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Independent correction curve method (CIC method), for quantitatively measuring DNAN content, of GC/AED

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

Active Publication Date: 2019-04-02
XIAN MODERN CHEM RES INST
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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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  • Independent correction curve method (CIC method), for quantitatively measuring DNAN content, of GC/AED
  • Independent correction curve method (CIC method), for quantitatively measuring DNAN content, of GC/AED
  • Independent correction curve method (CIC method), for quantitatively measuring DNAN content, of GC/AED

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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: 190°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] Using acetone as solvent, prepare 644ug / mL DNAN 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 of DNAN according to the CIC...

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 mixed explosive, the formula of which is DNAN, 3,4-dinitrofurazanyl oxide furazan (DNTF), nitrocellulose, Octogen, wherein the routine test method of DNAN It is a liquid chromatography external standard method that requires DNAN standard substance. By the method established in this study, the content of DNAN in the explosive formulation can be determined by using diphenylamine which is not itself and non-energetic material.

[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 ~60 minutes until the organic components are completely dissolved. Add 20 mL of distilled water dropwise under constant shaking to precipitat...

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Abstract

The invention discloses an independent correction curve method (CIC method), for quantitatively measuring DNAN content, of GC / AED. In a gas chromatography method, the used chromatographic column is anHP-5 weak-polarity capillary column, the sample inlet temperature is 200 DEG C, the column temperature box is 190 DEG C, the split ratio is 20:1, the sample injection volume is 0.5 ul, and the columnflow velocity is 3 mL / min. AED parameters are as follows: the transmission line temperature is 220 DEG C and the cavity temperature is 250 DEG C; the used detection element is C with a wavelength ofC193 nm; the used reaction gas is O2 and H2; and the complementary gas is He with pressure of 200 KPa. The quantitative detection method for DNAN is analyzing diphenylamine and DNAN by utilizing a chromatography method, detecting C elements of the diphenylamine and the DNAN by utilizing an AED detector at the detection wavelength of C193 nm, and calculating a C element content of the DNAN by taking a C element content of the diphenylamine as a standard so as to obtain a compound content of the DNAN. The element chromatography method is favorable in peak shape, and compound quantification adopts non-self and energy-free guide samples, so that the correctness is high and the repeatability is relatively strong.

Description

technical field [0001] The invention belongs to the technical field of explosives, and in particular relates to a quantitative determination method of 2,4-dinitroanisole (DNAN) 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 quant...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/74G01N30/86
CPCG01N30/02G01N30/74G01N30/8679
Inventor 张皋刘红妮苏鹏飞罗西胡银王歌杨杨彩宁陈曼温晓燕
Owner XIAN MODERN CHEM RES INST
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