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Method for detecting N,N-diglycidyl-4-glycidol-oxo-aniline in plastic product

A technology of diglycidyl and glycidyl oxygen is applied in the field of analysis and detection to achieve the effects of good reproducibility, low detection limit and increasing analyte content

Active Publication Date: 2018-06-22
GUANGZHOU GRG METROLOGY & TEST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It can be seen that it is very necessary to establish an appropriate method to determine the content of N,N-diglycidyl-4-glycidyloxyaniline in the product. However, most of the detection of such compounds is aminophenol. Rare reports on the detection of residual N,N-diglycidyl-4-glycidyloxyaniline in products

Method used

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  • Method for detecting N,N-diglycidyl-4-glycidol-oxo-aniline in plastic product

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for detecting N,N-diglycidyl-4-glycidyloxyaniline in plastic products, comprising the steps of:

[0031] S1. Sample pretreatment: take a representative plastic sample A, cut it into pieces, the largest size does not exceed 2 mm, weigh 1.0 g (accurate to 0.1 mg) of the sample, put it into a 60 ml reaction bottle, add 10 ml of acetone solvent, Put the cap tightly and put it into an ultrasonic cleaner, set the temperature at 60°C, and extract for 60 minutes. After taking it out, cool it to room temperature, take the extraction solution for centrifugation, filter the sample with a 0.45 μm filter membrane, and put it into the injection vial;

[0032] S2. Perform qualitative and quantitative tests on the gas chromatography-mass spectrometer on the above-mentioned sample to be tested,

[0033] Preparation of standard solution: Accurately weigh 10 mg of N,N-diglycidyl-4-glycidyloxyaniline standard substance with a precision electronic analytical balance (the specific s...

Embodiment 2

[0038] Embodiment 2 detection result

[0039] (1) The peak of N,N-diglycidyl-4-glycidyloxyaniline

[0040] figure 1 with figure 2 It is the gas chromatogram and mass spectrogram of N,N-diglycidyl-4-glycidyloxyaniline, obtained by figure 1 and figure 2 It can be seen that through the optimal setting of the instrument analysis parameters, N,N-diglycidyl-4-glycidyloxyaniline can obtain symmetrical chromatographic separation peaks within 13.2 minutes. When acetone is used as the extraction solvent, the There is less matrix interference.

[0041] (2) Standard working curve equation

[0042] Table 1 and image 3 is the linearity and linear correlation coefficient of N,N-diglycidyl-4-glycidyloxyaniline, from Table 2 and image 3 The standard working curve of N,N-diglycidyl-4-glycidyloxyaniline shows that in the concentration range of 0.5 mg / L~10mg / L, N,N-diglycidyl-4-glycidyl The linear correlation coefficient R of oxyaniline 2 It is 0.9991, meeting the test requirements ...

Embodiment 3

[0056] A method for detecting N,N-diglycidyl-4-glycidyloxyaniline in plastic products, comprising the steps of:

[0057] S1. Sample pretreatment: Take a representative plastic sample A, cut it into pieces, the largest size does not exceed 2 mm, weigh 1.0 g (accurate to 0.1 mg) sample, put it into a 60 ml reaction bottle, add 10 ml of toluene solvent, Put the cap tightly into an ultrasonic cleaner, set the temperature at 60°C, and extract for 60 minutes. After taking it out, cool it to room temperature, take the extraction solution for centrifugation, filter the sample with a 0.45 μm filter membrane, and put it into a sample injection vial;

[0058] S2. The gas chromatography-mass spectrometry instrument is used to perform qualitative and quantitative tests on the above-mentioned sample to be tested, and the gas chromatography and mass spectrometry conditions are the same as in Example 1.

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Abstract

The invention discloses a method for detecting N,N-diglycidyl-4-glycidol-oxo-aniline in a plastic product. The method comprises the following steps: S1, performing sample pretreatment, namely putting5-20ml of an organic solvent into 0.1-1.0g of a sample, performing ultrasonic extraction for 45-120 minutes at 40-70 DEG C, cooling to a room temperature, and filtering so as to obtain a sample to betested; S2, preparing a standard solution of N,N-diglycidyl-4-glycidol-oxo-aniline; S3, performing qualitative quantitative testing on the sample to be tested by using a gas chromatograph-mass spectrometer. The invention establishes a method for testing N,N-diglycidyl-4-glycidol-oxo-aniline in a plastic product by using gas chromatograph-mass spectrometry, and the method is simple, convenient andrapid, small in matrix interference and excellent in separation effect. Under an optimal analysis condition, the time of a symmetric spectrum separation peak is 13.2 minutes, the method is low in detection limit, good in precision and high in sample adding standard recovery rate, and testing requirements of N,N-diglycidyl-4-glycidol-oxo-aniline in plastics can be met.

Description

technical field [0001] The invention relates to the field of analysis and detection, and more specifically relates to a detection method for N,N-diglycidyl-4-glycidyloxyaniline in plastic products. Background technique [0002] N,N-diglycidyl-4-glycidyloxyaniline, TGPAP for short, with molecular formula C15H19NO4, is a reddish-brown viscous liquid, easily soluble in acetone, ethanol, ether and other organic solvents. N,N-diglycidyl-4-glycidyloxyaniline, as an important intermediate, is widely used in many fields such as industrial formulations, adhesives, polymer materials, and fine chemicals. Although it has good chemical properties, studies have confirmed that it is irritating to the eyes, respiratory system and skin, may cause genetic defects, and may cause organ damage after long-term or repeated exposure. Because of its persistent, bioaccumulative and toxic hazards, it has attracted great attention from all walks of life. Recently, according to the proposal of the Dani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 李支薇王华严洪连林炼锋
Owner GUANGZHOU GRG METROLOGY & TEST CO LTD
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