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Method for extracting and separating trace neptunium in liquid sample

A liquid sample and separation method technology, applied in the field of trace analysis sample pretreatment, can solve the problems of Np element loss, complicated process, laborious and other problems, achieve rapid separation and concentration, simplify the extraction and separation process, and achieve the best concentration effect

Inactive Publication Date: 2018-05-18
中国人民解放军陆军防化学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the TBP extraction chromatographic column only adsorbs tetravalent and hexavalent elements, and the pentavalent 237 Np elements are not adsorbed, resulting in pentavalent 237 Np element bleeds from the column
To avoid pentavalent 237 The Np element is lost from the column, and the 237 Np is adjusted to pentavalent, so that the liquid sample first passes through the TBP extraction chromatography column, and the uranium interfering elements are adsorbed and removed, and then the 237 Np is reduced to tetravalent, and then 7402 quaternary ammonium salt is used to extract the chromatographic column to absorb the tetravalent 237 Np element, but this process requires two-step extraction operation, the process is complex and laborious, and the addition of complexing agent is also harmful to the subsequent detection of inductively coupled plasma mass spectrometer (ICP-MS) when the 7402 quaternary ammonium salt extraction chromatography column is desorbed. influences

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Mix 60mL TOA and xylene as a solvent (V TOA :V 二甲苯 =1:4) was added into a beaker containing 30g polytetrafluoroethylene powder, then placed in a fume hood and stirred for 1h with an electromagnetic stirrer to make the xylene volatilize completely; 3 After the aqueous solution I was adjusted to a slurry state, the column was wet-packed, and the equipped chromatographic column was rinsed with 50mL deionized water first, and then the chromatographic column was equilibrated with 15mL nitric acid aqueous solution II with a concentration of 2.0mol / L, and the nitric acid was controlled. The flow rate of aqueous solution II is 1.5mL / min;

[0023] Wherein, the material of the chromatographic column used is glass, the inner diameter is 10mm, the bed height is 50mm, and the two ends of the chromatographic column are filled with polytetrafluoroethylene wire;

[0024] (2) Combine 5μg uranium and 5ng 237 Np was added to 10mL of nitric acid aqueous solution with a concentration...

Embodiment 2

[0028] (1) Mix 60mL TOA and xylene as a solvent (V TOA :V 二甲苯 =1:4) was added into a beaker containing 30g polytetrafluoroethylene powder, then placed in a fume hood and stirred for 1h with an electromagnetic stirrer to make the xylene volatilize completely; 3 After the aqueous solution I was adjusted to a slurry state, carry out wet packing, first wash the equipped chromatography column with 50mL deionized water, and then equilibrate the chromatography column with 15mL nitric acid aqueous solution II with a concentration of 2.0mol / L, and control the concentration of the nitric acid aqueous solution The flow rate of II is 1.5mL / min;

[0029] Wherein, the material of the chromatographic column used is glass, the inner diameter is 10mm, the bed height is 50mm, and the two ends of the chromatographic column are filled with polytetrafluoroethylene wire;

[0030] (2) Combine 5μg uranium and 5ng 237 Np was added to 10mL of nitric acid aqueous solution with a concentration of 2.0m...

Embodiment 3

[0034] (1) Mix 60mL TOA and xylene as a solvent (V TOA :V 二甲苯 =1:4) was added into a beaker containing 30g polytetrafluoroethylene powder, then placed in a fume hood and stirred for 1h with an electromagnetic stirrer to make the xylene volatilize completely; 3 After the aqueous solution I was adjusted to a slurry state, carry out wet packing, first wash the equipped chromatography column with 50mL deionized water, and then equilibrate the chromatography column with 15mL nitric acid aqueous solution II with a concentration of 2.0mol / L, and control the concentration of the nitric acid aqueous solution The flow rate of II is 1.5mL / min;

[0035] Wherein, the material of the chromatographic column used is glass, the inner diameter is 10mm, the bed height is 50mm, and the two ends of the chromatographic column are filled with polytetrafluoroethylene wire;

[0036] (2) Combine 5μg uranium and 5ng 237 Np was added to 10mL of nitric acid aqueous solution with a concentration of 2.0m...

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Abstract

The invention relates to a method for extracting and separating trace neptunium in a liquid sample, and belongs to the technical field of trace analysis sample pretreatment. According to the method, mainly trioctylamine is used as an extraction filling material, and the concentration of a leaching nitric acid solution is strictly controlled, such that the high distribution coefficient and the strong adsorption ability for neptunium are ensured while the interference caused by high abundance uranium is removed so as to achieve the good extraction and separation effect; the hot mixed acid solution of oxalic acid and nitric acid is used as an eluant, and the concentration of the mixed acid solution is strictly controlled, such that the neptunium recovery rate is high so as to achieve the goodconcentration effect; and with the extraction and separation method, the trace neptunium in the liquid sample can be simply and rapidly separated and concentrated, the trace neptunium analysis sensitivity under the uranium matrix interference can be improved, and the method has advantages of stable and reliable neptunium analysis result and good reproducibility.

Description

technical field [0001] The invention relates to an extraction and separation method, in particular to trace neptunium ( 237 The invention relates to an extraction and separation method of Np) element, which belongs to the technical field of trace analysis sample pretreatment. Background technique [0002] nothing natural on earth 237 Np, in the environment 237 Np comes from nuclear weapons testing and nuclear fuel reprocessing, the content is very low, and it is also interfered by the matrix of uranium during analysis. therefore, 237 The difficulty in the analysis of Np elements lies in the separation and separation of the uranium matrix. 237 Concentration of Np. Extraction chromatography is a separation method widely used in the separation of transuranic elements. It has a good separation effect, can separate and enrich trace and trace elements, and has the advantages of simple operation and easy implementation. At present, the use of extraction chromatography for tra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/40G01N1/34
CPCG01N1/34G01N1/405G01N1/4055G01N2001/4061
Inventor 赵晓光聂亚峰卢彩虹白晓波张爱红周黎明周建梅刘波王宁吉艳琴
Owner 中国人民解放军陆军防化学院
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