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Topic: Concentrated nitric acid  (Read 2482 times)

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Offline hexanite

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Concentrated nitric acid
« on: September 09, 2014, 07:00:22 PM »
Hi, I'm trying to make concentrated nitric and was wondering what the best way to accomplish this would be.  Here is what I did the first time:
1.  Obtained ~30% concentrated sulfuric acid
2.  Boiled the water out of the solution.  I have not yet tested the concentration of this acid, but I'm assuming it's 95%+
3.  Mixed 200g KNO3 with 106mL of the acid in a flask, connected to a graham condenser.  I have a liebig one too, but it didn't seem to cool off the fumes fast enough for it to condense because there was a lot of nitric acid fumes escaping from it.
4.  Distilled
The acid came out very colored and according to http://www.chemicalforums.com/index.php?topic=9198.0, it is very impure. They suggested using a 60% concentration of sulfuric acid to make a less concentrated solution of nitric acid, but I was wondering how I could then concentrate the nitric acid.  I read that I could use sulfuric acid as a dehydrating acid, but I don't really understand how this works and was wondering if someone could explain.

Offline Zyklonb

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Re: Concentrated nitric acid
« Reply #1 on: September 12, 2014, 02:29:10 PM »
Quote
1.  Obtained ~30% concentrated sulfuric acid
2.  Boiled the water out of the solution.  I have not yet tested the concentration of this acid, but I'm assuming it's 95%+
Don't assume. Know. Did you boil it until dense white fumes where coming off? They start at around 85-90% so if not, you don't have very concentrated acid.
200 grams of potassium nitrate is nearly two moles. 106 mL of 98% sulfuric acid is 193 grams, or 1.98 moles. So, you did the calculations correctly if you assume that the potassium bisulfate also produces a mole of nitric acid. However, this only happens at much higher temperatures, so likely your yields were cut in half.   

Offline Zyklonb

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Re: Concentrated nitric acid
« Reply #2 on: September 18, 2014, 11:44:56 AM »
Due to lack of time, I was unable to finish, now the edit function is unavailable, so I will continue here.
Sulfuric acid ionizes like this: H2SO4 +H2:requil: H3O+ + HSO4. The resulting bisulfate ion ionized again - but to a much smaller extent: HSO4 + H2:lequil: H3O+ + SO4.
Thus, with a nitrate salt: H2SO4(aq) + XNO3(s/aq) → HNO3(g) + XHSO4(s/aq).
With considerable heating, the volatility of nitric acid over X-bisulfate causes the reaction to go further to completion. Heating to this temperature cause much decomposition to the nitric acid: 2 HNO3 → H2O + 2 NO2 1/2 O2. This reaction is mostly irreversible. Some of the NO2 might dissolve in the nitric acid, but it won't be oxidized to the +5 oxidation state. This acid is called RFNA or red fuming nitric acid. You can oxidize the dissolved NO2 (or at lower temperatures, more correctly called N2O4) by adding concentrated hydrogen peroxide to the solution, or bubbling dry air or oxygen through it. When nitric acid is free of N2O4, it will become colorless, an excellent indicator.

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