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Analytical method of hydroxylamine when hydroxysemicarbazide coexists

A hydroxysemicarbazide and analysis method technology, applied in the field of hydroxylamine analysis, liquid chromatography analysis of hydroxylamine analysis, can solve the problems that have not been reported in the literature such as the analysis method of hydroxysemicarbazide hydroxylamine, and achieve high sensitivity, good repeatability, and simple operation Effect

Active Publication Date: 2021-01-12
SHANGHAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, no method for the analysis of hydroxylamine in the presence of semicarbazide has been reported in the literature

Method used

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  • Analytical method of hydroxylamine when hydroxysemicarbazide coexists
  • Analytical method of hydroxylamine when hydroxysemicarbazide coexists
  • Analytical method of hydroxylamine when hydroxysemicarbazide coexists

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Embodiment Construction

[0027] Below in conjunction with specific implementation example, above-mentioned scheme is described further, and preferred embodiment of the present invention is described in detail as follows:

[0028] Main experimental instruments:

[0029] Agilent 1100 high performance liquid chromatography, including online degassing device, quaternary pump, column thermostat and ultraviolet detector, chemical workstation.

[0030] In this embodiment, a method for analyzing hydroxylamine when hydroxycarbazide coexists, using chemical derivatization and liquid chromatography to analyze hydroxylamine, includes the following steps:

[0031] 1) Preparation of hydroxylamine standard solution:

[0032] The amount of solvent added according to the volume ratio is accurately prepared with the standard substance hydroxylamine 2.0×10 -3 mol / L hydroxylamine standard solution; take seven 10mL volumetric flasks, add 1.0ml to the concentration of 2×10 -3 mol / L hydroxycarbazide, and then add differe...

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Abstract

The invention discloses a hydroxylamine analysis method in a coexistence of amino hydroxyl urea. The method comprises the following steps of neutralizing and diluting a to-be-detected amino hydroxyl urea coexisting sample, then putting into a volumetric flask, adding a nitrobenzaldehyde solution, then carrying out constant volume and evenly shaking by using an acetic acid solution, and standing atroom temperature; then, analyzing the to-be-detected sample by using a method for combining a high performance liquid chromatography column and an ultraviolet detector so as to obtain the peak area of hydroxylamine, and calculating to obtain the concentration of hydroxylamine in the to-be-detected sample by using a standard working curve of hydroxylamine. The lowest detecting concentration of hydroxylamine can reach 2 * 10 <-7> mol / L, and the relative standard deviation of the analysis method of the embodiment is 0.8%. According to the method, chemical derivatization - liquid chromatography method is established to analyze hydroxylamine, and analysis of hydroxylamine is not influenced by liquid chromatography method, the method is simple to operate, high in sensitivity and good in repeatability.

Description

technical field [0001] The invention relates to a method for analyzing hydroxylamine, in particular to a method for analyzing hydroxylamine by liquid chromatography, which is applied to the technical field of analytical chemistry. Background technique [0002] my country is vigorously developing nuclear power, and the rapid development of nuclear power will inevitably produce a large amount of spent fuel, that is, used nuclear fuel. These nuclear fuels are highly radioactive, and will pose a great threat to the environment and ecology if left untreated. If the spent fuel is reprocessed, not only the unused nuclear fuel uranium-235 and the newly generated nuclear fuel plutonium-239 can be recovered, but also the volume of radioactive nuclear waste can be greatly reduced, thereby facilitating the final disposal of radioactive waste. Semicarbazide is a new salt-free reducing agent used for the separation of uranium from plutonium and ammonium in the reprocessing of spent fuel....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/74
CPCG01N30/02G01N30/74
Inventor 王锦花王平石莹杨卓王思宇肖松涛欧阳应根
Owner SHANGHAI UNIV
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