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Method for quantitatively measuring infinitesimal amount of uranium in steel

A quantitative measurement, extremely trace technology, applied in the preparation of test samples, fluorescence/phosphorescence, material excitation analysis, etc., can solve problems such as interference with the accuracy of measurement results, inability to directly determine the uranium content of iron and steel solutions, and achieve accurate measurement results. Reliable, small sampling volume and broad application prospects

Inactive Publication Date: 2014-02-19
CHINA INST FOR RADIATION PROTECTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the laser fluorescence method cannot directly measure the uranium content in molten iron and steel, because there are a large number of matrix metal ions in the dissolved iron and steel samples, which will seriously interfere with the accuracy of the measurement results

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Use an electronic balance to accurately weigh 1.0 g of smelted and decontaminated carbon steel shavings in a beaker, add 10 mL of 3 mol / L nitric acid to dissolve, then add 5 mL of 98 wt % concentrated sulfuric acid, heat and stir to make the solution Cool naturally to 30-40°C, add water to dissolve, transfer the obtained iron and steel sample solution to a 50mL volumetric flask to constant volume; adjust the pH value of the iron and steel sample solution to 3 with sodium hydroxide, add 10mL of ascorbic acid with a concentration of 2wt% The solution pretreats the steel sample solution, stirs and places it for 3 to 5 minutes; the pretreated solution flows through a 201-type strong alkaline anion exchange column at a flow rate of 2 to 3mL / min to absorb uranium, and then rinses with deionized water For the column, the washing rate is 2-3mL / min, until the effluent is dripped with potassium ferricyanide solution until the blue color does not appear; use 0.5mol / L nitric acid so...

Embodiment 2

[0021] Use an electronic balance to accurately weigh 0.6g of smelted and decontaminated stainless steel chips into a beaker, add 10mL of aqua regia to dissolve, then add 5mL of concentrated sulfuric acid with a concentration of 98wt%, heat and stir, and let the solution naturally cool to 30-40°C. Add water to dissolve, and transfer the obtained steel sample solution to a 50mL volumetric flask to constant volume; adjust the pH value of the sample solution to 2 with sodium hydroxide, add 5ml of ascorbic acid solution with a concentration of 5wt% to pretreat the steel sample solution, stir After leaving it for 3-5 minutes; flow the pretreated solution through a 201-type strong basic anion exchange column at a flow rate of 2-3mL / min to absorb uranium, and add deionized water to rinse the column at a rate of 2-3mL / min , and rinse until the effluent is not blue when adding potassium ferricyanide solution dropwise; use 1mol / L nitric acid solution as the analytical agent to analyze ura...

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Abstract

The invention relates to a method for quantitatively measuring an infinitesimal amount of uranium in steel. The method comprises the following steps: 1, dissolving a steel sample, naturally cooling to 30-40DEG C, and adding water for continuous dissolving to a constant volume; 2, adjusting the pH value of a steel sample solution obtained in step 1 to 1-3, and adding 1-5wt% of an ascorbic acid solution for pretreatment to fully reduce F3<3+> into Fe<2+>; 3, allowing the pretreated steel sample solution to flow through a highly basic anion exchange column for absorbing uranium, leaching the column with deionized water until no blue color appears when a potassium ferricyanide solution is added in a dropwise manner, resolving uranium with a nitric acid solution, collecting the uranium-enriched resolving solution in a volumetric flask, adjusting the pH value to 3-4, and adding a liquid to a constant volume; and 4, determining the concentration of uranium in the resolving solution through a laser fluorescence method, and reckoning the content of uranium in the steel sample. The method has the advantages of simple operation, small sample volume, accurate and reliable measure result, and very wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of uranium analysis and determination, and in particular relates to a method for quantitatively measuring extremely trace amounts of uranium in iron and steel. Background technique [0002] my country's current national standards or industry standards have methods for the analysis and determination of uranium in media such as air, water, soil, rocks, and organisms, but there is still a lack of methods for the analysis and determination of extremely trace amounts of uranium in steel samples. For example, in the decommissioning process of nuclear facilities, a large amount of uranium-contaminated steel will be produced. After these uranium-containing steels are smelted and decontaminated, the uranium content in the steel ingot will often drop to 1-10ppm, and the quantitative measurement value of the uranium content in the steel ingot is An important basis for judging how to use steel ingots. Due to the low co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64G01N1/40
Inventor 张涛革梁宇刘东张晓文安凯媛
Owner CHINA INST FOR RADIATION PROTECTION
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