CN103792222A - Quantitative determination method for crystal forms of hexanitrohexaazaisowurtzitane - Google Patents
Quantitative determination method for crystal forms of hexanitrohexaazaisowurtzitane Download PDFInfo
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- CN103792222A CN103792222A CN201410053202.2A CN201410053202A CN103792222A CN 103792222 A CN103792222 A CN 103792222A CN 201410053202 A CN201410053202 A CN 201410053202A CN 103792222 A CN103792222 A CN 103792222A
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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
The present invention relates to a kind of Hexanitrohexaazaisowurtzitane crystal formation quantitative measurement technology, specially refer to a kind of Hexanitrohexaazaisowurtzitane crystal formation method for quantitatively determining.
Background technology
Hexanitrohexaazaisowurtzitane (be commonly called as CL-20, be abbreviated as HNIW) is the cage compound of finding in recent years synthetic novel high-density, high-energy, high detonation pressure, high explosion velocity, is the highest single chmical compound explosive of energy of applying up to now.CL-20 is synthesized the earliest by USN's weapon center NieIsen, is referred to as " breakthrough the 4th generation energetic material " by US Experts, is " the non-nuclear explosives that power is the most powerful ".CL-20 stable existence α at normal temperatures and pressures-, β-, γ-and ε-tetra-kind of crystal formation, the CL-20 character each variant (as sensitivity, detonation property etc.) of different crystal forms, and these character are extremely important to the application of CL-20.In four kinds of crystal formations of CL-20, ε-crystal formation density maximum, thermal stability is best, and sensitivity is also minimum, and that in weaponry, applies is ε-CL-20.In the time that the CL-20 of other crystal formations is converted into ε crystal formation, not only require the chemical purity of CL-20, and require crystal formation purity, how this just must solution differentiate various crystal formations and how to confirm ε crystal formation and these two problems of other crystal formation content.
At present, the quantitative analysis method of crystal formation mainly contains: infra-red sepectrometry, X-ray diffraction method etc.For infra-red sepectrometry, conventionally need compressing tablet, sample preparation is extremely loaded down with trivial details, and infrared peak is conventionally very wide, is unfavorable for quantitative test.X-ray diffraction method sensitivity is lower comparatively speaking, is not suitable for the quantitative test of the less or low content material of sample size.Therefore, need to develop a kind of quick, accurate, easy method the crystal formation of CL-20 is carried out to qualitative and quantitative analysis, to solve the problem of the loaded down with trivial details and insufficient sensitivity of the sample preparation existing in the quantitative test of current CL-20 crystal formation.
Summary of the invention
Object of the present invention is just to provide a kind of and has solved that prior art adopts that Raman spectroscopy measures that the Raman spectrum vibration frequency that Hexanitrohexaazaisowurtzitane CL-20 crystal formation exists is weak, Raman peaks peak shape complexity and peak position is overlapping and the comparatively method for quantitatively determining of the problem such as difficulty of spectrum analysis.
To achieve these goals, the technical solution used in the present invention is: a kind of Hexanitrohexaazaisowurtzitane crystal formation shape method for quantitatively determining, and method is as follows,
A. first the different α of the many groups of configuration-and ε-, β-and ε-and γ-and the Hexanitrohexaazaisowurtzitane CL-20 blend sample of ε-crystal formation proportioning,
B. adopting fourier transform raman spectroscopy method to measure respectively CL-20 potpourri wave-number range is 810-870cm
-1the Raman spectrogram in region,
C. set up respectively the linear relation of α-CL-20, β-CL-20 in relative peak height and CL-20 potpourri or γ-CL-20 crystal formation content by the peak intensity rate of change of nitro characteristic peak,
D. when quantitative measurement take this linear relation as benchmark, the sample of other α-CL-20, β-CL-20, γ-CL-20 crystal formation constant concentration in preparation ε-CL-20 is carried out to Raman test, with reference to the typical curve of setting up, carry out content quantitative determination experiment;
As preferably, in step a, the preparation of sample and Purity, according to solvent recrystallization method prepare respectively α-, β-, γ-and ε-tetra-kind of crystal C L-20 sample, and characterize its purity with XRD;
As preferably, in step b, will carry out Raman spectrum detection by Fourier Raman spectrometer through pretreated sample, obtain the Raman spectrogram of this sample; The parameter of Fourier Raman spectrometer used arranges as follows: instrument: Nicolet DXR SmartRaman spectrometer; Test condition: optical maser wavelength is 532nm, laser energy is 5mW, and wave-number range is 3500-50cm-1, and resolution is that 4cm-1 background times of collection is 32 times, and sample collection number of times is 32 times;
As preferably, in step c, α in described relative peak height and CL-20 potpourri-, β-or the method for building up of the linear relation of γ-crystal formation content is as follows, calculating many group blend sample wave-number ranges is 810-870cm
-1the Raman spectrogram in region the strong sum in peak; Set up equation with one of them peak intensity divided by two peak intensity sums, can obtain the sign curve with respect to crystal formation content; Number percent take crystal formation content is mapped as the longitudinal axis as transverse axis, the two strong rate of change in peak, obtains the two strong rate of change in peak and is linear increase with respect to the number percent of crystal formation content, fits to straight line, that is: with data point in scheming
X＝a+kY
In formula, X be CL-20 potpourri α-, β-or γ-crystal formation content, a is constant, k is coefficient, Y is the two strong rate of change in peak, its value can be by being 810-870cm to wave-number range
-1the Raman spectrum map analysis in region obtains;
As preferably, in step a, the blend sample group number of configuration is more than five groups or five groups.
Compared with prior art, the invention has the advantages that: Raman sample preparation and easy, only need be bonded at sample on sample stage direct-detection.Therefore, we introduce explosive check field the Raman spectroscopy that more and more shows in recent years advantage in the material evidence field of identifying especially.Find by research, in Raman spectrum detects, the CL-20 spectrogram difference of four kinds of crystal formations is obvious, and along with the proportioning of different crystal forms is mixed, characteristic peak intensity also changes thereupon.Finally, we can obtain the typical curve of different crystal forms mixture ratio, utilize the typical curve of setting up, and can realize the quantitative test to CL-20 different crystal forms content.
Accompanying drawing explanation
Fig. 1 XRD characterizes the CL-20 of four kinds of different crystal forms;
Fig. 2 α-, β-, γ-and Raman spectrogram of ε-tetra-kind of crystal C L-20;
Fig. 3 is β-CL-20 Raman abosrption spectrogram of different proportionings in example one;
The typical curve of % β-CL-20 in Fig. 4 example one;
Fig. 5 is γ-CL-20 Raman abosrption spectrogram of different proportionings in example two;
Fig. 6 is the typical curve of % γ-CL-20 in example two;
Fig. 7 is α-CL-20 Raman abosrption spectrogram of different proportionings in example three;
Fig. 8 is the canonical plotting of % α-CL-20 in example three.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
Embodiment 1: for technological means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with concrete diagram, further set forth the present invention.
The present invention is the calculating of the Raman peaks area change rate of four kinds of CL-20 crystal based on Raman spectrogram, typical curve matching, thereby the method for quantitative measurement.The Raman spectrum figure analytic method based on four kinds of different crystal forms CL-20 and the method to tetra-kinds of crystal formation quantitative test of explosive CL-20 are provided.
1. the preparation of sample and data test
1.1 first, and reference literature method obtains the pure sample product of four kinds of crystal formations of CL-20, and carry out crystal formation sign with XRD, as shown in Figure 1, obtained spectrogram and standard spectrogram compared, and guarantees the purity of crystal form samples.
Secondly 1.2, before setting up four kinds of crystal C L-20 Raman Spectra picture libraries, first respectively to α-, β-, γ-and ε-tetra-kind of a crystal C L-20 sample carry out Raman mensuration.Take 3-5mgCL-20 sample and adhere on objective table, keep sample surfaces smooth, directly carry out Raman test, obtain the Raman 50-3500cm of four kinds of crystal C L-20
-1spectrogram, as shown in Figure 2, the CL-20 Raman peak position of four kinds of different crystal forms has subtle difference, overlapping part is more, peak shape complexity, is calculated feature peak position is carried out to spectrum elucidation by theory, can provide very abundant information to the crystal formation the Nomenclature Composition and Structure of Complexes feature of CL-20.
2. density functional method carries out Raman spectrum elucidation
2.1 calculating molecular vibrations and Raman spectrogram are pointed out
First, adopt B3LYP to mix functional and 6-311G (d) group of functions method, utilize density functional theory (DFT) to calculate respectively the molecular vibrational frequency of tetra-kinds of crystal formations of explosive CL-20, the conventional Raman spectrum of CL-20 molecule has been carried out to detailed pointing out, its vibration mode is belonged to, calculate according to theory, the vibration peak displacement of CL-20 that contrast experiment obtains, can draw the place peak position of each characteristic group.
The Raman peak position of explosive CL-20 is resolved, as shown in the table:
3. quantitative test
Get β-and the CL-20 pure sample of ε-two kind of crystal formation.So that β-with ε-carrying out equal proportion mixes, every part of total amount is 0.2g, makes two groups of samples, concrete proportioning is respectively:
First group: β-100%, β-10%+ ε-, β-20%+ ε-, β-30%+ ε-, β-30%+ ε-, β-40%+ ε-, β-50%+ ε-, β-60%+ ε-, β-70%+ ε-, β-80%+ ε-, β-90%+ ε-, ε-100%
Second group: β-1%+ ε-, β-3%+ ε-, β-5%+ ε-
Every duplicate samples is all carried out ground and mixed with mortar, makes it to mix.
(β-, ε-) CL-20 potpourri of different proportionings is at 810～870cm
-1the Raman abosrption spectrogram in region, as shown in Figure 3, by calculating 838cm
-1, 828cm
-1the strong sum in peak of these two characteristic peaks, sets up equation with one of them peak intensity divided by two peak intensity sums, can obtain the sign curve with respect to % β-CL-20.The characteristic peak two strong rate of change mappings in peak by β-CL-20 concentration to (β-, ε-) CL-20 potpourri, obtain Fig. 4, the visible increase along with β-CL-20 percentage composition, the variation of absorption peak strength is linear to be increased, and in figure, data point fits to straight line, wherein fitting correlation coefficient R
2=0.9974, SD=0.0158, N=3, proves that data point linear relationship is good, therefore, the method can be used for the content of the beta-crystal in quantitative test ε-CL-20.Then, prepared the sample of beta-crystal constant concentration in ε-CL-20, be respectively D: β-20%+ ε-CL-20, E: β-40%+ ε-CL-20, F: β-60%+ ε-CL-20, G: β-80%+ ε-CL-20, with reference to the typical curve of setting up, carries out other content quantitative determination experiments.Reference standard curve, calculation deviation is not more than ± and 4%.
Between the sensitivity of the method for the present invention, prepare again the sample of the fixing low content of beta-crystal in ε-CL-20, be respectively A: β-1%+ ε-CL-20, B: β-3%+ ε-CL-20, C: β-5%+ ε-CL-20; Utilize Raman spectrum to carry out crystal formation quantitative measurement experiment, reference standard curve, calculation deviation is not more than ± and 0.5%.Utilize Raman spectrum to carry out crystal formation quantitative measurement experiment, therefore, the method has good sensitivity and accuracy for crystal formation quantitative test, can be used for existing in ε-CL-20 the Quantitative Study of low content beta-crystal sample.
Working sample and deviation list β-ε %, as shown in the table:
Embodiment bis-:
1, get γ-and the CL-20 pure sample of ε-two kind of crystal formation.So that γ-with ε-carrying out equal proportion mixes, every part of total amount is 0.2g, makes two groups of samples, concrete proportioning is respectively
First group: γ-100%, γ-20%+ ε-, γ-40%+ ε-, γ-60%+ ε-, γ-80%+ ε-, ε-100%
Second group: γ-10%+ ε-, γ-30%+ ε-, γ-50%+ ε-, γ-70%+ ε-,, γ-90%+ ε-
Every duplicate samples is all carried out ground and mixed with mortar, makes it to mix.(γ-, ε-) CL-20 potpourri of different proportionings is at 810～870cm
-1the Raman abosrption spectrogram in region, as shown in Figure 5.By calculating 849cm
-1, 828cm
-1the strong sum in peak of these two characteristic peaks, sets up equation with one of them peak intensity divided by two peak intensity sums, can obtain the sign curve with respect to % ε-CL-20.The characteristic peak two strong rate of change mappings in peak by α-CL-20 concentration to (γ-, ε-) CL-20 potpourri, obtain Fig. 6, the visible increase along with γ-CL-20 percentage composition, the variation of absorption peak strength is linear to be increased, and in figure, data point fits to straight line, wherein fitting correlation coefficient R
2=0.9962, SD=0.0147, N=3, proves that data point linear relationship is good, therefore, the method can be used for the content of the γ-crystal formation in quantitative test ε-CL-20.Then, prepare the sample of γ-crystal formation constant concentration in ε-CL-20, be respectively A: γ-10%+ ε-CL-20, B: γ-30%+ ε-CL-20, C: γ-50%+ ε-CL-20, D: γ-70%+ ε-CL-20, E: γ-90%+ ε-CL-20, with reference to the typical curve of setting up, carries out other content quantitative determination experiments.Utilize Raman spectrum to carry out crystal formation quantitative measurement experiment, reference standard curve, calculation deviation is not more than ± and 3%.Therefore, the method has good sensitivity and accuracy for crystal formation quantitative test, can be used for existing in ε-CL-20 the Quantitative Study of low content r-crystal form samples.Working sample and deviation list r-ε %, as shown in the table:
Embodiment tri-:
Get α-and the CL-20 pure sample of ε-two kind of crystal formation.So that α-with ε-carrying out equal proportion mixes, every part of total amount is 0.2g, makes two groups of samples, concrete proportioning is respectively
First group: α-100%, α-20%+ ε-, α-40%+ ε-, α-60%+ ε-, α-80%+ ε-, ε-100%;
Second group: α-10%+ ε-, α-30%+ ε-, α-50%+ ε-, α-70%+ ε-,, α-90%+ ε-.
Every duplicate samples is all carried out ground and mixed with mortar, makes it to mix.(α-, ε-) the CL-20 potpourri that gathers different proportionings with Raman spectrometer is at 810～870cm
-1the Raman abosrption spectrogram in region, as shown in Figure 7.By calculating 849cm
-1, 828cm
-1the strong sum in peak of these two characteristic peaks, sets up equation with one of them peak intensity divided by two peak intensity sums, can obtain the sign curve with respect to % ε-CL-20.The characteristic peak two strong rate of change mappings in peak by α-CL-20 concentration to (α-, ε-) CL-20 potpourri, obtain Fig. 8, the visible increase along with ε-CL-20 percentage composition, the variation of absorption peak strength is linear to be increased, and in figure, data point fits to straight line, wherein fitting correlation coefficient R
2=0.9842, SD=0.0172, N=3, proves that data point linear relationship is good, therefore, the method can be used for the content of the α-crystal formation in quantitative test ε-CL-20.Then, prepare the sample of α-crystal formation constant concentration in ε-CL-20, be respectively A: α-10%+ ε-CL-20, B: α-30%+ ε-CL-20, C: α-50%+ ε-CL-20, D: α-70%+ ε-CL-20, E: α-90%+ ε-CL-20, with reference to the typical curve of setting up, carries out other content quantitative determination experiments.Utilize Raman spectrum to carry out crystal formation quantitative measurement experiment, reference standard curve, calculation deviation is not more than ± and 2%., therefore, the method has good sensitivity and accuracy for crystal formation quantitative test, can be used for existing in ε-CL-20 the Quantitative Study of low content a-crystal form samples.
Working sample and deviation list a-ε %, as shown in the table:
Above to Hexanitrohexaazaisowurtzitane crystal formation shape method for quantitatively determining provided by the present invention, carry out detailed introduction, applied specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, to be possible to change of the present invention and improvement, and can not exceed design and the scope of accessory claim defined, in sum, this description should not be construed as limitation of the present invention.
Claims (5)
1. a Hexanitrohexaazaisowurtzitane crystal formation shape method for quantitatively determining, is characterized in that: method is as follows,
A. first the different α of the many groups of configuration-and ε-, β-and ε-and γ-and the Hexanitrohexaazaisowurtzitane CL-20 blend sample of ε-crystal formation proportioning,
B. adopting fourier transform raman spectroscopy method to measure respectively CL-20 potpourri wave-number range is 810-870cm
-1the Raman spectrogram in region,
C. set up respectively the linear relation of α-CL-20, β-CL-20 in relative peak height and CL-20 potpourri or γ-CL-20 crystal formation content by the peak intensity rate of change of nitro characteristic peak,
D. when quantitative measurement take this linear relation as benchmark, the sample of other α-CL-20, β-CL-20, γ-CL-20 crystal formation constant concentration in preparation ε-CL-20 is carried out to Raman test, with reference to the typical curve of setting up, carry out content quantitative determination experiment.
2. Hexanitrohexaazaisowurtzitane crystal formation shape method for quantitatively determining according to claim 1, it is characterized in that: in step a, the preparation of sample and Purity, according to solvent recrystallization method prepare respectively α-, β-, γ-and ε-tetra-kind of crystal C L-20 sample, and characterize its purity with XRD.
3. Hexanitrohexaazaisowurtzitane crystal formation shape method for quantitatively determining according to claim 1, is characterized in that: in step b, will carry out Raman spectrum detection by Fourier Raman spectrometer through pretreated sample, and obtain the Raman spectrogram of this sample.
4. Hexanitrohexaazaisowurtzitane crystal formation shape method for quantitatively determining according to claim 1, it is characterized in that: in step c, α in described relative peak height and CL-20 potpourri-, β-or the method for building up of the linear relation of γ-crystal formation content is as follows, calculating many group blend sample wave-number ranges is 810-870cm
-1the Raman spectrogram in region the strong sum in peak; Set up equation with one of them peak intensity divided by two peak intensity sums, can obtain the sign curve with respect to crystal formation content; Number percent take crystal formation content is mapped as the longitudinal axis as transverse axis, the two strong rate of change in peak, obtains the two strong rate of change in peak and is linear increase with respect to the number percent of crystal formation content, fits to straight line, that is: with data point in scheming
X＝a+kY
In formula, X be CL-20 potpourri α-, β-or γ-crystal formation content, a is constant, k is coefficient, Y is the two strong rate of change in peak, its value can be by being 810-870cm to wave-number range
-1the Raman spectrum map analysis in region obtains.
5. Hexanitrohexaazaisowurtzitane crystal formation shape method for quantitatively determining according to claim 1, is characterized in that: in step a, the blend sample group number of configuration is more than five groups or five groups.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104833652A (en) * | 2015-04-15 | 2015-08-12 | 北京理工大学 | Method for rapidly analyzing content of cellulose nitrate in mixed material |
| CN108760719A (en) * | 2018-08-17 | 2018-11-06 | 北京理工大学 | A method of utilizing the crystal form purity of Raman spectrum analysis CL-20 |
| CN108956661A (en) * | 2018-05-22 | 2018-12-07 | 广西壮族自治区食品药品检验所 | Measure the powder X-ray diffractometry of alpha-crystal form content in glycine bulk pharmaceutical chemicals |
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| CN112067596A (en) * | 2020-08-24 | 2020-12-11 | 西安近代化学研究所 | In-situ analysis method for HNIW crystal form crystal transformation rate in propellant powder |
| CN112067640A (en) * | 2020-08-24 | 2020-12-11 | 西安近代化学研究所 | Method for determining crystal form purity value of HNIW crystal form standard substance |
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| CN112098623A (en) * | 2020-08-24 | 2020-12-18 | 西安近代化学研究所 | Method for determining crystal form purity value of alpha-HNIW crystal form standard substance |
| CN112098444A (en) * | 2020-08-24 | 2020-12-18 | 西安近代化学研究所 | Gamma-HNIW crystal form standard substance crystal form purity value determination method |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214325A (en) * | 2013-04-01 | 2013-07-24 | 中国工程物理研究院化工材料研究所 | Preparation method of hexaazaisowurtzitane crystal |
-
2014
- 2014-02-17 CN CN201410053202.2A patent/CN103792222A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214325A (en) * | 2013-04-01 | 2013-07-24 | 中国工程物理研究院化工材料研究所 | Preparation method of hexaazaisowurtzitane crystal |
Non-Patent Citations (6)
| Title |
|---|
| 刘进全等: "ε-HNIW在不同溶剂中的晶型稳定性", 《含能材料》, vol. 14, no. 2, 30 April 2006 (2006-04-30), pages 108 - 110 * |
| 孟征等: "用傅立叶变换拉曼光谱定量分析HNIW的β-和ε-晶型混合物", 《含能材料》, vol. 19, no. 3, 19 October 2011 (2011-10-19), pages 339 - 342 * |
| 孟征等: "用傅立叶变换拉曼光谱定量分析HNIW的γ-和ε-晶型混合物", 《火炸药学报》, vol. 33, no. 5, 15 October 2010 (2010-10-15), pages 13 - 14 * |
| 徐金江等: "CL-20重结晶过程中的晶型转变研究进展", 《含能材料》, vol. 20, no. 2, 31 December 2012 (2012-12-31), pages 248 - 255 * |
| 王慧等: "CL-20拉曼光谱的密度泛函理论计算及晶型定量分析研究", 《2013年第二届全国危险物质与安全应急技术研讨会论文集》, 15 November 2013 (2013-11-15), pages 219 - 224 * |
| 高海燕等: "六硝基六氮杂异伍兹烷的ε与γ型混合物的定量分析", 《火炸药学报》, vol. 23, no. 2, 8 January 2004 (2004-01-08), pages 1 * |
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| CN112067596A (en) * | 2020-08-24 | 2020-12-11 | 西安近代化学研究所 | In-situ analysis method for HNIW crystal form crystal transformation rate in propellant powder |
| CN112098623B (en) * | 2020-08-24 | 2022-10-25 | 西安近代化学研究所 | Method for determining crystal form purity value of alpha-HNIW crystal form standard substance |
| CN113030061B (en) * | 2021-03-11 | 2022-08-02 | 湖南大学 | Method for rapidly characterizing purity of titanium dioxide |
| CN113030061A (en) * | 2021-03-11 | 2021-06-25 | 湖南大学 | Method for rapidly characterizing purity of titanium dioxide |
| CN113640277A (en) * | 2021-08-26 | 2021-11-12 | 中国工程物理研究院化工材料研究所 | Method for rapidly identifying eutectic explosive structure based on chemometrics |
| CN113640277B (en) * | 2021-08-26 | 2023-08-22 | 中国工程物理研究院化工材料研究所 | Method for rapidly identifying eutectic explosive structure based on chemometrics |
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