tom haggen
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Drying Nitro
Can I dry nitromethane the same way a lot of people dry nitroglycerin? Say add some sodium chloride, filter, and let it stand for a couple days till
the water evaporates.
P.S. my nitromethane kind of smells like chemical candy. Is that normal or am I fucked up in the head.
[Edited on 15-2-2004 by tom haggen]
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Mephisto
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Take anhydrous calcium chloride or sulphate for drying. Sodium chloride can be used in this case to get the rest of nitromethane from a very aqueous
solution. After simple distillation at normal pressure you'll get almost pure nitromethane.
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vulture
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Is your nitromethane pure or is it a mixture and/or emulsion?
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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tom haggen
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I think there might be some methyl alcohol emulsified with my nitro. I distilled it with an old coke bottle, a plastic tube from the fish store, and
an oil bath. I'm noticing some white goo that seems to be precipitating out, I think its plastic particles that came over with the nitromethane
and the methyl alcohol during the distillation process. I think the Nitro, and the methyl alcohol reacted with the plastic. But the plastic particles
are small and i'm going to filter them out. Anyway, I have a solution of Nitromethane, Methyl alcohol, and possibly a small amount of water. The
castrol oil is gone. Where should I go from here to get pure Nitromethane? My distillation setup is so primitave that I think it will be hard to
separate the Nitromethane and the Methyl alcohol. Could I just add a lot of water? I think I read somewhere on here that Nitromethane is not miscible
with water, and methyl alcohol is. so I could add water to separate the two. Extract the nitromethane, and then add my calcium chloride?
[Edited on 15-2-2004 by tom haggen]
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tom haggen
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Or I suppose I could just distill off the remaining methanol at like 70 degrees. Then Dry my nitromethane with calcium chloride. whats a good way to
test an make sure your nitromethane is pure?
[Edited on 15-2-2004 by tom haggen]
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The_Davster
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I've used the plastic tubing from the petshop to distill ethanol and I got fine white precipitate in my product too.
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Haggis
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That's happened to me as well. It is a degredation of the plastic, that is the best explanation I have come up with. If you do it enough, the
tubing will become opaque or white. Hopefully you did not drink this ethanol you produced, as it was contaminated with plastic products.
Another explaination is the fact that you could have had tap water bump up into your condenser, clouding the water with carbonate contamination.
Back on topic...
Great ideas often receive violent opposition from mediocre minds.
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The_Davster
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No, I did not drink it, it was just to prove to myself that I could make "moonshine"
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tom haggen
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Thats all fine and dandy but I was distilling methanol and nitromethane. Never the less I'm sure the methanol reacted with the tubing the same
way that your guy's ethanol did. My tubing even turned opaque. I filtered that crap out with ease though. Anyway Back to the topic. whats the
best way do separate my nitromethane and methonal solution? Whats a good way to test my nitromethane to make sure its pure. I have already let my
solution sit out in the open for like 24hrs so some methonal has probably already evaporated. I figure once I get pure nitromethane I will add some
dry calcium chloride to make sure there is no H20 in my nitromethane. The reason I didn't just distill off the methanol and discard it, and then
turn up the heat and distill off my nitromethane is because I used an oil bath at like 200 Celsius and it was just easier for me to do it that way.
[Edited on 16-2-2004 by tom haggen]
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The_Davster
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In my experiance, methanol will evaporate very easily. I spilled a bit on my hand and it evaporated in about 5s. Anyway, about what is the ratio of
methanol to NM? I myself would probally just leave it in a warm area in a watch glass or shallow plate and let the methanol evaporate by itself.
However, I'm not sure of any tests for nitromethane.
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vulture
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I myself would probally just leave it in a warm area in a watch glass or shallow plate and let the methanol evaporate by itself
Won't work. This would work if nitromethane wasn't miscible with methanol.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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tom haggen
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This is definitely a dilemma. I'm sure if I get off my lazy ass, I will be able to extract Nirtomethane from my Nitro, Methyl alcohol solution.
Thanks for your expert advice vulture.
[Edited on 16-2-2004 by tom haggen]
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tom haggen
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Alright screw this thread. sorry for starting it. I think i'm going to go post on an exsisting thread on this same topic over on E&W. This
problem of extraction is starting to give me a headache. Once again sorry for starting this thread. It was not worth it.
[Edited on 16-2-2004 by tom haggen]
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Tacho
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I'll will busy for the next couple of days and am in a hurry right now but here it goes:
in a test tube, mix some drops of nitrometane with some ml of 30% aquous NaOH, add some cristals of NaNO2 (sodium nitrite). Dilute to twice the volume
and add 50% aquous H2SO4 dropwise. The appearance of a blood red color that dissapear with total acidification and reappears with the addition of
alkali is a positive test for nitrometane.
From: Praticas de quimica organica-Eloisa Mano & Affonso Seabra -third edition.
This test works anyway, but I remember when I did it, it worked better if I did something like ( I cant really remember) heating a bit or waiting a
while before adding the acid. Hope is clear that it turns red after you add a bit of acid. The red seems more like brick red to me
I posted a precise description of my experience distilling nitromethane a few days ago. Read it and you will have a better Idea as to how to get rid
of methanol.
Forget extractions.
Good luck!
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tom haggen
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Ok one last post for me on this topic. this time it relates to the title. Can I dry nitromethane with silica gel or will this soak up Nitromethane
along with H2O?
P.S. Tacho I wish I had some sodium nitrite. I would make DDNP. Yo nesicito practico quimica mucho.
[Edited on 17-2-2004 by tom haggen]
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rdm3006
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NITROMETHANE WORK UP
Go to http://www.orgsyn.org/orgsyn/default.asp?formgroup=&data... for a recipe for Nitromethane from ORGANIC SYNTHESIS Collective Volume I. 401.
[Edited on 18-2-2004 by rdm3006]
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vulture
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If you had bothered to read the thread, you would have noticed that this thread is NOT about synthesizing nitromethane! 
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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tom haggen
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So if I placed some silica gel in a jar containing about 95% nitromethane, and a small layer of H2O floating on top. Will it sucessfully absorb the
H2O?
[Edited on 18-2-2004 by tom haggen]
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Polverone
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He mentioned that the workup of nitromethane is given in Organic Syntheses. In the synthesis, water needs to be removed from the nitromethane as the
last step.
"The total yield of moist product is 125–135 g.; on drying with a little calcium chloride and distilling, 115–125 g. of pure nitromethane,
boiling at 98–101°, is obtained (35–38 per cent of the theoretical amount)."
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