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Quantitative determination method for crystal forms of hexanitrohexaazaisowurtzitane

A technology of hexanitrohexaazane and isowurtzitane, which is applied in the field of quantitative determination of hexanitrohexaazaisowurtzitane, can solve the problems of peak overlap and spectral analysis difficulties, weak vibration frequency of Raman spectrum, and low pull-through frequency. Problems such as the complex shape of the Mann peak

Inactive Publication Date: 2014-05-14
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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Problems solved by technology

[0004] The object of the present invention is to provide a solution to the problem of weak Raman spectrum vibration frequency and complex Raman peak shape in the determination of hexanitrohexaazaisowurtzitane CL-20 crystal form by Raman spectroscopy in the prior art. Quantitative determination method for problems such as peak overlap and spectral analysis are difficult

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  • Quantitative determination method for crystal forms of hexanitrohexaazaisowurtzitane
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  • Quantitative determination method for crystal forms of hexanitrohexaazaisowurtzitane

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Embodiment 1

[0026] Embodiment 1: In order to make the technical means, creative features, goals and effects of the present invention easy to understand, the present invention will be further elaborated below in conjunction with specific illustrations.

[0027] The present invention is based on the calculation of Raman peak area change rate of four CL-20 crystals of Raman spectrograms, standard curve fitting and quantitative determination method. The analysis method of Raman spectrum based on four different crystal forms of CL-20 and the quantitative analysis method of four crystal forms of explosive CL-20 are given.

[0028] 1. Sample preparation and data testing

[0029] 1.1 First, refer to the literature method to obtain pure samples of four crystal forms of CL-20, and use XRD to characterize the crystal forms, such as figure 1 As shown, compare the obtained spectrum with the standard spectrum to ensure the purity of the crystal sample.

[0030] 1.2 Secondly, before establishing the R...

Embodiment 2

[0046] 1. Take pure samples of CL-20 in γ- and ε-crystal forms. Mix γ- and ε- in equal proportions, each with a total amount of 0.2g, and make two sets of samples, the specific ratio is

[0047] The first group: γ-100%, γ-20%+ε-, γ-40%+ε-, γ-60%+ε-, γ-80%+ε-, ε-100%

[0048] The second group: γ-10%+ε-, γ-30%+ε-, γ-50%+ε-, γ-70%+ε-, γ-90%+ε-

[0049] Each sample was ground and mixed with a mortar and pestle to obtain a homogeneous mixture. (γ-,ε-)CL-20 mixtures with different proportions are at 810~870cm -1 The Raman absorption spectrum of the region, such as Figure 5 shown. By calculation 849cm -1 、828cm -1 The sum of the peak intensities of these two characteristic peaks is established by dividing one of the peak intensities by the sum of the two peak intensities to obtain a characteristic curve relative to %ε-CL-20. The concentration of α-CL-20 was plotted against the change rate of the two characteristic peaks of the (γ-,ε-)CL-20 mixture to obtain Image 6 , it can...

Embodiment 3

[0052] Take α- and ε-two pure samples of CL-20. Mix α- and ε- in equal proportions, each with a total amount of 0.2g, and make two sets of samples, the specific ratio is

[0053] The first group: α-100%, α-20%+ε-, α-40%+ε-, α-60%+ε-, α-80%+ε-, ε-100%;

[0054] The second group: α-10%+ε-, α-30%+ε-, α-50%+ε-, α-70%+ε-, α-90%+ε-.

[0055] Each sample was ground and mixed with a mortar and pestle to obtain a homogeneous mixture. Raman spectrometer was used to collect different ratios of (α-,ε-)CL-20 mixtures at 810-870cm -1 The Raman absorption spectrum of the region, such as Figure 7 shown. By calculation 849cm -1 、828cm -1 The sum of the peak intensities of these two characteristic peaks is established by dividing one of the peak intensities by the sum of the two peak intensities to obtain a characteristic curve relative to %ε-CL-20. The concentration of α-CL-20 was plotted against the change rate of the two characteristic peaks of the (α-,ε-)CL-20 mixture to obtain Fi...

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Abstract

The invention discloses a quantitative determination method for crystal forms of hexanitrohexaazaisowurtzitane. The quantitative determination method comprises the following steps: classifying the calculation results according to a main ingredient analysis method, selecting an analysis area, establishing the equation of change parameters to the content of two crystal forms to obtain a standard curve, performing raman test on the constant content of other alpha-, beta- and gama- crystal forms in the prepared epsilon-CL-20 by taking the standard curve as standard, and performing the quantitative content determination experiment reference to the established standard curve. Compared with the existing determination method, the raman spectroscopy in the field of evidence identification of recent years is introduced in the field of explosive detection, the study proves that the CL-20 spectrogram difference of the four crystal forms is obvious in the raman spectroscopy detection, the characteristic peak strength is changed along with the proportional mixing of different crystal forms, finally the standard proportion curve of different crystal form mixture can be obtained, and the quantitative content analysis for different Cl-20 crystal forms can be realized by utilizing the established standard curve.

Description

technical field [0001] The invention relates to a technique for quantitatively determining the crystal form of hexanitrohexaazaisowurtsane, in particular to a method for quantitatively determining the crystal form of hexanitrohexaazaisowurtsane. Background technique [0002] Hexanitrohexaazaisowurtzitane (commonly known as CL-20, abbreviated as HNIW) is a new clathrate compound with high density, high energy, high detonation pressure and high detonation velocity discovered and synthesized in recent years. Highest elemental explosive. CL-20 was first synthesized by NieIsen, the U.S. Naval Weapons Center, and is called "a breakthrough fourth-generation energetic material" by American experts and "the most powerful non-nuclear explosive." CL-20 exists stably in four crystalline forms of α-, β-, γ- and ε- under normal temperature and pressure. Different crystalline forms of CL-20 have different properties (such as sensitivity, detonation performance, etc.), and these properties...

Claims

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Application Information

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IPC IPC(8): G01N21/65
Inventor 何璇王慧徐金江鲁洪齐天骄王蔺罗毅威
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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