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Author: Subject: nitroglycerin
Totenkov
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[*] posted on 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.



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Boomer
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[*] posted on 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).
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pdb
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[*] posted on 23-4-2008 at 04:36


Boomer, check your U2U please.
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Pulverulescent
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[*] posted on 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
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gregxy
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[*] posted on 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.
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[*] posted on 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
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[*] posted on 5-5-2008 at 04:55
Drain openers?


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?
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[*] posted on 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.




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texaspete
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[*] posted on 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.
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[*] posted on 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]




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[*] posted on 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)




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[*] posted on 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



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[*] posted on 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!

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[*] posted on 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]




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The_Davster
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[*] posted on 1-6-2009 at 17:12


Wet NG is white. Dry NG is colorless.



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[*] posted on 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.




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[*] posted on 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...
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[*] posted on 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]
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[*] posted on 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.




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[*] posted on 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?
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[*] posted on 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??.





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[*] posted on 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!
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[*] posted on 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. . .
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[*] posted on 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!
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[*] posted on 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.
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