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mewrox99
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HMTD safety
I'm thinking of making some HMTD sometime. Simply because it seems like an interesting substance.
I have no intentions of detonating it. I just think that deflagrating <100mg amounts with my 200mW laser would make for a cool youtube video.
I have some questions though.
Is spontaneous detonation likely? If taking precautions against shock and static electricity. I have made organic peroxides before and my limbs are
intact.
Am I following a safe synthesis.
25mL of 6% H2O2 is chilled
In an ice bath 1.4g of Hexamine is added slowly and dissolved
2.1g of Citric Acid is added with stirring in small portions
It is stirred slowly.
It is left in a ice bath for three hours.
The crystals are collected and left to dry in a dark place.
I have played with organic peroxides before. But I've heard HMTD is really really dangerous.
Which synthesis is safer, citric acid or HCl
I also did research on legality and where I live HMTD is not listed as a controlled explosive. Neither is TATP.
[Edited on 29-9-2010 by mewrox99]
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hissingnoise
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FLchem10 had a disquieting experience with HMTD.
You might want to scroll down and read his thread.
IMO, the safest synthesis for HMTD is the one in COPAE.
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mewrox99
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I read that before posting scary stuff.
I'll be using a lot less. Whats COPAE
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hissingnoise
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It's "The Chemistry of Powder and Explosives" by Tenney L Davis and it can be downloaded from the site library. . .
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franklyn
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http://www.sciencemadness.org/talk/viewthread.php?tid=14514#...
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Engager
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HMTD is a mess. Personally i think that acetone peroxide is much safer to handle. One exotic manner about HMTD is that it can produce spontaneous
explosions on storage and during crystallization. I heard many stories about it, some people on forums here in Russia propose even to store it in
numerous small batches scattered in different places since in this way it is less likely that the whole mass go boom spontaneously. I personally heard
a story then carefully deacidified and phosphate stabilized HMTD exploded then guy was doing vacuum cleaning of carpet at his room, one another story
was that stored HMTD exploded from shock of closing room door.
One of the main disadvantages of HMTD is that it is slowly decomposes at storage, rendering it's behavior unpredictable. Acetone peroxide is volatile
and looses mass on storage due to vaporization, but it is not decomposed at common temperature (then carefully deacidified and stabilized of course).
So i advise to handle HMTD with great care and dispose of it as soon as possible.
1. This ref describes spontaneous explosions of HMTD (on Russian language):
Attachment: Spontaneous Explosions Of HMTD (Fogelzang).djvu (1.3MB)
This file has been downloaded 1662 times
2. Decomposition of a Multi-Peroxidic Compound: Triacetone Triperoxide (TATP), Propellants, Explosives, Pyrotechnics 27, 209 ± 216 (2002).
Attachment: Propellants, Explosives, Pyrotechnics, Volume 27, Issue 4 (p 209-216).pdf (212kB)
This file has been downloaded 1727 times
3. Decomposition of a Multi-Peroxidic Compounds. Part II. Hexamethylene triperoxide diamine (HMTD). Thermochimica acta 388 (2002) 215-225.
Attachment: HMTD.pdf (162kB)
This file has been downloaded 1808 times
4. Some insights on spontaneous explosion problems on crystallization can be found in this book: Fast reactions in solids / F.P. Bowden and A.D.
Yoffe. In chapter 8. I can attach this book here, but i have only Russian version. Details on original English book: http://catalogue.nla.gov.au/Record/769453
[Edited on 4-10-2010 by Engager]
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mewrox99
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I have made TATP before. Is it safer than HMTD.
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Engager
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Yes it is. It is also far more stable if properly purified from acid. It can be stored in frost camera of freezer for many years without any change.
Some long time ago i personally stored it for at least 5 years in form frozen with some water, after defrost i recovered completely unchanged
material.
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DDTea
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If you only want to set off ~100 mg batches of HMTD with a laser, why are you trying to make >1 g quantities? Prepare as much as you're going to
use so you don't have to worry about storage, which will create an added headache for you.
"In the end the proud scientist or philosopher who cannot be bothered to make his thought accessible has no choice but to retire to the heights in
which dwell the Great Misunderstood and the Great Ignored, there to rail in Olympic superiority at the folly of mankind." - Reginald Kapp.
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madscientist
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Acetone peroxide sublimes when stored, forming crystals that you won't want to break.
Nothing with "peroxide" in the name is safe. Period. It's only a matter of time and chance before something goes off semi-randomly. If you must make
organic peroxides, keep the amounts small enough that you could live with them going off at any point during handling.
I weep at the sight of flaming acetic anhydride.
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The WiZard is In
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Quote: Originally posted by Engager  | HMTD is a mess. [snip]
4. Some insights on spontaneous explosion problems on crystallization can be found in this book: Fast reactions in solids / F.P. Bowden and A.D.
Yoffe. In chapter 8. I can attach this book here, but i have only Russian version. Details on original English book: http://catalogue.nla.gov.au/Record/769453 |
I can.
Attachment: Fast Reactions in Solids Ch 8.pdf (1.1MB)
This file has been downloaded 1322 times
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Rosco Bodine
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The meaning of the word "safe" is highly relative, qualified, and subjective.
Is the electricity which powers our modern world safe ?
Is the fire under the teakettle safe ?
A little knowledge, too little knowledge, is often a very dangerous thing.
We do all live in a universe where the laws of probability generally apply.
Great safety is enjoyed in the presumption that everyone will do their
own "risk assessments" with regards to their own conduct and choices.
That safe presumption extends to include that some who would assert
their fitness to govern others will then seek to impose upon others the effect
of their own risk assessments, whether those assessments be "reasonable"
or right or wrong.
It is also of significant doubt that the "safest" world is a thing desirable.
Where is challenge met and any real accomplishment found for risk free enterprise, where all is done in "safety" ? Do not misunderstand that I
mean by the question to advocate recklessness.
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The WiZard is In
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HMTD TATP 1st Use
First terrorist use ca. 1983.
Attachment: HMTD TATP.pdf (781kB)
This file has been downloaded 1749 times
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mewrox99
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I think I might just steer clear of organic peroxides.
Why take the risk? I'll just make some NC to light with my laser.
There is just so many things that could go wrong with TATP or HMTD.
Nitrocellulose will give the effect I'm trying to achieve (fireball) and is safer on every level. Annoyingly I don't have any HNO3. So will have to
make do with KNO3/H2SO4
[Edited on 5-10-2010 by mewrox99]
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the Z man
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surely NC is the best choice. Actually NC was my first "good" HE (made tiny amounts of AP before but I was too scared even to let it dry completely).
With NC I learned the basics of nitration and I spent a lot of time to optimise the ratios and temperature of reaction. Finally I managed to make NC
with NH4NO3/H2SO4 that burned almost as fast as the one made with nitric acid 
While researching on NC I started to use roguesci and this forum as my first reference.
Sorry for the OT but nitrocellulose always reminds me the good old times and a lot of entertainment 
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mewrox99
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Should I use KNO3 or NH4NO3.
My KNO3 is a dry powder, while my NH4NO3 is prills
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the Z man
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I haven't tried with KNO3 but I have the feeling that using AN will make the nitrating solution less thick, and since the good quality is given by the
complete absorbtion of the nitating mix I think AN is the best choice.
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mewrox99
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Ok will try tomorrow! Time to calculate the stoichiometry.
0.5mol NH4NO3 = 20.00g
0.25mol H2SO4 = 24.52g *1.84 = 45.1mL
Can anyone tell me if i did it wrong
Also do I have to grind the NH4NO3 or can I use prills
[Edited on 6-10-2010 by mewrox99]
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DDTea
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| Quote: Originally posted by mewrox99 | Ok will try tomorrow! Time to calculate the stoichiometry.
0.5mol NH4NO3 = 20.00g
0.25mol H2SO4 = 24.52g *1.84 = 45.1mL
Can anyone tell me if i did it wrong
[Edited on 6-10-2010 by mewrox99] |
Check your calculation. 1.84 is your density, correct? Density has units of 1.84 g/mL.
[Edited on 10-6-10 by DDTea]
"In the end the proud scientist or philosopher who cannot be bothered to make his thought accessible has no choice but to retire to the heights in
which dwell the Great Misunderstood and the Great Ignored, there to rail in Olympic superiority at the folly of mankind." - Reginald Kapp.
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the Z man
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errr... excuse me for the question but have you ever performed a nitration before? Stoichiometry is almost useless with nitrations (especially
synthesis of nitroesters and using nitrate salts instead of nitric ) as you always have to use large excess of acids and different ratios for every
synthesis. Nitrations are more like an "empirical" type of reaction.
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mewrox99
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Damm your right. DDTea
That's why you shouldn't calculate things when you haven't had enough sleep.
I tried the 20g AN in 50mL H2SO4. Seem to work fine. Let it nitrate for about 20mins.
The cotton is now a slight yellow color. I'll test it tomorrow when it's dry
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mewrox99
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I took some of the not so dry stuff and put it on my hot plate at max heat. It took a lot longer then expected to ignite and still left ash.
Anyway I'll get some HNO3 someday in the near future. Also this thread has gone of topic as it's initially about HMTD
I think I used to much cotton and under nitrated. I used enough to completely absorb the nitration solution
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KNO3me
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| Quote: Originally posted by Rosco Bodine | The meaning of the word "safe" is highly relative, qualified, and subjective.
Is the electricity which powers our modern world safe ?
Is the fire under the teakettle safe ?
A little knowledge, too little knowledge, is often a very dangerous thing.
We do all live in a universe where the laws of probability generally apply.
Great safety is enjoyed in the presumption that everyone will do their
own "risk assessments" with regards to their own conduct and choices.
That safe presumption extends to include that some who would assert
their fitness to govern others will then seek to impose upon others the effect
of their own risk assessments, whether those assessments be "reasonable"
or right or wrong.
It is also of significant doubt that the "safest" world is a thing desirable.
Where is challenge met and any real accomplishment found for risk free enterprise, where all is done in "safety" ? Do not misunderstand that I
mean by the question to advocate recklessness. |
I couldn’t have said it better Rosco Bodine, that’s what the nanny states around the world just don’t seem to understand for some reason.
Anyway, back on topic, I have synthesized HMTD only once and it didn’t turn out right. The deflagrations were very slow and I think it may have been
because I rinsed with plenty of sodium bicarbonate and didn’t rinse the explosive of sodium bicarbonate.
I plan on synthesizing HMTD again later on and I’m wondering if it’s okay to rinse with denatured alcohol rather than methanol, after I wash with
distilled water?
This time I’ll be using Tenney L. Davis’ Hexamethylenetriperoxidediamine synthesis. He say’s to rinse with alcohol after thoroughly washing with
water but Davis doesn’t specify on which alcohol.
"If we knew what we were doing, it wouldn't be called research." - A. Einstein
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FLchem10
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Yes I was the one who labeled my post "HELP ME" but I have made energetic materials for years.....I work in a college lab I should of asked for an
opinion not said help.....Yea HMTD is very dangerous but that being said it has alt of history of being made and HELL ALL OF THIS STUFF PEOPLE MAKE IS
DANGEROUS!!
I had a fluke mishap which happend but thats science with Energetics and I had it all in a very safe place.....If you were to go ahead and make it HCL
and Citric are both tricky to add without using proper procedures.....
My thread got bash by someone who believes I didnt know what I was doing as he should because I look on here alot and see KIDS, 13 year olds, doing
things that they should NEVER BE DOING... If your going to do any of this type of chem. you have to be aware that things go wrong and you should be
prepared.
Anyways if you make your own HMTD make a small amount at a time....keep it in a container that is not glass....much like a specimen jar that are
usually plastic and put it in a plastic bag like the one's people use for pot dime bags and leave it in, if you have one a safety cabinet if you plan
to store it but even a high watt light bulb will heat it to combustion and all the other FLUKE things that might happen but you can be safe making
such things...
If you ask me half of the things people make here are MUCH worse that that!!
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quicksilver
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There is no "worse". The term has very little relevance to the subject.
Energetic materials are subject to stimuli. Education as to the threshold of stimuli basis for initiation is an issue that reflects the inherent
danger. Without it anything can be dangerous (don't run with scissors).
......"Pot dime bags"? Static and plastic bags have a unique relationship.
Frankly the amount of actual synthesis is low compared to the level of reading and discussion of the subject matter. I have no idea how many people
synthesize [what level] of materials within the Forum. I suspect that it's relatively minor. Yet have no idea; nor would I suggest that 13 year old
children do so. The educational level of an individual is fairly obvious when they post.
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