CN102721585A - Method for treating sample for particle size test of hexanitrostilbene - Google Patents
Method for treating sample for particle size test of hexanitrostilbene Download PDFInfo
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- CN102721585A CN102721585A CN2012102111917A CN201210211191A CN102721585A CN 102721585 A CN102721585 A CN 102721585A CN 2012102111917 A CN2012102111917 A CN 2012102111917A CN 201210211191 A CN201210211191 A CN 201210211191A CN 102721585 A CN102721585 A CN 102721585A
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Abstract
The invention discloses a method for treating a sample for a particle size test of hexanitrostilbene. The method comprises the steps of placing 0.05-0.1g of hexanitrostilbene particles to be tested in a 50 mL of beaker, adding 20-25 mL of deionized water, and adding 0.1-0.3 mL of Twain-80 with the concentration of 1%-2% (by weight) at the temperature of 15-25 DEG C into an ultrasonoscope to be subjected to ultrasonic oscillation for 8-12 seconds. The method is mainly used for treatment of the sample for the particle size test of the hexanitrostilbene.
Description
Technical field
The present invention relates to the sample processing method that the testing graininess of a kind of hexanitro Stilbene (HNS) is used.
Background technology
In the testing graininess the whole bag of tricks, what usually adopt at present is the laser particle size method.In order to obtain comparatively accurately test result, the laser particle size method of testing need carry out pre-treatment to sample before testing graininess.The normal at present process for dispersing that adopts is supersonic oscillations, tested sample is fully disperseed in medium, and then carry out the test of granularity.
Usually during explosive sample laser particle size method testing graininess sample processing method to adopt step be that tested explosive sample is put into the medium of being made up of deionized water and low quantity of surfactant, and carry out ultrasonicly, after reaching abundant dispersion, carry out testing graininess again.For example, be that RDX is put into the medium of being made up of deionized water and OPEO (OP10) during the RDX testing graininess, and carry out ultrasonic dispersion, reach abundant dispersion after, carry out the test of granularity again.Above-mentionedly be used for the dispersion medium that the explosive sample processing method uses and do not play the fine dispersion effect for hexanitro Stilbene (HNS).It is because of being that hexanitro Stilbene (HNS) particle is an acicular crystal; There is very high surface energy between the hexanitro Stilbene particle; Cause the reunion between the particle, hexanitro Stilbene particle can not certainly will be carried out for a long time to the hyperoscillating of hexanitro Stilbene particle in order to reach the fine dispersion purpose by effective dispersion under the sonic oscillation of short time is handled; But hexanitro Stilbene particle can be smashed by ultrasound wave in long sonic oscillation process, and the particle diameter result was inaccurate when this all can make testing graininess.
Summary of the invention
The technical matters that the present invention will solve is deficiency and the defective that overcomes prior art; The sample processing method that provides a kind of hexanitro Stilbene testing graininess to use; This method not only avoids long sonic oscillation to cause the grain breakage of hexanitro Stilbene; Hexanitro Stilbene particle is fully disperseed, and can obtain the testing graininess result of hexanitro Stilbene particle comparatively accurately.
Design of the present invention: select suitable surfactant, can play the capillary effect that reduces liquid, can make hexanitro Stilbene particle and water better wetting, reach hexanitro Stilbene particle and in aqueous medium, effectively disperseed through surfactant.
In order to solve the problems of the technologies described above; Technical scheme of the present invention is: the hexanitro Stilbene particle that 0.05-0.1g is to be tested places the 50mL beaker; Add the 20-25mL deionized water; Under 15-25 ℃ temperature, add the Tween-80 of 0.1-0.3mL 1%-2% (weight) again, place ultrasonoscope sonic oscillation 8-12s.
Optimal technical scheme of the present invention is: the hexanitro Stilbene particle that 0.1g is to be tested places the 50mL beaker, adds the 25mL deionized water, under 20 ℃ temperature, adds the Tween-80 of 0.1mL 1% (weight) again, sonic oscillation 10s in ultrasonoscope.
Advantage of the present invention: sample processing method of the present invention can make hexanitro Stilbene particle obtain fine dispersion; It is that 8s just reaches good dispersion in the sonic oscillation time, and carries out ultrasonic dispersion in the medium that available technology adopting deionized water and OP10 form, and hexanitro Stilbene particle is at sonic oscillation 10s; Still can not effectively disperse; Can influence the testing graininess result, and long ultrasonicly cause the grain breakage of hexanitro Stilbene, make that the testing graininess result of hexanitro Stilbene particle is inaccurate.
Embodiment
Through specific embodiment the present invention is done further explain below.
Testing graininess instrument: Mastersizer 2000 laser particle analyzers
Contact angle testing tool: DCAT 21 type dynamic contact angle measuring instruments
The surfactant selection method
After surfactant joins in the deionized water; Deionized water changes to the contact angle of HNS; The amplitude that the different surface active agents contact angle changes is obviously different; Based on this, can select the optimum surfactant of maximum surfactant of contact angle reduction as hexanitro Stilbene particle dispersion.
Surfactant preferably specifically may further comprise the steps:
Step 1, the WS of preparation different surface active agents
Choose each 0.5g of peregal, neopelex, OPEO, Tween-80 and polyglycol; Use the 10mL deionized water dissolving, the 3min that in ultrasound wave, vibrates is behind the placement 24h; Again in ultrasonoscope while shaking the vibration 3min; After treating that surfactant dissolves fully, be diluted to 50mL respectively, be configured to concentration and be 1% the WS.
Step 2, the test of contact angle
The test of contact angle: take by weighing totally 7 parts on the HNS sample of 0.6g, be placed on the dynamic contact angle powdered sample respectively and test in the special-purpose test tube, rap while add on the table, make powder ram-jolt, the height of powder in test tube is fixed as 15cm.
Earlier test a copy of it sample quality curve over time in normal hexane supposes that the contact angle of HNS powder in normal hexane is 0, obtains powder capillary rising constant C; Test the contact angle of HNS powder in the deionized water that does not add surfactant neutralizes the water that has added the different surfaces activating agent more respectively.
Step 3, the confirming of surfactant
According to the size of the contact angle that obtains, selection adding different surfaces activating agent WS contact angle minimum, the surfactant in the hexanitro Stilbene granularity test dispersion process promptly obtained.
The contact angle of table 1HNS sample in the water that has added the different surfaces activating agent
| The surfactant title | HNS sample contact angle |
| Deionized water | 89.99° |
| Deionized water+polyglycol | 89.94° |
| Deionized water+neopelex | 89.05° |
| Deionized water+OP10 | 88.86° |
| Deionized water+peregal | 87.78° |
| Deionized water+Tween-80 | 37.21° |
According to the data in the table 1, select the surfactant of Tween-80 as hexanitro Stilbene testing graininess of granule sample processing method used medium.
Embodiment 1:HNS sample grain graininess
Take by weighing HNS powder 0.1g, place the 50mL beaker, add the 25mL deionized water, under 20 ℃ temperature, add the Tween-80 that 0.1mL concentration is 1% (weight) again, place ultrasonoscope sonic oscillation 10s.
Scattered sample is measured on Mastersizer 2000 laser particle analyzers.Obtain the result and list in table 2:
The particle diameter of table 2HNS sample
| Dispersion medium | HNS volume of sample meta particle diameter D (50)/μ m |
| Deionized water+Tween-80 | 17.76 |
| Deionized water+Tween-80 | 17.50 |
Embodiment 2:HNS sample grain graininess
Take by weighing HNS powder 0.05g, place the 50mL beaker, add the 25mL deionized water, under 20 ℃ temperature, add the Tween-80 that 0.3mL concentration is 1% (weight) again, place ultrasonoscope sonic oscillation 12s.
Scattered sample is measured on Mastersizer 2000 laser particle analyzers.Obtain the result and list in table 3:
The particle diameter of table 3HNS sample
| Dispersion medium | HNS volume of sample meta particle diameter D (50)/μ m |
| Deionized water+Tween-80 | 17.57 |
| Deionized water+Tween-80 | 17.45 |
The influence of ultrasonic time in the pre-treatment of embodiment 3:HNS sample particle testing graininess
Take by weighing 5 parts of HNS powder 0.1g, place beaker, add the 25mL deionized water, all add the Tween-80 of 0.1mL 1% (weight) in every part of sample, place the ultrasonoscope different time of vibrating.
Scattered sample is measured on Mastersizer 2000 laser particle analyzers.Obtain the result and list in table 4:
The particle diameter of HNS sample under the different ultrasonic times of table 4
| Ultrasonic time | HNS volume meta particle diameter D (50)/μ m |
| 5s | 21.03 |
| 8s | 17.72 |
| 10s | 17.76 |
| 12s | 17.40 |
| 15s | 16.81 |
| 60s | 13.27 |
HNS volume of sample meso-position radius result can find out that the sonic oscillation time, grain graininess was more stable in the 8-12s scope in the table 4; Explain that HNS sample particle dispersion is better; The sonic oscillation time, particle was not scatter fully, behind 12s less than the 8s time; The particle diameter result is obviously less than normal, and this is because particle broken causing in the process of sonic oscillation.
Comparative Examples 1: the particle diameter of HNS sample when being dispersion medium with water merely
Take by weighing HNS powder 0.1g, place beaker, add the 25mL deionized water, under 20 ℃ temperature, place the ultrasonoscope 10s that vibrates, scattered sample is measured on Mastersizer 2000 laser particle analyzers.Obtain the result and list in table 5:
The particle diameter of HNS sample under table 5 different dispersion
| Dispersion medium | HNS volume of sample meta particle diameter D (50)/μ m |
| Deionized water | 30.01 |
| Deionized water | 29.92 |
HNS volume of sample meso-position radius result can find out in contrast table 2 and the table 5, and under identical ultrasonic time, the particle diameter of the sample that the adding Tween-80 disperses is much smaller than the sample that directly disperses with deionized water; Under ESEM, observe, there is tangible particle agglomeration phenomenon in the sample that directly disperses with deionized water, and it is good to have added the sample dispersion effect that Tween-80 disperses, and does not almost see agglomerated particle.
Comparative Examples 2: the particle diameter of HNS sample when adding OP10 as dispersion medium with water
Take by weighing HNS powder 0.1g, place beaker, add the 25mL deionized water; Under 20 ℃ temperature; Add the OP10 that 0.3mL concentration is 1% (weight) again, place the ultrasonoscope 10s that vibrates, scattered sample is measured on Mastersizer 2000 laser particle analyzers.Obtain the result and list in table 6:
The particle diameter of HNS sample under table 6 different dispersion
| Dispersion medium | HNS volume of sample meta particle diameter D (50)/μ m |
| Deionized water+OP10 | 21.12 |
| Deionized water+OP10 | 20.83 |
HNS volume of sample meta particle diameter result can find out in contrast table 2 and the table 6, under identical ultrasonic time, with deionized water add OP10 as the volume meta particle diameter result of dispersion medium test greater than add the particle diameter result of Tween-80 with water as medium.This explanation water adds OP10 and effectively the HNS sample is not scatter as dispersion medium.Under ESEM, observe, add the sample in the OP10 dispersion medium at deionized water, the 10s that vibrates in the ultrasonoscope,, still have tangible particle agglomeration phenomenon.
Claims (2)
1. the sample processing method used of the testing graininess of a hexanitro Stilbene; Comprise that step is following: the hexanitro Stilbene particle that 0.05-0.1g is to be tested places the 50mL beaker; Add the 20-25mL deionized water; Under 15-25 ℃ temperature, adding 0.1-0.3mL concentration is the Tween-80 of 1%-2% (weight), places ultrasonoscope sonic oscillation 8-12s.
2. the testing graininess of hexanitro Stilbene according to claim 1 is used sample processing method; Comprise that step is following: the hexanitro Stilbene particle that 0.1g is to be tested places the 50mL beaker; Add the 25mL deionized water; Under 20 ℃ temperature, add the Tween-80 that 0.1mL concentration is 1% (weight) again, place ultrasonoscope sonic oscillation 10s.
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| CN103342649A (en) * | 2013-07-26 | 2013-10-09 | 南京理工大学 | 3-amino-2, 4, 6-trinitro-distyrene compounds and preparation method thereof |
| CN111982763A (en) * | 2020-08-17 | 2020-11-24 | 上海普康药业有限公司 | Method for determining particle size and particle size distribution of coenzyme Q10 |
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| CN103342649A (en) * | 2013-07-26 | 2013-10-09 | 南京理工大学 | 3-amino-2, 4, 6-trinitro-distyrene compounds and preparation method thereof |
| CN103342649B (en) * | 2013-07-26 | 2015-08-26 | 南京理工大学 | 3-amino-2,4,6-trinitro-diphenylethylene compounds and preparation method thereof |
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