wafflotron
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Methanol and Nitric Acid?
I'm working out of my Chemistry teacher's fumehood after school, and unfortunately don't have much in the way of distillation equipment myself. I've
been trying to make Concentrated Nitric Acid via KNO3 and Concentrated Sulfuric Acid, and unfortunately mechanical problems are holding me back. (My
teacher only has a 2000 ml flask for his distillation apparatus) I have no desire to make NO2 and have extremely low yields (I make the H2SO4 myself),
and so have come up with an alternate solution to which I see no flaws. (Then again, I don't usually see them anyway) My new plan is to distill some
Methanol from wood since it has a lower boiling point than Nitric Acid and add it to a beaker which will contain the Potassium Bisulfate and the
Nitric Acid, decant it, and then boil/distill off the Methanol. I think this would work, but I'm really not sure. If there are any alternate methods
out there Id love to hear them, and if Methanol reacts with Nitric Acid somehow I'd love to hear that before I try it too!
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aga
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I like to type a lot of words on internet websites and use absolutely no punctuation or paragraphing which makes my posts clear and easy to read and i
have this amazing idea to make nitric acid via a totally standard route yet introduce an unrequired reagent derived from an ancient process in order
to try to add interest to my otherwise unintersting post which is generally the way that these troll posts start off and wind up dumped into detritus
or simply blow away with the wind and this is now pretty much one of the Standard methods aka M.O. by which these threads start.
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wafflotron
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Quote: Originally posted by aga  | | I like to type a lot of words on internet websites and use absolutely no punctuation or paragraphing which makes my posts clear and easy to read and i
have this amazing idea to make nitric acid via a totally standard route yet introduce an unrequired reagent derived from an ancient process in order
to try to add interest to my otherwise unintersting post which is generally the way that these troll posts start off and wind up dumped into detritus
or simply blow away with the wind and this is now pretty much one of the Standard methods aka M.O. by which these threads start.
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Sorry. I did mention I can't make the Nitric via distillation due to mechanical reasons. I did use
punctuation, believe it or not. I just wanted confirmation that this would work is all. I'm a high school chemist using OTC chems, not an internet
troll. Didn't mean to offend. This is the beginning chemistry forum, so I thought the people here would be helpful, not condescending.
[Edited on 27-2-2016 by wafflotron]
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gdflp
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This will most certainly not work, and attempting it would be quite dangerous. See OrgSyn for a description of how to synthesize methyl nitrate, it essentially entails what you are proposing here, except with substantially better cooling.
Once the methyl nitrate is formed, attempting to boil off the methanol will detonate the mixture with near certainty and, considering that methyl
nitrate is a high explosive, I wouldn't want to anywhere near that reaction. Flying glass shrapnel is remarkably dangerous and can have severe
consequences for obvious reasons. I recommend you search this site and find another method which is more suitable for you among the wealth of
information on this topic.
@aga
You're one to criticize someone for using incorrect grammar.
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wafflotron
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| Quote: Originally posted by gdflp | This will most certainly not work, and attempting it would be quite dangerous. See OrgSyn for a description of how to synthesize methyl nitrate, it essentially entails what you are proposing here, except with substantially better cooling.
Once the methyl nitrate is formed, attempting to boil off the methanol will detonate the mixture with near certainty and, considering that methyl
nitrate is a high explosive, I wouldn't want to anywhere near that reaction. Flying glass shrapnel is remarkably dangerous and can have severe
consequences for obvious reasons. I recommend you search this site and find another method which is more suitable for you among the wealth of
information on this topic.
@aga
You're one to criticize someone for using incorrect grammar.
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Thank You so much! This is exactly why I asked!! 
[Edited on 27-2-2016 by wafflotron]
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ave369
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What's so hard about distilling HNO3 from nitrate and sulfuric acid? I've done that in a goddamn retort. Retort, Carl! With no fume hood, in the same
conditions in which Johann Glauber did this. No NO2 escaped the apparatus.
Addendum: NO2-phobia is a medical condition that plagues young chemists. I'm no psychiatrist, but I think some mild herbal anxiolytics will help one
overcome it.
[Edited on 28-2-2016 by ave369]
Smells like ammonia....
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byko3y
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The best method for making methanol I know with basic equipment is electrolysis of NaOAc on graphite electrodes.
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Magpie
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I tend to agree with this. In my youth, before I knew better, the fun thing to do with nitric acid was to drop a copper penney in it. I had no fume
hood and I inhaled some N2O4 fumes. IMO the smell is not unpleasant.
The single most important condition for a successful synthesis is good mixing - Nicodem
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Texium
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Yeah, scratch the methanol idea. Regarding acquiring methanol though, distilling it from wood is a very impractical way to get it. At best, you'll get
an impure product in very low yield. If you need to get it OTC, buy HEET antifreeze (not iso-HEET, that's isopropanol), which is practically pure
methanol. It's also sold nearly pure as windshield washer fluid sometimes, but normally it's dyed.
Secondly, I don't see why having "only" a 2000 mL boiling flask is a problem. That's the size of my largest flask, and I rarely use it. When I distill
nitric acid normally, I do it on a 500 mL flask scale, and that gives me enough near azeotropic acid to keep me going for a few months, usually.
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Marvin
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For me the major problem with NO2 is not that it's toxic, and it is toxic, but that it's insidious.
I had a substantial breath of the stuff when a nitration went oxidising and it felt like nothing, the next day I had a bad lung 'infection'. At the
time I assumed the gas had weakened my lungs immune function and let a bug in. Wasn't till a lot later I discussed it with a good doctor. When lung
tissue dies quickly, your body usually assumes you have a virus and it mobilises your immune system to wipe it out, with severe exposures often in
ways that can kill you.
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PHILOU Zrealone
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1°)Wood methanol is impure.
2°)Methanol and methyl nitrate have too close boiling point for separation by distillation
3°)Methanol and not concentrated enough HNO3 will lead to runnaway exotherm because of oxydation into CH2=O (formaldehyde), formic acid and carbonic
acid...the counterpart is NO and NO2... CH2=O is uncompatible with HNO3...heating for distillation is even worst idea...
4°)Methyl nitrate is a high explosive apparented to nitroglycerine, but much more volatile and flamable...displaying related cardiovascular effect
and headaches. It is shock sensitive and displays a velocity of detonation about 20 times faster than the speed of sound (6300 m/s)...at such a speed
glass, plastic and metal are shredded into high speed schapnells.
5°)Impurities of wood methanol will favourise HNO3 decomposition and the runnaway reaction.
6°)Your teacher, school, parents ...and the police will not be happy.
[Edited on 29-2-2016 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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vmelkon
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If you don't want to distill, get yourself Ca(NO3)2.
Dissolve in water.
Add H2SO4 (not 98%, go for 30% and above.).
You get HNO3 in solution and solid CaSO4.
Then filter with filter paper.
You will have reasonably pure HNO3 solution.
Signature ==== Is this my youtube page? https://www.youtube.com/watch?v=tA5PYtul5aU
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Marvin
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Have you actually tried this vmelkon?
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Metacelsus
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In my experience, strongly acidic solutions tend to eat filter paper (even concentrated sodium bisulfate will do this). You might be able to
use settling and decantation, but I haven't tried this method.
[Edited on 3-9-2016 by Metacelsus]
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Zephyr
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I really like the simplicity of vmelkon's idea, and it looks like a great alternative for those without distillation setups..
In regards to the acid, a fritted funnel should work well.
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hissingnoise
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| Quote: | | You will have reasonably pure HNO3 solution. |
Very dilute solution! It still needs to be reconcentrated to be of real use . . . ?
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ave369
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Well, no one forces you to poke your nose inside the distillation apparatus and sniff NO2 from there. When distilling HNO3 from saltpeter, the dioxide
only accumulates inside the apparatus, it does not break out to the outside.
Smells like ammonia....
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James Ikanov
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This is a bit off topic, but somewhat relevant to something that was addressed?
I have a retort (I quite like the thing, even if I don't get much use out of it) but I'm not sure of the best way to heat it? I intended to use it to
distill off nitric acid, but finding a proper way to heat it, especially with only a hotplate has proven rather challenging for me to figure out.....
“To do good work one must eat well, be well housed, have one's fling from time to time, smoke one's pipe, and drink one's coffee in peace” -
Vincent Van Gogh
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Brom
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A heat gun should work well for heating a retort
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hissingnoise
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| Quote: | | I have a retort (I quite like the thing, even if I don't get much use out of it) but I'm not sure of the best way to heat it? I intended to use it to
distill off nitric acid |
Retorts are only suitable for distilling small quantities!
The sidearm gets warm just too quickly for any sustained distillation . . .
http://www.sciencemadness.org/talk/viewthread.php?tid=25209&...
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XeonTheMGPony
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Filtering Acids use clean fibre glass, pull off a small amount flatten on a plastic screen then filter, don!
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hissingnoise
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A lot of the fibreglass I see is polymer-sized which makes it worse than useless . . .
A fritted-glass filter, though, is a real boon ─ well, except when it needs cleaning?
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