Capillary electrophoresis uantitative analytical method for impurities content in refined p-phthalic acid

A technology of purified terephthalic acid and capillary electrophoresis, which is applied in the direction of material analysis, analysis material, and measurement device by electromagnetic means, which can solve the requirements of instrument stability and sampling accuracy, the time-consuming external standard method, and the measurement accuracy. Not high problems, to achieve reliable quality control method, easy operation, good accuracy and repeatability

Inactive Publication Date: 2009-07-22
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The capillary electrophoresis method can adopt the external standard method and the internal standard method for quantitative analysis. At present, in PTA, the method for measuring p-TOL, 4-CBA and BA is the quantitative analysis of the external standard method, but the external standard method has great influence on the stability and stability of the instrument. Sampling accuracy is critical, and a calibration curve needs to be determined before each measurement
Therefore, in actual analysis, the external standard method is time-consuming and the measurement accuracy is not high.

Method used

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  • Capillary electrophoresis uantitative analytical method for impurities content in refined p-phthalic acid
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  • Capillary electrophoresis uantitative analytical method for impurities content in refined p-phthalic acid

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Experimental program
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Embodiment

[0033] 1. Accurately weigh 1.0000g of p-TOL and S, and place 0.1000g of 4-CBA and BA in a 100mL volumetric flask, add 14mL of ammonia solution to dissolve each, dilute to the mark with water and shake well.

[0034] 2. In five 50mL volumetric flasks, weigh 1.0000g of pure PTA, add 14mL of ammonia solution to dissolve it, then add different volumes of p-TOL, 4-CBA, BA and S, electrophoresis detection, according to p- TOL, 4-CBA, BA and S peak area ratio and mass ratio to calculate the respective relative correction factors, see the table:

[0035] serial number

[0036] serial number

[0037] serial number

[0038] The calibration factor of the component has a certain linear relationship with the area ratio of the internal standard compound and the component, so the mass ratio of the component to the internal standard compound is the ordinate, and the peak area ratio of the component to the internal standard compound is the abscissa to draw the stan...

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Abstract

The related CE inner-scaling analysis method for the impurity in fine TPA comprises: selecting one of PPA, PMXPA and PTBBA as the inner scale, and quantitative analyzing the impurity content in the fine TPA. This invention is simple and fast for real-time monitor and analysis.

Description

technical field [0001] The present invention is a capillary electrophoresis internal standard quantitative analysis method of impurity content in purified terephthalic acid, specifically p-toluic acid (p-TOL) and p-carboxybenzene in purified terephthalic acid (PTA). A capillary electrophoresis internal standard quantitative analysis method for the content of formaldehyde (4-CBA) and benzoic acid (BA). Background technique [0002] PTA is one of the important organic chemical raw materials. It is mainly used for esterification polymerization with ethylene glycol to produce PET polyester (polyethylene terephthalate) chips and polyester fibers. Among many polyester products, PET is widely used in chemical fiber, film, insulating material, beverage packaging and other fields due to its excellent performance. As a monomer of PET, the quality of PTA directly affects the success or failure of the polymerization reaction. In particular, the main impurities in PTA, 4-CBA and p-TOL, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/447G06F19/00
Inventor 康经武王兆彦
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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