Duster
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So Im setting up a distilling setup
Finally anyway. Decided to make it all 24/40 and my primary distilate will be HNO3 (of course) for now. I know the price will probably even out a
little under $300 for everything... Thats alright though I plan to put it together over a couple months.
I got a couple parts but the next thing I want to get is a reflux colum. Im thinking a Vigreux, 300mm... Would this be too much for nitric? I was
always under the impression that more was better but I read somewhere that for certain substances a shorter colum is best. I wanted to make sure
nitric isnt one of those.
Next is the actual condenser. I so very much wanted a grahm but it only recently occured to me it has to be vertical to be properly used. While its
easy enough to go verticle I dont think I would have enough clearance between a 2000ml RBF and a 1000ml RBF to use one. If I could I would, but I dont
think I can, so I think I will go with a 400mm Liebig. How does that sound?
Of course this will be a vacuum setup with (im thinking) a nice little homemade heating mantle... If not, then a bunsen burner.
I think thats about all the questions I have, though im always looking for more tips so if you have an idea let me know.
Also, I did a search on this and found a really nice thread on condensers in general but I also wanted to know, what sort of yields do you get? Reason
why I want to know, if I get a 2000ml boiling flask, what size should the other flask be? Is 500 not enough, or is 1000 just right? Just curious, and
looking to save money!
Lastly, how many types of nitric are there? I knwo theres white, and fuming, and I think I say another type.. Whats the diffrence between all this?
Thank you!
Duster
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neutrino
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I am tempted to just answer your questions, but, in the spirit of the forum, I will instead tell you to search. These topics have been discussed ad
nauseam on this forum and especially over at RS (they have an entire section on this chemical, for crying out loud!)
To clear up a bit of confusion, a Vigreux column is only used in a fractional distillation. Simply distilling nitric acid from sulfuric acid and a
nitrate only yields one product, so fractionation is not necessary.
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Duster
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Thats part of why I asked, because it HAS been discussed so much some of it intersects with itself. For example, I read that by having a reflux colum
you get a more pure product. Alas this is not the case, however I was also pointed that it could be depending on your products. For example, using
drain cleaner. You dont know what sort of nasty stuff is mixed in there and you dont know their boiling points, thus a reflux colum helps insure you
get a more pure product.
I have no problem with this being locked or deleted, I just wanted to see, basically, if I was flat out screwing myself over or not. I think I'll
be fine but if im throwing in this kind of money I figured a post would be in order to make sure im not running in circles.
Duster
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neutrino
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It would probably be easier just to boil your acid for a while and thus get rid of the volatile impurities before they can contaminate your product.
Adding a nitrate to boiled acid shouldn’t produce anything volatile but nitric acid.
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MadHatter
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Price
Duster, $300 seems like a lot of cash for a distilling rig. Search this forum and checkout
BrainFever's method. If your needs for nitric acid are low, this may be the ticket. BrainFever
produced white nitric acid using the simplest of apparatus.
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
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Mumbles
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If you wait around, you could easily get everything you need off of ebay for less than $100. Since you said you were going to be vacuum distilling I
might recomend united glass tech. They are very nice to deal with, and have some very high quality glassware from my experience.
The only things left from my original distillation apparatus are my two UGT adapters and a 1L Ace glass flask.
www.unitedglasstech.com
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vulture
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Most confusion about distillation is caused by the fact that people make wrong assumptions and/or don't have the basic theoretical knowledge.
Before proceeding on any distillation you should educate yourself on the laws of Raoult-Henry, azeotropes, vapor pressure and the effects thereof on
separation.
If you would have done so, you'd know that a vigreux column is actually going to detoriorate your nitric acid, whilst it will be beneficial for
distilling alcohol. Why this is the case I'll leave for you to find out.
As said before, this has been discussed ad nauseam.
Closed.
[Edited on 26-4-2005 by vulture]
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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