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GC-AED (gas chromatography-atomic emission detector) irrelevant calibration curve (CIC) method for quantitatively determining DNTF content

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

Active Publication Date: 2019-03-26
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

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  • GC-AED (gas chromatography-atomic emission detector) irrelevant calibration curve (CIC) method for quantitatively determining DNTF content
  • GC-AED (gas chromatography-atomic emission detector) irrelevant calibration curve (CIC) method for quantitatively determining DNTF content
  • GC-AED (gas chromatography-atomic emission detector) irrelevant calibration curve (CIC) method for quantitatively determining DNTF content

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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: 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 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, 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 as follows: 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 chromatog...

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Abstract

The invention discloses a GC-AED (gas chromatography-atomic emission detector) irrelevant calibration curve (CIC) method for quantitatively determining the DNTF content. A chromatographic column usedin the disclosed gas chromatographic analysis method is an HP-5 weakly polar capillary column, the temperature of an injection port is 200 DEG C, the temperature of a column oven is 170 DEG C, the split ratio is 20:1, the injection volume is 0.5 mu L, and the column flow rate is 2 mL / min; AED parameters are as follows: the temperature of a transmission line is 220 DEG C and the temperature of a chamber is 250 DEG C; C is adopted as a detection element, and the wavelength is C193 nm; O2 and H2 are adopted as reaction gases; and the gas pressure of supplemental gas He is 200 KPa. The disclosed method for quantitatively detecting the DNTF comprises the steps of analyzing benzoic acid and the DNTF with a chromatographic analysis method; detecting the C element of the benzoic acid and the C element of the DNTF through an AED detector, wherein the detection wavelength is C193 nm; and calculating the C element content of the DNTF with the C element content of the benzoic acid as a standard toobtain the compound content of the DNTF. The elemental chromatographic analysis method has a good peak shape, the compound is quantified based on a non-self and non-energetic standard sample, and high accuracy and high repeatability are achieved.

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 Applications(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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