CN102954951B - Explosive crystal quality characterization method - Google Patents
Explosive crystal quality characterization method Download PDFInfo
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Abstract
The invention discloses an explosive crystal quality characterization method. The explosive crystal quality characterization method comprises the following steps of: filling an explosive crystal sample in a color comparison dish, adding a refraction matching fluid, utilizing a spectrophotometer to test transmissibility, and utilizing the difference of the transmissibility to perform explosive crystal quality characterization. The method provided by the invention can realize the rapid analysis and characterization of the quality of an explosive crystal, due to difference of the internal defect of the explosive crystal and the crystal self refractive index, the permeation of visible light with a certain wavelength is inconsistent between the crystal itself and a defect region, and the quantitative statistics analysis of the defect of the explosive crystal is realized. The method provided by the invention has the advantages that the operation is simple and the principle is simple, and is free from environmental limit; the required instrument equipment is an universal light microscope and spectrophotometer, and the method can be popularized and used in a large-scale manner by explosive production and researching units; and in addition, the method can be further optimized so as to realize the quantification of volume ratio of the defect explosive crystal in the total explosive crystal.
Description
Technical field
The invention belongs to explosive crystal quality characterizing method, exactly, is that a kind of refractive power coupling spectrophotometric method that adopts is carried out the method for quantitative test to the explosive crystal quality.
Background technology
Total institute is known, the quality of explosive crystal quality has determined detonation property, burning performance and the acting ability of explosive, as a rule, the explosive crystal quality is mainly carried out synthetic determination by crystal defect, granularity size, apparent pattern and particle density etc., wherein crystal defect is the key factor of judging the explosive crystal quality, is also the main parameters of evaluating at present the explosive crystal quality, generally speaking, the explosive crystal quality is higher, and the crystal defect of microcosmic is just fewer.At present, the explosive crystal that larger improvement is arranged in order to obtain combination property, the research of high-quality explosive becomes a focus of present fiery explosive research field, increasing explosive researcher wishes and can reduce the defective of explosive crystal inside by crystallization technique and efficient post-processing technology, obtain more perfect high-quality explosive crystal, thereby obtain detonation property and energy explosive material preferably.
Height how to judge what and quality of explosive crystal inherent vice is the key point that realizes high-qualityization of explosive crystal.Although also there is no unified standard for the explosive crystal Quality Identification, yet do not form system, some employing density measuring methods, think that density is higher, the defective of crystals is contained just relative less as air and solvent, although this method is considered to relatively feasible at Explosive Industry, but it is consuming time longer to measure explosive crystal density, and needs special-purpose density gradient instrument, and density measure is subjected to the impact of other factors larger in addition.Can carry out the instrument and equipment of accurate analysis to explosive crystal microstructure state and defect distribution at present in addition also few, and have relatively high expectations, operating process and disposal route are also comparatively complicated, can not satisfy general explosive production producer and carry out the accurate control of production journey.For this reason, seek a kind of fast and convenient and efficient explosive crystal quality discrimination method and seem particularly urgent.
Summary of the invention
The objective of the invention is to be to provide a kind of analysis simple and efficient, the explosive crystal quality that is applicable to apply is on a large scale differentiated and analytical approach.For process control and the control with raw material of explosive crystal production provides a kind of means of differentiating fast.
For achieving the above object, the present invention is by adopting refractive power coupling spectrophotometer analytical approach, utilize explosive crystal inherent vice part material and crystal itself and refractive power matching fluid index of refraction inconsistent, produce different light penetrations the explosive crystal quality is carried out express-analysis and evaluation.The inventive method belongs to a kind of quantitative crystal defect and Quality Analysis Methods, can be used for screening and the control of explosive crystal (starting material).The equipment that this method adopts and instrument is easy is easy to get is used on a large scale and promotes the use of.
A kind of explosive crystal quality characterizing method of the present invention is that the explosive crystal sample is packed in cuvette, then adds the refractive power matching fluid, utilizes spectrophotometer test transmitance, utilizes the difference of transmitance to carry out explosive crystal quality sign.
Wherein: the index of refraction coefficient of described refractive power matching fluid is approximate identical with the index of refraction coefficient of explosive crystal sample.Generally prepare and screen according to the geometric mean index of refraction (abbreviation index of refraction) of testing sample.For example, index of refraction for explosive hexogen (RDX) sample is about 1.58 to 1.60, generally select the potpourri of toluene and oil of bay to prepare, the index of refraction of oil of bay is about 1.602 to 1.614, the index of refraction of toluene is about 1.496 to 1.528, thereby the index of refraction of potpourri that makes toluene and oil of bay is between 1.58 to 1.60.
Wherein: the screening of described refractive power matching fluid in the following way: adopt ordinary optical microscope, evenly be positioned over a small amount of explosive crystal on microslide, and drip the refractive power matching fluid in the above, covered, examine under a microscope, judge according to the color consistency of the crystal in imaging and refractive power matching fluid, choose the refractive power matching fluid that the best refractive power matching fluid of consistance is used as final analysis.
Wherein: the optical path of described cuvette is the standard colorimetric ware of 2mm to 10mm.
Wherein: the granularity size of described explosive crystal sample is less than 250um, and is not dissolved in the refractive power matching fluid.
Wherein: the described refractive power matching fluid that adds is the refractive power matching fluid is slowly splashed into and soak full cuvette, and vibrating compacting gently, at 20 ℃ of standing 2h to 10h of constant temperature.
Step can be as follows more specifically for explosive crystal quality characterizing method of the present invention:
The preparation of 1, refractive power matching fluid.Prepare according to the index of refraction of explosive crystal sample to be measured, make the refractive power matching fluid index of refraction after preparation approximate identical with the index of refraction of testing sample, wherein index of refraction carries out test analysis with Abbe refractometer.
The screening of 2, refractive power matching fluid.Adopt ordinary optical microscope, evenly be positioned over a small amount of explosive crystal on microslide, and drip the refractive power matching fluid in the above, careful covered, examine under a microscope again, judge according to the color consistency of the crystal in imaging and matching fluid, and choose consistance and mate preferably as analyzing and use the refractive power matching fluid.
3, the wavelength of spectrophotometer is selected.Generally speaking, according to the state of testing sample, select wavelength to be that the visible light of 550nm to 600nm carries out the transmittance analytical effect better, but can not negate the analysis result that uses other wavelength.
4, the preparation of blank reference sample.The refractive power matching fluid that step 1 is prepared slowly splashes in the certain blank cuvette of optical path, splashing into should note in process not catching touches the smooth transparent surface of cuvette, and the assurance matching fluid is not overflowed, the cuvette that then will load the refractive power matching fluid carries out spectrophotometric determination, and with it as reference, its transmittance can be made as 100%.
5, accurately taking a certain amount of explosive crystal sample to be measured is filled in the certain blank cuvette of optical path, the optical path size is determined according to the granularity size of explosive crystal sample to be measured, be generally less than the cuvette that the 100um optical path is 2mm, 100um to 250um is the cuvette of 5mm with optical path.The laser particle analyzer analytical approach is adopted in the test of explosive crystal granularity size.
6, the refractive power matching fluid that step 1 is configured slowly splashes into and soaks and expire in the cuvette that is filled by step 5, and vibrating compacting gently.
7, step 6 is soaked the cuvette of full refractive power matching fluid at 20 ℃ of standing 2h to 10h of constant temperature.
8, the cuvette after step 7 processing is carried out the transmittance test of spectrophotometer, calculate corresponding transmittance according to the calculation procedure that instrument is set, and make a record, this transmittance can reflect the quality of explosive crystal quality.
9, sample aftertreatment.Explosive crystal sample after step 8 test is completed recycles.
The present invention has advantages of as follows:
Method of the present invention can realize express-analysis and the sign of explosive crystal quality, difference by explosive crystal inherent vice and crystal (refractive power matching fluid) index of refraction itself, thereby cause between crystal itself and defect area seeing through of the visible light of certain wavelength inconsistent, to realize the quantitative statistical analysis (with the transmittance reflection) to the explosive crystal defective.This method is easy and simple to handle, and principle is simple, is not subjected to environmental restraint, and the instrument and equipment that requires is also comparatively general optical microscope and spectrophotometer, can promote the use of on a large scale in explosive production and research unit.In addition, this project can also further be optimized, and realizes the quantification to the shared explosive crystal cumulative volume of explosive crystal defective ratio.
Description of drawings
The refractive power of RDX-1 coupling microscope figure in Fig. 1 embodiment 1;
The refractive power of RDX-2 coupling microscope figure in Fig. 2 embodiment 1;
The refractive power of HMX-5 coupling microscope figure in Fig. 3 embodiment 2;
The refractive power of HMX-3 coupling microscope figure in Fig. 4 embodiment 2;
Embodiment
The present invention will be further described by reference to the accompanying drawings below by embodiment.Following embodiment only is used for the present invention is described in detail, but not limitation of the present invention.
Embodiment 1
(1) for hexogen to be measured (RDX) crystal, By consulting literatures and data, its geometric mean index of refraction is about 1.58 to 1.60.
(2) choose the preparation that oil of bay and toluene carry out the refractive power matching fluid.By consulting literatures or the index of refraction that records both with Abbe refractometer are respectively: 1.608 and 1.512, and according to percent by volume 9:1,8:2,7:3,6:4,5:5,4:6,3:7,2:8,1:9.Can also be with the further refinement of ratio if need.
(3) adopt refractive power coupling microscopic analysis method that the refractive power matching fluid is screened.Sticking the taking a morsel of RDX crystal grain (granularity is 75um to 125um) trembled gently on microslide, splash into the refractive power matching fluid that step (2) is prepared on crystal, according to the color consistency of crystalline region and liquid regions, choose the refractive power matching fluid.This example selects oil of bay and volume of toluene than being the refractive power matching fluid of 8:2, and recording its index of refraction with Abbe refractometer is 1.5844.
(4) the refractive power matching fluid of step (3) being determined slowly evenly splashes in the cuvette that optical path is 2mm, as blank reference.
(5) open spectrophotometer, after instrument state is stable, regulate seeing through light wavelength, this routine adjusting wavelength is 550nm.
(6) blank sample of step (4) is done the transmittance analysis on the spectrophotometer that step (5) is established, and to set its transmitance be 100%.
(7) take also vibrating compacting gently in the RDX crystal filling of 100mg as cuvette that optical path is 2mm.
(8) splash into the refractive power matching fluid that step (3) determines in step (7) fills the cuvette of RDX, immerse to whole RDX crystal, and stablize 2h in 20 ℃ of constant temperature.
(9) cuvette of step (8) is put on the spectrophotometer that step (5) establishes and done the transmittance analysis, the foundation that the transmittance record is differentiated as quality.
(10) repeating step (7) is made another sample to step (9).Test result sees Table 1.
The transmittance result of table 1 different crystal quality RDX
By above transmittance analysis result, can find out that the transmittance of RDX-2 sample is the highest, be namely that its crystal quality is the highest, and the reappearance of test result is better; The crystal quality of RDX-1 is the poorest, and this mates with refractive power, and on microscope, observable result is consistent.Compare with refractive power coupling microscopic analysis method, the result that this method obtains has statistical significance, and has realized the quantitative test of crystal defect.
Attached Fig. 1 and 2 has also shown the difference of RDX-1 and RDX-2 intuitively, can find out from accompanying drawing 1,2, and RDX-1 obviously has a lot of defectives and flaw, affects transmittance, and the quality of RDX-2 wants better.
Embodiment 2
(1) for HMX (HMX) crystal, consult pertinent literature and data, its geometric mean index of refraction is 1.595.
(2) according to embodiment 1 step (2) preparation refractive power matching fluid.
(3) be suitable for the refractive power matching fluid of HMX crystal (granularity is about 70um to 100um) according to embodiment 1 step (2) screening.This example selects oil of bay and volume of toluene than being the refractive power matching fluid of 9:1, and recording its index of refraction with Abbe refractometer is 1.5949.
(4) the refractive power matching fluid of step (3) being determined slowly evenly splashes in the cuvette that optical path is 2mm, as blank reference.
(5) regulate spectrophotometer according to step (5) in embodiment 1.
(6) do the analysis of blank sample transmittance according to step (6) in embodiment 1.
(7) the HMX crystal that takes 100mg is packed in the cuvette that optical path is 2mm and vibrating compacting gently.
(8) splash into the refractive power matching fluid that step (3) determines in step (7) fills the cuvette of HMX, until all the HMX crystal immerses the refractive power matching fluid, and stablize 2h in 20 ℃ of constant temperature.
(9) cuvette of step (8) is put on the spectrophotometer that step (5) sets and done the transmittance analysis, the foundation that the transmittance record is differentiated as the HMX quality.
(10) repeating step (7) to step (9) is made another sample.Test result sees Table 2.
The transmittance result of table 2 different crystal quality HMX
By above transmittance analysis result, can find out that the transmittance of HMX-3 sample is the highest, be namely that its crystal quality is the highest, and the test result reappearance is better.Method according to the above analysis, the crystal quality of above-mentioned 5 kinds of samples is sequentially: HMX-3＞HMX-1＞HMX-4＞HMX-2＞HMX-5.
Accompanying drawing 3 and 4 has also been explained the difference of HMX-3 and HMX-5 intuitively.
Claims (1)
1. an explosive crystal quality characterizing method, is characterized in that comprising the steps:
The preparation of step 1, refractive power matching fluid: prepare according to the index of refraction of explosive crystal sample to be measured, make the refractive power matching fluid index of refraction after preparation approximate identical with the index of refraction of testing sample, wherein index of refraction carries out test analysis with Abbe refractometer;
The screening of step 2, refractive power matching fluid: adopt ordinary optical microscope, evenly be positioned over a small amount of explosive crystal on microslide, and drip the refractive power matching fluid in the above, careful covered, examine under a microscope again, judge according to the color consistency of the crystal in imaging and matching fluid, and choose consistance and mate preferably as analyzing and use the refractive power matching fluid;
The wavelength of step 3, spectrophotometer is selected: the selection wavelength is that the visible light of 550nm to 600nm carries out the transmittance analysis;
The preparation of step 4, blank reference sample: the refractive power matching fluid that step 1 is prepared slowly splashes in the certain blank cuvette of optical path, splashing into does not catch in process touches the smooth transparent surface of cuvette, and the assurance matching fluid is not overflowed, the cuvette that then will load the refractive power matching fluid carries out spectrophotometric determination, and with it as reference, its transmittance is made as 100%;
Step 5, accurately take a certain amount of explosive crystal sample to be measured and be filled in the certain blank cuvette of optical path, the optical path size is determined according to the granularity size of explosive crystal sample to be measured, be the cuvette of 2mm less than the 100um optical path, 100um to 250um is the cuvette of 5mm with optical path; The laser particle analyzer analytical approach is adopted in the test of explosive crystal granularity size;
Step 6, the refractive power matching fluid that step 1 is configured slowly splash into and soak and expire in the cuvette that is filled by step 5, and vibrating compacting gently;
Step 7, step 6 is soaked the cuvette of full refractive power matching fluid at 20 ℃ of standing 2h to 10h of constant temperature;
Step 8, the cuvette after step 7 is processed carry out the transmittance test of spectrophotometer, calculate corresponding transmittance according to the calculation procedure that instrument is set, and make a record, and this transmittance can reflect the quality of explosive crystal quality;
Step 9, sample aftertreatment: the explosive crystal sample after step 8 test is completed recycles.
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| CN110487815B (en) * | 2019-09-16 | 2021-10-29 | 中国工程物理研究院化工材料研究所 | Explosive crystal internal defect quantitative characterization method based on laser scattering technology |
| CN113008853B (en) * | 2021-02-25 | 2023-01-24 | 中国工程物理研究院化工材料研究所 | Method for in-situ marking and visual tracing of explosive based on fluorescent energetic molecules |
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| JP2006003243A (en) * | 2004-06-18 | 2006-01-05 | Nuclear Fuel Ind Ltd | Crystal particle discriminating method of oxide nuclear fuel |
| CN101403604A (en) * | 2008-10-22 | 2009-04-08 | 中国科学院上海技术物理研究所 | Extension thin film surface protection test technology |
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| JP2006003243A (en) * | 2004-06-18 | 2006-01-05 | Nuclear Fuel Ind Ltd | Crystal particle discriminating method of oxide nuclear fuel |
| CN101403604A (en) * | 2008-10-22 | 2009-04-08 | 中国科学院上海技术物理研究所 | Extension thin film surface protection test technology |
| JP2012052997A (en) * | 2010-09-03 | 2012-03-15 | Sigma Koki Kk | Optical measurement method and optical measurement device for measuring apparent refraction factor of rough surface of solid body |
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