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Method for analyzing content of rubber accelerator thiocarbanilide

A technology of diphenylthiourea and diphenylthiourea, which is applied in the field of analysis of rubber accelerator content of diphenylthiourea, can solve the problems that cannot truly and effectively reflect the purity and quality of products, and achieve small errors and high accuracy , the effect of simple process

Active Publication Date: 2012-04-25
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, only the melting point is used as the detection standard in the industry, which cannot truly and effectively reflect the purity and quality of the product

Method used

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  • Method for analyzing content of rubber accelerator thiocarbanilide
  • Method for analyzing content of rubber accelerator thiocarbanilide
  • Method for analyzing content of rubber accelerator thiocarbanilide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Weigh 10 mg of diphenylthiourea standard product with a high-angle weighing bottle, add 10 ml of methanol solution to it, put it in an ultrasonic cleaner and vibrate for 5 minutes, take it out, transfer it to a 1000 ml volumetric flask, dilute to the mark with methanol, and shake well , filtered to prepare a 0.01mg / mL solution; keep the room temperature at 20°C, the liquid chromatograph is a VWD detector, the column model is EXTEND-C18, the liquid chromatograph uses water and methanol as the mobile phase, the flow rate is 1ml / min, VWD detection The wavelength of the detector is 254nm, inject 5μl of sample into the liquid chromatography with a micro injector, and its gradient program is: when the injection time is 0 minutes, the proportion of water in the mobile phase is 90%, and the proportion of methanol is 10%; 15 minutes , the proportion of water in the mobile phase was 30%, and the proportion of methanol was 70%; at 22 minutes, the proportion of water in the mobile p...

Embodiment 2

[0014] Weigh 50mg of diphenylthiourea standard product with a high-angle weighing bottle, add 50mL of chromatographically pure methanol solution into it, put it in an ultrasonic cleaner and vibrate for 10 minutes, take it out, transfer it to a 1000ml volumetric flask, dilute to the mark with methanol, Shake well and filter to prepare a 0.05mg / mL solution; keep the room temperature at 23°C, use water and methanol as mobile phases in liquid chromatography, flow rate is 1ml / min, VWD detector wavelength is 254nm, use micro injector to liquid chromatography Inject 5 μl of sample, and the gradient program is as follows: when the injection time is 0 minutes, the proportion of water in the mobile phase is 90%, and the proportion of methanol is 10%; at 15 minutes, the proportion of water in the mobile phase is 30%, methanol The proportion was 70%; at 22 minutes, the proportion of water in the mobile phase was 0%, and the proportion of methanol was 100%; at 30 minutes, the proportion of ...

Embodiment 3

[0016] Use a high-angle weighing bottle to weigh 100 mg of diphenylthiourea standard product, add 100 ml of methanol solution to it, put it in an ultrasonic cleaner and vibrate for 20 minutes, take it out and transfer it to a 1000 ml volumetric flask, dilute to the mark with methanol, and shake well , and filtered to prepare a 0.1mg / mL solution; keep the room temperature at 27°C, use water and methanol as the mobile phase in liquid chromatography, the flow rate is 1.0ml / min, the wavelength of the VWD detector is 254nm, inject The sample is 5 μl, and the gradient program is as follows: when the injection time is 0 minutes, the proportion of water in the mobile phase is 90%, and the proportion of methanol is 10%; at 15 minutes, the proportion of water in the mobile phase is 30%, and the proportion of methanol 70%; in 22 minutes, the proportion of water in the mobile phase was 0%, and the proportion of methanol was 100%; in 30 minutes, the proportion of water in the mobile phase w...

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Abstract

The invention relates to a method for analyzing the content of a rubber accelerator thiocarbanilide. Employing a liquid chromatogram to measure thiocarbanilide content, the method comprises: preparing a diphenylthiourea methanol solution, and putting the solution into an ultrasonic cleaner for oscillation, uniform shaking and filtering; maintaining the detection room temperature at 20-30DEG C, adopting VWD (variable wavelength detector) as the liquid chromatogram, choosing a chromatographic column in the type of 250*4.6mm EXTEND-C18, taking water and methanol as the mobile phase of the liquid chromatogram, controlling the flow velocity at 1ml / min and the detection wavelength of the VWD at 254nm, and injecting 5 microliters of a sample into the liquid chromatogram with a micro sample injector. The method carries out gradient elution to the solvent, and the liquid chromatogram analysis method measures that the retention time of thiocarbanilide is 14-17min. The method provided in the invention has simple process, high accuracy of analysis result and minor error.

Description

technical field [0001] The invention relates to a method for analyzing the content of rubber accelerator diphenylthiourea, belonging to the technical field of rubber accelerator analysis. Background technique [0002] Rubber vulcanization accelerator diphenylthiourea (CA) is a fast vulcanization accelerator, mainly used in natural latex and neoprene latex products, and can also be used in the manufacture of vulcanization bladders, water tires, tire sealants, wires and cables , industrial products, rubber shoes, etc. At the same time, it can also be used as a heat stabilizer for emulsion polyvinyl chloride, especially suitable for soft products. The general dosage is 0.2-0.5%. It will not color the plastic products, but it cannot prevent the products from being discolored by light. Diphenylthiourea is also an intermediate of medicine and dyes, used in the production of indigo, methyl indigo, sulfur dyes, flotation agents, anti-acid agents, etc. It is also an important interm...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 安静
Owner KEMAI CHEM
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