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Detection and Analysis Method of Methylphosphonic Acid

A technology of methylphosphonic acid and ion chromatography, which is applied in the field of ion detection and analysis, and the qualitative and quantitative detection and analysis of organic acids in complex phases, can solve the problems of requiring organic reagents and complicated sample pretreatment, and achieves simple and efficient sample pretreatment methods. The effect of high accuracy and small amount of sample

Inactive Publication Date: 2016-11-16
SHANGHAI UNIV
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Problems solved by technology

This method is more convenient than the former, saving time and money, but the sample pretreatment is still complicated and requires organic reagents
For the analysis of methylphosphonic acid in the organic phase solution, there is no literature report yet

Method used

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  • Detection and Analysis Method of Methylphosphonic Acid
  • Detection and Analysis Method of Methylphosphonic Acid
  • Detection and Analysis Method of Methylphosphonic Acid

Examples

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Embodiment Construction

[0032] Preferred embodiments of the present invention are described in detail as follows:

[0033] In this example, see Figure 1 ~ Figure 3 A method for detecting and analyzing methylphosphonic acid, using ion chromatography to analyze methylphosphonic acid, comprising the following steps:

[0034] 1. Preparation of 5000 ppm methylphosphonic acid standard solution: Accurately weigh 0.25g of methylphosphonic acid in a 50mL volumetric flask, dilute to the mark with ultrapure water, oscillate repeatedly, and dilute into standards of different concentrations as needed when using liquid;

[0035] 2. Pretreatment of irradiated samples: P350 / C with an absorbed dose of 200 kGy 12 h 26 / 2.0M HNO 3 The mixture sample is used as the sample to be tested, diluted with quantitative NaOH solution to a pH value greater than 7.0, centrifuged for 5min, and the lower aqueous phase is the sample extract;

[0036] 3. Preparation of the ion chromatograph: correctly load the anion chromatograp...

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Abstract

The invention discloses a method for detection and analysis of methylphosphonic acid. The steps are as follows: firstly, a standard product of methylphosphonic acid is dissolved in pure water to prepare a standard stock solution; , to obtain the ion chromatogram standard spectrum, draw the standard working curve of methylphosphonic acid; weigh the sample to be tested again, dilute with quantitative NaOH solution, centrifuge, and extract the lower layer of water phase as the sample extract to be tested; then in the same ion Under chromatographic conditions, carry out ion chromatographic analysis, measure the peak area of ​​the ion curve of the sample extract to be tested, use the standard working curve, obtain the methylphosphonic acid concentration in the sample extract to be tested by calculation, thereby obtain the formazan in the sample to be tested The concentration of phosphonic acid. The present invention adopts ion chromatography, which can quickly analyze methylphosphonic acid in the organic phase. The sample pretreatment is simple, does not involve organic reagents, and does not involve the derivation of methylphosphonic acid. The method of the present invention is accurate in analyzing methylphosphonic acid. higher.

Description

technical field [0001] The invention relates to an ion detection and analysis method, in particular to a qualitative and quantitative detection and analysis method for organic acids in complex phases, which is applied to the technical field of analytical chemistry. Background technique [0002] Methylphosphonic acid is a decomposition product of methylphosphonate, which is acidic and has the molecular formula CH 5 o 3 p. Soluble in water, slightly soluble in methanol, acetonitrile and other organic solvents. As the price, storage capacity and environmental pollution caused by conventional energy such as oil, natural gas and coal have become increasingly prominent, the status of nuclear power in the international energy structure has gradually increased. my country adopts the technical route of nuclear fuel closed cycle, that is, reprocessing spent fuel. Dimethylheptyl methylphosphonate (P350) is a promising extractant for spent fuel reprocessing. Spent fuel reprocessing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/64
Inventor 王锦花曹晓军张岚李瑞芬王聪聪张东平徐刚吴明红
Owner SHANGHAI UNIV
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