Analysis method for trace oxalic acid root in mother liquor of plutonium oxalate precipitation

A technology for precipitating mother liquor and analysis methods, applied in the direction of analysis materials, measuring devices, material separation, etc., can solve the problems of nitric acid interference, analysis time extension, etc., to avoid measurement interference, analysis time extension, high sensitivity and accuracy Effect

Active Publication Date: 2014-04-30
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when ion chromatography detects oxalate, it is easily interfered by nitric acid in the mother liquor, and the analysis time is prolonged. Therefore, it is necessary to establish a method for analyzing the concentration of oxalate with less matrix interference and high accuracy.

Method used

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  • Analysis method for trace oxalic acid root in mother liquor of plutonium oxalate precipitation

Examples

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Effect test

Embodiment 1

[0028] The analysis method of trace oxalate in the plutonium oxalate precipitation mother liquor, this method is to utilize chromatography to measure the oxalate content, and concrete steps are:

[0029] (1) Take a certain volume of 0.5mL simulated sample of the plutonium oxalate precipitation mother liquor, dilute it to 5mL with deionized water, and add 2g / L hydroxyurea solution to destroy the potassium permanganate in the plutonium oxalate precipitation mother liquor;

[0030] (2) Put the test solution obtained in step (1) on the IC-H column, where IC-H is a polystyrene-divinylbenzene strong acid column, and remove Na in the solution + 、K + , Mn 2+ Other cations;

[0031] (3) Put the solution collected in step (2) into a container and heat it at a temperature of 45°C. At the same time, the upper surface of the solution is blown with air until it is completely dry, and the air flow rate is 2L / min;

[0032] (4) Wash the beaker several times with deionized water, collect the...

Embodiment 2

[0039] The method and steps used in Example 1 are the same, except that the heating temperature used is 50° C., the air flow rate is 4 L / min, and the reducing agent used is N,N-dimethylhydroxylamine.

Embodiment 3

[0041] The method and steps used in Example 1 are the same, except that the sample solution is diluted 20 times, the heating temperature used is 58° C., the air flow rate is 6 L / min, and the reducing agent used is hydrazine.

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Abstract

The invention belongs to the technical field of spent fuel reprocessing, and discloses an analysis method for a trace oxalic acid root in a mother liquor of plutonium oxalate precipitation. The analysis method comprises the following steps that: (1) the mother liquor of plutonium oxalate precipitation is diluted by 10 to 20 times, and a reducing agent is added to destroy potassium permanganate in the mother liquor of plutonium oxalate precipitation; (2) the test solution prepared in the step (1) is placed on an IC - H column to remove the positive ions in the solution; (3) the solution collected in the step (2) is placed into a container and heated under a temperature condition of less than 60 DEG C, and a gas is used to purge the upper surface of the solution to full dry at the same time; (4) a beaker is washed with deionized water for many times, the washing liquor is collected for fixing a volume, and the content of the oxalic acid root in the solution is measured by an ion chromatography. The analysis method has the characteristics of small interference of matrix, high accuracy and simple device adopted.

Description

technical field [0001] The invention belongs to the technical field of spent fuel reprocessing, and in particular relates to a method for analyzing trace amounts of oxalate in plutonium oxalate precipitation mother liquor. Background technique [0002] In the Purex process, oxalic acid is usually used as a precipitant for plutonium at the plutonium product end to form a plutonium oxalate precipitate. The mother liquor after precipitation needs to be returned to the extraction process for further recovery of plutonium. The separation efficiency of uranium and plutonium in the mother liquor has a great influence, so the oxalic acid contained in the mother liquor should be removed as much as possible. Potassium permanganate is generally used to destroy the oxalate in the mother liquor, so that the concentration of oxalate is lower than 10 μg / mL. For this reason, it is necessary to establish a measurement method for trace amounts of oxalate, and determine the concentration of o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/12
Inventor 付建丽谈树苹吴继宗邓惟勤
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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