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Method for measuring content of zirconium and impurity elements in uranium-zirconium alloy

A technology of impurity elements and determination methods, applied in the field of chemical detection, can solve problems such as unseen, element zirconium hydrolysis, loss, etc.

Pending Publication Date: 2020-06-19
CHINA NUCLEAR BAOTOU GUANGHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] There are relatively few detection methods for uranium-zirconium alloys at home and abroad, and most of them are mainly acid-soluble methods. Due to the insoluble characteristics of zirconium alloys, the addition of an appropriate amount of hydrofluoric acid can dissolve the sample well, and the addition of hydrofluoric acid will affect the The determination of some impurity elements will be affected; at the same time, if the hydrofluoric acid is removed, the element zirconium will be hydrolyzed, and some impurity elements will be co-precipitated and lost during hydrolysis.
Therefore, the dissolution of the sample and the elimination of the interference of the component element zirconium on other impurity elements are the focus and difficulty of the establishment of the detection method. Through literature research, there are no relevant reports in the existing literature, and there are no corresponding standards and patents.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1 sample dissolved

[0059] 1.1 Composition zirconium element:

[0060] Accurately weigh 0.1g sample, accurate to 0.0001g, place it in a 100mL quartz beaker, and prepare a mixed acid prepared from purified concentrated nitric acid and hydrochloric acid solution with a concentration of 6mol / L at a ratio of 1:3-1:4 Dissolve the sample in 3 mL of the solution. After the reaction is stable, add 0.3 mL of hydrofluoric acid dropwise. After the sample is completely dissolved, add 0.5 mL of 5% sulfuric acid solution. Evaporate the sample to about 2 mL, remove and cool to room temperature.

[0061] 1.2 Impurity elements:

[0062] Accurately weigh 0.5g sample, accurate to 0.0001g, place it in a 100mL quartz beaker, and prepare a mixed acid prepared from purified concentrated nitric acid and hydrochloric acid solution with a concentration of 6mol / L at a ratio of 1:3-1:4 Dissolve the sample in 3 mL of the solution. After the reaction is stable, add 0.5 mL of hydrofluoric acid dropw...

Embodiment 2

[0091] 1 sample dissolved

[0092] 1.1 Composition zirconium element:

[0093] Accurately weigh 0.1g sample, accurate to 0.0001g, put it in a 100mL quartz beaker, and prepare a mixed acid prepared from purified concentrated nitric acid and hydrochloric acid solution with a concentration of 9mol / L at a ratio of 1:3-1:4 Dissolve the sample in 3 mL of the solution. After the reaction is stable, add 0.4 mL of hydrofluoric acid dropwise. After the sample is completely dissolved, add 0.5 mL of 5% sulfuric acid solution. Evaporate the sample to about 2 mL, remove and cool to room temperature.

[0094] 1.2 Impurity elements:

[0095] Accurately weigh 0.5g sample, accurate to 0.0001g, put it in a 100mL quartz beaker, and prepare a mixed acid prepared from purified concentrated nitric acid and hydrochloric acid solution with a concentration of 9mol / L at a ratio of 1:3-1:4 Dissolve the sample in 3 mL of the solution. After the reaction is stable, add 0.75 mL of hydrofluoric acid dropwi...

Embodiment 3

[0124] 1 sample dissolved

[0125] 1.1 Composition zirconium element:

[0126] Accurately weigh 0.1g sample, accurate to 0.0001g, place it in a 100mL quartz beaker, and prepare a mixed acid prepared from purified concentrated nitric acid and hydrochloric acid solution with a concentration of 12mol / L at a ratio of 1:3-1:4 Dissolve the sample in 3 mL of the solution. After the reaction is stable, add 0.5 mL of hydrofluoric acid dropwise. After the sample is completely dissolved, add 0.5 mL of 5% sulfuric acid solution. Evaporate the sample to about 2 mL, remove and cool to room temperature.

[0127] 1.2 Impurity elements:

[0128] Accurately weigh 0.5g sample, accurate to 0.0001g, place it in a 100mL quartz beaker, and prepare a mixed acid prepared from purified concentrated nitric acid and hydrochloric acid solution with a concentration of 12mol / L at a ratio of 1:3-1:4 Dissolve the sample in 3 mL of the solution. After the reaction is stable, add 1.0 mL of hydrofluoric acid d...

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Abstract

The invention relates to a method for determining the content of zirconium and impurity elements in uranium-zirconium alloy. The method comprises the following steps: step 1, dissolving a sample; (1)dissolving a sample for measuring zirconium content; (2) dissolving a sample for determining the content of impurity elements; 2, extracting and separating a uranium matrix; (1) extracting and separating a uranium matrix from a zirconium element content sample; (2) extracting and separating a uranium matrix from a sample for determining the content of impurity elements; step 3, sample determination; (1) determining zirconium; and (2) determination of impurity elements. The detection method for determining the contents of the components and the impurity elements in the uranium-zirconium alloy through the plasma emission spectrometry is successfully established, the contents of the to-be-determined element impurities can be accurately determined by utilizing the experimental conditions listed in the content of the invention, accurate detection data is reported, and the method is effectively matched with special production.

Description

technical field [0001] The invention belongs to the field of chemical detection, and in particular relates to a method for determining the contents of zirconium and impurity elements in uranium-zirconium alloys. Background technique [0002] There are relatively few detection methods for uranium-zirconium alloys at home and abroad, and most of them are mainly acid-soluble methods. Due to the insoluble characteristics of zirconium alloys, the addition of an appropriate amount of hydrofluoric acid can dissolve the sample well, and the addition of hydrofluoric acid will affect the The determination of some impurity elements will be affected; at the same time, if the hydrofluoric acid is removed, the element zirconium will be easily hydrolyzed, and some impurity elements will be co-precipitated and lost during hydrolysis. Therefore, the dissolution of the sample and the elimination of the interference of the component element zirconium on other impurity elements are the key poin...

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/28
CPCG01N21/73G01N1/28
Inventor 马妍琳代燕赵竹霞
Owner CHINA NUCLEAR BAOTOU GUANGHUA CHEM IND
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