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High performance liquid chromatographic analysis method for pyromellitic dianhydride

A technology of pyromellitic dianhydride and high performance liquid chromatography, which is applied in the field of analysis, can solve the problems of difficult testing, cumbersome process, and high boiling point, and achieve simple sample processing and analysis procedures, good chromatographic peak shape, and reproducible good sex effect

Inactive Publication Date: 2014-08-06
常熟联邦化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Pyromellitic dianhydride has a large molecular weight (218.12) and a high boiling point (398°C). It is difficult and ineffective to analyze and test its purity by conventional methods.
At present, the industry mostly uses gas chromatography to analyze the purity and organic impurities of pyromellitic dianhydride. This method has high measurement accuracy and precision, but it must undergo two-step esterification reaction to convert the sample into low-boiling esters. The analysis process is cumbersome, and the degree of esterification will affect the accuracy of the test results
In addition, it has also been reported that reversed-phase liquid chromatography using distilled water as the mobile phase can quantitatively detect pyromellitic dianhydride. The principle is mainly to convert pyromellitic dianhydride into pyromellitic acid, and then detect Indirect analysis of pyromellitic acid with formic acid can effectively realize the detection of various organic impurities, but the inherent pyromellitic acid in the sample seriously affects the accuracy of the analysis results

Method used

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Embodiment 1

[0040] 1. Prepare 1L mobile phase: Accurately weigh 1g of tetramethylammonium bisulfate and dissolve it in 100mL of acetonitrile. After ultrasonic oscillation for 1-10min, add 600mL of n-hexane and 300mL of tetrahydrofuran in sequence, ultrasonically oscillate for 30-60min to mix evenly, and use 0.45 Filter through a μm membrane for later use.

[0041] 2. Prepare PMDA standard solutions with concentrations of 20 mg / L, 40 mg / L, 80 mg / L, 120 mg / L and 160 mg / L: Accurately weigh 25-2000 mg of PMDA standard product to the nearest 0.1 mg, and place In a 50mL volumetric flask, dilute to the mark with the above-mentioned mobile phase, mix evenly by ultrasonication for 5min, seal and cool and let stand, when the liquid in the volumetric flask returns to the scale line, accurately pipette 2mL of the solution into a 50mL volumetric flask, and use The mobile phase was diluted to the mark, mixed by ultrasonication for 5 minutes, and then filtered with a 0.45 μm filter membrane.

[0042] 3...

Embodiment 2

[0049] Based on the standard curve in Example 1, PMDA sample A solution was prepared and analyzed. Accurately weigh PMDA sample A 1000mg, preparation method, chromatographic conditions and integral calculation method are with embodiment 1 thereafter. The spectrum is attached Figure 4 As shown, the purity of the sample was 99.80%.

Embodiment 3

[0051] Based on the standard curve in Example 1, PMDA sample B solution was prepared and analyzed. Accurately weigh the PMDA sample B 1000mg, and then the preparation method, chromatographic conditions and integral calculation method are the same as in Example 1. The spectrum is attached Figure 5As shown, the purity of the sample was 95.73%.

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Abstract

The invention discloses a high performance liquid chromatographic analysis method for pyromellitic dianhydride. The method comprises the following steps: (1) adopting chromatographic conditions, (2) preparing a mobile phase, (3) preparing a PMDA standard solution, (4) building a standard curve, (5) preparing a PMDA sample solution, and (6) carrying out quantitative analysis by using an external standard percentage method. The invention provides the method for quantitatively analyzing pyromellitic dianhydride, which fills the technological gaps of corresponding fields. The method has the advantages of simple sample treatment and analytical procedure process, good peak shape, high analysis result accuracy, good reproducibility and the like and has an important practical significance in the fields of quality analysis and quality control of PMDA.

Description

technical field [0001] The invention relates to the technical field of analysis, in particular to a high performance liquid chromatography analysis method of pyromellitic dianhydride. Background technique [0002] Pyromellitic dianhydride (PMDA) is mainly used in the production of polyimide films, engineering plastics, coating additives, plastic additives and adhesives, etc. Among them, polyimide has excellent mechanical and electrical properties , physical and chemical properties, are widely used in electromechanical, aerospace, nuclear energy and electronics industries and many other fields. Since the performance of polyimide is greatly affected by the purity of pyromellitic dianhydride, in recent years, polyimide manufacturers have put forward higher requirements for the purity of pyromellitic dianhydride. [0003] The structural formula of pyromellitic dianhydride is as follows: [0004] [0005] Pyromellitic dianhydride has a large molecular weight (218.12) and a h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 张京通赵海峰陈燕丹陈丽萍柏彩萍袁敏红
Owner 常熟联邦化工股份有限公司
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