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Method for detecting primary amine in anti-aging agents TMQ

A detection method and technology for an anti-aging agent are applied in the detection field of primary amines, which can solve the problems of inability to measure the content of primary amines, inability to completely detect the content of primary amines, etc., and achieve the effects of simple operation, simple instrument and high accuracy.

Inactive Publication Date: 2013-01-16
KEMAI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But now only the HPLC method is used to determine the aniline content of one of the primary amines, and the HPLC method cannot be used to determine the content of all primary amines
Existing methods cannot fully detect the content of primary amines, but can only detect the content of aniline in primary amines

Method used

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  • Method for detecting primary amine in anti-aging agents TMQ
  • Method for detecting primary amine in anti-aging agents TMQ
  • Method for detecting primary amine in anti-aging agents TMQ

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 0.1044g of analytically pure aniline and dissolve it in 30ml of 2N hydrochloric acid in a 100ml volumetric flask. Then, the solution was diluted with methanol to the mark of the volumetric flask as an aniline standard solution.

[0042] Use a pipette to transfer 1ml, 2ml, 3ml, 4ml, 5ml, 6ml of aniline standard solution into six 100ml volumetric flasks, and then add 2N hydrochloric acid solution 39ml, 38ml, 37ml, 36ml, 35ml, 34ml in sequence. Add 20ml of DMAB solution to the solution, then add methanol to fill most of the remaining volume, and swirl gently to mix the solution. Let stand for 5 minutes and dilute to the mark with methanol.

[0043] After 45 minutes of reaction, use methanol as a reference and record the maximum absorbance at about 437nm:

[0044]

[0045] Weigh 0.7257g of TMQ sample and dissolve it in 50ml of chloroform with a separatory funnel. Then, 50ml of 2N hydrochloric acid was added and shaken rapidly for 2 minutes. After separation int...

Embodiment 2

[0053] Take 8 parts in parallel with the same antiaging agent TMQ sample, utilize the calibration curve that makes among the embodiment one, carry out sample analysis by the analytical operation method in the embodiment, the result is as follows:

[0054]

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Abstract

The invention relates to a method for detecting primary amine in anti-aging agents TMQ. The method comprises the following steps of: preparing aniline standard solutions with different concentrations and a standard reference solution, respectively measuring the absorbance of the different aniline standard solutions under the condition of the wavelength of 437 nanometers by using an ultraviolet and visible spectrophotometer and the 1cm optical path of a cuvette, and drawing a standard curve of the aniline standard solutions by using the standard reference solution as a comparison solution; measuring the absorbance of a sample solution by the same method by using a sample reference solution as a comparison solution; performing quantitative analysis by the aniline standard curve to obtain the content of the primary amine in the anti-agents TMQ in a sample. By the method, the content of the primary amine in the anti-aging agents TMQ can be accurately detected, instruments are simple, and the method is easy and convenient to operate and high in accuracy.

Description

technical field [0001] The invention relates to a method for detecting primary amines, in particular to a method for detecting primary amines in rubber anti-aging agent 2,2,4-trimethyl-1,2-dihydroquinoline polymer (TMQ). The invention belongs to the technical field of rubber antioxidant analysis. Background technique [0002] Anti-aging agent TMQ is one of the varieties of rubber anti-aging agents with excellent performance. The existence of the harmful component primary amine in this product will affect the reversion of insoluble sulfur. When the content of primary amine is high, the unvulcanized rubber made with it is prone to Blooming phenomenon. The detection of primary amine content is an important means to ensure the quality of antioxidant TMQ. But now only the HPLC method is used to measure the aniline content of one of the primary amines, and the HPLC method cannot be used to determine the content of all primary amines. The existing methods cannot completely detec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
Inventor 朱洁
Owner KEMAI CHEM
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