NurdRage - 2020-10-31
In this video we purify and concentrate dilute nitric acid using a combination of fractional distillation and drying agents to produce azeotropic nitric acid and fuming nitric acid. Donate to NurdRage! Through Patreon (preferred): https://www.patreon.com/NurdRage Through Youtube Memberships: https://www.youtube.com/channel/UCIgKGGJkt1MrNmhq3vRibYA/join Through Bitcoin: 1NurdRAge7PNR4ULrbrpcYvc9RC4LDp9pS Glassware generously provided by http://www.alchemylabsupply.com/ Use the discount code "nurdrage" for a 5% discount. Twitter: https://twitter.com/NurdRage Reddit: https://www.reddit.com/r/NurdRage/ Instagram: https://www.instagram.com/nurdrageyoutube/
Wait, you don't want to add toluene to dry your nitric acid? I never would have guessed that overly aggressive nitration of toluene would be a problem.
@MaxSeidel1 pours in toluene, song pops into head (acdc: tnt oy oy tnt im a power load tnt watch me explode...)
TNT? ; ) Not sure if an obvious joke, Nurdrage already said fuming and dilute are like two different reagents lol
@O K A Y i just pictured that in my head and couldnt stop laughing
You’d also be missing a critical ingredient.
@Andrew Gregory Hansen sulfuric acid?
Your patients, devotion to science, and willingness to share your experience with us is truely priceless. I wholeheartedly thank you.
thanks for watching!
Just a thought. Since Nighthawkinlight is refining the process of producing rubies at home, do you find it suitable to make a video/experiment regarding this topic? I think these kind of topics are fun and informative like your sodium and pyramethamine series. Anyways nice video as always, Nurd!
This is one of those experiments that should really be performed in a proper fume hood. Definitely don't want to be working outside when out of nowhere the wind changes direction and that brown cloud you are trying to avoid has trouble avoiding you.
A discourse in the construction of a workable fume hood would be sweet. I play with PM recovery and even a whiff of HCl fumes can lead to respiratory distress. The exhaust hood in mom's kitchen can get you killed if Mom doesn't do it first
I use a fan to ensure the wind doesn't change just cuz ur outside doesn't mean u have to be at the mercy of nature all the time.
It would be interesting to see a video covering the careful use of heat to decompose some metal salts while leaving precious metal salts intact, as a means of partial purification. It would be interesting to compare the labor and material costs of this versus established purification routes. Using heat to reduce the amount of unwanted components so that later purification might be more efficient.
Awesome video! I’m a big fan of packed columns for fractional distillation. If you use glass rings packed in a straight column, you can get orders of magnitude more surface area in the same length as compared to a standard vigreux column. I also built a refluxing condenser a while back that is internally subdivide to return 1/3 of the product back into the top of the column. This is much more ideal and allows the column to operate over a wider range without flooding. FYI, I use PTFE grease when distilling acid. Yeah, it’s a lot more expensive, but you only need a drop per joint. Can’t wait till the next video!
Very interesting! Learned a lot. So it's possible to make fuming HNO3, just from normal HNO3 and some easy made Magnesiumnitrate.
Buying conc. H2SO4 is very hard these days and distilling the diluted to conc. H2SO4 on your own, is at least the same work, as recycling the Magnesiumnitrate. So this is very helpful information for many backyard chemists I am sure.
Thank you - keep up the great work.
Excellent video! That's how such chemistry videos should be. I'd recommend this for for teaching chemistry, maybe with adding one or two basic formulae (only for completeness).
As so often, a very thorough and clear video. Great stuff; well done, and thank you.
You can avoid the loss of fuming acid due to air exposure by prefilling the flask with argon/nitrogen gas blend which is sold as a wine preserver. It comes in a can similar to the old WD-40 with the attachable straw so you can expel the air from deeper in the flask.
To obtain clear fuming nitric acid, you can distill it under vacuum. In this way you will work with lower temperatures and the decomposition of nitric acid in NO2 is strongly limited. I used this way to concentrate nitric acid, using H2SO4 as dessiccant agent.
Thanks for this new video!
Damn, NileRed, NurdRage, ThoiSoi2 and Chemical Force upload a video on the same day, well well, science
@greensunrise ya no1 remembers
Too bad ex&fire didn't. He's taking a break now
@John Doe why is he? I saw the vid just didn’t bother to check it
@Bxnkroll supposedly to continue his phd uninterrupted
@John Doe o wow
Dear Nurdrage, thank you very much for the explanation and presentation of this process !
A question: could you use cheap, dry zeolithe placed next to your flask with dilute nitric acid inside a closed container to achieve azetropic nitric acid, when you let it rest for a few days/weeks? Could you also use aluminium silicate zeolithes for making fuming nitric acid by just adding it into the azeotrope? I know, you spoke of molecular sieves, that would degrade, but was it also refering to zeolithe molecular sieves?
Zeolites and molecular sieves are the same thing. Just zeolites refers to a broad category of materials, while molecular sieves is a specific sub-class that's been engineered for a particular composition and thus gives defined and reliable results. They'll both get destroyed by strong acid.
Just so you know, Climbing chalk is made of Magnesium Carbonate, it may have other impurities, but as far as I'm aware its close to pure.
its those other impurities i'm worried about. So i decided to go with epsom salts and sodium carbonate since i knew what was in them.
it may be MgCO3, but it might also contain a lot of Magnesium Silicate (Talc), so it's a good idea to go with what you know for sure.
Thank you so much, Again. Where I reside nitric acid is well, unattainable. I have been working on a project to recover fine silver and all I had to work with was kno3 and copper sulfate. Your work here has shown me new paths to nitric acid that I was unaware of. Thank you so much.
Plumber's tape is something that has so many uses and is always found in bulk in my box of lab items. It's so cheap and so useful.
Love the channel man still watching your videos 10 years later. Quick question?, I wonder in the dry process of making nitric acid with a 150g Of Sodium Bisulfate monohydrate and 49g of Calcium ammonium nitrate. Can I Substitut the monohydrate with anhydrous for higher % of acid?
My friends watch cooking videos for relaxation, and I'm here learning how to distill acid :)
Well, chemists often say "to cook" when it means to perform appropriate reactions to produce some desired substance, so it's also a sort of cooking :)
Marta is cute ._.
tak
chemistry and cooking is the same thing, as demonstrated by breaking bad
So youtube is good tool for all
"Do not attempt to handle boiling hot sulfuric acid" - Nobody should have to be told this, but here we are.
Your videos really are some of my favorite in the ametueur chemistry area.
as always, a very interesting and informative video 👍
Science and chemistry is awesome. Learning and experimenting is good for us
A wow mate. Keep it up. There are times you just have to go backand do things like this. And a long time has passed since you bid those vids. 👏👏👏👌👍 Still as amazing any way.
I had hoped you included and compared the density’s of both fuming nitric acids and therefore give their concentrations. Did you measure them?
they're both the same at ~1.51g/ml or 100%. I didn't put it on screen because i told you directly at the beginning it was 100%
Hey NurdRage, can you do titration of the acquired product from magnesium nitrate method, I wonder how actually concentrated the fuming nitric got in the end.
A much simpler method I've found for dealing with nitrogen dioxide coloration is to simply add a few drops of hydrogen peroxide to the solution.
"that's not a good idea, because you tend to make explosives" I lol'd hard at that. Mainly because I was recently rereading "things I won't work with" over at Pipeline again. Derek Lowe is hilarious.
Thanks again .I like to see every tip about nitric acid! Keep good work
Always a treat to watch one of your awesome videos, thanks for sharing :D
There are a few fully halogenated greases you can use for your ground-glass joints, I believe one of them is called Kel-F grease, I haven't tested the reaction of RFNA with several of these but I'm reasonably sure they can be used if needed.
Great video as always!
Krytox and Teflon tape are essential tools.
You can also use ozone to covert it from red fuming to white fuming. This of course requires a good ozone source.
Fractional distillation is intriguing, mostly cos I have no clue how it works, especially when you take a sludge like crude oil and manage to get so much out of it using the process... :)
Hello nurdrage, any chance of exploring the catalytic oxidization of ammonia to produce nitrogen oxide? I fear with the current political climate soon all nitrate salts will become off-limit to civilian.
I was surprised when he tilted the flask. That's the solution I came up with and I'm not use to being right about anything in these videos.
"I't called fuming nitric acid... because it fumes. You never cease to amaze me.
That beimg said, I hope you are well on your way to a new lab and resuming your epic path.
I was wondering if instead of using magnesium nitrate to remove the water from the acid, if anhydrous magnesium sulfate can be used instead?
KNO3 and H2SO4 was the only otc way I knew. Na2S04 and N03 salt dry is an awesome idea. Thanks Dr t-Butyllithium
Hi.. can you help with obtaining lead from lead sulfate?
Would it be similar to how you obtain copper from copper sulfate?
Did you measure/test the concentration of the two results nitric acid?
Interesting, thanks for the lesson. Best to you Cheers!
PTFE tape and cable ties are like 50% of my apparatus contructions.
Hahaha me too
Lol
Good job! Please remake a video about Sulphuric Acid Concentration and Purification (with temperature control).
The temperature control is actually not an issue here (it should be about 320 °C in the end). The real problem here is that concentrated sulfuric acid tends to superheating when it boils and the usage of boiling stones or a magnetic stirrer is a must here unless you are fine with splashes of hot concentrated sulfuric acid.
"because you tend to make explosives" The 10 year old in me perked up at that.
@Kelvin Pino those are VERY unreliable, there are better information sources for energetics synthesis
@Kiro no, the worst
2020 ;\
@Kelvin Pino anarchist cookbook recipes are a good way to meet Darwin.
@1320crusier I made a few recipes and all of them were a success, as long as you make little quantities and follow all de basic security measures you will be fine
@1320crusier having survived my teenage years these books will kill you.!!!!!!!!!!!!!!
its great for recovering all the gold sitting in our closets. just set up a pentium dual core today running linux and its working as well as newer units .however i kept thinking about how heavy the gold was on these chips wishing for a gallon or two for metal recovery.
Informative video. One thing though: fractionating columns work best under adiabatic conditions and using aluminum foil is both inefficient and wasteful. I read a paper that researched column insulation in order to stop students from wasting foil & improve performance. They decided on foam pipe insulation - the kind from the hardware store. I have sections cut to my column lengths and even wrap them with foil, but permanently. I get a lot of use before having to replace them and I’m hoping to make the cover of Vogue ;) Also, the delta T between the top & bottom of the column can help with how “hard” you can drive the column. I recommend reading both while distilling.
I do agree that pipe insulation is much better. I just use aluminum foil because it's quick and easy for the amateur. Perhaps in the future i'll upgrade. as for being wasteful... I actually use the same bunch of foil for many months!
Would using a round bottom flask avoid the molten salt problem or make it worse and unavoidable?
these videos are the best one dollars I've ever spent
these videos cost money to watch?
@O K A Y They cost money to make
I was wondering if phosphorous pentoxide, however, can remove the water from nitric acid, after you distilled 2 different fractions of acids. but it sometimes makes dinitrogen pentoxide. Which is an anhydrous form of Nitric Acid, It Can Nitrated Organic Without Sulphuric Acid.
When I get a locked joint, I just let it cool down completely and then it is easier to twist loose. I also use glicerine to lubricate the joints.
NurdRage - 2020-10-31
This video took a month and a half to make because fractional distillation is @#$!# slow. And i actually ran dozens of distillations to determine if my results were reproducible. At least now i have a decent amount of nitric acid.
Alek Escalante - 2020-12-04
Have u ever thought of using the birkeland eyde reactor
θ-θ σ-σ - 2021-07-09
@highlander723 lots of copper needs dissolving 😗😉
MyNameIs - 2021-10-07
Unfortunately Mg(NO3)2*6H2O decomposes upon heating, even at 170 degrees celcius, instead of releasing the water...
Andrew Gregory Hansen - 2021-10-30
@Patrick Sweetman I probably could. The tricky part would be actually measuring the flow without eating up a sensor. Best thing to do would probably be to have a sensor under the collecting flask, to effectively count the drips.Then right a function to equate the rate (approximately) to the ml/s. A sensitive/high resolution load cell might work as well, to equate the rate. I’m both cases, you’ll be making a priori assumptions about the density of the HNO3.
Not sure if I have time for something like this right now, but maybe in the future.
Patrick Sweetman - 2021-10-30
@Andrew Gregory Hansen Yes, weight would work, although I was thinking of the drops from the condenser interrupting a light beam. With the Arduino you could keep track of the temperature, the rate of distillation, and the total volume to change the receiving container.