HMTD

[VX]

My ‘friend’ is interested in making some HMTD again.

But he has one major problem, he has no Citric acid, and no way of getting any in the foreseeable future. (chemists seem to be not selling it any more and treating you with extreme suspicion when you ask for it….. probably due to several people being arrested for manufacturing it with ‘terrorists intent’ over the last few months.) :mad:

Anyway if the H* ions in the citric acid acts as a catalyst for the reaction, why can other common acids not be used, such as Sulphuric for example. This would be useful to me as I have some of this lying around doing nothing.

Can sulphuric be used or is it crucial that the acid is citric, if so could someone please tell me why as I am very curious, and web searches have not proven fruitful.

Thanks,

VX :)

[BrAiNFeVeR]

Though this has been covered more then enough ...

Since the acid just works as a catalyst when making peroxides, you can use them all !!

I, for one, recommend HCl, since it completely vaporizes while drying, unlike H2SO4, and it is cheap and easy to find.

Edit: Just noticed that the answer is right under your nose (below your thread).
Shame on you !!

[ 07 March 2002: Message edited by: BrAiNFeVeR ]

[VX]

I know that any acid can be used to manufacture AP, my friend himself has used three different acids to do so.

However i've just re-read the below forum, and nowhere does it say that any acid can be used to make HMTD. Infact the whole of the internet seems to say that only citric can be used :rolleyes:.

Before trying this method I wanted an answer specific to HMTD and sulphuric acid, so I was sure I was not going to kill myself or others.

I am curious to know if any acid can be used, why is a weak organic acid used commonly used instaed of of the cheaper, stronger inorganic acids.

Also how much H2SO4 would be used?

PS: sorry if this seems like a kewl question, I assumed any acid could be used but wanted to be absolutely sure. I can remember a thread on the old forum which discussed using glacial ethanioc acid, but have never seen it written that a strong acid can be used as well.

[ 07 March 2002: Message edited by: VX ]

[Madog555]

what about oxalic acid?

in makeshift arsenal it gives a method for useing HCl but it is vauge and says that its unreliable and doesn't always work.

i tried it once but it failed, i wasn't that precise with the measurements and mixing though.

i think i also tried oxalic acid but it didn't disolve very well or something weird happened, i can't realy remember.

[VX]

Thanks for that, i'll look into the oxalic acid method.

I'll still particularly apeciate any info on using strong acids though, if anyone has any that is :)

[xoo1246]

HCl and HTMD is imcopatible, ascorbic
acid too and mineral acids.... stick to citric or concentrated acetic acid.

Ohhh, and I hate that fucking makeshift arsenal.
How to build a fucking rocket launcher? Do you really need a manual to figure out you could put a rocket in a pipe, connect it to some electrical ignition then put it on you sholder fire and have shrapnel all over your face.

[VX]

Ahh brilliant... Just the info I needed, dissapointing though. Oh well i'll have to find one of those then.

Thanks again,

VX

[A-BOMB]

What planet are you from zoo?
It is just a catalist in the reaction nothing more. And to this point in many of my "dreams" I used HCL with great success and the HMTD had a great shelf live of like a year or so, (like 11 months) and still was able to detonate (in the dream it was stored in a old brown glass budwiser bottle in a coffee can full of sand on a shelf in my old generator shed.

[Madog555]

do you have the ratios and/or method you used?

[ALENGOSVIG1]

i Have a method i use for HMTD that uses HCl in my PDF. You can use different cocentrations of HCl and H2O2. You just have to calculate it.

Download it at http://www.angelfire.com/linux/aleng/

[DBSP]

There is a method that uses HCl at Mr cools page aswell!

[Madog555]

ok, thx, i think im gona try this out again

[00Buckshot]

I didn't know if this should be under a new topic or not.
I am starting my first batch of HMTD, and still have a question or two.
I was wondering if before I add any citric acid does the H2O2 and hexamine need to be mixed together slow, and cold?

Is there even a reaction between just the H2O2 and hexamine? And does it create heat without any citric acid?

Does HMTD have a trimer and dimer version similar to AP?

Thank you

[RTC]

Doesn't really matter what you add to what in my "tests" it's always worked no matter what I added first.

Just as long as there cooled and kept in an ice bath.

[00Buckshot]

Thanks for the speedy reply.

Right now I have the H2O2 mixed with the Hexamine, and its cooling in an ice-bath, and the whole thing is being kept in the freezer.
I didn't notice any rise in temp, so far.

I'm really curious if there is a dimer and trimer version to HMTD?
Would making HMTD without the ice-bath result in a more unstable form of HMTD? And therefore, is it the colder the better?

Thanks

[kingspaz]

the ice bath is used to keep the temperature low so there is less risk of a fast reaction creating alot of heat resulting in a possible explosion. it is also used as the HMTD will be less soluble in a cool solution than a warm one. therefore if cooled you will get a better yield.
as seen on the picture you can only get one version of HMTD due to the nitrogen having 3 unpaired electrons for bonding.
<a href="http://www.angelfire.com/mo3/kingspaz/hmtd.gif" target="_blank">http://www.angelfire.com/mo3/kingspaz/hmtd.gif</a>
need to copy and paste the link.

<small>[ March 21, 2002, 06:27 PM: Message edited by: kingspaz ]</small>

[Zambosan]

Kingspaz: I think your GIF of HMTD is a little incorrect; it should look like:

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">code:</font><hr /><pre style="font-size:x-small; font-family: monospace;"> (CH2)-O-O-(CH2)
/ \
N-(CH2)-O-O-(CH2)-N
\ /
(CH2)-O-O-(CH2)</pre><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">You're absolutely right about there only being one form, however.

[kingspaz]

ahahahahha, i knew i should have checked that diagram!
i found it on the net ages ago, hadn't actually looked at it properly until now! i'd seen it...just not actually took it in and realised!
thanks

[tango]

This might be a kewl question, but what should my HMTD look like three hrs into the reaction. At the moment it looks like a cloudy/misty water, cloudy patches throughout the beaker.

[DBSP]

It seems allright. After the cloudy phase it schould get a bit clearer and the crystals schould settle at the bottom of the beaker.

[xoo1246]

White and cloudy, maybe some powder on the bottom, yes that should be HTMD.

[tango]

I'v just woke up to filter my HMTD and thier is hardly no HMTD, I don't even think it is HMTD. HOW MUCH SHOULD I GET OUT OF,

100 ML H2O2
2 TEASPOONS OF HEXAMINE
4 TEASPOONS OF citric acid

time left to react: 15 hrs
It just looks like Hexamnine not dissolved

[DBSP]

Whats the conc of your H2O2? I hate measuring things in "tablespoons" and similar I it's a powder the ammount can gety very wrong using tablespoons. Get a scale!!! There is no way of telling how much you schould end uo with when making HMTD I get a different ammount every time. With AP it's easier to predict how much you schould end up with.

[tango]

My H202 is 6%, would you recommend using digital scale?

[DBSP]

Any scale that is accurate enaugh can be used. I use a electronic scale 0-2000g +/- 1g (0-1000g) +/- 2g (1000-2000g). About a gram +/- is what I expect from a scale. Used for normal things, but if you are weighting smaller ammounts a +/- 0.1g is required.

I've allways made HMTD with 35% H2O2 so I don't know of what to expect from 6% H2O2.

[kingspaz]

if your using 6% then leave it a couple of days in the fridge.
what do you mean it looks like the hexamine hasn't dissolved?....maybe it did and what you looking at now is HMTD.

[00Buckshot]

I have had my HMTD mix sitting in the fridge for about 60hrs and still I still have no HMTD cryatals. This is my first time but I followed directions.

My mixture is very cloudy, but is also very yellow in color. Is the yellow color normal?

I made sure all the hexamine crystals dissolved when I added them.

The only time I didn't follow directions is with the H2O2. I used the 3% and I used 10X's as much to compensate. I understand this would slow the reaction time but this has been c ouple days now. Next time I will use the 35% I can buy, but didn't to save a couple bucks.

The entire first day the mixture was in the freezer, and since then has been in my very cold fridge. Do you think I should leave it sit at room temprature for awhile? Maybe that would speed this reaction up.

[kingspaz]

add some extra cirtic acid. that should get the reaction going. when you used 10 times more you dilute the acid by 10 times also which means you need more acid too.
since this is your first time heres some advice:
1. wash your HMTD a few times then neutralise the HMTD by soaking it in bicarb (soidum hyrdrogen carbonate) solution for a couple of hours. this is very important as it will make your HMTD much safer. it will removed residual acidity which would remain if only washed. acidity make HMTD much more unstable.
2. avoid all forms of friction. handle it VERY carefully.
3. if you store it, store it damp with water.
4. don't leave it in the sun to dry!

[tango]

thanx guys i'll do that next i make HMTD. I have filterd the powder out of the mixture, and it's pasty. should it look like that?

Yea i quess that was a stupid question about the HMTD looking like udissolved hexamine.

[tango]

I'v lit some damp HMTD and it burnt like flash cotten, is this correct.

[vonK]

Tango, it looks to me like your method is crap.
I use - 45ml 6% H2O2
- 2 1/2 teaspoons Hexamine
- 4 1/2 teaspoons citric acid
Yeild is 1 1/2 to 2 teaspoons HMTD.
I never wash my HMTD with bicarbonate solution and have had no problems. I just rinse the reaction jar with tap water and pour that over the HMTD in the filter then do the same again with meths. The meths makes it fall off the sides of the filter and clump in the bottom.
I find damp HMTD splutters a bit but dry HMTD makes a nice "THUMP".
Yes It should look a little pastey.

[Anthony]

Yes, it does appear pasty if the HMTD is a fine powder.

Seriously, do include the neutralisation step. Personally I only leave it to soak for a few minutes in the bicarb solution and give it a good stir. I have had an accident with a batch of CTAP that wasn't neutralised, so now I always do it. You might not get problems with your HMTD process because the citric acid is such a weak acid. Still worth getting into the habit of including a neutralisation step though for when you start using mineral acids like HCl and H2SO4 as catalysts, rather than citric.

[Yikes]

HMTD can look pasty if there's still some citric acid in it.
If it flashes like 'guncotton' when still wet: don't worry. HMTD will burn that way when it's dry too: perfectly normal. It will detonate when confined.

[00Buckshot]

It has now been a very long time, about 80hrs and I'm pretty sure that HMTD will not form, but I'm not going to dump the mix yet. Just in case.
I did add more citric acid, an hour later I took it out of the fridge and for the first time the mix sat at room temp. Now the mixture has turned from murky yellow to a dark red/amber color. And it has bubbles comming up, when I stir the mix it fizzes.

Has anyone made HMTD and seen the mix turn yellow, or red like that?
Is it dangerous to keep the mixture for more than a few days?

[tango]

Yes i'v had my 2nd mixture turn from Completly black to lime green.
The colures were very funky

[tango]

I forget to mention that i added H2SO4 and citric acid into the hexa-peroxide solution, i added alot of each chemical this time and i have a larg amount of powder forming.

[vonK]

What the hell are you guys doing!
I must have made HMTD about 30 times and not once have I had a colour change.
My H2O2 is colourless, my hexamine is white, my citric acid is white. The solution is colourless except for the HMTD, which is white (and forms on the bottom and the top of the solution) and a few bubbles.
What are you doing that makes such screwed up colours.

<small>[ March 24, 2002, 04:42 AM: Message edited by: vonK ]</small>

[0EZ0]

Read closely vonK. Many H2SO4 solutions like Drain Opener contain addatives like detergents which would explain the colour. <img border="0" title="" alt="[Wink]" src="wink.gif" />
Am i right?

[xoo1246]

Colored HTMD, good one. :D
No, I would dump it, could be unstable.
Try using citric acid and tell us if you still get colored HTMD.

<small>[ March 24, 2002, 06:17 AM: Message edited by: xoo1246 ]</small>

[00Buckshot]

Hmmm, this is strange, because I am not using any H2SO4 Im using citric acid, hexamine, and H2O2 3%.

Since I took it out of the fridge it turned from yellow, to redish, and this morning it has turned into a vey dark red, almost black. I think it will be black by this afternoon.

I don't want to dump, just to see if any HMTD will form. Unless someone knows this is risky???
Nobody has had HMTD chage colors? Hmmmm this is my first time, but I did follow directions.

[Anthony]

You almost certainly have contaminents. Either introduced by one of your chemicals being impure, or more likely, like did you use to stir the mixture with?

Whatever the cause, chuck it. You're unlikely to get any precipitate by now and if you did, god knows what kind of sensitizing contaminents it'd have in it.

[DBSP]

Like Xoo says dump it!! I once made a batch of AP when my thermometer broke and the stuff in it went out in the solution. Is it some kind of alcohol in it?? When it had dryed I testd the sensitivity and it was far greater than usual so i dumped it.

[00Buckshot]

Ok I just dumped it.

I did use a metal kitchen spoon for stirring, if anyone thinks that was the problem.

[Pu239 Stuchtiger]

Don't use metals, or anything reactive to stir it. Preferrably use a glass stirring rod; if that isn't available, then use a plastic spoon. You probably ended up with contamination by a metal citric acid salt.

[kingspaz]

the metal could react with either the H2O2 or the acid, likely both!
also, the metal will catalyse the decompostion of the H2O2 decreasing its concentration therefore stopping the reaction progressing to completion.

[EventHorizon]

tango: If I read your post correctly you added BOTH H2SO4 AND citric acid? If that was the case you are most likely getting some kind of side reaction between the citric and and H2SO4. Try using hexamine, peroxide and HCl, that seems to me the best way to make it for me as all reactants are liquids. The citric acid method seems to make a less storgae stable product and the solution is much harder to filter, even with vacuum filtration.

[vonK]

I've made many, many batches of HMTD using citric acid and it works perfectly.
No storage problems at all. I still have some of my very first batch that is nearly three years old.
Why would you need vaccum filtration? HMTD filters fine using common old gravity filtration through a paper towel in a kitchen funnel.
Citric acid is also dirt cheap in NZ. I get it from any supermarket at around $1 per 100g. Much cheaper than HCL which is $32 per liter at hardware stores.

Tango, where are you getting your H2SO4 from. In my early days I boiled down battery acid but now I get it through an industrial chem supplier.
I don't think H2SO4 is sold in NZ as a drain opener

[kingspaz]

i think HCl is the ideal acid to use in HMTD manufacture because it will evaporate leaving no residue - HCl acid is hydrogen chloride (boils at about -85*C) dissolved in water, water evaporates along with the hydrogen chloride.
when useing H2SO4, with a MUCH higher boiling point of around 300*C if i remember correctly (which i often don;t!), it will not evaporate and will remain as an acidic residue in the HMTD = unstable HMTD.

[EventHorizon]

Either method is fine, tho most I think prefer the HCl method. Here I can get 1 qt. (~.95L) for $2.38USD so of course that is the method to use here, but at $32/L, common sense dictates the use of citric acid. I use vacuum filtration to get every little bit I can from a batch, mainly because I have the equipment handy.

[tango]

vonK i got alot of H2SO4, mainly from getting it from car batteries. And yes they don't sell it as Drain poener in NZ, how much was your HCL and what store did you get it from i'm having problems getting it.

[vonK]

Ah...I already said HCL was $32 per liter at any Hardware store, did you mean H2SO4.
I got my H2SO4 through a cleaning supply store, they had to order it for me as they aren't allowed to store it for more than three days. I got 10L of 98% H2SO4 for $98.00 .
It came from Andrew Industrial, they also sell acetone, HNO3 and concentrated H2O2.
I told the lady in the store I wanted it for a science fair project, converting wood into methanol as an alternative fuel using the H2SO4 to break down the lignin that binds the cellulose together. I'm not sure if thats right but it worked a charm and your free to use the same excuse if you like.

[DBSP]

32$ for 1L HCl is extremely expensive. I get it for 3$ a liter, 30%. I've never made HMTD with HCl but I might try it soon.

[00Buckshot]

My first attempt at HMTD failed, it changed colors. I used the cheap 3% H2O2.

Yesterday I made my second attempt at HMTD. This time using 35% H2O2.
Today I found lots of HMTD in the reaction vessel. Success!!
When I thought the reaction was done I washed with sodium bicarbonate twice, and then with pure water twice.

Now my concern is when I took the HMTD out of the coffee filter it was a very thick constincy and it collected into mushy chunks. I can't break the chunks into powder because its wet. So I think I'll have to crush the chunks of HMTD as it dries? Is it dangerous to crush the dried HMTD if I do it gentle? How do you do it?
I didn't use any sovents for a fianl wash to speed drying.

[kingspaz]

if its in chunks then the crystal lattice of each little grain must be merged somewhat. this means as you crush it you break crystal lattices = possible BOOM! don't do it! throw it away and make a new batch! its not worth the risk.

edit: just thought, let it dry first it may crumble down into a powder. if however it remains in big hard chunks dispose of it.

<small>[ March 26, 2002, 06:40 PM: Message edited by: kingspaz ]</small>

[00Buckshot]

Any idea why the crystals would merge like that?

I was expecting it to look more like re-crystalized KNO3 which I have more experiance with.

[nobody]

I think, this chunks are not crystals. So break them down very carefully with a plasticspoon or something like that when they're dry. Use small batches, maybe 0,2g. If thish really detonates, it doesn't matter.

[EventHorizon]

Use a face shield and heavy leather gloves (ear protection is a good idea too) and roll the "chunks" using a plastic dowel on a piece of paper. The HMTD powder forms clumps but not big crystals, the trick is to gentley break it all up into powder. A 1/2" or 3/4" teflon rod works great for this. If it doesn't want to powder eaisly, as in gentle pressure, then DON'T force it.

[xoo1246]

I have never had this kind of problem, my HTMD is allways very finely divided. Anyway 0.2 grams of HTMD wont detonate unconfined.

[00Buckshot]

Last night I tested my first HMTD batch. It was my first time ever seeing something that powerful. And it dropped my jaw.

I put my HMTD into 2 paper triangle salutes, each was about the same size as we make our normal traingles with black powder. We were just hoping that the HMTD would explode the entire triangle, unlike bp which would only blow the trainlge into a few big chunks.

Well I put one about a foot away from a free in the snow, and was shockd to notice the tree had some bark blasted off of it.
Next one we put right up against a small tree and it shredded it up pretty good.

Im very impressed with HMTD, after last night regular bp will never be the same.

[DBSP]

Just wait untill you see the real ones. <img border="0" title="" alt="[Wink]" src="wink.gif" />

[EventHorizon]

xoo: .2g HMTD won't detonate by flame, but WILL by impact/scrape. Trust me, my ears rang for an hour when I was attempting to do a flame test with one of those long lighters. Was kneeling and got off balance and shoved the end into the little pile which was on concrete. My flame test turned into a scratch test and a detonation ensued.

[Zambosan]

I can't picture that tiny of an amount doing much of anything!

<small>[ July 18, 2002, 01:24 AM: Message edited by: Zambosan ]</small>

[00Buckshot]

I had a batch of HMTD get out of hand the other night. I used 35% H2O2. It was making loud gurggle noises, and was steaming heavily. I dumped and flushed it with water as soon as I noticed.

I think it happened because I was rushing. Patience was my problem.

I thought I would speed the reaction time by taking the mix out of the freezer, and ice bath, after about 3 hours. So I let it sit at room temp.
Then when it warmed up the precipitation of HMTD began, but I again rushed it, by stirring it for a few minutes to speed the reaction up. The glass was still cold, it seemed fine. Then 30 minutes later it went crazy.

I admit I only have some real experiance with low explosives, and only made HMTD afew times before. This scared me. The glass was very hot when I dumped, I thought it may even break.

What would have happend if I wasn't around to spot it? Could it explode? Or would it have calmed down in a few minutes?

<small>[ March 28, 2002, 04:59 PM: Message edited by: 00Buckshot ]</small>

[Yi]

I've had an HMTD reaction react too quickly when I wasn't there. All it did was spray the mixture everywhere and the splashes also had HMTD crystals on them. It was annoying to clean and that was all. Luckily I don't have anything near beakers that have reaction mixtures in them.

[00Buckshot]

Does anyone have a negative experiance with HMTD?
Has anyone ever had some HMTD explode when you didn't want it to go off?
If you have, please post what happened.

I use citric acid in the reaction. Wouldn't the citric acid be "safer" to use than those stronger acids?

Furthermore, why does it seem that most people choose AP as their peroxide of choice? I don't think AP is safer than HMTD? Or is it just because people can't get the Hexamine? It seems in the forum, and even the FTP have plenty of info about AP, which is fine. But what about HMTD?

[S. Toppholzer]

Reminds me of my first batch of HMTD I made. I used 30% H2O2 for making it. I left it out in the open (t'was wintertime) and forgot about it for a week.
When I came back to check the result... It was incredible: a huge amount of loong-needled HMTD crystals was waiting for me! Unfortunately, the cover was blown off and some dirt (dry leaves and stuff) went into the HMTD. I just threw away the whole batch becasue I was afraid the impurities might have rendered the product unstable. If I could repeate that great result I wouldn't throw it away again.

[Anthony]

Big crystals are bad!

AP does seem to be more common, performance wise there isn't a lot bewteen AP and HMTD, I guess acetone is just easier to get than hexamine.

Personally I prefer HMTD as it is less volatile.

[kingspaz]

00Buckshot, i beleive most HMTD accidents result from people not cleaning and neutralising the HMTD properly. this results in it being very unstable. all HMTD batches should be neutralised with a bicarb solution, and washed in alot of water.
i beleive the best acid for explosive peroxide production is HCl since it will evaporate with the water and not leave an acidic residue as H2SO4 or citric would. this would result in a much more stable product and therefore greater safety. HMTD has a larger gas volume produced than AP i think and a similar VoD therefore making it a slightly better explosive. i also beleive it is slightly less sensitive, although i have no experimental evidence to back this up. its is MUCH more stable in storage and will last a few months without degrading perfomance significantly.

[DBSP]

AP can last months to but if you would compare the two and see wich one that has lost most weight the AP would definately have lost more weight. I've had AP and HMTD for months and I haven't found them to become more sensitive or anything the only thing that has happened is that they've lost some of the weight because they are both violate substances.

[Rat Bastard]

I just finished a batch of HMTD last night and it worked great!

<img src="http://members.shaw.ca/raydawg/pics/hmtd.jpg" alt="" />

vonK , thanks for the recipie!

I washed it several times with water, and then a final time with Isopropol Alcohol. When lit, it flashes and makes a nice THUMP!

I put a small amount (a matchead size pile) of my HMTD on a metal block and struck it a few times with a hammer, after 3 blows, BANG!!!!!

Both of my ears are ringing! damn!

--
P.S: what is all this stuff about a Bicarb solution? My stuff worked fine, being washed by water & Isopropol.

<small>[ April 04, 2002, 08:18 PM: Message edited by: Rat Bastard ]</small>

[Anthony]

Basically, after filtering and rinsing your AP/HMTD you dump it into a few percent sodium bicarbonate solution to neutralise it, you then filter it out, rinse again and then let dry as normal.

[Rat Bastard]

Thanks anthony. Now one thing, when HMTD burns, it burns fast and flashes like flash cotton. And when you strike it, it seems to Detonate (DAMN it was loud! next time ill wear ear protection). Now if I had a paper triangle salute filled with HMTD with a visco fuze, is it actually detonating?, or is it just burning and acting like normal compositions like Black Powder (only better).

Im kinda confused about this detonating/burning thing with HMTD.
.
.
P.S: I added a pic of my HMTD in my previous post.

<small>[ April 05, 2002, 12:45 AM: Message edited by: Rat Bastard ]</small>

[Anthony]

When struck HMTD will detonate. When ignited - spark, flame etc it will deflagerate like a low explosive such as BP. If there is sufficient confinement (a layer of tissue paper is enough) then the HMTD will make the deflageration-to-detonation transition and detonate just like when struck. So yes, the HMTD in crackers does detonate.

[DBSP]

And if it's a lumb of it or AP and the size of it is a bit larger than a pea it can detonate if a flame is put to it because of the selfconfinement.

[00Buckshot]

Ok thanks for those tips.
I have have a few more questions about HMTD.

I try to keep the mix in the freezer until the reaction is done. However for some reason the reaction will not even start if its kept in the freezer.

Then after about 48hrs, I usually take it out of the freezer and let it sit at room temp. The temp rises and the reaction starts, and then every time it goes crazy, boils and steams. So I add some water to dilute it, then I must put it back in the freezer to cool it. Otherwise it gets hot.

Im using 35% H2O2, and none of the methods I've seen give good ratios for 35% and citric acid?
Is this because I'm using 35% H2O2? Maybe I'm using to much acid? Does this happen with AP? Maybe I should switch to making AP?

[Zambosan]

Just use simple algebra to solve for the amount.

<small>[ July 18, 2002, 12:30 AM: Message edited by: Zambosan ]</small>

[jin]

you may have probelms geting citric acid from chemists in the uk because its used to purify heroin before injecting so some chemists will not sell it anymore.

[0EZ0]

I have never had a problem obtaining Citric Acid. I get it from the local supermarket in a shaker container for use in cooking. I found it in the spices section.

[tango]

I find it really easly to obtain Citric acid, if they ask you what you want it for, just say you want to make some sherburt because that's the main ingrediant.

<small>[ April 09, 2002, 02:05 AM: Message edited by: tango ]</small>

[00Buckshot]

Citric acid is getting harder to find here in Canada. A year ago it was available everywhere. Now I can only get it at one drug store. In the bulk barn they keep trying to tell me that absrobic acid is the same as citric acid, just a different name. The thing I don't get is if citric acid is used for food and drinks, why wouldn't it be in the grocery store, and not the pharmacy?

Anyways May 24 will be here soon. Im going camping as usual, and I want to bring some HMTD into the deep bush. Its about 6 hours by car, and 3 hours of those are bumpy and rough dirt road. I'm a little nervous about transporting the HMTD, I figure I'll keep it in the center of a cardboard box filled with tissue paper around it to cushion it. That should keep it safe? Or should my priority be to keep it cool? Should I keep the whole thing in a cooler? With cold packs?

[A_W]

I`m considering to start making HMTD. I have NO experience with high explosives, and I thought it sounded as a good explosive to start out with. It recuires no dangerous chemicals, (3%H2O2 is not dangerous, according to my encyclopedia hexamine is not poisonus, and citric acid is used for food) wich I like after my bad experiences with the nitrocellulose prosess. :(

I hope to make very small quantitys (under 1/2 teaspoon) wich I plan to pour into a cardboard cartridge and set off with a small firecracker or simply a fuze. I will try it as soon as I can get the chemicals.

Edit: I never had any problems getting citric acid here in Norway. It is sold at supermarkets and is used in many sorts of food (it is also used for making wine, I think)

<small>[ August 30, 2002, 01:52 PM: Message edited by: A_W ]</small>

[mr.evil]

why don't you press out an lemon? than you got Citric Acid(i don't use the juice, i use a sort of crystalls buyed at the Drugstore)

[Anthony]

Citric acid is indeed available for home brewing.

Buckshot, it might be better to take the precursors with you and make the HMTD or AP on site? It'd save the hassle of safely transporting and storing it and you could make it up as you need. Or dissolve it in a solvent, or soak with water or alcohol and evaporate the solvent/wetting agent, to recover the HMTD.

[00Buckshot]

The idea of preparing it on site isn't to good for me, because we are pretty busy fishing and doing other camping stuff. Also I don't want to make it drunk with many distractions.
But the idea about dissolving it in a liquid sounds good. However I don't want to use water, because it would dry slow, and I don't want to use the sun to dry it.
So I guess I'd use acetone? I don't have access to the type of alcohol recomended in the chem lab for drying HMTD. If I did use acetone would it dry clean and neutral pH? Or do would I wash it with the sodium bicarbonate and then dissolve in the acetone?

Also everything I read says HMTD is very heat sensative. Well you know how if you leave you're car in the sun with the windows up, it becomes a sauna in there? Would that set HMTD off? or would that just degrade the explosive power tof the HMTD?

Thanks
Buckshot

[Anthony]

I'd say ingition temperature of HMTD and AP is going to be at least, or around 100*C, sunlight and hot cars shouldn't be a worry. Unless your HMTD/AP is for some reason (contamination etc) more sensitive than it should be. High ambient temperatures may well make HMTD/AP, like other explosives, more sensitive.

The HMTD/AP will need to be pure and neutralised before it goes into the acetone. The acetone will evaporate completely and leave everything behind, that includes and contaminants.

I got to ask though, if you're going to be too lashed to make HMTD, are you going to be capable of handling and using the finished product safely?

[Zambosan]

Sunlight certainly can detonate quantities of even unconfined HMTD. I've seen a picture of the aftermath before... I'd link to it if I could remember where it was. I wouldn't want to leave it in a hot car.

[Anthony]

If it was these ones:

<img width=400 height=300 src="http://www.xinventions.com/main/pyro/images/hmtd_boom.gif">

<img src="http://www.xinventions.com/main/pyro/images/hmtd_boom2.gif" alt="" />

Then it was the Xinventions place. IMO the guy doesn't really know what he's doing and his forum is over-run with kewls. I haven't heard of anyone here having found properly washed and neutralised HMTD or AP to be sensitive to sunlight.

<small>[ April 09, 2002, 03:32 PM: Message edited by: Anthony ]</small>

[A_W]

How do I make a good ice bath for HMTD manufacture? Back when I was making nitrocellulose I just glued a small glass vessel into a glass bowl. The problem with this is that it does not chill the bottom of the reaction vessel. As the ice bath is for HMTD, I really want it to cool the bottom to.

[Yi]

Get a small ice box (ie, those things you take to picnics), fill it with ice put your beaker in there & close the lid. It will take the ice approx 20hours to melt.

[A_W]

Are you sure that the beaker (reaction vessel) does not have to be attatched to the ice bath container in any way? There is a chanse of the beaker tipping over inside the icebath when the ice melts if the beaker is smaller than the ice bath container.

[DBSP]

One thing you can do to keep it from tipping over is filling the ice bath with paper or something similar or rapping it arround the reaction vessel.

[nbk2000]

I've used a large piece of styrofoam with a hole cut in the center. This floats in the water and will always keep the flask upright and above water.

[A_W]

When I hear about people dumping their HMTD for some reason, I tought that it would be safer to have a chemical neutralizing the HMTD into harmless chemical(s) rather than dumping it into the woods or flushing it down the sink. Is there such a chemical and is it easy available?

[S. Toppholzer]

Talking of HMTD:
Whenever I dream of making a detcap with HMTD as a primary I get worried because of the wires touching/being embedded in HMTD and thus a possible reaction of the nichrome or lightbulb wire. Usually I fill a piece of plastic straw with Armstrong's mixture in which I embedd the bulb wire. The straw in turn is being iserted in the much wider, plastic coated detonator whose top is being filled with some HMTD. So the Armstrong sets off the HMTD and that goes straight to my favorite, TNP.
I did make a couple of HMTD batches but I am still somewhat fearful of that substance. Could anyone tell me if HMTD generally is more or less sensitive as Armstron's when it comes down handling the dry stuff?

[A-BOMB]

You use Armstrongs mix to set off the HTMD <img border="0" title="" alt="[Eek!]" src="eek.gif" /> what are you nuts?

[S. Toppholzer]

excuse my ignorance - I was thinking of possible side reactions caused by HMTD getting i direct contact with the igition wire.
The amount of Armstrong's used is pretty small - if wetted down to a claylike mass you might have the amount of maybe half a pea.
But I have been thinking again about the question of sensitivity of HMTD. I guess it mus be less sensitive than Armstrongs since if one tried filling a toy revolver cap with HMTD insead with Armstrong's I am pretty sure the HMTD won't explode.

[VX]

I've just come back from the chemist from where I bought some citric acid <img border="0" title="" alt="[Wink]" src="wink.gif" /> , however it's kept behind the counter. When i asked the assistant for it the look on her face was one of real shock, she stood there in silence as if not knowing what to do. Just then the actual pharmacist came running from around the back and asked me why I wanted citric acid!! Although caught somewhat off guard buy this I managed to come up with a story that must have convinced them i was neither a terrorist, or anarchist, and eventually she gave me the small 50g box of citric. Apparently they now have to ask what customers want it for, and must limit its sale....although she wouldn't say why.

This must be some sort of result of the large no. of people arrested recently for trying to make HMTD in this country.

I thought this was worth a mention as they seemed pretty concerned and I imagine that the restriction is country wide. <img border="0" title="" alt="[Frown]" src="frown.gif" />

[nbk2000]

Next thing you know they'll be spraying the orange groves of florida with agent orange (pun) to eradicate "the scourge of citrus".

Lemons will be by license only, with strict sales on this important "precursor".

Lemonade will be banned as being a ready supply of material aid to terrorists.

:rolleyes: :D

[tango]

<a href="http://www-weapons.desert-storm.com" target="_blank">http://www-weapons.desert-storm.com</a> Link to the pic. And that page was don in 2 secs didn't have time for frontpage. So don't call me a Kewl

This was the final colour change, first when all ingrediances were mixed it changed from red to lime green then finally to the dark orange as shown in the picture.
This is an effect of mixing dirty H2SO4 and citric acid into an Hexaperoxide solution.

100 ml of H202
2 Table spoons of Hexamine
20 ml of H2S02
2 Table spoons of Citric acid
And yes i know it was stupid, the the HMTD still worked.

p.s sorry about the way the picture is i had problems loading the page.

<small>[ April 13, 2002, 04:56 AM: Message edited by: tango ]</small>

[vonK]

Hey Tango, is that after you filtered out the HMTD or is it still in there?
If it's still in there it's not much of a yeild.
Also, where did you get the beaker. Is it "borrowed" or did you buy it somewhere?
And where are you getting your H2O2?, if you don't know already hydroponics stores sell 50% H2O2 at $49.00 for 2L.

[tango]

Vonk the HMTD isn't filtered, and yea it was a poor yeild. (i used 6% H202)
I nicked the beaker from the science lab hehe, and i planning on getting alot so if you want buy a few just e-mail me dude.

p.s thanx for the TIP on where to buy the H202 :)

[EventHorizon]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">
I've just come back from the chemist from where I bought some citric acid , however it's kept behind the counter. When i asked the assistant for it the look on her face was one of real shock, she stood there in silence as if not knowing what to do. Just then the actual pharmacist came running from around the back and asked me why I wanted citric acid!! Although caught somewhat off guard buy this I managed to come up with a story that must have convinced them i was neither a terrorist, or anarchist, and eventually she gave me the small 50g box of citric. Apparently they now have to ask what customers want it for, and must limit its sale....although she wouldn't say why.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">I got some citric a while ago, but I think I got a bit much....5# (2,268g). :D LOL HCl works better tho.

As far as wires in the HMTD is concerned, I'....errr....a friend has made some HMTD caps and stored them for over 6 months with no problem. They even taped them to the end of a 4' dowel and struck them repeatedly against a wall until the plastic containers they were in split without setting off the HMTD.

[A_W]

Will wet (not damp) HMTD detonate unconfined if initiated with a small firecracker? I really don`t feel like drying the HMTD completely the first time(s) I make it.

[Zambosan]

I think it's very insensitive to flame even when slightly damp.

<small>[ July 18, 2002, 12:34 AM: Message edited by: Zambosan ]</small>

[vulture]

This could be the decomposition of the hydrogen peroxide. How pure is your hexamine and how old is it? If it has decomposed a little bit, there will be ammonia in the solution which will immediatly start decomposing the hydrogen peroxide.

Also, in which order do you add the reactants?

[tango]

My Hexamine is pure i guess, i got ot from a camping shop.(don't know how pure that is though)The Hexamine is new, they had to order it for me. I think my H2SO4 had small peices of Al in it as i got it from a car battery, that could one reason for the strange colour.

[Zambosan]

Doubt it's aluminum... sulfuric would oxidize the aluminum to Al2S04 (aluminum sulfate, alum) pretty quickly, methinks.

[A_W]

The pieces in your acid is not Al, but probably pieces from the electrodes, wich is lead and lead dioxide.

[S. Toppholzer]

please would answer anybody this question:
I learned that HMTD shouldn't come in contact with metals.
What about the ignition/bridge/lightbulb wire?
Any dangerous substances that could form there that would propagate premature detonation?
If so: How do you handle that problem?

<small>[ April 16, 2002, 01:18 PM: Message edited by: S. Toppholzer ]</small>

[xoo1246]

Metals can decompose HTMD, If enough heat is built up then you could get a premature detonation. Maybe this isn't likley to occur(especially with a thin wire), but it's better to be safe(r) then sorry, right? I would suggest you use some ignition composition around your wire, enclosed in a small (non metallic)container.

[S. Toppholzer]

thanks, xoo - exactly what I thought. Makes me wonder why A-Bomb was so astonished about the way I'm igniting HMTD. A small amount of Armstrong's Powder (extracted from toy caps) in a straw wherin a lightbulb wire is embedded. that piece of straw (leghth approx 1,5 cm) sits inside the tube where the HMTD is. Can't see what's wrong with it. I realized Armstrong's very sensitive when it comes down to friction - but so is HMTD. AS long as I am avoiding this... hell, I carried a bunch of these Armstrong's initial caps (only the straws comlete with the lightbulb wire) in my car for more than a year.

[vulture]

That's it, lead in the solution -> heavy metals decompose H2O2 already in trace amounts.

Why could someone be making all that fuzz about citric acid? In Europe you can buy it in 50- 350g quantities in supermarkets to remove CaCO3 from coffeemachines. My mother uses it all the time for that purpose. Damn, just press a few lemons and pour it into the reaction vessel! :D

[xoo1246]

Sure, both of them are friction sensitive, I have no experience from Armstrong's mixture, but I have heard it's really sensitive(ignites when your snap your fingers with it on them). You could use simple blackpowder in that straw, or like me, take a box of (saftey)matches, hit their heads with a pestle, they fall apart, collect them and then soak them with aceton(to avoid ignition by friction), then grind them up. When it dries you have a easy to ignite powder sutible for your purposes. (potassium chlorate and antimony trisulfide). A large box gives six grams if I'm not misstaken. Those little fellows when sealed propperly explodes instantly when you press the switch and have never failed me (yet).

Edit: I agree with you vulture, it's a sick world we live in when people belive you are a terrorist when you buy citric acid. I have never been asked questions about my purposes when buying any chemicals ever. The only question I got once, was if I new how to handle 35% H2O2 safely.

<small>[ April 16, 2002, 02:31 PM: Message edited by: xoo1246 ]</small>

[Anthony]

According to Improvised Primary Explosives, dry HMTD will react with: aluminium, copper, brass, zinc, antimony, iron and lead.

So nichrome wire (nickel and chromium) *should* be ok, however the copper in the wires you use to connect the bridge will not be. Neither will it be if you use a strand of steel wool for a bridge.

[Zambosan]

That may not be an exhaustive list. I'd just err on the side of caution and assume HMTD reacts with all metals.

<small>[ July 18, 2002, 12:35 AM: Message edited by: Zambosan ]</small>

[xoo1246]

Another possible solution is to dip the wire in NC, although it doesn't really mather.

[Sparky]

The following is a dream
I tried making hmtd about a two weeks ago by Megalomania's synthesis and failed. I was wondering why it didn't work, maybe someone could suggest something?. I made half of the amount on Mega's page. A Long winded, detailed description of what I did follows...(written the day after so it should be accurate in that regard):

I measured out 7 grams of Hexamine (esbit tablets). I put the hexamine in a plastic bag and crushed it in a vice to make a coarse powder so it would dissolve faster. Then I measured 13 grams of citric acid. This is slighly more than called for because I read on The Forum that more acid should be used for making acetone peroxide when the hydrogen peroxide concentration is low, I assumed the same for HMTD. Then I measured out 125 ml of 6% hydrogen peroxide because Mega recommends 50 ml of 30% H2O2. I measured with a large syringe. Then I made a concentrated solution of salt water to make salt-ice cubes out of for my ice bath. I put all the ingredients in the fridge and the salt water in the freezer of course. It turns out the ice bath was around -3 degrees.
Then 2 days later I used a fire extinguisher (it was handy! :) ) and a pot to crush some of the ice (salt water ice crushes easier than regular ice) to give a better contact with the container (a Pyrex measuring cup), then I put the ice in a Tupperware container. I used all clean glass ware in the reaction vessel so there were no contaminants from that area. I nestled the measuring cup in the ice bath and poured the hydrogen peroxide in. Then I measured the temperature at around 2 degrees C. I left the thermometer in and added the hexamine kinda slowly, stirring carefully with my rod so as not to hit the thermometer. When it was all in and I think most of it was dissolved (hard to tell). I added the citric acid slowly. There was no noticeable rise in temperature as I added the acid. I stirred for about seven minutes after all the stuff was added together and noticed no change. There were white crystals floating on top of the mix that I assume were non- dissolved hexamine. I came back three hours later and took the solution out of the bath. It had gone down to around minus 2 C but wasn't frozen or anything. It sat out of the bath in the room for two hours. When I came back nothing had changed except the temperature had gone up to around 13 C. The tiny amount of white crystals were still on top. I filtered them, washed them in a baking soda solution then dried them out. I left them on the coffee filter because there was so little. When I came back today I burned the filters and the white powder melts but does not do anything as the filter smolders away (it does not burn like a normal coffee filter). I think the filter might be smoldering instead of burning because of baking soda on it.

I later tried a procedure detailed by somone who posted about their first batch of HMTD and said it worked. I got some HMTD but unfortunately the procedure used volume measurement.
For even newer newbies than myself that might read this, I have some details on my site (http://pyropage.50megs.com) that will help if you want to make it but I left them out because they aren't relevant in this post.

[vonK]

Did you only leave the solution to react for 2 hours?
If using 6% H2O2 you will need to leave it for at least 24 hours.
Also your hexamine and citric acid should easily dissolve in the H2O2.

It might have been me that posted the procedure using volume.
45ml H2O2.
2 1/2 teaspoons hexamine.
4 1/2 teaspoons citric acid.
Thats the way I always do it (scaled up though) and it has worked every time for about 30 batches.
I keep it in an ice bath the whole time and stir it for half an hour after everthing has dissolved then stick it in the fridge for 24 hours.
Yeild is about two teaspoons.
My next batch however will be made with 50% H2O2 and HCL, I'm wondering if all the hexamine will dissolve in this conc of H2O2 or will I need to dilute it.

Kurt.

[S. Toppholzer]

Buck: I am using 25% H2O2 as well - just the last batch I made up last week wasn't reacting at all - same problem as you had. I took it out of the freezer and added a knifetip full of citric acid. This seemed to have started the reaction.

I always used 35% H2O2 - and the way it seems one needs more acid if you keep the stuff in the freezer. If you'd use the same amounts and put it in the fridge the reaction would surely start. At least that's what I noticed.

@ Sparky:
I am using Esbit, too. The white stuff floating on top of the solution are impurities, aka binder material. Some say it's wax, I belive it's some sort of plastic. Anyway: the best method might be crushiung up just a bit more than the recommended amount of Hexamine coming from Esbit fuel tablets (compensating the amount of filler), adding just al little bit more of the given amount of H2O2 (compensates for loss of H2O2 at the filtering process) and filter the now dissolved Hexamine along with the impurities through a white coffee filter into the reaction vessel you want to use.
Thus you dissolved and purifed pretty easy.

I for my part crush all Esbit bars up at once, add just enough hot water so that all will dissolve, filter it and re-crystallize it by putting the solution into an empty lightbulb which is placed on top of a candle. After a while it starts to boil happily. As soont there is almost no water left on top of the crytals that settle at the bottom, I filter them and put them on a sheet of paper which rests over an enclosed 25W lightbulb. As soon as the Hexamine cake becomes really dry, I crush it up and store the powdered hexamine in a plastic zip-lock bag.

<small>[ April 18, 2002, 01:04 PM: Message edited by: S. Toppholzer ]</small>

[Rhadon]

I also use to make HMTD using Esbit. The impurities are only present in minor amounts, so I didn't remove them at all. Up to now I didn't have any problems with these impurities in my HMTD, but if I ever did I would regard S. Toppholzer's removal method as the best one. Though, I wouldn't adjust the amounts: The amount of hexamine is a bit less than the amount of Esbit, and some H2O2 stays in the filter. Thus it would be easier to adjust the amount of the last remaining ingredient used, which is a catalyst. Since I always use more acid than necessary (I use HCl, with good results) this doesn't matter, too. Adjusting the amounts of chemicals wouldn't be a disadvantage, of course.

<small>[ April 20, 2002, 07:39 PM: Message edited by: Rhadon ]</small>

[S. Toppholzer]

Just yesterday I made another batch of HMTD - it was remarkable.
I had some eight grams of citric acid left and decided to use that. Since the acid crytals were pretty big I had the strange idea in dissolving them in a bit of boiling water and then recrystallize 'em. I found out that this won't work since after almost all of the water evaporated over a low flame, the stuff became like a syrup - like honey.
I poured this syrup on a ceramic platter and after it cooled, I crushed the stuff up until it was like face powder. I was heating this stuff in an empty light bulb so I decided to leave the acidic residue inside, added 35% H2O2 to it plus the rest of the powdered acid. The whole process was somewhat strange because I didn't do any calculation regarding how much H2O2 or hexamine I would have to add. Just did it by guessing. After the citric acid dissolved, I slowly added approx. 12 or 13 grams of hexamine. Initially, I didn't cool the mixture while adding the hexamine. After a while though I realized it was getting somewhat warm, so I put the vessel in an ice/salt bath to dissolve the rest securely. After about fifteen (!) Minutes, lots of crystals started to percipiate (sp?) and just to be sure that this wasn't unreacted hexamine I added a small amount of H2O2. The crytals dissapeared for another ten minutes and reappered then. I decided just to put that stuff (the ice in the icebath bas already melted) in the fridge (approx 4°C). Two hour later I checked again and to my utter astonishment there was almost no liquid left in the lightbulb which itself was half filled of HMTD!
I just sucked up a little bit with a plastic syringe, washed with water and bicarb, left it to dry. Upon touching the dried HMTD with a burning cigarette, it went off extremely fast.
I washed the whole stuff twice with water and then with a bicarb solution and put it into the glass bulb in some water wher it rests now. I had some loss - but the bulb ist still almost half full.

My only question regarding my strange making of HMTD:

How dangerous is mixing the reactants together without properly measuring them?

[10fingers]

*

<small>[ May 09, 2002, 01:20 AM: Message edited by: 10fingers ]</small>

[Rhadon]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">HMTD is slightly more powerful than AP...</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Is it really? At least the detonation velocity of AP is slightly higher than that of HMTD, if I remember correctly. Perhaps this is just a question of how you define "powerful".

[Madog555]

by power he means the amount of gasses produced by it. for example ethly nitrate has a high VOD but is not very powerful at all, and PETN is more powerful than RDX but has lower VOD.

[0EZ0]

An explosive with a high VOD has a more shattering effect. That is why ANFO with a low VOD of around 3500/4000ms (depending on density of charge) has a heaving effect and is perfect for earth-moving applications.

[10fingers]

*

<small>[ May 09, 2002, 01:22 AM: Message edited by: 10fingers ]</small>

[Celtick]

On Mr Cool's site I found these ratios for HMTD manufacture with HCL:

225mL of 6% hydrogen peroxide solution,
150mL of 15% hydrochloric acid,
20g of hexamethylenetetramine,

Since I have 32%HCL and only 3%H2O2 I converted the ratios to:
</font> <font size="2" face="Verdana, Arial, Helvetica"> H2O2;
100 ml of 3%= 3ml h2o2
225ml of 6%= 13,5ml H2O2
---------> 450ml 3%= 13,5ml H2O2</font></li> <font size="2" face="Verdana, Arial, Helvetica"> HCL;
150ml of 15%= 22,5ml HCL
---------> 150/(32/15)= 70,3125ml
70,3125ml of 32%= 22,5ml HCL
</font></li><font size="2" face="Verdana, Arial, Helvetica">Can anyone tell me if these ratios will work if using the same amount of hexamethylenetetramine :confused: , or will the concentration of H2O2 be too low for a decent reaction?

<small>[ April 28, 2002, 05:09 PM: Message edited by: Celtick ]</small>

[00Buckshot]

I never use a scale nowadays. I just add plenty of H2O2 (35%) about 50ml. Then after I mix in the hex, I mix in about twice that amount of citric acid. The reaction never works for me if I leave it in the freezer. Maybe if I leave it in the freezer for a couple days it would work, but I just use the fridge.

I want to try the Hcl method because it would be easier to mix compared to citric acid. But I wonder "if" someone was in a situation where they couldn't wash the HMTD, which acid would be safer?

In my tests I noticed a HUGE difference in "power" depnding on how dry the HMTD is. I place my wet HMTD on newspapers to speed dry it. I don't use the methanol. Just change the wet newspapers every 20 minutes or so and it will be dry in a few hours. But there is a big difference between "almost" dry HMTD, and "bone" dry HMTD. Example for me is a filled a film container with almost dry HMTD, and it blasted the bark off a tree, but thats it. Then with fully dry HMTD I destroyed a similar tree with half the amount of HMTD. The slightly damp stuff apeared dry to the touch, but it pays off to make sure it is 100% dry. If its not 100% dry it is still much more powerful than black powder, but the dry stuff will fully detonate. I wedged the corner of a paper triangle salute into a rotting stump and blew it apart with about a gram of dry HMTD. Im rambling.

I read somewhere in the ftp or maybe it was that rec.pyro forum that a mix of 50:50 HMTD/AN will work pretty good. Anyone tested this? Or would it just be better to use the HMTD as a cap to start pure AN or some AN mix? I was planning on a film container full of the 50:50 mix, I figured it would be more stable then pure HMTD, but would it be more or less powerful?
Thanks

[A_W]

I have finally got my hands on some H2O2. I found it on a pharmacy, and the lady who worked there was very friendly and not suspicious at all. She said that they had 3%, 6% and 10%. I was not sure what to buy; 6% or 10%, but I bought the 6%, since it is the most common to use (except from maybe 30%)

Anyways, I have now started the manufacture of my first high explosive ever; a small batch of HMTD! (all of my newbie questions lately have finally payed off!!) Since this is the first time I make such an explosive, I cut the ratios down, and the recipe was not followed exactly.

The original ratios are follows: 9 teaspoons 6% H2O2, 4 1/2 teaspoons of citric acid, and 2 1/2 teaspoons of hexamine. (yes, I know: volume bad--weight good, but I don`t have a scale, and teaspoons are so much easier! A proper teaspoon is about 5 ml. I have small plastic spoon used to measure spices, wich is 1 ml. I used this one in stead of a teaspoon to cut down on the amounts. I used 4 1/2 "spice spoons" (not sure what they are called) of citric acid, 2 1/2 of hexamine and 9 peroxide. According to my calculations; this would yield approx. 2 ml of HMTD, wich is perfect. Yes, I am aware that this will be a very small batch of HMTD, but this is exactly what I want.

All of the additions went really well. When the temp. had fallen to 5*c, I found that it would be safe to start adding the hexamine. At first, I was really nervous, and added it in REALLY small portions. I stirred with a thermometer, and what I noticed was that the temperature was actually falling. Even when I started adding the acid, the temperature still kept falling.

For an ice bath I used a plastic container with a lid. The reaction vessel itself was an ordinary glass bowl. The ice-bath was filled with 1 litre of crushed ice and some water. It is now about 40 min. into the reaction, and the whole thing is being kept outdoors. The temperature is still around 2-3*c.

I`ll take pictures, but since I don`t have a digital camera, I may not get to post them ever. Any tips or comments on my little project? I can`t wait to test the final stuff!! :D

<small>[ April 28, 2002, 02:23 PM: Message edited by: A_W ]</small>

[A_W]

I just woke up this morning, and went out to check my reaction. Success!! White HMTD is lying on the bottom of the reaction vessel. :D And this was after only 11 hrs. I think I`ll leave it for a few days to get maximun yield.

[mr.evil]

what will happen if you light a 3metre or more?(organic peroxides) would it just burn with an enormous speed, or will it detonate?

maybe a nice test :) anyway, i will do something with detcord.

[S. Toppholzer]

I made another batch of HMTD - again.
Funny - if I melt the citric acid first and then dissolve it at room temperature with H2O2 and then adding hexamine in tiny batches slowly the crytallisation process sets in within ten minutes. I also found out that the yield seemingly isn't affected if I store the finished mix afterwards in a fridge or leave it at ambient temperature.

This time though after completely drying the HMTD, I found out that its burning speed is considerably lower than average. I guess there's still some unreacted hexamine in it.
Would it be dangerous mixing up another H2O2/citric acid mix and add the powder again to react the leftover hexamine?

Talking of det. velocities - could HMTD be used for making a shaped charge or is that substance's det. velocity too slow for that?
Would HMTDAN work for that? I somewhat doubt it.

<small>[ April 30, 2002, 05:03 AM: Message edited by: S. Toppholzer ]</small>

[Demolition]

HMTDAN will work for shaped charges.Have a look in the ANAP thread,Yi has a link to his website where he tested a shaped charge using HMTDAN with good results.

[S. Toppholzer]

Hey, thanks!

[A_W]

When I had filtered out the HMTD, I thougt; what the hell. I`ll just pour some NaHCO3 sol. into the funnel with the HMTD still in it.

It bubbled over in the funnel, and I lost the small amount I had managed to filter out. Damn! :mad:

However, this was due to my own stupidity. I have now started my second batch, wich I have to find another way of neutralizing.

[mr.evil]

i just wash my HMTD,i never neutralize it with NaHCO3. Never had any problems with it.

[A_W]

Yes, that sounds alot easier and quite tempting, but earlier in the thread, someone said that the explosive will be very sensitive and unstable if not neutralized properly. I think I`ll stick to neutralizing it until I have some experiance with the explosive.

[00Buckshot]

To neutralize I use the coffee filter as a tea bag, and just hold under the tap for a minute or so, then I dunk the tea bag into the bicarb mix a few times making sure that all the bubbles stop. Then I hold it under the tap again for a minute.

[A_W]

Thanks alot, 00Buckshot! Great idea! :D I never would have thought of that. My HMTD has now been reacting for about 30 hrs, and there is a large amount (compared to the small amounts of HP/Hex/CA I used) of white powder in the reaction vessel. I will try your method when the reaction has completed.

[A_W]

I have now filtered out the HMTD, and neutralized it (again, I wish to thank 00buckshot for the very good method). I have done some small tests, by putting some (approx 1-2 match-heads) of the MHTD/water paste on a long broomstick. The paste is left to dry. Then, the end of the broomstick is slammed agains a wall. It made a loud crack. The wet HMTD burned like nitrocellulose when ignited unconfined.

[kingspaz]

A_W, 'I think I`ll stick to neutralizing it until I have some experiance with the explosive.'
that seems to imply your not going to neutralise it when you have experience. just make sure u allways neutralise it. that way you'll live to 60 and have all your fingers!

[vonK]

A_W, your HMTD sounds rather impact sensitive (to me anyway).
When I make HMTD it won't go off due to impact while it is still wet, and even when it is dry it takes one hell of a thump with a hammer on a brick, more often than not the brick breaks before the HMTD does.
I'd like to know other peoples experiences with HMTD's impact sensitivity.
Just for the record, I personaly never neutralize my HMTD (I use citric acid) and have never had any problems with accidental ignition, I just rinse it with tap water and meths.

[Zambosan]

I'd imagine even a small rap with a hammer would set it off! Organic peroxides are notoriously sensitive in all the literature.

<small>[ July 18, 2002, 12:37 AM: Message edited by: Zambosan ]</small>

[A_W]

Thanks kingspaz. From now on, I will always neutralize my HMTD properly.

When neutralizing the previous batch of HMTD, I dipped the filterpaper into the NaHCO3 bath, but had to hold it there by hand. This took very long time, so I figured that the neutralization was only necessary if it was to be stored over time, so I aborted the neutralization process after a few minutes, while it was still acidic. I don`t know if this made the explosive more sensitive, or if it has to go some time.

vonK: The HMTD was left to dry, until it was only a little moist (much of the water was absorbed through the wooden stick). The stick was slammed pretty hard to a concrete wall, so I (but I don`t know much about primarys) don`t find it very sensitive, for a primary that is.

Today I tried to detonate a larger (but still a small) amount of HMTD. The paste was poured on a cardboard sheet, and left do DRY COMPLETELY. I put a fuse on the explosive, and another cardboard sheet over that, wich was pressed GENTLY on the explosive, and attatched with some tape. I figured that this would be enough confinement, so I went up into the woods, lit the fuse, expected a boom that never came. When I went to check, I first thought that the fuse had gone out, but I found all of the HMTD to be gone. The charge seemed to have to little confinement. My next charge will probably be loaded into a small cracker. Can the HMTD be loaded into the cracker when still wet?

Finally; can someone tell me how much in teaspoons 1 gram of HMTD is?

[kingspaz]

A_W, there is not answer to that question. HMTD is a powder so has a variable density since it contains air spaces. compressed HMTD weiging more per teaspoon than uncompressed HMTD. this means everytime you take a teaspoon of HMTD it will be a different mass.
you really should invest in some cheap scales or make a mass balance which i've been told can be made to measure very accurately.

[A_W]

Oh, I see. I have thought of that, but I never thought it would make that much difference if it was pressed or not.

The reason I asked, is because of a picture from the makeshift arsenal. It showed the massive damage done to a metal bird feeder by a 2.5 gram charge of HMTD. As I don`t really know how much 2.5 grams is, I wanted to know how much of the explosive needed in volume to make such damage. A rough estimation would be good enough.

[kingspaz]

ok, according to chemistry of powder and explosives its density after being lightly tapped is 0.66g/cm^3 therefore i would expect the loose powder to be around 0.5g/cm^3.
one level table spoon is about 5cm^3 so:
0.5*5 = 2.5g
so its about one level table spoon full of HMTD or 5ml.

[A_W]

Thanks kingspaz. If that damage was caused by 1 tablespoon, I`d like to set off a full coke-can of HMTD :)

Today, I filtered out another batch of HMTD. (the explosive is so easy to make, it has become nearly routine to make it every 2-3. days)
Anyways, I did some (routine) impact tests with the good old broomstick. A quantity the size of half a pea, made a deafening bang (when I was 1 meter from it). Then I decided to try to set some of it off with a fuze. I poured a pea-size (maybe slightly larger) pile of HMTD paste on some duct-tape, inserted a fuze, and left it to dry (not completely though). I wrapped the duct tape around the explosive, and went up into the woods to set it of. I tried this procedure twice, without any detonation. What did I do wrong? Does it have to dry completely? (it was as dry as the explosive set off with the broomstick, wich again was damp) Is duct-tape not enough confinement?

I have now used up all of my HMTD, so I guess I`ll have to start another batch now.

[Anthony]

It's because it's harder for the HMTD to make the deflageration to detonation transition when it is wet or damp.

To get an idea of how impact sensitive it can be, try metal-on-metal. Place the sample on an anvil, thick steel plate etc and tap it with a hammer. It only takes a drop of a few inches with a regular hammer to detonate the sample in this fashion.

[kingspaz]

don;t set off a coke can full! thats insane. all it takes is the can slips out of your hand and your missing half a leg.
keep using small amounts but don't get careless.
i think the reason it didn't go off would be because it was damp. its still impact sensitive when damp but like anthony said it cannot make the deflagration (burning fast like BP) to detonation very well when like this.
dry it out completely and pour some into a thick walled card tube...say 3cm long and 1cm wide. also the addition of a small amount of black powder where the fuse meets the HMTD will aid initiation.

[xoo1246]

Remove

<small>[ December 11, 2002, 01:03 PM: Message edited by: xoo1246 ]</small>

[A_W]

Thanks xoo1246. I will try that, probably tomorrow when the HMTD has finished reacting. What about just putting a fuze directly into the cracker itself, instead of heating it with blackpowder from the outside? This would be more practical if the charge was to be placed into a hole or something.

Aluminum foil is aluminum pressed to a very thin sheet. Some of the aluminum reacts with the air, producing a thin layer of Al2O3 coating the aluminum foil, if this is what you ment with aluminum oxide. Will this be completely safe to use with HMTD? (metals+HMTD=bad,
metal oxides+HMTD=?)

I have thought of drilling a hole into a piece of wood (or a tree), filling it with HMTD, fuzing it, and put some duct-tape over the opening. I think I will try this, after some experimenting with xoo1246`s crackers.

If you go to the June 2001 Archive, and look up a topic called:
"A Big charge of Ap", some guys have set of AP charges as big as a full coke can, and even as much as a pound <img border="0" title="" alt="[Eek!]" src="eek.gif" /> (I belive the power between AP and HMTD is pretty much the same). I don`t plan to do this, as it is not worth the risk to me.

[kingspaz]

A_W, make sure you use the foil crackers straight away. with storage the HMTD will react with the aluminium (dispite the Al2O3 layer)....or maybe it react with the layer too...fuck knows!....but it does react. so use them within a few days!

[Zambosan]

I used to enjoy scaring the crap out of my college roommate by placing a couple of toy caps on a stovetop burner, and turning it on low. Gives you just enough time to nonchalantly walk out the door. I placed a quarter on top of one once just for shits 'n giggles, and it accelerated the center of the quarter so fast it deformed it into a shallow cup shape. :D

<small>[ July 18, 2002, 12:18 AM: Message edited by: Zambosan ]</small>

[0EZ0]

Lol. Zambosan, that'd scare the shit out of me. Especially since i'de be wondering whether or not it was a stash of assorted pyro\explosive stuff going off :D . Hehehe.

With the Al foil idea, i used to experiment with lead styphnate that way. Depending on the amount of foil you've wrapped it in, you get quite a delay. :p

[A_W]

I`ve just set off a pea-sized quantity of HMTD wrapped into some duct-tape. It detonated, but not very loud or powerful. The HMTD was completely dried this time (I flame-tested a small pile unconfined, MAN that burned fast!)

I`m pretty sure that if filled into a metal-casing, the HMTD will detonate much louder. I`m very tempted to fill some into one of those very small cartridge casings (.22), but I don`t know how long it will take the HMTD to react with the brass. Will it, like aluminum, react over a few days, or will it, like I`ve read on another page, react very fast? Because aluminum is much more reactive than brass, I think it will be quite "safe", but I`d like to hear some opinions first.

[Anthony]

Unlikely to happen. I've loaded HMTD into Al tube and 22LR casings before with no problem, but they were used immediately. This isn't to say it's safe though, remember the story about the guying making a HMTD COB which reacted and heated up as he was filling it.

Generally speaking though, casing doesn't make a lot of difference to HE explosions. Pea sized isn't a lot of explosive, probably half a gram or less. You won't get a boom from this, more a sharp, high crack/bang. I'd recomend a small carboard/plastic tube, or small plastic container (film canister, little bottle, bottle cap etc) with a few grams of HMTD in it. That should give a more impressive effect.

[A_W]

Thankyou Anthony, I will try a .22 shell.

If you check out the makeshift arsenal, there is a picture of a .22 magnum shell of HMTD, detonating in a toy car. The detonation looks pretty powerful. MAGNUM, simply means that the shell is a little longer (not much). I don`t know how much HMTD (in grams, unpressed) will fit ino a .22 shell though.

[Anthony]

You should be able to get 0.75-1gm in there. Be careful and try to avoid holding the brass directly, hold it still in pliers/vice etc and carry by the fuse when complete. Might seem a bit OTT, but better safe than sorry afterall.

[A_W]

I`ve been thinking of making a HMTD plastique by mixing it with a small amount of mineral- or soy oil, if this is possible. This has been discussed before (in the archives), but I still have some questions (wich may sound a bit stupid):

Will this still be a primary, and require confinement to detonate (in small amounts), or will it detonate unconfined when initiated with a small detonator? How sensitive will this be? Will a small firecracker make a good "detonator" for this?

[kingspaz]

A_W, the mineral oil and HMTD makes a crumbly mix which makes a very hot burning incedary mix which must be lit with a naked flame. it is no longer fuse sensitive although still a sensitive mix. therefore it must be initiated with a cap under confinement to stop the stuff scatering although i haven't actually tested it as a secondary.

[Zambosan]

It would probably be less spark & flame sensitive, but treat it as sensitive!

<small>[ July 18, 2002, 12:17 AM: Message edited by: Zambosan ]</small>

[A_W]

I have now done some (successful) testing with HMTD. It was filled into .22LR casings.

I first filled one slightly more than 1/4 of the casing. It went off as loud as a firecracker, but it sounded different (more of a cracking sound). The casing was ripped open.

Another was filled almost 1/2, and taped to a not so lucky plastic soldier, wich was split in half :D This was made into a shaped charge, wich proved to be very effective.

The last test was a casing filled almost 3/4 to the top. I did this one right outside our house. The bang was very loud, and the casing was totally deformed.

Conclusion: The tests were successful, and I will never touch blackpowder again :) In my next tests, the charge probably will be placed inside a piece of wood.

I really have no place to set of big things, but in the summer, I will go to my grandparents. Huge, endless areas of forest :D

[xoo1246]

Don't use brass, if you are unlucky you will injure yourself. Al foil is safer(but not safe at all) since it's coated with oxide or other coating. As kingspaz said, they should be used instantly.

There is no need to use metalic shells(not even Al), the confinement from a plastic straw is often enough if sealed in the ends.

This guy loaded HTMD into a shell containing copper. Obviously he didn't know about metal incompatibility.

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">
Well At the July of 1989 It happened, I was damping HMTD into a .22
LR copper cartridge, with a standart match, you see holding that
cartridge in my left hand ,when it suddendly detonated, A HUGE explosion,
and I found that for some reason, my hand was bleeding abt 1/2 liter
of blood per min ( 1/9 gallon per min ) , and I could see my bone
'shining' through scraped human tissue.

Epiloque. Never NEVER load B-caps in your hand, Always use special
tamping device when loading Blasting caps - any other use for HMTD is
silly - Believe me, I had hitted HMTD with a Hammer, It didn't
detonate, and now, when I try to load that stuff from same batch into
a copper container, It detonates, even I press with maybe 1/2 kg
( = 1 pound ) force it.
Maybe the batch was impure, but believe me, It really explode
without no reason. I must say that HMTD is a good explosive, but It's
truly unpredictable. I'm sure that there are many others in this
newsgroup who can tell the same thing - months of hard handling, and
then, a explosion by a minumum force.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">

[A_W]

Yes, I have read that one before, and it did give me second thoughts about .22 shells (any shells).

The nice thing about high-explosives, is that the confinement isn`t really that important. If it detonates, it detonates, and you don`t need that strong containers. LE charges seem to increese in power along with the strenght of the container. (a cratermaker with 1 tablespoon of BP is much louder than a cardboard cracker with 3 tablespoons)

Drinking-straw you said? Good idea. No metals, no shrapnel, and easier to obtain. Will some duct tape at the ends be enough confinement? I will test it tomorrow anyway. I just filtered out my last batch of this wonderful explosive :) .

********************************************

I`ve just returned from my "testing grounds" under our front porch. I tested the drinking-straw idea. I filled a fuzed piece of the straw with HMTD and tapped it to make it more dense. The charge was placed under a plastic bucket. The piece of straw was no longer than 3 cm long.

I just have to say: OH MY GOD! That shit was powerful! I was standing 2 metres from it (holding my ears of course). I could feel the shockwave (not sure if this is possible with such a "small" charge, but it felt that way). My ears hurts like hell!

The bucket layed 1 meter from where it had been placed. I picked it up, only to discover that it was split almost in half, barley hanging together!

This is just as good as metal-containers, and much more safe. I underestimated the power of this explosive. My next test will be carried out in the woods.

<small>[ May 15, 2002, 09:59 AM: Message edited by: A_W ]</small>

[andreas]

A little question more on topic again.
Just to get things straight:
The reason to cool the hmtd reaction is to reduce reaction rate so you will not get a run a way reaction, am I right?
This I can imagine will not be a problem with 3% peroxide because of the cooling effect of al the water present.
a bit of feedback would be nice.

[A_W]

You`re probably right; low conc. of H2O2=low temperature rise. But I think that an ice-bath still is a good idea with 3%. I use 6%, and the temperature rises quite much, if I add larger amounts of the hexamine at the same time. Not using an ice-bath, means that you`d have to add the chemicals slower, wich really is boring work.

You could try not using a cooling system, but I don`t reccomend it.

[andreas]

whell I have made 2 batches without cooling an as far as stability goes have found no negative effects. This would be due to the non-existence of isomere's of hmtd(right?)
A bit off topic but when making tnp with h2so4 and nh4no3 why doesn't the tnp form ammoniumpicrate. I would expect this due to the free ammonium-ions present.

[Zambosan]

That's a good question, andreas, I'd like to know that myself - I have no direct experience. Ammonium picrate is formed by reaction of TNP with ammonium hydroxide, which is a base. My guess is that since the H+ and OH- ions titrate to form water, this leaves only the ammonium and the picrate ions, so they re-associate when the liquid is evaporated. Without the OH- ion eliminating the H+ ion, the picrate ion would be happier retaining it's H+ ion, as it has a stronger charge than the NH3+ ion. Feel free to critique and flame, this is just conjecture. :D

<small>[ July 18, 2002, 12:21 AM: Message edited by: Zambosan ]</small>

[andreas]

Whell I think I can live with that you made one fault by including a NH3+ ion. But the rest must be okee another suggestion might be some sort of reaction that tnp just is a little less soluble than dunnite and precipitates easier. Like what we call a neerslag(downfall) reaction. Just like adding sodiumsulphate and and calciumchloride.

Come to think off it this must be crap since then there would be no chance dunnite could be made with ammonium a whell I had a couple of beers so don't flame me for such a stupid suggestion

Whell today I thought about it and I think I found the solution. To free the nitrate from the ammonium ion it reacts with with the sulphuric acid to form sa sulphate witch isn't a strong enough base to react with the tnp.
same thing with potassiumnitrate why shouldn't it for potassiumpicrate because it forms potassiumsulphate first and this dissolves in water but doesn't react further.

<small>[ May 18, 2002, 07:14 AM: Message edited by: andreas ]</small>

[Zambosan]

DOH! NH4+, sorry. I seem to always be mixing my ammonia and ammonium... :p
Anyways, sulphates must be much more water-soluble than the TNP, no? Or wouldn't a substantial amount precipitate out with the TNP upon crash-cooling in an ice bath?

[nitriees]

I experience the "overhit" problem 3 times out of 5 times I try to
make HMTD.
I use 200ml H2O2 ( 38%), 4 tea spoon Hexamine and 5 tea spoon
citric acid as experiment try.
I mix this stuffs under ice bath and seems no reaction happen and
the solution is below 5 degree celcius, I left it in ice bath for
5 hours and taken out to room temperature after that. No reaction
within 30 minutes. I go out to work.
When came back after 8 hours, the solution already boiled to half
of original volume, found some HMTD still sticked on outside the
biker.
Anybody know what is the cause of it, is it more Hexamine put in
caused the overhit or not long enough keep in ice bath?

[A_W]

I think that your ratios are wrong. I use 45-50 ml H2O2, 2 1/2 ts hexamine, and 4 1/2 ts citric acid. And my H2O2 is 6%. I belive that your amount of H2O2 is way too much.

I'm not sure if this is the source of your problems, but that's one of the mistakes I see. Try my ratios, and see what happens.

If you mean "overheat", the reason is simply that you remove it from the ice-bath. Keep it in there at all times! Especially with your high conc. H2O2. Try adding the hexamine slowly, as that is the chemical that reacts forming heat. Not the acid. (At least not when I make it. I can add all of the acid at once without any rise of temp.)

[Zambosan]

I think if the reaction vessel is kept too cold, the reaction will not start.

<small>[ July 18, 2002, 12:23 AM: Message edited by: Zambosan ]</small>

[S. Toppholzer]

I think the type of reaction vessel is crucial in order to prevent a runaway reaction. I made many batches of HMTD and haven't had any such reaction yet - even though I use 35% H2O2 and mix the ingredients at room temperature. Sometimes the stuff got somewhat warm and placig it into a salted ice bath immediately put it back to normal temperatures. A good thing is that the forming of HMTD takes usually not more than one hour.
My reaction vessel: A clear, empty light bulb with tne metallic threads around its neck removed.

[00Buckshot]

I find the freezer to cold, and room temp is to hot.

I used to get over heated reactions often, and it destroys the yeild.
But I have a system down that works well for me, and I use 35% H202. I think the 35% H2O2 is much more prone to over heating.
I pre-chill each chem in the freezer, then mix them and keep it in the freezer for a half hour or so, to keep that initial warming down. Then I put it in the fridge. Why use the ice bath, if you have a fridge? Its not like its gonna blow your fridge apart....hehe. The reaction starts within a few hours and works great.
And I found a great hexamine fuel tablet. For all you Esbit users out there try other brands. This box is black and has absolutely nothing on it but the words fuel tablets and made in China. No wax at all. If your not sure just smell it.

<small>[ June 13, 2002, 11:23 PM: Message edited by: 00Buckshot ]</small>

[nitriees]

Thank you for all of yours suggestion and information. Now l have better understanding.
Last night, I try again to make HMTD with dilute 5 tea spoon Hexamine
into 150 ml H2O2 (38%) by using a glass bottol with plastic cap.
Taken in and out from ice water to maintain the temperature below 25
degree celcius.
Add citric acid by everytime one tea spoon and shake the solution
vigorously. Until the reaction start, put into ice water once I saw the HMTD crystal start to form.
Left this for 5 hours, the yield is the most l ever get before but seems like more acid need to used.
Most of the HMTD is float on above,arround 80%. Is it any different
between this 2 stuffs in term of characteristic?

[Arkangel]

Mega's lab says you should stir for 3 hours or so, while keeping it cool, but a lot of folks seem to just leave it. How important is the stirring?

I was thinking about using one of those little battery operated drinks mixers mounted on a frame, with some kind of plastic or glass stirrer. Those of you without magnetic stirrers, how do you manage it?

[Zambosan]

The dimensions of the container will have quite an impact on the thermal transfer characteristics and thereby the conditions under which thermal runaway will occur.

<small>[ July 18, 2002, 12:24 AM: Message edited by: Zambosan ]</small>

[A_W]

I agree with you Zambosan; an ice-bath is the best thing. A fridge sounds fine, but the problem there is that you'd have to mix the chems. at room-temp. When adding the hexamine is (in my experience) the step that emits most heat. Therefore, the chems. should be chilled when mixing, not after. This is just what I prefer.

If kept in an ice-bath, I don't find stirring very important. I just stir until all of the chems. are dissolved, and leave it in the ice-bath until the reaction is complete, occasionally checking the temp. the first hours.

[Celtick]

I know that the synthesis procedure for HMTD has been discussed many times, but here is a personal problem. I tried to make HMTD yesterday, but after more than 24 hours there are still no crystals formed in the reaction vessel. Here is my procedure;
I dissolved my Esbit tablets in distilled water and filtered off the wax binder, I boiled off the excess water and dried the white crystals.
I mixed 100ml of 10%H2O2 with approx. 10gr of Hexamine. And added 50ml of 32%HCL, the temperature raised to about 30 degrees Celsius (I mixed all the chems in a ice-bad). I left the solution in the fridge and stirred occasionally. Now after more than 24 hours no crystals have formed, what is the problem: did I use too little quantities or is the temperature too low? (There are also many little bubbles on the inside of my plastic reaction vessel)

[kingspaz]

i don't knowthe correct ratios but to me that looks like too much acid as i'd say you only need around 25ml.

[Anthony]

Within the next day or two, I'll be posting a synthesis of HMTD with pictures of each step. It might be of some help to you.

[Rat Bastard]

I usually make my HMTD with 6% H202, but a while ago I obtained some 30% H202, and tried that.

My problem? Even after 2 days I got a crappy yield (pretty much the same yield as the 6%)

(I used mega's recipie)

Anthony, what % of H202 are you using in your detailed pic synthesis?

<small>[ July 15, 2002, 10:53 PM: Message edited by: Rat Bastard ]</small>

[KinePak]

DO any of yall know if you can use that Trioxane shit, casue thats the only thing i can find around here, i mean i can order the hexamine, but if the trioxane is the same, can someone let me know thanks alot

[A_W]

Trioxane (or metaformaldehyde) is not the same as hexamine (or hexamethylenetetramine), and I therefore assume that it cannot be used for HMTD.

[Celtick]

There still aren’t any crystals formed, I left it out off the fridge now for approx 20 hours. I finally got a supplier that sells me 30%H2O2 and I placed an order last week so that should be delivered next week, but since I’m going to Spain Monday, there will be no experimenting for about three weeks.

<small>[ July 16, 2002, 01:44 PM: Message edited by: Celtick ]</small>

[S. Toppholzer]

yesterday I wanted to make some more HMTD. This time I didn't have any scale at hand and I thought I'd give it a try anyways. So I took some H2O2, added quite some citric acid and a good helping of Hexamine and mixed it at room temperature - close to an ice bath in case it should get more than lukewarm. It didn't.
At first everything seemed fine and some HMTD fell out. Since the amount was pretty shitty I thought I'd give it more time and let it sit overnight. This morning though even the HMTD already formed was gone again! Too much H2O2?

[Flake2m]

I am making some HMTD, I have just mixed Hexamine, citric acid and 6% H2O2 togther in a glass jar. I am waiting for it to precipate.

I am not sure of the exact masses of the chemicals mixed, as i dont have access to a scale :( . I believe it was something like; 100ml of 6% hydrogen peroxide, about 5g of hexamine and roughly 25g of citric acid. I put a few ice blocks in the jar to keep it cool. My method descibed is kewlish, but this is my first batch of hmtd so I have much to learn about its synthesis.

I have a few questions on the synthesis :confused: ;
1. Currently my experiment is a colourless and odourless liquid with a few white specks, and has been for the past 3 hours. Is this unusall?
2. Is it nessacary to keep the temperature at 0C to get the greatest yeild? My mixture is quite cold but not at 0C.
3. Does the amount of citric acid added in affect the yeild, I have added too much citric acid so will this affect the experiment?

[Anthony]

I used 6% H2O2.

The thread is here:

<a href="http://www.roguesci.org/ubb/ultimatebb.php?ubb=get_topic;f=2;t=000441" target="_blank">http://www.roguesci.org/ubb/ultimatebb.php?ubb=get_topic;f=2;t=000441</a>

[lucifer]

I tried to detonate some ANNM in a bottle under water, but the detonation failed.
The detonator was made out of 3 gram HMTD and 4 gram PETN, a 1N4148 and some perchlorate / sugar and sulfur mix to get the detonator ignited electrically from the 1N4148.

I did tried to detonate the bottle twice.
The first time i heard a small explosion and after the recovery of the detonator i saw that the HMTD was only partial gone . And the PETN was still there.

On the second attempt again a small explosion and now all the HMTD was gone but the PETN was still there.

After this I tested both the HMTD and PETN from the same batch and there was nothing wrong with it.
So why didn’t it work with the perchlorate / sugar and sulfur mix ?

I’m quite sure that the HMTD didn’t got wet.

Is it possible that the HMTD didn’t detonated but only burned very fast, because it was ignited from a very low
temperature? (the perchlorate sugar mix)

[Celtick]

Today I dreamt my new HMTD experiment. I dissolved 7 Esbit tablets into boiling distilled water; I filtered the wax binder off and boiled the excess water off. I dried the Hexamine crystals for more than 24 hours.
I cooled 40ml of 30%H2O2 and mixed it with the hexamine (the reaction vessel already placed into an ice-bad). I measured out 70ml of 32%HCl and poured in 5ml at a time.
First the solution was slightly salmon coloured, after approx. 10ml of HCl the solution turned plain again and after 35ml it turned salmon again. After another 5ml, crystals started to form rapidly and I stopped HCl addition.
Since all my ice was melted at this time, I put the reaction vessel plus ice-bad into the refrigerator (after each addition the temp raised rapidly).

After my solution has cooled a bit I will add the other 30ml of HCl and let it stand for a while.

[Celtick]

After an hour a thick layer of HMTD crystals was floating on top of the solution, there were also crystals floating around at the bottom. I dried some crystals that stuck on my thermometer; they ignited with a very rapid and impressive flame. I poured the other 30ml of HCl into the solution (in portions of 5ml at a time). But after another hour al my crystals disappeared! <img border="0" title="" alt="[Eek!]" src="eek.gif" /> Now, two hours later, I only have a clear solution left :( . I shall wait another 12-24 hours before my final conclusion, but it seems to me that there was too much acid, it seems that 40ml should have been enough.

[drshneb]

I've been looking at alot of different methods for hmtd and decided to go by heart,
I used 400ml 6% H2O2, 24g hexamine and 37.5g of citric acid. 16 hours has gone by with minimal amount forming. I have kept the solution fairly cold untill this morning where i put it at room temp which is when the hmtd started forming. Last time i synthesised it i left it at room temp constantly and precipitation started much earlier than this batch, the only difference was i scaled this new batch up. Can anyone explain how by going against the advice to keep it in the fridge could actually help the reaction? maybe it has something to do with the citric acid reacting endothermically?

and if you can see something wrong with this mixture is there anything i can do to save it or increase the yield?

[kingspaz]

the idea is this:
mix the reactants and leave them for 30 mins or so to REACT. then put it in the fridge to cool the solution. this will result in a decrease in solubility of the HMTD so the maximum amount will precipitate out from the solution.

try leaving the mixture at room temp for 5 hours then cooling overnight in the fridge.

[Macgyver]

Originally posted by kingspaz
the idea is this:
mix the reactants and leave them for 30 mins or so to REACT. then put it in the fridge to cool the solution. this will result in a decrease in solubility of the HMTD so the maximum amount will precipitate out from the solution.

try leaving the mixture at room temp for 5 hours then cooling overnight in the fridge.

HMTD is pretty insoluable in *anything*....

Soluability for HMTD in 100g of solvent at 20 degree celsius.

Water - 0.1g
Ethanol - 0.01g
Diethylether - 0.017g
Carbondisulphide - 0.01g
Carbontetrachloride - 0.013g
Acetic acid, 100% - 0.14g
Chloroform - 0.64g
Acetone - 0.33g
Ethyleneglycoldiacetate - 0.9g

(Soluability data taken from Swedish Infomania "PYROKEMI 2000", and since I know the guy who did this research I also know the results are from a reliable source....).

The point is that you do not need to put it in the fridge unless you care about loosing a fraction of a gram or are using vast amounts of solvents to clean your HMTD.

I'd say just leave the rection mix overnight and then filter off and clean your HMTD.......

[Sparky]

A few days ago I had an amazingly realistic dream about making HMTD. I followed Megalomania's synthesis quite closely (but not exactly). I have read about people making HMTD and got the idea that getting about half as much HMTD as hexamine used is normal. I used 14 grams (as per synthesis) hexamine and got 15 (+- 1g) grams HMTD! Does anybody know what the theoretical yield is? I recorded my dream (with pictures) at this page:

http://pyropage.cyberarmy.ca/HMTDsynth/HMTDSynthDream.htm

I have two/three questions:
1. I stored it under acetone. In real life, would this be at all dangerous - any incomptibilities?

2. It seems to be much more sensitive and powerful than last time I made HMTD in my sleep. Judging from the test results on the page can anybody say whether my dream HMTD was of expected sensitivity/power? Mostly I would like to know about sensitivity. Is washing it once with distilled water and twice with sodium bicarbonate good enough?

[kingspaz]

your purification should do the job ok. it may be an idea to wash with alternate bicarb and water. like, wash with water, then bicarb, then water, then bicarb then finally with water again. that should neutralise it well enough. 32*C is very hot room temperature! at that slightly elevated temperature your HMTD will likely decompose at an accelerated rate.
from COPAE:
% mass lost at over 24hrs -> 60*C 75*C 100*C
0.50 1.30 67.98
it is likely then that long term storage of HMTD in your climate is not the best thing to do. it may not lose much mass but over say 3 months and you lose 0.5% of mass you will have contaminents in there as a result.

it is a good page you have written though. now somebody was asking about what gets respect. IMO this gets respect :)

as for the acetone storage being safe...i'm not sure at all. it depends if HMTD is soluble in acetone. at 32*C though you might aswell just store under water...

[Sparky]

Thanks kingspaz, I chose acetone because even though it is very hot this time of year it is also humid.
I plan to continue my dream and use it up within two weeks so no problems there.
From Mcgyvers table it seems HMTD is not very soluble in acetone, so hopefully it will be ok.

[Sparky]

Hello all. I have had yet another dream about HMTD. I made another web page about my experience.

http://pyropage.cyberarmy.ca/HMTDSynth2/HMTDDream2.htm

This synthesis did not go as smoothly as the first one. It was a little rushed and not as well controlled. But mostly I just made a stupid mistake. I experienced some sort of runaway reaction when the beaker was accidentally heated to 48 C during the 2 hour room temperature period. So, the reason I am posting is to ask about what exactly happened. The thing I find strange about this occurance is that the reaction did not occur when the solution was heated but rather when I tried to cool it down.
To me, more important than what happened is what will the finished product be like? I am worried about extra sensitivity (I'm paranoid).

Edit: I guess I should have read McGyvers post more carefully!
"But then again, for HMTD I really prefer 60-99% acetic acid, for HMTD production. I find it has much less potential for runaway reactions a few hours into the synthesis.

But beware of citric acid, using citric for HMTD *will* cause a runaway reaction unless proper temperature control is used throught the whole process. It's not a question about if, rather about when it's about to happen.

Also try to make HMTD in batches using around 10g of hexamine (HMTA), making bigger batches also increases the risk of runaway reactions."

[Trinitrotoluene]

I had to dream of puriflying the hexamine for HMTD. I added a 12 gram crushed esbit fuel tablet into 20ml of water, brought it to a boil the hexamine dissolved into soloution the wax remained it was filitered. The soloution was left outside in the sun to evaporate the water, after leaveing it there for 4 days all water evaporate. There was dirt contamination in the material, and 30ml of 30% H2O2 was added. Before I add the HCl I wanted to know would any of the dirt contamination affect the stability of the HMTD?
If it does I'll dream of dumping out the soloution.

[IPN]

I have had batches gone wrong because impurities (I'm using 35% H2O2) so I would recommend that you try it again, this time making sure no impurities are present.

A good way of getting the water off the HMTA is to place it in a wide dish and in to a warm place (not outside of course, we don’t want the impurities again) to ensure good evaporation of water.

[nitriees]

I try to make HMTD last night with divide it two step,
1) Add hexamine to 50% H2O2
2) Add citric acid to the above mixture with ice bath
But i don't have enough time to complete the synthesis within that night, i decide to make first
step, let it sit and will carry out next step the next day.
After all the hexamine diluted, the solution is very warm and i put this into water bath to cool it down. The water bath is arround 24 degree celcius, after the solution temperature drop to same as water bath i leave it sit there.
15 minutes later, i heard a " Hizzzzzzz..... " sound and the whole solution is boiling, unfortunately the glass bottle used for this solution is half fasterned with plastic lid, the pressure build up unable to escape, the glass bottle shatter and a nasty gas filled the whole kitchen.
Without citric acid added, what is happening???.......
The exothermic reaction happen because of HMTD forming even without citric acid or hexamine
oxidation will caused.

[Sonny Jim]

50% H2O2 is too concentrated to make HMTD without risk of what happened to you. I recommend you dilute it down to at least 30%. You did not keep the solution anywhere near cool enough either.

This may help you:

http://angry_jack.tripod.com/hmtd.html

[nitriees]

By control the temperature below 5 degree celcius during whole process start from addition of hexamine to 50% H2O2 until HMTD finish formed, take me 3.5 hours to get satisfied yield.
By volume 1:1 ratio of hexamine and H2O2 (50% concentration), i obtained almost 60% by volume from the solution is HMTD.
Use higher concentration of H2O2 have higher risk of run-away reaction but with careful temperature control, the reaction time is shorter with higher yield.
Still not sure what reaction actually happen for previous boiling hexamine and H2O2 solution
without catalyst present and already cool to room temperature?

[Sonny Jim]

Impurities in the hexamine? Contact with metal? At that concentration H2O2, it would not surprise me if the hexamine and H2O2 reacted without a catalyst by themselves. The reaction is exothermic, and therefore self sustaining, leading to spontaneous temperature increase.

[Trinitrotoluene]

I am wondering if you can use Boric Acid as a catalyst in the manufacture of HMTD? It seems to be more commonly found in the pharmacy, and sometimes it's almost impossable to obtain citric acid. It is said that most weak mineral acids will work, so is it possable?

[blindreeper]

I don't know about boric acid but this text book I have here has a table of some common carbonic acids:

Formic acid
Acetic acid
Butyric acid
Benzoic acid
Glycine
Oxalic acid
Citric acid

Citric having the biggest molecule and formic the smallest. This makes me think shouldn't all of these be able to be used in the production of HMTD? Acetic, benzoic, oxalic and citric are very common so I think any of them could be used. I also have heard of reports where glacial acetic acid was used and received yeilds of up to 80% theoretical!
I would try boric acid because that jsut adds another to the list of potential catalysts :)

[Boomer]

I tried both Mega’s and Mr. Cools’s method, adjusting the amounts according to my precursor concentrations. With 30% H2O2 and 33% HCl I had yields varying randomly between zero and 7g from 14g Hexamin, with the same chemicals from the same bottles. No idea why I sometimes got no product with exactly the same process!

With 21g citric I got no product even after 4 days in the fridge. But when I added 5ml of 60% acetic to the beaker within one hour I got 17.5g of product from 14g Hexamin. Assuming the figures on Mr. Cool's site are correct (29.7g from 20g = 100%), this equals 84% yield!

Could it be that the mix of citric + acetic acid makes a better catalyst, or was this super yield coincidence? I will repeat the synth and let you know.

P.S. Funny to be a newbie again after 20 years of ‘blasting around’….

[Wild Catmage]

I use the same ratio and materials as A_W. I usually leave my mix to precipitate over a period of about 24 hours at room temperature. I find that my yield is more than enough to fill two empty 5.56mm cartridge cases.

I also wash my HMTD with sodium bicarbonate/sodium hydrogen carbonate solution. I find that if I don't, it ends up with a "sticky" feel to it.

i also tried improvising a mini-more out of a soap dish, although with little success. I guess that this is because the detonation velocity/rate of expansion of the explosive is too low.

10:05 11/11/03 - ...to be edited later

[invcdr]

Today I attempted to make HMTD for the first time.

I used 55ml of 28% H2O2, 14g of hexamin and 21g of citric acid.

1. I prepared pre-chilled H2O2 and poured into glass bottle in the ice bath.

2. I added hexamin at once and stirred until it dissolved properly.

3. Then I added citric acid slowly while stirring the solution continuously.

4. After dissolving all the ingredients, I put the solution in the fridge for 3 hours, strring for 3 minutes at each 15 minutes.

5. I put the solution in room temperature after 3 hours.

Soon the solution became 'milky', and white foamy material was generated in reaction vessel.

The temperature increased continuously.

Finally the solution boiled and this experiment went failure.

I wonder why this over-heating happened...

Thank you.

[xyz]

The overheating happened because you had fairly strong H2O2 and poor cooling.

It would be a good idea to use a salt ice bath instead of putting it in the fridge. If you don't want to do this, it would be a good idea to use less citric acid so that the reaction doesn't go so quickly (the citric acid is just a catalyst so the amount that you use won't affect the HMTD, just the speed at which it is produced).

If you use a salt ice bath then you should be fine, I use 50% H2O2 and conc. HCl in my AP synths and a salt ice bath is fine to stop it from overheating.

[Boomer]

He said he had it out of the fridge by then, at room temp. The same happened to me, when taking it out after 4 days without any yield, it cooked away in the sink two hours later. It seems to react only above 0 deg. C, so now I take it out, but leave it in a big water bath at 20 deg. C. This works and prevents overheating. It is also a good idea to use ‘much too big’ reaction vessels, they have more surface for cooling (ditto for NG etc).

What yields do you normally get? Was the 84% yield I once got with acetic (see 4 posts above) pure luck? It is much better then what Mr. Cool mentions, and he should know how to do it!

P.S. Funny to be a newbie again after 20 years of ‘blasting around’….

[simply RED]

Now HMTD is the primary i use!
The synthesys in my experience never works with so low temperatures.
I add the hexamine to 30% peroxide then add the citric acid.
Then heat to 50-60 degrees. No reaction untill all the solution becomes white and cloudy.
Then left at 30 degrees for 20 minutes until the reaction is over.
Maybe my peroxide is 10-20 not 30 as it is written.
The yield is high.

The acid is not a catalysator of the process.
It takes part in the process and changes after all.
(CH2)6N4 + 3H2O2 + 2HCl = N2(CH2)6(OO)6 + 2NH4Cl

[Desmikes]

If the acid is indeed part of the synthesis, then why is it that other acids work just as well (gl-l acetic for example?)

[xyz]

@Simply RED, Anthony managed to do an HMTD synth using HCl (search and you should find it, it is called "HMTD synth with pics" or something like that), and that worked fine.

There are many members that use HCl for HMTD synths.

[simply RED]

Any acid will work for the process. Only oxidizer- acids will not work.
The process is:

Hexamin + H2O2 <=> HMTD + NH3

Adding acid you connect the NH3 to form NH4+
NH3 + H+ = NH4+
The concentration of NH3 becomes lower and the equation goes to the right. Anyway the acid becomes chemically changed, thats why it is not catalysator.
Also a catalysator affects both reactions in the chemical balance, which is not seen here.

[scarletmanuka]

I first tried HMTD synthesis not long ago.
The first attempt was with 50% H2O2 and 30%HCl using Mr Cool's method. Instead of the recommennded 30mL acid for my ingredients, I added 6mL. The temperature was at a stable 10C for several minutes and then spiked rapidly upwards with the solution boiling over and reeking of formaldehyde.
The second attempt was with citric acid using Mega's synthesis. However, I had 50% peroxide and added the acid all at once. It was stable for a little while, but then this time, the runaway happened again leaving lots of smoke and semi-carbonised resin in the beaker.
My final attempt I used Mega's synthesis again, but this time diluting my peroxide to 30%. The temp of the solution did not rise for several hours ie. stayed at 10C, and the solution stayed clear. I took it out of the ice bath and left it to stand for another hour wherethe HMTD precipitated to the point of creating a thick glue like deposit. It is yet to have fully dried, but I have taken small amounts and dried to prove it is indeed HMTD.
As far as I can see, the moral is to lower the concentration of HMTD. BTW the initial precipitation collected at the top of the solution.

[Blackhawk]

You mean lower the conc H2O2 right? There shouldn't be a problem with runaways if you go slow, you said you added your acid all at once? I haven't tried HMTD but I think it would be advantageous to add drop by drop and stir to avoid hotspots. Also are you cooling all your chems before starting the reaction? because that may help as well.

When I try AP I will probably be bringing 6% H2O2 up to 30% so I shouldn't have a problem with too strong a soloution ;)

[scarletmanuka]

Blackhawk- I only added the citric acid all at once, the HCl I did drop wise. I figured that the citric being a weak acid would not create hot spots. I am stirring the solution with electronic stirrer, but it is just as easy for me to dilute the peroxide and not have to worry about slowly and laboriously adding the acid to prebent runaways. Probably stick to AP though, it is a lot cheaper and less labour intensive.

[lucas]

I dreamed of HMTD synth last night, based on Mega's lab. I used 50% H2O2. Since the amount of liquid involved and particulary water, is so much lower, (less than half the water as compared to using 30% H2O2), I decided to use 1/3 the citric acid. This proved to be a quite sufficient amount of acid. Cloudy precipitation was observed 1:45 into synth. I was making a scaled down batch, and the ice bath was kept in the freezer between regular agitation. After filtering the first precipitation, the remaining liquid however was still reacting and became hot. Addition of Ice to the vessel halted the reaction. The filtration happened at 4 hours. This is a good lesson that the reaction should be allowed to complete fully before recovering the product.

[chemistr1]

Pure HMTD production is relatively easy but has anyone actually managed to succesfully plasticise HMTD into a useable secondary type explosive?

[Rosco Bodine]

There is one patented composition which consists primarily of
HMTD / AN claimed to have practical usefulness , however it
would seem to me that it would be vulnerable to storage issues
and there are simpler ways of manufacture using milder conditions
than those described by the particular inventor . See GB415900
and GB397600 , GB339024 . Also a related hexamine dinitrate patent
by the same inventor GB421138 . At one time HMTD was contemplated
as a practical material for priming mixtures. See US2341263 .
Original German patents also supposed practical value for HMTD ,
see DRP563459 and DRP274522 . But the truth is that HMTD
is inherently unstable in storage except in the cold , and does
gradually deteriorate even at ordinary temperatures , so its
usefulness is limited to near term use and it must be kept
cold and dry in storage . One possible exception suggested
by the Callery patents is the formation of a possible double salt
of HMTD and ammonium nitrate . If such a double salt does
exist , it could have better stability than HMTD alone , or HMTD
in simple mixtures . An unusual route of synthesis for HMTD is
suggested by the Callery patents . Direct formation of HMTD should
occur from dissolving hexamine dinitrate in 27 per cent peroxide
( in slight excess of theretical requirement ) . HMTD should
result from a self-neutralizing reaction which proceeds at
low temperature if the mixture is kept in the cold ( very cold )
for two or three days . Cold and low acidity favor the hexamine peroxide
formation , while higher temperatures and acidity favor the hydrolysis
of the hexamine which decomposes the hexamine before the peroxide
can form . Kept in the freezer for three days , even HCl as the neutralizer
results in a nearly quantitative yield of HMTD , if only the theoretical
amount of HCl is used , or a slightly lesser amount of HCl than theory ,
however even a slight excess of HCl increases the hydrolysis of hexamine .
I have verified this to be true by experiments . The "ammonia neutralizer"
in an HMTD synthesis is a real reagent , not the same as an acid catalyst
as is the acid in ketone peroxidations . So the quantity of whatever
acid used should be only that amount just barely sufficient to neutralize
the two ammonias which are byproduct for each mole of HMTD .
The same hydrolysis avoidance applies in the formation of hexamine dinitrate
by neutralization of hexamine with nitric acid , warm temperatures
or any excess acidification will be detrimental to the yield due to
hydolysis of the hexamine directly , or the hexamine compounds
already formed . So careful neutralization of HMTD is entirely valid
for chemical reasons . However , if the Callery patents are correct ,
the inherent acidity of ammonium nitrate is not sufficient to be a serious
decomposition influence upon HMTD made by the cumbersome
Callery patent process . HMTD made by more refined syntheses
may fare as well in reaction mixtures or dry or plastic compositions
which are mixtures with ammonium nitrate . HMTD mixtures with AN
have been reported in this forum and also addition of AN to the solution
from which HMTD is precipitated has been reported here to improve
crystalline form and yield of HMTD . That report could possibly be
Callery's "double salt" if indeed an HMTD / AN double salt exists .
And this possibility is very interesting . Philou Zrealone has mentioned the
possibility that HMTD may also form a nitrate . So there is reason for
interest in further work along these lines of experimentation with HMTD .

[xyz]

chemistr1, someone has been able to plasticize HMTD by adding a few % heavy mineral oil.

Search and you should find it.

[Trinitrotoluene]

SWIM did atempt to synthesize HMTD using boric acid as a catalyst, but the results was a failure, the boric acid woulden't dissolve into the H2O2/hexamine mixture.
The mega's procedure was used, citric acid was substuted with boric. The ration of 14 grams hexamine 50ml 30% H2O2, and 21 grams of boric, when the PH was checked it was PH 6.
Aftter 6 hours, the boric acid was filtered away, and whatever was left, HCl was added to it and HMTD is now forming.
The simple answer boric dosen't work.

[Zeitgeist]

I had a runaway reaction making HTMD recently - the solution boiled, and became a thick orange substance like honey. Does this sound like normal runaway HTMD - What could the decomposition products be?

[lucas]

I have seen the same result from a runaway. The smell of the smoke prduced was similar to that of the haxamine used. Cant help regarding te actual products formed in the situation.

[markgollum]

I also have attempted synthesizing HMTD with citric acid, and 35%H2O2.
Which always lead to the solution boiling over, no matter how slowly I added the acid (over about an hour and a half).
Then, I went to the university library, and read about Citric acid in the CRC Encyclopaedia of Chemistry and Physics (I think that was the book, perhaps not).
The book explained that citric acid is oxidized quite easily to acetonediecarboxylic acid,
oxalic acid, carbon dioxide, and water, depending on the conditions.
Quote
"Citric acid is easily oxidized by a variety of oxidizing agents such as peroxides, hypochlorite, persulfate, permanganate, periodate, hypobromite, chromate, manganese dioxide, and nitric acid. The products of oxidation are usually acetonediecarboxylic acid,
oxalic acid, carbon dioxide, and water, depending on the conditions used"

CH2-COOH (O) CH2-COOH COOH
HO-C-COOH ------ > C=O + COOH+CO2+H2O
CH2-COOH CH2-COOH

So, when I read that, I thought, the peroxide is oxidizing the acid, and oxidations are exothermic, so, to try to keep the solution from boiling, I wont use an oxidizable acid.
When I tried the synth again, using HCl instead of citric acid, I found it quite easy to keep the temperature under control.
Since then, I have used HCl for making HMTD

(EDIT tried to fix the reaction equation).

[metafractal]

I am astonished to hear stories about all these runaway reactions with citric acid! I use a salt ice bath with 50% H2O2 and my reaction is always stable. I dont pre-chill reagents, dont monitor the temperature, and add my citric acid in about five proportions with five second intervals and stirring. It is quite difficult to achieve a runaway with citric acid as it initially reacts endothermically with the solution. Only if you manage to protonate the solution so rapidly that it becomes self sustaining can it become exothermic (i.e. runaway).

So, I thought I might just post some pictures and an explanation of my cooling apparatus to help all these people getting runaways. It's nothing special, but I've never actually seen any post spell out exactly how a salt-ice bath is constructed. I know some of the senior members might laugh at this, but I think it will be very helpfull to the newbies.

The vessel used for a 100ml beaker is a plastic container that was originally a chinese takeaway container. The has a diameter of 13cm compared to 5cm of the flask (1) (http://www.imagestation.com/picture/sraid99/pad19de11ba173af9ae73faa0c7e927db/f9f6e20d.jpg).

Ice cubes are added to the vessel (2) (http://www.imagestation.com/picture/sraid99/pe06f6feb7941451497bd9ecc2279a130/f9f6e205.jpg) . A generous amount of table salt, sodium cloride (about 30g) is sprinkled on top of the ice (3) (http://www.imagestation.com/picture/sraid99/p64581e0d6cd40be9bcaf85bba194dc6c/f9f6e1fc.jpg) . Then water is poured evenly over the salt and ice in order to rise to approximately 1/4 - 1/3 of the height of the vessel.

Finally, the beaker which the hexamine reaction shall take place in is submerged 3/4 of the way as close to the center as you can get it (4) (http://www.imagestation.com/picture/sraid99/p9d8d8936cf7358eedb68641575d8b882/f9f6e1f2.jpg).

This provides sufficient cooling for an organic peroxide reaction. For reactions which require stricter cooling, I will crush the ice and salt together in a blender. I dont know why I havn't seen people do this more often, as it provides excellent cooling.

On another note, I've always found the purification process of hexamine from camping stove fuel tablets tedious and highly lossy. When using high concentration peroxide it is acceptable to just mix a chilled saturated hexamine solution with the peroxide before the addition of the acid.
EDIT(s): Finally, all the pics are up and working.

[xyz]

If you construct your salt ice bath like that, what is the point of the salt?

I have always thought that the reason that salt is added is because it lowers the freezing point of water, (i.e. a frozen salt solution will be colder than frozen water) but if you add the salt after the freezing then what is the point of adding it?

[Blackhawk]

I think the idea with adding the walt is that it makes the ice melt at a faster rate so the salt ice bath will be colder for a shorter period of time.

[chemoleo]

hmmm.... salt lowers the freezing poing because it lessens the ability of H2O to form a crystal lattice. Hence, NaCl/water is *liquid* below 0 deg C (as crystal formation is impeded). It is therefore a desired cooling mixture because it enables the experimenter to achieve reaction vessel temperatures below or equal zero deg C. Conversely, a normal water/ice mixture will never get below 0 deg C, thus the temperature in your reaction vessel is above it, normally around 2-4 deg C. For your HMTD preps, add NaCl to the water/ice so as to have a greater temperature gradient, and so as to achieve temperatures close to 0 deg C, or preferably below it.

[Mumble]

Adding the salt makes the ice melt at a lower temperature, and therefore makes the solution even colder. Ice water can only be close 0. The salt lets it get down to lets say -4. Its true that it does melt faster though. Adding Ice to salt water would allow a cooler bath temperature, because of the ions dissolved. I forgot the formula, but it's so many degrees for every mol of ions dissolved.

[Bert]

It also takes energy to dissolve the salt. The energy comes from the salt/ice mix's heat. Net result, dissolving the salt cools the mix further- Didn't any of you ever make ice cream the old fashioned way?

[Blackhawk]

I thought that they used to make ice cream in a water/KNO3 bath, at least thats what they did on that reality TV show that was set last century :P

[Bert]

Hmm. Australians do things differently? Rock salt is what we used.

[Blackhawk]

I'm not sure, I think this was a British series. But then again you live in the USA/Canada area don't you? so things are likely different there. Not sure what was used in AUS, would be nice to buy some KNO3 for 'Ice Cream' making though :P

[kingspaz]

enough of the icecream guys - we're making HMTD :)

[Wild Catmage]

Speaking of which, my current batch has turned a faint pinkish-orange colour :eek:

I was using citric acid as the catalyst and 9% OTC hydrogen peroxide, but accidentally left a stainless steel spatula in the flask, after stirring the mixture. The spatula was in the flask for about 30 minutes, and the liquid is now tinted pink. As the crystals have not yet formed (although lots of tiny bubbles have), I don't know how this will affect the end product. I guess I'll just have to wait and find out.

NB - There's no visible sign of rust or any other deposits on my spatula, and I cleaned all my glassware and equipment before using them. My guess is that this is either rust, or some iron compound formed by the steel reacting with the citric acid.

On runaways, I haven't experienced any yet. When I add the acid, I cannot feel any change in temperature, at least, not any increase in temperature. This is probably due to me using a solution of only 9% hydrogen peroxide. I'll try using a thermometer next time.

EDIT - It's about 2 hours into the reaction now, and small white crystals are forming. Some are rising outwards to the surface of the liquid, clinging to the outsides of tiny bubbles. Others are falling slowly towards the bottom of the reaction vessel, to form a carpet of HMTD. I'll have to buy me a digital camera :p

EDIT #2 - The HMTD finished forming some 18 hours later. after neutralising the citric acid with sodium bicarbonate, I left the batch to dry out at room temperature.

[Blackhawk]

Perhaps a tiny amount of forming HMTD reacted with the stainless steel as HMTD does, but I wouldn't think it too likely as the HMTD wasn't even visibly forming at the time.

[atlas#11]

I have heard of HMTD's incompatibility with metals and tested it(to some extent). here is what came of it. For stainless steel I left less than a gram of pure dry hmtd on a spoon over night, in the morning the entire ammount of crystals had turned brown red like Fe2O3 and were much more sensitive to a hammer blow, for lead I used filings off a bullet and noticed no changes over night and was just as sensitive and seemed compatible(dont bet on it or any thing). And lastly I tested copper, the one said to be the worst(they were right). it formed in to a brown green pile of crap that went off with the slightest tap with the hammer. As for it reacting with metals in it's reaction vessel i havent tried it but i would guess it would. All of my synth have been successful in that i got decient yields(around 60-70%), and I use simmered down 3% H2O2 to about 15% and it dosent seem to want to react until it is cold. All of my synth are done outside in a snow bank and they have never been slow either. I let them react over night to be sure and get every last miligram of it.

[Ammonal]

No runaway with 9%??? I had my first HMTD runaway using 200ml 6% H2O2, added the hexamine, cooled and added the HCl, the temperature rose and sat on 7 degrees C. I had the reaction vessel sitting in an ice bath and 10 mins later I returned to check on proceedings and the temperature had risen to 70 degrees C. I got no yield and burnt fingers from touching the reaction vessel.
Second to that I cool everything and take every precaution within reason and have had pretty good success with every batch since. A saying comes to mind about relaxed procedures causing accidents and mishaps... just follow other peoples directions and when they say add the acid slowly; add it slowly and so on.

[Wild Catmage]

Wow, I just lit a half-pea sized lump of HMTD in a fume cupboard (because it has a screen) and the lump detonated with a loud bang. There was no flash that I nor any of the two other observers noticed, and our ears were ringing afterwards. This has taught me new respect for HMTD.

[Sonny Jim]

I decided to test out this runaway theory for myself, just now. I used 200ml 9% H2O2 and 28g hexamine, but instead of using cirtic acid I used 91% sulphuric. The reaction ran very hot but did not foam or anything like that. In 5 minutes 50% by volume of my reaction vessel was filled by a dense layer of HMTD, floating on top of the liquids.

[crazyUser]

In my dreams I often do some experiments and runaways only occured if i added all the hexamine at once (within ~30sec) AND if the ammount of H2O2 was more than ~25ml AND only with h2o2 concentration > ~15%.
With very small batches <25ml I never experienced overheating problems..
I don't know if it was mentioned before, but if you put an hmtd reaction beeing overheated/going runaway into an icebath/waterbath soon enough,
the reaction will continuously 'loose energy' and so will stop beeing selfsubstained after some time.

Now a little question from me :
In the dream I had yesterday I made a little bit bigger hmtd only charge (paper casing/5cm heigth/3.5cm width, shaped like a tube (don't know whether this is the right word, forgive me please), pressed). What do you think how much hmtd would this be (i think ~30 - 40g, right ?).
I detonated it about a mile away from our village in a field with very wet soil.
I sticked it in the ground that only the fuse was looking out and placed a ~3mm thick aluminiumplate directly in front of it in the soil.
After det. there was a crater about 40 inches wide/30 inches deep (which is pretty impressive I think) but the plate only got a big dent (4-5cm deep). Is this ok or should the plate be penetrated ?
The sound of the explosion could clearly and very loudly be heard in the village as my mom told me and i felt somewhat like a shockwave beeing about 70feet away (not in the air, only in the ground, due to its wettness i think).
And just for comparism, what would a same sized charge of petn have done to the aluplate and soil ?

One last thing :forgive me for my english which surely isn't as good as it should be, hope you enjoyed my dreams ;)

[Zeitgeist]

I've never experienced any flash or flame with HTMD (or AP), provided it's dry so that it detonates and doesn't just deflagrate.

I'm not surprised it got hot SonnyJim, it's that concentrated H2SO4, you don't need that so strong.

[Boomer]

And just for comparism, what would a same sized charge of petn have done to the aluplate and soil ?


The crater would be only slightly bigger (2 x size = 8 x volume!), but the plate would be penetrated. I blew a hole into a 3mm STEEL plate with 1/4 that amount of PETN, no confinement and without a cavity or even a real SC (with liner).

[al93535]

I tried the synthesis of HMTD per Mega's instructions, with small variations. I used one Esbit tablet (14 grams) 100 ml of 15% H2O2 (guessing concentration), and 35 grams of citric acid. I never really noticed any substantial temerature rise, with the addition of Hex or the acid, a few degrees. I let the mixture react for 26 hours and got a dry yield of 4.7563201 grams, apparently 51% theoretical yield. I will try again with a known 27% concentration of H2O2. My Esbit smelled a bit fishy as well, so I suppose it decomposed a bit. I also found that I had to neutralize quite a bit more using the citric, as compared to using HCL for AP.

[Sylla]

I've tried to calculate HMTD enthalpy and have found it to be -1000.5 kJ/mol. It's pure theory so I wonder if someone here can tell me if it's correct (with an small error like ~5% of course) ? Considering the formula, density (1.41) and enthalpy I found these values which seems to be correct :

C6H12N2O6 -> 6.0 C + 6.0 H2O + 1.0 N2 + 0.00 O2

M = 208.1 g/mol
Oxygen Balance = -92.24%
0.754 l/g of gaz
0.034 mols/g of gaz

Enthalpy of Explosion = -451.1 kJ/mol (-2167.55 J/g)
Explosive Power = 1633.82 (60% Of Picric Acid)

Approximated Temperature : 1743 Kelvin
Approximated VOD : 4727 m/s

On megalomania's webpage it is said that the VOD is about 4500m/s which is really close to my theorical value...

What do you think about this ?

[simply RED]

The reaction of the explosive decomposition of HMTD must be different. Like in all oxigen difficient explosives you never have only H2O and Carbon.
See TNT.