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Liquid chromatogram analysis method for rubber sulfuration accelerant MBTS

A liquid chromatographic analysis and rubber vulcanization technology is applied in the field of liquid chromatographic analysis of dibenzothiazole disulfide, a rubber vulcanization accelerator, and can solve the problems of large errors and high analysis results, and achieves small errors, simple process and high accuracy. high effect

Inactive Publication Date: 2009-06-24
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the analysis method of MBTS purity is mainly based on QB-2001.02. The analysis results obtained by this method are generally high and the error is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0009] Weigh 10 mg of MBTS sample with a high-angle weighing bottle, add 20 ml of dichloromethane with a concentration of 95% to it, put it in an ultrasonic cleaner and vibrate for 5 minutes, transfer it to a 100 ml volumetric flask after taking it out, and use a concentration of 95% dichloromethane Dilute dichloromethane to the mark, shake well, and filter; keep the room temperature at 20°C, use water and methanol as the mobile phase in liquid chromatography, the flow rate is 0.5ml / min, and the wavelength of the ultraviolet detector is 280nm. Chromatographic injection of sample 10 μl, after 10 minutes the purity of the sample MBTS was obtained with an accuracy of ±0.2%.

example 2

[0011] Weigh 50 mg of the MBTS sample with a high-angle weighing bottle, add 80 ml of dichloromethane with a concentration of 96% to it, put it in an ultrasonic cleaner and vibrate for 10 minutes, transfer it to a 250 ml volumetric flask after taking it out, and use a concentration of 96% dichloromethane Dilute dichloromethane to the mark, shake well, and filter; keep the room temperature at 23°C, use water and methanol as the mobile phase in liquid chromatography, the flow rate is 2.0ml / min, and the wavelength of the ultraviolet detector is 280nm. Chromatography injected 30 μl of the sample, and the purity of the sample MBTS was obtained after 20 minutes with an accuracy of ±0.2%.

example 3

[0013] Weigh 70 mg of MBTS sample with a high-angle weighing bottle, add 100 ml of dichloromethane with a concentration of 99% to it, put it in an ultrasonic cleaner and vibrate for 20 minutes, transfer it to a 500 ml volumetric flask after taking it out, and use a concentration of 99% dichloromethane Dilute dichloromethane to the mark, shake well, and filter; keep the room temperature at 27°C, use water and methanol as the mobile phase in liquid chromatography, the flow rate is 3.0ml / min, and the wavelength of the ultraviolet detector is 280nm. Chromatography injected 40 μl of the sample, and the purity of the sample MBTS was obtained after 25 minutes with an accuracy of ±0.2%.

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Abstract

The invention discloses a liquid chromatographic method of a thiofide MBTS, which comprises the steps as follows: 10 to 100mg of MBTS samples are weighed with a high angle weighing bottle, and methylene dichloride of 5 to 200ml is added in, wherein, the concentration of methylene dichloride is 95 to 99 percent; the mixed liquid is put in a supersonic cleaner and is oscillated for 2 to 20 minutes, then is taken out and transferred to a volumetric flask whose volume capacity ranges from 100 to 1000ml, and is shook up and filtered after being diluted to reach the scale by using methylene dichloride whose concentration is 95 to 99 percent; and the room temperature is kept from 20 to 30 DEG C, a liquid chromatogram takes water and methanol as a mobile phase, the flow rate is 0.5 to 5.0ml / min, the wavelength of a UV detector ranges from 100 to 500nm, samples of 10 to 50 mul are injected to the liquid chromatogram through a trace sample injector, the purity quotient of the samples MBTS is obtained after 10 to 50 minutes, and the precision error is within 0.2 percent. The liquid chromatographic method has the advantages of simple process, high accuracy rate of analysis results and small errors.

Description

technical field [0001] The invention relates to a liquid chromatography analysis method for rubber vulcanization accelerator dibenzothiazole disulfide (MBTS), belonging to the technical field of rubber vulcanization accelerator MBTS analysis. Background technique [0002] With the development of the rubber industry, people pay more and more attention to the research and production of vulcanization accelerators. Vulcanization accelerator plays a very important role in the rubber vulcanization process. It can greatly accelerate the reaction between rubber and vulcanizing agent, improve productivity, and at the same time improve the physical and mechanical properties of vulcanized rubber. MBTS is an indispensable one in the rubber industry main accelerator. The purity of vulcanization accelerator MBTS has a great influence on the quality of downstream rubber products. Therefore, accurate analysis of the purity of MBTS is of decisive significance for the production of downstrea...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 孙桂英王树华洪学斌王树领王树恒
Owner KEMAI CHEM
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