Booze
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White Fuming Nitric Acid
Hello. I got interested in WFNA, as it has very little info on wikipedia. My current guess on its prep is a nitric acid synthesis without water, and
maybe bubbled with air afterward? Or added a little bit of urea? Can someone clarify a little bit? Thanks
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j_sum1
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There are YT vids on the synthesis. Not dissimilar from making azeotropic NA. Simply distil from sulfuric acid and a dry nitrate.
Red fuming nitric acid occurs is you get any evolution of nitrogen oxides. Then you need to redistil.
But really, why? 68% is suitable for nearly everything. And WFNA is painful to store.
Make in small volumes as you need it.
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Booze
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Quote: Originally posted by j_sum1  | There are YT vids on the synthesis. Not dissimilar from making azeotropic NA. Simply distil from sulfuric acid and a dry nitrate.
Red fuming nitric acid occurs is you get any evolution of nitrogen oxides. Then you need to redistil.
But really, why? 68% is suitable for nearly everything. And WFNA is painful to store.
Make in small volumes as you need it. |
I wasn't going to make much, or keep it for very long.
Possible RDX synth.
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Melgar
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Before I could get 68% nitric acid OTC, my nitric acid was always WFNA, because I had to make it myself. It's actually not that bad, in my opinion.
I just stored it in a dark brown polyethylene bottle and never had a problem. Basically, if you vacuum-distill sulfuric acid and 68% nitric acid, or
sulfuric acid and a nitrate salt, you get WFNA. If you distill it without a vacuum, it's less white and more red. Of course, the vapors will destroy
just about anything that you'd use to pull a vacuum except an aspirator, so keep that in mind.
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Praxichys
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I usually distilled KNO3 and H2SO4 without a vacuum to get RFNA and then used a fishtank air pump to blow dry air through it to kick out the
NOx until water clear.
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Booze
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| Quote: Originally posted by Praxichys | | I usually distilled KNO3 and H2SO4 without a vacuum to get RFNA and then used a fishtank air pump to blow dry air through it to kick out the
NOx until water clear. |
I have a pump, but really don't want to risk destroying it. I will do that.
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ave369
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I've made WFNA successfully using battery acid boiled down to 90%, fertilizer grade potassium nitrate and a retort. Density measurements showed the
concentration to be 95%. The trick is not to overheat the distilling flask, or you'll get RFNA instead.
Smells like ammonia....
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CuReUS
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While we are on the topic of W/RFNA,could someone answer these questions please -http://www.sciencemadness.org/talk/viewthread.php?tid=71219#...
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akmetal
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| Quote: Originally posted by Booze | | Quote: Originally posted by j_sum1 | There are YT vids on the synthesis. Not dissimilar from making azeotropic NA. Simply distil from sulfuric acid and a dry nitrate.
Red fuming nitric acid occurs is you get any evolution of nitrogen oxides. Then you need to redistil.
But really, why? 68% is suitable for nearly everything. And WFNA is painful to store.
Make in small volumes as you need it. |
I wasn't going to make much, or keep it for very long.
Possible RDX synth. |
Very easy to just get an ATF permit, and if you use it the same day you dont have to have a magazine, even if you have to build a magazine its not
that big of a deal unless you live in a highly urban area.
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thermochromic
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| Quote: Originally posted by akmetal | | Quote: Originally posted by Booze | | Quote: Originally posted by j_sum1 | There are YT vids on the synthesis. Not dissimilar from making azeotropic NA. Simply distil from sulfuric acid and a dry nitrate.
Red fuming nitric acid occurs is you get any evolution of nitrogen oxides. Then you need to redistil.
But really, why? 68% is suitable for nearly everything. And WFNA is painful to store.
Make in small volumes as you need it. |
I wasn't going to make much, or keep it for very long.
Possible RDX synth. |
Very easy to just get an ATF permit, and if you use it the same day you dont have to have a magazine, even if you have to build a magazine its not
that big of a deal unless you live in a highly urban area. |
Someone can correct me if I am wrong but I am pretty sure you do not need any permit from the AFT to simply synth rdx or other energetic (minus a few
outlawed by name like TATP). Permitting is required for transportation, storage, or if you are making a destructive device. Is far is the “ if you
use it on the same day” statement, I think you are thinking of ffl 07/SOT requirements for serializing and logging destructive devices. Perhaps
there is a similar requirement for record keeping of explosives but like I said, if you are making some, not transporting, and using experimentally
the same day on your own property, no licensing is needed, federally at least
[Edited on 24-12-2023 by thermochromic]
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Rainwater
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In the US, federal level, your correct.
But every state has different restrictions, and every county, more restrictions.
There is not a one size fits all answer here.
Best to ask your local authorities.
Most will be understanding, some will think your a nut job.
Mine wanted to see me workspace and lab logs.
Since moving into a more populated area, i was granted permission for quantities less than 0.1g.
and local noise/firework restrictions apply.
[Edited on 24-12-2023 by Rainwater]
"You can't do that" - challenge accepted
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ManyInterests
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I'm going to bump this up, because while I have made very high concentration WFNA (and yes, it is for RDX synthesis as mentioned by Booze, as it is
the only thing that really needs WFNA. PETN and others can be made with 68% + sulfuric acid). But while I did sometimes succeed in making them with
distilling a dried nitrated salt and sulfuric acid, it is often very hit and miss, and even blowing air through it sometimes adds moisture even when I
tried my best to dry the air with dry calcium chloride.
So I just want to say that going forward I plan on making nitric acid with sodium or potassium nitrate and sodium bisulfate, and then I would
redistill that nitric acid with sulfuric acid in order to further concentrate it. Since adding sulfuric acid to nitric acid will purge it of all NO2,
I won't be blowing air or adding urea/hydrogen peroxide to the acid beforehand.
My question is making sure I reclaim the sulfuric acid afterward for reuse. Would adding hydrogen peroxide to the sulfuric acid after the 2nd
distillation and boiling it again bring it back to the pure 95-98%? I think it would be, but I just want to make sure.
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Fery
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ManyInterests - it should work. Here somebody used (NH4)2S2O8. Very likely Na2S2O8 and K2S2O8 could be used too. Using H2O2 avoids adding Na/K/NH4
salts so you should be able to recover pure H2SO4 after boiling out water.
https://www.sciencemadness.org/whisper/viewthread.php?tid=13...
[Edited on 2-12-2024 by Fery]
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ManyInterests
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There is also another thing I would like to know in terms of reusing sulfuric acid after certain projects. For example, making glacial acetic acid. I
made some a long time ago (it is probably around 95% and not 100%... and it's been so long I probably need to redistill it anyway) I know that
sulfuric acid is a good drying agent, but once all the acetic acid is distilled over all I got left is the sulfuric acid. I am wondering if also
cleaning the sulfuric acid with H2O2 and reboiling will also render my H2SO4 pure again.
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Sulaiman
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Boiling concentrated sulphuric acid is oxidising enough without H2O2,
If you have something to serve as an air condenser then distillation is a good (but scary) option.
Collect distilled dilute acid first,
when near azeotropic you can collect the acid from the boiling pot,
or continue with distillation to get distilled azeotropic acid.
CAUTION : Hobby Chemist, not Professional or even Amateur
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