CN109580589A - A kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide - Google Patents
A kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide Download PDFInfo
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- CN109580589A CN109580589A CN201811608745.0A CN201811608745A CN109580589A CN 109580589 A CN109580589 A CN 109580589A CN 201811608745 A CN201811608745 A CN 201811608745A CN 109580589 A CN109580589 A CN 109580589A
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Abstract
A kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide, comprising the following steps: S1: weighing 0.2840g uranium dioxide sample and be placed in 50ml crucible, and 1.0ml concentrated hydrochloric acid and 2ml concentrated nitric acid is added, and places and dissolves by heating on electric hot plate；S2: being heated in crucible after existing without obvious liquid, removes placement and tantalum element is then carried out elution with uranium with nitration mixture upper prop and is separated to room temperature, and connect leacheate and be settled in 10ml volumetric flask, as sample solution；And uranium dioxide sample will be free of, only contain the solution of nitration mixture as reagent blank sample；S3: setting operating condition, after instrument stabilizer, by low mark solution and high standard solution on ICP spectrometer sample introduction, carry out the drafting of each elemental standards curve to be measured, S4: the sample solution and reagent blank sample in S2 are measured by sample channel wash with distilled water on iCAP spectrometer.
Description
Technical field
The invention belongs to analysis fields in nuclear fuel cycle, and in particular to a kind of for Determination of Trace Tantalum in uranium dioxide
ICP-AES measuring method.
Background technique
Important source material of the uranium dioxide as nuclear power enriched uranium.With the continuous development of China's Nuclear Electricity, to product matter
The control requirement of amount is stringenter, and the superiority and inferiority of product quality will directly ring the stable operation for arriving nuclear power.Therefore, it is necessary to dioxy
The measurement for changing impurity content in uranium is accurate as far as possible, comprehensive, guarantees that the reliability of analysis result is very important.It establishes
The analysis method of tantalum in uranium dioxide, purpose are exactly to provide strong analysis guarantee to hex product quality.
At present for the measurement of tantalum element mainly based on chemical method, specific operation process are as follows: dissolved first with concentrated nitric acid
After sample, there is (Ta2O5 does not dissolve in nitric acid) in tantalum in the form of Ta2O5, will be in water phase with TBP xylene extraction matrix uranium
Ta2O5 adds hydrofluoric acid dissolution, and calcination destroys the TBP of remaining, then with hydrofluoric acid dissolution residue, after low temperature is evaporated, with hydrofluoric acid-nitre
It is measured after acid-mixed acid solution low-grade fever dissolved residue.The shortcomings that chemical method is that analytical cycle is long, cumbersome, and accuracy and
Precision is all poor.It is unable to satisfy the analysis demand of tantalum in uranium dioxide, therefore we establish spectrographic determination two by experiment
The analysis method of tantalum element in urania, the method has the characteristics that easy to operate, accuracy, precision are high can meet two completely
The analysis of tantalum needs in urania.
Summary of the invention
It is an object of the invention to: it establishes a set of with high sensitivity, the analysis side that measuring speed is fast, analyst coverage is wide
Method meets the analysis demand of tantalum in uranium dioxide, provides reliable data for technique and supports.Thorium in uranium dioxide is improved simultaneously
Analysis method.
Technical scheme is as follows: a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide, including
Following steps:
S1: weighing 0.2840g uranium dioxide sample and be placed in 50ml crucible, and 1.0ml concentrated hydrochloric acid and 2ml concentrated nitric acid is added,
It places and is dissolved by heating on electric hot plate；
S2: being heated in crucible after existing without obvious liquid, removes placement to room temperature, then uses nitration mixture upper prop by tantalum element
Elution is carried out with uranium to separate, and connects leacheate and is settled in 10ml volumetric flask, as sample solution；And it will be tried without uranium dioxide
Sample only contains the solution of nitration mixture as reagent blank sample；
S3: setting operating condition, iCAP spectrometer RF power: 1150W；Fixed nebulizer flow: 0.5L/min；Assist gas
Flow is 0.5L/min；The time of integration: 1s；Elemental analysis line: iCAP spectrometer is arranged in 2400nm, and according to tantalum element analytical line
ICAP spectrometer is adjusted, after instrument stabilizer, sample introduction, progress are each to be measured on ICP spectrometer by low mark solution and high standard solution
The drafting of elemental standards curve,
S4: sample channel wash with distilled water, by the sample solution and reagent blank sample in S2, on iCAP spectrometer
It is measured.
In the S1,0.2840g uranium dioxide is weighed, it is quasi- to 0.1mg, with the calculating of 250mg uranium.
In the S1, the temperature of electric hot plate is 80 DEG C~100 DEG C.
In the S1, uranium dioxide sample is placed in 50ml tetrafluoroethene crucible.
In the S2, nitration mixture is 2g/L oxalic acid, 0.1mol/L hydrofluoric acid, 5mol/L nitric acid.
In the S3, low mark solution is the mixed acid solution in S2, and high standard solution is that the tantalum of 1 mcg/ml adds mixing in S2
Acid solution；
In the S4, sample channel 1min wash with distilled water.
In the S4, it is as a result accurate to μ g/mL.
Remarkable result of the invention is: this method is the particularity based on tantalum element in acid medium and establishes,
Tantalum is easy precipitating, is not easy to be eluted by general acid and uranium can not separate.Conventional analysis method is the nitric acid with 5mol/L
Tantalum element is eluted, the rate of recovery of tantalum element only has 80% or so, and uses nitration mixture as leacheate and tantalum element and uranium may be implemented
Be kept completely separate, the rate of recovery reaches 95% or more, and relative standard deviation is better than 10%.Specific feature is as described below:
1) have analytical cycle short, analyze the feature more than sample.Chemical Treatment tantalum element must carry out uranium with centrifuge
It separates, can only once handle 6 samples, each centrifugation time is 60 minutes, then carries out extraction calcination and destroys TBP, general to divide
The period is analysed at 3 hours or so.Once most multipotency analyzes 15 samples to spectroscopic methodology, and the general analysis period was at 2 hours or so.
2) have the characteristics that accuracy is high.With nitration mixture (mixed acid solution: oxalic acid 2.0g/L, hydrogen when analysis of spectral method tantalum element
Fluoric acid: 0.1mol/L, nitric acid: 5mol/L) elution separation is carried out, the rate of recovery is 95% or more.Chemical recovering method rate generally exists
80% or so.
3) have the characteristics that it is simple to operation, entire analytic process only include dissolution, separation, constant volume, measurement 4 steps.
Detailed description of the invention
Fig. 1 is ICP-AES measuring method flow chart of the present invention for Determination of Trace Tantalum in uranium dioxide；
Specific embodiment
A kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide, comprising the following steps:
S1: it weighs 0.2840g (quasi- to 0.1mg, with the calculating of 250mg uranium) uranium dioxide sample and is placed in 50ml tetrafluoroethene earthenware
In crucible, 1.0ml concentrated hydrochloric acid and 2ml concentrated nitric acid is added, places and is dissolved by heating on electric hot plate, the temperature of electric hot plate is 80 DEG C~100
℃；
S2: being heated in tetrafluoroethene crucible after existing without obvious liquid, removes placement to room temperature, then uses nitration mixture upper prop
Tantalum element and uranium are carried out elution to separate, nitration mixture is 2g/L oxalic acid, 0.1mol/L hydrofluoric acid, 5mol/L nitric acid, and connects leacheate
It is settled in 10ml volumetric flask, as sample solution；And uranium dioxide sample will be free of, only contain the solution of nitration mixture as reagent
Blank sample
S3: setting operating condition, iCAP spectrometer RF power: 1150W；Fixed nebulizer flow: 0.5L/min；Assist gas
Flow is 0.5L/min；The time of integration: 1s；Elemental analysis line: iCAP spectrometer is arranged in 2400nm, and according to tantalum element analytical line
Adjust iCAP spectrometer, after instrument stabilizer, by low mark solution and high standard solution on ICP spectrometer sample introduction, it is automatic by instrument
The drafting of each elemental standards curve to be measured is carried out, wherein low mark solution is the mixed acid solution in S2, high standard solution is 1 microgram/milli
The tantalum risen adds the mixed acid solution in S2；
S4: sample channel 1min wash with distilled water, by the sample solution and reagent blank sample in S2, in iCAP spectrum
It is measured on instrument, is as a result accurate to μ g/mL.
Claims (8)
1. a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide, it is characterised in that: the following steps are included:
S1: weighing 0.2840g uranium dioxide sample and be placed in 50ml crucible, and 1.0ml concentrated hydrochloric acid and 2ml concentrated nitric acid is added, and places
It is dissolved by heating on electric hot plate；
S2: being heated in crucible after existing without obvious liquid, removes placement to room temperature, then uses nitration mixture upper prop by tantalum element and uranium
Elution separation is carried out, and connects leacheate and is settled in 10ml volumetric flask, as sample solution；And uranium dioxide sample will be free of,
Only contain the solution of nitration mixture as reagent blank sample；
S3: setting operating condition, iCAP spectrometer RF power: 1150W；Fixed nebulizer flow: 0.5L/min；Secondary air amount
For 0.5L/min；The time of integration: 1s；Elemental analysis line: iCAP spectrometer is arranged in 2400nm, and adjusts according to tantalum element analytical line
ICAP spectrometer, after instrument stabilizer, by low mark solution and high standard solution on ICP spectrometer sample introduction, carry out each element to be measured
The drafting of standard curve,
S4: sample channel wash with distilled water carries out the sample solution and reagent blank sample in S2 on iCAP spectrometer
Measurement.
2. a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide according to claim 1, feature exist
In: in the S1,0.2840g uranium dioxide is weighed, it is quasi- to 0.1mg, with the calculating of 250mg uranium.
3. a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide according to claim 2, feature exist
In: in the S1, the temperature of electric hot plate is 80 DEG C~100 DEG C.
4. a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide according to claim 3, feature exist
In: in the S1, uranium dioxide sample is placed in 50ml tetrafluoroethene crucible.
5. a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide according to claim 1, feature exist
In: in the S2, nitration mixture is 2g/L oxalic acid, 0.1mol/L hydrofluoric acid, 5mol/L nitric acid.
6. a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide according to claim 1, feature exist
In: in the S3, low mark solution is the mixed acid solution in S2, and high standard solution is that the tantalum of 1 mcg/ml adds the nitration mixture in S2 molten
Liquid.
7. a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide according to claim 1, feature exist
In: in the S4, sample channel 1min wash with distilled water.
8. a kind of ICP-AES measuring method for Determination of Trace Tantalum in uranium dioxide according to claim 7, feature exist
In: in the S4, as a result it is accurate to μ g/mL.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111650142A (en) * | 2020-07-09 | 2020-09-11 | 中国原子能科学研究院 | Method for analyzing concentration of nitrous acid in uranium-containing organic phase |
| CN112147081A (en) * | 2019-06-28 | 2020-12-29 | 中核陕西铀浓缩有限公司 | Method for determining B, Si in uranium hexafluoride product |
| CN112697777A (en) * | 2021-01-20 | 2021-04-23 | 中国核动力研究设计院 | Method for determining content of lithium, sodium, magnesium and calcium in uranium compound |
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| CN105246683A (en) * | 2013-05-28 | 2016-01-13 | 柯尼卡美能达株式会社 | Gas-barrier film and process for producing the same |
| CN108083324A (en) * | 2017-12-25 | 2018-05-29 | 畅的新材料科技（上海）有限公司 | A kind of doped stannum oxide material of near-infrared reflection and preparation method thereof |
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2018
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Patent Citations (2)
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| CN105246683A (en) * | 2013-05-28 | 2016-01-13 | 柯尼卡美能达株式会社 | Gas-barrier film and process for producing the same |
| CN108083324A (en) * | 2017-12-25 | 2018-05-29 | 畅的新材料科技（上海）有限公司 | A kind of doped stannum oxide material of near-infrared reflection and preparation method thereof |
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| 李金英等: "萃取色层分离ICP/M S 测定U3O8 中Zr、N b、T a 和Ru", 《质谱学报》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112147081A (en) * | 2019-06-28 | 2020-12-29 | 中核陕西铀浓缩有限公司 | Method for determining B, Si in uranium hexafluoride product |
| CN112147081B (en) * | 2019-06-28 | 2024-03-19 | 中核陕西铀浓缩有限公司 | Method for measuring B, si in uranium hexafluoride product |
| CN111650142A (en) * | 2020-07-09 | 2020-09-11 | 中国原子能科学研究院 | Method for analyzing concentration of nitrous acid in uranium-containing organic phase |
| CN112697777A (en) * | 2021-01-20 | 2021-04-23 | 中国核动力研究设计院 | Method for determining content of lithium, sodium, magnesium and calcium in uranium compound |
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Application publication date: 20190405 |