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Method for determining content of sucrose octaacetate in double-base propellant

A technology for the determination of sucrose octaacetate, which is applied in the field of determination of the content of sucrose octaacetate in double-base gunpowder, can solve problems such as insufficient determination methods, and achieve the effects of high accuracy, strong selectivity, and simple operation

Active Publication Date: 2020-10-23
宜宾北方川安化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the deficiencies of existing assay methods, the invention provides a method for assaying the content of sucrose octaacetate in double-base gunpowder

Method used

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  • Method for determining content of sucrose octaacetate in double-base propellant
  • Method for determining content of sucrose octaacetate in double-base propellant
  • Method for determining content of sucrose octaacetate in double-base propellant

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0053] Preparation of standard curve:

[0054] Weighing content is 0.146 (converted into 2g gunpowder sucrose octaacetate content is 3.00%), 0.290g (converted into 2g gunpowder sucrose octaacetate content is 6.005%), 0.398g (converted into 2g gunpowder sucrose octaacetate content is 6.005%) Acetate content is 8.002%), 0.488g (converted into 2g gunpowder and sucrose octaacetate content is 10.030%), 0.596g (converted into 2g gunpowder and sucrose octaacetate content is 12.000%), 0.733g (converted into 2g The content of sucrose octaacetate in gunpowder is 14.995%) of sucrose octaacetate, accurately add 50mL chloroform respectively, fully dissolve and shake up, then test its optical rotation respectively, according to the optical rotation measured and its content plotted, get standard curve as figure 1 Shown:

[0055] Standard solution content and measured optical rotation corresponding data table

[0056] Optical rotation, ° 0.000 0.146 0.290 0.398 0.488 0.596 ...

Embodiment 1

[0065] A kind of assay method of sucrose octaacetate content in double base gunpowder, it may further comprise the steps:

[0066] 1) Sample processing: Process the gunpowder sample into flower flakes with a scraper;

[0067] 2) Put filter paper in the extraction cell, add a certain amount of silicon dioxide, the volume of silicon dioxide is about two-thirds of the volume of the sample cell.

[0068] Put 2 g of the sample treated in step 1) into the extraction cell in 4 times. After each transfer, crush the sample with a glass rod, then mix the sample and silica evenly, and tighten the cap of the extraction cell.

[0069] Turn on the quick extraction instrument, after the instrument is preheated, put it into the extraction pool, then add the extractant dichloromethane, perform extraction according to the following conditions, and collect the extract in the collection bottle.

[0070] Extraction conditions:

[0071]

[0072] 3) The liquid in the collection bottle was trans...

Embodiment 2

[0082] Adopt same product to adopt existing method and the method step in the embodiment of the present invention 1 to carry out ten times of measurement respectively, and measurement result contrast is as follows:

[0083] Adopt the present invention and existing method to measure same product result comparison table simultaneously

[0084]

[0085] It can be seen from the above data that the accuracy of the analysis results of the present invention is higher, and the precision of the analysis results is better.

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Abstract

The invention relates to the technical field of organic analysis and measurement, in particular to a method for determining the content of sucrose octaacetate in double-base propellant. The determination method comprises the following steps of: 1) sample treatment, which is implemented by treating a propellant sample into a flower sheet shape; (2) putting the treated samples into an extraction tank in batches, then uniformly mixing the samples with a filler and adding an extraction agent into the mixture for extraction; 3) evaporating an extracting agent from the obtained extracting solution by adopting water bath to dryness to obtain an extract; 4) adding trichloromethane into the extract, fully dissolving the mixture, uniformly shaking the dissolved mixture and carrying out suction filtration on the solution by using a microfiltration membrane; 5) turning on a high-precision polarimeter, and measuring the optical rotation of the filtrate subjected to suction filtration; 6) drawing astandard curve; and 7) calculating to obtain the content of sucrose octaacetate according to the measured optical rotation and the standard curve. The method has the advantages that the operation is simple, the analysis time is short, the selectivity is strong, other components do not interfere with the measurement, the separation is not needed, the repeatability is good, the result is accurate, and the content of the sucrose octaacetate in the double-base propellant can be effectively controlled through adopting the method.

Description

technical field [0001] The invention relates to the technical field of organic analysis and determination, in particular to a method for determining the content of sucrose octaacetate in double-base gunpowder. Background technique [0002] The main components of double-base gunpowder containing sucrose octaacetate are: nitrocellulose, nitroglycerin, vaseline, neutralizing agent, sucrose octaacetate and catalyst, etc., and sucrose octaacetate is a common component in double-base gunpowder. Sucrose octaacetate is obtained by esterifying sucrose with acetic anhydride in the presence of a catalyst, and this species is recorded in the 2015 edition of the Chinese Pharmacopoeia. This variety is also collected in the 36th edition of "United States Pharmacopoeia", and the content determination method included in it is residual titration method. The operation steps are: take sucrose octaacetate and dissolve it in an appropriate amount of 70% ethanol, use phenolphthalein as indicator, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/21G01N1/28G01N1/40
CPCG01N21/21G01N1/28G01N1/4055G01N1/4005G01N2001/4061
Inventor 曹远洋罗伦忠江林陈轶肖俊峰李胜超王艳王宏李华川刘中云陈勇
Owner 宜宾北方川安化工有限公司
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