Chemguy Posted November 13, 2006 Posted November 13, 2006 Ok to clear things off to start with I am NOT asking how to make it, I allready know that, but I don't know how you make . I haven't really tried to make pure HNO3 as I don't have the equipment, yet. So I make NO2 from KNO3 and NaHSO4 and lead it into warm water which gives a dilute solution, the other way I know is KNO3 with HCl, but that makes KCl and HOCl aswell, but it is quite concentrated, that is it reacts violently with copper. So how do you make it, or buy it?
h0lx Posted November 13, 2006 Posted November 13, 2006 I used to distill boiled down battery acid with KNO3 with my ghetto "still" which hade a condensed made of aquarium tubing, a plastic box and silicon sealant. Now I have a source for 58%.
XenoN Posted February 4, 2007 Posted February 4, 2007 Would the nitric acid simply dissolve your rubber tubing and silicone? I have a glass still it works great for solvents and such, but is way to small for nitric acid. I was to make a still out of 4 foot 12mm glass tubing (maybe its 20 mm I forget) And a 1 inch acrylic tube as a water jacket. Silicone tube as a water in and out. The only problem what should i use to seal the still up? Epoxy is attacked by nitric acid and so is silicone. Also I want to use dry ice and ethanol, methanol, or acetone as my coolant. I want this still to be very efficient when making nitric acid. I'm just not sure if these solvents will destroy my tubing. Any ideas.
hashashan Posted February 4, 2007 Posted February 4, 2007 hot HNO3 fumes will attack practically everything. I used once a glass still with one Teflon part and it dissolved it (very weired though .. the guys in the chem shop said that it holds almost any acid). anyway you can use glass and most of the polyethylenes and I don't know about any other stuff you can use.and about your tubings, the rubber ones will just catch fire.
Mumbles Posted February 5, 2007 Posted February 5, 2007 Chances are if the nitric dissolved the teflon, it had something not teflon in it. I've never had an issue with nitric attacking teflon ever. The only things off hand I know that will contain high conc nitric acid are Glass, teflon, and Aluminum.
Frozentech Posted February 5, 2007 Posted February 5, 2007 hot HNO3 fumes will attack practically everything. I used once a glass still with one Teflon part and it dissolved it (very weired though .. the guys in the chem shop said that it holds almost any acid). anyway you can use glass and most of the polyethylenes and I don't know about any other stuff you can use.and about your tubings, the rubber ones will just catch fire. http://www.vp-scientific.com/Chemical_Resistance_Chart.htm PTFE (Teflon) is good against anything you can throw at it, except Flourine gas in high concentrations. The first industrial use was enriching Uranium for the Manhattan Project ( I didn't know that before... so it *wasn't* spin-off of the space program LOL) because it could resist UF6.
hashashan Posted February 5, 2007 Posted February 5, 2007 thats what i thought also. but i bought it in a chem shop, and that was a surprise to me when fuming nitric started dripping on my table ... not a very fun thing . i got into a gas mask and started cleaning the room.
Boomer Posted February 5, 2007 Posted February 5, 2007 My nitric still is a glas liebig conected to a 1 liter RBF with a bent Al tube. The two joints are simply wrapped with alu foil followed by duct tape. Extremely ghetto but works, after some ten distillations you have to replace the foil/tape though. BTW tap water is enough for cooling, dry ice is a waste. And don't worry, you *will* notice when it leaks, so mount it in the bath tub.
XenoN Posted February 6, 2007 Posted February 6, 2007 My glass still just doesn't have a long enough condenser on it. The plastic pieces that keep the joints from separating where destroyed last time i tried nitric acid. I mixed ammonium nitrate and sulphuric acid together and got massive amounts of white vapor but nothing condensed. I figured it was because the vapors didn't have time to condense and i have a few 4 foot pieces of glass tube left over from my carbon dioxide laser.
h0lx Posted February 7, 2007 Posted February 7, 2007 Yes it attacked my still, the rubber stopper was useless after 2 batches and the silicone got nitrated(turned yellow) but the silicon, didn't degrade at all.
Boomer Posted February 7, 2007 Posted February 7, 2007 ??? If it works for solvents, it should work for nitric too. Many solvents condens lower than nitric. I even wrap foil around the upper part, or too much condenses in the neck and claisen and runs back down before reaching the condenser! Also I never see white vapour clouds, only on mixing. Once the burner is adjusted right (1-2 drops per second coming over), the headroom in the distilling flask looks clear. Maybe you did not heat it enough? It needs lots of heat to come all over, the flask will go above 100C! And don't worry about the orange plume that comes first, just discard the first 5ml. It will get nearly colourless after some minutes.
Mumbles Posted February 7, 2007 Posted February 7, 2007 From the description, it almost doesn't sound like Xenon heated it at all. I've personally never had much luck with distilling nitric myself, but I've only tried a few times and have a poor heating aparatus.
hashashan Posted February 7, 2007 Posted February 7, 2007 what kind if a condenser you guys use?i had a lot of problems with my spiral condenser. anyone managed to distill HNO3 with a spiral?
Mumbles Posted February 7, 2007 Posted February 7, 2007 I have a 400mm Liebig condenser. I need to start covering the neck of the flask and the 3-way adapter with foil, as I get a lot of nitric condensing there and dripping back in..
XenoN Posted February 7, 2007 Posted February 7, 2007 I heated mine slightly with a hot plate. I added a tube to vent un-condensed vapors. The vapors melted the tube before i was even able to completely heat. I was forced to evacuate because my lab completely filled with vapors. Also i was told to use very little heat or else you will decompose the acid vapor to NOx. This is my exact still: http://unitedglasstech.com/distillingKIT5.htm One last thing are there any sealants made from teflon? If not are there any ways to obtain teflon so maybe i could dissolve it in a solvent like MEK and make my own sealant?
hashashan Posted February 7, 2007 Posted February 7, 2007 i had most of the nitric stuck in my spiral. I'm thinking to buy a Leibig.btw XenoN whats the column for?
XenoN Posted February 7, 2007 Posted February 7, 2007 It uses the air as a coolant to condense a lot of the vapor or get it very close to its condesation point. It slows down the still but increases its efficiency. Well i guess ill go pick up some H2SO4 tomorrow and try it again with a bunson burner. Plus its been around -15*C around here latley and i keep my methanol water coolant outside i think it should work pretty well this time. In order to raise the percent of nitric to around 100% i was thinking distill it twice but the second time add additional H2SO4 as a dehydrator.
ewest Posted February 8, 2007 Posted February 8, 2007 One last thing are there any sealants made from teflon? If not are there any ways to obtain teflon so maybe i could dissolve it in a solvent like MEK and make my own sealant? Would Teflon tape work?  It's found in the plumbing section of the hardware store and is used as a sealant for threaded pipe. It comes in a small roll like tape. For threaded pipe, you wrap it around the threads of your pipe in a clockwise motion then screw the pipe into the threaded fitting and the Teflon will fill any gaps and seal the pipe. Maybe it'll work the same in your application? Don't know.
Boomer Posted February 8, 2007 Posted February 8, 2007 If you could dissolve PTFE to make a paint it would not be that resistant would it? And take that vigreux out or the nitric will be 95% refluxing, 5% coming over (if you have a shorter 3-way). Or at least wrap it in several alu foil layers with air between. BTW the kit is overpriced, but LOTS better than my setup. And even that makes RDX-grade nitric with ghetto parts.
weknowpyro Posted March 6, 2007 Posted March 6, 2007 This is a picture of the process I use to make hydrogen nitrate.Should give thanks to Brainfever, as i use the way he decribe's on his website.HNO3 droplets are visble on top of the film.
weknowpyro Posted March 6, 2007 Posted March 6, 2007 Another picture of the cling film. As you can see, alot of HNO3 has condensed on the film and has now made a large droplet in the middle.
treelover Posted March 22, 2007 Posted March 22, 2007 I´m surprised no one mentioned DCM extraction. In the early days I used to get my nitric from AN and SA (drain cleaner stuff, 98%) by distillation with an RBF and liebig in an oil-bath. I found AN to be the best xNO3 for distilling NA since it produces by far the least NOx while distilling without vacuum.  Some time ago I found a OTC source for 38% nitric for only 30 Euro's per 20 liter. Now I simply let it boil to the azeotrope (which corresponds to plusminus half of the original volume), and when I need conc. nitric I do the H2SO4/DCM extraction. Works wonders for me, leaves me with crystal-clear fuming NA.
mr.pyro Posted April 18, 2007 Posted April 18, 2007 Has anyone ever used an all glass setup under vacuum to distill nitric? If so can you describe your experience and the rate at which the nitric came over?
durfeedog Posted April 25, 2007 Posted April 25, 2007 Mr. Pyro ask if anyone has used vacuum distilation for NA and what was the results? I did it with SA/68% NA and strong vacuum It worked good if dry ice cooling of the reciveing flask was used. I think NA has a hard time condensing when under strong vacuum. (< 50 torr)(best if done twice) and whih excess SA.
pyromainiac420 Posted May 15, 2007 Posted May 15, 2007 This guy seems to have a decent homemade setup...http://www.geocities.com/brainfevert/hno3.html I've never made Nitric acid before, I find I have good success with kno3 or AN with h2so4. Worked to make many things for me, you can actually use this nitrating mixture for alot more explosives than you think. Although I plann on getting some HN03 next time I have the time to set up an apparatus.
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