Method for determining residual quantity of anti-aging agent 4020 in rubber by high performance liquid chromatography-DAD method

A high-performance liquid chromatography and anti-aging agent technology, applied in the field of physical and chemical inspection of harmful substances in rubber, can solve the problems of poor sensitivity and quantitative accuracy, inability to perform quantitative detection, complicated operation, etc., and achieve short detection time and high detection efficiency. Lower limit and limit of quantitation, simple pre-treatment effect

Pending Publication Date: 2021-10-29
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above two methods can only be used for general qualitative or simple semi-quantitative detection, but cannot be used for quantitative detection.
And when anti-aging agent 4020 is detected (such as anti-aging agent 4020 in the rubber milk tube), the pretreatment method of pyrolysis or solvent extraction adopted needs to use equipment such as special instrument or extractor, heat source, etc. As a result, there are problems such as complicated operation, long time-consuming, poor method sensitivity and quantitative accuracy.

Method used

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  • Method for determining residual quantity of anti-aging agent 4020 in rubber by high performance liquid chromatography-DAD method
  • Method for determining residual quantity of anti-aging agent 4020 in rubber by high performance liquid chromatography-DAD method
  • Method for determining residual quantity of anti-aging agent 4020 in rubber by high performance liquid chromatography-DAD method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1 A kind of high performance liquid chromatography-DAD method measures the method for the residual amount of antioxidant 4020 in rubber

[0035] according to figure 1 The detection process, the detection method includes the following steps:

[0036] (1) Reagents and instruments

[0037] Anti-aging agent 4020 (TSC Shanghai Chemical Industry Development Co., Ltd.); acetonitrile and dichloromethane are both HPLC grade (Shanghai Macklin Biochemical Technology Co., Ltd.); distilled water meets the requirements of first-grade water in GB / T6682.

[0038] American Agilent G6125B / G7117C high performance liquid chromatography (with DAD detector)-DAD instrument; chromatographic column: Agilent EC-C18 (4.6×100mm, 2.7μm); 0.22μm needle filter (Guangzhou Qingfeng Biochemical Technology Co., Ltd. ); KQ5200DE CNC ultrasonic instrument (Kunshan Ultrasonic Instrument Co., Ltd.); UPTC ultrapure water machine (Shanghai Lichen Instrument Technology Co., Ltd.); AR224CN electroni...

Embodiment 2

[0048] Embodiment 2 A kind of high performance liquid chromatography-DAD method measures the method for the residual amount of antioxidant 4020 in rubber

[0049] Select another brand of natural rubber / styrene-butadiene rubber mixed rubber on Taobao, follow the sample pretreatment and measurement method described in Example 1, and measure the residual amount of antioxidant 4020 in the sample: 932 μg / g.

Embodiment 3

[0050] Embodiment 3 method detection limit and quantitative limit

[0051] With acetonitrile / dichloromethane mixed organic solvent (acetonitrile:dichloromethane=6:1) as solvent, prepare standard working curve, represent detection limit and limit of quantification with signal-to-noise ratio of 3 times and 10 times respectively, concrete preparation and The detection process is as shown in Example 1, and the results are shown in Table 1.

[0052] As can be seen from Table 1, the detection method of the present invention is used to detect the anti-aging agent 4020 in the rubber milk tube, and the detection limit is 0.005 μg / mL, and the quantification limit is 0.01 μg / mL.

[0053] Table 1 Method Standard Curve Equation, Correlation Coefficient, Detection Limit and Limit of Quantification

[0054]

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Abstract

The invention belongs to the technical field of physical and chemical inspection of harmful substance residues in rubber, and particularly relates to a method for determining the residual quantity of an anti-aging agent 4020 in rubber by a high performance liquid chromatography-DAD (Direct Amplification Detection) method, which comprises the following steps: preparing standard working solutions of the anti-aging agent 4020 with different concentration gradients, detecting by the HPLC-DAD method, quantifying by an external standard method, and drawing a peak area-concentration standard curve, so that a linear equation is obtained, the anti-aging agent 4020 in a rubber sample is extracted by adopting a convenient and simple soaking-ultrasonic extraction method, and finally, according to the peak area of the anti-aging agent 4020 measured by HPLC-DAD, the residual quantity of the anti-aging agent 4020 in the rubber is calculated through the linear equation. The method disclosed by the invention makes up the current situation that the existing detection method of the anti-aging agent 4020 is scarce, meanwhile, the method disclosed by the invention is simple in pretreatment, short in detection time and high in sensitivity, the detection limit and the quantitation limit are greatly reduced, and quantitative detection can be realized.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical inspection of harmful substance residues in rubber, and in particular relates to a method for measuring the residual amount of antioxidant 4020 in rubber by high performance liquid chromatography-DAD method. Background technique [0002] Rubber anti-aging agent 4020 belongs to p-phenylenediamine anti-aging agent. It is one of the main varieties with excellent performance in the amine anti-aging agent, and it is also one of the representative varieties of anti-aging agent in the future development; this anti-aging agent can not only resist ozone, oxygen, heat, Aging phenomena such as flex cracking can also inhibit harmful metals such as copper and manganese. It is often used in the preparation of natural rubber and various types of rubber. The application range includes pneumatic tire parts, solid tires, conveyor belts, rubber hoses, milk hoses, etc. . The structure of rubber antioxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/04G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74G01N30/86
CPCG01N30/482G01N2030/484G01N30/02G01N30/06G01N30/04G01N30/30G01N30/32G01N30/34G01N30/74G01N30/8679G01N2030/062G01N2030/065G01N2030/047G01N2030/3007G01N2030/324
Inventor 王志伟原晓喻胡长鹰
Owner JINAN UNIVERSITY
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