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Quantitative determination of DNTF content by the independent calibration curve method (CIC method) of GC-AED

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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  • Summary
  • 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

Method used

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  • Quantitative determination of DNTF content by the independent calibration curve method (CIC method) of GC-AED
  • Quantitative determination of DNTF content by the independent calibration curve method (CIC method) of GC-AED
  • Quantitative determination of DNTF content by the independent calibration curve method (CIC method) of GC-AED

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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: 2mL / 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 740ug / mL DNTF 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 DNTF 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, and the formula of this explosive is 2.4.6-trinitrotoluene (TNT), DNTF and benzotrifuran nitrogen oxide compound (BTF), wherein the routine test method of DNTF needs Liquid chromatography external standard method of DNTF standard substance. Through the method established in this study, benzoic acid, which is not itself and non-energetic material, can be used as a standard sample to determine the content of DNTF in the explosive formula.

[0042] The pretreatment steps of the sample are: Weigh 0.1g of the sample into a clean and dry 50mL volumetric flask, add 30mL of acetone, plug the bottle, sonicate until completely dissolved, dilute to the mark with acetone, and mix well. After filtering with an organic solvent filter, the samples were injected for analysis. The C element chromatographic sepa...

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Abstract

The invention discloses an irrelevant calibration curve method (CIC method) of GC‑AED for quantitative determination of DNTF content. The chromatographic column used in the disclosed gas chromatography analysis method is a HP‑5 weak polar capillary column, the temperature of the injection port is 200°C, and the column The temperature box is 170°C, the split ratio is 20:1, the injection volume is 0.5uL, and the column flow rate is 2mL / 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 DNTF is to analyze benzoic acid and DNTF respectively by using a chromatographic analysis method, and use an AED detector to detect the C element of benzoic acid and DNTF, and the detection wavelength is C193nm, and the C element content of benzoic acid is As a standard, the C element content of DNTF is calculated, and then the compound content of DNTF 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 3,4-dinitrofurazanylfuroxan (DNTF) 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...

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 罗西苏鹏飞刘红妮张皋胡银郭锐杨彩宁王歌杨陈曼温晓燕
Owner XIAN MODERN CHEM RES INST
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