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497
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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..
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hissingnoise
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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. . .
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Bikemaster
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problem with my nitroglyrcerine
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
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hissingnoise
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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???
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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]
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Bikemaster
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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???
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hissingnoise
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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!
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Bikemaster
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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
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hissingnoise
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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]
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Bikemaster
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I was also worry about the stiring method... Maybe it could be better using some compressed air to stir the mix.
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densest
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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.
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hissingnoise
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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]
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Microtek
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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.
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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.
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hissingnoise
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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.
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Bikemaster
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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.
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hissingnoise
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| 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...
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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?
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Bikemaster
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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???
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hissingnoise
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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!
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Bikemaster
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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]
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User
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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]
What a fine day for chemistry this is.
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hissingnoise
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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.
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Microtek
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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).
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Zinc
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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.
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hissingnoise
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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!
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quicksilver
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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]
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Zinc
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| 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!
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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.
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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.
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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]
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