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Liquid chromatography method for purity of rubber vulcanization accelerator MBTS

A liquid chromatography analysis and rubber vulcanization technology, applied in the field of rubber vulcanization accelerator MBTS analysis, can solve the problems of high analysis results and large errors, and achieve the effects of simple process, small error and high accuracy

Inactive Publication Date: 2009-12-02
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 95% chloroform 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 95% chloroform Dilute chloroform to the mark, shake well, and filter; room temperature is kept at 20°C, the liquid chromatography is a VWD detector, the column model is 20RBAXRX-C18, the liquid chromatography uses water and methanol as the mobile phase, and the flow rate is 1.0ml / min , the wavelength of the VWD detector is 123nm, inject 10μl of sample into the liquid chromatography with a micro-injector, the gradient program is: when the injection time is 0-2 minutes, the proportion of water in the mobile phase is 25%, and the proportion of methanol is 75%; 2 to 15 minutes, the proportion of water in the mobile phase is 0%, and the proportion of methanol is 100%; 15 to 20 minutes, the proportion of water in the mobile phase is 0%, and the proportion...

example 2

[0011] Weigh 50 mg of the MBTS sample with a high-angle weighing bottle, add 80 ml of chloroform 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% chloroform Dilute chloroform to the mark, shake well, and filter; room temperature is kept at 23°C, the liquid chromatography is a VWD detector, the column type is 20RBAXRX-C18, the liquid chromatography uses water and methanol as mobile phases, and the flow rate is 2.0ml / min , the wavelength of the VWD detector is 280nm, inject 30μl of sample into the liquid chromatography with a micro-injector, the gradient program is: when the injection time is 0-2 minutes, the proportion of water in the mobile phase is 30%, and the proportion of methanol is 70%; during 2 to 15 minutes, the proportion of water in the mobile phase was 5%, and the proportion of methanol was 95%; during 15 to 20 minutes, the propor...

example 3

[0013] Weigh 70 mg of the MBTS sample with a high-angle weighing bottle, add 100 ml of chloroform 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 99% chloroform Dilute chloroform to the mark, shake well, and filter; keep the room temperature at 27°C, the liquid chromatography is a VWD detector, the column model is 20RBAXRX-C18, the liquid chromatography uses water and methanol as the mobile phase, and the flow rate is 04.0ml / min , the wavelength of the VWD detector is 352nm, inject 50μl of the sample into the liquid chromatography with a micro-injector, and its gradient program is: when the injection time is 0-2 minutes, the proportion of water in the mobile phase is 35%, and the proportion of methanol is 65%; 2 to 15 minutes, the proportion of water in the mobile phase was 10%, and the proportion of methanol was 90%; 15 to 20 minutes, the proportion of water in ...

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Abstract

The invention discloses a liquid chromatography method for purity of a rubber vulcanization accelerator MBTS. The method comprises the following processes: using a high-angle weighing bottle to weigh 10 to 100 milligrams of an MBTS sample, adding 5 to 200 milliliters of 95 to 99 percent trichloromethane into the MBT sample, putting the mixture into an ultrasound cleaner and oscillating the mixture for 2 to 20 minutes, then taking the mixture out and transferring the mixture to a volumetric flask of 100 to 1,000 milliliters, using the 95 to 99 percent trichloromethane to dilute the mixture to the scale, and shaking up and filtering the mixture; and keeping the mixture for 20 to 30 DEG C at room temperature, then injecting 10 to 50mu l of sample into liquid chromatography by using a trace sample injector, and obtaining the purity of the sample MBTS after 35 minutes, wherein the liquid chromatography is a VWD detector, the model of a chromatographic column is 20RBAXRX-C18, the liquid chromatography uses water and methanol as flow phases, the flow rate is 0.5 to 5.0 milliliters per minute, the wavelength of the VWD detector is 100 to 400 nanometers, and the precision is + / -0.2 percent. The method has the advantages of simple process, high analysis result accuracy and small error.

Description

technical field [0001] The invention relates to a liquid chromatography analysis method for the purity of a rubber vulcanization accelerator dibenzothiazole disulfide (MBTS), and belongs 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 produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34
Inventor 孙桂英王树华洪学斌王树领王树恒
Owner KEMAI CHEM
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