CN104330500B - Use the method that cemented explosive main component is analyzed by liquid-phase chromatography method - Google Patents
Use the method that cemented explosive main component is analyzed by liquid-phase chromatography method Download PDFInfo
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- CN104330500B CN104330500B CN201410674913.1A CN201410674913A CN104330500B CN 104330500 B CN104330500 B CN 104330500B CN 201410674913 A CN201410674913 A CN 201410674913A CN 104330500 B CN104330500 B CN 104330500B
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Abstract
The present invention relates to cemented explosive component analyzing method, a kind of method using liquid-phase chromatography method that cemented explosive main component is analyzed.Solve the technical problem that current cemented explosive composition analysis result error is bigger.A kind of method using liquid-phase chromatography method to be analyzed cemented explosive main component, comprises the following steps: cemented explosive sample to be measured is completely dissolved in acetone by (a), prepares testing sample solution；B RDX standard substance is completely dissolved in acetone and prepares RDX standard liquid by ()；C () uses C18 chromatographic column, testing sample solution carries out at wavelength 230nm chromatography, and uses external standard method to calculate the content of RDX in testing sample.The present invention solves the deficiencies such as relatively big, the analytical cycle length of result error when product is analyzed by current gravimetric method, and more save time, laborsaving, the degree of accuracy is high.
Description
Technical field
The present invention relates to cemented explosive component analyzing method, be specially one and use liquid-phase chromatography method to cemented explosive master
Want the method that composition is analyzed, it is adaptable in cemented explosive, flame arrest medicine, poly-black series products, RDX weight/mass percentage composition divides
Analysis.
Background technology
Along with the development of modern industry, more and more higher to the performance requirement of explosive, also the analysis to explosive proposes higher
Requirement, it is to use gravimetry that conventional cemented explosive analyzes method, the method to sample solvent in sample
Binding agent dissolves, and general selection chloroform dissolves binding agent, but due to the binding agent dissolution velocity in a solvent of solidification
Slowly, solubility is little, dissolving is incomplete, and portion of binder is not completely soluble in solvent, when being therefore centrifuged separating, easily causes
Not exclusively, the analysis result causing same sample is on the low side compared with theoretical value, adds the gravimetric analysis cycle in portion of binder washing
Long, again owing to there are aquadag in some product, cause binding agent to separate with graphite unclear, it has to take calcination
Method is to reduce analytical error, and therefore analysis result is unstable, it is difficult to Instructing manufacture properly functioning.
Summary of the invention
The utility model is to solve the technical problem that current cemented explosive composition analysis result error is bigger, it is provided that one is adopted
Method cemented explosive main component being analyzed with liquid-phase chromatography method.
The present invention adopts the following technical scheme that realization: a kind of employing liquid-phase chromatography method is to cemented explosive main component
The method being analyzed, comprises the following steps: cemented explosive sample to be measured is completely dissolved in acetone by (a), prepares to be measured
Sample solution；B RDX standard substance is completely dissolved in acetone and prepares RDX standard liquid by ()；C () uses C18 chromatogram
Post, carries out chromatography at wavelength 230nm, and uses external standard method to calculate RDX in testing sample testing sample solution
Content.
This method uses acetone component each to sample all to dissolve, and sample is used through dissolving, after ultrasonic, filtration treatment
High performance liquid chromatograph, with RDX standard substance preparing standard solution at wavelength 230nm, uses external standard method in sample
RDX carries out the mensuration of weight/mass percentage composition, is processed by data, thus calculates containing of other compositions in cemented explosive
Amount.
The present invention solves relatively big, the analytical cycle length of result error when product is analyzed by current gravimetric method etc. no
Enough, and more save time, laborsaving, the degree of accuracy is high.
Detailed description of the invention
During actual analysis, use acetone that sample is dissolved, with supersonic oscillations instrument, solution processed 5 minutes,
Make sample be completely dissolved, then with 45 μm filter membranes, solution is filtered, remove the insoluble matter in solution, then use high-efficient liquid phase color
Spectrometer is measured.During mensuration, the solution of 1.0mg/ml RDX standard substance preparation is used to select wavelength, by testing black rope
Modern have preferably absorption at the 230nm of ultra-violet (UV) band, and we select 230nm as the wavelength measuring RDX.Use RDX standard
Solution, in using external standard method to cemented explosive at 230nm wavelength, RDX is analyzed measuring.
1 reagent and instrument
1.1 reagent
Acetone GB686 analyzes pure；
Methyl alcohol GB683 chromatographically pure；
Acetonitrile HGB3329 chromatographically pure；
Redistilled water；
RDX working stamndard sample uses the standard RDX 99.99% that country's explosive wastewater one-level measuring station produces
1.2 instrument
Electronic balance scale division value 0.01mg；
Liquid chromatograph LC 2010AHT
Supersonic oscillations instrument
Sand core filter
0.45 μm filter membrane
Vavuum pump
2. analytical procedure
The preparation of 2.1 solution
The preparation of sample solution: weigh sample 0.1g (being accurate to 0.0002g), be placed in the volumetric flask of 100ml, use acetone
Dissolve, shake up, and be diluted to scale.
The preparation of standard liquid: accurately weigh the RDX standard substance of (0.095-0.100) g, be placed in the appearance of 100ml
In measuring bottle, with acetone solution, shake up, and be diluted to scale.
2.2 testing conditions:
UV-detector wavelength: 230nm；
Flowing phase: acetonitrile/methanol/water=14/22/64 (V/V)
Column temperature: constant temperature at (30～40) DEG C, temperature fluctuation is less than 1 DEG C；；
Sample size: 10 μ L；
2.3 methods of operating:
Start instrument, under the experimental condition of calibrating, continuous sample introduction three times.Take RDX peak area in three testing liquids
Mean value as the peak area of RDX in testing liquid.RDX area flat in each three calibration solution before and after taking mensuration
Average, as the peak area of RDX in solution.
3, data process
RDX content calculates as the following formula:
In formula: W3-RDX percentage composition；ssThe peak area of RDX, unit in the solution to be measured that-chromatography draws
mm2；mcThe quality of RDX, unit g in-standard liquid；scThe peak area of RDX in the standard liquid that-chromatography draws,
Unit mm2；The quality of m-sample, unit g；
Binder content calculates as the following formula: W=100-W3, in formula: W-binding agent percentage composition；W3-RDX percentage
Content.
Claims (1)
1. one kind uses the method that cemented explosive main component is analyzed by liquid-phase chromatography method, it is characterised in that include with
Lower step: cemented explosive sample to be measured is completely dissolved in acetone by (a), prepares testing sample solution；Testing sample solution
Preparation method is as follows: weigh testing sample 0.1g, is placed in the volumetric flask of 100ml, with acetone solution, shakes up, and is diluted to carve
Degree；
B RDX standard substance is completely dissolved in acetone and prepares RDX standard liquid by ()；The wherein preparation of standard liquid
Method is as follows: accurately weighs the RDX standard substance of 0.095-0.100g, is placed in the volumetric flask of 100ml, molten with acetone
Solve, shake up, and be diluted to scale；
C () uses C18 chromatographic column, at wavelength 230nm, testing sample solution is carried out chromatography；Concrete operations are as follows:
Testing conditions:
UV-detector wavelength: 230nm；
Flowing phase: acetonitrile/methanol/water=14/22/64, V/V；
Column temperature: constant temperature at 30～40 DEG C, temperature fluctuation is less than 1 DEG C；
Sample size: 10 μ L；Start instrument, under the experimental condition of calibrating, continuous sample introduction three times；Take black rope in three testing liquids
The mean value of modern peak area is as the peak area of RDX in solution to be measured；RDX in each three standard liquids before and after taking mensuration
The mean value of area, as the peak area of RDX in standard liquid；
Equation below is used to calculate the content of RDX in testing sample:
In formula: W3-RDX percentage composition；ssThe peak area of RDX, unit in the solution to be measured that-chromatography draws2；
mcThe quality of RDX, unit g in-standard liquid；scThe peak area of RDX, unit in the standard liquid that-chromatography draws
㎜2；The quality of m-sample, unit g；
Binder content calculates as the following formula: W=100%-W3, in formula: W-binding agent percentage composition；W3-RDX percentage contains
Amount.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410674913.1A CN104330500B (en) | 2014-11-21 | 2014-11-21 | Use the method that cemented explosive main component is analyzed by liquid-phase chromatography method |
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| CN201410674913.1A CN104330500B (en) | 2014-11-21 | 2014-11-21 | Use the method that cemented explosive main component is analyzed by liquid-phase chromatography method |
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| CN104330500A CN104330500A (en) | 2015-02-04 |
| CN104330500B true CN104330500B (en) | 2016-08-24 |
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| CN201410674913.1A Active CN104330500B (en) | 2014-11-21 | 2014-11-21 | Use the method that cemented explosive main component is analyzed by liquid-phase chromatography method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8585840B2 (en) * | 2003-08-29 | 2013-11-19 | G.D.O., Inc. | Recovery of the energetic component from plastic bonded explosives |
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