HMTD Synth With Pics

[Anthony]

Being impressed with ALENGOSVIG1's pictorial synthesis posts, I thought I'd give it a go with the humble HMTD synthesis, seeing as I need to replenish my small stock anyway.

This would have been posted yesterday, but a last minute BBQ and 13 beers got in the way... :) Don't worry though, I'm paying for it now :(

We start with the precursors:

<a href="http://www.geocities.com/eawfuk/HMTD01.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD01.jpg</a>

200ml of 6% H2O2
18gm Hexamine
75ml of 30% HCl

The bottle of H2O2 has previously been chilled in the fridge.

Next, dissolve, with the aid of stiring, the hexamine in the cold H2O2:

<a href="http://www.geocities.com/eawfuk/HMTD02.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD02.jpg</a>

Then place the reaction vessel into an ice and gradually add the HCl, with stirring:

<a href="http://www.geocities.com/eawfuk/HMTD03.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD03.jpg</a>

Note that you should ideally check the temperature of the solution with a thermometer during the catalyst addition. But I managed to break my thermometer sortly before doing this synthesis so I resorted to a highly scientific method of dipping my finger into the solution to check that the temperature had not risen.

The reaction vessel is then placed in the refrigerator for 24-48 hours. I noticed reasonable crystal formation within three hours, with almost complete formation in under 24 hours. In the following day, little more crystals fell out of solution.

The reaction vessel 48 hours later:

<a href="http://www.geocities.com/eawfuk/HMTD04.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD04.jpg</a>

Note that most of my crystals had formed on the bottom of the reaction vessel with a thin layer on the surface - as is normal, untill shaking of the vessel resulted in a floating foam which would not settle. So I recomend avoiding aggitiation of the solution.

Then, using a piece of cloth as a filter, filter the crystals from the solution and discard the filtrate:

<a href="http://www.geocities.com/eawfuk/HMTD05.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD05.jpg</a>

Note that usually you will need to add some cold water to the reaction vessel, swill around and then dump into the filter in order to remove the crystals left clinging to the walls of the reaction vessel.

Filtration complete and the crystals in the filter:

<a href="http://www.geocities.com/eawfuk/HMTD06.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD06.jpg</a>

<small>[ September 21, 2002, 07:43 PM: Message edited by: Anthony ]</small>

[Anthony]

Gather up the corners of the filter cloth to form a little "bag" and run a stream of water through it from the tap, to wash the crystals:

<a href="http://www.geocities.com/eawfuk/HMTD07.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD07.jpg</a>

Next, prepare an approximately 4% solution of bicarbonate of soda with 200ml of cold water and 8gm of bicarb:

<a href="http://www.geocities.com/eawfuk/HMTD08.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD08.jpg</a>

Add the crystals to the solution and aggitate with stirring for a few minutes. The purpose of this is to neutralise any traces of the acidic catalyst left in the crystals:

<a href="http://www.geocities.com/eawfuk/HMTD09.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD09.jpg</a>

Then filter the crystals as before, but ensure that if the same filter cloth is used, that it has been thoroughly washed to avoid cross-contamination:

<a href="http://www.geocities.com/eawfuk/HMTD10.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD10.jpg</a>

Note that at this stage, I was also furnished with a cup of tea. Although eating/drinking is usually discouraged in a lab, I'm sure you will be fine if, like me, you avoid contaminating your drink with chemicals or worse, your synthesis with tea.

Then it's back under the tap for another rinse:

<a href="http://www.geocities.com/eawfuk/HMTD07.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD07.jpg</a>

The filter and its contents is then spread out on a newspaper and placed out of direct sunlight to dry:

<a href="http://www.geocities.com/eawfuk/HMTD11.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD11.jpg</a>

24 hours later, the crystals are dry and ready to use:

<a href="http://www.geocities.com/eawfuk/HMTD12.jpg" target="_blank">http://www.geocities.com/eawfuk/HMTD12.jpg</a>

Final yield was 12gm, hardly fantastic but then this is using pretty dilute OTC chemist H2O2.

Price break-down:

H2O2 - £0.69
Hexamine - £0.19
HCl - £0.19
TOTAL: £1.07

Cost per gram: £0.09

<small>[ September 21, 2002, 07:47 PM: Message edited by: Anthony ]</small>

[Eliteforum]

Excellent, very informative. If your HCl the One Shot drain cleaner? Or something else? And did you get it at B&Q?

[Anthony]

"Spirit of Salts" - local DIY shop

[Mr Cool]

Lol, soon you'll start getting people saying HCl doesn't work for HMTD, only CTAP! Maybe now they will see the truth, and realise that it does work but they fucked it up.
Eliteform: HCl drain opener? I think you mean H2SO4 (that is what is normally called "One Shot"). The HCl can also be found at B&Q etc., as a stone cleaner.

Nice pics, very informative.

[kingspaz]

well done Anthony. the newbies now have a full good quality HMTD synth using easy to get chemicals. hopefully no more new threads 'Howz can i makez HMTD?'. i like all the pictures. they allways say what words never can which is good as it shows exactly whats happening.

[Resident Evil]

I'll do a AP synth with pics tomorrow if I have the time.

[ALENGOSVIG1]

Dont wase your time taking pics of AP synthesis. Thats been done already. Do something original.

Its good that your trying to contribute though.

Oh and nice job anthony.

<small>[ July 17, 2002, 07:57 PM: Message edited by: ALENGOSVIG1 ]</small>

[NERV]

Looks like I will have to try the HCL method again. Last time I tried to do it I didn’t get any crystals.

[sinstar]

My yeild of HMTD is really shitty, well its very powerful but to make a decent cap I have to make two batches, Is this normal? And mine is not very sencitive, I've tryed hitting it with a hammer, rubbing it between house bricks, shouting at it, swearing at it evreything! I use the lab out of KIBC, except I replace the 6% with 9% hydrogen peroxide, I don't think I need to change the ratios as theirs not much difference between the 6% and the 9%, or do I? Oh and good work Anthony!

[xyz]

Just sharing a thought for your amusement(a bit off topic, I know): I'd love to see Mr. Bean trying this, especially the bit about accidentally getting the cup of tea mixed in with the synthesis :) .

[None]

My HMTD isn't that shock sensitive either. It takes a hard blow with a hammer to detonate it, I was quite suprised.
I would adjust the amount of hexamine you are using. 6-9% is quite a difference, thats probably why you are getting such low yields. Besides, you might as well adjust it, because (for me at least) H2O2 is more expensive than hexamine.

I don't have very accurate scales and only ever make small batches. Does anyone know if adding too much hexamine would reduce the yields? As mentioned before my H2O2 is expensive and i would rather waste hexamine than risk wasting H2O2.

[Rat Bastard]

Nice Job Anthony.

Whenever I made HMTD I would use this formula (it worked pretty well with me)

- 45ml 6% H2O2
- 2 1/2 teaspoons Hexamine
- 4 1/2 teaspoons citric acid

( I got it from a member here but I can't remember his name)

I later tried Mega's recipie using 30% H202, but to my suprise I had pretty much the same yield as my 6%. Any suggestions?

[S. Toppholzer]

Ratz Bastard - could you please for clarity's sake use grams instead of "teaspoons"? I'm a European and I can't make head nor tail out of that sort of measurement.

[Arkangel]

Hmmmmm:

Coke, Diet Coke, Stella, Orangina, HMTD and if I'm not mistaken a tango bottle at the back. Nicely stocked fridge Anthony! :D

As a newbie to this aspect of our hobie I can't tell you how valuable these guides are. I'd seen Alen's pages and was thoroughly impressed and this adds to it. To anyone that's thinking of similar things, I for one would really welcome it. Cheers <img border="0" title="" alt="[Wink]" src="wink.gif" />

[Anthony]

I'll do a similar thing for a PETN synth with H2SO4 and KNO3 when I get some more nitrates (my bank balance needs to take a turn to the happier side first). I'll be doing NG my the same method again soon, I'll photograpgh if it would be considered too repeatitive of ALENGOSVIG1's NG synth with distilled HNO3.

Close on the drinks. Left to right: bottle of god-awful French beer, stella, smirnoff ice, orange "Glitz" (cheap, pretty nasty mixed vodka drink from COOP...), stella, Lime "Vodka69".

"tango?" I thought, I don't know how you did it, but I went and checked and there is actually a can of tango at the back. God knows how long it's been there, the use-by date is July 2002... But it must be the bretheren of the one I had the other week. I'd stumbled into the kitchen at 6am, grabbed the can, opened the can, noted that no gas escaped, I poured it into a glass and it formed two distinct, dark orange layers and was very flat, gross. I drank it anyway though because I was badly hung over and in dire need to liquid :)

Before anyone calls me a Southern Fairly, those drinks are leftovers (I drink what I buy :) ), the closest I have to those girly drinks is Shit Faced.

Ok, I think that's my masculinity established :D

[ALENGOSVIG1]

Ive already taken pics of the xNO3/H2SO4 method for nitro but I didnt get very good pics. Click on the link in my sig to see the nitro sythesis.

I cant wait to see the PETN pics synthesis though.

Oh and the HCl method works almost all of the time except 2 out of 20 times ive made HMTD it didnt work. Quite strange really. I dont know what happened. Still, i always use HCL becuase it cheaper then citric acid for me.

<small>[ July 18, 2002, 07:46 PM: Message edited by: ALENGOSVIG1 ]</small>

[Anthony]

My bad, I did check your website, but must have followed an old link to and old version, and saw that NG via H2SO4/xNO3 wasn't listed.

[marky]

Can someone do the AP Synth soon?
anyway just a sugestion...
thankyou

[ALENGOSVIG1]

That's already been done by many poeple including myself. check out the link in my sig for AP synthesis with pics.

[Flake2m]

My HMTD experiment turned out to be a flop. the yeild was so bad that the cyrstals could be hardly seen. The main problems were avalibility of chemcials (I could only buy 100ml of 6% H2O2). I also didn't have access to a scale or a thermometre.
I will try to make some more HMTD again, but not until I can get some 30% H2O2.

Is there a major difference in yeild if you use HCL rather then citric acid ?

[sinstar]

So does this lab need changing? 45ml of 9% hydrogen peroxide(in KIBC they say to use 6% but I can only get 9%), 2 and a half tsp of hexamine,4 and a half tsp of citric acid. The power of the final yeild is very good but getting a good amount is about as rare as rocking hourse shit. The final amount I get is about half of Anthonys.

<small>[ July 20, 2002, 11:36 AM: Message edited by: sinstar ]</small>

[Mr Cool]

No, it does not need changing.

[sinstar]

So if it does not need(HA! got it right this time)changeing why is my yeild so poor?

[Anthony]

Using HCl, citric acid, or even H2SO4 shouldn't directly affect the yeild as it is only a catalyst.

To keep the ratios the same, but using 9% H2O2, use 50% less H2O2. It's all linear with different concentrations of H2O2 so it's just simple maths to work out how much you need (e.g 100ml of 3% = 10ml of 30%).

[kingspaz]

rc, if HCl reacts with hexamine to form ammonium chloride and formaldehyde then would H2SO4 react with it to form ammonium sulphate and formaldehyde (H2SO4 being more acidic)? this seems to be leading to the actual reaction mechanism which produces HMTD.

[sinstar]

So Anthony, instead of useing 45ml of 9% H2O2, I would use 22 and a half mls of H2O2?

[None]

No, I'm pretty sure you would use 30ml of 9% instead of 45ml 6%. I think he may have meant 50% of the 30ml or something.

[Celtick]

Since I have the 30% H2O2 now, and I have probably the same HCL (thanks to Arkangel <img border="0" title="" alt="[Wink]" src="wink.gif" /> ) I converted the ratios into:

200ml of 6% H2O2 - 40ml of 30% H2O2
50ml of 30% HCl - 50ml of 30% HCl
18gm Hexamine - 18gm Hexamine

But I when I converted Mr Cools ratios I got:

225mL of 6% H2O2 - 45ml of 30% H2O2
150mL of 15% HCL - 75ml of 30% HCL
20g of Hexamine - 20gm of Hexamine

Not much of a difference, but it seems to me that there is to much acid in both of the reactions. But since I don’t know how to cut the ratio down, could you give me the proper ratios with these chems.

[kingspaz]

the HCl is a catalyst for the reaction so the amount present will only affect the rate. if you need the HMTD fast use more acid. if you want to save on acid use less but you'll have to wait a few days. the amount of HCl used should be independent of the other two chemicals.

[Celtick]

I know that the HCL just works as a catalyst, but your last reply on my other HMTD problem was:
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">I don't know the correct ratios but to me that looks like too much acid as I’d say you only need around 25ml. </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">I thought that maybe by using too much acid you could sour your reaction.

[kingspaz]

it won't sour the reaction. unless you use waaaaaaaaaaaaaaay too much. but if you use less it saves you money :) . so i'd use mr cools recipe but with 40ml of 30% HCl.

[Celtick]

The amount of HCl wont mind since I got 6 litres for free :D But thanks for the advice! I will experiment and post the results when I’m back from Spain (I’m leaving tomorrow)

[Anthony]

Interesting point on the role of the acid, thanks for pointing that out.

I just noticed a mistake in my original post. I used 75ml HCl, not 50ml as previously stated, I'm not sure why I mixed that up because the picture clearly shows the 100ml measuring cylinder to be 3/4 full.

I was shit tired when I made that last post so I will try to clarify the ratios issue:

The easiest way is to work out how much actual (pure) H2O2 there is in the stuff you have.

E.g in 200ml of 6% H2O2, there is 6ml of pure H2O2 per 100ml of total volume. So that's 12ml in the 200ml total.

So whatever concentration of H2O2 you use, you need to work it so that the amount of pure H2O2 stays constant at 12ml.

For 30%: 30%/12ml = 2.5, 100/2.5 = 40ml - which is what you worked out.

[Celtick]

Ok, so when using your recipe I should use:
40ml of 30% H2O2 - 50ml of 30% HCl and 18gm Hexamine
But because of the high concentration of the H2O2, shouldn’t I use less HCL since the reaction doesn’t need so much catalyst?

[kingspaz]

i personly don't think it matters although my thinking could very well be wrong. if you use less less HCl (30% HCl is 70% water <img border="0" title="" alt="[Wink]" src="wink.gif" /> ) then theres less water added to dilute the H2O2 (but less actual HCl to catalyse) but if you use more acid then the H2O2 is diluted more by the extra water added (but made up for by more HCl present to catalyse). so either way the reaction rate would be similar.

[Celtick]

Kingspaz, today I tried to make HMTD with the above ratios. And (as for now) it didn’t work, in my opinion due to too much acid. Take a look at the <a href="http://www.roguesci.org/cgi-bin/ewforum/ultimatebb.cgi?ubb=get_topic;f=2;t=000414;p=3#0001 92" target="_blank">HMTD threat</a> for the whole story.

[kingspaz]

celtik, check out your post in the other thread: 35 + 5 + 30 = 70ml
in the ratios above it says to use 50ml. i think HMTD could be soluble in HCl or decomposed by the high acidity of HCl.

[Celtick]

I converted the above ratios from Anthony:

200ml of 6% H2O2 - 12ml pure H2O2
18gm Hexamine - 18gm Hexamine
75ml of 30% HCl - 22,5ml pure HCl

12ml pure H2O2 - 40ml of 30%H2O2
18gm Hexamine - 18gm Hexamine
22 ml pure HCl - 70ml of 32%HCl

[kingspaz]

sorry celtick, i didn't realise you had converted them. well, the reason citric acid is usually prefered for HMTD is because it is not as acidic as HCl. HMTD seems to be very sensitive to acid contamination so need to be washed well. maybe this is due to acidity breaking it down. my complete and utter guess would be that if theres too much H+ present then the HMTD will decompose faster. i'd say it would be better to use less catalyst than needed although it will take longer you will not lose much HMTD (hopefully). hope that helped but remember i made ALOT of guesses <img border="0" title="" alt="[Wink]" src="wink.gif" />

[Anthony]

It would make sense, as with the high concentration H2O2 that you are using, there is considerably less water to dilute the HCl, thus giving an overall higher acidity to the reaction solution.

[Flake2m]

I tried making HMTD again using 200ml of 6% H2O2, about 14-16 grams of hexamine and a generous amount of citric acid. Yet again it is a flop. The experiment has been in the fridge for a little over 24 hours and there has been no visable reaction :( . I am pretty sure I used pure hexamine as the stuff smelt like fish. What am I doing wrong? or is it just the g[m]ods of chemistry are stuffing me around?

[None]

Flake2m, I have had bad luck making HMTD with low percentage H2O2 as well, although mine was 3%. Hydroponics stores in Australia sell a product called Oxyplus which is 50% H2O2. Or you may have better luck with AP and 6%.

Has anyone else found HMTD to be more sensitive to shock when made with HCl rather than citric acid? It may have just been one batch, as i have only made it with HCl once, but it seemed quite a bit easier to detonate with a hammer. It was properly washed and neutralised.

[kingspaz]

Flake2m, we are not stuffing you around because this is a place to learn. we are throwing ideas at the problem trying to solve your troubles. we obviously can't gaurantee its going to work since we are not the ones doing it. YOU are.
generous amount (too much H+?)? try about 12g of citric. if that doesn't work then maybe it could be your fishy hexamine.

[zaibatsu]

Flake2m, here's an interesting quote for you
"No disrespect or flaming of any moderator or administrator will be tolerated"

Do you want to stay here?
ATB, Zaibatsu

[nbk2000]

There's only one kind of person allowed here at The Forum...people wiling to learn and share what they've learned in an open and truthful manner.

NO ONE who deliberatly passed on false or misleading information would be allowed to remain here. Not member, mod, or even admin. Simply because such stupidity could get a person killed and further vilify an already endangered (and dangerous) hobby.

So your suggestion that a staffer would deliberately "stuff around" :confused: about an explosives synth is insulting in the extreme. :mad:

But since I don't think you meant it in an insulting manner you'l get to stay here. But be careful in the future about how you phrase things, eh? After all, the staffers have been here for years, and don't take kindly to having their hands bitten by ungrateful newbie dogs. <img border="0" title="" alt="[Wink]" src="wink.gif" />

(PS: YOU are ultimately responsible for any failures or successes you may have after following advice offered to you here on the Forum.)

[Anthony]

I think we have a missunderstanding here :)

I think Flake2m meant the gods of chemistry, like the crystalisation fairies who decide, based upon abosutely nothing, whether you get a precipitate or not - actually applicable to this situation incidentally.

Flake2m, First thing I'd do, it confirm that your hexamine actually is, as there's some similar substances used for cooking purposes. Secondly, I'd try using an alternative catalyst, maybe HCl, to eliminate another variable. I presume your H2O2 is pharmacutecal, so that should be fine.

If still no joy, give up and try AP :)

[Flake2m]

Firstly, I am apologising to any m[g]od or admin that may have been insulted by my previous post, I had no intention of flaming or abusing anyone. I am willing to learn and share information at this forum.

Secondly, Good news :D the HMTD synth is working, the reaction just took a little longer to get going. This probaly just shows I am a little impatient. The HMTD cyrstals have been forming for a liitle over 24 hours, I will filter and dry them in about 24 hours time.
My HMTD synth is at room temp and it seem to be doing just fine :) .

[kingspaz]

good to hear its working!
just make sure you neutralise it thoroughly using anthony's method above and treat it with much more respect and gentler than BP. this is powerful stuff!

[Mic]

Me too I have hexamine who smell like fish. I Try searching the forum and I didn't find anything about the smell of hexamine. Is your's smell fish too ? or it's that my hexamine have impurities? Mine is like esbit fire starter but it's another brand.

I tried making HMTD with it but I have used all my 9% H2O2 to make CTAP. So I took 3% but I have not very much so i take only 50 ml. To this, I add 2.5 gm fishy hexamine and 10 ml HCl. I put it in the fridge 3 days ago and nothing. I will wait until there is something in the bottom of the solution and i will tell u guys soon.

Ciao

[kingspaz]

mic, you need to add catalyst aswell. add some citric acid or HCl like you would for AP.

[Mr Cool]

He added 10mL HCl <img border="0" title="" alt="[Wink]" src="wink.gif" /> .

[Celtick]

I succeed now in making HMTD with 30% H2O2/32% HCl check out my page for synthesis:

<a href="http://www.angelfire.com/goth/celtick/" target="_blank">Celtick's Page</a>

[Mic]

Ok, there is nothing yet about my HMTD so I add 10 others ml HCl. I think this will speed up a little the reaction.

Nobody's answer about my hexamine's question! What is the smell of hexamine ?? is it normal that it smell like fish or is my hexamine impure ????

Ciao

[0EZ0]

Someone didn't look hard enough <img border="0" title="" alt="[Wink]" src="wink.gif" />

Try <a href="http://www.roguesci.org/ubb/ultimatebb.php?ubb=get_topic;f=14;t=000006" target="_blank">this</a> .

[kingspaz]

mic, don't get annoyed that nobody answered your question. don't just come here and demand answers we're not a fucking school and we don't get paid so be thankful for what you do get.

[PrimoPyro]

Your hexamine has undergone partial hydrolysis to produce that familiar rotting fish smell of methylamine and/or formaldehyde.

Haha, you just made a List 1 chemical buddy! Better turn yourself in before the Karma Police get you! :p

PrimoPyro

[Mic]

kingspaz: sorry, im not getting annoyed.. :(

oezo: ooops <img border="0" title="" alt="[Eek!]" src="eek.gif" /> I haven't seen that :rolleyes:

and well, there's nothing yet about my HMTD... I'm waiting for it

[Flake2m]

I am probaly going to get another 200 k3w| points for this but anyway:
I pressed about a gram of HMTD into a small plastic container I found (15mm X 10mm ). I used a chop stick to press the HMTD, I then put a small piece of carboard on top. I then pressed some BP on top of the cardboard. I didn't have any fuse so i tried using i bit of rolled up newspaper, this of course didn't work so I settled for plan B. I used a pair of pliers to move the small container I then threw it into the fireplace we have. Mum was nearby a saw me through it in, "that didn't do much she said :rolleyes: " as the BP ingnited, then 2 seconds later BANG <img border="0" title="" alt="[Eek!]" src="eek.gif" /> , the pressed HMTD detonated and all the ash in the fire place went all over the floor, as well as some hot coals. I was lucky the room had a tiled floor <img border="0" title="" alt="[Eek!]" src="eek.gif" /> .
I have also gained much more respect and care for this stuff.

[NERV]

I think that is one of the most k3wl things I have ever heard. Throwing a primary explosive like HMTD into A fire is just plain stupid. You could have a piece of flaming wood stuck in your head.

[kingspaz]

if he did he would deserve it. that stupid irrelevent crap does not fit into this topic as its about HMTD synthesis not hot to be a fucking idiot with explosives. people like you give pyros and explosives a bad reputation.
now back to the topic at hand, HMTD synthesis.

[Flake2m]

The point of the post was HOW NOT TO TREAT HMTD (someone out there now knows). I just choose to learn the hard way :( (and believe me I have learnt because I had to clean up the mess! <img border="0" title="" alt="[Eek!]" src="eek.gif" /> ). I have also learnt not to underestimate the power of HMTD :rolleyes: .

The yield of HMTD I got from that synthesis was much less than expected. I only managed to get about 1-2 grams of HMTD. In conclusion, the next batch I make I will be more patient and let it precipitate over a week, instead of 3 days.

Thank you to the g[m]ods for helping me with the HMTD synthesis :D .

[parabolic]

in my dream i attempted to make my first HMTD with 60g 6% h2o2, same as Anthony's peroxide, same make too :) , also 6g of powdered hexamine, 20g granulated citric acid. i added the citric acid first with no heat problems, then added the hex in small amounts whilst stiring until all was desolved. i noticed that there was still no heat at all. after that i left the mix to react, checking for any heat, but still no heat after 1 hr. all i could see after the solution settled was a frothy white substance floating an top of the solution, nothing on the bottom, and the solution looked as if it was carbonated with loads of still bubbles in it. but not bubbling.

i left it 24hrs at room temp, and the solution looks the same, to me it looks like no reaction has taken place.

should i add more citric acid, as ive read in some threads to start the reaction off, or just leave it?.

The hex i used is labled "Highlander solid fuel tablets", i smelt them and they smell slightly of fish, and are pale white, slighty grey. they powder up really well too.

The other hex tablets i have are in a black box labled "Portable cooker, 8 solid fuel tablets", these REALLY stink of fish, so bad i have to keep them in the box, and they are pure white, i havent tried these ones yet, wanted to try the other brand first.

also, i have a bottle of "cleaner and descaler" bought from b&q it says on the back, ..this product contains hydrochloric acid.

but it dont say what % of HCI is in there and i have not got any ph paper or anyother way of testing to see what strength of HCI i have.

i wouldnt mind trying Anthony's method which uses HCI, but i dont want to try this cleaner and descaler until i find out if it has a suitable amount of HCI in it.

any ideas.

thanks for reading.

para.

[zaibatsu]

Hi parabolic, good to see more people from the UK, even if you are from Scotland <img border="0" title="" alt="[Wink]" src="wink.gif" />

Back on topic:
The commonly available "brick cleaner" HCl is around 10-15%, and is suitable for use in HMTD (be careful still, nto sure about the impurities).

If there isn't a problem with the Citric (I'm guessing you either bought it from a chemists or a homebrew section of a shop), and I guess you're using H2O2 from a chemist, then that can't be the problem either. Therefore I reckon its the hexamine!

So I say try the pure-white tablets, they sound like they will work, HTH.

<small>[ August 19, 2002, 06:05 PM: Message edited by: zaibatsu ]</small>

[kingspaz]

smells like the hexamine is the problem (sorry for the poor joke :) ). the fishy smell is down to the hexamine decomposing. nice new fresh hexamine is what you need! grey hexamine tablets sound really shitty. as zaibatsu said pure white coloured ones are what you need.

[parabolic]

thanks guys for the advice, btw i was born in salford, manchester so really iam from england and have lived in scotland for the past 15 years :) , anyway, the white greyish hex is the new hex i recently bought and doesnt really smell, it is the one i tried with the experiment that didnt seem to werk. to me the hex i used would seem the worst to use as i have reason to belive from reading past threads on hex, that the fishy smell is a BIG sign to tell me it is the real stuff., and the fishy stuff is pure white., anyway what ill do is try the exact same experiment but with the other hex, the one that really smells :) .

ill keep you updated and hope i get sume HTMD.

thanks again.

para

[parabolic]

Hi folks, in my dreams it was a success!!, I finally made it . I tried using the old type hex I got from a camping store, the white and really bad fishy smelling hex. The amounts were, 60grams of 6% h2o2, 20grams citric acid granules and 6grams of powdered hex. The solution after mixing was very clear, no heat just a nice cold solution at room temp. I left the jar out of sunlight at room temp for 48hrs, still no heat was felt during all this time as I checked it often., anyway I noticed It had white stuff at the bottom of the jar and frothy stuff at the top after 48hrs, I filtered it all and poured water over it. I then took a small swob on a pencil and tried to light it with a lighter but nothing happened. So I used a hair dryer to dry the small amount I had on this pencil. I then tried to light it again, and to my total astonishment it flashed as quick as I could blink.. this was amazing. I though black powered was fast.

My only hope is that I can get another couple of boxes of this hex to keep me stocked up, or try the same again with the newer hex that didn’t seem to work the last time, caus all it had was froth, maybe the froth was HMTD and I should of dried that out and tried it?

Anyway this was most enjoyable, and I can see how carefull I shoud be with this stuff.

Was wanting to know if I should keep the water and HMTD together in a jar, until I need it, then all I have to do is dry it out, but will this destroy the HMTD over time by having it I water?

I couldn’t achieve this with out the expert knowledge of you guys, ta.

Para.

<small>[ August 22, 2002, 04:06 PM: Message edited by: parabolic ]</small>

[kingspaz]

parabolic, make sure you wash the HMTD with bicarb solution as detailed in anthony's posts at the begining of the topic. if you do not do this then expect an accident. this is one of the reasons HMTD has a bad reputation. avoid contact with sulphur also as it is acidic.
avoid all scrapes and forms of friction and whatevr you do do not get comfortable making it because thats when it'll go off, when you least expect it to <img border="0" title="" alt="[Wink]" src="wink.gif" />
good luck and be careful! and also avaoid the hair dryer for the main batch as the heat will cause sublimation and accelerated decomposition and therefore a loss of product.

[parabolic]

Well, my hmtd works very well, nice loud bang from a 1 gram charge.

Anyway, I have been very disappointed in the amount of hmtd I get from my experiments, I have been using, 60grams of 6% h2o2, 20grams of citric acid and 6grams of hex. My final yield after 48hours is a rather wimpy .7grams :(

I have tried adding 10grams of hex, but the yield hasn’t really changed, and I was wanting to know if anyone can tell me if I could improve the yield by adding more or less of any of the ingredients.

I do not use "spoons" as a measurement as this is very silly I use only grams or grains, as this is the only way to measure accurately.

[kingspaz]

ok, i think you are using too little H2O2. i haven't got the equations infront of me to work out how much to use but try using 200g H2O2 with the rest of the ingredients the same (20g citric, 6g hex) and see if that improves yields at all. if it doesn't then atleast you know the H2O2 isn't the problem.

[darkdontay]

Just found this while looking for some more experinces with it...
<a href="http://seattlepi.nwsource.com/local/75332_fill20.shtml" target="_blank">http://seattlepi.nwsource.com/local/75332_fill20.shtml</a>

the thing happend about 100 miles from where I live.. I never remember hearing about it though....

It just goes to show you Kewls come in all profile brackets

Oh yeha some info on the FBI analyzing it
<a href="http://www.fbi.gov/hq/lab/fsc/backissu/oct2001/bartick.htm" target="_blank">http://www.fbi.gov/hq/lab/fsc/backissu/oct2001/bartick.htm</a>
[Not what that guy had made, this is a report on HMTD its self I found.. WARNING this is a FBI.gov site] "
Analysis of a Suspect Explosive Component:
Hydrogen Peroxide in Hair Coloring Developer"

<small>[ October 16, 2002, 11:29 AM: Message edited by: darkdontay ]</small>

[nobody]

Have a look at the second page darkdontay posted (fbi.gov) -&gt; this is the patent-recipe. You'll get more HMTD than hexamine used. The reaction needs 12h, I usually filter after 24h. No cooling needed, just mix all of the hexamine and the citric acid and dissolve in the H2O2.
I never tried the method with HCl, citric acid is much easier to obtain and cheaper.

<small>[ October 16, 2002, 11:20 AM: Message edited by: nobody ]</small>

[Aaron-V2.0]

I tried the HMTD synthesis last weekend three seperate times and they resulted in nothing! :mad: I used Mega's method to the word (Only I substituted 10X 3% H2O2 for 30%)

500ml 3% H2O2
14 grams Hexamine (First two used Esbit tablets, last I used Colhams tablets.)
21 grams Citric Acid

First batch I mixed the crushed Esbit tablets into the H2O2 and the wax was left on top (No harm to the synth I've heard.) and lowered the temperature to 10C. I then started mixing in the citric acid (Particle size is similar to tablesalt.) and the temperature started... DROPPING! :o

I kept stirring it and after about half an hour and putting all 21 grams of citric acid into the mix it had reached a temp of about 3.9C.

I was pissed so I dumped it.

The second attempt was more or less just to check if it was my chemicals. I had plenty of supplies to waste so I put in the exact same amount of chems (This time finely ground.) into a capped bottle and shook it up for a minute, with no temp rise at all!

So, the next day I went into a lovely camping/hunting store and I see a small package of Colhams tablets that're labled "Hexamine fuel tablets". The interesting thing is that the Esbit brand of hexamine is 14 grams to one tablet (Something like 1"x.5"x.75") and the Colhams are round disks measuring 1" across and .5" tall, they weigh 14 grams to 3.5 tablets! Very bulky for "pure" hexamine" and it had no wax binder at all.

And I mix it all together like the first time, with no temp rises except a brief 3C rise and that's it. I leave it overnight for 12 hours and it's still just a milky H2O2 mix. I looked at the bottle of Hydrogen Peroxide and it says "Stabilized Hydrogen Peroxide." Could that be it? Stabilized?

I'll go find some 30% and try it then, hopefully it's just my H2O2.

[ALENGOSVIG1]

I'd say its either your citric acid is bad or your already weak H202 has been degraded.

[NoltaiR]

NEVER USE 3% H2O2!!! I know that many people have claimed that it works (well I think maybe just a couple people claimed it, then the rest just assumed they were rigth), but in all the lab tests that I have ever done, none have ever worked with 10 times the amount of 3% H2O2. All you have to do (and it is sooooo easy) is boil it down to 1/10th of the original volume... and then presto!

And the reason it is 'stabilized', is because there is so much damn water in it that it couldn't possibly cause much of a reaction (if any).

<small>[ November 02, 2002, 12:58 AM: Message edited by: NoltaiR ]</small>

[Aaron-V2.0]

I learn something everyday on this website. The fact that Mega's synth mentions using 3% is why I tried it, and when I think about it boiling down a small bottle of H2O2 should be easy as turning on the burner. :) Now then... I just have to wait until I'm away from my house... again... In a month or so.

Damn parents. <img src="http://www.roguesci.org/ubb/icons/icon17.gif" alt=" - " />

[ShockWave]

since my Ng detonates with the Flah, I don't use the HMTD anymore, so I did my 18gr HMTD in a very small bag and I lighted the fuse, the bag was just on the ground, nothing on top of it, I ran away and expected a loud kaboom, but it just deflagrates, when you light 18gr AP it detonates no doubt about it, but i'll guess that HMTD needs to be more confined or the HMTD was not good,

[ShockWave]

HMTD was good i think, I forgot to read this from mega's site

HMTD will detonate if struck, but will only burn if heated.

sorry !

[Anthony]

Ok, let's clear a couple of things up at first. "Stabilized" H2O2 is perfectly normal, a small amount of phosphoric acid is added by the manufacturer to reduce decomposition of the H2O2 (by sunlight etc).

Secondly, although I haven't personally used 3% H2O2, I'm sure it must work, and I don't have any trouble with comparitively weak 6%.

In fact, I made a batch with 9% H2O2 the other day, and within 30 minutes the reaction was pretty much over. Yield was approx 1/4 the volume of the reactants (with 50ml 30% HCl).

Shockwave, HMTD doesn't need any more confinement than AP. It must have still been damp.

Don't expect a temp rise when using citric acid, it's the hydrolosis of the acid that produces the heat. Citric is a piss weak acid so theres really no heat produced. Even with HCl, I notice very little, if any temp rise. Now, 90%+ H2SO4 is where you have to watch out for the heat production.

[jarrod]

Anthony, a little off topic but I tried your synthesis and it didn’t work for me.

First I dissolved the hexamine (which were really old army heating tablets, crushed) in the cold H202 (6%)
All seems ok. This took about 5 min but there were “chunks” of hex floating on top about 1mm square.

I slowly added the HCL over a period of 10min. But when the acid came in contact with H2O2/hexamine it went a brown colour like tea.

The HCL was at a 32% concentration.

Now I have a jar of what looks like tea with no crystals or any sign of crystals forming, after about 40 hours in the fridge.

I think the tablets could have had impurities in them, any suggestions or ideas are welcome

[0EZ0]

One thing would be that the H2O2 is not concentrated enough. Shop around, you are bound to find a source of higher concentration.

Also something you should know is the Hydrochloric Acid decomposes the hexamine. Citric Acid is also favoured over HCl as it seems to be harder to produce HMTD correctly using the mineral acid (HCl)

Now about the colour the solution went with the addition of HCl. How old was the bottle that you had? Old HCl tends to make some funky colours in reactions, from personal experience. Probably due to decomposed plastic in it or something along those lines(that is if your HCL was in a plastic container).

I would try the citric acid method if you can get ahold of the it. It should not be too hard to find, hell it can be found in grocery stores, eg. Safeway or Coles.

Good luck to you :)

<small>[ December 18, 2002, 07:19 AM: Message edited by: 0EZ0 ]</small>

[TheBear]

In the swedish infomania's textfilecollection called "the library" (this is perhaps their least respectable collection but still) I found a statement claiming that HCl + formaldehyde would yield one of the most carcinogen chemicals known, just even letting their fumes combine will form this chemical. It is not stated what chemical is formed but if anyone knows what happens I'd appreciate you telling me :) .

After I read this I didn't think much about just trying to remember "never mix HCl and formaldehyde". And now I was thinking of making some HMTD, when I realised that during the reaction HMTA is decomposed into ammonia and formaldehyde and if HCl forms this carcinogen chemical I sure don't want to use HCl to catalyse the reaction.

(for the swedes with the library on hand and whant to check for them selves open "Kemiska reaktioner.txt", 1.3 Cancerframkallande!)

[Anthony]

TheBear, I think we should reserve judgement on the dangers of HCl catalysed HMTD until we have more than just a vague reference from a "text phile"... Chemical name would be a starter... Studies or preliminary research done into it's carcinogenity etc.

Jarrod, since your from Aus, you might be using "Digger" brand HCl? If so, this seems to be a widely experienced reason for HMTD synths going brown in colour - as can be seen in the Makeshift Arsenal.

I would first suspect the "hexamine" tabs, being old they may have decomposed through age, if they were even hexamine to begin with. Does the packaging say "hexamine" on it somewhere?

If your hex isn't the problem, then trying with citric acid, as suggested would be well worth. Some ways just work better with different folks.

Plus it helps if the Crystal Fairy is smiling on you, else no precipitate for you!

[Mic]

I tried making HMTD 2 times with HCl. The first time I used 10mL 9% H2O2 with I don't remember how much hexamine and I don't remember neither the quantities of HCl but I have taken the recipe in one post from here. The second time I tried with HCl, It was also a recipe from here and I don't remember witch but it as work very well and I have gotten a very good yield.
Sorry for bad english <img border="0" title="" alt="[Wink]" src="wink.gif" />

[jarrod]

I am using “diggers” brand Hydrochloric acid so should I change brands, or is it not important.

And the pack for the tablets said “FUEL COMPRESSED HEXAMINE.”

I have had trouble if finding citric acid, where should I look. I tried “coles” and “bi-lo” should I look in a chemists?

thanx

[0EZ0]

You should have no trouble finding citric acid, you just have to know where to look.

It can be found in little containers at most supermarkets sold near the spices under the name 'Citric Acid'.
It is also sold as a 'Black spot remover' at most pool chemical shops, though it may come in 25 kilo bags.
It is used in home-brewing and is sold in about 1kg lots.

Most information regarding sale of chemicals can easily be found using an internet search engine relavent to your area of the world.
One should not need to ask about the places to purchase most items, as keeping your eyes and ears open is just as fruitful, if not more so :p .

About the 'Diggers' brand HCl, I have found that it does produce some funky colours if used in most reactions as Anthony has said. If it worries you, just head down to a hardware store and purchase another brand.

The Hexamine that you have should be ok, but if it is rather old then head out and buy some more, fresh. Decomposed hex can have an effect on the yield of HMTD.

Have fun :D .

(Edit): I provide a few sources of Citric Acid as it is a plentiful chemical and has quite legitimate uses. Due to the stupidity of the Politicos most of my other chemical sources I have now made a vow to protect. Just something i needed to say..

<small>[ December 19, 2002, 12:02 AM: Message edited by: 0EZ0 ]</small>

[nuxvomica]

The best site about HMTD and all other explosives of interest could be found at <a href="http://swi.1av10.nu" target="_blank">Swedish Infomania</a>. You would probably understand the recepies, although they are in Swedish, otherwise you could ask Stanley who writes excellent English. :)

[kingspaz]

or the best site in english <a href="http://roguesci.org/megalomania/" target="_blank">http://roguesci.org/megalomania/</a>

[Celtick]

Last week I took for about hundred boxes of ‘army’ Hexamine with me from leftovers after a exercise :D . Just to prove it to myself I made another batch of HMTD with it tonight (previously I made it with the famous Esbit tablets) I also use 32% HCL, and it never failed me since I got the right quantities for myself!
Again the results were good, the only thing I do extra is to purify the Hexamine tablets, there is a lot of wax binder coming of from the 'army' ones. I also used this Hexamine for my HDN synthesis.

<a href="http://www.angelfire.com/goth/celtick/HMTD.html" target="_blank">HMTD synth</a>

[static_firefly]

I used 50%H202 35% HCl and Hexmine. I winged it so my measurements wernt very accurate. I mixed the HCl and the H202 in around equal parts then chilled it in the fridge. I added hexmine powder and then just placed in a strip of Hexmine. After about 2hours i pulled the strip out believing that the soultion was saturated. After 24hours nothing. The reaction wasnt working, or so i thought. In about a week i checked again and whoa the container was like a slurpy (it was a small fishhook size container). The crystals worried me a little. I had only ever use AP before and was used to a fine powder however these crystals were around 3mm long. It was powerful but the fact that people have claimed to have it go off from exposure to light has prevented me from making any more. Id much rather use ap or mekp.

[Mr Cool]

I find HMTD to ppte in very very small crystals (smaller than AP), and also it is very much more stable than any other peroxide I've encountered. It is the only peroxide to have had any commercial interest.
Maybe if you followed some form of recipe, rather than blindly stumbling forward, then you might have better results?

Has anyone ever found something that can solvate HMTD? AP can be recrystalised from acetone which will improve its purity, but I don't know of any solvents that can be used with HMTD in practical amounts.

[Yak]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">
kingspaz
i personly don't think it matters although my thinking could very well be wrong. if you use less HCl (30% HCl is 70% water ) then theres less water added to dilute the H2O2 (but less actual HCl to catalyse) but if you use more acid then the H2O2 is diluted more by the extra water added (but made up for by more HCl present to catalyse). so either way the reaction rate would be similar.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">If I remember from school (were doing reactions and such at the moment) it doesnt matter how much it is diluted because the reaction will be the same but take more time.
Therfor you can make one experment with say 10ml of 30% H202 and one with 100ml of 3% H202 and they would make around exacly the same amount of HMTD (if both are made same time and its a fair test, so there might be a small difference) but the 30% would finish faster and the 3% would take much longer but still make the same amount.

ps. Im sorry if this has been said before, i must of missed it if it has.

p.p.s
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">
nuxvomica
The best site about HMTD and all other explosives of interest could be found at Swedish Infomania. You would probably understand the recepies, although they are in Swedish, otherwise you could ask Stanley who writes excellent English.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica"><img border="0" title="" alt="[Eek!]" src="eek.gif" /> all I can really say is welcome to Megalomania's forum,The Explosive and Weapons Forum, the best explosive forum there is!

<small>[ December 23, 2002, 09:09 PM: Message edited by: Yak ]</small>

[kingspaz]

yak, that wasn't the point i was making. read the post above the one you quoted.

[Yak]

Sorry I miss read what you were saying but the quote saying E&W forum is the best E&W forum there is, still stands :)

[1337bomber]

Has anyone here ever successfully made HMTD with H2SO4? I am having a hard time getting HCl, but I have a bunch of H2SO4 just sitting around...

[vulture]

I have said this before somewhere here, but I discourage making HMTD with mineral acids because they decompose hexamine into ammonia and formaldehyde.
Therefore, using H2SO4 should be avoided but it will work if you use diluted H2SO4.

[NERV]

Just to warn you ahead of time. If you do use H2SO4, your going to have some real shitty yields (even with dilute acid). I wouldn’t even bother with using H2SO4 because of how crummy the yields are. If your going to make HMTD I highly suggest using citric acid, it can be easily found in the spices section of your local super market.

[1337bomber]

Thanks people! I will save the H2SO4 for AP and TMP. If anybody is looking for hexamine, I found 1 lb of it on ebay for 15 bucks US. I can't get it into Canada, but it is technical grade and if you are in the US it seems like a good deal!

[EP]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> it can be easily found in the spices section of your local super market.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">True some places but not others. I see we are both in the US, but I've tried several stores and asked for it with no luck. I actually sorta found out a place but not really (long story) that didn't work out, but I guess it was some more specialized cooking store. It's also used for making soap, so whatever kind of store caters to the soap maker folks would have it. I just ended up ordering 2lbs of it from ebay (just got it today! :) ) I also saw that hexamine, and might buy it so nobody else bid! :p

edit: I also ordered some hexamine from another place and it should be here in a few days so I can make HMTD. I don't think I'll ever use up two pounds of citric acid however...anything else it can be used for?

<small>[ January 24, 2003, 12:59 AM: Message edited by: EP ]</small>

[nbk2000]

I've found citric acid in the canning supplies section of the grocery store. It's used to prevent discoloration of food when canning.

[Rat Bastard]

Where I live, you can buy it at almost any pharmacy. A tad expensive though; about $8 CAN for 100 grams:
<img src="http://krimzonpyro.com/rat/boardimage/citric.jpg" alt=" - " />

[EP]

Mine was $5 a pound! :D :p

The canning thing is interesting, I'll look there and try to remember this for when I write about getting it on my site.

<small>[ January 24, 2003, 02:34 AM: Message edited by: EP ]</small>

[Evil_Empire]

http://www.ressotami.blogsite.org/book/Bookindex.htm
stupid noob has a good idea on purifying H2O2 so you can get a higher concentration.
good luck and just a point the HCl method does work, i find that concentraions and volumes etc have to be acurate but thats just me.
Empire.
note: ive only made a few batches so i wont be to perfect at it.