CN105300957B - A kind of explosive eutectic structure authentication method - Google Patents
A kind of explosive eutectic structure authentication method Download PDFInfo
- Publication number
- CN105300957B CN105300957B CN201510737960.0A CN201510737960A CN105300957B CN 105300957 B CN105300957 B CN 105300957B CN 201510737960 A CN201510737960 A CN 201510737960A CN 105300957 B CN105300957 B CN 105300957B
- Authority
- CN
- China
- Prior art keywords
- explosive
- raman
- eutectic
- peak
- btf
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a kind of explosive eutectic structure authentication method, first determines the Raman spectrogram of cocrystallized explosive sample and single chmical compound explosive sample, obtains corresponding Fingerprints peak；B3LYP mixing Functional Approachs are used again, calculate the vibration frequency of explosive molecules respectively using DFT density functional theories, then the Fingerprints peak of explosive molecules is pointed out, its vibration mode is belonged to；Finally the Raman spectrogram of cocrystallized explosive sample and two kinds of single chmical compound explosive samples is contrasted, according to the vibrations peak shift at the Fingerprints peak of two kinds of single chmical compound explosive samples, the vibration mode of cocrystallized explosive sample is belonged to, and by Raman signatures displacement, analyzes the reason for eutectic structure is formed.The present invention is using single chmical compound explosive, single chmical compound explosive is simply mixed two-by-two and single chmical compound explosive react two-by-two after the Raman spectrum of eutectic that is formed it is inconsistent, produce different Raman peak positions to change and to carry out explosive eutectic quick analysis and identification.
Description
Technical field
Embodiments of the present invention are related to energetic material field, more specifically, embodiments of the present invention are related to a kind of fry
Medicine eutectic structure authentication method.
Background technology
In energetic material field, researchers are directed to developing energy height, the explosive that sensitivity is low, cost is low always.At present
Mainly there are two thinkings to the development approach of high-energy insensitive explosive：The exploitation of new single chmical compound explosive, and to existing explosive formulation
It is modified.Because the research and development of new single chmical compound explosive are difficult to make a breakthrough in a short time, and the mistake of modification explosive formula
It can also be related to mixing uneven, thermal coefficient of expansion not parity problem in journey, both approaches exist more in practical study
Problem, make slow progress.Therefore, if from molecular level, different explosive molecules are mixed to form cocrystallized explosive, such side
Method is of increased attention.Research shows, by forming cocrystallized explosive, can effectively improve the oxygen balance of part explosive,
Sensitivity, its sudden-heat, acting ability and security etc. are improved, there are wide Research Prospects.In addition, the formation of cocrystallized explosive also can
Enough improve other performances such as solubility property, the fusing point of part explosive, different use demands can be met.Therefore, cocrystallized explosive
Thought catered to the world today to explosive high energy and the unwise demand for development helped to change, carried to develop serial high Energy Density Materials
Supply to instruct, there is important learning value and wide application prospect.
However, although eutectic technology have passed through the development of long period, but it analyzes and identifies means and immature, usually goes out
The situation that existing eutectic cannot be distinguished by with single chmical compound explosive.Therefore, development is quick, and effective explosive eutectic authentication method can be in reality
Distinguish whether single chmical compound explosive raw material has formed eutectic in production, and simple substance is separated from cocrystallized explosive, re-start eutectic
Synthesis.To the purity of explosive eutectic, adjusting eutectic production technology in good time has extensive and far-reaching practical significance.At present, characterize
The method of co-crystal structures is a lot, there is powder X-ray diffractometry (PXRD), single crystal method of X-ray diffractometry, infrared spectrum (IR), drawing
Graceful spectrum, terahertz time-domain spectroscopy (THz-TDS), differential scanning calorimetry (DSC), nuclear magnetic resonance etc., wherein PXRD and monocrystalline X
Ray diffraction method is to characterize the most commonly seen means of cocrystallized explosive, and it is respectively intended to carry out crystal species analysis and structure determination with dividing
Analysis.However, both approaches are more to the dosage demand of sample, quality also requires higher, and eutectic can be formed for some, obtains
Less explosive is measured, then is less applicable.
Raman spectrum is found therefore Raman also obtains Nobel's thing by India's physicist's Raman first in nineteen twenty-eight
Neo-Confucianism prize.First feature of Ramam effect is that each material (molecule) has the Raman spectrum of oneself, can be used as and characterize
This speciality is used.The bands of a spectrum number of Raman spectrum, band intensity, displacement etc. caused by each molecule are directly and molecule
Vibration and rotate it is associated, so Raman spectrum belongs to the vibration and rotation spectrum of molecule, usual abbreviation molecular spectrum.Raman
Spectrum, as excitation source, realizes lossless not exposure test using low power laser light source.Because laser beam is very thin, analysis
The spatial resolution of sample is very high, it is possible to achieve micro- micro-zone analysis, so for solid granulates mixture analysis have it is larger
Advantage.However, Raman spectrum vibration frequency is weaker, the bad differentiation of Raman peaks.
The content of the invention
Instant invention overcomes the deficiencies in the prior art, there is provided a kind of explosive eutectic structure authentication method, it is expected to be
The process control of explosive eutectic production and control with raw material provide a kind of quickly discriminating means.
To achieve the above object, the present invention is by using fourier transform raman spectroscopy analysis method, using single chmical compound explosive,
Single chmical compound explosive is simply mixed two-by-two and single chmical compound explosive react two-by-two after the Raman spectrum of eutectic that is formed it is inconsistent, produce not
Same Raman peak position change to carry out explosive eutectic quick analysis and identification.The inventive method belongs to a kind of qualitatively eutectic knot
Structure and Components identification analysis method, can be used for the screening and control of explosive eutectic.The equipment that this method uses is easy with instrument
It is easy to get, is used in and promotes the use of on a large scale.
The requirement that Raman spectrum is prepared to sample is very low, substantially without sample preparation, and does not contact, sample will not be made with sample
Into pollution and destroy.And very low is required to sample size, the sample of Gamma Magnitude is with regard to that can be detected.Therefore, we are in recent years
The Raman spectroscopy for increasingly showing advantage especially in material evidence identification field introduces explosive inspection field.Due to spectrum vibration frequency compared with
It is weak, the bad differentiation of Raman peaks, if desired the Raman peaks of molecule are pointed out, then the help that Need Hierarchy Theory calculates.
Density functional theory (DFT is theoretical) can be used for calculating the structure and vibrational spectrum of molecule., will using DFT method
Theoretical and experiment value compares can be with apparent understanding intramolecule information.
The explosive molecules normal Raman spectrum such as TNT, CL-20, BTF has been carried out using Raman spectrum it is detailed point out, it is right
Its vibration mode is belonged to, and according to theoretical calculation, contrast experiment obtains the vibration peak shift of explosive molecules, to two kinds of explosives
Eutectic carries out vibration mode differentiation.And by Raman signatures displacement, eutectic Crack cause is inquired into, is a kind of new explosive eutectic point
The method that analysis characterizes identification.
The explosive eutectic identification characterizing method of the present invention uses following technical scheme：
A kind of explosive eutectic structure authentication method, comprises the following steps：
S1, the Raman spectrogram for determining using fourier transform raman spectroscopy analysis method cocrystallized explosive sample to be identified respectively
And the Raman spectrogram of two kinds of single chmical compound explosive samples of the cocrystallized explosive sample to be identified is formed, show that eutectic to be identified is fried respectively
The Fingerprints peak of medicine sample and two kinds of single chmical compound explosive samples；
S2, using B3LYP mixing Functional Approachs, calculate the fried of two kinds of single chmical compound explosives respectively using DFT density functional theories
The vibration frequency of medicine molecule, according to result of calculation respectively to the Fingerprints peak of the explosive molecules of two kinds of single chmical compound explosive samples
Progress is detailed to be pointed out, and its vibration mode is belonged to；
S3, the Raman spectrogram of the Raman spectrogram of cocrystallized explosive sample to be identified and two kinds of single chmical compound explosive samples carried out pair
Than according to the vibrations peak shift at the Fingerprints peak of two kinds of single chmical compound explosive samples, to the vibration mode of cocrystallized explosive sample
Belonged to, and by Raman signatures displacement, analyze the reason for eutectic structure is formed.
For the instrument that the step S1 measure Raman spectrogram uses for Fourier Raman spectrometer, its test condition is as follows：Swash
Light wave a length of 532nm, laser energy 5mW, resolution ratio 4cm-1, background times of collection is 32 times, and sample collection number is 32
It is secondary.
Raman collection of illustrative plates of the reason for eutectic structure formation is analyzed described in step S3 including analyzing cocrystallized explosive sample to be identified
Peak intensity reason of changes and peak shift reason.
It before eutectic structure identification, need to first judge whether cocrystallized explosive sample to be identified really forms eutectic structure, judge
Method is：By the Raman spectrogram of the step S1 cocrystallized explosive samples to be identified obtained with forming the cocrystallized explosive sample to be identified
The Raman spectrograms of two kinds of single chmical compound explosive samples contrasted, if the Raman spectrogram of cocrystallized explosive sample to be identified is two kinds of simple substance
The simple superposition of the Raman spectrogram of explosive sample, and the red shift without peak position or blue shift movement change, then illustrate that eutectic to be identified is fried
Medicine sample does not form real cocrystallized explosive, it is impossible to carries out eutectic structure identification；Conversely, then illustrate cocrystallized explosive sample to be identified
Product form real cocrystallized explosive, can carry out eutectic structure identification.
Technical scheme is further parsed below.
Technical scheme includes following steps in practical operation：
1st, eutectic sample is prepared.The technology of preparing of cocrystallized explosive has had more open source literature, is remembered according to these documents
The technology of load prepares cocrystallized explosive, such as BTF and Cl-20 cocrystallized explosive or TNT and Cl-20 cocrystallized explosive.
2nd, composite explosives are prepared.Two kinds of single compound explosives of cocrystallized explosive are taken to carry out equal proportion mixing, every part of total amount is 0.2g,
Every part of sample is all ground mixing with mortar, is allowed to well mixed.Such as BTF and ε-crystal formation two kinds of single chmical compound explosives of Cl-20
Ratio is mixed and ground, or TNT is mixed and ground with the Cl-20 equal proportions of ε-crystal formation.
3rd, the Raman spectrogram collection of single chmical compound explosive and peak position are pointed out.3-5mg single chmical compound explosive pure sample product are weighed respectively adheres to Fu
On vertical leaf Raman spectrometer objective table, keep sample surfaces smooth, directly carry out Raman test, obtain single chmical compound explosive such as Cl-20,
TNT, BFT etc. Raman 2000-200cm-1Spectrogram, test condition：Optical maser wavelength is 532nm, laser energy 1mW, resolution ratio
For 4cm-1, background times of collection is 32 times, and sample collection number is 32 times.
After the Raman spectrogram for obtaining single chmical compound explosive, using G03W quantum chemistry software kit theoretical calculation single chmical compound explosives such as Cl-
20, TNT, BFT etc. Raman spectrum, molecular configuration are constructed by GaussView 5.0, select RB3LYP/6-311G (d) method
Calculate, keyword is opt=(gdiis, tight) freq=raman.
4th, the Raman spectrogram collection of composite explosives.3-5mg composite explosives samples are weighed respectively adheres to Fourier Raman spectrum
On the objective table of instrument, keep sample surfaces smooth, directly carry out Raman test, obtain composite explosives such as CL-20 and TNT respectively and mix
The Raman spectrogram that the Raman collection of illustrative plates or CL-20 of conjunction mix with BFT.
5th, the Raman spectrogram collection of cocrystallized explosive.3-5mg cocrystallized explosive samples are weighed respectively, such as BTF and Cl-20 eutectic
Explosive or TNT and Cl-20 cocrystallized explosive etc., is adhered on the objective table of Fourier Raman spectrometer, keeps sample table
Face is smooth, directly carries out Raman test.
6th, according to single chmical compound explosive, the Raman spectrogram of composite explosives and cocrystallized explosive, with reference to simulation result of calculation, to Raman spectrum
Figure carries out peak position parsing and pointed out.
Compared with prior art, one of beneficial effects of the present invention are：The method of the present invention can realize explosive eutectic knot
The Rapid identification and sign of structure, using single chmical compound explosive, single chmical compound explosive be simply mixed two-by-two and single chmical compound explosive react two-by-two after shape
Into eutectic Raman spectrum it is inconsistent, produce different Raman peak position to change and to carry out explosive eutectic in quick analysis and mirror
It is fixed.This method is easy to operate, and principle is simple, and not by environmental restrictions, required instrument and equipment is also more general Raman spectrum
Instrument, it can be promoted the use of on a large scale in explosive production and research unit.In addition, this project can also further optimize,
Realization analyzes and identifies to unknown multi-component explosive eutectic.
Brief description of the drawings
Accompanying drawing 1 is explosive BTF configurations simulative optimization figure of the present invention；
Accompanying drawing 2 is explosive CL-20 configurations simulative optimization figure of the present invention；
Accompanying drawing 3 is the Raman spectrogram of three kinds of explosive pure samples；
Accompanying drawing 4 explosive BTF, CL-20 and the Raman spectrogram of eutectic that both are formed；
Explosive TNT, CL-20 the configuration simulative optimization figure of accompanying drawing 5
Accompanying drawing 6 explosive TNT, CL-20 and the Raman spectrogram of eutectic that both are formed.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Embodiment 1
The CL-20 pure samples of ε-crystal formation are taken first, and BTF pure samples carry out equal proportion mixing, and every part of total amount is 0.2g, is entered with mortar
Row ground and mixed, it is allowed to well mixed.And eutectic sample is prepared using the cocrystallized explosive preparation method for having reported document record.Point
Also known as take 3-5mg CL-20 pure samples, BTF pure samples to adhere on Fourier Raman spectrometer objective table, keep sample surfaces smooth, directly
The test of row Raman is tapped into, obtains explosive CL-20, BTF Raman 2000-200cm-1Spectrogram, and biased sample is drawn successively
Graceful sign, the Characteristic Raman peak for being respectively present two kinds of explosives is can see from the Raman collection of illustrative plates of biased sample, and peak position is not moved
Move and split a point phenomenon, by analysis, do not interact between the two.
Structure optimization is carried out to single chmical compound explosive CL-20 etc. according to density functional theory (DFT) and vibration mode is simulated, molecule
Configuration by GaussView 5.0 construct as shown in Figures 1 and 2, by the comparison of Fig. 3 and table 1 can be seen that theoretical calculation and
The Raman spectrum slightly difference of the CL-20 molecules measured is tested, but it is basically identical.Some peak positions are in actual measurement explosive in theoretical calculation
In do not occur, be because theoretical calculation have in itself certain error either due to the actual measurement normal Raman spectrum of explosive molecules
In corresponding spectral peak amplitude it is too small caused by.Binding isotherm calculates and experiment gained spectrogram, and we will divide Raman spectrum elucidation
The situation of sub- vibration mode and Raman peak position has carried out careful analysis, and is listed in table 1,2 respectively.Table 1 is explosive BTF Raman
Feature peak position parses, and the feature peak position that table 2 is explosive CL-20 parses.2900-3100cm-1The main coexpress in fundamental vibration area
For the stretching vibration at C-H peaks in single chmical compound explosive.In actual test, the stretching vibration only by C-H peaks is difficult to conclude single chmical compound explosive
In significant condition, so in specific eutectic characterizes identification, we do not account for careful analysis this scope, but emphasis
Investigate the Raman peaks situation of the characteristic groups such as nitro.
The explosive BTF of table 1 Raman peak position parsing
| Raman peak position/cm-1 | Vibration mode |
| 1572 | ν(C-N)[a] |
| 1658 | ν (C=C) ring |
| 1290 | δ(CH)ring[b]+ν(C-C) |
| 1089 | δ(CN)ring |
[a] ν, stretching vibration；[b] δ, flexural vibrations
From Fig. 1 combinations table 1, BTF Raman peaks are simpler, in 1000-1600 cm-1Qiang Feng areas, in 1572cm-1、1658 cm-1There is two strong and point characteristic peak at place respectively, belongs to the characteristic peak of C=C scissoring vibrations on C-N and phenyl ring,
In 1290 cm-1、1089 cm-1The stretching vibration and flexural vibrations at place, then c h bond, the C-N keys being respectively belonging on phenyl ring.
The explosive CL-20 of table 2 Raman peak position parsing
| Raman peak position/cm-1 | Vibration mode |
| 250-300 | Cage type stretching vibration |
| 810-870 | Ring-type stretching vibration, NO2The flexural vibrations of-scissors |
| 1000 | N-N stretching vibrations |
| 1200-1400 | NO2Symmetrical stretching vibration |
| 1550-1630 | NO2Asymmetric stretching vibration |
| 3010-3070 | C-H stretching vibration |
From Fig. 2 combinations table 2, in 1000-1200cm-1Qiang Feng areas, the CL-20 of ε-crystal formation is in 1125cm-1There is one
Strong and point characteristic peak, and in 810-870cm-1Scope in, ε-CL-20 are in 828cm-1And 841cm-1Place shows nitro respectively
The characteristic peak of scissoring vibration.
Then, the eutectic sample for weighing 3-5mg CL-20 and BTF respectively is adhered on objective table, keeps sample surfaces smooth,
Directly carry out Raman test.The method tested with Raman spectrum can be by the spectrogram of determinand and the single group open score for forming eutectic
Figure is contrasted, and carrys out the preliminary formation for judging eutectic with the thought of peak type matching.To BTF and CL-20 eutectics, as shown in figure 4, fried
The Raman peak intensity of medicine eutectic has declined relative to the Raman peak intensity of sterling single chmical compound explosive, shows in explosive eutectic system, pole
Rate has reduced, and cloud density is more evenly distributed, and relative to single chmical compound explosive, explosive eutectic system shows more stable.
Meanwhile pass through comparative analysis, it can be seen that the Raman signatures spectrogram of two eutectic samples has certain red shift, in 200-
1000cm-1In the range of, C-H cage type stretching vibration and the strong peak that is formed of ring-type stretching vibration are all sequestered in BTF in CL-20
In, do not occur significantly in the Raman spectrogram of cocrystallized explosive.And the nitro and 1000-1500cm more paid close attention at us-1
In the range of, BTF C-N peaks are there occurs red shift, while a small peak occurs in the left shoulder at the peak, is attributed to NO2It is not right
Claim stretching vibration.It in research before, may also indicate that by single crystal data, most hydrogen formd in eutectic system
Key, the cloud density of system can be lowered, so that the property such as the energy of eutectic system, sensitivity becomes more excellent.
Embodiment 2
Explosive TNT pure samples are taken first, and the CL-20 pure samples of ε-crystal formation carry out equal proportion mixing, and every part of total amount is 0.2g, is made
Two groups of samples, every part of sample are all ground mixing with mortar, are allowed to well mixed.3-5mg pure sample product are weighed respectively adheres to Fu
On vertical leaf Raman spectrometer objective table, keep sample surfaces smooth, directly carry out Raman test, obtain explosive CL-20, TNT
Raman 2000-200cm-1Spectrogram, and biased sample is subjected to Raman sign successively, biased sample, which can see, has been respectively present two
The Characteristic Raman peak of kind explosive, peak position is not mobile and splits a point phenomenon, by analysis, does not interact between the two.
Structure optimization is carried out to single chmical compound explosive TNT etc. according to density functional theory (DFT) and vibration mode is simulated, molecule structure
Type is constructed by GaussView 5.0 as shown in figure 5, can be seen that some peaks in theoretical calculation by the comparison of Fig. 5 and table 3
Position does not occur in explosive is surveyed, and is because theoretical calculation has certain error either due to the actual measurement of explosive molecules in itself
Caused by corresponding spectral peak amplitude is too small in normal Raman spectrum.Binding isotherm calculates and experiment gained spectrogram, and we are to Raman
Spectrum elucidation, the situation of molecular vibrational mode and Raman peak position is subjected to careful analysis, and is listed in table 2,3 respectively.Table 2 is
Explosive CL-20 Raman signatures peak position parsing, the feature peak position that table 3 is explosive TNT parse.2900-3100 cm-1Fundamental vibration
The main coexpress in area is the stretching vibration at C-H peaks in single chmical compound explosive.In actual test, only by C-H peaks stretching vibration very
Difficulty concludes the significant condition in single chmical compound explosive, thus specific eutectic characterize identification in, we do not account for careful analysis this
Individual scope, but the Raman peaks situation of the characteristic group such as high spot reviews nitro.
The explosive TNT of table 3 Raman peak position parsing
| Raman peak position/cm-1 | Vibration mode |
| 1365 | ν(NO2)[a] |
| 1616 | ν (C=C) ring |
| 1167 | δ(CH)ring[b]+ν(C-C) |
| 1206 | δ(CH)ring |
| 1527 | ν(NO2) |
[a] ν, stretching vibration；[b] δ, flexural vibrations
From Fig. 5 combinations table 3, TNT Raman peaks are simpler, in 1000-1600 cm-1Qiang Feng areas, in 1365 cm-1、1527 cm-1There is two strong and point characteristic peak at place respectively, the characteristic peak of nitro scissoring vibration is belonged to, in 1167 cm-1、
1206 cm-1、1616 cm-1The stretching vibration and flexural vibrations at place, then c h bond, the C=C keys being respectively belonging on phenyl ring.
Then, the eutectic sample for weighing 3-5mg TNT and CL-20 respectively is adhered on objective table, keeps sample surfaces smooth,
Directly carry out Raman test.The method tested with Raman spectrum can be by the spectrogram of determinand and the single group open score for forming eutectic
Figure is contrasted, and carrys out the preliminary formation for judging eutectic with the thought of peak type matching.As shown in fig. 6, to TNT and CL-20 eutectics, together
Sample, the Raman peak intensity of explosive eutectic has declined relative to the Raman peak intensity of sterling single chmical compound explosive, shows in explosive eutectic
In system, polarizability has reduced, and cloud density is more evenly distributed, and relative to single chmical compound explosive, explosive eutectic system shows more
For stabilization.Then, two kinds of such simple substance and their explosive eutectic are contrasted, likewise, in 200-1000cm-1In the range of, CL-
C-H cage type stretching vibration and the strong peak that is formed of ring-type stretching vibration are all sequestered in TNT in 20, in the Raman of cocrystallized explosive
Do not occur significantly in spectrogram.And the 1000-1500cm more paid close attention at us-1In the range of, TNT nitro peak and CL-
20 NO2Asymmetric stretching vibration coincides, and it is 1367cm to be changed into a stronger peak-1.In research before, pass through monocrystalline
Data be may also indicate that, most hydrogen bond is formd in eutectic system, can lower the cloud density of system, so that
The properties such as the energy of eutectic system, sensitivity become more excellent.
Above-described embodiment measures single chmical compound explosive CL-20, TNT, BTF Raman spectrum, the theoretical calculation vibration of molecule
Frequency, the Raman spectrogram that Binding experiment obtains, the vibration frequency of molecule is made and pointed out than more comprehensively ownership.What is observed shakes
Dynamic frequency is identical well with the calculating frequency after scale and specifically with being previously reported by unanimously, this shows close some vibration ownership
Degree Functional Approach is understanding that molecular vibration spectrum message context has good reliability.Then, using Raman spectroscopy, I
Raman detection has been carried out to two kinds of explosive eutectics of three kinds of single chmical compound explosives, parsed by Raman spectrum, it has been found that eutectic
Raman spectrogram contrast single chmical compound explosive have larger difference, be not the simple superposition of two kinds of single chmical compound explosives, and have Dependent Red Shift and
Peak position is disappeared, and explosive eutectic composition and Crack cause are studied, and the Raman spectrum of corresponding similar system can be become
Change from theoretical and experimental and provide beneficial information.By the fourier transform raman spectroscopy for analyzing explosive eutectic and single chmical compound explosive
Figure, appraisal basis can be provided to develop a kind of spectrographic technique of quick discriminating cocrystallized explosive.
Although reference be made herein to invention has been described for multiple explanatory embodiments of the invention, however, it is to be understood that
Those skilled in the art can be designed that a lot of other modifications and embodiment, and these modifications and embodiment will fall in this Shen
Please be within disclosed spirit and spirit.More specifically, can be to theme combination layout in the range of disclosure
Building block and/or layout carry out a variety of variations and modifications.Except the variations and modifications carried out to building block and/or layout
Outside, to those skilled in the art, other purposes also will be apparent.
Claims (1)
1. a kind of explosive eutectic structure authentication method, it is characterised in that comprise the following steps：
The CL-20 pure samples of ε-crystal formation are taken first, and BTF pure samples carry out equal proportion mixing, and every part of total amount is 0.2g, is ground with mortar
Mill mixing, is allowed to well mixed；3-5mg CL-20 pure samples are weighed respectively, BTF pure samples adhere to Fourier Raman spectrometer objective table
On, keep sample surfaces smooth, directly carry out Raman test, obtain explosive CL-20, BTF Raman 2000-200cm-1Spectrogram,
And biased sample is subjected to Raman sign successively, it can see from the Raman collection of illustrative plates of biased sample and be respectively present two kinds of explosives
Characteristic Raman peak, peak position is not mobile and splits a point phenomenon, by analysis, does not interact between the two；
Structure optimization is carried out to single chmical compound explosive CL-20 according to density functional theory and vibration mode is simulated, molecular configuration passes through
GaussView 5.0 is constructed, and to Raman spectrum elucidation, it is careful that the situation of molecular vibrational mode and Raman peak position has been carried out
Analysis, and table 1,2 is listed in respectively；The Raman signatures peak position that table 1 is explosive BTF parses, and table 2 is explosive CL-20 feature peak position
Parsing；2900-3100cm-1The main coexpress in fundamental vibration area is the stretching vibration at C-H peaks in single chmical compound explosive；In actual test
In, the stretching vibration only by C-H peaks is difficult to conclude the significant condition in single chmical compound explosive, is identified so being characterized in specific eutectic
In, high spot reviews includes the Raman peaks situation of the characteristic group of nitro；
The explosive BTF of table 1 Raman peak position parsing
[a] ν, stretching vibration；[b] δ, flexural vibrations
As shown in Table 1, BTF Raman peaks are simpler, in 1000-1600cm-1Qiang Feng areas, in 1572cm-1、1658cm-1Punishment
There is not two strong and point characteristic peak, the characteristic peak of C=C scissoring vibrations on C-N and phenyl ring is belonged to, in 1290cm-1、
1089cm-1The stretching vibration and flexural vibrations at place, then c h bond, the C-N keys being respectively belonging on phenyl ring；
The explosive CL-20 of table 2 Raman peak position parsing
As shown in Table 2, in 1000-1200cm-1Qiang Feng areas, the CL-20 of ε-crystal formation is in 1125cm-1There is one strong and point feature
Peak, and in 810-870cm-1Scope in, ε-CL-20 are in 828cm-1And 841cm-1Place shows the spy of nitro scissoring vibration respectively
Levy peak；
Then, the eutectic sample for weighing 3-5mg CL-20 and BTF respectively is adhered on objective table, keeps sample surfaces smooth, directly
Carry out Raman test；The method tested with Raman spectrum can enter the spectrogram of determinand with forming the one pack system spectrogram of eutectic
Row contrast, the preliminary formation for judging eutectic is come with the thought of peak type matching；To BTF and CL-20 eutectics, the Raman peaks of explosive eutectic
Decline relative to the Raman peak intensity of sterling single chmical compound explosive by force, shown in explosive eutectic system, polarizability has reduced, electricity
Evenly, relative to single chmical compound explosive, explosive eutectic system shows more stable sub- cloud Density Distribution；Meanwhile by score
Analysis, it can be seen that the Raman signatures spectrogram of two eutectic samples has certain red shift, in 200-1000cm-1In the range of, CL-
C-H cage type stretching vibration and the strong peak that is formed of ring-type stretching vibration are all sequestered in BTF in 20, in the Raman of cocrystallized explosive
Do not occur significantly in spectrogram；And in nitro and 1000-1500cm-1In the range of, BTF C-N peaks are there occurs red shift, simultaneously
There is a small peak in left shoulder at the peak, is attributed to NO2Asymmetric stretching vibration；It may also indicate that by single crystal data,
Most hydrogen bond is formd in eutectic system, the cloud density of system can be lowered.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510737960.0A CN105300957B (en) | 2015-11-02 | 2015-11-02 | A kind of explosive eutectic structure authentication method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510737960.0A CN105300957B (en) | 2015-11-02 | 2015-11-02 | A kind of explosive eutectic structure authentication method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105300957A CN105300957A (en) | 2016-02-03 |
| CN105300957B true CN105300957B (en) | 2018-03-27 |
Family
ID=55198466
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510737960.0A Active CN105300957B (en) | 2015-11-02 | 2015-11-02 | A kind of explosive eutectic structure authentication method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105300957B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106076646A (en) * | 2016-06-20 | 2016-11-09 | 曹飞 | A kind of screening technique of new copper sulfur collecting agent |
| 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 |
| CN114199852B (en) * | 2021-12-07 | 2024-03-01 | 天津大学 | Characterization method of pharmaceutical eutectic performance |
| CN116874340B (en) * | 2023-07-10 | 2024-04-05 | 湖北航天化学技术研究所 | Phenyl explosive energetic eutectic compound and preparation method thereof |
-
2015
- 2015-11-02 CN CN201510737960.0A patent/CN105300957B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| HMX/TATB 共晶炸药的制备和表征;沈金朋;《CNKI中国优秀硕士学位论文全文数据库》;20120515;第42-43页 * |
| LC-20拉曼光谱的密度泛函理论计算及晶型定量分析研究;王慧等;《2013 年第二届全国危险物质与安全应急技术研讨会论文集》;20131114;第219-224页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105300957A (en) | 2016-02-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105300957B (en) | A kind of explosive eutectic structure authentication method | |
| Khanna et al. | Infrared spectrum, force constants, and thermodynamic functions of SiF2 | |
| Berrod et al. | Inelastic and quasi-elastic neutron scattering. Application to soft-matter | |
| Bodo et al. | Interaction of a long alkyl chain protic ionic liquid and water | |
| Rodriguez et al. | Hyper‐Raman and Raman scattering in paratellurite TeO2 | |
| Citroni et al. | Crystal structure of nitromethane up to the reaction threshold pressure | |
| Sharma et al. | Hydrogen bonds and polymerization in acrylamide under pressure | |
| Emmons et al. | High‐pressure infrared absorption spectroscopy of poly (methyl methacrylate) | |
| Ruta et al. | Nonergodicity factor, fragility, and elastic properties of polymeric glassy sulfur | |
| Tan et al. | Discovery of high-pressure polymorphs for a typical polymorphic system: oxalyl dihydrazide | |
| Fernando et al. | Visible/infrared dissociation of NO3: Roaming in the dark or roaming on the ground? | |
| Salzmann et al. | The Raman spectrum of ice XII and its relation to that of a new “high-pressure phase of H2O ice” | |
| Zhang et al. | Imaging the Pair-Correlated HNCO Photodissociation: The NH (a 1Δ)+ CO (X1Σ+) Channel | |
| Chang et al. | Striking isotopologue-dependent photodissociation dynamics of water molecules: The signature of an accidental resonance | |
| Busson | Doubly resonant SFG and DFG spectroscopies: An analytic model for data analysis including distorted and rotated vibronic levels. II. Applications | |
| Allis et al. | The solid-state terahertz spectrum of MDMA (Ecstasy)–a unique test for molecular modeling assignments | |
| Yu et al. | New spectral assignment of n‐propanol in the C―H stretching region | |
| Kuś et al. | Spectroscopic characterization and crystal structures of four hydrochloride cathinones: N-ethyl-2-amino-1-phenylhexan-1-one (hexen, NEH), N-methyl-2-amino-1-(4-methylphenyl)-3-methoxypropan-1-one (mexedrone), N-ethyl-2-amino-1-(3, 4-methylenedioxyphenyl) pentan-1-one (ephylone) and N-butyl-2-amino-1-(4-chlorophenyl) propan-1-one (4-chlorobutylcathinone) | |
| Qin et al. | Supramolecular Gel‐to‐Gel Transition Induced by Nanoscale Structural Perturbation via the Rotary Motion of Feringa's Motor | |
| Cavagnat et al. | Raman Microspectrometry as a New Approach to the Investigation of Molecular Recognition in Solids: Chloroform− Cryptophane Complexes | |
| Ishiwata et al. | Analyses of the Infrared Absorption Bands of 15NO3 in the 1850− 3150 cm− 1 Region | |
| Aguiar et al. | Medium-range order in cesium borate glasses probed by double-resonance NMR | |
| Wen et al. | Joint Experimental− Theoretical Investigation of the Lower Bound States of the NO (X2Π)-Kr Complex | |
| Yu et al. | Nuclear hyperfine interaction of rotating hydrogen: A spectroscopic investigation of hydrogen-OCS van der Waals complexes | |
| Wright et al. | High-resolution infrared and electron-diffraction studies of trimethylenecyclopropane ([3]-radialene) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |