CN102262086A - Method for precisely measuring uranium by extraction photometry - Google Patents
Method for precisely measuring uranium by extraction photometry Download PDFInfo
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- CN102262086A CN102262086A CN2011100974715A CN201110097471A CN102262086A CN 102262086 A CN102262086 A CN 102262086A CN 2011100974715 A CN2011100974715 A CN 2011100974715A CN 201110097471 A CN201110097471 A CN 201110097471A CN 102262086 A CN102262086 A CN 102262086A
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- Prior art keywords
- uranium
- extraction
- chromium
- potassium dichromate
- micrometric measurement
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- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 43
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000000605 extraction Methods 0.000 title claims abstract description 36
- 238000005375 photometry Methods 0.000 title abstract description 3
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000005259 measurement Methods 0.000 claims abstract description 25
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 239000012074 organic phase Substances 0.000 claims abstract description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 10
- 239000011651 chromium Substances 0.000 claims abstract description 10
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims abstract description 10
- HNVACBPOIKOMQP-UHFFFAOYSA-N uranium(4+) Chemical compound [U+4] HNVACBPOIKOMQP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical group CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 238000000638 solvent extraction Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000005185 salting out Methods 0.000 claims description 4
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 238000005070 sampling Methods 0.000 abstract description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003758 nuclear fuel Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 241000030614 Urania Species 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 description 2
- AAORDHMTTHGXCV-UHFFFAOYSA-N uranium(6+) Chemical compound [U+6] AAORDHMTTHGXCV-UHFFFAOYSA-N 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BFGKITSFLPAWGI-UHFFFAOYSA-N chromium(3+) Chemical compound [Cr+3] BFGKITSFLPAWGI-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for precisely measuring uranium by an extraction spectrophotometry, which comprises the steps of weighing a uranium sample, pretreating, adjusting the valence to uranium (IV), adding excessive potassium dichromate after the valence is adjusted to uranium (IV) to oxidize the uranium (IV) to uranium (VI), then adding an organic solvent to extract excessive chromium (VI), and measuring chromium in an organic phase by a spectrophotometry, wherein the excessive potassium dichromate is added so that the added excessive amount accounts for 0.3-0.5% of the total amount of potassium dichromate. The method for precisely measuring uranium by the extraction photometry provided by the invention has the advantages of high precision, high selectivity, simplicity in operation, small sampling amount, accurate and reliable measurement result and easiness in realization.
Description
Technical field
The present invention relates to the nuclear fuel cycle technical field, particularly a kind of method of extraction spectrophotometric method micrometric measurement uranium.
Background technology
Uranium is important nuclear fuel, and the micrometric measurement technology of uranium is all having critical role aspect each link of nuclear fuel cycle and the nuclear safeguards.
Have bibliographical information to adopt direct photometry micrometric measurement uranium content, this method uranium sampling amount is 2.5g, and the measurement result relative standard deviation is 0.05%.This method is directly carried out the mensuration of chromium (VI) without separation.Source of error is many, and the uncertainty component of introducing is many; Mo (VI), Cu (II), Fe (III), V (V) and U (VI) etc. measure the chromium (VI) of surplus all interference, in order to eliminate the interference of foreign ion, must increase the uranium sampling amount, with the accuracy of raising method.This method adds excessively with the titrant potassium dichromate is disposable, the vessel aridity is had relatively high expectations, and poor stability, uranium sampling amount is big.And potentiometric titration and other spectrophotometric method micrometric measurement uranium need add important reagent of sulfuric acid vanadium acyl in the mensuration process, and this reagent needs preparation voluntarily before mensuration, and this is the main cause that causes the procedure complexity.
The applicant did concise and to the point report to the method for extraction spectrophotometric method micrometric measurement uranium content in 2008 in China Atomic Energy Science Research Institute's annual report, but the thinking that the applicant sets up the method just briefly set forth in article, and the accuracy of the method is set forth and verified.The concrete processing step and the parameter of the unexposed method of article, and concrete processing step and parameter are to realize the gordian technique of pin-point accuracy and high precision.
Summary of the invention
The present invention has overcome deficiency of the prior art, provide a kind of high precision, simple to operate, sampling amount is little, measurement result is accurate, the method for extraction spectrophotometric method micrometric measurement uranium reliable, that easily realize.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A kind of method of extraction spectrophotometric method micrometric measurement uranium, comprise and take by weighing uranium sample, pre-service, readjust prices, add excessive potassium dichromate with U (IV) oxidation U (VI) to uranium (IV) back described the price modification to uranium (IV), the chromium (VI) that adds the organic solvent extraction surplus then, adopt the chromium in the spectrophotometry organic phase, key is that the excessive potassium dichromate of described adding accounts for 0.3%～0.5% of potassium dichromate total amount for adding excess quantity.
Add salting-out agents sodium chloride in the process of described extraction of chromium.Add excessive potassium dichromate to uranium (IV) back and do not add vanadium sulfate acyl solution in U (IV) oxidation U (VI) process described the price modification.The ratio of organic phase after the described extraction of chromium and water is 1: 2～1: 3, and the ratio of preferably selecting organic phase and water for use is 1: 3.Described pre-service is for to add strong phosphoric acid, potassium bichromate solution, sulfuric acid solution, sulfaminic acid solution stirring successively with the uranium sample that takes by weighing.Described adding organic solvent extraction chromium (VI) is for adding behind surfactant Tritonx-100 solution, DPC solution, the organic solvent fully oscillation extraction successively.Described organic solvent is an isoamylol.
Compared with prior art, the invention has the beneficial effects as follows:
The potassium dichromate excess quantity that adds in this method accounts for 0.3%～0.5% of potassium dichromate total amount, can greatly improve the accuracy and the precision of measurement result like this.Add excessive potassium dichromate to uranium (IV) back and do not add vanadium sulfate acyl solution in U (IV) oxidation U (VI) process readjusting prices, avoided the interference of vanadium, saved the time for preparing vanadium sulfate acyl voluntarily simultaneously measuring.Excessive chromium (VI) measures after by extraction, wherein chromium (III) with DPC reaction, eliminated simultaneously Mo (VI), Cu (II), Fe (III), V (V), U (VI) and with the interference of foreign ion such as phosphoric acid generation complex reaction.In the process of extraction, this method adds salting-out agents, accelerates extraction process, realizes the precision measurement of uranium in a small amount.This method can realize that sampling amount is the micrometric measurement of 10mg uranium content.
Description of drawings
The operational flowchart of Fig. 1 method
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described in further detail:
The method of a kind of extraction spectrophotometric method micrometric measurement uranium as shown in Figure 1, this method comprises and takes by weighing uranium sample, the uranium sample that takes by weighing is added strong phosphoric acid, potassium bichromate solution, sulfuric acid solution, sulfaminic acid solution stirring successively carries out pre-service, adding copperas solution readjusts prices uranium (VI) to uranium (IV), add excessive potassium dichromate then, wherein the amount of the potassium dichromate surplus of Jia Ruing accounts for 0.3%～0.5% of potassium dichromate total amount.By potassium dichromate U (IV) is oxidizing to U (VI), needs after the oxidation to add surfactant Tritonx-100, reach the effect of absorbance enhanced sensitivity.The chromium of organic solvent extraction surplus (VI) adopts the chromium in the spectrophotometry organic phase at last.Thereby the amount of the potassium dichromate that consumes in the time of can calculating urania (VI), thereby the micrometric measurement of realization uranium content.
The concrete operations step of this method is as follows:
Take by weighing uranium content and be about the 0.10000g uranium solution in the 250ml conical flask, add 40ml strong phosphoric acid, 0.2ml0.2mol/L potassium bichromate solution, 5.0ml (1: 1) sulfuric acid solution, 10ml 3mol/L sulfaminic acid solution, 5.0ml 1.0mol/L copperas solution successively, solution placed on the magnetic stirring apparatus stir, regulate temperature to 30～35 ℃, add 10.0ml 1% oxidizing agent solution.When solution becomes crineous, crineous is taken off in 40s.Continue to stir 2.5mins, leave standstill 30s.(pass through stoichiometric calculation by taking gravimetric method to add a certain amount of potassium bichromate solution then, make its surplus), this method draws the excess quantity that adds potassium dichromate by test of many times and accounts for 0.3%～0.5% of potassium dichromate total amount, so just can reach the requirement of pin-point accuracy to be solved by this invention, high precision.Do not add vanadium sulfate acyl solution at uranium in U (IV) oxidation U (VI) process, broken through the constraint that adds vanadium sulfate acyl in traditional assay method, reduced the interference of vanadium sulfate acyl.
Add 1.5ml 0.2%Tritonx-100 solution, 2.0ml 0.5%DPC solution, 50ml organic solvent more successively, abundant oscillation extraction 2min, behind the standing demix 60min, aqueous phase discarded.Wherein organic solvent can adopt TBP, ethyl acetate, ether, isoamylol etc.This example preferably adopts isoamylol, and the isoamylol effect of extracting is best, and phase-splitting is fast, and the interface is clear.And in extraction process, add salting-out agents, and can accelerate extraction process like this, measure again after can placing a period of time after adopting this method extraction to finish.
Wherein, consider the influence of water and organic phase, extraction time, need quantitatively to add isoamylol in this enforcement and make in the ratio 1: 2～1: 3 of extraction back organic phase and water and the extraction time 1～3min scope extraction more complete the complex absorbance.Preferably select for use and be in a ratio of 1: 3, extraction time 2min.
Adopt the chromium (VI) in the spectrophotometry organic phase, with the reagent blank is reference, measure the absorbance of complex in the 546nm place with the 1cm cuvette, find the amount (being about to the amount of uranium (IV) complete oxidation) of the chromium (VI) of correspondence then to the superfluous potassium dichromate in uranium (VI) back from working curve, thereby the amount of the potassium dichromate that consumes in the time of can calculating urania (IV), thereby the micrometric measurement of realization uranium content.
Claims (8)
1. the method for an extraction spectrophotometric method micrometric measurement uranium, comprise and take by weighing uranium sample, pre-service, readjust prices, add excessive potassium dichromate with U (IV) oxidation U (VI) to uranium (IV) back described the price modification to uranium (IV), the chromium (VI) that adds the organic solvent extraction surplus then, adopt the chromium in the spectrophotometry organic phase, it is characterized in that the excessive potassium dichromate of described adding accounts for 0.3%～0.5% of potassium dichromate total amount for the excess quantity that adds.
2. the method for a kind of extraction spectrophotometric method micrometric measurement uranium according to claim 1 is characterized in that, adds salting-out agents sodium chloride in the process of described extraction of chromium.
3. the method for a kind of extraction spectrophotometric method micrometric measurement uranium according to claim 1 is characterized in that, adds excessive potassium dichromate to uranium (IV) back and does not add vanadium sulfate acyl solution in U (IV) oxidation U (VI) process described the price modification.
4. the method for a kind of extraction spectrophotometric method micrometric measurement uranium according to claim 1 is characterized in that, the ratio of organic phase after the described extraction of chromium and water is 1: 2～1: 3.
5. the method for a kind of extraction spectrophotometric method micrometric measurement uranium according to claim 4 is characterized in that, the ratio of organic phase after the described extraction of chromium and water is 1: 3.
6. the method for a kind of extraction spectrophotometric method micrometric measurement uranium according to claim 1 is characterized in that described pre-service is for to add strong phosphoric acid, potassium bichromate solution, sulfuric acid solution, sulfaminic acid solution stirring successively with the uranium sample that takes by weighing.
7. the method for a kind of extraction spectrophotometric method micrometric measurement uranium according to claim 1, it is characterized in that described adding organic solvent extraction chromium (VI) is for adding behind surfactant Tritonx-100 solution, DPC solution, the organic solvent fully oscillation extraction successively.
8. according to the method for claim 1 or 7 described a kind of extraction spectrophotometric method micrometric measurement uranium, it is characterized in that described organic solvent is an isoamylol.
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| CN 201110097471 CN102262086B (en) | 2011-04-19 | 2011-04-19 | Method for precisely measuring uranium by extraction photometry |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207153A (en) * | 2013-03-11 | 2013-07-17 | 中国原子能科学研究院 | Precise determination method for small amount of uranium |
| CN106932529A (en) * | 2015-12-30 | 2017-07-07 | 中核北方核燃料元件有限公司 | A kind of UO2The assay method of uranium content in-BeO pellets |
| CN107576654A (en) * | 2017-08-11 | 2018-01-12 | 泰兴协联众达化学有限公司 | A kind of test device and method of testing of phthalic anhydride total acidity |
| 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 |
| CN110243778A (en) * | 2019-07-10 | 2019-09-17 | 福州大学 | The spectrophotometry of uranyl ion in a kind of measurement solution |
| CN110715922A (en) * | 2019-11-20 | 2020-01-21 | 福州大学 | Br-PADAP-uranyl ion spectrophotometry |
| 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 |
-
2011
- 2011-04-19 CN CN 201110097471 patent/CN102262086B/en active Active
Non-Patent Citations (4)
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| LEONARDO SENA GOMES TEIXEIRA等: "Spectrophotometric Determination of Uranium Using 2-(2-Thiazolylazo)-p-Cresol (TAC) in the Presence of Surfactants", 《J. BRAZ. CHEM. SOC.》 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207153A (en) * | 2013-03-11 | 2013-07-17 | 中国原子能科学研究院 | Precise determination method for small amount of uranium |
| CN106932529A (en) * | 2015-12-30 | 2017-07-07 | 中核北方核燃料元件有限公司 | A kind of UO2The assay method of uranium content in-BeO pellets |
| CN107576654A (en) * | 2017-08-11 | 2018-01-12 | 泰兴协联众达化学有限公司 | A kind of test device and method of testing of phthalic anhydride total acidity |
| 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 |
| CN110243778A (en) * | 2019-07-10 | 2019-09-17 | 福州大学 | The spectrophotometry of uranyl ion in a kind of measurement solution |
| CN110715922A (en) * | 2019-11-20 | 2020-01-21 | 福州大学 | Br-PADAP-uranyl ion spectrophotometry |
| 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 |
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