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Method for quantitatively measuring RDX content by correction irrelevant method (CIC method) of GC-AED (gas chromatography-atomic emission spectrometry)

A calibration curve and quantitative determination technology, applied to measuring devices, instruments, scientific instruments, etc., can solve problems such as potential safety hazards, high sensitivity, and explosives, and achieve high accuracy, good separation, and good peak shape.

Active Publication Date: 2019-03-22
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In addition, energetic compounds are flammable, explosive, and highly sensitive. If energetic compounds are used as standards, there will be certain safety hazards in the transportation process of such compounds. Therefore, non-self, non-energetic Quantitative analysis of propellants and explosives components is a technical problem to be solved urgently in this field

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  • Method for quantitatively measuring RDX content by correction irrelevant method (CIC method) of GC-AED (gas chromatography-atomic emission spectrometry)
  • Method for quantitatively measuring RDX content by correction irrelevant method (CIC method) of GC-AED (gas chromatography-atomic emission spectrometry)
  • Method for quantitatively measuring RDX content by correction irrelevant method (CIC method) of GC-AED (gas chromatography-atomic emission spectrometry)

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Experimental program
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Effect test

Embodiment 1

[0022] The experimental apparatus of this embodiment:

[0023] Agilent 7890A gas chromatograph, autosampler with 16 sample turrets, JAS AEDⅡPlus multi-element detector, JAS multi-element detector software.

[0024] The test condition of this embodiment:

[0025] Chromatographic column: HP-5 chromatographic column;

[0026] Injection port temperature: 200°C;

[0027] Column temperature: 170°C;

[0028] Split ratio: 20:1;

[0029] Injection volume: 0.5uL;

[0030] Flow rate: 3mL / min;

[0031] AED detector transfer line temperature: 220°C;

[0032] AED detector chamber temperature: 250°C;

[0033] C element detection wavelength: C193nm;

[0034] The reagent gas is O 2 , H 2 ;

[0035] The supplementary gas He gas pressure is 200KPa.

[0036] Use acetone as solvent to prepare 919ug / mL RDX solution; injection volume: 0.5uL; after the instrument stabilizes, inject 6 times to obtain the average value of the peak area, and obtain the C element concentration of RDX accordin...

Embodiment 2

[0040] The experimental apparatus and test conditions used in this embodiment are the same as in Example 1.

[0041] The sample tested in this embodiment is a certain propellant, the formula of this propellant is nitrocellulose (NC), nitroglycerin (NG), black sogen (RDX), octokin (HMX), No. II neutralizer ( C 2 ), Jina (DINA), Vaseline (V), lead salt, copper salt, nickel powder, aluminum powder, carbon black. Among them, the routine test method of RDX is the liquid chromatography external standard method that needs RDX standard substance. Through the method established in this study, the DBP of non-self and non-energetic material can be used as the standard sample to determine the content of RDX in the propellant formulation.

[0042] The pretreatment steps of the sample are: weigh 0.2g (accurate to 0.2mg), place it in a dry Erlenmeyer flask with a stopper, accurately add 60mL of acetone with a pipette, add a magnetic stirring bar, stopper the bottle and stir for 30 minutes ...

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Abstract

The invention discloses a method for quantitatively measuring the RDX content by a correction irrelevant method (CIC method) of GC-AED (gas chromatography-atomic emission spectrometry). In a gas chromatographic analysis method disclosed by the invention, the used chromatographic column is: an HP-5 weakly polar capillary column, the sample inlet port temperature is 200 DEG C, the column temperaturebox is 170 DEG C, the diversion ratio is 20:1, the sample inlet amount is 0.5 muL and the column flow velocity is 3 mL / min. AED parameters are: the transmission line temperature is 220 DEG C and thecavity temperature is 250 DEG C; the used detection element is C and the wavelength is C193nm; the used reaction gas is O2, H2; and the gas pressure of the complementary gas He is 200 KPa. The RDX quantitative detection method disclosed by the invention comprises the following steps: analyzing DBP and RDX separately by a chromatographic analysis method, detecting the C element of the DBP and RDX by an AED detector (the detection wavelength is C193 nm), and calculating the C element content of the RDX by taking the C element content of the DBP as standard so as to obtain the compound content ofthe RDX. The element chromatographic analysis method has good peak shape, compound quantification adopts a non-self and non-energetic standard sample, the accuracy degree is high and the repeatability is high.

Description

technical field [0001] The invention belongs to the technical field of propellants and explosives, and in particular relates to a method for quantitative determination of RDX by a gas chromatography-atomic emission spectrometry-independent calibration curve method (CIC method). Background technique [0002] The qualitative and quantitative analysis of organic components in explosives is one of the core tasks of physical and chemical testing researchers, including the qualitative and quantitative analysis of unknowns in the synthesis of energetic materials and the quantification of organic components in the formulation of explosives. At present, mass spectrometry (MS), infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), and chromatography (GC / LC) techniques are mainly used for qualitative and quantitative analysis of organic impurities in compounds; quantitative analysis of organic components in gunpowder usually uses Solvent extraction method, followed by quantit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/74G01N30/86
CPCG01N30/02G01N30/74G01N30/8679
Inventor 苏鹏飞刘红妮张皋罗西杨彩宁胡银王歌杨温晓燕陈曼
Owner XIAN MODERN CHEM RES INST
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