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Method for determining purity of pyromellitic dianhydride by using liquid chromatography

A technology of pyromellitic dianhydride and liquid chromatography, which is applied in the field of measuring the purity of pyromellitic dianhydride by liquid chromatography, can solve the problem of measuring the purity of pyromellitic dianhydride and cannot directly detect pyromellitic acid Problems such as the purity of dianhydride, to achieve the effect of good stability, good reproducibility, and simple operation

Pending Publication Date: 2020-09-25
ANHUI GUOFENG PLASTIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the purity of pyromellitic dianhydride cannot be directly detected, there is no unified national standard to determine the purity of pyromellitic dianhydride

Method used

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  • Method for determining purity of pyromellitic dianhydride by using liquid chromatography
  • Method for determining purity of pyromellitic dianhydride by using liquid chromatography
  • Method for determining purity of pyromellitic dianhydride by using liquid chromatography

Examples

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Embodiment 1

[0031] A method utilizing liquid chromatography to measure the purity of pyromellitic dianhydride, comprising the following steps:

[0032] S1. Weigh an appropriate amount of the sample to be tested and the standard pyromellitic dianhydride, and prepare a solution of the sample to be tested and a standard solution with a concentration of 0.05g / L;

[0033] S2, carry out liquid chromatographic detection to described sample solution to be tested and standard solution with liquid chromatograph, the sample solution to be tested, standard solution are sequentially sampled, and the injection volume is 60uL, and chromatographic condition is: adopt three kinds Mobile phase carries out isocratic elution, mobile phase A is the triethylamine solution that concentration is 0.01mol / L, mobile phase B is methanol, mobile phase C is acetonitrile, the volume ratio of mobile phase A, mobile phase B, mobile phase C The flow rate of the mobile phase is 80:5:15, and the flow rate of the mobile phas...

Embodiment 2

[0036] A method utilizing liquid chromatography to measure the purity of pyromellitic dianhydride, comprising the following steps:

[0037] S1. Weigh an appropriate amount of the sample to be tested and the standard pyromellitic dianhydride, and prepare a solution of the sample to be tested and a standard solution with a concentration of 0.05g / L;

[0038] S2, carry out liquid chromatographic detection to described sample solution to be tested and standard solution with liquid chromatograph, the sample solution to be tested, standard solution are sequentially sampled, and the injection volume is 60uL, and chromatographic condition is: adopt three kinds Mobile phase carries out isocratic elution, mobile phase A is the triethylamine solution that concentration is 0.01mol / L, mobile phase B is methanol, mobile phase C is acetonitrile, the volume ratio of mobile phase A, mobile phase B, mobile phase C The flow rate of the mobile phase is 80:5:15, and the flow rate of the mobile phas...

Embodiment 3

[0041] A method utilizing liquid chromatography to measure the purity of pyromellitic dianhydride, comprising the following steps:

[0042] S1. Weigh an appropriate amount of the sample to be tested and the standard pyromellitic dianhydride, and prepare a solution of the sample to be tested and a standard solution with a concentration of 0.05g / L;

[0043] S2, carry out liquid chromatographic detection to described sample solution to be tested and standard solution with liquid chromatograph, the sample solution to be tested, standard solution are sequentially sampled, and the injection volume is 60uL, and chromatographic condition is: adopt three kinds Mobile phase carries out isocratic elution, mobile phase A is the triethylamine solution that concentration is 0.01mol / L, mobile phase B is methanol, mobile phase C is acetonitrile, the volume ratio of mobile phase A, mobile phase B, mobile phase C The flow rate of the mobile phase is 80:5:15, and the flow rate of the mobile phas...

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Abstract

The invention discloses a method for measuring purity of pyromellitic dianhydride by liquid chromatography, which comprises the following steps: S1, weighing a proper amount of sample to be measured and a pyromellitic dianhydride standard substance, and preparing a sample solution to be measured and a standard substance solution; S2, respectively carrying out liquid chromatography detection on theto-be-detected sample solution and the standard substance solution by using a liquid chromatograph, adopting three mobile phases for isocratic elution, the mobile phase A being a triethylamine solution with the concentration of 0.01 mol / L, the mobile phase B being methyl alcohol, the mobile phase C being acetonitrile, and recording chromatograms of the to-be-detected sample solution and the standard substance solution; and S3, comparing the chromatograms of the to-be-detected sample solution and the standard substance solution, determining the peak positioning of pyromellitic dianhydride in the chromatogram of the to-be-detected sample solution according to the retention time, and calculating the purity of pyromellitic dianhydride in the to-be-detected sample by adopting an area normalization method. The method disclosed by the invention is simple to operate, good in stability and good in reproducibility.

Description

technical field [0001] The invention relates to the technical field of substance purity analysis, in particular to a method for measuring the purity of pyromellitic dianhydride by liquid chromatography. Background technique [0002] Pyromellitic dianhydride is white crystal, soluble in dimethyl sulfoxide and dimethyl formamide. It is mainly used to make polyimide resin, high temperature resistant electrical insulating varnish, PVC plasticizer, synthetic resin crosslinking agent and epoxy resin curing agent, and is also used to make phthalocyanine blue dye, etc. It is an important chemical raw material. Since the purity of pyromellitic dianhydride cannot be directly detected, there is no unified national standard to measure the purity of pyromellitic dianhydride. Contents of the invention [0003] Based on the technical problems existing in the background technology, the present invention proposes a method for measuring the purity of pyromellitic dianhydride by liquid chro...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74G01N30/86G01N2030/324
Inventor 孙小强程露何祥勇
Owner ANHUI GUOFENG PLASTIC