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Carbonyl compound analysis method in after-treatment technique process

A carbonyl compound and analysis method technology, applied in the field of carbonyl compound analysis in the post-processing process, can solve the problems of affecting carbonyl condensation reaction, solubility degree, methanol toxicity, etc., to reduce large errors, avoid water bath heating, and avoid precipitation Effect

Inactive Publication Date: 2013-10-02
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The methanol used in this method has certain toxicity, which is harmful to the health of personnel; the preparation of 1g / L 2,4-dinitrophenylhydrazine solution is difficult, and the degree of solubility is also affected by temperature; the absorbance is measured at 480nm, which is in the middle of the absorption line In the descending stage, a slight deviation of the absorption spectrum will cause an increased error; and no acid is added during the reaction process, which will also affect the progress of the carbonyl condensation reaction

Method used

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  • Carbonyl compound analysis method in after-treatment technique process
  • Carbonyl compound analysis method in after-treatment technique process
  • Carbonyl compound analysis method in after-treatment technique process

Examples

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Embodiment 1

[0032] In this example, using methyl nonyl ketone as a standard substance, dilute methyl nonyl ketone or samples with ethanol, and react with 1 g / L acidic 2,4-dinitrophenylhydrazine-ethanol-water solution at room temperature After a certain period of time, use KOH-ethanol-water solution to constant volume, develop color for 12±1min, and use a spectrophotometer to perform colorimetric analysis at the trough 490nm of the carbonyl compound absorption curve, as shown in figure 1 shown.

[0033] In this example, the method described in Example 1 of the present invention is also used to study the analysis of carbonyl compounds under conditions such as plutonium concentration in the organic phase, reduction and stripping in the post-treatment process, and acid-base washing in the reuse process of dirty solvents. The impact of the process provides a method for the analysis of carbonyl compounds in the process. The specific analysis steps and analysis results are as follows:

[0034] ...

Embodiment 2

[0065] In this example, ethyl octyl ketone was used as a standard substance, ethyl octyl ketone was diluted with ethanol, and reacted with 0.9 g / L acidic 2,4-dinitrophenylhydrazine-ethanol-water solution at room temperature for 30 ±2min, then dilute to volume with 110 g / L KOH-ethanol-water solution, develop color for 12±1min, and use a spectrophotometer to perform colorimetric analysis at the trough 492nm of the carbonyl compound absorption curve, as Figure 9 shown.

[0066] Can find out that the present invention has following remarkable effect according to above-mentioned embodiment:

[0067] 1) The present invention uses an acidic 2,4-dinitrophenylhydrazine-ethanol-water solution with an accurate concentration (0.8-1g / L), and measures the absorbance at the trough of the absorption spectrum at 490±2nm, which improves the accuracy of the measurement;

[0068] 2) The operation process of the method described in the present invention is safe and convenient, and is suitable fo...

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Abstract

The invention relates to a carbonyl compound analysis method in an after-treatment technique process, which belongs to the technical field of chemical analysis of a solvent radiolysis product. The method disclosed by the invention comprises the following steps of: diluting a standard substance, namely undecanone, or a sample through high-purity alcohol; reacting the diluted material with an acidic 2,4-dinitrophenylhydrazine-ethnaol-water solution at room temperature; making up to volume through a KOH-ethanol-water solution, and developing; and carrying out colorimetric analysis at a trough part of a carbonyl compound absorption curve by a spectrophotometer. The method disclosed by the invention is suitable for analysis on a carbonyl compound generated by radiolysis in an after-treatment process, and can reduce great errors caused by absorption peak excursion and prevent an operator from being in contact with methanol; the whole process can be carried out at room temperature and water-bath heating is avoided.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis of solvent radiolysis products, and in particular relates to a method for analyzing carbonyl compounds in a post-treatment process. Background technique [0002] The PUREX process, which uses tributyl phosphate (TBP)-diluent as the extraction solvent, is currently the only commercial water process for spent fuel reprocessing in the world. The solvent after extraction and stripping in the post-treatment process can be recycled and reused through acid-base washing. The radiolysis products of TBP are mainly DBP and MBP, which can be removed after acid-base washing, but the radiolysis products of the diluent cannot be removed by acid-base washing, and their slow accumulation will reduce the performance of the TBP extraction system, and even cause plutonium The retention of such metals affects the normal operation of the extraction process. Among them, carbonyl compound is an important di...

Claims

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Application Information

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IPC IPC(8): G01N21/31
Inventor 苏哲李辉波丛海峰宋凤丽刘占元王孝荣袁洁琼
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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