Hexamethylenetramine Dinitrate

[A-BOMB]

I copied this out of AlENGOSVIG1's .pdf call myfile. Does anyone know anything about this explosives properties? Or even what typ of explosive is it.

Hexamethylenetramine Dinitrate:

Materials:

50g of hexamine
287mL of 34% hydrochloric acid
100g of ammoniu nitrate

Procedure:

1) Add 287mL of 34% hydrochloric acid to a beaker.
2) Add 100g of ammonium nitrate to the beaker and stir until it all disolves.
3) Cool the beaker to 0 degrees Celsius in an ice bath.
4) While vigorously stirring, add 50g of finely powdered hexamine and stir until is all dissolces.
After it dissolves, a white prcipitate should form almost immediately.
5) Quickly filter out the precipitate and let it dry.

<small>[ May 29, 2002, 01:14 PM: Message edited by: A-BOMB ]</small>

[Madog555]

look on mr cool's site for some good info on yields ect. the yields with the NH4NO3 method suck. i have made it twice.

here is some info that i was provided with by Mr Cool. thanks!

myn was white and i washed it in acetone. yieilds for 5g of hexamine were like ~4.1g

Colorless crystals, soluble in water, insoluble in alcohol, ether, chloroform and acetone.
gross formula: C6H14N6O6
molecular weight: 266.2
energy of formation: -393.2 kcal/kg = -1645 kJ/kg
enthalpy of formation: -422.1 kcal/kg = -1766 kJ/kg
oxygen balance: -78.3%
nitrogen percentage: 31.57%
heat of explosion: 788 kcal/kg = 3297 kJ/kg
melting point (decomposition): 158*C = 316*F
lead block test: 220 cm3/10g
impact sensitivity: 1.5 kp m = 15 N m
friction sensitivity: 24 kp pistill load

it is of medium sensitiveity and isnt taht powerful. i once used some to fill excess space in a detonator when i didnt have enough PETN and i needed it to be full to have the detonator operate correctly.

[mr.evil]

i've used the methode below, i used 60% HNO3 and it worked, i will try it with 70% also...
When adding the HNO3 to the mix, and i cool it suddenly all crystalls apear in one second, the first time i did it i looked something like this: <img border="0" title="" alt="[Eek!]" src="eek.gif" /> now i think it's kinda cool :)
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> )a) Hexamethylenetetramine Dinitrate (with HNO3, much better yield)

You will need:

14g of hexamethylenetetramine,
20mL of 70% nitric acid,
Distilled water,
Three 150mL beakers,
A thermometer,
A filter funnel,
Filter papers,
An ice bath,
A fridge,
Acetone.

1) Dissolve the hexamethylenetetramine in 100mL of water in one of the beakers (it will help if you heat it up, to around 80*C). Put it into the fridge after it's all dissolved, and cool it to around 5*C.
2) Measure out the nitric acid into another 150mL beaker.
3) Slowly, while stirring with the thermometer and keeping the temperature below 5*C (with the ice bath), add the nitric acid to the hexamethylenetetramine solution.
4) After the nitric acid has been added, cool the solution to 0*C.
5) Filter out the precipitate, and add it to 100mL of acetone in the third 150mL beaker.
6) Use the thermometer to crush it up and stir it around under the acetone.
7) Filter out the solid, and leave it to dry. Protect it from moisture.

</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">

[da man]

I've also made this explosive using the 70% HNO3 method, it worked very well, good yields of course. It isn't VERY powerful, with a V.O.D between 6000-7000 m/s, but thats not bad considering how easy it is to make. The major problem i have with this exploaive is that it is very hogroscopic, not as bad as ammonium nitrate, but if you leave it out overnight, it will be pretty wet the next day. So you will have to dry it in the oven, on low, about 60*C.

[cutefix]

Da man ,How did you get such a high detonation velocity for hexamine dinitrate(6000-7000m/s)?

[Mr Cool]

I believe Philou mentioned a figure for VoD like that here a while ago, or on alt.engr.explosives. I thought it was quite high at first, but I think it could reach 6 km/s despite its very negative oxygen balance because I expect that the structure of hexamine is fairly stressed, so it'd release quite a lot of energy upon detonation.

[mongo blongo]

It just so happens that I just made some. The yield doesn't look that bad (made it with HCL and NaNO3). I will be trying to make some RDX out of it when I get some free time.

[Zambosan]

The second procedure with nitric acid sounds an awful lot like RDX, with a lower concentration of HNO3, and no heating. I have to ask, why would you make HDN instead of RDX in the first place, if the precursors are practically the same??

[Bitter]

Any ideas about the sensitivity of this stuff ?

[Mr Cool]

Zambosan: Some people can't make RDX because they can't make good enough HNO3 (no distillation equipment), and HDN is a quick, easy explosive to make if you just want a bang, and aren't too bothered about power.
HDN can also be used to make RDX if you get it dry enough; half the nitric acid required is already in the crystals, so you don't need to distil as much HNO3.

[A-BOMB]

Thank you, guys because this sound like a nice explosive for me to use in strenghting caps because of the use of hydrocloric acid,AN (NH4NO3), and hexamine. All chemicals that I have in mass quanties, unlike HN03. And does anyone know if its conpatable with metals, or AP,HMTD?

[DBSP]

I've allso made this explosive using the NH4NO3 HCl method. I still haven't detonated any of it. I made it last august when the HMTDN thread was active. I've got 7-8g, how much do you think is needed to detonate it using AP in a metal pipe?

[cutefix]

Qoute:
"I thought it was quite high at first, but I think it could reach 6 km/s despite its very negative oxygen balance because I expect that the structure of hexamine is fairly stressed, so it'd release quite a lot of energy upon detonation."

There is indeed a reason to believe that theoretically, it can have a detonation speed in the vicinity of 6000-7000 m/s,as confirmed by calculations.
However this is not a reliable yardstick for explosive performance.
Does any of you were able to compare its performance with ANNM which is the nearest material for comparison.?

[da man]

A-BOMB, from my experience with Hexamethylenetetramine dinitrate, it is compatible with all things that i have used it with, acetone peroxide, HMTD, and metals. I don't think it is a very reactive chemical, like ammonium nitrate, so it should be fine with most things i think.

[mongo blongo]

Hi
I was just looking at my HDN that I made yesterday. Some of it has disappeared (still had a bit of HCL in it because I didn't wash it because it would dissolve the HDN).
I know why this happened but there was a funky smell coming from it. I took a closer sniff of it and it fucked up my nose and my throat is stinging a bit! Does anyone have an idea of what this(decomposition?) gas being evolved from it is? (Not HCL because I used 15%)
Next time I will wash it with acetone or something

[Mr Cool]

The gas is formaldehyde, nasty stuff.
If you get it very dry then almost none seems to come off.

How have you guys been drying yours?

[Microtek]

When I make HDN for use in RDX synthesis, I wash it in cold ethanol or acetone which it is almost insoluble in. Drying is then no problem.

[mongo blongo]

Thanx Mr Cool, I thought I recognized the smell.

[Zambosan]

Mr. Cool: Thanks! Interesting to know.

<small>[ July 18, 2002, 12:08 AM: Message edited by: Zambosan ]</small>

[Madog555]

people use HDN for a substitute to hexamine while makeing RDX, you dont need as mutch HNO3 and the yields are supose to be better, ect.

[cutefix]

I am likely to agree with you.
If you can make HDN with lower quality acids and were able to extract good yields with it;then You can save a lot of the precious pure nitric acid for its conversion to RDX.
As I do not find HDN to be a worthy explosive to play with,and for me its value is worthy only as an intermediate to the preparation of other powerful explosives(HMX and RDX).

[Madog555]

i have made HDN twice and i only used it in detonators to take up space when i was low on PETN

[nbk2000]

When your hobby is homemade explosives and weapons, cancer is the least likely thing to kill you. <img border="0" title="" alt="[Wink]" src="wink.gif" />

[Mr Cool]

Concerning the R-salt to RDX reaction: I actually distilled the NH4NO3 and H2SO4, and used the HNO3 formed, but forgot to edit the method. I only realised recently. So if you try that NH4NO3 + H2SO4 mixture, be careful...

HDN isn't very bad, not compared to other things common in even home-labs. I suppose it combines the toxicity of hexamine and HNO3, but it's not as bad as HNO3 because it isn't volatile or easy to splash into eyes etc., and hexamine is a base so even if it does get in your eyes it wouldn't be as bad as free HNO3.

[mr.evil]

i'm scared to get cancer, does nobody of you guys do? :confused:

Hexamine dinitrate is a funny explosive, but when the crystalls did have disappeared, you must filter it VERY quickly or it will disappear(form a solution with H2O)
i guess put the reaction fluid with the crystalls in a buchner funnel and rinse it with Alcohol or acetone, so the water will evaporize and leave dry crystalls, as it isn't soluble in alcohol, acetone(and chloroform)

<small>[ May 31, 2002, 12:33 PM: Message edited by: mr.evil ]</small>

[mongo blongo]

Yea I use an improvised buchner funnel because I find normal filtering too slow (and a bit tedious). After I add the hex, I stir it for about 30 secs to make sure all hex is dissolved and all the HDN has enough time to form. I have weigh the yield and it was 93% (based on the hex used) which is quite good. I have just wiped up another batch and when it is dry I will have a go at making RDX with it.

[mr.evil]

i've made Hexamine dinitrate, but everytime is was to slow with filtering :p , so i will look for a buchner funnel...

[Mr Cool]

When I occaisionally make it, it has always ppted in fairly large crystals. These don't need to be filtered, you can just put them into a sieve with small holes (a tea strainer works, but it's a bit small) and let the water drain out. Much quicker than filter paper, and you don't lose much. In fact, you may lose more by having it sit around in the water for hours while it's being filtered...
Then, you can use a bit of strong, fine cloth to get most of the remaining water out. Put the HDN onto the middle of the cloth, wrap it up and squeeze it HARD. Lots of water trickles out. Then put it into lots of acetone, strain and squeeze again. Then leave it out to dry.
It can be dried further in a dessicator over conc. H2SO4.

[mongo blongo]

To dry my HDN, I open up the filter, put it on some absorbent tissue and place it on a hot water bottle.
Anyway- I just tried to make some RDX with my HDN. YEEAAA! It worked very well. It's filtering right now and the yield looks VERY good! My HNO3 was not even that good (orange/yellow colour). The addition of the HDN was quite easy (controlling the temp) but when I heated it to 55 deg c it started to get a bit mad and hectic and hard to control the temp. I accidently splashed bit of the solution onto my finger and thumb and I have quite a nasty burn but it doesn't hurt to type. When it's dry I will weigh the yield. From looking at it now it looks around 6g (from 9g of HDN). This is much better than directly nitrating Hex.
C-Ya

Edit- Ok, my finger is starting to hurt now! :mad:

<small>[ June 01, 2002, 11:26 AM: Message edited by: mongo blongo ]</small>

[DBSP]

Has anyone got the chemical formula for HDN?
I'd like to know so that I can do some calculations.

[Mr Cool]

C6H12N4*2HNO3, or C6H14N6O6.

[Zambosan]

Thanks everyone. So the procedure is identical, other than substituting HDN for the hexamine. Mongo blongo: did you happen to write down your procedure? I'd like to know the amount of HDN & acid, etc. if you have it and don't mind typing a little more on that burned fingie... (hope it heals soon! <img border="0" title="" alt="[Wink]" src="wink.gif" /> )

Mr. Cool: You write the formula as C6H12N4*2HNO3, similar to how I'd write a hydrated complex (e.g. CuSO4*5H2O). Are coordinate bonds being formed between the hydrogens on the HNO3 and something on the hexamine molecule? Correct me if I'm wrong: The H-N bond in HNO3 is ionic, so there's a net positive charge on the hydrogen, similar to the polar water molecule, so I imagine it would be attracted to all four nitrogens on the hexamine tetrahedron. Since the HNO3's would be "bridging" multiple hexamine molecules together, they are "shared", with a ratio of 2 HNO3's to each C6H12N4 molecule.

Note - sorry I "think out loud" so much; I'm trying to grasp the fundamentals of some of these syntheses, and don't have any formal instruction to go on. So if some of what I'm going on about is just patently obvious to a lot of you, I apologize... you're all my teachers here, thanks for all your patience! :)

[mongo blongo]

Zambosan- No problem dude.
Wiegh out 60g of the best conc HNO3 you can make in a glass beaker and cool (In an ice bath) to 20 deg C.
Start to add 20g Hexamethylenetramine Dinitrate in small amounts and stir well. Keep the temp between 20-30 deg C (make sure all the HDN dissolves before you add more) Even when the HDN has dissolved, there will be some bubbling so wait until it stops . This bit should be easy to control the temp.
When all the HDN has been added, you need a hot water bath to heat the react mix to 55 deg C. Then you need to put the beaker in the Ice bath to cool it to 50 deg C. You should use this to keep the temp between 50 and 55 deg C for 5 mins.
This is when the mad stuff happens (in my experience).
I find it quite hard to keep the temp between these temps.
When you heat it to 54 deg C, then cool it again because the temp still rises and when it cools to 51 deg C start to heat it again.
The heating period should be for about 5 mins. If the temp goes over 60 deg C then it starts to bubble loads and it could turn into a runaway reaction.
When the heating period is over, put the beaker into the ice bath and cool it to 20 deg C quickly. Then take it out and let it stand for 10 mins.(no longer because RDX will start to break down)
Fill another beaker with 100ml or more with cool water and dump the reaction mix into it. You will instantly see a beautiful white precipitate of crude RDX.
I would recommend a buchner filter to obtain the best yield of RDX because it still decomposes a bit when in the water+react mix. Wash it with about 200 ml cold water and then with 50 ml 10% sodium bicarbonate solution to nutrilize the remaining acid. Wash again with 50 ml water.
Purify with acetone. (Mr cool has a good way of adding the bicarb when dissolved in the acetone to neutralize acid because the crystals have voids inside them which still contain acid)
Good luck dude :)
Post results :)

Edit- My finger is still yellow but I have to wait till the dead skin peals off. It doesn't hurt anymore. Thanks for asking :)

<small>[ June 03, 2002, 09:34 PM: Message edited by: mongo blongo ]</small>

[mr.evil]

Hey,
i've maked HDN yesterday again, but this time with 40% HNO3, SUCCES!!! no change in yeild etc. And strange thing was; the crystalls didn't form a solution with H2O in a few seconde(like always) so i could filter them all out in a fine sieve, and wash them with alcohol(i also store the crystalls in Aceton as HDN is very hygroscopic) :cool:

anyway, this afternoon i will make some RDX with it! :D

[mongo blongo]

The RDX is still a little damp and weighs 16.3g so when compleatly dry it's probably about 15.5 or something. I like this method <img border="0" title="" alt="[Wink]" src="wink.gif" />

Edit- It will depend on how good your HNO3 is. Mine was not that good.

<small>[ June 04, 2002, 12:05 PM: Message edited by: mongo blongo ]</small>

[mr.evil]

DBSP:
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> Has anyone got the chemical formula for HDN?
I'd like to know so that I can do some calculations.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">i've scanned a page of my Chemistry of Explosives(page 125) You can see the structure of HDN on it... <img border="0" title="" alt="[Wink]" src="wink.gif" />

(copy and past link)
<a href="http://www.geocities.com/tshadowpp/HDN.html?1023272237320" target="_blank">http://www.geocities.com/tshadowpp/HDN.html?1023272237320</a>

[DBSP]

Thanks, you could have given me the page in the book since I have COPAE, but I appriciate the effort.

[Madog555]

mr. evil, cool, thanks for posting that.

[mr.evil]

No problem <img border="0" title="" alt="[Wink]" src="wink.gif" />

Anyway, you can download the file from the FTP(i thought) if so, it will take a long time to download it :rolleyes:

[xtreme]

I have tried to make Hexamethylenetramine Dinitrate with the NH4NO3 / HCL methode.

My NH4NO3 does not disolve in the HCL (30%) ?!
I also have questionmarks by the purity of this methode because there must be NH4CL formed in the solution (if this methode works)

Somebody have succes with the NH4NO3 / HCL methode?

[mongo blongo]

xtreme- You got some strange stuff going on there!
Does anyone know if any HMX is produced in this method? Of so, does anyone have any rough ideas on how much will be produced as a percentage. I am thinking there will be as much produced as there will be in the K-process since xNO3 is added to form HDN as an intermediate just before the destructive nitration.

[cutefix]

Mongo I hope that this piece of information helps:
This was the procedure developed by Bachmann ,Wright et al in the late 1940’s.
In order to make HMX from HDN you have to convert it to the intermediate DPT.
A.Hexamine dinitrate to Dinitropentamethylenetetramine(DPT).
1)“ 0.10 mole of hexamine dinitrate(HDN)( 26.6 grams) and 0.92 mole of 90% H2SO4 (90 grams)wee mixed together over a 30 minute period.The reactant are added proportionately while stirring well at 8-15degC
2)When all the reactants were added to thereaction vessel,it is then maintained at 15degC with stirrring for 45 minutes.
3)Pour it into a 400 ml of ice and water.Filter.
4)Neutralize the filtrate to a pH 5.6-6.5 with 28% aqueous ammonia solution.The yield is 0.31mole of DPT.

B.Conversion of dinitropentamethylenetetramine(DPT) to cyclotetramethylenetetranitramine.(HMX)
1)Prepare a solution of 44 grams of NH4NO3in 47 ml of 98%HNO3,until the liquid is clear and ceased bubbling(gassing).
2)In a 2 liter three-necked flask equipped with a thermometer and mechanical stirrier was placed 100 grams of DPT and 460 ml of acetic anhydride.
3)Heat the resulting slurry to 60degC by means of a water bath.
*4)Add the nitric acid/ammonium nitrate solution over a period of 10 minutes.The temperature being held at 60-65deg C.
**5)Then the mixture is stirred while at 60-65degC for one hour.After 3 minutes of the completion of the reactant addition,crystals of HMX will appear.
6)At the end of one hour,the water bath was removed and the reaction mixture was allowed to col until it reached 50degC.
7)Add 400ml of cold water rapidly with stirring.You will notice that as cold water was added the temperature fall to 40deg C,and then rose t0 90degC.This was due to the hydration of acids mixture which creates the heat.
8)The reaction containing the slurry of crude precipitated HMX was heated under reflux(with condenser)in a steam bath for 12 hours.You will notice considerable gas evolution(consisting mostly of formaldehyde).The purpose of this step is to digest most impurities including unstable linear nitramines..
9)Cool the reaction mixture and filter.Actual yield was 102 grams of HMX which melts at 272-276degC.This corresponds to a purity of this crudeOctogen as 90% HMX and 10%RDX.
Notes:
*During the addition of HNO3/NH4NO3 mixture,you will note in the first 5 minutes a highly exothermic reaction.It was necessary to keep bath temperature 20-30degC.However during the last 5 minutes of reactant addition,the bath temperature rose to 40 degC requiring more cooling.
When the reaction is already half done,the mixture becomes clear and no trace of DPT remains.But as the addition is continued the mixture will become opaque.
**Heat was evolved for 5-10 minutes after the reactant addition is done;therefore care must be observed in controlling the temperature of the waterbath.

[mongo blongo]

Thanks Cutefix! That's an interesting process but I can't try it because I have no Acetic Anhydride and probably never will. :(
There is a way to separate HMX and RDX from a patent I once read. Maybe I could try that and work out how much HMX was present.
I wonder if there are any such linear nitramines that are produced in RDX processes which could make it more unstable.

[ALENGOSVIG1]

Ive got another method for DPT some of you might be interested in. cutefix's method is easier, but this ones probally cheaper. The procedure calls for 28-30% ammonia solution but mabe you could use a less concentrated solution.

Materials:
21g nitrourea
120 ml 37% formaldahyde solution
200ml 5% sodium hydroxide solution
250 ml 28-30% ammonia solution

Procedure:
add to the nitrourea to the formaldahyde solution and heat it to 45 celsius and stirr untill all of the nitrourea is dissolved. When it has alldissolved, take it off the heat and let it cool to room temperature. While stirring, add 200 ml of 5% sodium hydroxide solution and continue stirring for 1 hour. While, stirring heat the mixture to 65 degrees celsius for 1 hour while stirring. Remove the mixture from the heat source and let it cool to room temperature. Slowly add 200 ml of 28-30% ammonia (could probally use more less concentrated ammonia). Filter off the precipitate and set it aside. Add 100 ml of 28-30% ammonia to the filtrate and filter off the precipitate. Combine the precipitate and wash it with 1L of water.

total yeild is around 11 or 12 grams.

[da man]

Do you think that RDX could be produced with hexamethylenetetramine dinitrate, using potassium/ammonium/sodium nitrate with sulphuric acid, if you use the theoretical proper amounts to convert all the sulphuric acid? I think i remember reading a post a long time ago, by Mr. cool (i think) that said it could be made this way. Or can RDX be made this way from DPT as in cutefix's method for HMX without the acetic anhydride, and using a sulphuric acid and a nitrate instead of pure nitric acid?

Any help is greatly appreciated!

[mongo blongo]

You can oxidize Cyclotrimethylenetrinitrosamine into RDX using H2SO4 and xNO3.
If you are trying to make RDX from HDN this way it won't work because H2SO4 will decompose the intermediate products. If you converted all the H2SO4 to HNO3 then I don't know but you could try to filter out the HNO3 and add xNO3 again to be sure it's all converted but the resulting HNO3 would unpure. If it does work it will be a shit method.

[cutefix]

Qoute:
----------------------------------------------------------------------
I wonder if there are any such linear nitramines that are produced in RDX processes which could make it more unstable.
---------------------------------------------------------------------
In RDX synthesis,by direct nitration the main by products are formaldehyde and ammonia(which came from the central structure of hexamine ),about half equivalents or three CH2 and one aza nitrogen. Which is liberated directly as gaseous by products.
While if you convert it to HMX you will start with the 4 aza nitrogen intact.If using the pathway by means of DPT,methylene group decomposition is gradual.From the original six CH2 in hexamine or hexamine dinitrate it will be reduced to five CH2 in DPT.In which subsequent nitration (and acetylation) will liberate the fifth CH2 on its way to the formation of the tetranitramine structure.
Here in this stage a small part of the DPT will straighten out(uncyclisize) forming upon the presence of acetyl nitrate(from acetic anhydride and nitric acid) into linear nitramines which are explosive as well but not as stable as the cyclic nitramine HMX .These conditions is emphasized if the reaction temperature rises more than65 deg C. The result will be more of these linear nitramines and lesser yield of the cyclic nitramines.If these reaction by products is not remove it will make the resulting octogen very sensitive(and unsafe to use) aside from the fact that some of the isomers of HMX formed are more of the very sensitive (delta and gamma HMX which is as sensitive as primariy explosives) and not the alpha or the much more desirable and low sensitivity beta isomer.
BTW and example of the linear nitramine is the the1,9 diacetoxy 2,4,6,8 tetranitramine.
CH3COO-CH2-NNO2-CH2-NNO2-CH2-NNO2-CH2-NNO2-CHCOCH3.These product being less stable will decompose gradually.Any unreacted DPT is decomposed in this process also.
Further there is aquestion about using alkali nitrates instead of nitric acids.If applied to HMX by DPT intermediate,these will also favor formation of liear nitramines as catalyzed by alkali acetates(from reaction with acetic acid in the reaction medium).It can be a possible alternative for improvised RDX synthesis but the yield I anticipate is much lesser.

[pyromaniac_guy]

previous post ---

"HDN isn't very bad, not compared to other things common in even home-labs. I suppose it combines the toxicity of hexamine and HNO3, but it's not as bad as HNO3 because it isn't volatile or easy to splash into eyes etc., and hexamine is a base so even if it does get in your eyes it wouldn't be as bad as free HNO3."

No offense to the poster, but I think it's worth pointing out that this is an extremly dangerous and stupid philosophy to hold. A compund is not as toxic as it's constituant precursors. dont forget that CN is just carbon and nitrogen!!!!

[Zambosan]

Mr. Cool was stating that the toxicity & hazards presented by HDN are lower than most laboratory compounds, AND that it is safer than its precursors. Not making a blanket statement that reaction products are always safer than their precursors, which is what you are mistakenly accusing him of.

<small>[ July 18, 2002, 01:05 AM: Message edited by: Zambosan ]</small>

[vulture]

Look, hexamine was and is being used to preserve fish and to treat certain excretion or kidney problems. It's however banned in most industrialised country's because of the hazard of formaldehyde (=methanal), one of it's decomposition products.

[pyromaniac_guy]

Yes I realize the poster was saying that the material in question was probably less hazardous than other lab chemicals, but then he goes on to specifically say that it's toxicity is probably less than that of the reactants. on what grounds is that argument made? just because the product is not as volitile as the precursors, or because it cant be splashed into the eyes as nitric can, there may very well be other hazards that can not be identified based on the precursors...

I'm sorry if you have a problem with my pointing out a potentialy very unsafe way of thinking... better safe than dead i always say.... but if i ever notice you say something int he future that might end up getting yourself killed, I'll be sure to keep my holier than thou mouth shut! :)

[mongo blongo]

No one said anything about predicting hazards from precursors! Even though you can!!
As it stands HDN is not as dangerous as some other chems that we may use,including HNO3.

[Mr Cool]

Pyromaniac_guy: I know that CN- is just carbon and nitrogen, but perhaps you are not aware that they are joined by covalent bonds - you know, shared pairs of electrons?
In HDN, no covalent bonds exist between the hexamine molecules and the nitric acid molecules, therefore a solution of HDN is a solution of HNO3 and hexamine. Since the only way it could enter your blood/tissues is as a solution, it's toxicity will be similar to that of hexamine and HNO3. However, since it is not volatile etc., it will be safer to handle than HNO3.
I made no general comment that compounds always combine the toxicity of their precursors. Therefore what I said could only be dangerous to people like you, who are incapable of comprehending it and therefore take it as a blanket statement.

[cutefix]

Hexamine based explosives are considered toxic ;that includes RDX and HMX.Lesser nitrates/nitroderivatives of hexamine share the same defect(including HDN and DPT).Although its difficult to find LD50 information of these derivatives.
But does it make a difference?
You are not making food stuffs here;so why worry about getting poisoned when you will not consume internally your creation?
If you have handled these chemicals for long;then you know the precautions …. Regardless of the degree of toxicity for a certain component.

People who worry much about getting poisoned with his experiments must find another hobby(or career);say for example cookery… :D
That is a cool undertaking as well :cool: .

[nitriees]

I try to make HDN by H2SO4/KNO3/Hexamine.
Dissolve KNO3 into H2SO4 stir vigorously.
After all KNO3 dissolve, add Hexamine slowly and stir.
Let the solution sit for 1 hour, two layer appear with clear liquid
on top and white (fine crystal) layer on bottom.
Filter out the crystal and let it dry under sun for whole day.
The powder seems like never dry (may be hygroscopic).
I put a small amount into flame for 30 seconds, it seems like can not
be burn at all.(so it can not be a hexamine i guess)
I am not sure whether this is HDN?
If i press it into cap together with HMTD even a bit wet, can it be detonate?

[mongo blongo]

Dude, I have never seen a method using H2SO4! I would have thought the H2SO4 would decompose the HDN? You should use HCL and add the Hex all at once (not slowly)!! You should filter as quick as you can (let it sit for 1 hour??)the HDN will start to dissolve. You should wash it with acetone if you want it to dry quick. If you put it in a flame then it will not do anything (It's not a primary explosive).
It should be detonated by HMTD if it is dry enough.
I hope this helps :)

EDIT: look at Mr cool's web page for a good method.

<small>[ July 09, 2002, 11:14 PM: Message edited by: mongo blongo ]</small>

[DBSP]

I've just made some HMDN, using MR COOLs method with HNO3 only recalculationg the ratios for 62% HNO3 instead. Damm it's so easy this way it doesn't take more than 5 minutes to finnish it. And it precipates so quickly. It's allmost dry now since it's rinsed with acetone. I'll weight it as soon as it's dry.

I used an AN/water bath to chill the reaction (very effective) the reaction got as cold as -5 degrees, then I added the HNO3, quite quick since the temp didn't rise very fast, when I had added half the HNO3 the HMDN just fell out of the solution within a second or two. I'll try to make RDX with some of it tomorrow using XNO3/H2SO4 instead of HNO3, worth a try.

<a href="http://w1.478.telia.com/~u47804009/E&W/cold_bath_by_DBSP.JPG" target="_blank">http://w1.478.telia.com/~u47804009/E&W/cold_bath_by_DBSP.JPG</a>
<a href="http://w1.478.telia.com/~u47804009/E&W/HMDN_precipate_by_DBSP.JPG" target="_blank">http://w1.478.telia.com/~u47804009/E&W/HMDN_precipate_by_DBSP.JPG</a>
<a href="http://w1.478.telia.com/~u47804009/E&W/HMDN_drying_by_DBSP.JPG" target="_blank">http://w1.478.telia.com/~u47804009/E&W/HMDN_drying_by_DBSP.JPG</a>

[mongo blongo]

I think someone had a go at xNO3 and H2SO4 with HDN to get RDX a while back and it didn't work. The H2SO4 will decompose the HDN and fuck evrything up. It's a shame though.

[Microtek]

DBSP: I see you have been to Denmark. Matas is a nice shop, isn't it ?
The HDN can be washed with acetone to remove remaining water and nitric acid. This also makes it dry quickly.
For converting it to RDX, distilled HNO3 is neccessary but it doesn't have to have the NO2 removed.

[xoo1246]

Great DBSP, I'm going to Denmark too soon(in a few weeks). So, you are back from your vacation, did you fire anything off in the north?
But as mentioned higher up, if you use excess nitrate, so that most of the H2SO4 reacts, couldn't it work? If you react the H2SO4 and the nitrate before you add it to do the HMDN.
Microtech: Do know what kinds of chemicals matas can supply you except HNO3?

<small>[ July 23, 2002, 01:48 AM: Message edited by: xoo1246 ]</small>

[mongo blongo]

It is not absolutely necessary to remove NO2 from the HNO3. If you do it will increase the yield as NO2 will do some oxidizing itself leaving a little less intermediates to recondense into RDX. Adding Urea will also produce more HNO3 molecules which of course will increase the yield further.
Personally I can't be arsed to add Urea because my HNO3 is light yellow and there is not much NOx. It takes enough time to make the damn HNO3! Leaving it in an open beaker bubbling oxygen through it evaporates quite a bit of the HNO3 so it's just not worth it unless you have large amount of NOx present in which case I would just throw it away.

[Microtek]

Xoo: They have quite a selection when you consider that it is just a beauty shop. I can't remember them all but here's a few: 96% H2SO4, 100% acetic acid, anhydrous NaOH, tartaric acid and oxalic acid, 85 % glycerol, KNO3, sulfur powder, CaC2, citric acid, etc., etc.
Many of the names on the chemicals are archaic latin ones, so you'll have to figure out what it really is. There's usually also a more conventional name in small print ( in Danish ). Also, note that not every shop sells the same assortment of chemicals.

[xtreme]

Today I have (tryed) made RDX...

First I have made HDN by Mr.Evil methode (almost neighbours):

14 gram hexamethylenetetramine
20 ml HNO3 (38%)

Not a high yield....but ok, it's just a (first) test
HDN....not realy a problem

Then a convert it to RDX following mongo blongo (post 446) methode
Because of my low yield I have scaled everything down bij 50%
HNO3 = something like 95% I think (distillation 50:50 HNO3 65%/H2SO4 98%)
Keeping the temp (54 gr.C) wash not a problem....put just only the bottom of the glass beaker in the warm water bad and it will be much more under control (heating goes slower) <img border="0" title="" alt="[Wink]" src="wink.gif" />

Ok.....but then....filtering

I put the solution (HNO3 + hexamethylenetetramine = RDX) in the cold water (50 ml/5 gr.C). YES.....white precipitate ! :)
It looks like a good yield :D

But when filtering.....the Acid warmed up because of the addition of cold water :mad:
Then the acid (filtrate) and RDX (filter) start to bubble NO2
damn !! :mad:

Because I dont want again HNO3 al over te kitchen I dumped the most in water......what a wast !! :( So far....so happy.....why ?!

Now I have a very little bit of RDX.
I go to test it with some AP....just to see of it is RDX (no experience with RDX)

Next time.......more cold water (100....150 ml) and hope this will work. Thanks all for the usefull information about HDN/RDX ! <img border="0" title="" alt="[Wink]" src="wink.gif" />

[mongo blongo]

When you precipitated the RDX did you add the HNO3/RDX to the water or did you add water to the HNO3/RDX? If you add water to an acid it could boil up! Maybe that's what happened. If you did then next time add the HNO3/RDX to the water. Also make sure the water is very cold (I put it in the freezer until there is a thin layer of ice on top).

EDIT-What were you using as a filter? The HNO3 left over could have reacted with the filter. The acid is more dilute but I have had it react with my filter paper before! When I precipitate the RDX I add some sodium bicarbonate to neutralize some of the acid before filtering it.

<small>[ July 24, 2002, 04:24 PM: Message edited by: mongo blongo ]</small>

[xtreme]

I have HNO3/RDX to the water (I know...NEVER put water in strong acids)

The water was cooled to 5 deg.C
Neutralisation before filtering.....ok, I shall think about that
I think....first more water, then neutralize it with NaHCO3, water again and then filtering. I think I going to buy a buchner filter for faster filtering.

How long it takes the RDX to breakdown or to desolve in the water ?
Does it matter if I used....500ml of cold water (more time to filter/more stuff to desolve) ?

[Mr Cool]

If your "RDX" is dissolving or breaking down in water then it's not RDX, it's still HDN.

[xtreme]

Thanks Mr.Cool

So, I have all the time to neutralize it before filtering it !
Happy to hear that.....I allready making HDN again :)

I know RDX is much used for blastingcaps.
Is HDN usefull for blastingcaps too (in combination of Mercury Fulminate) ? I "hear" someone used HDN for blastingcaps instead of PETN (PETN = stronger than RDX :confused: ).

[kingspaz]

PETN and RDX are pretty well equal. HDN may be useful in blasting caps depending on how easily initiated it is. also its hygroscopicity may be a problem. but if loaded in a dry environment and sealed with wax then it should last some time in storage although tests would have to be carried out.

[A-BOMB]

HDN is not as hard to detonate as AN, but more difficult to detonate than PETN. It's like Pottassium chlorate in detonatablity.

[mongo blongo]

Xtreme- Simple test: Dissolve your product in acetone. If it dissolves then it's RDX and if not then it's HDN. :)

[xtreme]

My HDN is drying at the moment.
Tomorrow I going to distillate some HNO3 (HNO3/H2SO4) again and make some RDX again and test it with acetone.

Today I donate my very little RDX of yesterday.
It was to little to get a good impression of sound/power
How sounds RDX ? :)
Is it likely MF, AP, ANNM, .... what can I expect ?
Is it as painfull as ANNM for my ears <img border="0" title="" alt="[Wink]" src="wink.gif" />
When the results of the RDX are OK, I think I go to use it for blastingcaps. It's a littlebit expensive to make in large quantity's for explosives ("ESBIT" fuel tablets are not cheap and I have not very good yields of HDN)
I think that ANNM will be my favorite at this moment.
ANNM for boosters (ANFO detonations) & shaped charges.
RDX for powerfull blastingcaps.

[mongo blongo]

RDX= LOUD!!!
I'm wondering why people are getting such low yields for HDN? My yields have been around 90-95%(from 10g Hex batches using HCL and NaNO3). It could be that most people use NH4NO3 which is very soluble and leaves more room for the HDN to dissolve than there would using NaNO3. I also use a Buchner filter which can filter a batch from above in about 7 secs. My HCL contains detergents and is 15%. That's the only differences that I can think of. Maybe I'm just lucky. :p

[xtreme]

I have tried the NH4NO3/HCL methode
I used HCL with a concentration of 30%
Nothing happened....totaly nothing :(
NH4NO3 did NOT react/desolve with the HCL :confused:

I haven't NaNO3....but have someone tried KNO3 ?

Now I'am using HNO3 38% because I haven't a buchner filter at the moment and the HDN wil not disappeare (Mr Evil and I have the same HNO3). But filtering is not realy necessary so perhaps I can try HNO3 65%

I shall do some test later this day.

[mongo blongo]

Your NH4NO3 won't dissolve in your HCL?? Something is very wrong! KNO3 will also work.

[xtreme]

Damn !

My drying HDN vaporates in the air !! :mad:
I realy don't like HDN (bad yields, desolves in water and vaporates in the air).

42 grams Hexamine.....not 1 gram HDN

I think I go to try making TNT what is much less expensive.
Or is there a better way to make RDX without HNO3 99%....

[mongo blongo]

The trick is to get the HDN dry as quick as possible. While the HDN is wet it has a hydrolyzing effect on it which will decompose it. It will give off formaldehyde gas which to my expense I found when smelling it. <img border="0" title="" alt="[Eek!]" src="eek.gif" /> I wash it with acetone so it will dry within about 10 mins on a hot water bottle. It is a tricky procedure but with a bit of experience you will get a feel for it. It is a shame you are getting such bad yields.
"42 grams Hexamine.....not 1 gram HDN" <img border="0" title="" alt="[Eek!]" src="eek.gif" />
I can't think for the life of me what's going wrong. That was using 95% HNO3 as well? Are you 100% sure about the conc of your HNO3?
Have you tried it with KNO3 and HCl yet?
If you are getting such bad yields of HDN then I would advise using the normal destructive nitration of Hexamethylenetetramine. Oh yes you have NH4NO3 so you could try the K-process for better yields. <img border="0" title="" alt="[Wink]" src="wink.gif" />

[xtreme]

Yes, formaldehyde is coming off from my HDN, I can smell that.
My first part I have dried with acetone....yes that goes much faster.
I'am sure of my concentration of HNO3 38% (have 20 liter can from a agricultural shop, very cheap). I have 65% also (lab grade, very expensive)

ok.....a shall try it with other methods (KNO3, HNO3 65%)

[DBSP]

I don't know if someone has pointed this out before, as HDN dissolves in water it is natural for some of the HDN to dissolve in the liquid from espesially NO3/HCl. If the hex. doesn't dissolve fast enaugh the formed HDN dissolves before all hex is added, which in turn gives "shit yields", even though the yield actually might be very good. If you have no precipate after the addition of the hex, just boil all the liquid off and I can guarantie you that there will be plenty of HDN waiting for you. I know this from experiense. And as you can expect about 1,5 times as much HDN as hex, you most likely have about 60g of HDN dissolved in your bath, try evapourating it!

[xtreme]

I allready tried to vaporate the water/acid by slowly heating
This is not working. The HDN contains a lot of water/acid and when heating it desolves in the water/acid it contains, forming formaldehyde gas. The combination of HNO3 vapours and formaldehyde gas is neasty for eyes and nose. But on the first part I add acetone to dry and then slowly heating will work a lot better.

[mongo blongo]

You could try dumping the solution into cold acetone or ethanol to precipitate the HDN but it would be expensive.

[xtreme]

ok.....this looks like a MUCH better yield :)
Now I don't desolve the hexamine in water but put it spoon by spoon straight in the HNO3 38% (water/ice-bad and stirring solution). The temp. rises but it stay's under 20 degr.C
It looks that the HDN doesn't desolve in the solution anymore...so far

I let it cool to 0 degr.C (or lower) and than.....I think I will dump it in a acetone solution (have enough acetone, so w.t.f)
I don't care of the acid....I have 20 liters HNO3 38% :D

I hope this works.....

<small>[ July 27, 2002, 01:16 PM: Message edited by: xtreme ]</small>

[xtreme]

ok...yields are good.....but....

I can't dry HDN.
After filtering I washed it with acetone and put the HDN in a beaker.
When I slowly heat this it looks like it melts and doesn't get solid after that :confused:
The vapors are realy terrable voor eyes and nose :(

Is it possible to convert the HDN to RDX with stronger HNO3 directly without drying ? Or give the containing water problems in contact with the strong HNO3 ?

[kingspaz]

xtreme, did you try heating it over a flame to dry it? if so that will cause the decomposition of the HDN hence the shitty fumes. this is due to uneven heating of the container from the flame. try drying it in the sun or under a fan/lamp. this will be much less harsh and should dry it fine.
about using wet HDN for RDX...the purpose of useing HDN is to improve yields. wet HDN will introduce water to the HNO3 which will reduce yields as a high concentration of HNO3 is required for RDX.

[xtreme]

I was heating it (slowly/low temp.) on a electric plate.
It melts/going into solution and vaporates very fast.

I have distillated some HNO3 for making RDX.
My room is 30 degr.C (lot of running servers who generate a lot of heat :) ) The HDN is allready vaporating on this temp (I can smell it). So....I going to try undried HDN for making RDX and hopely keeping the temp. low

(b.t.w. bad room temp. for making NG :D )

[Mr Cool]

Undried HDN will give TERRIBLE yields of RDX. You probably won't get any at all. Don't try it, you'll just waste HNO3.
I don't see what the problem is; filter out the HDN, put it on some absorbent paper to suck out some of the water, mix it around in plenty of acetone, put it on more absorbent paper to suck out excess acetone, spread it out to dry, preferably below about 35*C. Don't heat it, it can cause hydrolysis due to remaining water. 10fingers told me it can be dried further by powdering it well and washing it with acetone again, and again drying it in a cool place.

Get out the excess water before putting it into acetone. Otherwise you can end up with an aqueous solution of HDN with acetone floating on top, and no crystals.

[xtreme]

ok, ok....I shall try it.....

I got some old filter paper that I don't use (yes it's, clean) and try to dry it with that. I let it dry in my toilet, it's cooler there.
heating below 35 degr.C :D , it's allready 30 degr.C in my room....and the HDN does not like it.

I try tommorow to make some RDX (it's 0:12 AM here). First I go to detonate my last 3 weeks old AP (17 grams) with 50 grams ANNM awakening some people :D It's dark, so I dont have to walk out the city....nobody can see me :rolleyes:

I have mixed some Methanol to the NM....just to test it.

I make some fresh AP tommorow too as booster for a ANNM-LSC test.

<small>[ July 27, 2002, 06:14 PM: Message edited by: xtreme ]</small>

[xtreme]

Ok....that was a good distraction (ANNM-blast) of my bad HDN results this day, the smile back on my face :D

I had standing the HDN in the filter/funnel

It's dripping like melting ice.....what a stuff

Ok....the solution, I hope:
I put it on a stack of filterpaper and set it the toilet (lower room temp.) Hopely this works and stops the HDN from "melting"/vaporating and drying it. Just waiting.......

Going to bed.....see ya later !

[xtreme]

HDN not completely dry (it won't be) and much of the stuf is vaporated (something of 50% is gone)
The vapors in my toilet are terrable (biting like Chlorinegas in eyes and nose)

Try to make RDX with it......very bad yields (the moisture in HDN)
The God of RDX realy hates me :(

It was a nice experiment but it's to bad for my health (vapors), costs to much time and is to expensive to continue.

[DBSP]

I tried detonationg a 15g HDN charge a week ago, it failed to detonate by a 2g HMTD/AP det. Does it need good confinement to detonate?

<a href="http://w1.478.telia.com/~u47804009/E&W/15g_HMDN_charge.JPG" target="_blank">15g HMDN charge</a>
<a href="http://w1.478.telia.com/~u47804009/E&W/failed_15g_HMDN_charge.JPG" target="_blank">failed 15g HMDN charge</a>

<small>[ July 31, 2002, 12:36 PM: Message edited by: nbk2000 ]</small>

[mr.evil]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> HDN not completely dry (it won't be) and much of the stuf is vaporated (something of 50% is gone)
The vapors in my toilet are terrable (biting like Chlorinegas in eyes and nose)

</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">The gas you've smelled is Formaldehyde gas(CH2O).

I've made some HDN a few months ago, and dried it with toilet paper.
After it was dry, i putted the HDN in a film cannister.
This morning i checkt the cannister and it was full of liquid!(not very surprising like it is very hygroscopic).

edit: some spelling mistakes

[ALENGOSVIG1]

I've never really had a problem drying hexmaine dinitrate. Just dry it while its damp with acetone under a 100 watt bulb for a couple hours.

If your hexmaine dinitrate is absorbing so much water that is becomes a solution, then mabe you shuld try storing it under acetone. But mabe the water (cheap brands conatin more then you think). in the acetone would hydrolyze the hexmaine dinitrate.

You could probally store it under anhydrous acetone.

[nbk2000]

You can dry out acetone using calcium sulphate/sulfate (depending on how you spell it). This is the white stuff in sheet rock used for building walls. Cut it up into small cubes and dry it out in an oven at 200 degrees C for a couple of hours to get it anhydrous. Then pour your acetone over the cooled cubes till they're just covered. Let sit an hour with occasional swirling. Pour through a filter into a warmed bottle and cap.

Epsom salt heated till dry might also be useful, instead of CaSO4.

[ALENGOSVIG1]

Yeah MgSO4 (epsom salts) work good. Pour the acetone over cooked MgSO4. To "cook" it, heat MgSO4 in an oven on a cookie sheet at 300f for 2 hours.

Repeate this process a couple times and you will have anhydrous acetone.

[Mic]

Old topic back.

Today I made HDN. I used the method on Mr. Cool site:
5g Hexamine,
10g NH4NO3,
35mL HCl.
I Mix the HCl and the NH4NO3 and I cool it down in the freezer. After, I add the hex and I filter very fast. The thing I have filtered burn faster than hexamine but HDN is not suppose to burn ?!
I Presume that this is just hexamine that does not have time to become HDN but i can't explain why it does not burn like hexamine.
I just have 0.8g of that.

Anyway I evaporate the solution and there was 15g of yellow (!) cristals.These cristals does'nt burn so I think that it's HDN even if they are yellow. Tomorow I will wash them in acetone so maybe there gonna become white.

[Mic]

Ok, This morning I wash the yellow cristals in Acetone and they don't dissolve. The white cristals dissolve in acetone and they both dissolve in water. I guest that the yellow cristals are Hexamethylenetetramine Dinitrate and the white are juste Hexamethylene. Am I right ?

[kingspaz]

from what you say it appears you are right. good luck experimenting!

[Madog555]

HDN burns like hexamine only more furiously

[Mic]

I don't remember who but somebody posted some times ago that HDN didn't burn. And why the thing that I got by evaporate the solution does not burn ? :confused: Anyway I will try again next weekend and try filtering very very fast !

[Madog555]

well, just think about it, hexamine is flamable, and HNO3 is a powerful oxidiser, and HDN is meerly a mix of HNO3 and hexamine. if you put HDN in water u will get a solution of HNO3 and hexamine. if it didnt burn it would be very weird.

NICE SIG!! that is a classic. The Hackers Manifesto has some of the truest words ever spoken. i wonder if The Mentor is still alive.

[ShockWave]

Well, the HDN I made didn't burn also, and it wouldn't detonate by putting 10gr HDN in a filmcanister with a 1gr AP blastingcap, so it is harder to detonate then ANNM/AL, I did all of my HDN away since I don't like this stuff anymore, I was looking for a better detonater, the searching continues.

[Mr Cool]

If it didn't burn then you didn't make HDN. Unless you left it wet of course, but I'm sure everyone has the common sense to dry things before they test them.

[ShockWave]

Yes it was very dry, and be carfull when you dry the HDN, there are very small cristalls you can't see, I was so stupid to put about 10gr. of HDN next to my hot air blower,!!! when I came to my kitchen you could hardly breath,and eye's and nose did really hurt, so watch out, why it woul'dn't burn I dunno, It made the HDN with 52% HNO3

[mr.evil]

The irritating fumes were almost surtenly formaldehyde :rolleyes:

Ah, another member from the Netherlands, can you please mail me?

<small>[ October 01, 2002, 08:22 AM: Message edited by: mr.evil ]</small>

[Celtick]

I made HDN yesterday, I used the instructions from Mr. Cool's site, and I must say I like this reaction. This was my first time for HDN and immediately great yields :rolleyes: I made some photo’s with my new handycam, so when I have a PCI card I will upload them. I also updatet the site <a href="http://www.angelfire.com/goth/celtick/HDN.html" target="_blank">http://www.angelfire.com/goth/celtick/HDN.html</a>

[Celtick]

Here are some photos of the HDN crystals (copy and paste links).

<a href="http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_Crystals_Close.jpg" target="_blank">http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_Crystals_Close.jpg</a>

<a href="http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_Crystals.jpg" target="_blank">http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_Crystals.jpg</a>

<a href="http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_in_Acetone2.jpg" target="_blank">http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_in_Acetone2.jpg</a>

<a href="http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_in_Acetone.jpg" target="_blank">http://www.angelfire.com/goth/celtick/HDN_bestanden/HDN_in_Acetone.jpg</a>

<small>[ December 23, 2002, 04:21 PM: Message edited by: nbk2000 ]</small>

[carbonated]

Celtick, what was the starting amount of hexamine? That looks like a lot of HDN, did you weigh (dry) yields?

[Celtick]

You could read it at my page; it was 15gm of hexamethylenetetramine. The yields lay about 83%, since I got 12-13gm of HDN :D .

[kingspaz]

celtick, that method of calculating yield is inconclusive as to how efficient the reaction was. i've noticed a few people calculating yields like this. the way to do it properly is to work out the theoretical yield of HDN using the reaction equation. then divide the actualy yield by the theoretical and multiply by one hundred. this will give you the actual yield as a fraction of the theoretical and thus tell how efficient the reaction was and how much HDN you lost along the way.

[Microtek]

So in fact your yield was only 46 %. Mol weight of hexamine = 142 g,
Mol weight of HDN = 266. So (15 g hex/142 (g/mol)) = 0.106 mol theoretically gives 0.106 mol HDN = 28.1 g.

[kabooom]

does it work?
make 3 saturated solutions, one containing 6 mol formaldehyde another 4 mol AN and the last one 1 mol HMTA. mix all the solutions, let dry (as much as possible) than sink the whole (probably wet) crystals in acetone, filter it the next day and let dry.
NH₄NO₃(s) --&gt; NH₄⁺(aq) + NO₃^-(aq)
6CH₂O(l) + 4NH₄⁺(aq) + 2H₂O(l) --&gt; C₆H₁₂N₂(NH⁺)₂(aq) + 2H₃O⁺(aq)
2H₃O⁺(aq) + C₆H₁₂N₄(aq) --&gt; C₆H₁₂N₂(NH⁺)₂(aq) + 2H₂O(l)
C₆H₁₂N₂(NH⁺)₂(aq) + 2NO₃^-(aq) --&gt; C₆H₁₂N₄.2HNO₃(s)
summarized reaction:
6CH₂O(aq) + 4NH₄NO₃(aq) + C₆H₁₂N₄(aq) --&gt; 2C₆H₁₂N₄.2HNO₃(s)

advantages(if my method works):
</font><ol type="1"> <font size="2" face="Verdana, Arial, Helvetica">2 mol HMDN product per 1 mol HMTA consumed </font></li> <font size="2" face="Verdana, Arial, Helvetica">no acid is used </font></li> <font size="2" face="Verdana, Arial, Helvetica">common and cheap starting materials </font></li> <font size="2" face="Verdana, Arial, Helvetica">good purity of product (no byproduct in theory) </font></li>[/list=a]<font size="2" face="Verdana, Arial, Helvetica">

[DBSP]

The whole point of using acetone when filtering is that it evapourates quickly thus the HMDN dries faster which is a necesity with this explosive. Thus you pour acetone through the filter from above so that the acetone pushes the water out of the crystal mass. When that has been done the acetone is quickly driven of by some heat.

[CyclonitePyro]

I made 13g HDN and I pressed it into a film canister then put a piece of paper in and then 2g of AP, and it didn't detonate the HDN, it was perfectly dry. Is it less sensitive than we thought? A single piece of paper between the HDN and AP couldn't prevent detonation could it? Has anyone set any off?

[ALENGOSVIG1]

I had trouble detonating hexamine dinitrate with 1.5g AP caps.

Now i usually use 2 or 3g of HE to initiate HDN with great success. I usually use RDX, TNP or NG.

[rooster]

I have been able to detonate HDN without any booster. I used about 3 grams of AP packed in a paper tube, with 50 grams of HDN surrounding the AP in a plastic tube. Nice and loud, although it cant even be measured with RDX.

[Einsteinium]

Yield is defined as the products molar quantity over the reactants molar quantity. 85g HMTA is 0,61 mol (molar mass 140,106g/mol) and 143g HDN (molar mass 266,097g/mol) is 0,54 mol. The yield is then 0,54/0,61=88,5%.

[piro]

Does anyone know what solvents Hexamine dinitrate is soluble in? Besides water:) :D

I know its not soluble in acetone or ethanol. Mabe toluene or methanol?

does anyone know? I'd like to store mh Hexamine dinitrate dissolved in some solvent.

[Sonny Jim]

Isopropyl alcohol comes to mind, as well as the ones you mentioned.

[ALENGOSVIG1]

I've tried ethyl alcohol, xylene and toluene. And we all know acetone doesnt work right? ;)

I didn't try chloroform or ether becuase both are too valuble to me for this kinda thing.

I'd like to make a saturated solution of HDN, add it to NH4NO3 (or other nitates, Ca(NO3)2 for Ex.) and let the solvent evaporate leaving an intimately mixed composition. I find HDN crystals are too large to intimately mix with NH4NO3, and there too hard to powder. Regardless, tommorow im going to try to detonate an 80/20 mix of CN/HDN. They could always be fused together, but thats too much trouble for me and it would probally be very insensitive due to the high density. I think HDN/nitrate would be a really good, powerful explosive if you could mix them intimately. HDN is surprisingly powerful and it has a very -OB so mixing it with a nitrate should make quite a powerful explosive. The yeild when making HDN with HNO3 is really good too.

As for storing HDN dissolved in a solvent, since it doesn't seem to be soluble in common solvents (haven't tried isopropyl or methanol though) i think your SOL. Why not just try to store it under acetone, or one of the other many solvents its not soluble in?

EDIT: Just got back from trying to detonate 130g of CN/HDN. 2g of NG/TNT and .3g of AP was used as the det. Upon detonation, there was a loud boom, but i found some powder/residue in the hole. It was a deep, loud explosion though; it sounded like most if it detonated. It was only confined in a plastic bag and placed on the ground.

Next time i'll try it in a stronger container and i'll bury it. Hopefully then i'll achieve a complete detonation. I still think the problem is that the HDN crystals dont intimately mix with the nitrate. Next time im going to add 1% fuel to the nitrate so even the particles of nitrate which aren't well mixed with the HDN will be sensitived by some fuel.

You guys complain about NH4NO3 being hygroscopic. Try playing with Ca(NO3)2 mixed with HDN! :eek:

[markgollum]

Well, I tried to detonate 12grams of HDN mixed with 3g KNO3 with 2g of HMTD mixed with .5g KClO3 in a paper detonator and failed :( . The charge was placed in a 3cm diameter hole, drilled into the top of a hard, 30cm diameter log, upon which was placed another log.
When the detonator was electrically initiated, I herd a dull thump, and the second log was lifted about 8cm off of the first log.
Upon inspection, it was obvious that none of the HDN had detonated.
The HDN was made via AN + HCl + hexamin, it was very dry, burns well, and the top half of the charge was only slightly pressed.

[Myrol]

Everybody who had succesfully detonated HDN, whats your opinion? Is HDN (probably mixed with AN) stronger or weaker than AP under conditions who you can mark as "good"! Yesterday i cacluated a mix out of HDN and AN and thats the result: 4 C6H14N6O6+ 13 NH4NO3--> 24 CO2+ 27 H2O+ 27 H2+ 25 N2. (At High Temperatures oxygen should be more prone to carbon than to Hydrogen). The Gasvolume per kg was around 1097 Liters the Energiecontent umm i believe it was 8170kj if im not wrong? A 5g 25/75 pressed APAN-det. should be a good choice to set off such a "Device". You can also take 3g PETN but thats not for everybody avialable! Only our nice US-Members have permanent Acces to PETN-precourcers ;)

[al93535]

I have been getting great yields of HDN, 98.8% theoretical. I dissolve 10 grams hexamine into 35 ml distilled water, then add 15 ml 70% HNO3. There is an immediate precipitation, I stir for one minute and immediately filter. After about 30 seconds most of the water is gone and I add 100ml dry acetone. I put the filter paper between paper towels and squeze, over and over until not much comes out. I dry it in the open until I can smell no more acetone, after that I put it in a dessicator overnight. Theorectical yield from 10 grams is 18.7323, I got 18.5191 grams, pretty damn good. :D

[JimmyJones]

I always get good results as well using 70% nitric acid. I once tried using the other method without using Nitric acid and got a poor yeild so I stick to making it with nitric acid in order to obtain better yeilds.

[Detonate]

I bought 1l 53% HNO3 and want to make HDN. Ive heared that HDN is carzinogen, is that right? If not ill make some HDN on weekend and try to detonate it with AP. Do you think that HDN is kompatible with NM? If yes you could make HDNNM!
thx

[Detonate]

I made HDN with great succes. I disloved 14g of hexamine in 50ml of hot water and cooled this solution to 2°C. Then i started to adding 25ml of HNO3 (53%). After i added 20ml of the HNO3 the HDN starts forming. I added the last 5ml of HNO3 and waited 10s under stirring. Then i filtered the HDN and washed it with 40ml of acetone. Now its laying on the filterpaper to dry completely. This way of preparing HDN is great. I once tried it with the HCl/AN method and it worked very very bad. I got 0,5g of HDN of 12g hexamine!

[Myrol]

Hi Detonate! Your results sounds good :) try a bigger batch and do a demolition test to compare HDN's power with perhaps AP or somewhat similiar. I know, HDN is very easy to prepare and a real friend for people who have insufficient time to prepare mighty Explosives like PETN or NIBGTN. Lots of People had bad misfires with HDN so to prevent a misfire I think its useful to confine HDN good (no Cardboard-> Metal!) and priming it with 4g AP or 5g APAN 50/50. If you have nice results with HDN ;) I will make also some HDN. Is it know stronger as AP or not?

[knowledgehungry]

Detonate try using a higher concentration of Nitric Acid, or more of it.

[Detonate]

How much HNO3 shuld i use for 14g of Hexamin? 30ml? Megalomania says to use 20ml 70%HNO3 so i tried it with 25ml 53%HNO3! It worked great. I got out (my HDN is dry now) 16g of HDN.

[Boomer]

For one mol hexamin (140g) you need two mol HNO3 (2x63g = 126g = 84ml).

As nobody has 100% nitric, you need more of course. What people forget is the density: You DO NOT replace 84ml of 100% with 168 ml of 50%, but 126g of 100% with 252g of 50%. This equals 190ml (density 1.33), not 168ml! I guess this is what knowledgehungry meant.

Or, if you cannot get stronger nitric, use less water for the hexa. You can use as little as 22ml for 14g. You can even dissolve the hexa in weak nitric directly (e.g. take only 15ml water and 10ml nitric, so it does not start to form a precipitate), then add the rest of the acid.

I adopted Mr Cools (Alengs …?) method (scaled up), but used much less water and slightly less acid (170ml instead of the calculated 210ml). Yield was about the same (84% instead of 85%) with only 50% nitric! :)

P.S. Ever wondered why the most common OTC nitric acid (at least in Germany) is 53% max? This is EXACTLY the limit where you cannot make nitro, no matter how much sulphuric you add (too much dissolves the ester again)! :mad:

[ProdigyChild]

No, that's not right, Boomer.
I've made my first nitro with 53% NA and 96% SA. It definitely works!

[Boomer]

OK, I meant "cannot make nitro" in useful quantities for terrorist etc.
And my acid was from a photo store, years old in a plastic bottle which was bleached nearly white. Perhaps it had decomposed to lower conc.

Anyway, what ratios did you use? I tried at least ten times with 53% (other bottles too) in all possible ratios, and got a product only twice, and only some drops.

According to the waste acid rule saying formation stops at 70% SA, 20% water and 10% NA, you should mix 78% SA(96%) and 22% NA (53%). This leaves 1.6% nitric which can react. Means <1ml NG for a 100ml batch, or <5% yield! There is more of the dinitrate though, could be you got some of that? Or did you extract what did not separate?

For distilled NA even the HOME yield is 92% (108ml NG from 125ml each of NA + SA, plus 62ml G). Even just boilling the 53% stuff down to 2/3 before adding the SA gives ten times as much product!

But back on topic: I would like to hear the yields people get for HDN. As it only a neutralisation, 85% cannot be the limit. I would not care much if my hexa wasn't so expensive (2 Euro for 20 tabs a 4g = 78g plus 2g wax binder!). The cheaper fuel bars you get everywhere are nowadays mostly the spongy type reeking of petrol, cheap (big) military hexa bars are harder and harder to find.

[Detonate]

Boomer im from "europe" too! I can buy 65% HNO3 but it costs me 9 euro a L! For the 53% HNO3 i payed 6 euro. I can buy pure Hexamine for only 11 euro a Kg! So i can make much HDN. But today i orderes 1l of 98% Ethylenediamine. Ill make some Ethylenediamine dinitrate. Its stronger than HDN!
thx for the Info about the nitric acid!

[Oktogen]

11 euros for one kilogram ?????
In Poland I pay 15złotych (about 3,5euro ) for one kilogram of heksamine, 2,5 euro for one liter of both nitric and sulphuric acid, but pure for analysis. I'll try HDN but as I said before I like nitroesters most :) . In poland it is possible to buy technical grade nitric and sulphuric acid for 0,25euro for one liter... :D :D :D

[ProdigyChild]

Boomer, that's a long time ago, but accoriding to one of my 'historical records' production was as follows:

100ml NA 53%
200ml SA 96%
17ml Glycerol

Yield 16ml Nitro. Not that bad if NA is the limiting factor.

I always did the reaction in the freezer, letting it react a long time, never rising temperature above 0&deg; while adding glycerol dropwise and stirring by hand with a glass rod.

I can remember, that one batch started to freeze with big crystals forming (cubic ones, IIRC). Maybe this one, maybe this had some positive effect. I did not analyze, what the cristals were I was shit scared by the production those days :(

I poured the mix into crushed ice + water to separate. I don't know the properties of the dinitrate, possibly there was much of this in my final product. Final product looked milky and turned transparent after a long time of sitting under water/neutralization solution.

However, that was the last batch of this kind, I preferred destilled NA later on.

[Detonate]

What, you can buy the chemicals so cheap?!! Wow! Then you can make a lot of HDN or nitric esters! You could try to detonate your HDN with NG. That shuld work. HDN is not toxic like NG or EGDN. So its better for me becaus i dont like those toxic HEs very much. But on the other hand i they are great (strong, easy to detonate etc.)!

[Oktogen]

Yeah, I can buy chemicals very very cheap.
My favourite explosive is PETN made from sulphuric acid 98% and nitric acid 65% , PE costs 6 euro for one kilogram. It's really powerfull ;) .
What procedure do you reccomend for HDN ? I mean what to do to dry it fast...? and how is storage like ? How long can it stay tightly sealed ?
Do you think a blasting cap 1,2g HMTD and 1,7g PETN could set it off ???

PS
look at the thread about PETN and see my video !

[Detonate]

Hi Oktogen! PETN is great. I think its possible to detonate the HDN with 1,2g HMTD and 2g PETN (i would use 2g!). Somone detonated it successfully with NG. So i see no reason why it shuldnt go with PETN.
I washed my HDN with plenty of Acetone. Then i dryed it on the coffeefilter. There are no storage problems yet!

[Oktogen]

Hi detonate !...
I make my Bcaps from 2ml plastic syringes from drugstore. I use 1,2g of HNTD and 1,7g of PETN and VISCO 3mm (1cm/s) fuse. I am going to make HDN when I get some pure acetone, cause the solvent one have some oil dissolved in it. I think that HDN would be a good booster to ANFO , but HDN used alone should be in large quanities such as 150-200grams.

PS
what type of anfo do you use ?
I use AN + acetone as the easiest to set off --> AN standing with 15% by weight of acetone forms sensitive nitrozooxyms of acetone...

[Detonate]

What are nitrozooxyms? What do you use as a booster for your acetone ANFO? I usually detonate no ANFO (too hard!). I use ANNM. But thats off topic!

[Pietruszkin]

What are nitrozooxyms? What do you use as a booster for your acetone ANFO? I usually detonate no ANFO (too hard!). I use ANNM. But thats off topic!

hi detonate!

some people think that when you storage AN/acetone mixture there are forming 'nitrozooxyms' ;)

personally, i don't believe it :p

greetings, pietruszkin :cool:

[Myrol]

Hi Guys :) Im very happy now, because the chances to get
the kg Potassium for FREE from my Lab (they want to remove it
out of the Chemistry Stockroom) is higher and higher! So in the
sooner Future I'll buy 3Liters pure NM and want to make some PLX.

Some guys had told that we can make Amines out of Halogenocarbons
and Ammonia prefered anhydrous Gas at higher Temperatures. If this
could work, I think its not to hard to make some Triaminomethane with
this way: Moist Alcohol (80% Et-Oh rest Water!) reacts with Chlorine
to form Chloralhydrate. It reacts very fast and easy with diluted Sodium
hydroxide to form pure Chloroform CHCl3 :D This and Ammonia--> CH(NH2)3, not?

Well, but I think it won't work, seems to be to easy :rolleyes: Methylamine can be easy prepared from Hexamine but its a GAS so I could also use the silly Ammonia way. Ok it works, but I want to see the maximum performance
wich NM can give me :D . That's why I need an Amine!

Holy Shit, Im very sorry. I thought Im in the Nitromethane Explosives
Thread..(Arrghh Damn!)....but I wasn't :p I appologize for my mistake, next time I watch more often in wich Thread Im in.

[nbk2000]

Acetone and bleach makes chloroform, with no bullshit intermediate steps required. :)

[Dr_Pind]

Just wondering. Has anyone tried mixing HDN with AN to give it a better oxygen ballance and more power? AN being hygroscopic shouldn't be a problem, since HDN is hygroscopic by it self. Might also make it more cap sensitive... :rolleyes:

[R_Chemist]

I tried HDN with 1.93 mol/L(according to my titration) nitric acid, available comercially as "pH down"
14g of hexamine was disolved in 50 mL distilled water and cooled to -10. 105 mL of the 1.93mol/L nitric acid was also cooled to -10. The cold hexamine solution was added to the cold nitric acid solution. Precipitation occured after about 1 minit at which time it was gravity filtered and washed with 200mL acetone. Yield was 8.1g which is 30% of theoretical.

I was hoping to have found a use for dilute OTC nitric but yields are too low. Oh well, back to using it for cleaning glassware :rolleyes:

[Detonate]

Hi! I know thats totally off topic but i think its not worth a new thread! Ive heard of Dinitropentamethylenetetramine. Is it an explosive? You can make it with HDN and H2SO4. You can convert this to Hexogen but im interestet in DPT itself. Has anyone experiences with it?

[Oktogen]

Hi !
ENGLISH ONLY! :mad: :mad: :mad:

Don't you think NM is expensive ? ANNM is extremely expensive...PETN is cheaper... ;)

[Detonate]

I couldnt detonate the HDNNM charge :-( The weather is so bad (rain, wind, cold). But i made a test: I wanted to know if HDN and NM is compatible. To 1g HDN I added 1g of NM. There was no reaction(within 20min). The HDN is NOT soluble in NM! When it is mixed it looks like ANNM. But it was a bit wet because it was a 50:50 mixture. I would say HDNNM would work. But can anyone confirm the solubility thing?

[Detonate]

The HDNNM charge failed! I added 3g of NM to 30g HDN. Detonator was made of 5g AP. There was a loud boom. But when I went to the blasting site i saw, that the HDN was spread over the earth. i think a little of the HDNNM detonated.

[VasiaPupkin]

By the way if you want to get a better HDN yeild calculate HNO3 quantity so that waste acid is 20% HNO3.
Because HDN has lowest solubility in 20% nitric acid than in water or NA with other cocentrations.
HDN preparing from book "Lab preparing of nitrocompounds" by Orlova E.Y.:
Dissolve 1 part hexamine in 1.5 parts of water. Then add 50-60% nitric acid (at 15-20C) in quantity sufficient to receive a 20% waste NA.
Filter crystalls and wash it with absolute ethanole. Dry it at 60C.

About DPT:
I think the best way to prepare it is described in US pat 4,338,442. It also possible to meke from hexamine and nitrourea with better yeild but I have no detailes.
I dont know about DPT explosive properties because its never used as explosive. Additionally DPT has poor stability to hydrolysis. DPT is a intermediate in HMX synthesis.
It possible to make a HMX with 75% yeild from DPT, NA and ammonium nitrate.

[The_Rsert]

11 euros for one kilogram ?????
In Poland I pay 15złotych (about 3,5euro ) for one kilogram of heksamine, 2,5 euro for one liter of both nitric and sulphuric acid, but pure for analysis. I'll try HDN but as I said before I like nitroesters most :) . In poland it is possible to buy technical grade nitric and sulphuric acid for 0,25euro for one liter... :D :D :D

By my local chem-supplier, 1kg normal (techn) PE costs 48€. 1kg Hexamine (95%) does cost 18€.
So, Oktogen, please, please open an online shop for selling chemicals in europe! So you can become rich!
Or can I get the address of your shop, please?
I'm living in Germany an maybe I can go to your chem shop. Does your shop sell PE and other interesting chemicals, too?
If you will have problems with the presentation of your online shop il will help you.
My e-mail: the_rsert@arcor.de

I have heard, that only 5-10g PETN(nitropenta) will break a big stable steelness padlock, if the PETN is stored in a little shaped charge. Is that true?

[The_Rsert]

I have just dissolved much as possible hexamine in about 250ml warm acetone (wasn't measured). Then I added without cooling 10-15ml of 70-75% HNO3 (wasn't measured).
After 30 seconds I filtered off. Yield was 9.5g; How much hexamine will dissolve in warm acetone?
Next time I will test it with an better dissolving agent and an longer reaction time.

[K9]

I just tried the synth via the HCl and NH4NO3 route. Everything went well - the hexamine dissolved and almost right away a precipitate came out of solution. I then filtered it. Now here's where the problem came in. The synth I was following (Mr. Cool's) did not indicate neutralizing the product, and now I know why. I poured some bicarb solution over the product which fizzed and disappeared. Now I just want to make sure that this was my only mistake. Can anyone help?

[The_Rsert]

Yes, I can help you.
HDN will decompose to formaldehyd very fast in water.
So, if you have to neutralize it, dissolve waterfree/dry sodium hydroxide in much hand-warm warm ethanol (94% minimum) until you will have a saturated solution.
Than shake the HDN and the saturated NaOH+EtOH solution together and test the PH.
If it's not neutralzed, add some more of the solution.
Than filter the HDN.
That's all. :)

[K9]

That is perfect, thank you very much for that. And now I remember seeing posts here saying how it decomposes like that. Stupid me. They said to run a solvent over it (like acetone) to remove any remaining water to prevent that.
But in regards to neutralizing, do I actually need to neutralize it anyways?

And one more small thing. Mr. Cool's synth calls for 15% HCl. I have 31.45% and that's what I used (adjusted ratios) and it worked fine. Alen's synth uses 34% so I'm assuming that Mr. Cool was just using the concentration he had access to. Does anyone know if that's correct?

[Rosco Bodine]

That is perfect, thank you very much for that.Perfect? Perfectly hilarious actually . And now I remember seeing a post here saying how it decomposes like that. It does decompose like that .Stupid me. It said to run a solvent over it (like acetone) to remove any remaining water to prevent that.
But in regards to neutralizing, do I actually need to neutralize it anyways?If you have a solution of ordinary salt , do you need to neutralize it ? Not if you had the right amount of reactants to produce salt with no excess of either reactant . Of course this scenario is a bit more complicated than that but certain fundamental principles will still apply to the formation of the acid salt of hexamine , and why you cannot "neutralize" it using anything that is a stronger base than hexamine itself , unless of course "freebasing the hexamine" instead of "neutralizing" is your intention . Using NaOH in ethanol to wash HDN is going to result in a precipitation of sodium nitrate and an ethanol solution of hexamine , and why would anyone reasonably expect a different result or suggest such a method which frankly makes no sense ?
And one more small thing. Mr. Cool's synth calls for 15% HCl. I have 31.45% and that's what I used and it worked fine. Alen's synth uses 34% so I'm assuming that Mr. Cool was just using the concentration he had access to. Does anyone know if that's correct?In these sort of double decomposition / precipitation reactions there will be an optimum ratio of reactants in solution at some optimum concentration at an optimum reaction temperature , reacted for an optimum time , and then the solution cooled (usually) or otherwise brought to an optimum temperature and concentration for filtering out the precipitate . Certain conditions will produce the highest yield or purest product and the conditions will be charted and determined by experiment , usually finding a "comprimise" parameter where the highest yield of reasonably purest product is obtained . Those conditions may be varied slightly to produce a purer product at the expense of yield . Since ammonium chloride and ammonium nitrate and hydrochloric acid and hexamine hydrochloride will be the potential impurities in the HDN , then conditions must be tailored to facilitate the separation of HDN directly in purest form .
Beyond rinsing it with alcohol or acetone thereafter , there isn't much you can do towards any purification . So for uses where pure HDN is required it is necessary to make HDN using hexamine in slight excess and nitric acid , which precipitates the pure HDN directly , requiring no further treatment than filtering and drying .

[K9]

Wow, thank you very much for that :) . That told me exactly what I needed and more. I really appreciate it.

So basically it just comes down to testing different concentrations of acid to see what work the best. Then testing there shall be. And again, thank you very much.

[Rosco Bodine]

The concentration of the acid is not what will be important so much
as will be the concentrations of all the reactants in the reaction system
and their interactive effect upon each others solubility , or as I call it
their "co-solubility" in the system at a given temperature . I believe the
usual term is the "common ion effect" but that seems an overly complicated
term for mixed solutions . It can be tedious to chart the results and
find the "sweet spot" for the concentrations of the various reactants which
produce the good yield of pure product desired , and these figures do not
translate directly to substituted acids and different salts that may be variations
on the method . What you chart as efficient for that mixed solution will
only apply to those particular salts and acids , and entirely different figures
will apply to the variations adaptable on that theme . For example if you use
a different acid , everything else does not remain equal , and the method
may not even work at all , or some double salt may be produced instead
of what you desire . Urea Nitrate can be made by a similar method , and
what are optimum conditions for one reaction scheme does not translate
directly to other schemes where different acids or nitrates are substituted .

[K9]

Ah ok I see what you're saying. I don't see the yield or purity changing by enough to really warrant testing it unless I have a lot of free time which I don't foresee happening. I'd only be charting specifically for the HCl, ammonium nitrate, and hexamine that I have available to me, but then again I guess it still doesn't matter too much. As for the urea nitrate, I'm going to test out synthesis of that with HCl/NH4NO3 using a procedure from Mr. Anonymous I saw posted on sciencemadness and see how that goes. Apparently the yield is 84.4%. But yes, I see how you can't compare methods where anything changes because even one change will throw everything else off.

[Rosco Bodine]

Ah ok I see what you're saying. I don't see the yield or purity changing by enough to really warrant testing it unless I have a lot of free time which I don't foresee happening. I'd only be charting specifically for the HCl, ammonium nitrate, and hexamine that I have available to me, but then again I guess it still doesn't matter too much.It is the molar ratios and particularly the molar concentrations in water which are the most important , particularly at the temperature which the product is filtered . As for the urea nitrate, I'm going to test out synthesis of that with HCl/NH4NO3 using a procedure from Mr. Anonymous I saw posted on sciencemadness and see how that goes. Apparently the yield is 84.4%. But yes, I see how you can't compare methods where anything changes because even one change will throw everything else off.That is an accurately reported result and method . First try the procedure exactly as described because it is optimized . Then try varying any parameter by even a few per cent and watch the yield and/or the purity of the product suffer , to confirm the optimization .