CN106932529A - A kind of UO2The assay method of uranium content in-BeO pellets - Google Patents

A kind of UO2The assay method of uranium content in-BeO pellets Download PDF

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Publication number
CN106932529A
CN106932529A CN201511026381.1A CN201511026381A CN106932529A CN 106932529 A CN106932529 A CN 106932529A CN 201511026381 A CN201511026381 A CN 201511026381A CN 106932529 A CN106932529 A CN 106932529A
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China
Prior art keywords
solution
potassium bichromate
concentration
acid
sample
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CN201511026381.1A
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Inventor
唐威
张庆明
许娜
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China North Nuclear Fuel Co Ltd
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China North Nuclear Fuel Co Ltd
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Priority to CN201511026381.1A priority Critical patent/CN106932529A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • G01N31/162—Determining the equivalent point by means of a discontinuity
    • G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Molecular Biology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention belongs to technical field of chemical detection, a kind of UO of specific design2The assay method of uranium content in-BeO pellets.The present invention comprises the following steps：Step 1, sample dissolving；Step 2, sample determination；Step 3, result are calculated.The present invention can accurately and rapidly determine UO2Uranium content in-BeO pellets, measurement result meets the requirement of technical indicator, and relative standard deviation is 0.05%.

Description

A kind of UO2The assay method of uranium content in-BeO pellets
Technical field
The invention belongs to technical field of chemical detection, a kind of UO of specific design2In-BeO pellets The assay method of uranium content.
Background technology
Uranium is the element that atomic number is 92, and its symbol of element is U, and being can in nature The most heavy element for finding.There are three kinds of isotopes in nature, with radioactivity, possess Half-life period very long.The micrometric measurement method of current uranium has coulometry and potentiometric titration.Storehouse Logical sequence method can survey constant material and can survey trace materials again, the primary standard of the method be galvanometer and Timer, electric current and time are easy to accurately measure, thus the degree of accuracy is higher.But analysis time It is more long, it is not suitable for quick analysis.The precision of ferrous iron reduction potassium dichromate oxidation potentiometric titration Degree and the degree of accuracy can compare favourably with coulometry, and instrument equipment is simple, in uranium content It is widely used in measure.
Both at home and abroad on UO2The achievement in research of the assay method of uranium content has no in-BeO pellets Open report.
The content of the invention
Present invention solves the technical problem that：The present invention provides a kind of UO2Uranium contains in-BeO pellets The assay method of amount, can in accurate measurement sample uranium content.
The technical solution adopted by the present invention：
Beneficial effects of the present invention：
A kind of UO that the present invention is provided2The assay method of uranium content, Neng Gouzhun in-BeO pellets Really, UO is quickly determined2Uranium content in-BeO pellets, measurement result meets technical indicator Requirement, relative standard deviation is 0.05%.
Specific embodiment
Below according to a kind of UO that specific embodiment is provided the present invention2Uranium contains in-BeO pellets The assay method of amount is described further.
A kind of UO2The assay method of uranium content, comprises the following steps in-BeO pellets：
Step 1, sample dissolving：
Weigh UO2- BeO sample 0.2g, are placed in 250mL glass beakers, are added in cup 10mL nitric acid, cap upper surface ware is placed on temp.-adjustable electric hot plate in heating 15min at 200 DEG C, 1mL hydrofluoric acid is added, continues to heat 15min, remove surface plate, continued heating and be evaporated, 40mL phosphoric acid is added, continues to be heated to sample to be completely dissolved, removed, be cooled to room temperature.
Step 2, sample determination：
The sample that will have been dissolved is placed on magnetic stirrer, adds stirrer, is added under agitation Enter 0.5mL sulfamic acid solutions, 5mL sulfuric acid solutions, 4.5mL are sequentially added after 0.5min Sulfamic acid solution, 5mL copperas solutions；Copperas solution should be applied directly in solution, Should not splash in walls of beaker；After being sufficiently stirred for 1.5min, 10mL nitric acid-ammonium molybdate is added Solution, after adding nitric acid-ammonium molybdate solution, solution becomes crineous, but this color is present Time must not exceed 40s；After continuing to stir 2.5min, then 0.5min is placed, add 10mL Vanadium sulfate acyl solution, adds 90mL water；Insertion platinum electrode is stirred with saturated calomel electrode, Current potential is 350~400mV, and potassium bichromate solution A is instilled by titration measuring cup, is to current potential 480~500mV；Continued that potassium bichromate B solution is added dropwise with 5mL microburets again, every time 0.10mL is added dropwise, the end of buret is washed after dropwise addition with water, treats that potential readings change in 5s During no more than 1mV, potential value and corresponding volume number are recorded；Drop to more than terminal, current potential It is 580~620mV, then 0.10mL potassium bichromate B solutions is added dropwise, writes down corresponding potential value； According to table 1, calculated with second derivative and reach the volume that equivalent point consumes potassium bichromate solution；
Table 1 titrates the volume calculating for consuming potassium bichromate B solution
Step 3, result are calculated：
It is calculated as follows uranium content：
In formula：
W (u) --- uranium content in sample, unit is expressed as a percentage (%)；
ρa--- the mass fraction of potassium bichromate A, unit is every gram of milligram (mg/g)；
ρb--- the concentration of potassium bichromate B solution, unit is every milliliter of milligram (mg/mL)；
The quality of m --- test portion, unit is gram (g)；
m1--- the titration bottle quality equipped with potassium bichromate solution A before titration, unit is gram (g)；
m2--- the titration bottle quality equipped with potassium bichromate solution A after titration, unit is gram (g)；
V --- the volume of the potassium bichromate B solution consumed during terminal, unit is milliliter (mL)；
2.4273 --- conversion factor of the potassium bichromate to natural uranium；
G --- relative atomic weight/238.029 of uranium in the uranium enrichment factor=sample.
In step 1, the concentration of nitric acid is 1.42g/cm3, the concentration of hydrofluoric acid is 1.18g/cm3, The concentration of phosphoric acid is 1.69g/cm3。
In step 2, the concentration of sulfamic acid solution is 150g/L, and the volume of sulfuric acid solution is dense It is 50% to spend, and the concentration of sulfamic acid solution is 150g/L, and the concentration of copperas solution is 280g/L, is 4g ammonium molybdates+500mLHNO in nitric acid-every liter of ammonium molybdate solution3, sulfuric acid In every liter of vanadium acyl solution be 31g vanadic sulfate+30mL sulfuric acid, potassium bichromate solution A it is dense It is 9.8mg/g to spend, and the concentration of potassium bichromate B solution is 0.5mg/mL.

Claims (3)

1. a kind of UO2The assay method of uranium content in-BeO pellets, it is characterised in that：Including Following steps：
Step (1), sample dissolving：
Weigh UO2- BeO sample 0.2g, are placed in 250mL glass beakers, are added in cup 10mL nitric acid, cap upper surface ware is placed on temp.-adjustable electric hot plate in heating 15min at 200 DEG C, 1mL hydrofluoric acid is added, continues to heat 15min, remove surface plate, continued heating and be evaporated, 40mL phosphoric acid is added, continues to be heated to sample to be completely dissolved, removed, be cooled to room temperature；
Step (2), sample determination：
The sample that will have been dissolved is placed on magnetic stirrer, adds stirrer, is added under agitation Enter 0.5mL sulfamic acid solutions, 5mL sulfuric acid solutions, 4.5mL are sequentially added after 0.5min Sulfamic acid solution, 5mL copperas solutions；Copperas solution should be applied directly in solution, Should not splash in walls of beaker；After being sufficiently stirred for 1.5min, 10mL nitric acid-ammonium molybdate is added Solution, after adding nitric acid-ammonium molybdate solution, solution becomes crineous, but this color is present Time must not exceed 40s；After continuing to stir 2.5min, then 0.5min is placed, add 10mL Vanadium sulfate acyl solution, adds 90mL water；Insertion platinum electrode is stirred with saturated calomel electrode, Current potential is 350~400mV, and potassium bichromate solution A is instilled by titration measuring cup, is to current potential 480~500mV；Continued that potassium bichromate B solution is added dropwise with 5mL microburets again, every time 0.10mL is added dropwise, the end of buret is washed after dropwise addition with water, treats that potential readings change in 5s During no more than 1mV, potential value and corresponding volume number are recorded；Drop to more than terminal, current potential It is 580~620mV, then 0.10mL potassium bichromate B solutions is added dropwise, writes down corresponding potential value； According to table 1, calculated with second derivative and reach the volume that equivalent point consumes potassium bichromate solution；
Table 1 titrates the volume calculating for consuming potassium bichromate B solution
Step (3), result are calculated：
It is calculated as follows uranium content：
W ( u ) = [ ρ a · ( m 1 - m 2 ) + ρ b · V ] × 2.4273 × G m × 1000 × 100
In formula：
W (u) --- uranium content in sample, unit is expressed as a percentage (%)；
ρa--- the mass fraction of potassium bichromate A, unit is every gram of milligram (mg/g)；
ρb--- the concentration of potassium bichromate B solution, unit is every milliliter of milligram (mg/mL)；
The quality of m --- test portion, unit is gram (g)；
m1--- the titration bottle quality equipped with potassium bichromate solution A before titration, unit is gram (g)；
m2--- the titration bottle quality equipped with potassium bichromate solution A after titration, unit is gram (g)；
V --- the volume of the potassium bichromate B solution consumed during terminal, unit is milliliter (mL)；
2.4273 --- conversion factor of the potassium bichromate to natural uranium；
G --- relative atomic weight/238.029 of uranium in the uranium enrichment factor=sample.
2. a kind of UO according to claim 12The measure side of uranium content in-BeO pellets Method, it is characterised in that：In the step (1), the concentration of nitric acid is 1.42g/cm3, hydrogen fluorine The concentration of acid is 1.18g/cm3, the concentration of phosphoric acid is 1.69g/cm3。
3. a kind of UO according to claim 12The measure side of uranium content in-BeO pellets Method, it is characterised in that：In step (2), the concentration of sulfamic acid solution is 150g/L, sulphur The volumetric concentration of acid solution is 50%, and the concentration of sulfamic acid solution is 150g/L, and sulfuric acid is sub- The concentration of ferrous solution is 280g/L, is 4g ammonium molybdates in nitric acid-every liter of ammonium molybdate solution +500mLHNO3, it is 31g vanadic sulfate+30mL sulfuric acid, weight in every liter of vanadium sulfate acyl solution The concentration of potassium chromate solution A is 9.8mg/g, and the concentration of potassium bichromate B solution is 0.5mg/mL.
CN201511026381.1A 2015-12-30 2015-12-30 A kind of UO2The assay method of uranium content in-BeO pellets Pending CN106932529A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109541126A (en) * 2018-12-19 2019-03-29 中核北方核燃料元件有限公司 The measuring method of uranium content in a kind of U-Mo Alloy
CN112710776A (en) * 2020-11-26 2021-04-27 中核北方核燃料元件有限公司 Oxidation-reduction titration detection method for uranium content in uranium tetrachloride
CN114323867A (en) * 2021-12-31 2022-04-12 中核二七二铀业有限责任公司 Method for analyzing and detecting uranium content in natural triuranium octoxide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102262086A (en) * 2011-04-19 2011-11-30 中国原子能科学研究院 Method for precisely measuring uranium by extraction photometry
CN102323377A (en) * 2011-09-16 2012-01-18 中核二七二铀业有限责任公司 Measurement method for uranium content in ammonium diuranate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102262086A (en) * 2011-04-19 2011-11-30 中国原子能科学研究院 Method for precisely measuring uranium by extraction photometry
CN102323377A (en) * 2011-09-16 2012-01-18 中核二七二铀业有限责任公司 Measurement method for uranium content in ammonium diuranate

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
国家技术监督局: "GB 11841-89 二氧化铀粉末和芯块中铀、氮、氟、钨和硅的测定", 《中华人民共和国国家标准》 *
李国华 等: "UO2芯块中铀(Ⅳ)、铀(Ⅵ)和铀总量的精密测定——恒电流库伦滴定法", 《中国核科技报告》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN108931625B (en) * 2018-05-22 2020-10-09 中国原子能科学研究院 Sub-stoichiometric UO2-xMethod for measuring uranium content in fuel
CN109541126A (en) * 2018-12-19 2019-03-29 中核北方核燃料元件有限公司 The measuring method of uranium content in a kind of U-Mo Alloy
CN112710776A (en) * 2020-11-26 2021-04-27 中核北方核燃料元件有限公司 Oxidation-reduction titration detection method for uranium content in uranium tetrachloride
CN114323867A (en) * 2021-12-31 2022-04-12 中核二七二铀业有限责任公司 Method for analyzing and detecting uranium content in natural triuranium octoxide

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