Beta-HMX crystal form purity detection method based on X-ray powder diffraction technology

A powder diffraction, detection method technology, applied in the direction of measuring devices, preparation of samples for testing, material analysis using wave/particle radiation, etc.

Inactive Publication Date: 2019-12-17
XIAN MODERN CHEM RES INST
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Problems solved by technology

[0005] The present invention proposes a β-HMX crystal form purity detection method based on X-ray powder diffraction technology to solve the technical problem of how to detect the crystal form purity of β-HMX containing α-HMX impurity crystal form

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  • Beta-HMX crystal form purity detection method based on X-ray powder diffraction technology
  • Beta-HMX crystal form purity detection method based on X-ray powder diffraction technology
  • Beta-HMX crystal form purity detection method based on X-ray powder diffraction technology

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Embodiment

[0046] 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 .

[0047] The purity of β-HMX crystal form is calculated according to the following formula:

[0048]

[0049] Where: ω β is the purity of β-HMX crystal form ...

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Abstract

The invention provides a beta-HMX crystal form purity detection method based on an X-ray powder diffraction technology. A beta-HMX crystal form purity quantitative correction model and a correspondingcrystal form purity test method are established by combining an X-ray powder diffraction technology with a chemometrics partial least square method. On the basis of a multivariate data analysis method, effective information can be extracted from crossed and overlapped spectrums, thereby realizing quantitative crystal form analysis without independent characteristic spectrum peaks. The beta-HMX crystal form purity can be accurately determined within 10 to 15 min and the sample dosage is smaller than 50 mg; no complex sample preparation is needed in the detection process and the operation becomes safe and rapid; and a problem that the purity of the crystal form of a trace amount of sample is difficult to detect in links of a synthetic sample lab test stage, product accident research factoranalysis and the like an be solved. Therefore, the reliable and efficient detection basis can be provided for quality control of beta-HMX products and crystal form stability research of a production process and a long-term storage process.

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 X-ray powder diffraction technology 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 quality of H...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/207G01N1/28
CPCG01N23/2076G01N1/28
Inventor 王明潘清陈智群李晓宇栾洁玉
Owner XIAN MODERN CHEM RES INST
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