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Quantitative determination of DNA content by GC-AED's irrelevant calibration curve method (CIC method)

A calibration curve and quantitative determination technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of potential safety hazards, high sensitivity, flammability, etc., 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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  • Quantitative determination of DNA content by GC-AED's irrelevant calibration curve method (CIC method)
  • Quantitative determination of DNA content by GC-AED's irrelevant calibration curve method (CIC method)
  • Quantitative determination of DNA content by GC-AED's irrelevant calibration curve method (CIC method)

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Experimental program
Comparison scheme
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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: 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] Use acetone as solvent to 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 C...

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 a GC-AED irrelevant calibration curve method (CIC method) for quantitative determination of DNAN 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 190°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 DNAN is to analyze diphenylamine and DNAN respectively by using a chromatographic analysis method, and use an AED detector to detect the C element of diphenylamine and DNAN, and the detection wavelength is C193nm, and the C element content of diphenylamine is As a standard, the C element content of DNAN is calculated, and then the compound content of DNAN is obtained. 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 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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Patent Type & Authority Patents(China)
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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