Sciencemadness Discussion Board - Short question / quick answer - Thread

Short question / quick answer - Thread

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ecos - 21-4-2014 at 02:59

I think it should work, but you're going to have to be very careful. You would need just enough water to increase the concentration as much as you can, but not enough that you start diluting it.

so i need to add water drops till the yellow color start to disappear ?

DubaiAmateurRocketry - 21-4-2014 at 04:15

ecos just freeze the nitric acid in your freezer, the coldest possible temperature, and it will become much more whiter, if you need it for RDX its good enough. If there is water during your RDX nitration, it will give some very dangerous by products according to what other members said.

ecos - 21-4-2014 at 06:39

Quote: Originally posted by DubaiAmateurRocketry

ecos just freeze the nitric acid in your freezer, the coldest possible temperature, and it will become much more whiter, if you need it for RDX its good enough. If there is water during your RDX nitration, it will give some very dangerous by products according to what other members said.

Thanks man but freezing will remove the NOx or just the color?!

so I need to let the container of HNO3 open to get the NOx out?

and what is wrong about adding the water drops ? i thought it will increase the concentration !

DubaiAmateurRocketry - 21-4-2014 at 07:58

When you distill HNO3 there will be traces of water condensing into your HNO3. Making a concentration around 97 98 or 95 depends on your setup, but im sure these water can dissolve the traces of NOx gases in the solution that makes this color. Lower temperature promotes solubility of NOx gases in water so freezing it is enough, the color should disappear meaning it dissolved.

Always keep your acid container sealed tightly, when you chill it the pressure inside the bottle will go down, no worry about build up of pressure

[Edited on 21-4-2014 by DubaiAmateurRocketry]

PHILOU Zrealone - 22-4-2014 at 01:37

Quote: Originally posted by ecos

while trying to make high conc HNO3 using nitrate salts , the result is RFNA , this is because of the NOx mixtures.

to convert RFNA to WFNA we need to make vacuum distillation.

I was thinking to add few drops of distilled water on RFNA to increase its concentration using this equation :

3 NO2 + H2O → 2 HNO3 + NO

i.e, make a reaction between NO2 in RFNA and H20 to get some more HNO3. would that work ?

Ref : http://en.wikipedia.org/wiki/Nitric_acid

[Edited on 20-4-2014 by ecos]

Simply bubble dry air through it in a closed vessel with exhaust drying tube and the NxOy will leave the system leaving you with WFNA

Jimbo Jones - 22-4-2014 at 01:57

http://www.sciencemadness.org/talk/viewthread.php?tid=13749#...

PHILOU Zrealone - 22-4-2014 at 02:35

Quote: Originally posted by DubaiAmateurRocketry

Quote: Originally posted by PHILOU Zrealone

Quote: Originally posted by DubaiAmateurRocketry

Can this be nitrated?
http://en.wikipedia.org/wiki/Dihydroxyacetone

And, can someone help me find synthesis of dinitroethane? or trinitroglycerin? Just interested to see the impact sensitivity and other properties of these liquid EM since the ONO2 group give much more impact sensitivity than NO2 group. I have searched on spinger and WOL, but not much related contents are shown. Thanks.

Dihydroxyaceton is not nitratable directly it is a strong reductor because in equilibrium with 2,3-dihydroxy-propanal...it has the ability to polymerize into dark polyphenolic stuffs (see its use as artificial suntanner).
Just as aceton (propanone) is unstable towards HNO3, so would DHA.
It could be nitrated by a derivated way via war gas lacrymator dichloroaceton and reaction with silver nitrate saturated solution...
Cl-CH2-CO-CH2-Cl + 2 AgNO3 --> O2N-O-CH2-CO-CH2-O-NO2 + 2 AgCl (s)
The molecule might suffer hydrolysis behavior (and unstability-explosive runaway) because of the cetonic group and enol-ceton equilibrium. This effect is seen in nitrosuggars (nitrate esters of suggars).

Dinitroethane can be 1,1 (geminal) or 1,2 (viccinal)... synthesis is pretty easy using the conventional synthesis pathways of nitroalcanes. I suppose you want the 1,2-DNE.
R-Br or R-I + AgNO2 (or LiNO2/NaNO2/KNO2 in DMF).

Trinitroglycerin is a confusing name for nitroglycerin; I suppose you meant 1,2,3-trinitropropane.

There is indeed very little info on those nitroalcanes of the family H-(CHNO2)n-H.

Edited:
Stil they are of much interest because surprisingly at a certain point of n, the linear polynitroalcanes (with one NO2 per carbon unit (cf nitromethane, 1,2-dinitroethane, 1,2,3-trinitropropane) surpasses in density equivalent lenght polymeric H-(CHONO2)n-H (with one ONO2 per carbon unit (cf methyl nitrate, EGDN, NG, ETN, XPN, MHN) by much; and polymeric H-(CHNHNO2)n-H (with one nitramino per carbon unit (cf methylnitramine, EDNA, propantrinitramine)) by a little.
So in theory it can lead to the highest density CHNO explosives this not counting with the fact each CH-NO2 unit:
-can react with formaldehyde to make (-C(CH2OH)(NO2)-)n which can be nitrated to make perfect OB polymer related to nitro-isobutyl-trinitrate ester and 2,3-dinitro-2,3-dimethylol-1,4-butanediol tetranitrate ester (O2NOCH2-(-C(CH2ON2)(-NO2)-)n-CH2ONO2)
-can react with nitrous acid to introduce a nitroso group in the place of the hydrogen increasing by much the density.
One should not pernitrosate the compound in a way to get perfect OB and some H bondings...1 nitroso per 3 unit would be optimum.
-(CHNO2-CHNO2-CHNO2-)n + HNO2 --> (-C(NO)NO2-CHNO2-CHNO2-)n + H2O
Pernitrosated compound would be denser but would be overoxygenated and would require some extra dense fuel to burn.

[Edited on 16-4-2014 by PHILOU Zrealone]

Thank you PHILOU Zrealone for anwsering my question in this detail. Interesting, a polymer with positive oxygen balance would be extremely interesting.

http://www.sciencemadness.org/talk/viewthread.php?tid=27095&...

In this post last reply, I uploaded a file on easily nitrating HTPB. Also for dinitroethane, is the carbon too acidic for use in propellant additives?

Also, what do you think about the nitronium cation nitration on HONH2? Will it yeild HON(NO2)2 ?

If you speak of CH3-CH(NO2)2, then the acidity will be present and in the range of carboxylic acids (thus corrosive towards metal casing and possible formation of sensitive dinitronates R-C(NO2)=N(O)-O(-)) and the stability of the compound due to geminal NO2 groups will be less than in O2N-CH2-CH2-NO2 (where NO2 are viccinal) because two geminal NO2 on a same carbon holding an hydrogen are very prone to nitro-nitrite rearrangment.

About nitration of hydroxylamine:
In "Traité de Chimie Organique, Tome XV, p 642, by V. Grignard, G. Dupont and R. Locquin: Diazoïques et Azoïques, Hydrazines, Hydroxylamines, Oximes et Azides.", they mention nitrohydroxamic acid as being HONH-NO2.
The molecule is in equilibrium with the aci-nitro form:
HO-NH-NO2 <==> HO-N=N(O)-OH
This later form decompose easily into nitrous acid and bivalent nitroxyle radical:
HO-N=N(O)-OH ==> HO-N=O + =N-OH

DubaiAmateurRocketry - 22-4-2014 at 12:47

Thank you SO much for that information. So atleast, that intermediate prodcut - HO-NH-NO2 product was stable enough to just be there and not decompose spontaneously. Good, I believe further nitration with nitronium cation's salts such as N2O5 will yeild a ''stable'' compound HO-N(NO2)2, just the hydroxyl version of dinitramideHN(NO2)2. Just like how ammonia ''H-NH2'' give HN(NO2)2 upon nitration with N2O5, HO-NH2 will probably yield HO-N(NO2)2? Just some guesses.

Also, is hydroxylammonium cation able to produce salts with dinitrourea? Such as dihydroxylammonium dinitrourea? [(HONH3)2]2+ [N(NO2)2]- This salt good density group contributers like the carbonyl group, further more it's oxygen positive with +17%OB(100%CO) balance. This compound should also have an density >1.8g/cm3

However... maybe by cation exchange? Because I have seen that a paper describe when they added hydroxylamine to dinitrourea, it did not protonate and no salts formed, instead, the nitro-hydroxy-urea was formed.

DubaiAmateurRocketry - 22-4-2014 at 14:16

http://en.wikipedia.org/wiki/High_Energy_Density_Matter

''High Energy Density Matter, or HEDM, is a class of energetic materials'' I thought HEDM = Energetic materials?

DubaiAmateurRocketry - 24-4-2014 at 08:42

What chemical reactions could make >N-H become >N-O-H on rings?

Can the N-H on position on 1,4 or 1 on these become N-O-H through some reactions? I have seen HOOH, oxone used however I have never saw any azoles having 2 N-O-H on a single ring yet.

EDIT :

Can fulminate and azide form tetrazole oxide?

[Edited on 24-4-2014 by DubaiAmateurRocketry]

NeonPulse - 27-4-2014 at 17:23

I just have a question on the OB of RDX. being ob negative does anyone think that if balancing it out with ETN would be ideal? Perfect OB is desirable but if the velocity will be reduced too much then I probably won't bother. I'm also struggling to find the correct VOD of ETN also. There are so many conflicting accounts of it vary from 6500 to 8100 km/s from many sources. Most of them say the it is in the 7000s. Does anybody really know? I know it depends on density too so lets say its at its max density?

Napolean Dynamite - 27-4-2014 at 18:15

I got 8100 m/s at 1.6g/cc for ETN from a reliable source but unfortunately I do not know where to find it right now.

Your question is interesting, RDX decomposes partially into CO2 and CO (-21%). ETN decomposes partially into CO2 and O2 (+5%) combining these figures makes an oxygen balance at 1:4.. RDX:ETN by mass.

In my opinion it is not something that can be calculated easily. How important is maximum explosive velocity? Remember RDX is only a fast detonating explosive because of it's higher density than ETN. Because they are C-H-N-O explosives with relatively close to zero OB (I say this because TNT has very poor OB leaving some Carbon unreacted upon detonation, and thus poor VOD at maximum density, even though it is a C-H-N-O explosive.)

Velocity is so much a function of density in ideal explosives (C-H-N-O) and you might find that an overall density of around 1.65-1.8g/cc is possible with a composition (unknown proportion) of cast ETN with RDX because RDX has density of 1.82g/cc and ETN is 1.6g/cc

see page 18 in regards to Octol density characteristics which could apply generally to ETN as a melt castable explosive: http://www.dtic.mil/dtic/tr/fulltext/u2/a053473.pdf

[Edited on 28-4-2014 by Napolean Dynamite]

Dany - 28-4-2014 at 00:35

The experimental properties of ETN has been studied experimental recently by Robert Matyáš et al. and published in Propellants, Explosives, Pyrotechnics journal ( for unkown reasons i can't access the article online) however we have the abstract:

"ABSTRACT: The physical and explosive properties of erythritol tetranitrate (ETN) are described herein. Although the chemical structure of ETN is simple and its preparation is undemanding, this explosive is only briefly described in the literature. Nowadays, it is widely prepared by amateur chemists and by criminals as well. Therefore, it is necessary to describe its physical and explosive properties for pre-explosion and post-explosion forensic analyses. However, as a nitric acid ester, it can also be potentially useful for some industrial applications. ETN was prepared in 83 % yield by the reaction of nitric acid/sulfuric acid with erythritol. The molecular structure of ETN was characterized by single-crystal X-ray diffraction. The structure of the ETN molecule is composed of a central carbohydrate chain and two pairs of facing coplanar ONO2 groups. The crystal density of ETN is 1.827 g/cm³. It is a non-hygroscopic compound, which is slightly soluble in water (the solubility in water was determined in a temperature range from 5 °C to 80 °C; the solubility at 20 °C is similar to that of PETN). The sensitivity of melt cast ETN to friction significantly differs from powdered ETN. Melt cast ETN is more sensitive to friction than PETN, whereas powdered ETN is less sensitive than RDX. The sensitivity of powdered ETN to impact is slightly lower than for melt cast ETN that is on the level of PETN. The detonation velocity of melt cast ETN is 7940 m/s at a density of 1.69 g cm³, which is slightly below the PETN level..."

Another paper by Oxley et al. found that ETN has a density of 1.72 g/cm³. The calculated VoD using CHEETAH 6.0 thermochemical code yield a VoD of 8.2 km/s. the density was measured using gas pycnometer.

The question if a zero OB of RDX and ETN mixture has a better performance? it depend on the final density, heat of formation and detonation products composition. Calculate the density of the mixture (use the crystal density of both explosive as a first try) and the heat of formation. Detonation velocity and pressure can be obtained using the Kamlet-Jacobs empirical method for fast and reliable calculations.

Dany.

[Edited on 28-4-2014 by Dany]

NeonPulse - 28-4-2014 at 03:05

thankyou for that dany, you seem to have access to a pretty big database of information concerning all things energetic. I was hunting for the VOD of ETN for a while now and i think that as i was looking in some older reference material, ETN does not seem to get much of a mention. Also as i mentioned the velocities all were different,given to the different methods used to test and calculate it but they were all fairly close to the numbers you provided.

Looking for details of No. 10 cap casing (NHN confinement)

Gargamel - 28-4-2014 at 09:15

Hey guys,

I wonder if NHN can be used as a primary on reasonable terms.

In this document here
http://www.niscair.res.in/sciencecommunication/ResearchJourn...

it is claimed that while NHN was not able to undergo DDT in a "No. 27" cap (which seems to be identical with a normal No. 8, a thin walled aluminium shell), I could be used alone in a "No 10" cap.

However, they don't give any information on the mechanical properties of the caps.

Now I'd like to know some details on that No. 10 cap - wall thickness, material, diameter...

Since this information is not given there, I assume this No. 10 cap is pretty common...?
I mean, without that information the statements aren't worth very much.

Bert - 28-4-2014 at 09:39

The paper is from India. A quick trip to Google shows the numbers given are standard types, incorporated into India's military and commercial products. Various standards and specifications given out for bidding on production are around the internet.

Go forth and google...

https://law.resource.org/pub/in/bis/S02/is.7632.1975.txt

Dany - 28-4-2014 at 11:24

Quote: Originally posted by NeonPulse

I just have a question on the OB of RDX. being ob negative does anyone think that if balancing it out with ETN would be ideal? Perfect OB is desirable but if the velocity will be reduced too much then I probably won't bother. I'm also struggling to find the correct VOD of ETN also. There are so many conflicting accounts of it vary from 6500 to 8100 km/s from many sources. Most of them say the it is in the 7000s. Does anybody really know? I know it depends on density too so lets say its at its max density?

I calculate for you the detonation performance for a zero Oxygen balance (OB) ETN/RDX:

the atomic composition of such mixture is : C_1.325H_2.118N_1.586O_3.712

by mass this is a 80.5/19.5 ETN/RDX.

The heat of formation of this mixture based on 100g @ 298°K is -28.90 kcal/100g (heat of formation for RDX is taken from MADER [1] and ETN from the Oxley et al. paper given above). the heat of formation at O°K (which are needed in BKW thermochemical code[1]) is -27.25 kcal/100g

the mixturedensity taken also from MADER for RDX and Oxley for ETN is 1.82g/cm³.

using the RDX parameter to calculate the detonation performance in BKW we obtain:

D_CJ= 8.61km/s
P_CJ= 337 kbar

these value are close to that of pure RDX at 1.80 g/cm³ which is:

D_CJ= 8.75 km/s
P_CJ= 347 kbar

experimental values taken from MADER.

as conclusion no enhanced detonation performance is expected over single crystal RDX from a zero OB mixture of ETN/RDX even at crystal density of this mixture.

Reference:

[1] Charles L. Mader, Numerical Modeling of Explosives and Propellants, Third Edition, 2008.

Dany.

[Edited on 28-4-2014 by Dany]

PHILOU Zrealone - 28-4-2014 at 12:04

Quote: Originally posted by NeonPulse

I also noticed the problem to find reliable info on ETN. Maybe the problem comes from the fact it is on the edge between solid and liquid (in the same polynitrate ester family of compounds propantriol trinitrate (nitroglycerine) is liquid at ambiant pressure and temperature(APAT);while xylitol pentanitrate is solid at APAT) ... Butantetrol tetranitrate (ETN) should be solid but is sometimes in overfusion or in solid solution (uncomplete cristalization) maybe due to traces impurities (nitrate-sulfate esters, oxydation products or uncomplete nitration products) but also to stereo-isomers mix ... those effects will lower the melting point.
Also a density of 1,6 can be 1,5-1,7 interval what is pretty vast.

Just to add a bit of confusion

the mixing of two compounds may have a lot of impact on the properties of the mix...properties are not always additive nor logical.
You may have:
-fusion of the two while appart they are solids
-contraction (good for density increase) or expension (bad for density)
-positive enthalpy of mixing (cooling-thus storing some more energy) or negative enthalpy of mixing (generates some heat)
-...

In the balance for VOD and brisance: the density variation of the binary mix vs RDX and the energy variation of the binary mix vs RDX and vs ETN.

[Edited on 28-4-2014 by PHILOU Zrealone]

Gargamel - 28-4-2014 at 12:21

Quote: Originally posted by Bert

The paper is from India. A quick trip to Google shows the numbers given are standard types, incorporated into India's military and commercial products. Various standards and specifications given out for bidding on production are around the internet.

Go forth and google...

https://law.resource.org/pub/in/bis/S02/is.7632.1975.txt

The text in your link only mentions the No.6 and No.8 Types.

Some older documents mention No. 10 caps with 2,8g MF.
But since they are all very old, I assume these where MF caps only.
More modern 2-stage caps are always called "No. 8", even if they are stronger.

There seems to be no modern No.10.

Maybe the used some very old cases like these here:
http://www.clickstersminingartifacts.com/captins_blasting/ca...
I would assume such brass caps to be stronger than typical aluminium caps.

robart - 28-4-2014 at 15:42

Quote: Originally posted by Bert

This would be a good place to learn about making Sodium azide from common over the counter products, rather than asking for information not really having much to do with learning chemistry.

Airbags are built with the intent NOT to ever come apart. Also most do not contain azide any more, the stuff is similar to cyanide in toxicity and was a liability for auto shops to have around.

I personally know an individual who tried to harvest Sodium azide from several 1990's era inflators back about 12 years ago. He succeeded once and failed twice. On the failed attempts, the inflators went off in his face. He lost hair, got 2nd degree burns and some eye damage the second time- The gas generated is very hot, those airbags are lined with fabric woven from stainless steel wire to stand up to the heat. People who have had their bare faces bounced off a working airbag usually are mildly burned from that contact.

Thanks for the information.
Ok so you think I could make sodium azide from over the counter chemicals, cool.
Not meaning to be an idiot but do you know of a topic that discusses that? I'll start looking for one.
Thanks for your help.
robart

Bert - 28-4-2014 at 16:39

Quote: Originally posted by robart

Not meaning to be an idiot but do you know of a topic that discusses that? I'll start looking for one.
Thanks for your help.
robart

The best way to "not sound like an idiot" is to read the FAQ BEFORE starting to post. Here: http://www.sciencemadness.org/madscifaq.html#2.1_Board_topic...

As far as finding your information?

Start by looking up at the top left corner of the page for this friendly little fellow:

Hint:

You'll find a WHOLE BUNCH of threads mentioning azides. You could read them all, it will take you a while though.

So maybe you should filter those down somehow?

Go to the top center of the page where there's a utility for finding out about members.

Shuffle that around, look for some people who have been here a while- like since 2002 to 2005? Then look at those names who also have high post counts... Then look at some of their the profiles, where it says which forum they are most active in. Find the one(s) that mostly posts in energetic materials. THEN search on "azide" and some of these old timer energetic materials guy's names...

That avoids you having to look at the many threads about 2 to 3 post long that start by a new guy saying: "How do I make/obtain Sodium azide? And end with a couple of people answering USE THE FUCKING SEARCH ENGINE! And then a moderator closes the thread.

Good luck, looking forward to hearing how you do with this.

Lerdan - 29-4-2014 at 09:44

Is it safe to make cast Ammonium Nitrate/ Aluminium powder ?
I'm hesitating to make it, because of safety concerns.
If I melt the AN and take the pot from the heating source and mix it with the Al powder at around 80° C (Randomly chosen, I have no idea what the lowest temperature is to still be able to mix it) is there a risk of ignition or detonation ?
Of course, I mean , if I don't throw a burning match or cigarette in it.

PHILOU Zrealone - 29-4-2014 at 10:09

Quote: Originally posted by Dany

The experimental properties of ETN has been studied experimental recently by Robert Matyáš et al. and published in Propellants, Explosives, Pyrotechnics journal ( for unkown reasons i can't access the article online) however we have the abstract:

"ABSTRACT: The physical and explosive properties of erythritol tetranitrate (ETN) are described herein. Although the chemical structure of ETN is simple and its preparation is undemanding, this explosive is only briefly described in the literature. Nowadays, it is widely prepared by amateur chemists and by criminals as well. Therefore, it is necessary to describe its physical and explosive properties for pre-explosion and post-explosion forensic analyses. However, as a nitric acid ester, it can also be potentially useful for some industrial applications. ETN was prepared in 83 % yield by the reaction of nitric acid/sulfuric acid with erythritol. The molecular structure of ETN was characterized by single-crystal X-ray diffraction. The structure of the ETN molecule is composed of a central carbohydrate chain and two pairs of facing coplanar ONO2 groups. The crystal density of ETN is 1.827 g/cm³. It is a non-hygroscopic compound, which is slightly soluble in water (the solubility in water was determined in a temperature range from 5 °C to 80 °C; the solubility at 20 °C is similar to that of PETN). The sensitivity of melt cast ETN to friction significantly differs from powdered ETN. Melt cast ETN is more sensitive to friction than PETN, whereas powdered ETN is less sensitive than RDX. The sensitivity of powdered ETN to impact is slightly lower than for melt cast ETN that is on the level of PETN. The detonation velocity of melt cast ETN is 7940 m/s at a density of 1.69 g cm³, which is slightly below the PETN level..."

Another paper by Oxley et al. found that ETN has a density of 1.72 g/cm³. The calculated VoD using CHEETAH 6.0 thermochemical code yield a VoD of 8.2 km/s. the density was measured using gas pycnometer.

The question if a zero OB of RDX and ETN mixture has a better performance? it depend on the final density, heat of formation and detonation products composition. Calculate the density of the mixture (use the crystal density of both explosive as a first try) and the heat of formation. Detonation velocity and pressure can be obtained using the Kamlet-Jacobs empirical method for fast and reliable calculations.

Dany.

[Edited on 28-4-2014 by Dany]

As explained a few posts ago, there are many discrepancies into various references about the density and VOD of ETN...
So I wonder could it be due to the use of accronyms? A single typo easily turns PETN into ETN...

[Edited on 30-4-2014 by PHILOU Zrealone]

Bert - 29-4-2014 at 11:43

Quote: Originally posted by Lerdan

Is it safe to make cast Ammonium Nitrate/ Aluminium powder ?
I'm hesitating to make it, because of safety concerns.
If I melt the AN and take the pot from the heating source and mix it with the Al powder at around 80° C (Randomly chosen, I have no idea what the lowest temperature is to still be able to mix it) is there a risk of ignition or detonation ?
Of course, I mean , if I don't throw a burning match or cigarette in it.

Why exactly do you WANT to mix powdered Aluminum into molten ammonium nitrate? If you have a reference for a use requiring this, please provide it?

If both the Aluminum and the oxidizer are pure, and temperatures are below decomposition temperature of the nitrate, it won't go off in your face.

Experimental ammonium nitrate/Aluminum compositions

But even a low level of contamination with a number of other chemicals can change that. Chlorine, chlorides, Sulfer, Zinc or Chromium compounds, urea and probably several other things I don't know of make for lowered decomposition temperature, increased reactivity of the Aluminum by destroying the Aluminum's oxide coating or BOTH. That could be exciting.

How pure are your chemicals?

TheAlchemistPirate - 29-4-2014 at 12:53

Has anyone here built an air bubbler with a drying system? I am planning to purify my nitric acid by removing the NOx contamination by bubbling dry air through it with urea being added, and I cant figure out how to dry the air being pushed through the system without spending a fortune. I am planning on connecting a fish tank bubbler to a Teflon tube(with holes poked into it) with silicone tubing, and have seen that the air needs to be dry so it wont contaminate/dilute with water the nitric acid or anything else I need to agitate. I have seen where people say to cycle the air through a container with an air dehydrating chemical, but wouldn't this just push the chemical through the system and contaminate whatever I am agitating? I have done many searches on google and cant find an answer to any of these questions, I am planning on using this bubbler in the future for agitating nitroglycerin and other syntheses that might be dangerous to mix by hand.

Napolean Dynamite - 29-4-2014 at 13:43

I made a glass jar with two holes in the lid, glued to make a seal. This is a reaction vessel that is the gas generator. In one tube I slowly squirt a liquid with syringe to make the reaction go, in the other tube comes the gaseous products (CO2, Acetylene etc.) this tube leads through the gas dehydrating chamber, a cylindrical plastic thing roughly 2 inches diameter full of powdered ammonium nitrate, the gas slowly passes through the AN and then through the rubber tube on the other side which connects to a teflon tube (sealed) and this sits in the nitric acid which would ideally be in a graduated cylinder. I tried nothing more than baking soda and vinegar to produce a fair amount of CO2 to pass through over the course of about 15 minutes, it worked well but nitric acid was still yellow.

hyfalcon - 29-4-2014 at 15:58

They also sell DampRid which is pure calcium chloride at most home stores.

Bert - 29-4-2014 at 16:02

Quote: Originally posted by Napolean Dynamite

this tube leads through the gas dehydrating chamber, a cylindrical plastic thing roughly 2 inches diameter full of powdered ammonium nitrate, the gas slowly passes through the AN and then through the rubber tube on the other side

Ammonium nitrate only will take air down to 40%+ relative humidity at STP, AFAIK?

Why not use cheap & "no questions asked" Silica gel? Easy to regenerate in the oven-

If I had to improvise from Walmart, oven baked Epsom salts would be my choices before ammonium nitrate as gas dryer.

Napolean Dynamite - 29-4-2014 at 17:21

Yes probably true Bert. I didn't know AN doesn't suck moisture out of air less than 40% rel. humidity, so I suppose living in a dry climate, the hygroscopic properties of AN are much less significant.

TheAlchemistPirate - 29-4-2014 at 17:47

So would I be able to pass the air slowly through a horizontal glass tube filled with dehydrated Epsom salts? I will need this for agitating reactions btw so I cant use CO2. I am planning on getting a used fish tank bubbler for restoring oxygen to water, then connecting this to a drying chamber with silicone tubing. The air will pass through the drying chamber, then with more silicone tubing connect to a short Teflon tube with small holes drilled in. I need to get a drying chamber efficient enough to maintain a decent amount of pressure in the setup while still sufficiently drying the air however.
EDIT: lack of info

[Edited on 30-4-2014 by TheAlchemistPirate]

Napolean Dynamite - 30-4-2014 at 12:56

I found a plastic syringe that had diameter about 2 inches this worked well for slowly passing air through the dehydrating material, I used AN but now realize AN won't dry air completely.

Trinitrophenol - 2-5-2014 at 07:36

Hello I have tryed to search using google for azides (sodium/lead azide etc...) compatibility with stainless steel but with no luck.
So i came here to ask this question to someone who might have read a bit more literature than me

PHILOU Zrealone - 2-5-2014 at 07:47

Quote: Originally posted by TheAlchemistPirate

Has anyone here built an air bubbler with a drying system? I am planning to purify my nitric acid by removing the NOx contamination by bubbling dry air through it with urea being added, and I cant figure out how to dry the air being pushed through the system without spending a fortune. I am planning on connecting a fish tank bubbler to a Teflon tube(with holes poked into it) with silicone tubing, and have seen that the air needs to be dry so it wont contaminate/dilute with water the nitric acid or anything else I need to agitate. I have seen where people say to cycle the air through a container with an air dehydrating chemical, but wouldn't this just push the chemical through the system and contaminate whatever I am agitating? I have done many searches on google and cant find an answer to any of these questions, I am planning on using this bubbler in the future for agitating nitroglycerin and other syntheses that might be dangerous to mix by hand.

This link drying column show you how it is usually made.
The flow of gas passes into a washing/dehydrating bottle (down to the bottom where it bubbles up...the upper part of the recipient has an exhaust that goes sometimes into a second washing/dehydrating bottle or a guard bottle (in the case some liquid is splashed from the first bottle into the exhaust).
It works with liquid concentrated H2SO4, but also with solid dehydratants like Ba(ClO4)2 (dryerite), CaO (chalk - Edited thanks to Bert

: quick lime), CaCl2 (usual humidity absorbant for home), ...

[Edited on 2-5-2014 by PHILOU Zrealone]

guanidine nitrate from guanidine.X

chemrox - 4-5-2014 at 15:17

It would seem a simple conversion to make guanidine nitrate from guanidine carbonate or HCl via treatment with base and extraction followed by nitric acid. Did I miss something about the base or can this be done so easily? (The guanidine thread seemed completely irrelevant to this question).

plante1999 - 4-5-2014 at 15:21

Simply add an excess of nitric acid to guanidine carbonate in about two time its weight in water, and let it dry, it will yield a crystalline solid.

Are you planning on making new youtube videos soon?

TheAlchemistPirate - 5-5-2014 at 15:00

I was recently considering making ETN, and have been planning what chemicals to get, the exact procedure, etc. and I saw that it required ethanol or methanol as a solvent to recrystallize it(acetone is too strong). As I don't have access to ethanol and methanol apparently makes lesser quality ETN crystals, I didn't know what to do. I was wondering if ethyl rubbing alcohol would work, as it is just ethanol diluted with water, and ETN isn't soluble in water. If that is true, why don't people use ethyl rubbing alcohol instead? I know that it is used as a solvent in other recrystallizations, and it evaporates, like other solvents for related synthesis. I have searched google and the forums but haven't found anything as ETN doesn't seem to be very popular.

Napolean Dynamite - 5-5-2014 at 17:53

Denatured alcohol is Ethanol, sold at home depot.

Here is my question: In general, how loud/far away could a 1kg Ammonal (90:10) charge be heard assuming flat ground?. I have experimented only with high RE explosives in 20g amounts, you'll barely hear it from over 500 yards away.

Lerdan - 6-5-2014 at 03:03

Quote: Originally posted by Bert

Quote: Originally posted by Lerdan

Thanks for your reply, Bert.
I want to make a charge to det.
I extract my AN from fertilizer. The bag says it has 27% nitrogen in it :
13.5 % ammonia nitrogen
13.5 % nitrate nitrogen
I think these 2 are delivered by the AN ?

And it has 4% magnesium oxide in it too (dissolvable in mineral acid)
There is a lot of brown stuff in my filter, that should be calcium (it's in the brand name of the fertilizer)

I dissolve everything in water and filter the liquid out, which I then would use to make cast AN/AL (That would save me a LOT of time and efforts).

The AL should be pure.

So I can safely mix them at +-80°C ?
The guy here did it too : http://www.youtube.com/watch?v=RNoV8Tr38Wg

Also ; recently I tried to det a mixture of
- 12.5 % H202 (50% concentration)
- 15 % Al powder
- rest AN

My 7 gr minibooster of ETN/AN/Al did not manage to det it.
Should I use a bigger booster or does somebody have a better idea for my ratios ? Keep in mind, this mixture was already liquid-like, so it should not be more liquid (the AL would sink) Also : when I added the H2O2 to the AN/AL, it bubbled, and the mixture was a bit warm for hours) : is the reaction safe ?

[Edited on 6-5-2014 by Lerdan]

[Edited on 6-5-2014 by Lerdan]

[Edited on 6-5-2014 by Lerdan]

VladimirLem - 6-5-2014 at 08:33

Quote: Originally posted by Lerdan

I want to make a charge to det.
I extract my AN from fertilizer. The bag says it has 27% nitrogen in it :
13.5 % ammonia nitrogen
13.5 % nitrate nitrogen
I think these 2 are delivered by the AN ?

Also ; recently I tried to det a mixture of
- 12.5 % H202 (50% concentration)
- 15 % Al powder
- rest AN

My 7 gr minibooster of ETN/AN/Al did not manage to det it.
Should I use a bigger booster or does somebody have a better idea for my ratios ? Keep in mind, this mixture was already liquid-like, so it should not be more liquid (the AL would sink) Also : when I added the H2O2 to the AN/AL, it bubbled, and the mixture was a bit warm for hours) : is the reaction safe ?

sounds like AN...

why are you wasting that many AL?
A composition of 90 (AN) - 8 (C) - 2 (AL) works fine with some strong Det-Cap (at 0.8-0.9g/cm3 bulk density)

50% H2O2 is strong but around above 70% its becomes an explosive by itself...maybe you made the AN "wet" with it and more difficult to detonate....and again, why wasting that good H2O2 ?

even with H2O2 you will not get a even moderate strong explosive (ok, if it was pure H2O2, then yes^^)...and by the way...the higher the density of you compound is the less easy tro ignite it is...

just take the well know compositions like ANFO, ANNM or Ammonal and you will have much fun without wasting chems...a booster (20-50g) is (especially at ANFO, a strong booster!) always good

thebean - 6-5-2014 at 09:33

When people use the acronym GAA, are they referring to glacial acetic acid?

thesmug - 6-5-2014 at 13:14

@Thebean yes. Or at least almost always.

Napolean Dynamite - 6-5-2014 at 14:23

Can an explosive that is cap sensitive like ANNM in 500g amounts undergo full detonation in massive amounts (100kg) with centre initiation with only blasting cap just as with the small charge or is the shockwave absorbed throughout the material in cases of large charge.

Also could a 1kg ammonal detonation (90:10) be heard from 5 miles away on flat ground no trees?

Worst strategies in making new EM?

DubaiAmateurRocketry - 6-5-2014 at 14:30

Since azoles especially tetrazoles have been considered green and energetic, many authors has made derivatives of it and published their results, of course I appreciate their effort, however some strategies are really not helping.

I have seen many authors adding a methyl group into tetrazole's derivatives, ending up with a list of compounds having VoD around 6000 to 8000 along with long synthesis procedures. Since TATB, RDX and TNT already have similar performance and low sensitivity, these compounds are not really needed. I personally think adding methyl group is actually the worst idea in terms of performance. Methyl group contribute least density compared to others such as NH2, NHNH2, NO2, NHNO2, C(NO2)3, etc. You see some tetrazole compound's density drop from a high 1.8 to a 1.5 after adding a methyl group. furthermore, It is also very oxygen negative and hydrogen bonds from methyl group are almost negligible, which barely help with the sensitivity. These oxygen-deprived compound will produce toxic gases like CO, and HCN upon deflagration, and still categorized under ''green EM'' which is little ironic.

[Edited on 6-5-2014 by DubaiAmateurRocketry]

Metacelsus - 6-5-2014 at 15:08

Quote: Originally posted by Napolean Dynamite

Also could a 1kg ammonal detonation (90:10) be heard from 5 miles away on flat ground no trees?

It depends on whether you still have eardrums left after your kewl-ness.

Napolean Dynamite - 6-5-2014 at 16:28

Huh? my family has some property on a ranch in Wyoming we go to and I'd like to test one ammonal charge around 1kg, it's about seven miles from a town.

I have perfectly working ears also If you mean to say "cool" yes I think HE detonations are cool.

PHILOU Zrealone - 8-5-2014 at 06:32

Quote: Originally posted by DubaiAmateurRocketry

Since azoles especially tetrazoles have been considered green and energetic, many authors has made derivatives of it and published their results, of course I appreciate their effort, however some strategies are really not helping.

I have seen many authors adding a methyl group into tetrazole's derivatives, ending up with a list of compounds having VoD around 6000 to 8000 along with long synthesis procedures. Since TATB, RDX and TNT already have similar performance and low sensitivity, these compounds are not really needed. I personally think adding methyl group is actually the worst idea in terms of performance. Methyl group contribute least density compared to others such as NH2, NHNH2, NO2, NHNO2, C(NO2)3, etc. You see some tetrazole compound's density drop from a high 1.8 to a 1.5 after adding a methyl group. furthermore, It is also very oxygen negative and hydrogen bonds from methyl group are almost negligible, which barely help with the sensitivity. These oxygen-deprived compound will produce toxic gases like CO, and HCN upon deflagration, and still categorized under ''green EM'' which is little ironic.

[Edited on 6-5-2014 by DubaiAmateurRocketry]

True that methyl group is not the best with regards to density increase. But to be greener and less toxic; they should go for ethyl dérivatives (bio-ethanol)

Note that:
-Sometimes it is good to have other different molecules for pure accademic study and populate a database of related molecules.
-Methyl group may enhance stability of a molecule that would be to unstable for practical use without it.
See nitramine (H2NH-NO2), methylnitramine and dimethylnitramine.
See hydrazoic acid HN3 and methyl azide.
-In the case of highly positive OB, a methyl group will allow to bring some extra fuel and hydrogen (what is important for propellant properties).

[Edited on 8-5-2014 by PHILOU Zrealone]

Manifest - 8-5-2014 at 07:37

Where can I find a working safe synthesis of ETN using potassium nitrate?

Bert - 8-5-2014 at 08:02

"Safe" is not something anyone else but you can determine.

However, Google on:

etn synthesis potassium nitrate

And the exact thing you're interested in showed up, about 4th relevant thread listed on a site you're a member of...

Someone posted that Google worked better than the forum search recently?

Quote: Originally posted by Manifest

Quote: Originally posted by bfesser

Mesa, Variscite , Oscilllator: Don't forget that the forum has a <img src="./images/xpblue/top_search.gif" /> <a href="search.php">Search</a> function.

The forum search function is well, crap.
It doesn't find much and when you search google you tend to find what you're looking for.

use "experiment you're looking for here site:sciencemadness.org"

[Edited on 8-5-2014 by Bert]

Manifest - 8-5-2014 at 10:22

Okay Bert! Sorry for being lazy, my laptop is getting repaired at the minute and I am stuck using a slow phone. It is the thread titled ETN synth lab, right?
Do you reckon 91% sulfuric acid will work in nitrating the ethyrionol without much loss?
I'm also worried about the potassium sulfate formed, will that not clump up the mixture?

[Edited on 8-5-2014 by Manifest]

Turner - 8-5-2014 at 10:56

If using potassium nitrate use excess sulfuric keep reaction at 25C I have done Erythtirol nitration at 45C with anhydrous nitric and sulfuric acid no runaway but only 60% yield

TheAlchemistPirate - 8-5-2014 at 14:19

Hey I have questions regarding ETN too, as you might see above I'm trying to make it.
I recently bought Crown denatured alchohol, and was wondering is if anyone has crystallized ETN with it. When checking the msds I saw that it contains methanol(works for recrystallization),ethanol(works too),isopropylene(solvent), and methyl isobutyl ketone(solvent). I figure that since all those chemicals are solvents that evaporate it wont affect anything, I would like your word on it. I have seen some threads on here regarding using OTC denatured alcohol and someone said that it wont work due to contaminates, but they didn't say mention a certain brand. I'm also not sure if it would be dumb to not recrystallize this batch at all, as I will use it the next day and will properly neutralize it with water and sodium bicarbonate. I haven't found any sure answers for these questions with google.

Napolean Dynamite - 8-5-2014 at 16:37

Yes denatured alcohol will never be pure ethanol otherwise it couldn't be sold as "denatured" it will work. At least try it. I found the "natural" one for denatured alcohol is 95% ethanol. You'd probably be OK to not recryst. if you use it the next day but storing for any amount of time recrystalize it is best, it may be more sensitive without the recrystalization as that is a purification process. My question is whether acid can or can't be trapped in the crystals? I assume it can be when it is dumped into water forming tiny crystals, but probably not when a slow recryst. is done in ethanol forming larger crystals...

TheAlchemistPirate - 8-5-2014 at 18:53

I just tried making pure erythritol crystals with Truvia sugar substitute, but it isn't crystallizing.
I used this method. http://www.sciencemadness.org/talk/viewthread.php?tid=26679
The only differences between this procedure and mine were:
1.More water used (shouldn't have mattered)
2.When the Truvia was dissolved into the water,and all throughout the process, it remained clear.
I now have a clear solution sitting in my refrigerator, and its been 3 hours. I put a Teflon stir bar in it in hopes of starting the crystallization. I will probably leave it in there until I know what's wrong.

[Edited on 9-5-2014 by TheAlchemistPirate]

NeonPulse - 8-5-2014 at 21:05

i have used denatured alcohol many times to recrystallize ETN with no problems. there are many brands available with different additives, and one cheap one i tried even smelled like some sort of petroleum based chemical was added. this particular brand i did not attempt using for ETN though. there have not been any problems that i am aware of so far and i have recrystallized the ETN by crashing a solution into iced water, also both slow and fast cooling of a ETN/alcohol solution with ice and just allowing it to get to ambient temp then cooling. the crystals were well formed crisp snow white needles. it works well but i have not used plain ethanol so i dont have a reference to see if there really is any difference. Also i am not sure if truvia is pure erythritol or not. it probably contains stevia as well too going by the name of it.

markx - 9-5-2014 at 00:06

Quote: Originally posted by TheAlchemistPirate

I just tried making pure erythritol crystals with Truvia sugar substitute, but it isn't crystallizing.
I used this method. http://www.sciencemadness.org/talk/viewthread.php?tid=26679
The only differences between this procedure and mine were:
1.More water used (shouldn't have mattered)
2.When the Truvia was dissolved into the water,and all throughout the process, it remained clear.
I now have a clear solution sitting in my refrigerator, and its been 3 hours. I put a Teflon stir bar in it in hopes of starting the crystallization. I will probably leave it in there until I know what's wrong.

[Edited on 9-5-2014 by TheAlchemistPirate]

I think the answer to your lacking cristallisation is obviously displayed in point nr 1. If you use more water, then the solution will not become saturated and will not precipitate the excess on cooling. Simply...just reheat the solution and dissolve an additional portion of truvia to match the ratios described in the process.

NeonPulse - 9-5-2014 at 19:43

You can buy pure erythritol on eBay. Its called ritolsugar and its around $10for a 1kg bag. I have used this with great results and you can nitrate it straight from the bag. Its pure erythritol without stevia or other additives like the trivia brand and it Just needs a little grinding. No need to recrystallize or purify and it lasts ages. Not really that sweet tasting though. Its worth paying for I think. Worth looking into if ETN is your interest.

TheAlchemistPirate - 10-5-2014 at 11:30

I got it to crystallize, as markx said I used way too much water. I am going to be making etn tonight, if my crystals would freaking dry out in time lol. I wonder if acetone would help... Anyways, I'm still not sure about how to set it off. I saw it regarded as a primary on one thread, a secondary on another, and as in-between somewhere else. I might put a propane torch to a tiny amount later, just to test it.

markx - 11-5-2014 at 12:23

Quote: Originally posted by TheAlchemistPirate

I got it to crystallize, as markx said I used way too much water. I am going to be making etn tonight, if my crystals would freaking dry out in time lol. I wonder if acetone would help... Anyways, I'm still not sure about how to set it off. I saw it regarded as a primary on one thread, a secondary on another, and as in-between somewhere else. I might put a propane torch to a tiny amount later, just to test it.

You sound eager to rush things without having a proper understanding and a clear goal...bad combination. Never rush anything when engaged in a HE synthesis or any related process (drying for example). Make sure you have everything planned and all the tools and accessories ready before starting. Discovering mid synthesis that you don't have a vital tool or vessel ready can turn things ugly very fast.
As for setting off your product do not take a torch to it....very bad practice, plus in all probability you will have a deflagration if a small amount (<10mg) is used. Then you feel tempted to use more and that's when things will turn bad. Wrapping a small amount of ETN in foil and attaching to a pyrotechnical composition (black powder or KNO3+sugar type e.g) and lighting it via a fuse to heat shock the ETN is a 50/50 probability method to get it to DDT and see the power that unfolds. Use a quality fuse and a good length of it! It just makes my neck hair rise to high heavens when I see another vid of someone setting off a monstrous charge with a 10cm piece of fuse.

Find attached an article regarding nitric esters thermal stability :

Attachment: thermal stability-nitric esters.pdf (984kB)
This file has been downloaded 890 times

Manifest - 11-5-2014 at 13:20

What synthesis do you guys follow for ETN?
Yes, I have U.T.F.S.E and followed the thread titled 'ETN lab synth report' twice with failure.

The problem is I am using potassium nitrate, and the mixture clumps up when left to nitrate.

numos - 11-5-2014 at 13:24

Quick question, I recently stripped a miniscule amount of gold from a couple electronics, and for lack of a better use I dissolved it in some piranha solution. (Conc. sulfuric and 30% H2O2, 3:1)

I was left with a greenish solution which was evaporated to leave a orangey, red substance. It dissolves in water and when sodium metabisulfite is added (in solution) gold precipitated.

Any idea what this orange stuff is? I was thinking chloroauric acid, but that can't be - no chlorine atoms were ever present.

markx - 11-5-2014 at 23:15

Quote: Originally posted by Manifest

What synthesis do you guys follow for ETN?
Yes, I have U.T.F.S.E and followed the thread titled 'ETN lab synth report' twice with failure.

The problem is I am using potassium nitrate, and the mixture clumps up when left to nitrate.

What constitutes as "failure"? No product at all or just a low yield? I assume you attempted the synthesis at a rather low temperature <10C?

To use the salt+sulfuric nitrating mixture one needs a sturdy mixing aid to keep things agitated during synthesis.
Also using excess sulfuric (10-20% depending on the gravity of the clumping problem) will alleviate the problem to some extent.
As will keeping the temperature of the nitrating mix around +20C. If you cool the mix in the fridge, it will clump up before even having the chance to add any erythritol to it.
As far as my experience, the erythritol nitrations seem not to be very prone to thermal runaways, but in some case there may be contaminants that provoke it, so do not count on it not happening. Use a small batch to test the higher temp! Proceed with caution and have a quenching bath ready.
One can also dissolve the erythritol in a separate batch of extra sulfuric acid and add that in small portions to the nitrating mix to aid in uniform distribution of the reagents. The erythritol dissolving process is slow and yields a viscous liquid...it will cling to the walls of the dissolving vessel, so expect some losses due to that.
In all probability the typical expected yield will be around 50% with this route.

Burning dissolved explosives

Nitrator - 12-5-2014 at 23:00

Would a solution simply burn if you dissolved ETN, AP, etc in an organic solent such as ethanol or acetone. I'd like to dispose of some materials in a clandestine manner, and was looking for the safest/quietest method. There would be a high ratio of solvent to solute, I don't want some sort of blasting gelatin. Would this consistently burn calmly, or would it have a tendency to explode?

DubaiAmateurRocketry - 13-5-2014 at 01:08

Quote: Originally posted by Nitrator

Would a solution simply burn if you dissolved ETN, AP, etc in an organic solent such as ethanol or acetone. I'd like to dispose of some materials in a clandestine manner, and was looking for the safest/quietest method. There would be a high ratio of solvent to solute, I don't want some sort of blasting gelatin. Would this consistently burn calmly, or would it have a tendency to explode?

What do you mean? Those solvents you mentioned are already very flammable themselves.

Me and my friend tried to dissolve a concentrated solution of ADN in ethylene glycol, and the impact sensitivity was high, it could deflagrate similar to nitromethane and ethylene glycol dinitrate

PHILOU Zrealone - 13-5-2014 at 05:15

Quote: Originally posted by Nitrator

The more dilluted, the safest.
I once disposed of a 100g CTAP (cyclo-triacetonperoxyde) in 100 ml nitromethane...CTAP fully dissolves into it.
I stikked a very long fuse, hoping for a big explosion.
The container was Polypropylene.
After the fuse was off, nothing happened...I came closer with caution...all was gone, the container was empty and intact...no flame, no noise, no explosion.
I was astounished because CTAP usually burns yellow (rich at carbon and negative OB).

So dillution with a solvent fuel is indeed a good way to burn HE with less danger. But each case must be studied because solvent properties and explosive properties interacts sometimes dangerously.

Bert - 13-5-2014 at 07:05

Quote: Originally posted by Nitrator

Dissolve explosive in an excess of a flammable solvent, spread evenly over/absorb into a large sheet of dry cardboard, before solvent can evaporate, light a DRY, DOWNWIND corner of the cardboard and get away.

This has been done to dispose of nitroglycerin and Erythritol tetranitrate samples safely, have not tried it with primary explosives though.

Manifest - 13-5-2014 at 09:07

Quote: Originally posted by markx

Quote: Originally posted by Manifest

I leave it to nitrate and am left with dried up shit, I try dissolving it in water and filtering what remains but when I burn it it is potassium nitrate and potassium sulfate.

NeonPulse - 13-5-2014 at 23:29

Most information for PETN re-crystallizing suggest that acetone is the best choice of solvent for this particular HE. i cant find anyone who has chosen to use Methyl ethyl ketone as a substitute for the acetone, so my question is can MEK be used in place of acetone without any issues? i would think that it would be OK. if anybody knows reasons why MEK can't be used then i would like to know. i did try ethyl acetate recently but the results were tiny low density needles. I was just going to try MEK as an alternative and see what sort of crystals form. i would be starting very small scale if no other information is available about it.

markx - 14-5-2014 at 00:23

Quote: Originally posted by NeonPulse

Most information for PETN re-crystallizing suggest that acetone is the best choice of solvent for this particular HE. i cant find anyone who has chosen to use Methyl ethyl ketone as a substitute for the acetone, so my question is can MEK be used in place of acetone without any issues? i would think that it would be OK. if anybody knows reasons why MEK can't be used then i would like to know. i did try ethyl acetate recently but the results were tiny low density needles. I was just going to try MEK as an alternative and see what sort of crystals form. i would be starting very small scale if no other information is available about it.

Refer to the according section of Urbanski for information on PETN solubility in different solvents vs temperature. MEK is not discussed there, but aside from the question of PETN's solubility in it I see no problem with using it as a recristallisation medium.

NeonPulse - 14-5-2014 at 01:41

Yeah, i did see that chart and through out the section on PETN there was a heap of other interesting data but there was nothing on using MEK that i could find, neither in any of the urbanski volumes that i have. i guess that is why i thought i would ask others in the know here. as i mentioned i will start with a small batch and see how it goes.

TheAlchemistPirate - 14-5-2014 at 11:50

I have seen many topics on this site and other ones about explosive "casting" , and after looking it up I became interested and want to know how to do it. I have picked up on several things about it, but there are a few things Im not sure of such as:
What equipment do I need?
How much experience do I need to do it?
Is it too dangerous?
What situations is it necessary in?
I do know that casting is practiced in order to get as much explosive as you can into a certain area, since there are no spaces for air when it is a solid form. I also know it is used since it increases the VoD because a casted explosive is a single form and not separated by spaces, therefore shockwaves are able to travel more freely throughout the form. I also know that it can be dangerous to do because it might be heated to much, and to never try to cast a primary. I doubt that I can just use a hot plate with a water bath to heat a beaker full of say TNT, and just pour that into any form I want. Unfortunately, there doesn't seem to be any tutorials on this on the internet, at all. So please if you can, give me a link or tell me if this is too dangerous.

Turner - 14-5-2014 at 12:34

I also want to find out more on the casting of explosives.
If you are going to cast ETN use nothing but a hot water bath and a plastic container for the ETN. 15g or less can be casted this way safely I suppose if the ETN is neutral and recrystalized. I suspect that large amounts of molten ETN (50g or more) would be more prone to spontaneous detonation, I don't know why this is however

An example of a use for cast explosive is pentolite boosters used for ANFO in blasting industry.

I tried making a cast of TNT (15g) by melting it under water that was heated by hotplate. It turned out OK. I did not try making a cast by melting the material dry though .

Pic:

I would comfortably heat a beaker full of TNT heated by water bath until all material is molten and pour this into a mold

Process for preparing pentolite:

http://www.google.com/patents/US2395341

[Edited on 14-5-2014 by Turner]

NexusDNA - 14-5-2014 at 13:07

I have a question! It's actually reagent acquisition but it fits energetics too.

I've been trying to find erythritol here in Brazil, with no luck. Are there any south american members that can help me with this?

TheAlchemistPirate - 14-5-2014 at 13:17

Quote: Originally posted by NexusDNA

I have a question! It's actually reagent acquisition but it fits energetics too.

I've been trying to find erythritol here in Brazil, with no luck. Are there any south american members that can help me with this?

Erythritol is in several artificial sweeteners, I used Truvia and purified it with recrystallization. Here's a link on how to do it
http://www.sciencemadness.org/talk/viewthread.php?tid=26679
There are also some listings selling erythritol on ebay as well.

NexusDNA - 14-5-2014 at 14:07

I've only found baking blend Truvia which contains too little erythritol to be a reliable source.

The major problem is shipping edible things from other countries... they have a nasty tendency of not making it to my place (I've tried to import tea twice).

Motherload - 14-5-2014 at 22:05

Quote: Originally posted by Turner

I believe it to be a matter of probability.
ETN compared to TNT is sensitive and unstable.
Smaller the quantity ..... Smaller are the chances of running into "that" molecule
that "falls apart" during casting.
Just my theory.

markx - 15-5-2014 at 01:25

Quote: Originally posted by Turner

I also want to find out more on the casting of explosives.
If you are going to cast ETN use nothing but a hot water bath and a plastic container for the ETN. 15g or less can be casted this way safely I suppose if the ETN is neutral and recrystalized. I suspect that large amounts of molten ETN (50g or more) would be more prone to spontaneous detonation, I don't know why this is however

An example of a use for cast explosive is pentolite boosters used for ANFO in blasting industry.

I tried making a cast of TNT (15g) by melting it under water that was heated by hotplate. It turned out OK. I did not try making a cast by melting the material dry though .

I would comfortably heat a beaker full of TNT heated by water bath until all material is molten and pour this into a mold

Process for preparing pentolite:

http://www.google.com/patents/US2395341

When considering a cast charge it would be wise to note that the critical diameter will usually be larger compared to a pressed charge. This can lead to failure on initiation if the dimensions are too close to the critical value. This in turn will mean a repetition of the casting process, putting the operator in harms way again. A practice that I would advise strongly against in amateur settings, especially with a sensitive group of substances like nitric esters.

Manifest - 17-5-2014 at 03:26

Finally worked out a working method for ETN.
Pour 60ml of 91% sulfuric acid into a conical flask and cool it using an ice bath! then slowly add 30g of potassium nitrate with swirling of the flask, waiting for it to cool down after each addition.
After swirling, get a stirring rod and break down all the bits of potassium sulfate into smaller pieces.
Swirl again and leave for 5 mins then transfer the liquid to another conical flask, making sure not to transfer any solids.
Then take off the ice bath and slowly add 8 grams of Erythritol to this slowly!
Swirl it and leave it for about 3 hours and it will thicken up then, stir it with a rod and wash out with water into 500ml water, stir and filter.

Recrystallisation may be necessary.

NeonPulse - 17-5-2014 at 04:21

Re crystallize it for sure. Just to eliminate any trapped acids and for purity sake. Unless you are planning to use it within a couple of days but even if you are going to use it quickly you still could recrystallize it for practice

Manifest - 17-5-2014 at 04:34

How much ethanol should I use to recrystallise?

Turner - 17-5-2014 at 05:50

Around 15g:100ml ethanol

Manifest - 17-5-2014 at 12:31

That seems like a lot, what a waste of precious ethanol!

Turner - 17-5-2014 at 13:41

Just boil an amount of ethanol and see how much ETN can dissolve then you will have a definite answer.

Liquid HE's = no recrystalization solvents needed

TheAlchemistPirate - 17-5-2014 at 14:28

I recently have been exploring HEs and the chemistry behind them, but have run into a problem. Basically, I cant set them off due to not having access to commercial blasting caps( Who would've thought?) . I realized I might have to make my own, but this seems very dangerous and possibly too expensive. I have been reading a lot about primaries and improvised blasting caps , etc. and cant decide on what to do. Optimistically I figured I could make a miniature aluminum melting oven with firebricks, a graphite crucible etc. , cast a blasting cap, fill it with lead azide and cyclonite and be done. Though when researching this I discovered this wouldn't be as simple as I thought. First, I found a castiing and metalworking website and looked into making my own aluminum casting setup, but this seems VERY dangerous for obvious reasons for things such as fumes, the fact you are handling molten metal with metal tongs , etc. I also searched for lead azide syntheses and saw and article of someone dying from ingesting one gram...ONE GRAM! I don't plan on eating it obviously, but what would several grams do to your skin? I know that several members on here detonate HEs which require blasting caps but they never seem to explain how. I know this isn't an explosive-focused site but I would rather take advice about HEs here than anywhere else. I am only 14, and I don't know if I'm even capable of safely handling these things...

Manifest - 17-5-2014 at 14:40

A better method for setting off secondaries may be using small firecrackers. I know where I live I can get them(illegally) for cheap near halloween, I might stock up on them.

TheAlchemistPirate - 17-5-2014 at 14:44

Where I live I can get very powerful firecrackers that are two inches long and half an inch thick (legally?) but I cant see them setting off things like gelatin dynamite and other things I plan making in the future. I plan on using cyclonite as a base charge by the way. I would very much prefer not making primaries at all as they are either very dangerous or a complete pain to make.

[Edited on 17-5-2014 by TheAlchemistPirate]

[Edited on 18-5-2014 by TheAlchemistPirate]

Turner - 17-5-2014 at 15:41

Firecrackers usually can't create enough pressure at the wave front because FP burns too slow. Even though firecrackers can sound pretty snappy and sharp, it is not a reliable initiation of secondary explosives.

Manifest - 17-5-2014 at 15:46

You can use it to set off ETN which would set off whatever you want then.

ETN can be used as a primary wrapped in aluminium foil and rapidly heated, it is very stable and has a very long shelf life.

gdflp - 18-5-2014 at 15:50

Just starting to experiment with EM, and decided to try potassium chlorate. I put as small quantity in a test tube(1-2g) and held the test tube using a clamp and heat resistant gloves. I heated the chlorate with a propane torch until it melted, then put a small amount of sugar into the tube. It started as I expected, then when it just started to get going, the bottom of the PYREX test tube fell out with molten liquid dripping out of it(it looked like glass). Is it normal for borosilicate glass to break like this, or were the test tubes low quality?

DubaiAmateurRocketry - 19-5-2014 at 11:48

Quote: Originally posted by gdflp

Just starting to experiment with EM, and decided to try potassium chlorate. I put as small quantity in a test tube(1-2g) and held the test tube using a clamp and heat resistant gloves. I heated the chlorate with a propane torch until it melted, then put a small amount of sugar into the tube. It started as I expected, then when it just started to get going, the bottom of the PYREX test tube fell out with molten liquid dripping out of it(it looked like glass). Is it normal for borosilicate glass to break like this, or were the test tubes low quality?

I Think so...

I ran PROPEP3 code with this assuming chlorate:sugar ratio was 2:1, and at melting point of potassium chlorate, the combustion temperature was around 3500 degree celsius or more.

Manifest - 19-5-2014 at 13:35

Yes gdflp that is normal, KClO3 + Sugar mix will create a lot of heat.

A brilliant method for setting off ETN is to get a thick cardboard tube from the inside of Aluminium foil rolls and to block off the bottom and pour a little bit of wax to block it off.

After the wax hardens I added KNO3/Sugar mixture in a 60:40 ratio and wrapped a few grams of ETN tightly in Aluminium foil and pressed on it to remove air, the aluminium with ETN is then inserted into the corner in the cardboard on top of the KNO3/sugar
A fuse is inserted into the KNO3/sugar

Cardboard tube

Wax melted to hold contents

Arial view of the tube

This method worked for me 6/6 times that I have tried this, the ETN needs to be tightly packed.

Bert - 20-5-2014 at 04:44

Yes, it's not unusual to have even Pyrex glassware break or melt from extremes of temperature- an organically fueled pyrotechnic mixture can do this, a metal fueled mix could easily melt steel, let alone Pyrex. The "gummy bear demo" works as it does partly because the fuel is a single "chunk", adding the fuel as a fine powder greatly speeds the reaction.

Try this (outdoors on a fireproof surface and wearing hand, face & eye protection!):

Mix a SMALL amount (1 gram total is PLENTY) of Potassium chlorate with table sugar in a 70:30 ratio (.7g chlorate:.3g sugar). Mix by placing on a sheet of paper and rolling it around by alternately lifting corners of the sheet, not by stirring with a hard object. Place the mix in a little pile on a brick or tile. Take a glass rod and dip it into concentrated sulfuric acid, then touch the pile with the acid wetted rod or drip a single drop of the acid onto the pile.

Stand back and observe- the pile will crackle, evolve gas and probably ignite. If you used powdered sugar (DON'T) and mixed it thoroughly, it may even explode.

Detonation of wet HE

Turner - 25-5-2014 at 18:10

So I did a few hammer tests with (150-200mg) solid chunks of cast ETN. I noticed that as soon as these pieces are wetted with water, they become insensitive to even a hard hammer hit. The times I have plasticized ETN I can still fairly easily hammer detonate 50mg pieces, but even with this little amount wet with water is insensitive to hammer.

I wonder if a mass of damp crystalline ETN (10% water by weight) could detonate from the force of a no. 8 detonator.

Could a mass of solid, cast pentolite detonate reliably even if there was water in the cap-well?

[Edited on 26-5-2014 by Turner]

APO - 29-5-2014 at 14:15

Damp ETN can easily go off with a detonator. In fact, water is sometimes used in explosives to make the detonation wave travel at a more consistent rate.

What do you mean by cap well?

Turner - 29-5-2014 at 14:39

With a solid cast melt explosive charge, the hole in the center for the detonator.

NeonPulse - 29-5-2014 at 20:24

Some time ago when i first made ETN, i was impatient and couldn't wait to set it off. This batch was still slightly damp and it still did detonate with its usual fury. it was damp to the level that if you squeezed some together it would all stick and hold its shape but still went off well. Another fact that ensured detonation was i went overkill with the initiator using 2.5g HMTD to set off 11g of loosely packed ETN. There was no trace of the half cinder block piece the charge was placed on.
As for water in the cap well i dont see why that should hinder a detonation as the cap well is only big enough for the cap so in placing that in the well you would push out a lot of the water anyway.

Morgan - 31-5-2014 at 15:44

I was toying with a neodymium magnet and wondered if a nearby gold plated coffee filter would be attracted to and it was. I have some gold plated nickel wire and I just became curious what the base metal might be on the filter.

http://www.seattlecoffeegear.com/frieling-23-karat-gold-plat...

arkoma - 13-6-2014 at 17:03

Is the specific gravity of liquids affected by altitude?

edit---oops, wrong quick questions thread!! (I did UTFSE, but didn't realize there were two quick questions threads, energetics ain't my thing)

[Edited on 6-14-2014 by arkoma]

Motherload - 14-6-2014 at 06:25

This is not directly related to energetics but I don't think it requires a new thread somewhere else..
I can't find any info reguarding electrolysis of concentrated H3PO4.
I am hoping it will yield at least some P2O5 dissolved in H3PO4.

Dornier 335A - 14-6-2014 at 13:58

Will pure H₃PO₄ conduct electricity? Surely there must be some water in it to create ions, and then you won't get any P₂O₅.

Motherload - 15-6-2014 at 10:50

H3PO4 cannot be distilled past 85% .... Anymore heating and it turns into meta phosphoric acid HPO3 which is a solid.

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