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freedompyro
holmes1880
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HMTD Decomposition Rate and Recrystallization
I have been searching around and I cannot find this information anywhere. Since it was once considered for commercial use it must be at least somewhat
storage stable when refrigerated.
Has anyone tested the decomposition rates of Citric Acid synthesized HMTD? What solvents are suitable for recrystallization of HMTD?
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Pulverulescent
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| Quote: | | Has anyone tested the decomposition rates of Citric Acid synthesized HMTD? What solvents are suitable for recrystallization of HMTD?
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I've never heard of HMTD being recrystallised . . . it certainly isn't soluble in any of the ordinary solvents!
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Adas
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Quote: Originally posted by Pulverulescent  | | Quote: | | Has anyone tested the decomposition rates of Citric Acid synthesized HMTD? What solvents are suitable for recrystallization of HMTD?
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I've never heard of HMTD being recrystallised . . . it certainly isn't soluble in any of the ordinary solvents!
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My friend used to recrystallize HMTD. I think it was ethanol or methanol.
Rest In Pieces!
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Pulverulescent
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He's winding you up!
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freedompyro
holmes1880
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LoL... Hilarious... I know Adas from elsewhere.
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Adas
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You mean HE forum? 
Rest In Pieces!
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niertap
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I don't think you can really recrystallize it, but as long as you started with fairly pure compounds it should be fine. It essentially recrystallizes
from the reaction, so further recrystallization probably would be futile.
As for decomposition: light, heat, and transition metals would speed it up. Peroxides decompose by homolysis of the o-o bond, creating two radicals.
These then go attack everything else. Adding an antioxidant like vitamin C or citric acid would probably increase shelf life significantly. The free
radicals make a chain reaction so the earlier you stop it, the more effective it would be.
Ignorance is bliss
Outliers in life are modeled by chemical kinetics
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NitricSynth
holmes1880
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After through testing I have found that the synthesis temperature controls the HMTD sensitivity and brisance. Temperature controls the reaction rate
which then effects particle size and crystal structure.
I have discovered that HMTD synthesized at room temperature with zero stirring acts more like a secondary and needs to be initiated by flash or inside
heavy confinement to detonate. Even inside two layers of Al foil and hammered to compaction. The HMTD will not detonate when hit by a torch. The HMTD
shows absolutely no signs of crystal faces of any type under a magnifying glass. No glints of light or anything.
HMTD synthesized at 0C-5C shows extreme brisance and will readily detonate in one layer of Al foil in 25 and 50mg amounts. Crystal faces are visible
even without a magnifying glass with this form of HMTD.
I would therefore recommend that that HMTD be synthesized at 18C with the HCl synthesis with a reaction time of under 20 minutes. This will product
when initiated by heat will not detonate in small amounts even compacted with 2 layer aluminum foil confinement but can readily be detonated via
Flash.
Summary... The colder the synthesis is done the more friction/impact/etc sensitive the HMTD is. It may be possible to synthesize HMTD with zero
agitation at -15 to -5C that is more sensitive than TATP... Be careful with cold synthesized HMTD!
[Edited on 26-2-2012 by NitricSynth]
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Rosco Bodine
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You recommend a synthesis under conditions which will produce none of the desired product. Why?
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Bot0nist
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Agree. I think your "secondary" HTMD is just infact highly contaminated with products of side reactions. Follow the proven procedures to get quality,
reproducible product.
[Edited on 26-2-2012 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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NitricSynth
holmes1880
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Botonist, with the temperature used and the extremely short reaction time it is impossible that a breakdown of the HMTD has occurred. I have run HMTD
upto runaway reaction temperatures a few times and I always synthesize a long ways below that. It has been stored for upto two months with no
measurable change in properties.
Futuremore either product in a HMTD/AN 17:83 composition produces exactly IDENTICAL plate dents.
If you want to get anywhere in business, science, etc... You have to be a entrepreneur and experiment and do what has not be done before. You'll get
nowhere and end up a bum trying to follow in others tracks.
A product that does not detonate in small amounts with light confinement is much safer to work with than a product which detonates with zero
confinement when compacted.
I don't like primary HE's as they raise my hair on end. The ability to desensitize HMTD to a near primary and farther desensitize it by making a
HMTD/AN 30/70 composition which initiates only under the confinement of 6mm plastic coated Al tubing via Flash has converted a dangerous primary into
something nearly at safe as a NPED.
[Edited on 26-2-2012 by NitricSynth]
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Rosco Bodine
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If your interest in primary explosives is based upon comparisons of other more practical materials to peroxides then that will provide a distorted
perspective.
There is no magic about HMTD, except it is piss stupid easy to make for a quick and dirty improvised use which will follow in the near term of days
not weeks or months. Other than that limited and qualified way it really has no interest and is not a practical material for anything else AFAIK.
[Edited on 26-2-2012 by Rosco Bodine]
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NitricSynth
holmes1880
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Well, the point is that nobody knows how to change HMTD sensitivity via differing crystal size and I figured out an easy way to do it with the HCl
synthesis. I'm done experimenting with it and off to mess with AgC2.AgNO3 when I get more free time.
I think that the salts static issues can easily be solved with graphite, but I'm not sure it's compatible with it. Also, the off color amateur
synthesis issues nobody has seemed to track down a solution for yet.
I already solved how to make reliable thermal shock NPED's in 6mm detonator tubing with MHN and ETN... At this rate I'm going to run out of stuff to
work on and get bored and go back to pyrotechnics and rockets.
[Edited on 26-2-2012 by NitricSynth]
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Rosco Bodine
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There are patented devices which operate on the "NPED" principle and are called "safety detonators". They are not as reliable as compound detonators,
but definitely are possible. That does not mean they are superior in principle or performance or safety in practical terms.. Cartridges for firearms
have been invented which are electrically fired. That doesn't mean cartridges fired by a conventional firing pin are unsafe or inferior. The same
applies for detonators.
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NitricSynth
holmes1880
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For the amateur with limited safety equipment NPED's reduce the risk of the common accidents tenfold or more.
It's not like you have to do the HMTD synthesis as warm as I do. At merely 10C with or without agitation you have a far less sensitive product than
0C. I may do farther testing to satisfy you guys. I have not tested 10-20C synthesis's with agitation. It's likely that 15C with heavy agitation
produces a product without any visible crystals under a magnifying glass too.
[Edited on 26-2-2012 by NitricSynth]
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Rosco Bodine
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Here we go again .......are you holmes1880 back for more?
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NitricSynth
holmes1880
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No, holmes is too chicken to even touch primaries. The closest thing he ever used to a primary was black powder mixed with ETN. Funniest part was that
actually worked with confinement...
Edit: I mean pyrodex. He wasn't using real BP.
[Edited on 26-2-2012 by NitricSynth]
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Rosco Bodine
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Okay ....consider the "reliability" aspect with regards to misfires, and they will happen with amateur made "safety detonators", and even happen with
commercial made safety detonators. The types of secondary explosives that would be most adaptable to the configuration are themselves as dangerous or
more dangerous than any of several primary explosives, excluding of course the peroxides. There are primary explosives which are useful in compound
detonators having a PETN base charge where the primary is more stable and less sensitive than the PETN. So a safety detonator can be a solution in
search of a problem that doesn't really exist, if you follow the logic. It comes down to what is your choices of components .....not a general issue
that primaries are "bad" . NG is the original NPED and is probably a bit more predictable in that regard than ETN. NG was used as an NPED even
before the invention of dynamite and the blasting cap. Those inventions were successful because the safety and reliability was improved over the NPED
configuration which came first. This you can confirm. So the idea of NPED is nothing new.
[Edited on 27-2-2012 by Rosco Bodine]
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NitricSynth
holmes1880
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LoL... Roscoe... Have you ever even synthesized or worked with secondary explosives? The way you talk about them tells me you have zero field,
military, or industrial experience in working with them.
Go out in the field and tell me how comfortable you are inserting a AgC2.AgNO3 cap into a block of PETN/ETN plastique and do the same with a non
primary device and tell me your comfort levels.
I have not discovered a design of NPED that uses NG that works within 6mm tubing. I have some ideas but nothing tested yet. Perhaps a mixture of
needle ETN, NG, and a touch of DBSP will yield a non flowing shock sensitive composition that can be initiated via Flash.
Even 1.5 Micron Aluminum 70/30 Flash cannot initiate MHN recrystallized any way you can think of at any density tested in 6mm Tubing. ETN... Don't
bother! It's only 1/4th more sensitive than PETN.
[Edited on 27-2-2012 by NitricSynth]
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Bot0nist
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Oh boy. Here it goes again. Call him a "dush" bag now. He loves that. Have you not read his semi-optimized TNP from ASA write up?
[Edited on 27-2-2012 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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NitricSynth
holmes1880
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Nah... I just think he's an idiot for considering crystalline HMTD with visible crystals safe... The Davis synthesis yields a product which can be
improved by highly decreased sensitivity via smaller crystal size with a mere 10C increase in temperature. It has and equivalent performance with
flash initiation.
Perhaps the synthesis could be improved without temperature change by the addition of micro-crystalline cellulose or dextrin.(If it's compatible.)
[Edited on 27-2-2012 by NitricSynth]
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Rosco Bodine
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Same crap ....different user name .....just as predicted by the head honcho
must have been prophecy .....divine inspiration
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SB15
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My experience with HMTD suggests that when the reagents and proportions from COPAE are used, the synthesis temperature doesn't significantly affect
the sensitivity of the final product to various stimuli, or its ability to DDT in light confinement. Pure, dry HMTD is a very sensitive compound
regardless of its crystal structure.
NitricSynth's experimental results have little value, mostly because the composition of each sample in question is not known. I suspect that a high
temperature reaction using a strong mineral acid like HCl as the catalyst may decompose the product and/or react with intermediates, resulting in a
contaminated sample with different burning characteristics.
Just my opinion.
Edit: Also, it should be known that NitricSynth is not dawson01912/holmes1880. They have similar writing styles and share a strong disdain for
theoretical chemistry, but they are not the same person.
[Edited on 2-27-2012 by SB15]
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Bot0nist
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This is my theory as well. Pure HTMD will detonate easily when confined. Even in the 50mg quantity. Not following the established procedure results in
a contaminated product, if any product at all, I would imagine. To think of HTMD (even if mixed with a lot of inert fillers) as a secondary is
laughable, IMHO. Have fun whilst excepting your Darwin's Award. Post mortem that is... 
Be safe NitricSynth.
[Edited on 27-2-2012 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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NitricSynth
holmes1880
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Yea right... The only thing I synthesize lots of is Nitroglycerin which is completely safe with my equipment. NG is amazing. Did you know you can make self hardening rock fuel compositions combining Composition + NG 25 parts +
NC 15 parts and it only hardens after staying at 40C for a number of hours? So much easier to work with than APCP...
I did the HMTD testing for a friend. I only use NPED's for charges.
Theoretical Chemistry is for nerds. Me and dawson are chemical engineers.
[Edited on 27-2-2012 by NitricSynth]
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