CN111812038A - Method for determining content of sucrose octaacetate in double-base gunpowder - Google Patents
Method for determining content of sucrose octaacetate in double-base gunpowder Download PDFInfo
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- CN111812038A CN111812038A CN202010503375.5A CN202010503375A CN111812038A CN 111812038 A CN111812038 A CN 111812038A CN 202010503375 A CN202010503375 A CN 202010503375A CN 111812038 A CN111812038 A CN 111812038A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/4055—Concentrating samples by solubility techniques
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
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- G01N2001/4061—Solvent extraction
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Abstract
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. The determination method comprises the steps of 1) sample treatment: processing the gunpowder sample into a flower sheet shape; 2) putting the treated sample into an extraction tank in batches, and then uniformly mixing the sample and the filler; adding an extracting agent for extraction; 3) evaporating the extractant to dryness in water bath to obtain extract; 4) adding trichloromethane into the extract, fully dissolving and shaking uniformly; then the solution is filtered by a microporous filter membrane; 5) starting a high-precision polarimeter, and measuring the optical rotation of the filtrate after suction filtration; 6) drawing a standard curve; 7) and calculating the content of sucrose octaacetate according to the measured optical rotation and a standard curve. The method is simple to operate and short in analysis time; the method has the advantages of strong selectivity, no interference of other components in determination, no need of separation, good repeatability and accurate result, and can effectively control the content of sucrose octaacetate in the double-base gunpowder.
Description
Technical Field
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
The components of the double-base gunpowder containing sucrose octaacetate mainly comprise: nitrocotton, nitroglycerin, vaseline, a stabilizer, sucrose octaacetate, a catalyst and the like, wherein the sucrose octaacetate is a common component in double-base gunpowder. Sucrose octaacetate is prepared by esterifying sucrose with acetic anhydride in the presence of a catalyst, and the variety is recorded in the 'Chinese pharmacopoeia' 2015 edition. The strain is also collected in United states Pharmacopeia 36, the content measurement method recorded by the strain is a residual titration method, and the operation steps are as follows: dissolving sucrose octaacetate in a proper amount of 70% ethanol, using phenolphthalein as an indicator, regulating the solution to be neutral by using a sodium hydroxide titration solution, precisely adding the sodium hydroxide titration solution, refluxing in a boiling water bath for 1h, then titrating excessive alkali by using a sulfuric acid titration solution, and calculating to obtain the sucrose octaacetate. The method has complicated operation steps, needs to observe a titration end point by naked eyes, is easy to bring errors, and is not suitable for measuring the content of sucrose octaacetate in the double-base gunpowder because components such as nitroglycerin, a neutralization reagent and the like need to react with sodium hydroxide.
At present, liquid chromatography is generally adopted by some manufacturers at home and abroad for analysis, and the specific operation steps are as follows: processing a sample into a flower sheet shape, performing reflux extraction by using organic solvents such as dichloromethane, diethyl ether and the like to separate sucrose octaacetate from components such as nitrocotton, a catalyst and the like, then determining the mixture in a volumetric flask with a certain volume, and then performing separation and measurement. The problems of the method are mainly as follows: the instrument is expensive, the extraction time is long, the extraction time needs more than 25 hours, and the sucrose octaacetate has weak absorption capacity in an ultraviolet light range, so the analysis sensitivity is low, the linear range is narrow, and the accuracy of a measurement result is low.
Disclosure of Invention
In order to overcome the problem of the deficiency of the existing determination method, the invention provides a method for determining the content of sucrose octaacetate in double-base gunpowder. The method adopts a rapid extraction instrument to perform direct extraction, the extraction is completed within 2 hours, and then the measurement is performed directly, so the operation is simple, and the analysis time is greatly shortened. In addition, the method has the advantages of strong selectivity, no interference of other components in measurement, no need of separation, good repeatability of measurement results, accurate results and the like, and the content of sucrose octaacetate in the double-base gunpowder can be effectively controlled by the method.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a method for measuring the content of sucrose octaacetate in double base powder comprises the following steps:
1) sample treatment: processing the gunpowder sample into a pattern sheet shape by a drilling machine or a scraper;
2) the extraction cell was loaded with a filter paper sheet and a certain amount of silica was added, the volume of silica being about two thirds of the volume of the sample cell.
Putting the sample (preferably 2-3 g) treated in the step 1) into an extraction tank for several times (preferably 3-5 times), mashing the sample by using a glass rod after each transfer, uniformly mixing the sample and a filler (preferably silicon dioxide), and screwing a cover of the extraction tank.
Opening the rapid extraction instrument, preheating the instrument, putting the instrument into an extraction tank, adding an extracting agent, extracting according to the following conditions, and collecting the extract in a collection bottle.
The extractant is dichloromethane; the addition amount of the extracting agent is 50ml-60ml/2-3g of sample.
Extraction conditions are as follows:
3) transferring the liquid in the collecting bottle to a beaker without damage, and evaporating the extractant from the extraction liquid obtained in the step 2) by adopting a water bath to obtain the extract.
The dichloromethane is preferably evaporated on a water bath at the temperature of 55-60 ℃.
4) Adding trichloromethane (preferably 50.00ml) into the extract in the step 3), fully dissolving and shaking up; then the solution is filtered by a double-layer 0.45 mu m microporous filter membrane;
5) starting a high-precision polarimeter (the precision is 0.001 degree), selecting a 20cm funnel polarimeter after the polarimeter is preheated, injecting trichloromethane, removing bubbles, putting the polarimeter into the polarimeter for 5 minutes, measuring, and then pressing a zero key; pouring out the trichloromethane in the polariscope, rinsing the filtrate subjected to suction filtration in the step 4) for three times, filling the filtrate with the optical rotation, removing bubbles, putting the filtrate into a polarimeter, waiting for 5 minutes (if the measurement result is not stable after waiting for 5 minutes), and measuring the optical rotation of the sample;
6) measuring the optical rotation of the standard solution by the same method, and drawing a standard curve;
7) and (4) calculating the content of sucrose octaacetate according to the optical rotation measured in the step 5) and a standard curve.
Preparation of a standard curve:
respectively weighing 0.146% (to obtain 2g of powder, the content of sucrose octaacetate is 3.00%), 0.290g (to obtain 2g of powder, the content of sucrose octaacetate is 6.005%), 0.398g (to obtain 2g of powder, the content of sucrose octaacetate is 8.002%), 0.488g (to obtain 2g of powder, the content of sucrose octaacetate is 10.030%), 0.596g (to obtain 2g of powder, the content of sucrose octaacetate is 12.000%), 0.733g (to obtain 2g of powder, the content of sucrose octaacetate is 14.995%), respectively and accurately adding 50mL of trichloromethane, fully dissolving and shaking, then respectively testing the optical rotation, and drawing according to the measured optical rotation and the content thereof to obtain a standard curve as shown in FIG. 1:
data table of standard solution content and measured optical rotation
The calculation formula is as follows:
the calculation formula of the content of sucrose octaacetate is as follows:
in the formula:
y is the content of sucrose octaacetate in units of%;
x-the measured optical rotation of the sample;
m-mass of sample, g.
Compared with the prior art, the positive effects of the invention are as follows:
the method is simple to operate, and analysis time can be effectively reduced.
And (II) the selectivity is strong, the repeatability is good, and the precision and the accuracy of a measuring result are good.
And (III) the determination of the low-content sucrose octaacetate has higher accuracy.
Drawings
Figure 1 is a standard graph of sucrose octaacetate.
Detailed Description
In order that the present disclosure may be more readily understood, the process of the present disclosure will now be described in further detail with reference to specific embodiments thereof. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
A method for measuring the content of sucrose octaacetate in double base powder comprises the following steps:
1) sample treatment: processing the gunpowder sample into a pattern sheet shape by a drilling machine or a scraper;
2) the extraction cell was loaded with a filter paper sheet and a certain amount of silica was added, the volume of silica being about two thirds of the volume of the sample cell.
Putting the sample (preferably 2-3 g) treated in the step 1) into an extraction tank for several times (preferably 3-5 times), mashing the sample by using a glass rod after each transfer, uniformly mixing the sample and a filler (preferably silicon dioxide), and screwing down an extraction tank cover.
Opening the rapid extraction instrument, preheating the instrument, putting the instrument into an extraction tank, adding an extracting agent, extracting according to the following conditions, and collecting the extract in a collection bottle.
The extractant is dichloromethane.
Extraction conditions are as follows:
3) transferring the liquid in the collecting bottle to a beaker without damage, and evaporating the extractant from the extraction liquid obtained in the step 2) by adopting a water bath to obtain the extract.
The dichloromethane is preferably evaporated on a water bath at the temperature of 55-60 ℃.
4) Adding trichloromethane (preferably 50ml) into the extract in the step 3), fully dissolving and shaking up; the solution was then filtered through a double-layer 0.45 μm microfiltration membrane.
The chloroform used here cannot be replaced by dichloromethane, which affects the accuracy of the operation.
5) Starting a high-precision polarimeter (the precision is 0.001 degree), selecting a 20cm funnel polarimeter after the polarimeter is preheated, injecting trichloromethane, removing bubbles, putting the polarimeter into the polarimeter for 5 minutes, measuring, and then pressing a zero key; pouring out the trichloromethane in the optical rotation tube, rinsing the filtrate subjected to suction filtration in the step 4) for three times, filling the filtrate with optical rotation, removing bubbles, putting the filtrate into an optical rotation instrument, waiting for 5 minutes, and measuring the optical rotation of the sample;
6) measuring the optical rotation of the standard solution by the same method, and drawing a standard curve;
7) and (4) calculating the content of sucrose octaacetate according to the optical rotation measured in the step 5) and a standard curve.
Preparation of a standard curve:
respectively weighing 0.146% (to obtain 2g of powder, the content of sucrose octaacetate is 3.00%), 0.290g (to obtain 2g of powder, the content of sucrose octaacetate is 6.005%), 0.398g (to obtain 2g of powder, the content of sucrose octaacetate is 8.002%), 0.488g (to obtain 2g of powder, the content of sucrose octaacetate is 10.030%), 0.596g (to obtain 2g of powder, the content of sucrose octaacetate is 12.000%), 0.733g (to obtain 2g of powder, the content of sucrose octaacetate is 14.995%), respectively and accurately adding 50mL of trichloromethane, fully dissolving and shaking, then respectively testing the optical rotation, and drawing according to the measured optical rotation and the content thereof to obtain a standard curve as shown in FIG. 1:
data table of standard solution content and measured optical rotation
| Degree of rotation, ° | 0.000 | 0.146 | 0.290 | 0.398 | 0.488 | 0.596 | 0.733 |
| Content (wt.) | 0.000 | 3.000 | 6.005 | 8.002 | 10.030 | 12.000 | 14.995 |
The calculation formula is as follows:
the calculation formula of the content of sucrose octaacetate is as follows:
in the formula:
y is the content of sucrose octaacetate in units of%;
x-the measured optical rotation of the sample;
m-mass of sample, g.
Example 1:
a method for measuring the content of sucrose octaacetate in double base powder comprises the following steps:
1) sample treatment: processing the gunpowder sample into a flower sheet shape by a scraper;
2) the extraction cell was loaded with a filter paper sheet and a certain amount of silica was added, the volume of silica being about two thirds of the volume of the sample cell.
2g of the sample treated in the step 1) is placed into an extraction tank for 4 times, after each transfer, a glass rod is used for mashing the sample, then the sample and silicon dioxide are uniformly mixed, and the cover of the extraction tank is screwed down.
Opening the rapid extraction instrument, preheating the instrument, putting the instrument into an extraction tank, adding an extractant dichloromethane, extracting according to the following conditions, and collecting the extract in a collection bottle.
Extraction conditions are as follows:
3) transferring the liquid in the collecting bottle to a beaker without damage, and evaporating the extractant from the extraction liquid obtained in the step 2) by adopting a water bath to obtain the extract. The temperature at which the water bath was evaporated to dryness was 56 ℃.
4) Adding 50ml of trichloromethane into the extract obtained in the step 3), and fully dissolving and shaking up; then the solution is filtered by a double-layer 0.45 mu m microporous filter membrane;
5) starting a high-precision polarimeter (the precision is 0.001 degree), selecting a 20cm funnel polarimeter after the polarimeter is preheated, injecting trichloromethane, removing bubbles, putting the polarimeter into the polarimeter for 5 minutes, measuring, and then pressing a zero key; pouring out the trichloromethane in the optical rotation tube, rinsing the filtrate subjected to suction filtration in the step 4) for three times, filling the filtrate with optical rotation, removing bubbles, putting the filtrate into an optical rotation instrument, waiting for 5 minutes, and measuring the optical rotation of the sample;
6) measuring the optical rotation of the standard solution by the same method, and drawing a standard curve;
7) and (4) calculating the content of sucrose octaacetate according to the optical rotation measured in the step 5) and a standard curve.
The standard curve and the calculation formula are the same as those of the specific embodiment.
Ten times of measurement is respectively carried out by adopting the same product and adopting the existing method and the method in the embodiment, and the measurement results are compared as follows:
the method and the existing method are adopted to simultaneously determine the result comparison table of the same product:
example 2
Ten measurements were carried out using the same product using the existing method and the method steps in example 1 of the present invention, and the results of the measurements were compared as follows:
comparison table for simultaneously measuring results of same product by adopting invention and existing method
From the data, the accuracy of the analysis result is higher, and the precision of the analysis result is better.
Although the present invention has been described in detail with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.
Claims (10)
1. A method for measuring the content of sucrose octaacetate in double base powder is characterized by comprising the following steps:
1) sample treatment: processing the gunpowder sample into a pattern sheet shape by a drilling machine or a scraper;
2) putting the sample treated in the step 1) into an extraction cell in batches, and then uniformly mixing the sample and the filler; adding an extracting agent, and extracting at the temperature of 98-100 ℃;
3) evaporating the extracting agent from the extracting solution obtained in the step 2) by adopting a water bath to obtain an extract;
4) adding trichloromethane into the extract obtained in the step 3), fully dissolving and shaking up; then the solution is filtered by a double-layer 0.45 mu m microporous filter membrane;
5) starting a high-precision polarimeter, and measuring the optical rotation of the filtrate obtained in the step 4) after suction filtration;
6) measuring the optical rotation of the standard solution by the same method, and drawing a standard curve;
7) and calculating the content of sucrose octaacetate according to the measured optical rotation and a standard curve.
2. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 1, wherein: the filler in the step 2) is silicon dioxide, and the volume of the silicon dioxide is two thirds of that of the extraction tank.
3. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 1, wherein: and 2) transferring the sample into an extraction tank for 3-5 times, and mashing the sample by using a glass rod after each transfer.
4. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 1, wherein the extractant in step 2) is dichloromethane; the extraction conditions were: the temperature is 98-100 ℃, the single extraction time is 8-12 min, and the extraction times are 4-6.
5. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 1, wherein: and (3) flushing after extraction, wherein the flushing volume is 60-100%, and the flushing time is 60-100 s.
6. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 1, wherein: the sample was taken at 2g-3 g.
7. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 1, wherein: the evaporation temperature of the water bath in the step 3) is 55-60 ℃.
8. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 1, wherein: step 4) the amount of chloroform added was 50.00 ml.
9. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 1, wherein: the precision of the high-precision polarimeter in the step 5) is 0.0010The optical rotation tube adopts a funnel type optical rotation tube with the length of 20 cm.
10. The method for determining the content of sucrose octaacetate in a gunpowder according to claim 9, wherein: the tube was placed in the instrument and the measurement was carried out after waiting 5 minutes.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2224504A (en) * | 1988-09-27 | 1990-05-09 | Tate & Lyle Plc | De-acylation of sucrose esters |
| JP2005314432A (en) * | 2005-06-08 | 2005-11-10 | Cambridge Biostability Ltd | Medicine liquid suspension |
| CN101178390A (en) * | 2007-12-12 | 2008-05-14 | 中国烟草总公司郑州烟草研究院 | Method for determining Cembrane diterpene alcoholate in tobacco and tobacco product by gas chromatography-mass spectrometry |
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- 2020-06-05 CN CN202010503375.5A patent/CN111812038B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2224504A (en) * | 1988-09-27 | 1990-05-09 | Tate & Lyle Plc | De-acylation of sucrose esters |
| JP2005314432A (en) * | 2005-06-08 | 2005-11-10 | Cambridge Biostability Ltd | Medicine liquid suspension |
| CN101178390A (en) * | 2007-12-12 | 2008-05-14 | 中国烟草总公司郑州烟草研究院 | Method for determining Cembrane diterpene alcoholate in tobacco and tobacco product by gas chromatography-mass spectrometry |
Non-Patent Citations (3)
| Title |
|---|
| A. CLARKSON ET AL.: "A spectrophotometric method for determining sucrose octa-acetate in propellant materials", vol. 87, no. 1040, pages 870 - 874 * |
| 叶丽等: "旋光法测定蔗糖脂肪酸酯中的游离蔗糖", vol. 39, no. 02, pages 274 - 275 * |
| 蔡莉莉等: "香料烟中蔗糖酯的气相色谱/质谱分析", 烟草科技, no. 03, pages 40 - 44 * |
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