after the distillation is done and cooled down, i recommend disassembling the apparatus with a 5gal bucket of water near by. as soon as you take it apart, you should set your glass into the bucket to keep fuming to a minimum, and also to minimize the amount of droplets that may hit the floor. much better than leaving trails of brown gas and nitric drippings on the way to the sink!
What size Polyethylene tubing fit onto the vacuum adapter? I am buying my kit, but I am unsure what size tubing I should get, I know that tubing is more bend/flex resistant than others. I just want to get the right size.
Long have I wanted to do aqua-regia. Nitric acid in appropriate concentration has been a bit of a sticky spot. Is there any other nitric salt besides ammonium nitrate that would work similarly?
@OAbrey Ammonium nitrate is by far the most suitable due to it's high solubility in sulfuric acid and if distilled at atmospheric pressure, the ammonium bisulfate will be molten when you're done, preventing an unstirrable crystalline mass like I got. I'd suspect sodium nitrate to be the next best due to it's higher solubility than potassium nitrate. You may want to dissolve in water beforehand, and have enough around to distill of the 69% azeotrope.
Is it possible to use a grahm condenser horizontaly? I have a 200mm grahm condenser and dont have the proper glass to use it vericaly and would like to use it. My theorey is that the vapors from the boiling liquid would push the distilate through. Does anybody definatively know wether I can use the grahm condenser horizontaly?
@99Chemicals I can't say I've ever tried. I'd test it with something like water before you do anything hazardous in case it goes badly. You should really invest in a liebig.
@UC235 I bought a distilation kit on Ebay and it had both West and Grahm condensers. I have used the West very sucsessfuly 3 times on simple distilation. I haven't used the Grahm yet. Isn't a Grahm a good reflux condenser?
@99Chemicals Not really. The tubing is narrow so liquid might have a difficult time draining back into the flask, especially with fresh vapor pushing up into the coil. Unless you are furiously boiling a solvent with a low b.p. (ether, DCM, etc.) a liebig/west condenser upright is fine for reflux. A downward grahm condenser is a very efficient condenser for the same low boilers when distilling them.
Question, how the heck do you avoid the fumes? They seem to diffuse out and it is impossible for me to use it without smelling a bit of it so I have never dealt with fuming nitric acid again. Burning in the throat isn't nice. : /
Why don't people just buy (water) aspirators, even though they are limited by vapor pressure and at best not as strong as a vacuum pump, they are completely acid proof(glass) and very in the case of metal aspirators. I have one with a closed loop system and it is good for everything except for high temp. boiling oils. They are also dirt cheap(15$).
I enjoyed seeing you get excited over the nitrogen oxides from the reaction with copper. It's often the little things in life... And for those of us who are chem nerds, those little things are usually quite strange--colorful gases, white solids, clear colorless liquids, and clean glass.
@bfesser I hadn't seen copper attacked by nitric acid (well, other than video) since my high school teacher who got me into chemistry showed us the standard dissolving penny years ago. I often don't practice before recording something (Though the intros where I talk for a long time take me half a dozen tries to get right since I make it up as I go) so that was my actual reaction.
@krazypunk50 You can buy teflon sheeting on ebay and cut it into rounds for lining caps. Pick something reasonably thick, not the thin sheets they sell for heat transfer. I happened on a case of bottles that came with pre-lined caps.
@hkparker Lucky find on ebay. It was $135 shipped and required a thorough dismantling and cleaning with acetone plus some replacement o-rings (fortunately not exposed to solvent/acid fumes so I just went with hardware store ones). If the dismantling sounds daunting, it isn't. They're made to be opened and cleaned so it's relatively simple and stupid-proof inside.
@UC235 Thats good. I'm not in the market for a pump right now as ill be going off to college soon here, but ill keep that in mind when I do get one, looks like a great find.
Nice video, but how can you be sure that your nitric acid doesn't also contain sulfuric acid? I figure that even though the temperature was far below its boiling point, some of it might have made it out as vapor and condense back, before reacting with the NH4NO3
@ignilc It probably contains traces of sulfuric acid; quite less than 0.5%, I'd expect. The still pot wasn't within 70 degrees of sulfuric's estimated boiling point under vacuum and the 3-way adapter was 150 degrees away from it. It was probably further from the actual boiling point because nomographs work best for nonpolar materials. More likely is that some sulfuric mist was kicked up by the boiling nitric which made it's way into the condenser. Vacuum fractionation would remove this.
@UC235 What tests could be done to determine whether there is sulfuric acid contamination? I was thinking by mixing your acid with a calcium chloride solution, if there was H2SO4 in there, CaSO4 would precipitate, right? I will also try this synthesis using KNO3 in the near future.
@ignilc CaSO4 would be too soluble, especially in concentrated nitric acid, and even in dilute nitric acid. Dilution with water and neutralization with BaCO3/(OH)2/(OAc)2 would give cloudiness or precipitate if sulfate was present (and the solution was still faintly acid). (do make a blank with known pure acid though, lest there be insoluble gunk in the Ba salt to give a false positive) I'm really not concerned about it for my uses. It's mostly just going to get mixed with sulfuric acid again.
You can always test for this by dilution followed by addition of aqueous silver(I) nitrate. Silver(I) sulfate is much less soluble than the nitrate. You could similarly use barium nitrate.
Thank you gentlemen, I have 40kg of KHNO3 I am trying to do something with. Was hoping I could substitute it without loosing too much strength...
OAbrey 1 week ago
after the distillation is done and cooled down, i recommend disassembling the apparatus with a 5gal bucket of water near by. as soon as you take it apart, you should set your glass into the bucket to keep fuming to a minimum, and also to minimize the amount of droplets that may hit the floor. much better than leaving trails of brown gas and nitric drippings on the way to the sink!
caliusoptimus 1 week ago
What size Polyethylene tubing fit onto the vacuum adapter? I am buying my kit, but I am unsure what size tubing I should get, I know that tubing is more bend/flex resistant than others. I just want to get the right size.
ISheLLShockI 2 weeks ago
where did you get your ammonium nitrate
crapbag1997 2 weeks ago
Long have I wanted to do aqua-regia. Nitric acid in appropriate concentration has been a bit of a sticky spot. Is there any other nitric salt besides ammonium nitrate that would work similarly?
OAbrey 3 weeks ago
@OAbrey Ammonium nitrate is by far the most suitable due to it's high solubility in sulfuric acid and if distilled at atmospheric pressure, the ammonium bisulfate will be molten when you're done, preventing an unstirrable crystalline mass like I got. I'd suspect sodium nitrate to be the next best due to it's higher solubility than potassium nitrate. You may want to dissolve in water beforehand, and have enough around to distill of the 69% azeotrope.
UC235 3 weeks ago
Is it possible to use a grahm condenser horizontaly? I have a 200mm grahm condenser and dont have the proper glass to use it vericaly and would like to use it. My theorey is that the vapors from the boiling liquid would push the distilate through. Does anybody definatively know wether I can use the grahm condenser horizontaly?
99Chemicals 1 month ago in playlist More videos from UC235
@99Chemicals of course you can use it
thegodofchemistry 1 month ago
@99Chemicals I can't say I've ever tried. I'd test it with something like water before you do anything hazardous in case it goes badly. You should really invest in a liebig.
UC235 1 month ago
@UC235 I bought a distilation kit on Ebay and it had both West and Grahm condensers. I have used the West very sucsessfuly 3 times on simple distilation. I haven't used the Grahm yet. Isn't a Grahm a good reflux condenser?
99Chemicals 1 month ago
@99Chemicals Not really. The tubing is narrow so liquid might have a difficult time draining back into the flask, especially with fresh vapor pushing up into the coil. Unless you are furiously boiling a solvent with a low b.p. (ether, DCM, etc.) a liebig/west condenser upright is fine for reflux. A downward grahm condenser is a very efficient condenser for the same low boilers when distilling them.
UC235 1 month ago
Question, how the heck do you avoid the fumes? They seem to diffuse out and it is impossible for me to use it without smelling a bit of it so I have never dealt with fuming nitric acid again. Burning in the throat isn't nice. : /
luftwaffe1111 1 month ago
Why don't people just buy (water) aspirators, even though they are limited by vapor pressure and at best not as strong as a vacuum pump, they are completely acid proof(glass) and very in the case of metal aspirators. I have one with a closed loop system and it is good for everything except for high temp. boiling oils. They are also dirt cheap(15$).
PyroPudding 2 months ago
Very Nice Video Bro
Mir03318480318 5 months ago
Great video, very informative, very helpful.
joshuamnr 6 months ago
Are the fumes dangerous if i want to do this?
xXAkitokunXx 7 months ago
@xXAkitokunXx Yes the fumes are very dangerous, it feels like you are inhaling fire.
Nitricthunder 5 months ago
Wow! this helped me! Seems interesting!
xXAkitokunXx 7 months ago
Do you think that sodium bisulphate can be used instead of sulfuric acid? (after replacing ammonium nitrate with sodium nitrate)
NaNO3+ NaHSO4--> HNO3+ Na2SO4
yellowmetalcyborg 7 months ago
A very well made video. Thank you!
ddoleiden 7 months ago
Where can i get a good chemistry book to start from?
Solingen1000 11 months ago
I enjoyed seeing you get excited over the nitrogen oxides from the reaction with copper. It's often the little things in life... And for those of us who are chem nerds, those little things are usually quite strange--colorful gases, white solids, clear colorless liquids, and clean glass.
Great video. Please keep them coming!
bfesser 11 months ago
@bfesser I hadn't seen copper attacked by nitric acid (well, other than video) since my high school teacher who got me into chemistry showed us the standard dissolving penny years ago. I often don't practice before recording something (Though the intros where I talk for a long time take me half a dozen tries to get right since I make it up as I go) so that was my actual reaction.
UC235 11 months ago
Great video! I've been searching for those ptfe lined caps for wfna storage for awhile now. Where did you get yours?
krazypunk50 11 months ago
@krazypunk50 You can buy teflon sheeting on ebay and cut it into rounds for lining caps. Pick something reasonably thick, not the thin sheets they sell for heat transfer. I happened on a case of bottles that came with pre-lined caps.
UC235 11 months ago
where did you get your glassware and equipment?
PyroAbsestion22 11 months ago
Great product! I wish I had a vacuum pump for my nitric acid setup. Where did you get that pump?
hkparker 11 months ago
@hkparker Lucky find on ebay. It was $135 shipped and required a thorough dismantling and cleaning with acetone plus some replacement o-rings (fortunately not exposed to solvent/acid fumes so I just went with hardware store ones). If the dismantling sounds daunting, it isn't. They're made to be opened and cleaned so it's relatively simple and stupid-proof inside.
UC235 11 months ago
@UC235 Thats good. I'm not in the market for a pump right now as ill be going off to college soon here, but ill keep that in mind when I do get one, looks like a great find.
hkparker 11 months ago
great video
coolliger 11 months ago
How big is that liebig? It looks huge in the video and Thanks for the link to the density table, it's much better than what I used.
Gyzmodium 11 months ago
@Gyzmodium The water jacketed portion is 400mm.
UC235 11 months ago
Nice video, but how can you be sure that your nitric acid doesn't also contain sulfuric acid? I figure that even though the temperature was far below its boiling point, some of it might have made it out as vapor and condense back, before reacting with the NH4NO3
ignilc 11 months ago
@ignilc It probably contains traces of sulfuric acid; quite less than 0.5%, I'd expect. The still pot wasn't within 70 degrees of sulfuric's estimated boiling point under vacuum and the 3-way adapter was 150 degrees away from it. It was probably further from the actual boiling point because nomographs work best for nonpolar materials. More likely is that some sulfuric mist was kicked up by the boiling nitric which made it's way into the condenser. Vacuum fractionation would remove this.
UC235 11 months ago
@UC235 What tests could be done to determine whether there is sulfuric acid contamination? I was thinking by mixing your acid with a calcium chloride solution, if there was H2SO4 in there, CaSO4 would precipitate, right? I will also try this synthesis using KNO3 in the near future.
ignilc 11 months ago
@ignilc CaSO4 would be too soluble, especially in concentrated nitric acid, and even in dilute nitric acid. Dilution with water and neutralization with BaCO3/(OH)2/(OAc)2 would give cloudiness or precipitate if sulfate was present (and the solution was still faintly acid). (do make a blank with known pure acid though, lest there be insoluble gunk in the Ba salt to give a false positive) I'm really not concerned about it for my uses. It's mostly just going to get mixed with sulfuric acid again.
UC235 11 months ago
@ignilc
You can always test for this by dilution followed by addition of aqueous silver(I) nitrate. Silver(I) sulfate is much less soluble than the nitrate. You could similarly use barium nitrate.
bfesser 11 months ago
Nice!
kuro96inlaila 11 months ago
That glassware would get me in jail in Australia, despite having a chemistry degree.
nucleochemist 11 months ago
@nucleochemist Thats horrible : <
Zaekk 11 months ago
Try to dissolve some human flesh next time (not your own!).
Poleschs 11 months ago
Another brilliant video! Great work, @UC235!
ScienceBroadcast 11 months ago