Method for detecting pyromellitic dianhydride based on Raman spectrum

A technology of Raman spectroscopy and detection method, which is applied in the field of homogenous anhydride detection based on Raman spectroscopy, can solve the problems of content deviation, it is difficult to ensure that homogenous anhydride does not hydrolyze, etc., and achieves short pretreatment time, avoids hydrolysis, and is convenient and quick to operate. Effect

Pending Publication Date: 2022-03-04
JIANGSU HUALUN CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is difficult to ensure that the homoanhydride will not be hydrolyzed during the pretreatment process, which will lead to huge deviations in the content

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In the first step, weigh 1 ± 0.05g of a homoanhydride sample with a known homoanhydride content of 98.24% and dissolve it in 100mL of ethyl acetate to prepare a homoanhydride sample solution;

[0033] In the second step, a Raman spectrometer with an excitation laser wavelength of 532nm, 785nm or 1064nm is selected to perform Raman spectrum detection on the homoanhydride sample solution;

[0034] The third step is to use the Origin integral to open the Raman spectrum data, and select the wavenumber at 278cm -1 、291cm -1 、495cm -1 、647cm -1 、758cm -1 、1301cm -1 、1325cm -1 、1625cm -1 、1792cm -1 、1866cm -1 The Raman peak is used as the characteristic peak;

[0035] In the fourth step, the Gaussian function or Lorentzian function is used for fitting, and the average anhydride sample content of 98.30% is calculated by using the established average anhydride Raman data model.

Embodiment 2

[0037] In the first step, weigh 1 ± 0.05g of a homoanhydride sample with a known homoanhydride content of 98.86% and dissolve it in 100mL of ethyl acetate to prepare a homoanhydride sample solution;

[0038] In the second step, a Raman spectrometer with an excitation laser wavelength of 532nm, 785nm or 1064nm is selected to perform Raman spectrum detection on the homoanhydride sample solution;

[0039] The third step is to use the Origin integral to open the Raman spectrum data, and select the wavenumber at 278cm -1 、291cm -1 、495cm -1 、647cm -1 、758cm -1 、1301cm -1 、1325cm -1 、1625cm -1 、1792cm -1 、1866cm -1 The Raman peak is used as the characteristic peak;

[0040] In the fourth step, the Gaussian function or Lorentzian function is used for fitting, and the average anhydride sample content of 98.91% is calculated by using the established average anhydride Raman data model.

Embodiment 3

[0042] In the first step, weigh 1 ± 0.05g of a homoanhydride sample with a known homoanhydride content of 99.61% and dissolve it in 100mL of ethyl acetate to prepare a homoanhydride sample solution;

[0043] In the second step, a Raman spectrometer with an excitation laser wavelength of 532nm, 785nm or 1064nm is selected to perform Raman spectrum detection on the homoanhydride sample solution;

[0044] The third step is to use the Origin integral to open the Raman spectrum data, and select the wavenumber at 278cm-1 、291cm -1 、495cm -1 、647cm -1 、758cm -1 、1301cm -1 、1325cm -1 、1625cm -1 、1792cm -1 、1866cm -1 The Raman peak is used as the characteristic peak;

[0045] The fourth step is to fit the Gaussian function or the Lorentz function, and use the established homogeneous anhydride Raman data model to calculate the homogeneous anhydride sample content of 99.57%.

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Abstract

The invention relates to a pyromellitic dianhydride detection method based on Raman spectrum, which comprises the following steps: weighing 1 + / -0.05 g of pyromellitic dianhydride sample and dissolving in 100mL of anhydrous organic solvent to prepare a high-content pyromellitic dianhydride solution; performing Raman spectrum detection on the high-content pyromellitic dianhydride solution; origin integral is adopted to open Raman spectrum data, characteristic peak height or peak area data is fitted through a Gaussian function or a Lorentz function, a pyromellitic dianhydride Raman data model is established, and the pyromellitic dianhydride content in a sample is calculated through the pyromellitic dianhydride Raman data model. The method can avoid hydrolysis of pyromellitic dianhydride in the detection process, can directly detect the content of pyromellitic dianhydride, and is short in pretreatment time and simple to operate.

Description

technical field [0001] The invention relates to a method for detecting homoanhydride based on Raman spectroscopy. The method adopts Raman spectroscopy technology as a detection means, detects the Raman scattering signal of the sample, and models the obtained Raman spectral data. The model quantifies the mean anhydride content. Background technique [0002] Homoanhydride is a main raw material of polyimide, which has broad development and practical value. Due to the high boiling point of homoanhydride, easy hydrolysis, sublimation and other properties, the content detection of homoanhydride has become a difficult problem. At present, there are two main methods for the detection of homoanhydride content: gas chromatography and high performance liquid chromatography, both of which require long-term pretreatment of samples to convert homoanhydride into other substances for detection. During the pretreatment process, it is difficult to ensure that the homoanhydride does not und...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/65
Inventor 陈忠平戴鑫冯建平潘学林李茉
Owner JIANGSU HUALUN CHEM
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