Beta-HMX crystal form purity detection method based on combination of intermediate infrared diffuse reflection spectrum technology with chemometrics partial least square method

A technology of purity detection and diffuse reflection, which is applied in the direction of measuring devices, material analysis through optical means, instruments, etc.

Inactive Publication Date: 2019-12-03
XIAN MODERN CHEM RES INST
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Problems solved by technology

[0006] The present invention proposes a β-HMX crystal form purity detection method based on mid-infrared diffuse reflectance spectroscopy technology to solve the technology of how to detect the crystal form purity of β-HMX with a sample size of less than 10 mg and containing α-HMX impurity crystal form question

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  • Beta-HMX crystal form purity detection method based on combination of intermediate infrared diffuse reflection spectrum technology with chemometrics partial least square method
  • Beta-HMX crystal form purity detection method based on combination of intermediate infrared diffuse reflection spectrum technology with chemometrics partial least square method
  • Beta-HMX crystal form purity detection method based on combination of intermediate infrared diffuse reflection spectrum technology with chemometrics partial least square method

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Embodiment

[0057] S1. Preparation of calibration set samples: Prepare 51 samples of mixed crystal forms of β-HMX and α-HMX with different component contents as calibration set samples. The mass of a single calibration set sample is about 200 mg, and the content of β-HMX is ≥80%. , and was more evenly distributed in the range of 80% to 100%. According to the requirements for the mass of a single sample and the content of crystal form components in the above-mentioned calibration set design, two crystal form standard samples of β-HMX and α-HMX were weighed to an accuracy of 0.01 mg. Put the two standard samples of crystal forms in the same agate mortar, transfer 5ml~8ml of chromatographically pure n-hexane, mix and grind for 3min, then transfer to a Ф25mm×25mm weighing bottle, dry in a vacuum oven at 40°C for 2h, and set aside .

[0058] The purity of β-HMX crystal form is calculated according to the following formula:

[0059]

[0060] Where: ω β is the purity of β-HMX crystal form ...

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Abstract

The invention, which belongs to the technical field, particularly relates to a beta-HMX crystal form purity detection method based on combination of an intermediate infrared diffuse reflection spectrum technology with a chemometrics partial least square method. According to the detection method, the beta-HMX crystal form purity quantitative correction model and a corresponding crystal form puritytest method are established by combining the intermediate infrared diffuse reflection spectrum technology with the chemometrics partial least square method. The established multivariable correction model can analyze the overlapped spectrum and the wide spectrum band and is suitable for analyzing the crystal form purity of a beta-HMX product containing the crystal form of the alpha-HMX impurity.

Description

technical field [0001] The invention belongs to the technical field of explosives, and in particular relates to a method for detecting the purity of β-HMX crystal form based on mid-infrared diffuse reflectance spectroscopy combined with chemometrics partial least squares method. Background technique [0002] Octometallic (HMX) is currently an explosive with high density, high energy, low sensitivity and excellent comprehensive performance among single explosives. It has been widely used as a model charge in the fields of high-energy mixed explosives, solid propellants and propellants. HMX has four crystal forms of α, β, γ, and δ, with 3,7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane (DPT) as the intermediate There are two crystal forms of α-HMX and β-HMX in the synthesized HMX terminal product, among which β-HMX has low sensitivity and high energy, which is a practical crystal form with excellent performance, and α-HMX is an impurity crystal form. In order to control the qu...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/3563
CPCG01N21/3563
Inventor 潘清王明苏鹏飞王民昌陈智群
Owner XIAN MODERN CHEM RES INST
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