELMI company of Ukraine); Analytical balance (resolving power 0.01mg); Be coated with sample heating arrangement (mass spectrograph is supporting special, and 0 ~ 3.0A heating current is adjustable); Electric hot plate (2000W, power adjustable); Uranium isotope thinning agent (uranyl nitrtate (UO
2(NO
3)
2) solution, the massfraction of uranium is 0.59065%, isotopic abundance:
234u:1.2367,
235u:88.1540,
236u:0.4346,
238u:10.1747), laboratory self-control; Nitric acid (AR); Hydrofluorite (AR); Hydrogen peroxide (AR), quartz glass beaker (5mL); Polytetrafluoroethylene beaker (50mL); Micropipettor (1 μ L); Filament plug-in unit (Re is with, and mass spectrograph is special);
(2) assay method: the Uranium Isotope Ratio of u-ni alloy measures: take about appropriate u-ni alloy sample in quartz glass beaker, add appropriate 7mol/L nitric acid, then add 2 ~ 3 hydrogen peroxide, heating for dissolving is complete, steams near dry; Add a certain amount of 0.1mol/L nitric acid, be mixed with the uranyl nitrtate sample solution that uranium-bearing is about 5mg/mL; Be placed in by filament plug-in unit and be coated with on sample heating arrangement, pipette 1 μ L sample solution, drop on filament, heating makes it be converted into the orange oxide (UO of Chinese red
3), proceed to mass spectrograph ion gun by after the sabot of filament plug-in unit; Take out instrument system vacuum, treat that ion gun vacuum pressure is less than 1 × 10
-4pa, analysis conduit vacuum pressure is less than 1 × 10
-5pa, injects liquid nitrogen to mass spectrograph liquid nitrogen cold trap; Raise ionization belt current to about 5.5A, make
187re
+ion current intensity is 0.3V ± 0.01V; Slowly raise evaporator strip electric current again to 2A ± 0.1A, make
238u
+ion current intensity is about 5V ± 0.1V, regulates mass spectrograph focusing parameter, makes peak shape best, and makes ion current signal intensity comparatively stable; Apply multiple Faraday cup receiver and receive measurement simultaneously
234u
+,
235u
+,
236u
+with
238u
+ion current intensity, is provided the Uranium Isotope Ratio value n(of u-ni alloy sample automatically by instrument
234u)/n(
238u), n(
235u)/n(
238u), n(
236u)/n(
238u), then according to radiometer calculate corresponding isotopic abundance; The preparation of recombined sample solution and isotopic abundance ratio thereof measure: take about 100mg u-ni alloy sample (accurately true to 0.01mg) in polytetrafluoroethylene beaker, add a certain amount of 7mol/L nitric acid, be placed in heating for dissolving on electric hot plate complete, then add 2 ~ 3 hydrofluorite to dissolving completely; Use weight reduction to take appropriate uranium isotope thinning agent (being accurate to 0.01mg), add in sample solution; Add appropriate 7mol/L nitric acid again, be heated near dry, be prepared into recombined sample; Add a certain amount of 0.1mol/L nitric acid in recombined sample, recombined sample is mixed with the uranyl nitrate solution that uranium-bearing is about 5mg/mL; Equally, application Thermal Ionization Mass Spectrometry, in measuring by the Uranium Isotope Ratio of u-ni alloy, follow-up same mass spectrometry procedure measures the Uranium Isotope Ratio value n(of recombined sample solution
235u)/n(
238u);
(3) by formula:
draw uranium content in U-Nb alloy.
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|---|---|---|---|
| CN201310535057.7A CN104597174A (en) | 2013-11-04 | 2013-11-04 | Isotope dilution mass spectrometry method for determining content of uranium in uranium niobium alloy |
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|---|---|
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| CN106198705A (en) * | 2016-06-27 | 2016-12-07 | 中国科学院地质与地球物理研究所 | Niobium pentaoxide is used for micro-example chromium isotope measuring technology as high sensitivity cast charge |
| CN106770610A (en) * | 2016-12-12 | 2017-05-31 | 中核北方核燃料元件有限公司 | A kind of abundance measurement method of boron 10 in boron and compound |
| CN107389661A (en) * | 2017-07-24 | 2017-11-24 | 中国科学院上海应用物理研究所 | A kind of method of uranium isotope composition on quick measure α disks |
| CN108931625A (en) * | 2018-05-22 | 2018-12-04 | 中国原子能科学研究院 | A kind of substoichiometric UO2-xThe measurement method of uranium content in fuel |
| CN109164162A (en) * | 2018-10-25 | 2019-01-08 | 中国工程物理研究院材料研究所 | It is a kind of with graphene oxide be ionize reinforcing agent uranium isotope abundance measurement method |
| CN109342481A (en) * | 2018-12-04 | 2019-02-15 | 中国工程物理研究院材料研究所 | A kind of method of FIB-TIMS measurement uranium-bearing particle isotope ratio |
| CN110310711A (en) * | 2019-06-26 | 2019-10-08 | 河南省人造金刚石微粉质量监督检验中心 | A kind of uncertainty evaluation method of diadust impurity content analysis result |
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| CN106198705A (en) * | 2016-06-27 | 2016-12-07 | 中国科学院地质与地球物理研究所 | Niobium pentaoxide is used for micro-example chromium isotope measuring technology as high sensitivity cast charge |
| CN106198705B (en) * | 2016-06-27 | 2018-12-21 | 中国科学院地质与地球物理研究所 | Niobium pentaoxide is used for micro-example chromium isotope measuring technology as highly sensitive cast charge |
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| CN107389661A (en) * | 2017-07-24 | 2017-11-24 | 中国科学院上海应用物理研究所 | A kind of method of uranium isotope composition on quick measure α disks |
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| CN110412107B (en) * | 2019-07-08 | 2022-03-29 | 中国石油天然气股份有限公司 | Method for developing oil source comparison by using uranium isotope |
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| CN110455843A (en) * | 2019-09-16 | 2019-11-15 | 核工业二三O研究所 | A kind of method that strontium internal standard-XRF solwution method measures uranium element in natural uranium product |
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| CN111505102A (en) * | 2020-04-29 | 2020-08-07 | 中国工程物理研究院核物理与化学研究所 | Uranium ore producing area classification method based on cluster analysis |
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