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Method for testing particle size and particle size distribution of 5-aminotetrazole

An aminotetrazole and particle size distribution technology, applied in particle size analysis, particle and sedimentation analysis, measuring devices, etc., can solve the problems of difficult selection of dispersants, difficult dispersion, easy agglomeration of powder particles, etc., and achieve simple and convenient measurement process, Good applicability and the effect of saving test time

Active Publication Date: 2018-04-10
HUBEI INST OF AEROSPACE CHEMOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wet laser diffraction test has not been used in the particle size and particle size distribution test of 5-AT because 5-AT powder particles are easy to agglomerate, difficult to disperse, and it is very difficult to choose a suitable dispersant

Method used

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  • Method for testing particle size and particle size distribution of 5-aminotetrazole
  • Method for testing particle size and particle size distribution of 5-aminotetrazole
  • Method for testing particle size and particle size distribution of 5-aminotetrazole

Examples

Experimental program
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Effect test

Embodiment 1

[0020] For a 5-AT sample with a batch number of 20151202, its particle size and particle size distribution are tested as follows: use the TopSizer laser particle size analyzer from Zhuhai Euro-American Instrument Co., Ltd., turn on the instrument, and preheat it for half an hour. Run the particle size test software, and use chloroform to clean the instrument pipeline. Adjust instrument centering and test instrument background in the software window. Take about 0.3g of 5-AT sample into a 100mL beaker, add about 20m of 0.2% sodium dodecylbenzenesulfonate + 0.1% P-40-chloroform solution, ultrasonically disperse for 5 minutes, and wait for the background test of the instrument to be completed Finally, add the sample solution into the sample cell until the refractive index is about 5%, click the test button in the software to test the sample, and the computer will automatically give the test result after the test is completed. Particle size test results are expressed as median par...

Embodiment 2

[0022] The particle size and particle size distribution of a 5-AT sample with a batch number of 20151204 are tested as follows: use a TopSizer laser particle size analyzer from Zhuhai Euro-American Instrument Co., Ltd., turn on the instrument, and preheat it for half an hour. Run the particle size test software, and use chloroform to clean the instrument pipeline. Adjust instrument centering and test instrument background in the software window. Take about 0.4g of 5-AT sample in a 100mL beaker, add about 30mL of 0.3% sodium dodecylbenzenesulfonate + 0.2% P-40-chloroform solution, ultrasonically disperse for 8 minutes, and wait until the background test of the instrument is completed Finally, add the sample solution into the sample cell until the refractive index is about 8%, click the test button in the software to test the sample, and the computer will automatically give the test result after the test is completed. Particle size test results are expressed as median particle ...

Embodiment 3

[0024] The particle size and particle size distribution of a 5-AT sample with a batch number of 20160101 are tested as follows: use a TopSizer laser particle size analyzer from Zhuhai Euro-American Instrument Co., Ltd., turn on the instrument, and preheat it for half an hour. Run the particle size test software, and use chloroform to clean the instrument pipeline. Adjust instrument centering and test instrument background in the software window. Take about 0.5g of 5-AT sample in a 100mL beaker, add about 40mL of 0.4% sodium dodecylbenzenesulfonate + 0.2% P-40-chloroform solution, ultrasonically disperse for 10min, and wait until the background test of the instrument is completed Finally, add the sample solution into the sample cell until the refractive index is about 10%, click the test button in the software to test the sample, and the computer will automatically give the test result after the test is completed. Particle size test results are expressed as median particle siz...

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Abstract

The invention relates to a method for testing the particle size and the particle size distribution of 5-aminotetrazole, wherein the particle size and the particle size distribution of an organic synthesis intermediate 5-aminotetrazole are tested by a wet laser diffraction method. According to the method, 5-AT particle size test is performed by using a trichloromethane solution containing 0.2-0.4%of sodium dodecylbenzenesulfonate and 0.1-0.2% of ethylphenyl polyethylene glycol as a dispersion system at an ultrasonic dispersion time of 5-10 min. According to the present invention, the relativestandard deviation of the multiple median particle size measurement results is not more than 6%, the precision of the method is good, and the wet laser diffraction method for testing the particle sizeof 5-AT has good applicability and can be used for the test of the particle size of 5-AT so as to be used for the quality control of the product.

Description

technical field [0001] The invention relates to a method for testing the particle size and particle size distribution of an organic synthesis intermediate 5-aminotetrazole. Background technique [0002] 5-Aminotetrazolium (hereinafter referred to as 5-AT) can be used as an intermediate in organic synthesis, and can be used as a raw material to prepare a variety of high-energy organic compounds with excellent properties. It can also be used in pharmaceutical synthesis in pharmaceutical and chemical industries. As a reagent, it can be used for organic ligands, and it can be directly coordinated with metals to prepare complexes. Particle size and particle size distribution are important quality control indicators of 5-AT, and the test methods for the particle size and particle size distribution of 5-AT have not been reported in the literature. [0003] At present, the most widely used particle size testing method is the laser diffraction method, which is divided into dry laser...

Claims

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Application Information

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IPC IPC(8): G01N15/02
CPCG01N15/0205
Inventor 刘发龙胡伟韩丽萍刘治国谭利敏蔡如琳王敏章园园赵华丽
Owner HUBEI INST OF AEROSPACE CHEMOTECH
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