Method for measuring trace uranium in vanadium pentoxide by laser fluorescence method
A technology of vanadium pentoxide and a determination method, which is applied in the field of measuring trace uranium in vanadium pentoxide by laser fluorescence method, can solve the problems of easy failure, short service life of laser tube, etc., and achieves good precision and high accuracy , the effect of long life
Pending Publication Date: 2021-11-30
核工业二三〇研究所
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Problems solved by technology
However, the application in the past 20 years shows that the laser tube of this type of instrument works under high pressure and is prone to failure. The service life of the laser tube is relatively short, and the shelf life is usually about one year.
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[0046] 1. Experimental part
[0047] 1.1 Instruments and performance indicators
[0048] The best working conditions and parameters for the determination of trace uranium in vanadium pentoxide:
[0049] 1. Micro-measurement uranium instrument: MUA type, Nuclear Industry Beijing Institute of Geology;
[0050] 2. Measurement object: directly measure liquid samples. For solid samples, after conversion to liquid, they can be measured without separation, enrichment and proper dilution.
[0051] 3. Lower limit of detection (D.L): When defined as three times the standard deviation, D.L≤0.03×10 -9 g / mL
[0052] 4. Measurement accuracy (RSD): 1) The uranium concentration is between 0.1 and 2×10 -9 In g / mL range, RSD≤±8%; 2) Uranium concentration is between 2 and 20×10 -9 In g / mL range, RSD≤5%.
[0053] 5. Measuring range: 20×10 -9 g / mL. Can be extended to 10 if changing the sensitivity -6 g / mL scale.
[0054] 6. Instrument linearity: correlation coefficient ≥ 0.995.
[0055] 7...
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Abstract
The invention discloses a method for measuring trace uranium in vanadium pentoxide by a laser fluorescence method. A vanadium pentoxide sample is decomposed by a nitric acid, a hydrofluoric acid and a perchloric acid, uranium exists in a test solution in a uranyl ion (UO2 < 2 + >) state, the UO2 < 2 + > ions and a fluorescence enhancer form a stable complex under the condition that the pH value is 7-9, fluorescence is generated under the irradiation of an ultraviolet pulse light source, the fluorescence wavelengths are 500 nm, 522 nm and 546 nm respectively, the fluorescence intensity is in direct proportion to the uranium concentration in the test solution, and the problems of pollution of a vanadium pentoxide product to an instrument, relatively large deviation of a result and the like can be avoided to a certain extent so that the target of high-efficiency and high-quality analysis work is achieved.
Description
technical field [0001] The invention belongs to the field of uranium detection, in particular to a method for measuring trace uranium in vanadium pentoxide by a laser fluorescence method. Background technique [0002] Vanadium pentoxide is an amphoteric oxide, but it is mainly acidic. It volatilizes significantly above 700°C, and decomposes into oxygen and vanadium tetroxide at 700-1125°C. This characteristic makes it a catalyst for many organic and inorganic reactions. As a strong oxidizing agent, it is easily reduced to various low-valent oxides. Slightly soluble in water, easy to form a stable colloidal solution. It is very soluble in alkali and can generate vanadate (VO 3- ). Dissolved in strong acid (generally dissolves at pH=2 or so) does not generate vanadate ions, but generates oxyvanadium ions of the same valence (VO 2+ ). As a toxic substance, the maximum allowable amount in the air is less than 0.5mg / m 3 . Uranium is a natural radioactive element that exis...
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IPC IPC(8): G01N21/64
CPCG01N21/64
Inventor 姚杰祖张鑫宋茂生柳金良范鹏飞刘朝鄢飞燕
Owner 核工业二三〇研究所