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Author: Subject: nitroglycerin
andrea
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[*] posted on 21-9-2003 at 03:17
nitroglycerin


Hi guys, I'm gonna make some nitroglycerin for the first time. I've got only 65-70% concentrated HNO3 and 96-98% concentrated H2SO4. In the megalomania's procedure they use 98% HNO3 and 98% H2SO4 in a 2:3 ratio. I wanna know if using a nitrating mixture with a different ratio of HNO3/H2SO4 I will be able to get successfully some NG. If yes what ratio of HNO3/H2SO4 should I use (with 65-70% HNO3)? Thanks for your answers
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[*] posted on 21-9-2003 at 04:28


How much do you consider some? You can get a little, but if your just doing it on guessing, I would recommend planning it out first or just synthesize something else... because if you mess up that synthesis....
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andrea
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[*] posted on 21-9-2003 at 05:39


I don't wanna do too much NG. For the first time 2 or 3 ml are enough. I'm not gonna make it without a precise plan. Indeed the only thing I've to know is (if it's possible) the HNO3/H2SO4 ratio if my HNO3 is 65-70% concentrated (and, of course, the related amount of glycerol I should use)
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[*] posted on 21-9-2003 at 08:52


use 30ml of HNO3 (65%) and 45 ml of H2SO4 for every 10ml of glycerine

and make it at least of those 10ml glycerine - the risk would not be considerably higher
2 to 3ml NG is nothing ;)
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andrea
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[*] posted on 21-9-2003 at 11:14


Thank you for the advice. But I considered it and your ratio is the same of Megalomania's. In fact 200:300 = 30:45;
the only difference is that megalomania's method uses 98-100% pure nitric acid while you use 65% NA. Are you sure it's the same thing? I thought the HNO3/H2SO4 ratio should change when acid concentration changes...
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palpy
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[*] posted on 21-9-2003 at 13:46


haven't done it myself, but a guy i know synthesized NG succesfully with this ratio.
the hint is intensive cooling and adding the glycerine DROP BY DROP
the yield should be about the volume of glycerine you started with (i'dont have the specific masses here at the moment, but i'm sure you can handle this :)
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[*] posted on 21-9-2003 at 18:46


Not related to the Nitric Acid... but just some common safety tips. 10 ml of Nitroglycerin can kill you, so be careful. Neutralizing the Nitroglycerin is extremely important- as I'm sure you know already from reading Megalomania's synth. Nevertheless, I still feel it necessary to hammer the point in :).

If the synth goes wrong and the reaction overheats, chances are it won't explode- you'll just get some nasty NO2 fumes. And finally, be patient with the Glycerin! Adding drop by drop does get boring, and can take a while. But for the sake of your safety, don't rush.
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[*] posted on 21-9-2003 at 21:37


I thought that NG would work fine with around 68% nitric acid. It works okay with mixed acids although the yields aren't spectacular(around 22g using 1.5 times the amount of acid stoichiometrically necessary for 40g and the stoich amount of glycerin for 40g). If your acid doesn't work just try mixed acids.
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[*] posted on 22-9-2003 at 02:50


Using the ratios given by palpy may give an undesirably high concentration of glycerol dinitrate in your product which will look like NG and explode if whacked with a hammer, but is quite inferior to pure NG.
For this reason, I recommend these ratios: 1 mL glycerine to 4 mL 62 % HNO3 and 6 mL 96 % H2SO4.
This corresponds to directions given by one of the old timers on the EW forum who was working in a lab that would sometimes need a little NG for unspecified testing.
They used 1 mL glycerine to 4 g NH4NO3 and 6 mL H2SO4 ( but this mix tends to freeze when cooled to around 0 C ).
Anyway, a good process for neutralizing NG is to add the crude product to about ten times its volume of bicarb soln and let it sit for a day with occasional swirling.
After this period, the NG will have absorbed considerable amounts of water and will appear milky. This is fixed by adding it to a saturated soln of NaCl in water and swirling it occasionally until clear.
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[*] posted on 24-9-2003 at 00:59


Do this synth in a well ventilated place or outside. This will reduce drastically your first-timer headaches. And by the way, you can do it with much smaller amount of H2SO4 if you have lots of time to wait the reaction to complete. If I remember right in nitration processes the sulfuric is always used only to start the reaction and tho catalyze it. So the amount is only a matter of time.
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[*] posted on 24-9-2003 at 04:34


The amount of H2SO4 should not be decreased. In nitration reactions of this kind, the sulfuric acid serves to dehydrate the nitric acid ( and to scavenge the water that is produced in the esterification of the glycerine ), thus effective ly increase the concentration of the nitric acid. As you know, HNO3 in high conc. is a nitrating agent, while low conc HNO3 is mainly an oxidizer.
So, using too little H2SO4 will lead to more oxidition and, at best, an inferior product or, at worst, a runaway with NOx plume, acid splatter, etc.
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[*] posted on 26-9-2003 at 11:35


Hi! Today I've made 3ml of nitroglycerin (or what I think it was) using Microtek's directions (1ml of glycerol in 4ml 65%HNO3 and 6ml 96%H2SO4). After adding all the glycerin I allowed the mixture to sit for 15 minutes monitoring the temperature at all times. I washed it as explained in Megalomania's method and I obtained a clear oily liquid. I drained off the water but didn't dry my NG, only drained off all the water I was able to drain off (I thought that the NG collected on the bottom of the cilinder was water free, specially after having washed it with a concentrated sodium chloride solution). So I tested it.
At first I put a drop of NG on a flame; it didn't burn unless I kept it on the flame: indeed while I was keeping it on my "Bunsen" a blue flame formed but only for fractions of a second. "Perhaps it is too a little amount of NG" I thought.
Then I let a drop of NG fall on the ground from a height of 5 feet: nothing happened.
At the end, raped by desperation, I tried to hammer it six or seven times: it detonated only twice. I worked always with a drop of NG: is this the matter? What should happen if a drop falls on the ground? Should it detonate? And what should be the behaviour of NG on the flame? Had my NG a normal behaviour? If not, why?
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[*] posted on 26-9-2003 at 12:58


Nitro should NEVER explode when a drop falls all of 5 feet. Also, here is a nice page with NG burn tests. http://www.geocities.com/brainfevert/tests.html



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Microtek
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[*] posted on 28-9-2003 at 07:56


When doing the hammer test, the NG must be absorbed into a piece of toilet paper. Otherwise, the hammerblow will more likely just scatter the NG as little droplets.
Generally, people who have experience with organic peroxides are surprised at how relatively difficult it is to make NG explode.
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[*] posted on 28-9-2003 at 12:19


Andrea, you mention you "washed" your NG with sodiumchloride, but it's not clear if you neutralized your NG, which is EXTREMELY important.



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andrea
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[*] posted on 1-10-2003 at 11:27


Of course I did it. I think I've found NG particularly difficult to set off perhaps because I was used to work with acetone peroxide (the first and last explosive I've ever made) which was much more sensitive (and dangerous I think...)
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[*] posted on 2-10-2003 at 11:21


I am planning to make NG too however i have to make it with NH4NO3 and sulfuric acid because is extremly hard to find nitric acid here. I was looking for some webpages that show step by step about the nitration of glicerine, i dun wanna start with a runaway nitration!
Beside that, i will try to nitrate sugar, mannitol, and glucose too, but like before, i don't have a good web guide to help about that..

I will start tonite, i hope i won't drown in deep brown fumes!

[Edited on 2/10/2003 by Nevermore]




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andrea
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[*] posted on 3-10-2003 at 11:09


Where do you come from? {Da dove vieni? (se preferisci l'italiano...) Forse ti potrei dare qualche informazione su dove trovare l'acido nitrico} Perhaps I may help you to find some nitric acid!
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[*] posted on 5-10-2003 at 03:19


dal sud, isole.
credo che mi arrangero' con il nitrato di ammonio e l'acido solforico..cmq se sai qualcosa...

im coming from the south, islands.
i think i will just go on with AN and sulfuric acid...




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[*] posted on 5-10-2003 at 16:14
NG and diatomaceous earth


Hi,
I found a source to obtain diatomaceous earth from. REalising that it has been used as the first dynamites ever, when soaked with NG, I wondered whether anyone has experience with it. Diatomaceous earth is a zeolithe, a SiO2 based substance with an extraordinarily high surface area, thus it is extremely capable of absorbing virtually any material, in this case NG. Also, I read that it sweats NG after a number of months (hence it is not used anymore these days), but for immediate use it is apparently totally safe to use.
Anyway, did anyone have some experience with it?
Cheers
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[*] posted on 9-10-2003 at 13:14


I need some info about which temp to perform the synth, i planned to use a small becker inside a large ice bath, but the freezing point of the NG scares me, it is just 13C so most probably i will end up below that temp. Is that safe to nitrate glycerine at that temp or should i care not to go lower than 15°C (that will be much harder)? Also should i avoid to mix with a glass rod, or use a wood one, or just swirl around? i will be using 58% HNO3 since i can't access higher conc one..



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[*] posted on 13-10-2003 at 02:38


I think I can help out a bit here.On BS theres a thread dedicated to this and I know how some of you feel about it but theres a lot of experiance with it at this link.

Also h2so4 and nh4no3 seems to give better yields and were looking into using nitrogen dioxide.
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[*] posted on 13-10-2003 at 06:25


uhm my opinion is that HNO3 gives better yelds for sure than NH4NO3..
Anyway, is worth a trial.




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[*] posted on 14-10-2003 at 04:37


I have a rough theory since sodium nitrate is better than potasium(it was tried out along time ago-bad ideas).I think that metal's interfere with the reaction.That would explain NaNo3 working better than KNo3 and nh4no3 woeking better than both.Though it could be a side effect of the the heat.THis line of thinking sugest like you sai than Hno3 would wok the best.But I really dont know much about chemistry.
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thumbup.gif posted on 14-10-2003 at 06:27


By the way, if anyone is interested in how to get the precursor glycerine, it goes (supposedly) like this:
(sunflower) oil+Ca(OH2)=>
=>glycerine+calcium soap
(water- insoluble, so I suppose
glycerine-insoluble as well).:cool:
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