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nitroglycerin

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Totenkov - 21-4-2008 at 18:47

I would recommend adding a little ethyl or methyl alcohol to that NG. It is defiantly a good idea to store it in plastic, should the NG get angry, but add alcohol for storage, if you plan to store it for more than about 2 weeks.

Boomer - 23-4-2008 at 02:34

pdb's accident is the only one I know of where nitro has gone off during a runaway in a home batch. Industrial hundred-gallon batches using fuming acids were known to go high order after burning some seconds with a hissing flame, at least when enough product had already separated.

In contrast, I've an old chemistry book that states "The procedure is without danger if the temperature is watched tightly"! They mean using HNO3, having a thick porridge with KNO3 may make even cooling harder. The main reason I used exclusively AN for the nitrate.

That is unless I used fuming nitric, which gives 92% yield at only 25-30% excess if the sulfuric is concentrated enough (i.e. no 90% drain cleaner).

pdb - 23-4-2008 at 04:36

Boomer, check your U2U please.

Pulverulescent - 23-4-2008 at 06:03

IMO, using AN in nitro-synth could be hazardous since FGAN is often impure.

Some FGAN is made from ammonia which comes from gas-liquors and can be contaminated by phenols and possibly pyridines and who knows what other organics!

Pdb's accident could have been caused by some contamination he wasn't aware of!

Use the strongest, cleanest mixed acids possible for your own safety!

I'd say glyceryl trinitrate demands it!

P

gregxy - 23-4-2008 at 10:10

One way to purify your acids would be to add the nitrate salt to the H2SO4 and then heat the mixture to 50C, hopefully this would oxidize any organic impurities. Cool before adding the glycerine.

The viscosity of the mix could effect the stability, in a thick mix local hot spots could form where the temperature is much higher than the surrounding regions. In a thinner mix currents would develop which would help spread out the generated heat and reduce the local temperature.

Runaways are not always bad, in fulminate production ethanol is added to HNO3 and the mixture is allowed to runaway. However since the ethanol, and other reaction products boil at a low temperature, the reaction temperature cannot go very high. In NG production, the only thing that boils below the NG detonation temperature is the nitric acid.

Pulverulescent - 23-4-2008 at 11:11

Quote:

Originally posted by gregxy
One way to purify your acids would be to add the nitrate salt to the H2SO4 and then heat the mixture to 50C, hopefully this would oxidize any organic impurities.

Is hopefully good enough, considering what you're doing?

What if some impurities are nitrated instead?

And what if an unstable mixture of nitrates forms?

Too many questions, use freshly distilled HN03!

P

Drain openers?

lucky123 - 5-5-2008 at 04:55

What concentration H2SO4 are the drain cleaners? Liquid fire and roto from Ace hardware there is another one from Lowes forget the name though? I also curious can these be used to make nitro since they have look funky with some kind of additive that's black... Will this effect the color of the final nitro? Or perhaps if making nitrocellulose will your cotton be dyed black in the end or does this not affect the final product in anyway?

ScienceGeek - 5-5-2008 at 05:00

Try to actually read the thread!

Quote:

Originally posted by hightechstuff
Hi Everyone,
I recently synthesized 10 ml of NG from Rooto drain cleaner, ammonium nitrate and glycerin. Now, I know this is a pretty $#!tty way to synthesize NG but it did work. I am a little concerned about the purity of the final product though. The AN was fertilizer grade and had some impurities in it and the 93% H2SO4 is obviously waste acid from some industrial manufacturing bottled up and sold as drain cleaner. The NG has the color of olive oil with only a slight haze. A major concern for me is that these impurities will make the NG more unstable and possibly react negatively unprovoked. Is their a way to purify my NG? Do I have a ticking time bomb on my hands? Any comments and suggestions would be greatly appreciated.
Thanks!
hightechstuff

Quote:

Originally posted by ScienceGeek
The hazyness is not a problem, as this is just a hydrated form of the nitroglycerin. This can be removed by desiccation.
The color, on the other hand, indicates (most likely) unwanted metal ions, probably from the H2SO4. This is a big problem when it comes to stability.

If it was me, I wouldn't dare desiccation, as it could detonate all on its own.

texaspete - 19-5-2008 at 17:43

Quote:

Originally posted by lucky123
What concentration H2SO4 are the drain cleaners? Liquid fire and roto from Ace hardware there is another one from Lowes forget the name though? I also curious can these be used to make nitro since they have look funky with some kind of additive that's black... Will this effect the color of the final nitro? Or perhaps if making nitrocellulose will your cotton be dyed black in the end or does this not affect the final product in anyway?

Usually 94%. I made a small amount of nitro with Floweasy and KNO3. I had a lot of trouble keeping the mixture cool, as the KNO3/H2SO4 formed a sludge that was nearly impossible to stir. In the end, the small amount of nitro that resulted was amber colored, but not too badly. Maybe AN will work better, but HNO3 is definitely best.

ADP - 19-5-2008 at 19:22

When it comes to mixed acids I've found that letting the mixed acids react overnight produces a nearly clear solution that can be used. I was experimenting with the "liquid lightning" drain cleaner which is a nasty black color. Last night I saturated the solution with as much NH4NO3 that I could while stirring the mix. Last night it went from black to an orange color but this morning it was completely clear with the NH4HSO4 floating on the top of the mix!

Needless to say was I excited at this and removed the sulfate salt. I personally vacuum distill the HNO3 before using it though. I'm not keen to mess with 'mixed acids'.

On the subject of NG however, I plan on using some 95%+ white fuming nitric acid with some ACS 98% H2SO4 to nitrate my glycerin. Would a 1:1 ratio of HNO3/H2SO4 suffice for my synthesis?

[Edited on 19-5-2008 by ADP]

crazyboy - 19-5-2008 at 19:31

Why waste 95% nitric on this just use 70% the ratios I use are:

100 ml of >95% H2SO4 (sulfuric acid)
70 ml of 65% HNO3 (nitric acid)
22 ml of 100% C3H5(OH)3 (glycerol)

(from brainfevert)

ADP - 19-5-2008 at 19:55

Considering I make the 95%+ nitric from my mixed acids and vacuum distillation, it's not a problem. It'd be better yield and easier honestly

jmneissa - 1-6-2009 at 12:48

Hey guys I recently about an hour ago I did a small nitration of glycerin to nitroglycerin. My yield was extremely poor only 1.5ml og NG for my original 10ml glycerin. I used sulfuric acid and potassium nitrate. I have written up the lab here it is:
Reactants:
60 ml H₂SO₄
25 ml KNO₃
10 ml C₃H₅(OH)₃

Procedure:

I mixed the KNO₃ with the sulfuric acid quite quickly in a salt ice bath. Some small amounts of Ammonia like fumes were given off. With the window open it was unnoticeable unless one purposely smelt the reaction. Upon adding the glycerin the temperature was maintained around 5˚C. After addition of all glycerin it was left to sit for 15 minutes in the ice bath. Upon adding twice volume of cold water the liquids separated. After repetitive washings and neutralization I was left with a very small amount of an oily yellow substance of about 1.5 ml

I was hoping you guys could see the flaw in my synthesis so that I could a good yield. Thanks!

User - 1-6-2009 at 17:06

Yes i can tell you whats wrong.
Nitrating this short amount off time doesn't do shit.
Besides after addition of the glycerol one could take the mixture out of the icebad and let it slowly gain temp, even 20 deg. wont cause runaway's as long as there are no jumps.
The temp is really important for the formation of nitrate esters.

I dont know about the balance of reagents, maybe you should look up some synthesis.

Btw pure NG always forms white blobs, at least in my case.

[Edited on 2-6-2009 by User]

The_Davster - 1-6-2009 at 17:12

Wet NG is white. Dry NG is colorless.

User - 2-6-2009 at 03:10

Yes sorry , i meant after crashing it, i wasn't thoroughly enough.
I mean if its yellow it means that it is contaminated.
Pure NG isn't a very stable explosive, contaminated NG is scary.

jmneissa - 2-6-2009 at 04:47

Thanks for your advice guys! Few questions, how much time should I let the mixture nitrate? 20 minutes, 30 minutes etc... Also what would cause the nitro to be contaminated and is there a way to remove these contaminates? I knew that it didn't look right this is why I destroyed it after washing it and neutralizing. Thanks...

hissingnoise - 2-6-2009 at 05:33

I'd advise using strong, clean mixed acid!
Fewer things can go wrong and you'll get ~22ml from your 10ml of glycerine. . .
Distillation of HNO3 isn't difficult and upping the conc. of H2SO4 is a breeze (cough)!
And since the thread is long and informative, I'd suggest you read the previous posts. . .
Failing that, there's always "COPAE" in the forum library!

[Edited on 2-6-2009 by hissingnoise]

User - 2-6-2009 at 05:48

The most nitrations that I do just sit around and stir for a couple of hours to ensure full nitration, it cant hurt to let it sit for a while.
30 min after last addition I take the mixture out of the ice bath and place it on a stirrer and let it gentle climb to room temp by itself and let it sit for 2/3 hours.
Reaction time multiply by a factor 2 for every 10 degrees iirc.
Do the math.

Rich_Insane - 2-6-2009 at 16:33

The glyceirn they sell around here as a skin protectant has tocepherol (Vitamin E). Should that be a big problem?

User - 3-6-2009 at 01:55

Trust me you dont want to mess around with impure reagents, especially not for making something like NG.
Obtainig pure glycerol shouldn't be to hard.
It is worth searching.
Do you have any idea what NG's properties are??.

Deceitful_Frank - 3-6-2009 at 04:06

Quote: Originally posted by hissingnoise

Fewer things can go wrong and you'll get ~22ml from your 10ml of glycerine. . .

That's just impossible... over 112% theoretical yeild!

You may be confusing millilitres with grams here but IMO advice dished out concerning manufacture of nitroglycerin should come with a healthy portion of anality!

hissingnoise - 3-6-2009 at 05:14

Anyone familiar with O-nitration knows those yields are typical for ngl. . .
NO2 is triatomic---think about it!
It's not rocket surgery. . .

Deceitful_Frank - 3-6-2009 at 13:09

22ml of NG weighs 34.98 grams. The maximum theoretical yield when fully nitrating 10ml (12.5 grams) of glycerol is 30.84 grams.

Forget rocket surgery... this is high school level chemistry and math!

Rich_Insane - 3-6-2009 at 14:44

It isn't that hard, but nowadays I'm wary of ordering stuff online. So using that glycerin is not possible? I'm going today to see if they have just pure glycerin.

497 - 3-6-2009 at 15:15

Ordering glycerin online is really not suspicious at all... Unless you somehow order it along with a bunch of conc. H2SO4 and HNO3 don't worry about it..

hissingnoise - 4-6-2009 at 03:25

Quote: Originally posted by Deceitful_Frank

You may be confusing millilitres with grams here!

Sorry Frank, you're entirely right, it should be grams.
I shouldn't rush-post without thinking. . .
It's good to know someone has their head screwed on.
And it isn't the first I've confused volume and weight.
Keep up the good work. . .

problem with my nitroglyrcerine

Bikemaster - 24-8-2009 at 07:21

I made some nitroglycerine, and after the neutralisaton with sodium bicarbonate, i let the nitro dry at room temp. one day after, all the nitro was clear and dry. But something make me freak a bit...because the nitroglycerine was fuming. Normal or not???
I make some test and i find that the nitro was slightly basic.
I also just was the nitro one time with water from the sink after the neutralisation.

What can be the cause of the fuming ng???
I also made a test on sensitivity and the ng is not really more sensible, but i think the degradation of the ng will just be faster, it is why i want to find the problem.

thx

hissingnoise - 24-8-2009 at 08:26

Quote: Originally posted by Bikemaster

I also just was the nitro one time with water from the sink after the neutralisation.
What can be the cause of the fuming ng???

Oh boy! There must be a serious water-shortage in your area?
You make a potent high explosive and then can't be bothered with its proper purification.
I hope for your sake the quantity was small. . .
You can't overwash nitro---use cold water with neutral pH several times.
That kind of carelessness can get you maimed or worse. . .

[Edited on 24-8-2009 by hissingnoise]

Bikemaster - 24-8-2009 at 11:06

Wait... i know that i am working with explosive. I am not stupid.

That was just a 7ml bacht, and when i see that, i destroye the ng. The last message was just to know it was normal or not and if not, what is the probleme (for other good and safe bachts...)

Also can i use dillued hcl to make it neutral if it turn basic???

hissingnoise - 24-8-2009 at 13:22

Bikemaster, forget about making nitro for a while!
Read up on it until you have a good understanding of what it is you're doing.
You've been lucky this time---7ml may not actuall kill you, but it'll sure mess up your life if it goes off when you're nearby.
And decomposing nitro is extremely shock-sensitive. . .
COPAE by Davis in the forum library is a good place to start.
Happy reading!

Bikemaster - 12-9-2009 at 14:43

test 2...

I start by reading a lot of text about NG but i find nothing more that i was already know about it.
But i made a intelligent purchase...ph paper. (before i was checking the ph with a solution of red of phenol).

So i made a batch of nitroglycerine as normal.
After wash it as normal, i test the solution with ph paper and it was neutral. But after puring the ng in the desincator, i saw some fume....
I was really discuraged, but i try put the ph paper directly into the NG...it turn red (1.5 of ph). I just step back...this is not a good felling to see really acidic NG drying on the fron of you... It is also the reason why I was not able to see if the ng was acid, because i was testing de solution on the top of the ng and not the ng...
So i retry to neutralise the ng with strong solution of sodium bicarbonate. But it has no impact on the NG ph...So think about the stiring method. Maybe that the stiring rod was not stiring enough to make a good contact between the basic solution and the NG. So i put a stir bar in the beaker and make it spin on the magnetic stirrer. After 30 sec, i stop the stirrer and i saw that the water have a color of soft yellow

. NO2 out of the nitro...good thing.
So i made this action many time, until the ng was really test neutral. After i wash it 4 time with water and i let it dry in the desicator.

The NG have dry 5 time faster that the last time, and it is as clear as water, and no more fume are coming out of the nitro. I was also really impressed by the real stability of the nitro, it is now really harder to make it blow by the hit of an hammer.

Thanks for the good advice you give to me

hissingnoise - 13-9-2009 at 07:59

You're welcome! I would be wary of stirrers when washing nitro because of the slight chance that friction between the stirrer-bar and the nitro might set it off.
A thorough neutralisation, though, will make washing easier.
It is the most important step, so don't skimp on it time-wise. . .
Use only dilute alkali and gently swirl, or rotate the beaker on a table-top, so that the blob of nitro rolls slowly around the bottom of the beaker; this will, by degrees, expose the interior of the nitro to alkali so that all of the residual acid within is removed.
The washings too, should be done by swirling until the used wash-water tests neutral to litmus---when it does, give your nitro a final wash for safety's sake!

[Edited on 13-9-2009 by hissingnoise]

Bikemaster - 13-9-2009 at 14:00

I was also worry about the stiring method... Maybe it could be better using some compressed air to stir the mix.

densest - 13-9-2009 at 17:18

Tenney L. Davis "The Chemistry of Powder and Explosives" Angrieff Press, Las Vegas: pp 203-204 "The nitroglycerin from the separator contains about 10% of its weight in dissolved acid... Most of this is removed by a drowning wash.... water ... while the mixture is agitated with compressed air."

"It is washed again with water, then with sodium carbonate solution (2 or 3%), and then with water until the washings give no color with phenolphthalein and the nitroglycerin is neutral to litmus paper"

Be safe - keep your fingers intact.

hissingnoise - 14-9-2009 at 09:50

Agitation by compressed air is totally unnecessary (and probably unwise) for small-scale synths.
Stick with slow swirling---it's safer.
Unless, that is, you're washing the product of a large industrial nitrator. . .

[Edited on 14-9-2009 by hissingnoise]

Microtek - 18-9-2009 at 05:04

According to Urbanski, it should be safe enough to stir NG and water(vol 2, pg 55):

Quote:

An emulsion composed of 200 parts of water and 100 parts of nitroglycerine is incapable of being initiated. In order to achieve complete safety, however, a ratio
of 300 parts of water to 100 parts of nitroglycerine should be chosen.

If you start by stirring the water at a relatively high rate and then slowly add the NG, it should be possible to form the emulsion immediately. With a sufficient amount of water it should be very safe, and much more efficient than other methods.
If glass/teflon friction still seems too risky, you could simply use a hand mixer and make sure that it doesn't get into contact with the vessel.
Another option would be to use a plastic container instead of a glass beaker. That way, impacts between the stirrer magnet and the container wall would be even less of a concern.

hissingnoise - 18-9-2009 at 06:40

A large tallish plastic container for the drowning water does seem a good idea.
With a large enough volume of cold water the drowning should remove most of the acid fairly quickly.
The wash-water could be partially decanted easily and hand-mixing the water non-hazardous.
I always stir the reaction mixture itself with a thermometer, hyperventilating each time it bangs off the glass. . .
I haven't the guts to try gravity-separation and anyway I'd probably lose some Ng that way while saving acid.

Bikemaster - 18-9-2009 at 08:28

A plastic beaker seem to be a very good idea. It will considerably reduce the force of the impact between the teflon stiring bar and the beaker.
Also, my beaker was really small (50 ml) and when the beaker it not perflectly center on the stirrer, the bar hit many time the beaker wall...I don't think the NG love that... So i really think that the plastic beaker is a judicius choose.

hissingnoise - 18-9-2009 at 09:08

Quote: Originally posted by Bikemaster

Also, my beaker was really small (50 ml) and when the beaker it not perflectly center on the stirrer, the bar hit many time the beaker wall...

A 50 ml beaker is way, way too small for what you're using it for Bikemaster,---are you trying to invite disaster, or what?

Bikemaster - 18-9-2009 at 16:51

I was not thinking that it was a big probleme. I only have 2 ml of ng in the beaker, and i put like 30 ml of water with it. Than is way over the 3 time more water that ng so i don't think it is really dangerous???

hissingnoise - 19-9-2009 at 06:33

OK, 2 ml doesn't seem like much but 30 ml wash-water is still on the low side. . .
And even 2 ml going off in a glass is enough to cause serious injury.
A 600 ml beaker would have been a safer bet!

Bikemaster - 19-9-2009 at 13:43

I agree with you, only 2 ml of ng can cause big injury, even 0,5ml can be dangerous...
I make a test with 3 drop of ng on an aluminium foil (many time foilded to slow the heating speed), and i put a flame under it (flame was remote and i was far from it). After some NOx escaping, a powerful detonation occure (more powerful that the same test with tatp). The aluminium foil shreaded in very small peices, so i don't want to see this in my glassware...
thanks for the tip, next time it will be in a bigger beaker.

[Edited on 19-9-2009 by Bikemaster]

User - 20-9-2009 at 05:51

I have quite some experience with NG resulting in finding it scary stuff.
That doesn't mean it cant be handled safely, still it tends too much towards a primary explosive.
Nowaday's I personally prefer EGDN/PGDN instead of NG.
The little difference in performance is definitely worth the safety.
I found that both egdn and pgdn are harder to set off by hammer than NG.

[Edited on 20-9-2009 by User]

hissingnoise - 20-9-2009 at 14:07

EGDN seems a good choice; as well as being less sensitive it's also slightly more powerful and has a higher VoD than nitro.
And according to Davis its synthesis is somewhat less hazardous than that of nitro; its weaknesses are its greater volatility and its higher solubility in water.

Microtek - 21-9-2009 at 03:17

Also, the zero oxygen balance of EGDN makes it less suitable for use as a propellant oxidizer (which is all I ever use NG for).

Zinc - 4-12-2009 at 10:37

Today I tried to make NG.

To 85 ml of H2SO4 I added 50 g of NaNO3. When the NaNO3 was added (in 3 min.) the mix heated up a bit and most of the NaNO3 dissolved. When the mix cooled to 15 C (in a ice bath) I started adding glycerine. 12.5 ml were added during around 20-35 min. When all of the glycerine was added, I let the mix stay 10 min in the ice bath and around 25-30 min outside of it. Then I poured the mix in around 500 ml of water. The solid part of the mix settled down, and I could see a small amount of some liquid that is not mixing with water float above the precipitate. I decanted most of the water and added a new portion of 500 ml water. Now most of the precipitate dissolved and I could still see some whirls of non water miscible liquid in the water, but the liquid never settled, it "dissapeared".

So has anyone an idea what did I do wrong?

All the chemicals were analitical grade, so I dont think contaminants could cause that. The same thing happened some time ago when I tried to make NG with boiled down battery acid and AN extracted from fertiliser.

hissingnoise - 4-12-2009 at 13:02

Your product would have been mono and dinitro glycerol; both are soluble but the dinitro will precipitate when small amounts of water are present.
Either there was too much water in the mix, initially, or you added too much glycerol. . .
You can correct it, next time!

quicksilver - 5-12-2009 at 09:42

If one uses a aquarium aerator pump (cheap too) and curves the hose to circle at the bottom circumference of the vessel, the result will be a gentle whirlpool, mimicking a stir-bar but with light air. Works well, little danger of a "bump". Speaking only personally, I would be quite hesitant about stirring manually with an object.

IF the glycerin were introduced at a slow level of drop by drop at 12.5ml @ 20-35 minutes he SHOULD have gotten SOME fully nitrated material. Sounds like the mixed acid was either MUCH too weak or H2SO4 was not at strength - HOWEVER, when the solid nitrate has not really gone into solution ("and most of the NaNO3 dissolve") I would think there is really not an appropriate mixed acid for even the di-nitrate. Not 100% sure but I think the di-nitrate would separate out. Aside from that leaving any existing solid within that type of nitration might provide a basis for friction or hot-spot.

Saline saturated water salted to the highest level of saturation possible together w/ and alkali of choice (a carbonate, etc) should produce a wash that sucks the water from the existing nitrated material; at least enough to see it as a layer. Leaving the existing nitrated product in such a wash for a 12 hour period should get you a good start.

-=-=-=-=-^-=-=-=-=-^-=-=-=-=-^-=-=-=-=-^-=-=-=-=-
I do have a somewhat off topic question however....If a material (solid) is recrystallized could not some acid PH level exist within the crystal in which any wash water would not display? Therefore a PH reading should be taken at several different times during a synthesis to circumvent that? Or would that acidic level always be readable even if the final solid does not go in the solution of wash (water)?
Or picture a scenario like a complex crystal lattice (a clathrate), couldn't a level of acidic condition exist in with one of the materials affecting the longevity of the clathrate?
I keep thinking about WHY the clathrate was not commercialized and pictured the picric acid compelling an acidic condition within the lattice, eventually deteriorating the final product. [This could take quite awhile] but I always wondered why the material was not a commercial standard when price / yield level vs. silver azide would make competitive sense.

[Edited on 6-12-2009 by quicksilver]

Zinc - 6-12-2009 at 06:23

Quote: Originally posted by hissingnoise

Your product would have been mono and dinitro glycerol; both are soluble but the dinitro will precipitate when small amounts of water are present.
Either there was too much water in the mix, initially, or you added too much glycerol. . .
You can correct it, next time!

Yes it could be that mono- and di- nitroglycerine formed. About the ratios I belive that they are quite good, perhaps I didnt let the glycerine long enough in the nitrating mix. Is one hour enough, perhaps two?

Quote: Originally posted by quicksilver

Sounds like the mixed acid was either MUCH too weak or H2SO4 was not at strength - HOWEVER, when the solid nitrate has not really gone into solution ("and most of the NaNO3 dissolve") I would think there is really not an appropriate mixed acid for even the di-nitrate. Not 100% sure but I think the di-nitrate would separate out. Aside from that leaving any existing solid within that type of nitration might provide a basis for friction or hot-spot.

The H2SO4 is surely concentrated, as it was the first time the bottle was opened so it could not absorb water from the air.

True, it is not safe to have undisolved material in such nitrations. But I dont understand why the NaNO3 didnt dissolve completely. It is a fine chrystaline powder. When added to H2SO4 a lot of it clumps and even when the clumps are broken by stirring it wont dissolve. I think that 85 ml of H2SO4 should be enough to completely dissolve 50 g of NaNO3 in 15-20 min.

Also after all the glycerine has been added to the mix, the mix was fuming almost as strongly as before any glycerine was added. Shouldn the fuming reduce as the formed nitric acid reacts with the glycerine?

Quote: Originally posted by quicksilver

Saline saturated water salted to the highest level of saturation possible together w/ and alkali of choice (a carbonate, etc) should produce a wash that sucks the water from the existing nitrated material; at least enough to see it as a layer. Leaving the existing nitrated product in such a wash for a 12 hour period should get you a good start.

Should the nitroglycerine/nitrating mix be poured directly into the base/NaCl solution, or first in water and then the NG be removed from the water and placed in the base/NaCl solution?

[Edited on 6-12-2009 by Zinc]

carbonfeind - 6-12-2009 at 16:18

I have never been able to get NaNO3 to dissolve completely even when using fresh sulfuric. I use a 50/50 NH4NO3/NaNO3 mixture.

quicksilver - 14-12-2009 at 15:47

I was going to wash glassware on a day off so I tried a fast experiment.
I re-crystallized several common nitrates, especially NaNO3 & KNO3. The source was stump remover and old bags of fertilizer. I was only doing it for the pictures (I take quite a few pictures of unique crystalline shapes) but was really surprised at the amount of inerts in the prilled materiel trapped in the filter paper.
Greenlight brand had certainly 20%+ clay and crap left over.
Grant's stump remover had roughly less about 15% (I wasn't going to dry out several just to be on the money to determine junk in a low grade material).
Bromide (NaNO3) had about 25% inert as well as being visually obviously filled with inferior and dirty material. Prills come from a drop tower and it's possible that the shute could be quite dirty and the last of the batch would be sold off at pennies, giving something like stump remover a huge profit margin.

Bagged prills had about 10-15% of clay and non-caking agents max. except for the ACE house brand Bromide (NaNO3) which was startling in how much materiel would just NOT go into solution in a rolling boil. In comparison I used very old bottle of NaNO3 and it disappeared in the hot water. As a very old technical grade I expected SOME insolvable material but the filter held virtually none at all.
The stump remover obviously had material that MAY have been there as just plain garbage from sweepings, etc But realistically with that level of garbage, the possibility of a poor mixed acid [from such a mix] is high.

The re-crystallized material was so clear, well-defined crystals as to be close to totally transparent. IF the project is worth doing (IMO) it's worth doing well. Too often I had guessed that prilled nitrates were lower grade than technical; but this was really too much!

Much of the H2SO4 is surplus acid and the blackened material id often too hard to determine. But at 93% (generally) heating it till white wisps of "smoke" appear will result in a very thin dark layer separated on the bottom of the heated vessel & is very easy to separate, leaving a higher grade percentage acid and a lack of "junk" that won't add anything positive to an experiment. Two hours and both solids and acid could be cleaned to nearly reagent grade. That would remove a great deal of problems that appear to have multiple origins.

Incidentally KNO3 can form very strong, thick glass-like needle crystals 3mm wide x 2cm long within a ph of slight alkalinity 7.6-8. Dropping the ph to 6.8 - 7.2 and the needles thin out to less than a millimeter & very fragile. Not only was this repeatable but no loss in weight could be recorded from either method. The thick, well formed needles were quite dense, while the thinner materiel was as thin as Nitroguanadine but dense in growth.

[Edited on 15-12-2009 by quicksilver]

Zinc - 20-12-2009 at 13:07

Today I again tried to make NG.

50 g of ammonium nitrate (contaminated with a few % magnesium nitrate) was added to 95 ml of conc. H2SO4. After adding the ammonium nitrate (I added it all at once) I put the mix into snow to cool it. After 15 min all of the NH4NO3 was dissolved. The solution was quite clear, only a little milky. When the mix cooled to 10 C I added 12.5 ml of glycerine in 10 min. The temp. rose only a little. Then I let the mixture to stand at room temperature for 1 hour. After one hour the mix is opaque and an approx. 1 mm thick clear layer formed on top of the mix. I will leave the mix to stand for some time more before pouring it in a NaHCO3/NaCl solution.

All reagents are analyical grade, except the ammonium nitrate wich was extracted from fertiliser.

[Edited on 20-12-2009 by Zinc]

hissingnoise - 20-12-2009 at 13:36

Did you swirl the mix as the glycerol was added or did you use a mixing rod?
Anyway, gentle, prolonged swirling before drowning might be a good idea.
The problem I have with NH4NO3 and NaNO3 is that they're more difficult to dry than KNO3 and once dry they start absorbing moisture almost straightaway.

[Edited on 20-12-2009 by hissingnoise]

Saftey is a good blowjob

DetaDude - 20-12-2009 at 14:08

Please, please, and this has been said before on this thread but bears repeating and take this to the bank from an old salt with the experience of many years of making NG DO NOT under any conditions stir the nitrating mix with anything but air. Buy a cheap aquarium pump and use glass tubing, an old pipet heated and bent in an "L" shape works fine.

You may get away with a stir bar or glass rod for awhile but not forever.

Please stay SAFE. NG is not the boogyman that it's reputation might lead you to believe but it is nothing to get careless with or lose respect for.

Zinc - 20-12-2009 at 14:09

Quote: Originally posted by hissingnoise

Did you swirl the mix as the glycerol was added or did you use a mixing rod?

I swirled the mix.

Quote: Originally posted by hissingnoise

The problem I have with NH4NO3 and NaNO3 is that they're more difficult to dry than KNO3 and once dry they start absorbing moisture almost straightaway.

Yes indeed they are very difficult to dry. To ensure that my NH4NO3 is dry before using it, I remove the mostly dry ammonium nitrate from the jar in wich it is stored and redry it with a hot air blower just before using it.

After the mixture was left to stand for an another hour and 10 min. the clear layer that separated on the top of the mix has considerably enlarged. Now it is around 5-6 mm thick. I will leave it stand for some more time, perhaps even more of it forms. It is chrystal clear, I belive that that is NG.

Should I pour all of the mixture in to the NaCl/NaHCO3 solution or just the NG?

[Edited on 20-12-2009 by Zinc]

hissingnoise - 20-12-2009 at 15:36

I haven't tried the nitrate method, but I'd pour as much as will go in and neutralise the residue in the beaker with a large portion of dilute NaHCO3 to recover all the ngl.
I used to use plain water as first wash, swirling, then decanting most of it before gently adding very dilute NaHCO3.
The drying wash was last!

Zinc - 20-12-2009 at 15:42

I extracted the NG from the top of the mix and poured it in the NaCl/NaHCO3 solution. I will wash it a few times and let it sit over night under the solution, tommorow I will check if it is stil acidic. If it is more washings will be done. Yield is around 10-15 ml I belive.

hissingnoise - 20-12-2009 at 16:05

There's still a possibility that what separated contains some dinitrate, so you just may end up with slightly less than you expected but even 8-9 ml would still be respectable.

Zinc - 21-12-2009 at 01:33

Well today I checked the NG. It is still acidic, but the solution under wich it sits is basic. So I dont see the point of removing the solution and adding a new portion as this one is still basic. Any ideas how to neutralize the NG?

hissingnoise - 21-12-2009 at 05:21

It's important that the ngl is neutralised quickly---when in the basic sol. it should be swirled immediately and for several minutes.
This exposes the interior of the ngl to the basic sol..
Letting it just sit without movement is very dangerous as it will start to decompose and become super sensitive.
If your ngl develops a yellowness it should be discarded straightaway, and carefully. . .

Zinc - 21-12-2009 at 06:39

So a few minutes of swirling is enough to neutralise it?

And is it better to neutralise the NG with an only NaHCO3 solution, or with a NaHCO3/NaCl solution?

I tried to set off some of the undried and partialy nutralized NG with a sparkler, but it didnt go off. The sparkler extinguished before the burning zone entered the NG (I know a stupid way to ignite dangerous materials). But a few drops when striked with a hammer detonate nicely

hissingnoise - 21-12-2009 at 06:55

The salt solution removes entrained water; washed, neutral ngl in contact with air will slowly clear without salt solution.
I'd use separate washes for safety---plain water, then neutraliser and saturated salt solution last.
How much did you get, BTW?

Zinc - 21-12-2009 at 08:55

Well I didnt mesure the whole amount but the amount I tried to detonate was 5.5 ml. Around the same amount is still in the jar so I guess I got 10-12 ml.

So after washing the NG with plain water it should be washed with a basic solution. And it should be only swirled in the basic solution for some time, not let standing under it?

User - 21-12-2009 at 09:15

Quote:

And it should be only swirled in the basic solution for some time, not let standing under it?

Could you be more specific?

The basic solution should be considered a wash to remove acid traces from the NG.
What i do is keep adding carbonate until the solution stops foaming/bubling.
Then leave it standing for a couple of hours.

hissingnoise - 21-12-2009 at 09:19

Zinc, you need to stand well clear if you're setting off 5.5 ml!
Small quantities, though, just burn with a bit of popping on ignition. . .
I've had ngl evaporate to dryness sitting in an aluminium bun-case over a burning hexamine tablet.
Ngl-soaked tissue deflagrated quietly when ignited by a Christmas-tree bulb.
Anyway, as soon as ngl is under water, NaHCO3 sol. or salt sol. swirling is pretty mandatory to continually expose fresh ngl to the action of the solution.
And as I said salt solution can be omitted if your ngl tests neutral and you're in no big rush.

Zinc - 21-12-2009 at 11:05

Quote: Originally posted by User

That is what I did, pour the NG in a basic solution, when the solution wasnt basic any more I added more of the basic solution and let the NG stand under it over night (now it has been under the solution for almost 24 h). I also swirled it quite a bit today. Now the solution is basic, but the NG is still acidic. Perhaps more swirling is in order

I will leave it again over night and check it tommorow.

[Edited on 21-12-2009 by Zinc]

User - 21-12-2009 at 11:51

Somehow NG and other esters of this kind are very good at trapping acid.
I once had the idea of adding acetone to take the NG in solution for more reaction surface with the base.
The downside is that it might get difficult to regain the product back from the solution.

Also stirring with a wooden rod or ice stick reduces friction.

Some time ago I placed the freshly made NG in a plastic container and added a stirbar and the base.
I let this stir for a couple of hours for better neutralisation.
The downside to this is that the NG is dissolved in the water which makes the yield suffer.
Another thing that i often noticed is that this material behaves very strange in water enviorment.
It somehow forms a film on the water and tiny droplets float to the surface that dont like to sink, maybe this is somekind of supension formation or that there is air trapped.
the longer it is stirred the more of this layer is formed.

[Edited on 21-12-2009 by User]

hissingnoise - 21-12-2009 at 12:39

Sometimes the droplets will sink but it's frustrating as there's always some ngl that refuses to drown.
The quantity, though, is smaller than it looks and doesn't represent any significant loss of product. . .

Picric-A - 24-12-2009 at 03:15

Add a couple of drops of washing liquid solution to the NG drops, should cause them to drop.

hissingnoise - 24-12-2009 at 04:59

Yes Picric-A, it could be a surface-tension thing---have you tried it?

User - 24-12-2009 at 08:10

Lol adding a bit of dishwash soap breaks surface tension.
Some times I got the drops down by letting a pippet suck and spit quickly just below the surface.

quicksilver - 24-12-2009 at 09:38

Quote: Originally posted by User

Somehow NG and other esters of this kind are very good at trapping acid.

This should be carved in stone in the labs of most hobbyists.

(IMO) people should stop ignoring "Plant-Level" methods of working with various materials. NG is left for at least a day or two in a completely saturated solution of anti acid and salt back when DuPont had to move his works due to a very tragic explosion. After they lost human life they learned that the solutions should be saturated and that the longer the better. The problem (like the liquor industry) is that people need the item NOW, not later. But a full 24 hours is not over-doing it. The salt and (baking soda) carbonate, etc- would be placed in a blender to totally saturate the water until not a molecule's room is left. Then the NG should be introduced (outside the blender of course) and will sink with "some" milky translucence. When it's totally clear, the water's out, but a ph should wait, lest you get a false reading from the solution. Safety takes time.

The surface tension issue has viability but I believe that a totally saturated solution may not have that issue unless there is a reasonable amount of dust or other floating particulate. Repeated success appears to balance on saturated solution of anti-acid and salt. Just an opinion.

[Edited on 24-12-2009 by quicksilver]

mfilip62 - 26-1-2010 at 10:04

I got some idea about NG that may be crazy
or great and simple...

What about toluene!?

Is it good idea to mix NG with toluene and will it dissolve NG!?
Pro is that they both don't mix with water.
NG/water emulsion will disappear instantly and you would get NG/toluene mix waiting to be evaporated.
And con is that NG is oxidizer and toluene is fuel, so I don't know will it
be dangerous to mix them!?

If so,that would be the best method to extract NG from water/acid mix.

I prepared my NG with 30g of 65%HNO3 /35g of 96% H2SO4 and 9g of glycerin.
Temperature never risen more than 30°C and I was stirring it for 30 min.Stupidly,I decided to neutralize whole acid/NG mix with baking soda...

It buns with nice bluish flame only when strongly heated with open flame,that leads me to the conclusion that it was only partially nitrated
or that acid leftover decomposed it during the night.

At least in theory,toluene wuld "crap out" ionic product(salts,acid remains...) and everything that has H-bounds(glycerine,H20...),
dissolwing only pure NG.

User - 26-1-2010 at 11:39

I also thought of this a couple of years ago.
It could be a yield improving method but there are some problems with it.
first of all .. is yield that important?
Secondly how are you planning to extract the NG from from the toluene when it is dissolved ?
And if it increases the purity by great extend it would have been used in the industry.

No i don't really think it practical but still I like the idea.

mfilip62 - 26-1-2010 at 12:16

You neutralize acids like before but then dump white NG/water emulsion in toluene and stirr a bit.
All water shuld sink.

How do you extract it from toluene.
Well,it is simple. Evaporate it at room temp. or under vacuum
of some kind!
Just don't heat it for Christ sake!

Or you can add NC directly in the toluene to make
gelignite,store it that way and evaporate it prior the use!

I recomend Celulose hexanitrate method from SamBarros page.

Will try it ASAP when I obtain chemicals.

That sounds one of the safest methods for making anything
related with NG in big batches and for long period storage.
Just make sure you neutralize it completly and suck up NOx with urea.

hissingnoise - 26-1-2010 at 12:30

Quote:

I got some idea about NG that may be crazy or great and simple...

Forget the great; it's more likely to be simply crazy!
You could end up with a very sensitive mixture.
Then you'd have to evaporate the toluene to recover the nitro.
That'd require some heat or a lot of time!
And any non-volatile toluene contaminents would remain in the nitro.
It's way too dangerous to try!
At least with the tried and tested procedure you know where you are.

nitro-genes - 26-1-2010 at 12:37

small detail...

Fully nitrated NC won't gel NG IIRC

Lambda - 26-1-2010 at 12:48

I personally find the swirling method used for very exothermic reactions close to the critical temperature, and in small liquid volumes, to be quit dangerous. Small volumes give faster temperature rise, and thus are harder to control. Unless the glycerin is added very slowly, by drop wise addition, and given plenty of time to fully react with the nitrating mixture, thus diminishing hot spot formation. Stirring one way with a mixing rod, is also a relatively inefficient way to mix fluids, unless used in the pattern of an 8. The stirring rod, is often the thermometer itself, and an accident/stupidity is lurking around the corner like tickling the tale of the devil. @DetaDude's air mixing method is my favorite, and by far the safest way to go. Multiple air outlets will also give more efficient mixing turbulences in the nitrating mixture.

Lambda

hissingnoise - 26-1-2010 at 12:51

Quote:

Fully nitrated NC won't gel NG IIRC

Are you sure, nitro-genes?
I thought it would dissolve - just more slowly. . .
And produce a stiffer gel!

Lambda - 26-1-2010 at 13:01

Highly nitrated guncotton contain ca. 13 % by weight nitrogen, while low-nitrated collodion wool contain ca. 11 % N

It's the collodion that is used for blasting gelatine. Probably the higher 13 % N will only swell, but you won't get the gelatin under normal conditions (pressure and temperature).

Lambda

User - 26-1-2010 at 16:23

Uhm @ mfilip62

You think evaporating the toluene of the ng is going to cut it without evapping a load of NG, any idea how volatile it is ?
Even at lower temps and normal pressure the NG wil probably enjoy itself at evaporating along with the toluene.
Thats why I asked u this, I'd thought you figured this yourself.

mfilip62 - 26-1-2010 at 17:04

Glycerine was added REALLY slowly in ice bath and constantly stirred,allmost no heat to be measured.

When I used to make bigger batches long ago I use altered blender with really slow stirring spead and teflon coated blade,biurete full of glycerine and all that in really cold ice bath.

I really didn't know that fully nitrated NC won't disolve in acetone!

Thanks for the tip but why is that!?

Made it just one time but found it not too much interesting.

I didn't wanted to dilute NG with toluene too much but add it just enought to separate it from water in emulsion.

That is why I aksed you abbout this!

Why is NG/acetone mix considered safe and you say that NG/toluene
mix wuld be dangerous?
They are both non-polar solvents.

My NG is in oppen bottle for weeks and allmost no reduction in volume can be observed,it is not that volatile.

Previously I stored it in acetone,evaporising aceton day or two prior the use,leaving NG with a bit of acetone behind.
It is powerfull and blasting cap sensitie explosive.

That or freezing it,both is good,but impatience will kill you,REALLY!
Everiting abbut NG must be slow,expecially final preparatio if
stored long time.

I preffer it ower AN/NG and TNT/NG dynamite becouse it is liquid!

nitro-genes - 26-1-2010 at 20:26

Who said anything about acetone? Correctly speaking, the process cannot be termed solubility anyway, hence "colloidal" or "collodion" NC, as Lambda pointed out...

Deceitful_Frank - 27-1-2010 at 00:01

I personally have never been able to (or taken the trouble to) to make NC with the ideal 11.5% nitrogen need to to set NG without the use of solvents but find the most straight forward method is to make up your nitration bath for your glycerin (or better 50:50 EG/glycerin) take your cotton wool and dip to soak with acids and set aside while you nitrate your polyols.

I think using acetone greatly speeds up gellation and saves time giving a more homogenous product. Just spread it out in a thin later on a dark coloured non stick baking sheet and leave out in the sun for an hour and the acetone will be gone. 50:50 NG EGDN is MUCH less volatile and probably safer to handle than NG and FAR less hassle and quicker to make and purify than pure NG.

Shoot for around 2.5% NC and it will just about hold its own shape but allow you to blend in some energetic dope or even 600 mesh flake Al if that tents your trousers!

[Edited on 27-1-2010 by Deceitful_Frank]

mfilip62 - 27-1-2010 at 04:48

Thanks nitro,didnt know that word in english so I didn't want to
sound like smartass!

You did not understood my question.
I didn't said you or someone else here said anything abbout acetone on this thread(doesn't matter),but I know that his mix
(NG/acetone) is widely accepted as safe method for storing NG,
why then you think it will be bad idea to stor it with toluene.
Chemically,there is no much difference between toluene and acetone
in this case,they are both oxygen pure volatile non-polar solvents,acetone being slightly less reactive.(I think...)

Why do YOU think it is bad idea to mix NG and toluene
if time needed for evap. is not crytical?
I ask you becouse I don't know and want to learn from someone who knows beter,not to make my point.

Frank,
I used EG much more than NG until cheap source of ethylen glycol
was withdra in my country becouse retarded children and old people
drank it,at least once...:
Now it can be found only in pharmacies (that "...won't sell you a poison for children!") or very diluted and contaminated in some brands of antifreez.

I never tried to nitrate glycerine and erythritol glycole in same batch,that sounds interesting,but don't really know what measures
shuld I take.Do you!?

We here have great explosive named "Vitezit" (made in neighbour Bosina,banana country with allmost no regulations at all.)
Friend of mine worked in factory,giving me a lot of precious info.
It is made of 60/40 EG/NG mix(depending on type 10-80%) and ammonuim nitrate with a bit of stabilizer FeO2 that gives him a nice red color.That is one great booster explosive that never let me down!

They allso newer mix-nitrated EG and NG,but combined it afterward.

hissingnoise - 27-1-2010 at 05:08

A colloid is a type of emulsion and collodion is a partially nitrated cotton!
They're not related in any way.
IIRC, toluene mixed with oxidisers like HNO3, TNM and NO2 forms very shock-sensitive and powerful HEs which are difficult to handle safely.
Separating nitro from water is simple, relatively safe and very effective!
Why take chances with life and limb?

mfilip62 - 27-1-2010 at 07:15

As I can remember, toluene forms nitrates only with highly concentrated HNO3 and H2SO4,and they are, under no mean unstable, most of them not even real explosives.

You think that leftower NO2 or even ONO2 groups in NG can react with toluene to form,what; MNT,DNT,TNT...all of them much less sensitive than NG,or did I overlooked something...

I don't,under any mean say I know more than you,it is interesting topic,thought...

And what about other water insoluble solvents like ether,how they may react!?

Ethers seems interesting,because they are most similar to the acetone,but don't mix with water!

And what about ethanol and methanol?!
They both mix with water and but not with NG!?
So you do it other way, put NG emulsion in some concentrated simple low alcohol like methanol/ethanol/propanol and mix it,
water from emulsion should be sucked up, leaving pure NG on the bottom. Only leftover may be some poppers that evaporate almost instantly!

Yes, it may be more expensive to use almost pure alcohol but
I don't care, just is it plausible!?

So, what are you bets;

toluene
ethers
simple alcohols
poppers

Who knows,we may found safer method for NG production?!
I found this step,the most dangerous of all.(handling emulsion)
Once it exploded in my garage, without any stimuli I know about,
obliterating table and blowing out windos!
No mices seen since then

Lambda - 27-1-2010 at 09:00

Quote: Originally posted by hissingnoise

A colloid is a type of emulsion and collodion is a partially nitrated cotton!
They're not related in any way...

Collodion is a flammable, syrupy solution of pyroxylin (low nitrated cellulose) in ether and alcohol, and with Nitroglycerin it forms a Gel when all the solvents (ether and alcohol) have been evaporated out.

Quote: Originally posted by hissingnoise

IIRC, toluene mixed with oxidisers like HNO3, TNM and NO2 forms very shock-sensitive and powerful HEs which are difficult to handle safely....

This citation is from:

Bretherick's Handbook of Reactive Chemical Hazards - Volume 1 - 6th Edition - Edited by P.G. Urben (Butterworth-Heinemann - 1999)

Page 208 (scan page 235)

Tetranitromethane

Hydrocarbons

1.Stettbacher,A., Z.Ges.Schiess.Sprengstoffw.,1930, 25,439
2.Hager,K.F., Ind.Eng.Chem.,1949, 41,2168
3.Tschinkel,J.G., Ind.Eng.Chem.,1956, 48,732
4.Stettbacher,A., Tech.Ind.Schweiz.Chem.Ztg.,1941, 24,265–271
5.Anon., Chem.Ztg.,1920, 44,497
6.Zotov,E.V. etal,.,Chem.Abs.,1980, 93,49732,49734

When mixed with hydrocarbons in approximately stoicheiometric proportions, a sensitive highly explosive mixture is produced which needs careful handling [1,2]. The use of such mixtures as rocket propellants has also been investigated [3]. Explosion of only 10g of a mixture with toluene caused 10 deaths and 20 severe injuries[4]. The mixture contained excess toluene in error[5]. Detonation characteristics of mixtures with benzene, toluene (and nitrobenzene) were studied[6].

Bretherick's Handbook of Reactive Chemical Hazards - Volume 1&2

Bretherick's Handbook of Reactive Chemical Hazards - Volume 1 - 6th Edition - Edited by P.G. Urben (Butterworth-Heinemann - 1999) 2129s.pdf (6.27 MB)
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Bretherick's Handbook of Reactive Chemical Hazards - Volume 2 - 6th Edition - Edited by P.G. Urben (Butterworth-Heinemann - 1999) 433s.pdf (1.41 MB)

as

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Password: Gonorrhea ... and I just don't seem to get rid of it, ... or maybe I should just stop visiting all those Hookers at night, ... for it's becoming exhausting !

I love Holland, and Amsterdam in the evening !

Enjoy !

Lambda

mfilip62 - 27-1-2010 at 09:21

Quote:

Explosion of only 10g of a mixture with toluene caused 10 deaths and 20 severe injuries[4].

Yeah,right!
That sounds like someting that crazy Japanese guy said abbout AP
and "DPPP".

"30 people were killed while stearing in the 1g of unobtanium meganitrate!!!"

That only has sense if detonation started fire and they all burned in building.

Your last post lacks sense,don't get what Amsterdam and you being kinky has to do with NG extraction methods!?!?

Lambda - 27-1-2010 at 09:40

Quote: Originally posted by mfilip62

Your last post lacks sense,don't get what Amsterdam and you being kinky has to do with NG extraction methods!?!?

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Enjoy Bretherick's Book, there is more Bang Bang to this Book than any other Book in this field !, and it may save your life one day !

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hissingnoise - 27-1-2010 at 09:48

So, you've finally lost your virginity Lambda?

mfilip62 - 27-1-2010 at 09:52

...or it may kill you in the very slow and paintfull manner!

Hate STD-s and dirty women!
NG on the other hand,if you don't drink it,it is relatively painless!

No really,has anyone any other idea on NG extraction/dehidration
with solvent!?

Deceitful_Frank - 27-1-2010 at 11:24

Quote: Originally posted by mfilip62

I never tried to nitrate glycerine and erythritol glycole in same batch,that sounds interesting,but don't really know what measures
shuld I take.Do you!?

What measures? Well you either mean safety measures or more likely you are asking amounts... I'll go with the latter.

I just go with an equal mass or glycerin and EG. This will be slightly more EG by volume as glycerin is more dense but the mix is just nitrated as if it was straight EG.

This makes nitration much more easy than using just glycerin. I squirt in 5ml at a time, mix with stirring rod (PTFE is good) wait for 3-4 minutes for temperature to come back to 12-13C and repeat. Towards the end you can reduces the waiting time between additions greatly. Adding the equivalent mass of glycerin to a nitration bath takes twice the time and stirring effort.

Your blasting oil has nearly identical power to NG or EGDN but is thinner so under a layer of saturated salt/NaHCO3 can be swirled and neutralized dry and clear within a few days.

The blasting oil won't be nearly as volatile and headachy as pure EGDN and with the NG it contains will be more energy dense if maybe a little less safe to handle but thats all relative.

Just don't go accidently throwing a litre bottle of it against a concrete wall!

mfilip62 - 27-1-2010 at 11:48

Nice,thanks!

I preffer my method with bledner/biurete/icebth/thermometar.
With your formula I can speed up the process and do it safer!

I will probably work with my frend that is electronic freak to make
something that adds AN to the icebath or cuts of glycerin if themp rises ower 30° and dumps mix in the cold water if ti goes ower 45°.

That will be interesting project!

I didn't understand this part;

Quote:

The blasting oil won't be nearly as volatile and headachy as pure EGDN and with the NG it contains will be more energy dense if maybe a little less safe to handle but thats all relative.

You mean a little bit less safethan pure EGDN or what!?

Deceitful_Frank - 27-1-2010 at 12:10

As far as impact sensitivity I would say safer than NG but not as safe as EGDN to handle but unless you are unlucky enough to have parkinson's AND tourettes I would not worry too much!

EDIT: Damn if you think you can let temperatures even APPROACH 30C you are gonna LOSE!

I suggest you read more!

[Edited on 27-1-2010 by Deceitful_Frank]

mfilip62 - 27-1-2010 at 14:18

That was kind of first experimental calibration.
No sinthesis done,where completed rig wasn't even finished in plans.

My synth never. goes over 20°C,it is usually arround 5-10°C
I once let intentionally small batch to go over 40 to see what will happen and what I need to care abbout.
Runnaway accours at arround 45°C,ad it is pretty nasty,but nothing
to worry abbout if you do it under 10ml and with complete safety gear,including gas-mask.

Biger batch,lower temp.
Actually I had industrila chart with temp/kilo ratio once!

I still preffer EGDN,much safer,and you allmost can't tell difference
in power.Need to find more good ol' antifreez!

[Edited on 27-1-2010 by mfilip62]

hissingnoise - 27-1-2010 at 15:39

Quote:

I once let intentionally small batch to go over 40 to see what will happen and what I need to care abbout.

Your nonchalance is going to be a real liability at some time in the future if you don't slow down and think more seriously about the inherent dangers of playing with high explosives.

mfilip62 - 27-1-2010 at 16:08

Hehehe,don't worry abbout me,I survivem more than you can imagine,99% not by my guilt!

Quite oposite!

You don't read what I write!

I left SMALL batch in SAFE enviroment to go nasty,to
see what can I expect in worst case scenario when I do it in larger batches,capish!?

I was 20m+ away observing it behing plexiglass with
high power binocular,batch contained 10ml of glycerine that was added in nitration mix withou stirring and cooling.

It gave me some pretty valuable information to predict
when the batch my go nasty!
(For example when NG/glycerine starts to act like lava lamp
it is quite critical but still menegable,and when it turns red/brown,bubbles are abbout to form,the big brown cloud and everything goes "Wuussssshhhhhh" with small det that blew glass.

That is something that reasonable and cautious person shuld do
before making bigger batches of any nitrate.
I made and detonate over 5kg of NG and EGDN,without any problem
exept mentioned incident in the garage.

it was 100% controled experiment,not something you do for fun
when you are drunk.

User - 27-1-2010 at 18:14

Still charges of 5kg EGDN/NG , sorry to say but your really out of your mind.

And yes nonchalance really fits the profile your are sketching right now.
On the other hand why not blow yourself up , as long as you don't hurt the neighbors.
If your handling chemicals is as correct as your grammar you should be just fine.

Amateur experimentalism.. right.

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