HMTD

[Myrol]

You're really good but not correct! Meyers Explosives Book says that HMTD had a Energie of Formation around -1608kj per kg! Thats a lot and also the reason why my Beaker a month ago turns crazy, fumes, hizzes and boils when i tried to make HMTD again but this time with pure Hexa and not Esbitfuel! You have also another mistake in the Formula of Decomposition! HMTD produces 6moles CO, 6 Moles H2 and one mole N2 per mole HMTD! The Standardgasvolume from HMTD is 1400Liters per kg and thats only makeble when HMTD decomposes into CO, H2 and N2!!! Have you not knewledge about the "Wassergasgleichgewicht"?? It says: C+ H2O--> CO+ H2 and CO+ H2O--> CO2+H2! It depends on the Temperature and is hardly pressed to the right side when the Gases have a temperature about 1000°C! Thats in fact true if you compare it with HMTD's Explosion Temperature!

[simply RED]

It is not possible to calculate the heat of detonation of unbalanced explosive (negative OB).
This is because you don't have only CO, CO2 and H2O!
SEE TNT:
Schmidt (1936) experimented with density effect on TNT with 1Kg
(4.4moles) did at D. 1.0 and 1.59g/cm^3:

D.= 1.0: 4.4 C7H5(NO2)3 --> 2.84 CO2 + 17.0 CO + 3.77 H2O + 2.49 H2 +
0.1 C(m)H(n) + 0.1 CH4 + 2.85 NH3 + 0.47 HCN + 0.2 C2N2 + 4.75 N2 + 10 C

Temperature of explosion= 3080 deg.C.
Heat of explosion= 910 Kcal/Kg
Gas volume= 773 L/Kg.

and D. = 1.59:

4.4 C7H5(NO2) --> 5.47 CO2 + 9.39 CO + 6.09 H2O + 1.63 H2 + 0.03 C(m) H
(n) + 0.42 CH4 + 1.5 NH3 + 0.32 HCN + 0.3 C2N2 + 5.39 N2 + 14.6 C

Temperature of Explosion= 3630 deg.C.
Heat of explosion= 1085 Kcal/Kg.
Gas volume= 685 L/Kg.

You can calculate the heat of combustion of a balanced explosive if the heat of formation is known. Heat of detonation will again be slightly different from thr heat of combustion (lower).
As everyone has niticed the smell after the detonation of HMTD, it is obvious that it forms many detonation products.

[Sylla]

Actually I know HMTD won't give 6.0 C + 6.0 H2O as it because there is the water gaz equilibrium. I just took it as a approximation of the produt of decomposition.

By the way, you can get a better approximation using the water gaz equilibrium constant at temperature T (given in the calculus). Then you have 'new products' which will give you a slightly different temperature of explosion. Repeat this process until the temperature doesn't change anymore. Computer are welcome for this, of course.

But, seeing the exact properties of explosives was not my goal. I'm just interrested in calculating enthalpy from pure theory. I explain :

Yesterday I learned from my chemistry lessons the "energy of binding" (don't know if it is the correct name in english) so I tried to use it. I've first calculated the enthalpy of Hexamine and then the enthalpy of HMTD. This method gives an approximation of the value, (ie following this way H2O has a enthalpy of 245.5kJ/mol).

So the method is not really accurate because of the enormous error in the value with the HMTD. -1000.5 kJ/mol means about 5 MJ/Kg !

The general approximation of the whole calculus gave me 4700m/s with 4500m/s on mega's website so I was very exited...

PS: I only know the Kistiakowsky-Springall rules listed in "The Chemistry Of Explosive" so if somebody here could give me more advice about general approximation on the properties of an explosive it would be fun ;)

PSS: Forgive me for the water gaz equilibrium, I was just seeking a very approximated solution, not rigourous chemistry ;)

[ossassin]

Every method that I've seen recommends washing the HMTD with methyl or ethyl alcohol. Would 99% isopropyl work?

[Myrol]

Yes Isopropyl should work well! 99% pure is a good choice to prevent shitty impurties because HMTD is typical instable in contact with "Dirt". I have another Question: How can i prevent a fucking runaway reaction like i had with my last Batch HMTD (30% H2O2, Hexa and Citric Acid) I dont want to dilute the mix because this reduces the Yield to much in the Cellar! Permanent chilling seems to be the only method good stirring too?

[ossassin]

I've never had a runaway reaction when making HMTD. You shouldn't have one as long as you keep it cool and add the citric acid slowly while stirring. As long as you have the beaker in an ice bath and do things carefully, you should be fine.

[Boomer]

To end the discussion which of the two is the better primary, I conducted some tests.

AP is a little more friction sensitive, but not much so. On the other hand, it can be used in metal caps (if not stored too long, and if slow reacting metals like aluminium or stainless are used), which HMTD can not. Even in electric plastic or glass caps, HMTD reacts with the bridge wire (filament of bulb), gets even more sensitive, and eventually eats up the wire.
I came to the conclusion that they are of equal usefulness, with AP being better for electric caps, and HMTD for fused ones.

Concerning the power, I tested both primaries pure, and compared to compound detonators. The ‘caps’ were refilled firecrackers, 6.5mm inner diameter, and 8cm long. The compound caps had 1cm of primary and 6cm of booster, the normal ones were 7cm primary only. They were hand-pressed with approx. 1000PSI (25kg / 0.33square cm), containing 1.5g respectively 2g for the compound ones.
The witness plates were 1mm x 8x8cm stainless steel, extremely hard/sturdy. I could hardly cut them with a cutting bench capable of twice the thickness of normal steel.

About the pics:
Left front is AP + picric acid which did not detonate from the AP. Right front is AP, left rear is HMTD and right rear is AP + MHN. The MHN version was distinctly stronger, while AP and HMTD made dents of exactly equal depth, with the HMTD dent being slightly sharper in the middle. But this could be caused by me pressing it a little harder than the AP - guess why… ;)

[Guerilla]

Sounds like a suitable comparison, however mind to describe a bit closer of that friction sensitivity test as there seems to be difference of opinion on this one and I personally consider HMTD more sensitive to friction than AP.. though it might not make all that big a difference in practice. I prefer HMTD over AP due to its better detonating properties in the similar density.

[tom haggen]

Out of all of the ranting in this long ass thread, I didn't see any references for ratios for this synthesis using sulphuric acid. Anyone have any ideas?
Or ratios for using glacial Acetic acid, which almost seems like an interesting synthesis. I saw somewhere in this thread that you might be able to get theoretical yields of 80% using glacial acetic acid. I'm just a little pissy cause I got some horrible yields using 77grams of hexamine, 250ml of 35% H202, and about 30ml H2SO4. The first time I made this primary with the same precursors I got excellent yields. I just wish I would have written down the ratios..

[nitrogeno]

the first advantage of HMTD is the stability, is one of the most stable on peroxides explosives. The citric acid works good, sulphuric and HCl -- and the yield is lower. Why use other acids if citric is available and cheap...?

[Myrol]

I know, this Thread becomes bigger and bigger but has someone ever done a Test how good the Yields with Acetic Acid are really be? Citric Acid works good, but I often heard that Acetic Acid give Yields around 80%....would be a devastating improvement, because I have more than 800ml 99,5% pure CH3COOH in my Cellar left and look every day for a nice usage.

I think If I have some H2O2 again I will DO this comparisment and Post my results. HMTD is stronger as most people here think.

The Energydensity per unit of Mass is good but near this from TNT (92mt for HMTD). BUT the Energydensity per unit of VOLUME is Great! If you press it to nearly maximum density (perhaps with some NM to make it more slippery if HMTD is with NM compatible) you get value of 142mt per Liter HMTD. (92mt 1,55g/ccm). ANNM 65/35 has a density of 1,25g/ccm so one Liter ANNM has 145mt (116mt 1,25g/ccm)! If someone doesn't agree with this density of ANNM please post your results! In a measuring cylinder I could fill up 100ccm with 125g ANNM. :)

[SantasL.Helper]

Question:

Yesterday i was making HMTD, i'd kept the temperature of the mix under 0 degrees celsius, added the citric in like half an hour time and continued keeping the mix below 0 for the first three hours (+- -2*), took it out of the bath, then waited for 2 hours. It was in a cool, not too brightly lighted room. Suddenly, i hear my stephdad screaming out my name, so i went down to check. When i got there i saw massive white collums of smoke (very clearly formaline in it, judging by smell) rising up from the beaker, so i grabbed the beaker and threw it outside on the gras (on doing this, i burned my finger due to the heat of the beaker). Then i went back in, there was still a lot of mixture boiling and smoking in the newspaper that was under the beaker, so i threw icewater over it (witch made the reaction stop) and then got the newspaper out. When later closely observing the newspaper, you could clearly see that it had actually burned. Can anyone tell me what happened? Cause this has never happened to me before.

[Macgyver]

Runaway reactions when making HMTD using citric acid are very common.

Try using acetic acid instead and you will not have this problem.

How large was your batch of HMTD? (Making too much in one batch also increase the risk of runaway reactions).

[Rosco Bodine]

I have gotten good yields of HMTD from prechilling in a freezer
60-70 ml of 27% H2O2 in a clean glass jar having a threaded lid .
Then 15 grams of hexamine is dissolved with stirring in the cold
H2O2 . 22-23 ml (not more) of 31.45% HCl is added gradually
swirling the mixture to a clear solution , the jar capped lightly
to allow for pressure relief , and returned to the freezer for 72 hours .
The jar is removed and few ml of ammonia is added with swirling ,
the mixture filtered , the crystals rinsed on the filter with cold distilled
water , and dried . The yield is 20-21 grams ~90% , or better .

Instead of the 15 grams of hexamine and 22 ml 31.45% HCl ,
28.5 grams of crystalline hexamine dinitrate may be substituted ,
although I have not tried this , it has been reported on a Russian
site .

[nitriees]

Constant stirring may solve the runaway problem when the temperature
control below 5 degree celcius.
When I used 35% concentration H2O2, the runaway can happen even
without citric acid addition at room temperature.
Constant stirring to prevent hotspot occur will greatly reduce the possibility
of runway.

[Rosco Bodine]

Metallic ions as impurities are the most likely cause of
decomposition problems with peroxide mixtures . Any
greater than needed presence of possible organic impurities
also may cause decomposition . So using a high molecular
weight organic acid as the ammonia neutralizer is just
asking for problems with decomposition . For every gram
more of the ammonia neutralizing acid required to be used
simply adds more trace metal ions and organic contamination
which favors decomposition . The notion that use of pure
hydrochloric or nitric acids is somehow inferior to citric acid
is simply a myth . So many folks want to keep using
the more expensive , more dangerous , and less logical
method using citric acid "grunge" , instead of sparkling pure HCl
which gives zero problems and higher yield of a purer product .

Why ?

[Boomer]

Because Mega uses it? Because it is in the original patent? Because they use low conc H2O2 and don't want to add any more water as would be tha case with HCl? :confused:

Anyway, I had runaways with both citric and muriatic acid, and success with both, plus with acetic. Keeping the batch small and the container large definitely helps.

Plus, adding crushed ice to the reaction mix can stopp a runaway and save the batch. :)

[Rosco Bodine]

If dilution is an issue for HCl , it would be better to
first concentrate the dilute H202 . Or perhaps try
the ammonium sulfate and formaldehyde method
which gives low yields but is reported to work with
dilute hydrogen peroxide . I haven't tested that method
to be certain , but see no reason for it to provide any
better yield than using hexamine with the acid neutralizing
equivalent directly , if the concentration of H2O2 is limiting .
Ammonium nitrate may possibly substitute in that method
where lower concentrations of H2O2 are used . A longer
time for reaction and lower yields are guaranteed when
low concentration H2O2 is being used .

There are patents which describe use of nitric acid ,
applied to large batches made on an industrial scale .

Acetic acid or formic acid would be more logical than
citric acid , if they are available . Introducing the least
amount of metallic or organic impurity gives the best
result , while using only the amount of acid required
for neutralizing the completed reaction , or to make it
very slightly acidic .

Anyway the H2O2 concentration of the reaction mixture ,
temperature , time of reaction , pH and level of
metallic and organic impurites are all important factors .
When those factors are optimized , the yield based upon
hexamine is often nearly theoretical , and the product
is a sparkling white reflective crystalline material which
accumulates on the bottom of a clear reaction residue ,
having almost no effervescence of free O2 from decomposing
peroxide , an occasional tiny bubble of O2 may be observed in
a reaction proceeding well . If something different is being
observed , then the mixture is contaminated and yields are
going to be lowered , and likely the stability of the end product
will also be lowered .

HMTD is a stronger initiator than AP when used as a primary ,
but HMTD is chemically unstable and has a very limited useful
shelf life at normal temperatures . It should be stored dry and
and in the freezer if it is to be kept for any time and not to be
used within a few days . It will keep well at freezing temperatures .
HMTD is absolutely ruled out as a primary or component for any
device or mixture which will be kept at ordinary temperatures for
more than a week or two at the outside , and even at that , not
at outdoor summer temperatures . HMTD is inherently unstable .
Heat , or acidic conditions , metallic ions , certain organic contaminants
will accellerate the decomposition .

In contrast , AP is a poorer initiator , but AP is much more chemically stable
and can be kept indefinitely at ordinary temperatures . Acidic conditions
alone do *not* adversely affect the stability of AP . Alkaline conditions
would likely be more of a problem for AP , and also metallic ions ,
but not nearly so much of a problem as for HMTD . AP has less problem with
organic impurities as well . The disadvantage of AP is due to its high vapor
pressure , and its constant sublimation and recrystallization from its own
vapors , which occurs in closed containers . The crystals of AP are constantly
reconstructing themselves and permeating every crevice , a solid having no
"steady state" through normal temperature fluctuations of the environment ,
the solid is in effect in constant motion , as if it were a genie endlessly trying
to escape its bottle . Where that task has it depositing into the crevices
of threaded closures or stoppers , a danger of potential spontaneous detonation
is created from the frictions attendant a manual removal of
the container closure , or perhaps even the smaller possibility that normal
expansions and contractions of containers and their closures may at some
point generate a sudden slippage against crystals entrapped in a crevice ,
to frictionally intitiate the trapped material and convey that small explosion
to the remainder of the bulk amount of AP in the container . Any storage
scheme should account for this known danger regarding the closure on
the storage container .

[Anthony]

I bought some citric acid many years ago to use in a HMTD synth. I never used it though, instead I used 32% HCl (industrial cleaner), and then everytime from then on. I never had any problems with runaways.

I wasn't even that careful with temperature control. I'd prechill the H2O2 (6 or 9%), mix, stir and then put into the fridge.

There is no reason not to use HCl. It's much simpler and you only need a few ml - 5ml in 200ml reactants works well. What the hell difference is ~3ml of water going to make? Why the hydrophobia ;) at all? It shouldn't make much difference how much water is in your reaction vessel, as long as the reactants are still there!

[Rosco Bodine]

Always be aware that the amount of acid to hexamine is
critical in HMTD synthesis , where the acid is a reactant
and not just a catalyst as is the acid in an AP synthesis
where the amount of acid is not critical .

The amount of acid required for HMTD synthesis is the
same amount of acid as would cause the hexamine to
form a salt of that acid , if such a salt is possible ,
for example hexamine dinitrate . This is because for
each mole of hexamine that is peroxidized , two moles
of ammonia byproduct must be neutralized to enable
the reaction to proceed to completion . If a hexamine
salt is used at the start , the correct amount of acid
is present already in the hexamine salt . But if hexamine
alone is used , then an equivalent amount of acid must be
added to form the hexamine salt in solution , and only
a very slight amount of acid in excess . Going too far
with the amount of acid kills the reaction and yield by
favoring the decomposition of the desired product as
fast as it forms , and/or causing the hydrolysis of the
hexamine precursor in favor to the formation of HMTD .

The stoichiometry is quite important for getting good
yields of HMTD . Never "guess" at the amount of acid .
Do the math , and use only the amount of acid required
to perhaps one per cent in excess , but never any generous
excess of theory . The H2O2 used is where generosity
of the amount should be applied , depending upon the
concentration .

[0EZ0]

Rosco, I am inclined to agree with you as to the importance of correct acid ratios in the synthesis of HMTD. I glanced on a similar theory about 12 months ago that there was alot more to the role of acid in the reaction mechanism. It had a little more to do with the reaction of the acid with the evolved ammonia to shift the state of equilibrium toward the formation of HMTD. Unfortunately it was limited due to the fact that no experiments were conducted to see the validility of this argument. At the time it seemed a plausible theory to help explain the situation.

What fueled speculation even more was the mention of the self neutralization reaction of Hexamine Dinitrate in hydrogen peroxide. Most probably by yourself, Rosco. Theoretically the reaction should run more smoothly due to the elimination of unstable intermediate salts of the chosen acid and hexamethylenetetramine and the ideal acid/HMTA ratio. However Hexamine Dinitrate also undergoes decomposition in aqueous solution. The extent of this decomposition I would think quite marked in a warm environment. It is noted that the self neutralization should theoretically be conducted in the cold, I can only assume for this reason.

Isolation of HDN from the reaction of HMTA with nitric acid and then peroxidation should give the best conditions in regards to the ideal acid/HMTA ratio. I guess that this is also the same assumption you made Rosco?

I wonder if there has ever been a paper published on the mechanics of HMTD syntheses. It would be very interesting to see what the findings were. From a theoretical perspective it is all quite interesting. While references to HMTD are far from rare there is little detail in all the literature I have read so far.

[Rosco Bodine]

The importance of the acid to hexamine ratio is a fact
which I have established by experiment , although I did
not chart the yields carefully , I did make sufficient notes
to discover that going even one percent too far with the acid
amount can drop the yield by ten times that amount or more ,
the effect increasing with temperature . What I am saying
is not just a theory , but a reported result which others can
easily duplicate . I generally use more complicated to make
but more powerful and storage stable initiators for tests of
the sensitivity to initiation of experimental composites or
for sensitivity tests of various crystal mesh / loading densities
and column diameters for sample evaluations . HMTD is
sort of an "oddball" initiator that I will try simply as a curiosity
about whether or not it may be useful as a sort of choice
of last resort , useful in some possible field scenario where better
options are unavailable . HMTD is your proverbial "quick and dirty"
initiator for that scenario where expediency and effectiveness
are the priorities , and mild temperatures and near term deployment
will permit the use of HMTD . In a pinch , HMTD will get the job done
so it retains some interest in that regard , even though it is not
practical at all in any other context , except perhaps as a chemical
intermediate , where even in that context it would be unusual .

I haven't checked the yield for hexamine dinitrate used directly .
It may be that the yield is excellent with no added acid at all for that
salt of hexamine . If the yield is below 90 per cent , then on the
next batch , I would suggest adding 3 or 4 drops of HCl or HNO3
to the solution at the start . At some point in the comparisons of
the yields using a very few such small adjustments , the absolute
optimum yield will be found .

HMTD is not compatable with metals , and probably not even compatable
with all plastics , or in contact with some explosive compostions it
may be desired to initiate , so its usefulness is definitely limited . It
is probably best used as a single component cap filler of 3 or 4 grams ,
lightly pressed in a polypropylene capsule , ~10 mm column diameter ,
where it is not even in physical contact with the fuse or igniter squib ,
but fired by a jet which punctures a film of poly covering the igniter .
It is best the HMTD is not in contact with any material , other than its
polypropylene enclosure , and the film covering its igniter . A short
length of heavy wall polyethylene tubing can be wrapped end over end
with several layers of teflon tape , and then the tape can be punctured
on one end to allow loading an igniter charge . This igniter module is
inserted in the bore of the capsule holding the HMTD and pressed against
the HMTD column . When the igniter fires , the jet will blow through the
teflon film and initiate the HMTD . A low order detonating igniter is best
to guarantee functioning , but even a feeble igniter should be able to
puncture the teflon film . HMTD is not by any means an initiator to
be recommended if better alternatives are available , but if it is to
be used , the method described is a logical approach for its use .
Such a cap will detonate urea nitrate and probably would be effective
for other relatively difficult to initiate compostions which would not be
reliably initiated by any reasonable amount of AP .

[SweNMFan]

In some formulas it is stated that the crystals should be rinsed with methanol, but when I did that the hmtd disolved.. Is that what is supposed to happend ? I don't like the idea of getting bigger crystals, it's plenty sensitive to begin with..

[Rosco Bodine]

I never tested the solubility of HMTD , but it is generally of reported low
solubility so it is surprising if HMTD would be that soluble in methanol ,
unless it reacted somehow . But that is interesting , because if HMTD is
soluble in methanol to such an extent without reacting , then you would
have found a good solvent for purification and recrystallization . Because
of the low solubility of HMTD you aren't going to get large crystals from
an aqueous reaction mixture , especially when that mixture is cold .

I have an idea for an experiment to make HMTD by a method that
hasn't been described before , using paraformaldehyde as the precursor ,
which is commonly available as mildewcide crystals sold in 3 or 4 ounce
cellophane packages in hardware and drugstores and some cleaning sections
in department stores . The para is inside a porous paper liner which can
be used to fumigate sealed storage containers in which books , clothing ,
ect. are kept . The label on the package says paraformaldehyde 91% and
the rest inert ingredients , but that is just an industry minimum content
rating , accounting for residual moisture and a little methanol trapped in
the para as formaldehyde solutions polymerize to para during manufacture .
The actual content of formaldehyde in para is closer to 97% . Anyway
the idea for my experiment is to depolymerize the para in alkaline water
and then to add an ammonium salt to the alkaline formalin solution ,
freeing ammonia from the salt to react with the formaldehyde and form
a hexamine solution in situ . The mixture is chilled and added to cold
peroxide and then the required amount of HCl is added and the mixture
placed into a freezer as usual . I have *not* done this experiment but it
should work fine as an alternative to making hexamine separately or
locating fuel tablets and going that route .

Experimental :

18.5 grams of paraformaldehyde are added to 50 ml distilled water .
In small portions with stirring or swirling is added 16 grams NaOH .
The depolymerization of the para and formation of a clear warm
solution should result . If not all the para "dissolves" , it should
dissolve during the next step . In small portions with stirring or
swirling add 34 grams of pure ammonium nitrate . The reaction mixture
needs to be warm to proceed , and supplemental heating should
be applied if necessary . A clear hot solution should be the result ,
having a stinky odor similar to the smell of fish . The solution should
contain .1 mole of hexamine and .4 mole of sodium nitrate byproduct
dissolved in water . Using a jar having a threaded closure chill the
mixture in the freezer . In a separate jar chill 75 ml 27% H2O2 .
If any crystallization occurs in the first solution , no problem .
Pour the cold H2O2 into the first jar and mix with stirring or swirling
until all is dissolved again . Then add exactly 21 ml of HCl 31.45%
in portions to the cold mixture , seal lightly to allow for pressure relief
and return the jar to the freezer for 72 hours . A precipitate of
HMTD should result . Neutralize the mixture with small additions
of baking soda until any effervescence ceases , and perhaps a
slight odor of ammonia is evident from the decompositon of the
slight excess of ammonium nitrate which was used . Filter and rinse
the HMTD crystals with distilled water . Air dry the crystals without
heat , and store the dried material in a sealed polyethylene container
in the freezer . Yield by this method is unknown , because I just
thought of it and have never tried it . Anybody else tried this method ?

[SweNMFan]

I usaly use 20g purifyed Meta tablets, 50ml 30% H202 and 30ml 30% HCL and get 21-23 g HMTD

[Rosco Bodine]

That's not bad yield . You could tweak it a little as follows .
For that reaction using 20 grams of hexamine , try increasing your
amount of 30% HCl to the range of 31.5 to 32 ml and use about
10 ml more of the 30% H2O2 . You should get at least an extra
three or four grams .

[SweNMFan]

Will try that next time.. I only use HMTD for caps.. And since 1g seems to do the trick on NM Plastique that I use, my batches last a while.. When stored in a cool dry and dark place it seems quite stable. (and away from metals)

I did an experiment with the synth.. I dumped in the HCl fast and at room temp.. had a runaway within 1 min.. So ice bath is recommended, nothing fancy just ice cubes seems to be sufficient.

The crystals I get is very small.. almost as fine powder as confectioner's sugar.

[Myrol]

SwedishNMFan: Yesterday I have managed a nice HMTD Synthesis with almost perfect ratios for Acid-Hexamine precourcors. HMTD is sometimes unfair instable, thats why I have such a BIG respect with that powerful stuff.

I mixed exakt 15g Hexamine with 43,3g 35% Hydrogenperoxide and stirred untill almost all Hexamine had been dissolved. The Solution warmed up gradually, I was good prepared, my Ice-Saltbath chilled it within 30sec. down to -11°C!!!! Perhaps it was a little to cold so I tooked the beaker and added 22,4g Citric Acid outside of the Bath.

The Reaction was very lazy, just a dull sense to know there must something happen in the small universe of the molecules :) Ok, today I washed everything and I must say, who hoo, the Yield looks amazing. Looks like more than 13g. Ha haa, I weighed it up, 14,7g! 66% theoretical even with Citric Acid. Im sure it was the high Peroxide concentration.

HMTD is really intresting for me. I thin I will do a yield test wich Acid is the best to make HMTD. I have Citric Acid, Hydrochlorid Acid 30%, Nitric Acid 65%, Sulfuric Acid 70%, Acetic Acid 99% and soon Formic Acid avialable. Six Batches à 2g Hexamine plus 35% Peroxide and the necessary Acid. We will see wich is the best. (but it needs time :rolleyes: )

Edit: Has someone the REAL Explosion Temperature of HMTD and perhaps of AP? I calculated just some unusual mist. 2260°C for HMTD, could be true but 1295°C for AP???? Absolutely to low! Every Explosive has a value called specific Energy wich is given in mt (metric tons). The Formula is: f=n*R*T.

n is the Number of moles Gas wich one kg HE produces in the Detonation.
R is the universal Gasconstant given as 0,0008478 and
T is the Temperature of Detonation in degree Centigrades °C.

If I change to equitation to T I have f/(n*R), this should be the Temperature of Explosion in °C. Well I have done it with HMTD. HMTD has 87,3mt and produces 48,05moles Gas if you take the new Value 1077Liters per kg, not 1400Liters per kg wich was definately to high! Bla bla bla......everything caclulated together gives: 2260°C. I have tested the formula with PETN's values, she is correct! PETN: 124,4mt, 4230°C, 34,81moles Gas per kg.

If someones know the exact specific Energy of AP: Scream it out :D Post it, we all need it.

But now another question: HMTD is quite unstable if mixed with Nitric esters or Metals....Ok, but I want to know if HMTD is even unstable against Nitromethane? It would be great if not, we could mix it 90/10 with NM to get a easiely pressable strong Explosive for small applications. I have a lot of NM here thats why I asked this!

[nuclearattack]

To Myrol:
your post is very interesting! I appreciated it!
About the NM/HMTD mix i don't think it is a good HE. First because the 90% of the mix is a peroxide and this means a weak composition. Second, the mixture is too much sensitive...you are using a primary as a main charge!
Third, a peroxide is not able to sensitize NM so you are wasting NM.
Fourth, if you want to use a primary just use NC with it to make AP putty, and if you want to use NM there are a lot of other compositions that work better. :D
However i have never tested this kind of mixture and this is only my opinion, surely older members are able to make better suggestions. :)

[Rosco Bodine]

It is likely not a good idea to mix HMTD with anything ,
particularly anything organic or metallic . HMTD is unstable .
This fact makes HMTD way more dangerous than AP , in
regards to special handling considerations . HMTD is not
a "substitute" for AP and can't be used the same way safely .
You can make putty and mix it with other things and it will
seem just fine until it spontaneously detonates unexpectedly ,
or more gradually deteriorates predictably .

In very limited uses respecting the peculiar instability of HMTD ,
and using it within sensible constraints , it is a more powerful
initiator than AP . There really aren't a whole lot of bright ideas
which can be safely explored for different ways to use HMTD ,
because of its instability . Trying to apply the same ideas which
are legitimate for AP to HMTD is generally inviting disaster .

[2,4,6-TNP]

Dear Rosco,

It is easy to agree with you! I'd rather use my hexamine to make RDX or HMX. To use, make stable exposives such as Lead Azide;Those who do so I consider wise. Tell it like it is, some explosives are just impracticle!

[Myrol]

Well, yes you all be right. HMTD is for me also just a primary or for very small charges 1-2g cheap stuff. The Idea with the NM cames just BECAUSE I need a energetic slipping agent wich makes HMTD much more easy dense without dangerous pressing (with high pressure). I see this often with ANNM. The single AN powder has a very low density wich is not that useful for brisant application. After adding the NM, the mass is fairly dense and has then the necessary brisance grade!

This is the same wich I want with my HMTD.....I dont want to use Paraffin Oil or something non-energetic shit. NM brings more Oxygen in the system even if it is oxygen lacking, HMTD has a much higher lack of O2 as NM. I think, 8,5g HMTD mixed with 1,5g NM are so easy pressable like 50% AN-Dynamite. Dry HMTD dont satisfyes me really. Even if I press it carefully with some force in a blasting cap, I never got more than 0,9g/ccm. More Force sounds stupid to me. I want my Hands until Im a teethless Grandpa :D . The wet mass is less prone to explode via friction. Has somebody an Idea what sorts of energetic liquids can be added to HMTD? (AVIALABLE ones!!).

APNM is quite nice. I have tested one charge 3,5g in a shotshell, it was significant stronger as straight AP. (3g AP and 0,5g NM). Very good for Detonators but the mix with HMTD sounds a lot better as with AP, but AP is very poor. :(

[Rosco Bodine]

I hesitate to recommend this because of the unknowns
with regard to what *may* occur , and I can't remember
if I tried using the mixed peroxide liquid of MEKP / AP as
a densifier for HMTD . But from a standpoint of chemical theory ,
unless there is some condensation reaction between the
different peroxides to form another compound that is more
unstable , instead of simply forming a mixture , the possibility
occurs that HMTD may follow the general trend which applies
to other organic peroxides , whose mixtures may be no more
dangerous than the least stable individual component in that
mixture . If it was an experiment of interest to me , then
the most likely candidate for a densifier for HMTD would be
the 50 / 50 liquid of coprecipitated MEKP / AP , used in just
sufficient amount to dampen the HMTD and exclude the airspaces
between the solid particles of HMTD when the mixture is lightly
pressed . The potential problem here is that HMTD is likely
soluble to some extent in such a liquid , and this may decrease
the already poor stability of HMTD . It is very possible that the
countdown to spontaneous detonation could start ticking the
moment the materials are mixed , or that the stability of the mixture
could be identical to HMTD alone , or (less likely) that stability
for the mixture could be increased , or that any of the three effects
may demonstrate purely dependant upon temperature . The rule
which governs the mixture on a fall morning may be just the opposite
to the rule which applies later that same day in the warmer afternoon .
I point this likelihood out because such little details could be the
difference between life or death to an uninformed person .

Personally I have no interest in exploring such a scenario of unknowns
involving HMTD . HMTD is sufficiently dense that it produces a satisfactory
loading when lightly pressed as a single material loading of 3 to 3.5 grams
in a 9.5 to 10 mm ID polypropylene tube , where the charge is not in contact
with other materials than its inert poly containment . In my own opinion ,
based upon what extent of knowledge is mine regarding HMTD , such a
scenario is the only way I would ever handle HMTD , and with some reluctance
about handling HMTD at all , even in that one limited way which would seem
sane to me . The other options and possibilities just seem unjustified to me
when the risk of different handling is considered . To get into more complicated
scenarios involving HMTD is an idea I would abandon in favor of applying any
added work to making a different primary which has better stability , safety ,
and storage and handling properties . If HMTD was a practical material then
its use would be recommended , instead of the fact that HMTD is generally
regarded as sort of a choice of last resort as an initiator , included as a member
of a group of other compounds which have failed to have any value for practical
use , because of their undesirable properties otherwise , than just being explosive .

There are probably hundreds of compounds that are highly explosive , but have
absolutely no practical value for use as explosives , beyond their ability to destroy
with predictability the surroundings where they are made , and or the persons
who try to make use of the materials . In a very real sense , HMTD does fit into
that category of impractical explosives , only having usefulness within a narrow
range of conditions .

To put it bluntly , what you think to do or want to do with HMTD , may not
be wise . HMTD has a high potential to maim or kill clever experimenters
who fail to have a rational grasp and respect for its properties , while
evaluating the merit of their ideas for ways HMTD may be used .

[Myrol]

Fuck, yes thats right :( ! Arrghh, Damn, to hell with the HMTD.....shit. I know there are a lot of "Blasters" who have made HMTD over and over again....well, oh Lord......even a Friend from me had a terrible Accident involving HMTD wich roasted him one Finger to a quollen "Bratwurst" (this word does not exist in America its an original german product!).

Ok, I see it doesn't take sense to stretch HMTD with other things wich will make it perhaps more unstable as I can ever imagine. The things with NC-Laquer speak for himself. I think the good old AP is a much better choice mixed with NM as to play russian roulette with HMTD. Wow, great...for what have I ordered 1kg pure Hexamine? Just making RDX and HDN is out of my capabilities. It needs to much Nitric.......Could you all guys not say that somewhat earlier? Now im a little pissed with so much Hexamine, ok 4Liters 65% Nitric Acid is also not less but thats the BLOOD of our Business!

P.s. If someone could be so nice: Where can I find original pictures of "Accidents" from "Youth's Experimental sense". I need sometimes such cruel pictures to refuze what for a dangerous hobby I'm in. I dont have a lot of them but they help wonders if your stupid friend sugests you to make Silverfulminate etc. Showing such pictures stop him almost instanteus to play with NI3 etc. Results from Palestinan are also ok (but dont think Im gory, HMTD reminded me very serious to this what you all explain here!) Thanks for your help! :) ;)

[Rosco Bodine]

HMTD is not a useless material , but it has very limited practicality
within a narrow range of conditions , outside of which it is not useful
and the material loses any value . So long as HMTD is kept within
"the envelope" of its limited practical use , then it does work well
as an initiator . But outside of "the envelope" the value of HMTD ends .
There is nothing wrong with experimenting with small quantities ,
taking precautions and establishing by careful tests what can be expected .
But nothing should be assumed about HMTD compositions which are
not well tested and proven .

It is a similar story for copper azide and silver fulminate , which are
not useless materials , but are only useful within a very limited context ,
which I suppose would make them seem "useless" in a general broader
sense , even though it isn't precisely accurate to regard such materials
as useless altogether . Actually silver fulminate is far more chemically stable
than HMTD , but more sensitive to friction or mechanical stress .
And so is copper azide .
The warnings attendant those two are
well known and justified , so that should help put HMTD in perspective .

[grendel23]

Myrol,
Bratwurst is well known in the US where German heritage is common. Required for a Green Bay Packers tailgate party!
Here is a link for the graphic explosives accident pictures you asked for; http://members.shaw.ca/gryphon223/consequences.html.

[Boomer]

Myrol:
Although you seem to have dismissed the idea: Let me remind you that apart from the (at least two) NC-laquer accidents HMTD once detonated right in front of my face when mixed with MHN/MNT (see somewhere up). Thank god less than a gram, no permanent damage done. :)

P.S: Pic No. 5 from the top is my right hand 11 month ago. Looks a little better now, but typing is gonna stay slow. (Actually it in from someone else, but the injuries are sooo identical to the millimetre on all 3 fingers that when holding a print next to my hand nobody believed it was not the same hand!) :eek:

P.P.S: For someone who really knows about this (medical/military staff): Can pic 5 be the result of 3g flash in cardboard? I suspect the victim told the doc/police etc about an M80 "from the flea market" instead of admitting he made something stronger himself. COB? Small pipe bomb?
And WTF caused the mess in the last pic? 30 pounds DBSP in a 6 inch x 4 feet steel pipe? This one definitely hurt least of all ... :D

[nuclearattack]

Oh my God! :eek:
I have seen a lot of injures in my work because i'm an ambulance driver but the last pic is tremendous! :(
I pray every day for every HE amateur that nobody of us will have this accidents...but praying is not sufficient we must stay sharp and know the safety procedures.
Why not a thread on safety?
I fear a lot primaries and i fear that my NG is not well washed this is why i convert it in dynamite immediatly, i also love ANNM because of it's great stability.
Damn i hope that my ambulance will never make a run for me!

[Chris The Great]

If he has holding it with his hand closed, 3 grams of good flash could probably do that. Also, pic3 is a from a blasting cap, which contains no more than 2 grams of primary, and look at what that did.

The last one could be done with only a few hundred grams of explosive in a thick metal pipe. Shrapnel does wonders to human flesh, as the majority of damage looks to me like shrapnel. Compare how cleanly the head has been cut in half, compared to pic 3 and pic 4. Also, the shrapnel from the CO2 cartridge went right through the kids leg, and he was probably a fair distance (maybe 10 feet as he'd be running like hell). It's a clean cut like the head in the last pic. I could be wrong, not having personal experience with pipebomb and shrapnel injuries.

We do have a thread on accidents....maybe a safety thread would be a good idea.......

[The_Rsert]

Does it give stable salts of HMTD?
Because HMTD is a weak acid and neutralizing with XOH or pure alkali metal will form a salt of HMTD and with the alkiali salts, you can form other salts and, and, and....
But almost they are instable!
Has anyone heard of a stable salt of HMTD?

[Myrol]

Ok, it's clear for now, HMTD is just a good choice for small applications like cratering in your Backyard with 0,5g perhaps. Good buried under mud even this "tiny" amount can blow funny holes :) More than 10g is reserved for ANNM etc. (my last ANNM was a misfire :mad: :o ).

The pictures are not bad! I say, very bad for the individuum, thats sure, but they teach me to do no stupid shit. Some Explosives are so unstable that it isn't it worth to make them or even if, just in small amounts like Silverfulminate or Nitro-gen tri-io-dide. You can just hate this stuff.

More than 10mg are uncomfortable if they detonate in front of you without Earprotection. 2 drops Nitroglycerine confined under Al-Foil pissed my ears so worse........., a slight but audible whistling is stalking my since this fucking day (29.11.02). Durable Noise is a pure torture for me :p , I know its off-topic, but contaminated HMTD can do for sure the same effect :D :(

But one thing is absolutely sure for me: HMTD IS STRONGER as AP. Some say its as same strong as AP, thats true for the Esbitfuel-tablet HMTD but not for the pure version! The pure one is VERY strong (for a Primary!)

[The_Rsert]

Again, lead block expansion an velocity:

Trimeric pure AP, 270ml/10g 3570m/s at 0.9g/ml up to 5300m/s at 1.2g/ml

Dimeric pure AP, 250ml/10g 3570m/s at 0.9g/ml up to 5300m/s at 1.2g/ml

HMTD, 340ml/10g 4511m/s at 0.9g/ml up to 511m/s at 1.1g/ml

So HMTD has very much more power than AP!

Esbit does contain almostly 95% hexa and 2-3% wax(insoluble in H202 or Water). In the producing of HMTD the insolouble wax can filteret off after you have dissolved the hexa in the hydrogen peroxide.

Sorry about my bad english.

[bobsuruncle]

I made HMTD using filtered fuel tablets (Highlander brand), 35% food grade peroxide and 10% dilute sulfuric acid. An initial <1g visco triggered detonator fired.

I recommend disolving the hexamine and filtering the wax in distilled water rather than peroxide, just to avoid contamination because the wax ruined my first attempt.

Anyway, I was wondering if it is possible to use electric matches to trigger HMTD detonators (1g)? Would it be safe to keep the HMTD in contact with the metallic wiring?

http://www.magnumrockets.com/ematch.jpg

http://www.emanator.demon.co.uk/bigclive/smartie3.jpg

[Rbick]

If you can find a way to make sure no metal touches it, go for it. But HTMD attacks pretty much any metal, creating heat and potentially detonation. So I wouldn't feel safe with ANY metal in contact with it. Take a look at the accidents website (http://members.shaw.ca/gryphon223/consequences.html) posted earlier, that made me rethink some of my saftey precautions :eek:

I remember a while ago there was a post by someone who added pictures of how to make a metal blasting cap with HTMD. I think he lined the inside with paper prior to adding the HTMD, and apparently it worked well. Maybe you could have a small BP charge on top of the HTMD but separated with paper or some other thin medium and have the Electric Match ignite the BP first, so you wouldn't have to risk metal touching the HTMD. Just an idea. Good luck.

[stupid939]

It would also be possible to wrap the head of the electric match in plastic wrap, or you could coat it in nitrocellulose lacquer a few times to ensure that no metal (the e-match composition could contain metal too) is left uncovered. Paper may even work, but plastic wrap and ping pong balls are so cheap...

[Charles Owlen Picket]

I think I remember a couple of attempts. One was the use of a drinking straw as a liner for a metal pipe design. Another was the spraying of clear lacquer inside some thin Al (6mm) pipe and sealing with wood / epoxy. All of these could work, I'm sure. But one issue that should be emphasized is that the tube should be sealed. There are so many considerations that peroxides demand; that they are really (IMO) a last ditch material when nothing else is available.

But they work well: HTMD especially. I once saw someone dispose of an experiment of HMTD by making a small firecracker with it. They placed about 3-4gr in a strong tube of cardboard with a visco fuse. It was not compressed. The results were astounding.

Some people don't know that peroxide's can be used as cleaning solvents.....Indeed! They can make fingers and eyes disappear like magic.

[bobsuruncle]

Would glycerin make a good lacquer?

[stupid939]

What Charles meant by lacquer was something kind of like spray paint. Although spray paint is technically not a lacquer, cellulose or resins dissolved in a solvent would be a lacquer. So, nitrocellulose would work, but I am sure that spray paints would work also. Just make sure that they do not contain any metals that might react with the HMTD

[Charles Owlen Picket]

To the best of my knowledge that is correct. However I believe that even metallic paints would be somewhat safe as most all the particulate matter in encased in the lacquer. And many "metallic" paints are not.....they use plastics and reflective particles. but the concept is not a new one.

When mercury fulminate was the standard in detonators, manufacturers often painted the whole of the cap to prevent corrosion. The absolute closest to the material used in modern detonators is the aluminum used in modern archery. This is very high grade Al that is quite brittle. Sourcing your aluminum pipe from arrows is very close to the real thing. The pipe will "shatter" upon detonation as it has very, very little stretch.

In addition the anodizing used in arrow production is also on the inside of the tube (Easton stuff) and does a good job of stopping corrosion from proceeding in itself. But with a coat of lacquer you would almost have a professional level detonator housing.

[Cindor]

Some paints do contain very fine metals powders. Why do you think you can buy powdered Al, among others metal, in a paint store ?

[Bert]

A long, long time ago, I found that a small squirt of silver spray paint into a "beer can cannon" was far superior to lighter fluid in noise production. Partly the more volatile flammable solvents in the spray paint, but also the fine Al powder if you fired it quickly enough.

[Emil]

Hey Guys.

First of all I just want to say great forum, with plenty of interesting topics.

A couple of days ago I decided to make my first batch of HMTD. It was my first time dealing with any High Explosives, after months of research and reading. I used the method which has previously been mentioned in this thread (45ml H202 at 6%, 2 1/2 teaspoons of Hexamine, and 4 1/2 teaspoons of Citric acid), with great success.

After reading posts from members stating some failed attempts at this synthesis, I decided to give it a go. I had minimum equipment for the experiment, thus being very skeptical towards the success, (No thermometer). However in this instance, using a reasonably weak catalyst I was confident there wouldn't be any aggressive temperature rise.

The mix was put in the fridge and left to react after all the additions were made. Being my first experiment with HE's, I was quite excited and anxious to see results, even though I had read to leave the mix sitting at least 24 hours when using 6% H202. With regular checks on the mix, I found nothing for a good few hours. The next time I checked I found a lovely cloudy mixture with two defined layers of HMTD at the top and bottom of the reaction vessel. This was about 7 hours into the reaction.

Being very pleased, I waited 48 hours in total before finishing the reaction to collect the HMTD. I neutralized the batch in a 4% Bicarbonate of soda solution and then washed with water. Due to poor filtering (Not having anything suitable to filter it out with) I didn't collect a brilliant yield, but like stated in previous posts, a estimate would of been 1 1/2 to 2 teaspoons of HMTD, had the filtering gone to plan.

After I let the explosive dry, I headed out to the back garden to do some small experiments with it. I was mainly just experimenting with the sensitivity issue. To my surprise, I found it very interesting that my HMTD would not actually detonate by striking on a smooth material, No matter how hard I struck it. I first tried to detonate it on my shed floor and it did not want to know.

At this point I decided to retrieve a rough house brick where I place a small amount. This time striking it, and successfully detonating it. This lead me to believe that it is much more sensitive to friction than it is to shock. Has anyone else noticed this?

However, I am planning to store my HMTD for a month, and then try again to see if there is any change in performance. I've noted a few times people have said it deteriorates with time.

[Unsunghero]

HMTD is not so good for storage, it decomposes over time, so I would suggest using it pretty quickly after you've made it. Personally I only keep my batches for 2 weeks tops.

I've never tried to detonate with friction or shock, but a lot of people say it takes a pretty good force to set it off. I WILL say it's pretty sensitive to static though, a buddy of mine found that out the hard way.

EDIT: This has been said in this thread more than once already..yeah..

[Chopper]

Gotta say gents,
I've heard time and time again that it doesn't store well, but I've got a dry sample that's been in open air for over a year and it still goes just fine..

I've also got a sample that's sitting in the (mostly) evaporated mother liquor in which it was made, this sample is well over a year old yet there has been no discernible change in either quantity or quality. I haven't ph tested the solution, but I can tell you that it's a saturated solution of citric acid.

On the other hand, a 3 week old sample was rendered virtually useless by careless washing after neutralization. It soaked up lots of water from the atmosphere - to the point of being slightly damp to touch, burned with a coal-like smell and left quite a dark smoke stain anywhere it was detonated.

The only times I've had issues with storage are after neutralizing it and failing to remove all of the neutralizer (I used bicarb). Best bet for storage is to ensure that it is _very_ well washed with plain water after it's been neutralized (though I must admit that the 1yr old dry sample was never neutralized - merely washed with 20 times it's weight, allowing the hmtd to settle before decanting and repeating 10 times. I used 10 batches of 2 litres to wash 100gms.

Yeah - I know 100gms was a less than sensible amount to make.:o

[Emil]

Well that's why I decided to experiment with the storage qualities of HMTD, beings as I have heard so many varied opinions on it.

It isn't a major deal to me, beings as I’m not planning on making a habit of storing a primary explosive anyway. It holds no great advantages. The best idea is to just synthesize it a couple of days before usage. Just more of an interest to see how bad the deterioration is.

I've had my small batch of HMTD for almost 3 weeks now and it still seems very dry, and also has not changed in quantity. I tested a small amount the other day and the sensitivity has not changed what so ever. I'll just hold onto it for a further few weeks and see how it behaves.

[Charles Owlen Picket]

The storage of any non-radioactive material is dependent on a variety of factors. If that material is impure then the factors affecting it's storage characteristics widen obviously. However IF the given material is pure then there really are only a few factors that can influence it decomposition. It's exposure conditions; temp, UV, and gases (or lack thereof - certainly air) are primary in determining "shelf life".

Thus it's almost a given that if a material is stored in a pure state and it's surrounding temp is controlled, not exposed to UV, & maintained in a vacuum it might exist unalterably. There is a hell of a lot of research surrounding energetic materials and their "shelf life". It is extremely important to note that much of this expressed "shelf life" is under storage conditions that are within what is termed "field conditions" & not an ideal situation.

Consider what [design differentiation] would be for "field condition storage" for an energetic material in the 1940's & one delivered from the factory in the 21st century.....

[Cobalt.45]

Thus it's almost a given that if a material is stored in a pure state and it's surrounding temp is controlled, not exposed to UV, & maintained in a vacuum it might exist unalterably.While a vacuum might be OK for some materials, it isn't a panacea for storing energetic materials. Lowered pressures invites evaporation, IIRC.

An inert atmosphere might be an adjunct to or replacement for a vacuum, in addition to the other above-stated conditions.

[Charles Owlen Picket]

While I can't speak to a vacuum in every situation and certainly agree with the concept of no panacea with energetics, I try to pay close attention to the type of packaging that certain things are stored in today vs many moons ago.

You know there is really no way to tell but I would guess that most of what many people say is unstable is simply materials that are subject to the influences of outside conditions or impurities......that's where I was going with the above.

I was a pretty active member of PGII some time back and some guys would talk of making some compositions and using an added "anti acid". Good in theory - but they would not do enough chemistry homework to find out what the addition of a carbonate would do if allowed to remain in contact with the principal ingredients.

If you want to find some really interesting stuff along these lines look at the what was termed "Yellow Powder" in the COPAE (pp 31). It was a composition that should NOT superficially explode unconfined..... but does! [KNO3, sulfur, potassium CARBONATE] The conditions are critical but it WILL explode all by it's lonesome self - providing conditions are right ... and they are quite controllable. Very unique experiment.

[Emil]

Well to anyone thinking of making HMTD, I would highly recommend using a higher concentration of H202 if possible. I've made HMTD 3 times now, the first 2 times I used 6% H202 with the tea spoon method mentioned through out this thread. However, I was receiving bad yields considering the amount of Hexamine and Citric acid I was using, literally just a couple of grams. The experiment was followed correctly as well (Cool temperature through out, leaving to react for at least 48 hours, and no impurities introduced into the reaction).

So I thought it was time to purchase some H202 with a higher concentration. All the hydroponics suppliers seemed to stock it at a 17.5% concentration, so I went for a liter of this.

When I tried my first attempt using the new H202, I used;

315g 17.5% H202, 54g Hexamine and 84g of Citric acid.

Compared to my old reactions I was really not expecting an incredible yield, but definitely an improvement. However, I was shocked by how much HMTD began forming. After 8 hours I checked on the beaker to find ALOT of it.

The next day I filtered the solution and left to dry. The final yield was 48g.
I was really impressed. I know that's around the yield most would expect, however, I was just emphasizing the vast difference between using different concentrations of H202. So to anyone out there making HMTD for the first time, or have been using 6% H202 because of easy access... Save your Hexamine and Citric acid, and get some better H202.
:D

[Enkidu]

H202

Remember: use an 'O' as the symbol for elemental oxygen and a '0' for the number zero. Thus, KMnO4 and KClO3 are correct, while KMn04 and KCl03 are not.

Thus, you must write H2O2 as the chemical formula for hydrogen peroxide, not H202.

[Rbick]

H202!? That's the craziest molecule I've ever heard of! :D Gotta be careful with those chemicals here on the forum...

In response to Emils post: Good to hear about your success. 48g of primary seems a little much though, just be careful! I usually keep my HMTD/AP batches at 25g or below. Anything more is asking for trouble, unless you're planning on setting off one big 48g HMTD charge, which seems pointless.

Also, if you look hard enough, you can find 50% H2O2 on the net for fairly cheap. It may take you a whole 5 nerve racking minutes searching on google. I live in the States, not sure on how easy it is to get elsewhere...

[Emil]

Yes of course, excuse my silly mistakes in the previous post. I'll make sure I correct that this time.

Rbick: Yes next time I will cut the reaction down and use half as many chemicals. If I knew I was going to yield 48g of primary, I would of never have done it like I did. Because of my prior reactions, I was expecting around the yield you said was safer to work with (25g). At least this time I know how much to really expect.

Well, I don't know how other UK residents feel about it, but I think the UK is definitely becoming stricter with chemicals. Finding a good source is getting harder and harder, but I expect it's the same with many other countries. It might be possible to get hold of 50% H2O2 here, but I’m not sure the hassle would really be worth it. At the end of the day, I know I can purchase the 17.5% type with minimal/no bother at all. Most chemical suppliers I've dealt with don't seem interested in dealing with domestic customers, and you usually seem to get treated like a suspect from the moment you call them.

[Rbick]

Yeah the UK is pretty tough about that stuff. Sorry to hear about your difficulties getting chemicals :(.

The amount of primary people consider safe to handle really depends on your saftey measures and what you're doing. If you were planning on making a 50g charge of HMTD and setting it off right away, then so be it (I wouldn't recommend it). Even 25g may seem crazy to some who only make a couple blasting caps a month. As for me, I adjust my yields to how much I think I will be using in the next week. If I'll need 25g because I'm setting off 10 big charges within the next few days, I'll make it. If I don't need it, I get rid of it by the end of the week. I usually stack all of my extra explosives in a pile and set them off all at once if I know I won't be using them for a while. My point is: Its never a good idea to handle and store primaries for an extended amount of time, or handle too much at once.

HMTD is a great primary to use though. It was considered for commercial use as it is very powerful, especially for a peroxide. It was of course scratched due to its sensitivity, which is near that of AP.

[Charles Owlen Picket]

HMTD is a great primary to use though. It was considered for commercial use as it is very powerful, especially for a peroxide.

The actual story of it's commercial testing is an interesting one. Many people whose hobby is reading and studying about energetic materials have found few disparaging issues about HMTD other than it's need for non-corrosive enclosure and some temperature related issues that have more to do with exposure to oxygen than temp fluctuations, per se'. These were however (at the time in history) of much more concern than they would be today.

The story I am aware of concerns the U.S. Bureau of Mines (USBM). Now defunct, but at one time the leading element of research & testing in energetic science. The powers that be, tested HMTD and found it to be a better initiator than Mercury Fulminate. Indeed, it was quite a bit better but could not be exposed to the standard of that day - the copper capsule. As I am aware - it was that reason more than it's shelf life in terms of exposure, that it was dropped. A glass capsule was deemed just too expensive to mass produce.

The background can still be studied if you can find old USBM bulletins and circulars as well as testing criteria from the historical archives at the Library of Congress web site:
http://www.loc.gov/index.html

As a matter of fact some of the most interesting material on energetics written in English from past history can be accessed via the old USBM!

[LibertyOrDeath]

SWIM just got done making HMTD for the first time, so here are his experiences. There's not much new here to report, but perhaps the following will add in some way to the "collective wisdom" on the subject, since sometimes there's conflicting information about these compounds.

Reactants:

80 ml 12% H2O2
12 g hexamine
18 g citric acid

Method:

The method used basically follows that described here:

http://www.roguesci.org/theforum/showthread.php?t=252

The H2O2 was chilled in a freezer until it became partially frozen (unintended). After thawing the H2O2, the hexamine was stirred in until it was all dissolved. This was then placed in an ice bath, and the citric acid was added gradually, with stirring, over the course of about a half hour. The temperature stayed at approximately 5 deg C throughout -- no appreciable increases in temperature were seen at any time. After stirring for another ten minutes or so, the solution was placed into a refrigerator overnight.

About 16 hours later, approximately 1-2 g of crystals were sitting on the bottom of the container. SWIM thought this to be a piss-poor yield for 16 hours of sitting, but he decided to end the reaction right there because his main purpose was to gain familiarity with the properties of HMTD at this point.

First, because SWIM wasn't sure how sensitive HMTD is when wet, he carefully extracted a small lump of crystals from the solution and hit them with a hammer: no explosion. Satisfied, SWIM then proceeded to filter the crystals through a coffee filter. About a liter of tap water was poured over these. Then they were washed with a bicarbonate solution as described in the link above. Finally, they were added to another container for washing with tap water, and this was done until the pH of the wash water went from slightly basic to neutral (tested with pH strips).

The crystals were allowed to dry slightly, then tested for sensitivity. They were very insensitive when wet; it was nearly impossible to get them to detonate with hammer-on-hammer hits, and somewhat less difficult to get them to detonate with hammer-on-concrete hits (probably because of the greater friction involved when the lump of wet HMTD spreads laterally under sudden force against a concrete floor).

After the crystals were completely dry, SWIM began to play with small amounts of them to gain familiarity with HMTD's handling characteristics.

Some findings:

1. Placing a few mg on a concrete floor and then rapidly scraping it with a hammer will set it off almost every time. Placing the same amount on a smooth metal surface and scraping with a hammer will almost never set it off. So the HMTD SWIM made wasn't so friction sensitive that he felt unsafe handling it, but not being a fool, he was careful nonetheless.

2. A very light rap of a hammer against the HMTD on another hammer sets it off almost every time. Hammer-on-concrete hits took a bit more force and often more than one hit, in contrast to the behavior of the wet material, which was more easily set off by hammer-on-concrete.

3. When lit with a flame unconfined, the HMTD burns extremely quickly and with a bright flash, but doesn't detonate. No surprise there.

4. Greater confinement was needed to cause detonation of HMTD confined in Al foil than was needed for ETN! For example, SWIM found that ETN can often be made to detonate merely by pressing a lump tightly between two flat pieces of Al foil (without folding) and then applying a flame. This didn't work for HMTD; it had to be tightly folded in the Al foil.

(BTW, SWIM is aware of the dangers of HMTD and metals, but he was not leaving the HMTD in contact with the foil for any appreciable length of time.)

5. Speaking of ETN, here's what's really strange: 20 mg of HMTD confined in Al foil seemed considerably more powerful than 20 mg of ETN when detonated by cooking off. Does anyone know what that's all about? ETN should be way more powerful than HMTD. Perhaps ETN only low-order detonates unless it's set off with a primary or in amounts larger than a certain threshold? I have read that ETN and PETN have comparable power only in amounts above 2 g or so, and that might be a clue. But has anyone else found HMTD to be more powerful than ETN in these tiny amounts?

[totenkov]

I have only made HMTD twice but quickly moved on because of the poor yeilds like you pointed out earlier. HMTD doesn't make nearly as good use of the H2O2 as AP does. In my opinion, HMTD is slightly more friction sensative, but that is really the only noticable difference.

HMTD is slightly more powerful than AP, and tends to have better initiation ability when compressed, and does have better storability than AP (doesn't sublimate, not made with acetone, which evaporates very easily) But will lodge itself in the threads of a container just like AP. Both peroxides are primaries, ETN is more powerful than both, maybe it looks like HMTD detonates more powerfully, but upon testing you will see that it doesn't.

I have noticed that HMTD actually lets of a small amount of visable smoke upon detonation, this doesnt happen with AP at all!

If you have plenty of H2O2 then go ahead and use HMTD for your primary, I feel safer handling HMTD than AP, however I wouldn't your luck.

[Charles Owlen Picket]

But has anyone else found HMTD to be more powerful than ETN in these tiny amounts?

Two entirely different animals (as I'm sure you know). Comparison of these would be similar to Pb2N3/PETN. ETN is simply a secondary, albeit a very sensitive one (comparison could be MHN). HMTD has very sensitive temp issues in it's synthesis, however it is a wonderfully effective initiator. ...Better than mercury fuminate, perhaps better than azides! ETN on the other hand is a fantastic secondary and [similar to MHN] could cross over to a "primary" in that it could be initiated by a EBW cap design. But that's really where the comparison would end.

If you are working with HMTD, you are working with a very effective [& close to profession level] primary. ETN is a fantastically sensitive secondary. Take a 100mg sample of both and utilize impact on each and you would see they yield a similar "noise" when initiated. Expand the size and they start to drift apart.

ETN at a 20 gram sample level will start to display a shock wave of 7000+ mps while HMTD will stay at about the 5k level. So to address the query directly; if you have a small sample and initiate via an exploding bridge wire or what-have-you, you may not see to big a differentiation. I believe that the HMTD will initiate effectively at smaller weights, however. But that would require testing equipment that is rather expensive & difficult to document. Remember also that the crystalline structure (especially of ETN) has such a large bearing on it's sensitivity and it's response to stimulus that it must be accounted for in any comparison.

Detonation by Fickett may have some mathematical modeling of azides (& possibly of MHN) from which to extrapolate.

[LibertyOrDeath]

Thanks for the responses, guys.

I have noticed that HMTD actually lets of a small amount of visable smoke upon detonation, this doesnt happen with AP at all!Yes, SWIM thinks he remembers seeing that as well.

Another interesting thing he noticed was that upon detonation, a "fishy" smell could be detected -- the same smell normally associated with (if memory serves) the decomposition of hexamine into methylamine (which has the smell) and formaldehyde. (All of his hexamine has that smell, so I suppose some amount of its decomposition is inevitable.)

If you have plenty of H2O2 then go ahead and use HMTD for your primary, I feel safer handling HMTD than AP, however I wouldn't your luck.SWIM will probably investigate other primaries, but it's nice to know that AP and HMTD are easily made if needed. Of the latter two SWIM prefers HMTD, but he really doesn't like its reactivity with metals. That makes blasting cap construction a bit of a pain, though of course it's still very doable.

Right now he's especially interested in DDNP, but of course that's a lot more work because picric acid has to be made first. He'll give it a shot when he gets a chance, and the results will be reported in an appropriate thread. He was also considering TACC because it's been said to be only capable of detonation when confined -- an excellent safety feature -- but that absorption of moisture is a turn-off.

In addition, SWIM is investigating the feasibility of an ETN-only (no primary) detonator, but there's nothing to report on that yet. I do know that it's possible at least in theory, because ETN can be easily cooked off (at least to low-order detonation, if not to full detonation) when completely dry and reasonably well confined. It's just a matter of making it reliable.

If you are working with HMTD, you are working with a very effective [& close to profession level] primary. ETN is a fantastically sensitive secondary. Take a 100mg sample of both and utilize impact on each and you would see they yield a similar "noise" when initiated. Expand the size and they start to drift apart.Ah, that's exactly what I wanted to hear. Because with 20 mg or so, there was no question that the HMTD was WAY louder. (I would definitely be keeping a bit of distance from 100 mg of that stuff going off.) Yet SWIM knows his ETN was reasonably pure, since it melted uniformly into a clear fluid right around 61 deg C.

I suppose the ETN just needs to be of a large enough diameter before that detonation wave can achieve full speed, whereas HMTD detonates to its full potential in very small amounts.

[Sweeper]

Stopp think talking away guys. Megas methos is working fine. A lower concentration of H2O2 will ever yield the same result.

I hate it when i go to a pharmacy and by some hair dyeing and phosphoric acid and much more admixtures make it impossible to manufacture HMTD.

A interesting point, HMTD is very good explosive and to store for long time.
It`s easy to fill it fluffily in a tube and a easy fuse will cause an explosion.

I like the smell of an real explosion and not of an flash !

[hokk]

Of the latter two SWIM prefers HMTD, but he really doesn't like its reactivity with metals. That makes blasting cap construction a bit of a pain, though of course it's still very doable.
You could use a straw instead of a metal enclosure for your blasting cap. I've heard it works very well with HMTD and TCAP, and I got good results with it using DDNP. It's also a bit more comfortable pressing the blasting caps not needing to worry about the metal sharpnel.


Right now he's especially interested in DDNP, but of course that's a lot more work because picric acid has to be made first.
There are a lot of work but its a great experience doing DDNP. But one of the most effective primary to do (if you can get NaN3) is AgN3. Very easy synthesis and good yelds.

[Charles Owlen Picket]

If you have access to a junk yard, you have access to azides. All of these things get simpler and simpler as the sources are understood (and kept from loss!)....

[PETERCPA]

Some paints do contain very fine metals powders. Why do you think you can buy powdered Al, among others metal, in a paint store ?

I got my highest quality atomized aluminum at the art supply store, as a fifth grader. Still buy a bottle when I'm there, for old times sake. They have a big rack of artist's acrylics, oils and pigments all in 1.5 to 2 oz bottles. There is usually a section for metallic paints and metallic powders including every shade of gold, bronze, copper and of course silver and aluminum. The "Silver" paint powder is the aluminum. Costs $1.89 for an oz now. It is extremely fine with the top layer floating in the bottle. In 1959, when I couldn't get my KNO3 powder crackers to explode like Macau crackers, I found a reference in the encyclopedia that said K chlorate or barium nitrate with Al is how modern firecrackers were made. After looking everywhere in the nearby towns, I discovered the Al.

I made a batch of flashlite crackers and they worked like I couldn't believe. I have been going to the art store ever since in a pinch. Often the powder is so light you can't feel it, even if you stick your forefinger in it and rub it between your thumb and finger. There was a book called After Dinner Science that detailed a spontaneous combustion reaction in it -AL + I2 +H20 . The Al powder also worked fine there. If you were an active experimenter, the right pharmacist would usually sell you what you needed. Half of them were pyros, anyway. The lbs of McKesson KNO3 were always on the shelf near the back. It was (is?) a diuretic for sheep and large pets - give 1 teaspoon. When the pharmacy ran out of sulfur flowers, you could always get a sulfur candle and crunch it up with a hammer. I always wondered what kind of crazy would ever light sulfur candles in their house. PeeYou. Come to think of it, I still do wonder...

This is my first post. I have been lurking for a year or so. I know I'm not meant "to ask until I have given" but if anyone knows why someone would ever burn a sulfur candle in their house, I would love to know. It would be the end to a fifty year mystery. I tried one of those candles in the fifth grade boys room and I'l tell you, it was not a big hit at all.

[megalomania]

Sulfur candles are used for fumigation, originally to disinfect hospitals, or what passed for hospitals in the 19th and early 20th century (sickhouses I guess). They can also keep rats at bay, hence their use in homes. They fill the area with sulfur dioxide gas, which kills just about anything exposed to it long enough.

You are supposed to seal up the building, light candles in all the rooms, and get out. They work like those fogger cans you can buy at the hardware store meaning you do not want to stick around and breathe the fumes once the thing gets going :)

[Yafmot]

If you have access to a junk yard, you have access to azides. All of these things get simpler and simpler as the sources are understood (and kept from loss!)....

I'm Having a rough time making the connection here. Is there some part of a modern automobile where azides can be scrounged?. The airbags, maybe? other than that, I'm stumped.

By the way, the beads from the old style catalytic converters can be used for many types of surface catalysis. as they contain Platinum Group metals with a lot of surface area. Just make sure the thing hasn't Been either chemically poisoned, like from lead, or themally poisoned, where the Alpha Alumina shifts to a Gamma phase, and glazes over the catalyst, as well as allowing it to dissipate into the ceramic matrix. The "honeycomb brick" type can also be used, although you can cut 'em up with a bandsaw and a Do-All blade. If theyre caked in Carbon, just hit em with an Oxidizing flame from an O-A rig. Or, if you want 'em really clean, send 'em out for a Cold Gas (Oxygen) plasma treatment.

[Charles Owlen Picket]

Yes, If you have a "rich" junk yard (wrecking yard) near you then azides are no problem - that's what I mean. However: PM me as I don't want to post sources anymore. If you work at it, a 500gr bottle of sodium azide in about two hours of work away.

Quite realistically automobiles are a very good source for a lot of things. Everything from high voltage parts to azides and metals - a good junk yard can pay off quite well IF you work it well.

[plutobound]

Most airbags do not contain azide based gas generants anymore and haven't for a few years (toxicity issues). You'll have to go for older models.

Watch out for pressurized bottles. Many current airbags (particularly sides) contain gases at pressures as high as 9000 psi. These can be drilled, but I wouldn't want to cut them open. Plus there isn't anything useful inside.

[Charles Owlen Picket]

There are specific years and types (pm only; let's keep them available!) that yield a rich level of material. Most everything from 2001 forward is not azide propelled. There is a group that will get about 200 grams per unit - that's what is appropriate.

The best method to open them is with a -=very large=- vise. The slow squeeze will allow for a leverage to get beyond the spot welds in their make-up. Units from a certain American manufacturer are IMO, the best as they have no method to pop except an electrical signal. Thus they seem safer to open. Others have a series of sensors that make them (again, my opinion only) more of a danger.

My personal place is the "pick-a-part" type junk yards as you can go about your business with no one fucking with you. The tools needed can sometimes be a problem but some of these places have electrical access, etc.

[dhemor_]

Hmm.. Here's something that popped into my heard recently..

Many people emphasize the fact that HMTD should NEVER be brought near a metal, as it forms extremely sensitive salts. To what degree are these salts considered sensitive? Would it be safe to assume, at least as sensitive as HMTD? Or even moreso?

I'm interested in knowing this, because it would give us the perspective of how dangerous the salt is (in regards to friction and shock), if it is made. I mean, what degree of sensitivity are we dealing with; as sensitive as HMTD..? AP? Ammonium Triiodide?

[Emil]

The mere fact that it's a general rule not to contact HMTD with a metal really answers part of your own question. The salts formed are certainly going to be a great deal more sensitive than HMTD itself, otherwise it wouldn't be a problem. The degree of the sensitivity?? Well I would assume most of the people who know this answer are either not with us, or are have a hard time typing these days.

In other words, it isn't worth worrying about. You don't want to further sensitize an already highly sensitive primary, so it shouldn't be considered at all. I would imagine the salts formed are more sensitive than AP, but personally have no interest in finding out. It might not just be more friction and shock sensitive either. It's quite possible it becomes temperature sensitive which is worse, beings as this is not an easily controlable factor.

I know metal caps are probably the most practical. But just as good caps can be made from other materials just as easily. Small glass test tubes are probably a popular choice, as glass reacts with basically nothing.

[dhemor_]

Aye, I didn't set out with a practical approach in mind ;). True, glass would be a safer alternative I think. Probably the best with regards to safety. I am stuck, at the moment, using a plastic straw :(.

[Charles Owlen Picket]

Don't quote me on this as it's from memory but the USBoM 1902 tests used Bake-O-Lite tubes that were reinforced with ridges along their length.

Once upon a time someone made a "firecracker" from HMTD and the results from a cardboard tube were impressive to say the least. It made very fine quality flash appear as black powder in comparison.

[drsx]

I think, HMTD does not form salt with metals (it is an amine, not an acid), but some metals catalytically breaks the peroxide bond.

[Yafmot]

So what's the big problem with using plastics? There's how many different varieties? Teflon, for one, doesn't react with much of anything. Ditto most grades of Nylon. UHMW polyethylene tends to stay intact, as well as other grades. I got about ten feet of 1/4" ID Nylon tubing for about $3 at Home Depot. Using a heat gun, or even a carefully handled butane torch, you can twist off the end to a point and have a perfect seal on one end.

So HMTD reacts with metal. So what? there are plenty of other materials that are more than adequate for this application. (And by the way, Charles, that's Bakelite, not "Bake-O-Lite." In fact, It's the direct forerunner of modern Phenolics which, among other things, are used for exhaust nozzles and exit cones on many missiles, as well as the heat shields on the first three US manned space programs. And the original Bakelite company is still doing business in Germany under the same name. And it's pretty damned inert.)

Anyway, I probably shouldn't get started on plastics. Ive been in aerospace composites for over 30 years, and I tend to go on incessantly about it without much encouragement. Suffice it to say that I just don't see why HMTD's reactivity with metal is such a big deal. Just don't use metal. Simple!

So, whaddaya' think?

[-=HeX=-]

Yafmot: You see, there is a common myth amongst newbs that detonator cases MUST Be copper or aluminum tubing for I to provide the correct confinement for the DDT to occur. This, of course, is not true. Also, seeing as they like the metal pipes, and most of them are stuck with either HMTD or TATP, and TATP being so bloody bitchy, they prefer to use HMTD and there is your problem.

Also HMTD is stupidly unstable and should be clasped with TATP as 'Dont even bother' and a new primary should be sought. There are many ways to make sodium azide easily OTC, and by easter I will have made my azides document available. But why not DDNP? Just avoid peroxides, please.

[totenkov]

HeX is quite right. I used to use the flexible copper tubing for blasting caps in my early years of HE. Any metal pipe packed with a high explosive especially peroxides is exceeding dangerous. I even cringe at the carelessness I had around these things in my own beginnings. Lucky I still have all ten fingers.

Metal may be used because with the production of flying shrapnel and a tougher casing, it may be thought to be a more powerful detonation, however I have nothing to back up my case, as I have only used blasting caps where they were absolutely needed.

I think the safest is a paper casing. I'm talking ordinary printer paper. Provided you are not tramping around in some shit infested marsh where is raining, paper makes an excellent casing, 98% dets I would say, based on the fact that I do ocationally make a faulty cap. Next is straws and pen casings, then spent .303 casings for bigger dets.

If you are thinking of experimenting with HMTD, I recommend you try, with very small amounts (less than 5g) and start doing tests. Get an idea for its sensitivity and how it reacts. Its important for people to fear and appreciate HE early on, and understand the damage they can cause, learning with peroxides maybe a good thing.

[Emil]

HMTD, like Hex stated, is often quite wrongly judged. It's name has been cursed because it is always compared to that of AP. It is actually quite a good primary and alot of people don't seem to understand it and mark it down as as unstable as AP which is wrong.

One or two small test sample from 7 months ago are still nice clean, bright white, dry powder which perform as good as it did day one. Not even recrystalized, just washed with Bi carbonate soda once. Not stored air tight either. Does that seem like the charecteristics of a stupidly unstable explosive?? I beg to differ.

My outlooks on primaries is at the end of the day, they are called primaries for a good reason. There is no such thing as a "safe" primary as their main duty is to be somewhat sensitive to shock,friction and heat. But I would still warn people not to use that rubbish they call AP.

I would personally warn against using metal materials for caps on a whole. Even with more stable primaries, there could still be nasty sharp pieces of swarf in your pipe (especially copper and Al tube) which could set it off at any given time. Most plastics serve well, and if you want to look flash, use glass (small test tubes). Like totenkov said, even paper or cardboard is good enough.

[-=HeX=-]

Emil: I was making the point that HMTD is dangerous shit that I class with TATP. In my experience, I only made HMTD twice, and was not pleased with it so I didnt make it since. Yes, chemistry of powder and explosives makes the point that it is a good primary, but it is most certainly not. It is just too sensitive.

Personally I prefer azides, double salts, and DDNP as my primaries as they perform better and are also much safer. I also only use half a gram of primary there days in a compound cap. Think safety guys, and enjoy the full use of ten digits. Even minor accidents are debilitating.

[Emil]

HMTD has very sensitive temp issues in it's synthesis, however it is a wonderfully effective initiator. ...Better than mercury fuminate, perhaps better than azides!

If you are working with HMTD, you are working with a very effective [& close to profession level] primary. ETN is a fantastically sensitive secondary. Take a 100mg sample of both and utilize impact on each and you would see they yield a similar "noise" when initiated. Expand the size and they start to drift apart.


Well you obviously had a bad experience with HMTD, but I'm not the only one who recognizes it's strong points. I have never found mine too sensitive at all, it takes a decent whack, or quite a decent amount of friction to set it off. However you must make sure it is acid free to get a decent product. AP is useless when it comes to storage, but HMTD stores very well if pure.

I recognize that there are better substitutes, but materials such as DDNP have long and picky processes for synthesis, which is ok if you have the time, materials to make it. I personally want to experiment with some other primaries soon. I have some silver nitrate so am looking to make some Silver azide. Should be interesting.

[-=HeX=-]

Emil: it IS an organic peroxide... So I therefore class it as dangerous. My bad experiences were with TATP mostly, however HMTD just frightens me after it went off so easily in the hammertest and I am a purity whore.

DDNP does have a horrible synth, but for safetys sake its worth it. What is more important to you, a few hours less in the lab or your fingers? I hope its your fingers... Also, silver azide is an excellent primary, expensive but so worth it. I only had a small bit but I loved it.

[totenkov]

This is off topic, but on your point of silver azide, acetylides may be something to look into, they are in the realm of the home chemist. Those who do not have access to sodium azide get screwed here. Take a look a the Silver acetylide thread. After 4 years I have yet to be able to initiate it with a hammer or drop test, flame however, that's a different story. :p

[Cobalt.45]

Personally I prefer azides, double salts, and DDNP as my primaries...OT, but how's the 'OTC lead azide' synth coming along?

[-=HeX=-]

Well, the extraction from cigarette loads is coming along nicely, so far 15 to 20 of them ground down carefully has been enough to detonate ETN, the problem is that they are only a small bit lead azide and a lot of dextrin. Its more extraction than synth. Is dextrin soluble in acetone or water? lead azide is not so that could be a viable extraction method.

[Alexires]

UTSFE - "Dextrins are water-soluble..." from the Wiki article.

From what appears to be the MSDS "Dextrin is soluble in water but is precipitated by alcohol"

I'd say water is a good way to go.

[-=HeX=-]

Thanks Alexires, I knew I had asked a newb question, once I get more of the cigarette loads I will use water to dissolve the dextrin binder and filter out the (Supposed) lead azide. Once that is done I will dry it off and use it in a cap as a test. I know that the stuff is a Damn good primary already and believe it to be an azide, if not lead azide.

Dont worry, testing will be soon.

[Yafmot]

Hex, I believe those loads are Silver Azide.

[Cobalt.45]

What's in those little "Penny Poppers"? They look like a little tissue ball with a tail. They have ~ 1.5mm bits of sand coated w/what I always thought was silver azide.

[ex1ge]

There has been threads on them in the past ("Penny Poppers" as you described), and I believe the general consensus was that the explosive contained was Silver Fulminate, which is unfortunately too sensitive for practical application.

[-=HeX=-]

Yafmot: thanks for informing me on which azide it is, Well in my opinion silver azide (For the experimenter) is better than lead azide. Now lead azide gives the same performance when cleverly dextrinated, but that is not so easy for us to do. That is why silver azide interests me so much.

The silver fulminate can be extracted from the snaps with ammonia I believe. However it is far too sensitive for practical work.

[thelasttrueone]

Ok forumites, lets talk HCl. As of yet I have never found and citric acid OTC. With HCl in such great abundance I have decided to just use that. However I think there may be a problem with using HCl in HMTD synthesis. When I add my HCl my reaction mixture bubbles. I also noticed that there were two layers of crystals in the reaction mixture just before I filtered it. Lastly the reaction mixture turned slightly yellow at times during the reaction. These observations, combined with the fact that HCl reacting with hexamine is a known way to produce methylamine make me suspect that HCl causes nasty side reactions, possibly the production of ammonium chloride which would dissolve into the water used to wash the HMTD.

My starting reagents were: 70 mL of 27% H2O2, 15g of hexamine purified from camp stove tablets and 22 mL of 31.45% HCl. My procedure was the one described many times in this thread. Once the product is done drying I will report it's weight as well as properties.

[-=HeX=-]

Hmmm the hydrochloric acid never caused problems who I made it, and now you have tempted me to synth the shit again. I will make two or three batches with various acids before halloween. One with sulphuric. One with hydrochloric and one with citric if I can find any.

I will have to get more hexamine first though, I used most of it camping :D

[Cobalt.45]

I've read that mineral acids caused problems, even ascorbic acid has been said to form unstable compounds, though there's no empirical examples I have been able to find.

Ascetic and citrus acids are all that I've been able to be certain of, so TLTO's results should be interesting.

...and 22 mL of 31.45% HCl.BTW how did you come up with 22ml of HCl?

[thelasttrueone]

Earlier in the thread (page 11?) someone had ratios that used 27% H2O2 so I used his ratios. Also, the weight of the product was 18 grams and it behaves like HMTD (burn, explode).

[Alexires]

When I add my HCl my reaction mixture bubbles.

Is your mixture cold? Because I would say this is from spot heating/heating in general that breaks the H2O2 down to O2 and H2O, hence your bubbling. If you don't keep it cool, you will possibly have a run away, bubbling H2O2 and HCl everywhere.

[Yafmot]

Sorry Hex, but I screwed up on post # 345. The cigarette loads contain Silver FULMINATE, not Azide. If I were you, I'd plan on getting rid of it. Or maybe there's some way of transferring the nitro group onto Mercury or some other substance.

Perhaps there's a way of loading small quantities into those plastic caps for toy pistols that come on a ring or a rack, although it'd be pretty easy to tear the gun apart, which itself might make for some good video.

[thelasttrueone]

Hmm that may be the cause of the bubbles, I let my reaction get to 40 degrees C before I ran to get cooling. I'll have to do another batch with proper cooling.

[Rbick]

40* C? :eek: That is much too hot. You'll be making formaldehyde, ammonia, and oxygen gas at that temperature. Formaldehyde is a known carcinogen, so we probably want to stray away from that. With HMTD, keep the temp at no higher than 5-10*C. Preferrably 0-5. The higher it gets and the longer it remains above the recommended temperature, the lower your yield will be.

I know its tempting just to dump the Hydrogen Peroxide into the mixture and get it over with, but you should take your time. Just remember to watch the temp and keep it cool while letting it react.

I also noticed a lot of animosity towards HMTD in some of the previous posts. I've been working with it continuously for years and never had an issue. My secret? Small quantities, purification, and careful handling. HMTD is indeed an effective primary that is worth your time if you're willing to give it the respect it deserves.

As for metal casings for BCs, I haven't used those in a while. I stick with straws unless the situation dictates other wise. With liquid explosives for example, I don't use straws but use test tubes since the open end of a straw can leak easily unless sealed really well.

[-=HeX=-]

Sorry Hex, but I screwed up on post # 345. The cigarette loads contain Silver FULMINATE, not Azide. If I were you, I'd plan on getting rid of it. Or maybe there's some way of transferring the nitro group onto Mercury or some other substance.

Perhaps there's a way of loading small quantities into those plastic caps for toy pistols that come on a ring or a rack, although it'd be pretty easy to tear the gun apart, which itself might make for some good video.

:EEK: So I carried a tube of 500mg Silver fulminate pressed on top of 5 grams ETN in my pocket on a bicycle for 2 miles to my blasting site and STILL have my legs? Now thats odd... I did not find it exceptionally sensitive like the silver fulminate from 'drop pop's' was. I am still inclined to think it was the azide but I will take your word for it, anyways I recently managed to order 100 grams sodium azide :D

Back on topic of HMTD, today I found a film can of it in my lab. It was as good as the day I made it and made a nice bang when I set it off with a cap taped to the side of the can. I detonated it buried in the garden and only heard a small 'thump'. Still, it was just more 'ordinance disposal'.

Any European members who want a source for Azide, PM me.

[Hephaestus]

Synthesis and Observations of HMTD

1. In a glass container, 250ml of 40 volume Hydrogen peroxide (12%) was cooled to a temp of -2C in an ice/salt bath.
2. Slowly, and with constant stirring, there was added 28g. of "Esbit" brand Hexamine (2 tablets). The temprature never went over 0C.
(There is quite a bit of "foam" floating on top of the solution, and some fine white particles in suspention)
3. After all soluables were in solution, the solution was vacuum filtered to remove the wax left behind.
(You must use a vacuum filter, it will never gravity filter)
4. After returning the beaker to the ice bath, there was added, in 5g portions, 42g of chilled Citric Acid over a period of 10 min. Stirring was never halted.
(The mix appears to be cloudy)
5. Stirring was continued once every 15 min over the next 3 hours. During this time the solution was kept in the freezer.
(Still looks cloudy, with tiny particles in suspension)
6. After the 3 hours the beaker was moved to the refrigerator where it was stored, undisturbed, for 18 hours.
(now there is quite a bit of PRODUCT in the bottom of the beaker, and some floating on the top)
7. The beaker was given a good stir and allowed to stand at room temp for 15 hours.
(almost all of the product is now floating on top of the liquid. it appeares to be a loose mass, slightly foamy)
8. The solution was poured into a coffee filter and allowed to gravity filter over the course of 2 hours.
(it takes a very long time to gravity filter)
9. The now empty beaker was rinsed with 100ml of water, and the water was poured over the HMTD in the filter.
10. The HMTD was then rinsed with 100 ml of 91% Isopropyl Alcohol.
11. The final product was spread out on a glass platter and allowed to dry at room temp. Yield: 15g.

[Emil]

Hephaestus

Always make sure that you neutralise your materials with a sodium bicarbonate solution to destroy most of the remaining acid. I know that you rinsed it with isopropanol, which sounds like you just poured the alcohol over it in the filter. But It is very important to add your product to a 5-10% solution of Sodium Bicarbonate and stir for a good few minutes. Sometimes people even repeat the step a few times. This makes sure that all your product is under the solution, as rinsing is a very hit and miss way to do it. You are likely to leave bits missed out.

I’m very you surprised that you stated gravity feeding less than 500ml of solution took over 2 hours.... It should only take around 5-10 minutes most. Maybe your coffee filters you are using are to thick. I use the unbleached (brown) ones, which seem to filter very well.

[-=HeX=-]

HMTD is very dangerous to use when pure, and when it still has the acids mixed in, its just too unstable. It however is the best peroxide, and was considered for use in commercial caps. I do not have the figures on me, but it performs better than mercury fulminate in COPAE, and I was surprised to see DDNP being better than Pb(N3)2 in the sand crush test, it was even better than AgN3. I wonder is sand crushing ability really the best test of initiatory capabilities. I personally doubt it, however I am currently researching the matter.

I am still searching for data on initiation so if anyone has any data which includes HMTD I would be grateful.

[Hephaestus]

Emil
thanks for the tip. I have read conflicting reports about using bicarb on HMTD. Some say that it reduces the shelf life. I just took 1g of my HMTD (2 days old) and stirred it with 25ml of water. It came back completely neutral. On the other hand, I used the same proportions with Citric acid and Water. It came back with a pH of about 6. This is probably the 10th batch of HMTD that I have made, and Ive never had any issues with storage. I still have caps I made about a year ago using 5/16 aluminum tubing pluged with bondo. They still survive an 8ft drop onto concrete with no problems. Im not saying that HMTD should not be rinsed with bicarb, im just saying that Ive never had any problems with not doing it. Any additional input would be appreciated.

[ginkgo]

Hi guys, am about to synthesize my first batch of HMTD! I've got some ETN, and thanks to people on the ETN thread, I now have some confidence in making HMTD.

Problem however is the hexamine. I've got these fuel tablets from a company called Mill Com. I tried to google this brand to find out what they put in their fuel tablets as I highly doubt its pure hexamine. But google came back with nothing, I belive some companies use wax as some sort of binder.

Now the question is, how does one purify the hexamine from these tablets? I've tried googling it, and went upto page 35 in the results but didnt get any info! Also I think it may also be mixed with trioxane, so I need a way to remove all this gunk before I can synthesize my HMTD.

Any help would be appreciated.

[Hinckleyforpresident]

First off, had you UTFSE here you would have found this:

http://www.roguesci.org/theforum/showthread.php?t=6713&highlight=hexamine+extraction

Second, I would recommend going to the manufacturers website, and either finding or requesting an MSDS for the tablets in question. They are required to tell you what's in them. With the information they provide, you should be able to find an adequate solvent for extraction by UTFSE.

[ginkgo]

Do not quote whole posts.

Believe me, I have tried to find the manufacturers website, but for some reason they dont seem to exist!! The manufacturer is a company called mill com, try google it see what you find! Its not any of the companies listed, I went all the way to page 15 after which the results make no sense as the word mill or com is nowhere to be seen!

Also, has anyone tried making HMTD by just crushing the fuel tablets and using them as is, impurities and all? I know this could have the potential to be rather unstable?

[Hinckleyforpresident]

Believe me, I have tried to find the manufacturers website, but for some reason they dont seem to exist!! The manufacturer is a company called mill com, try google it see what you find! Its not any of the companies listed, I went all the way to page 15 after which the results make no sense as the word mill or com is nowhere to be seen!

I am very reluctant to believe that a camping company has managed to stay completely off the internet's radar. Post a picture of the box that they came in, maybe that will help find the MSDS.

[ginkgo]

There we go, here is a picture of the box that they came in, I have really tried hard to google and find the website or contact details of this company.