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GC-AED's independent calibration curve method (CIC method) for quantitative determination of RDX content

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

Active Publication Date: 2021-11-23
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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  • GC-AED's independent calibration curve method (CIC method) for quantitative determination of RDX content
  • GC-AED's independent calibration curve method (CIC method) for quantitative determination of RDX content
  • GC-AED's independent calibration curve method (CIC method) for quantitative determination of RDX content

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Experimental program
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Embodiment 1

[0022] The experimental apparatus of this embodiment:

[0023] Agilent 7890A gas chromatograph, autosampler with 16 sample turrets, JAS AED Ⅱ Plus 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 accord...

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 GC-AED irrelevant calibration curve method (CIC method) for quantitative determination of RDX content. The chromatographic column used in the disclosed gas chromatographic analysis method is a HP-5 weakly polar capillary column, the inlet temperature is 200°C, the column oven is 170°C, the split ratio is 20:1, the injection volume is 0.5uL, and the column flow rate is 3mL / min. AED parameters are: transmission line temperature 220°C, cavity temperature 250°C; the detection element used is C, the wavelength is C193nm; the reaction gas used is O 2 , H 2 ; Supplementary gas He gas pressure is 200KPa. The disclosed quantitative detection method of RDX is to analyze DBP and RDX respectively by using chromatographic analysis method, and use AED detector to detect the C element of DBP and RDX, and the detection wavelength is C193nm, taking the C element content of DBP as the standard, Calculate the C element content of RDX, and then obtain the compound content of RDX. The element chromatographic analysis method of the present invention has good peak shape, and non-self and non-energetic standard samples are used for compound quantification, with high accuracy and strong repeatability.

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 Patents(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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