Nitric Acid Concentration and Purification (Azeotropic and Fuming)
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- Опубликовано: 30 окт 2020
- 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.
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![Eminem - Houdini [Official Music Video]](http://i.ytimg.com/vi/22tVWwmTie8/mqdefault.jpg)
The funny thing about forgetting stuff is you don't realize you've forgotten it. I'm really glad these videos are available to rewatch before attempting a process.
YOUR ONE OF MY IDOLS
up to shenanigans again are we?
Careful you dont do anything that warrants another visit from the fun police cody 🤣
@zer-zd4gc this glycerin isn't going to nitrate itself
Love being able to find videos on stuff like this instead of having to look for literature or scholarly articles that are just explanations without visuals. Things are so much easier to find now than when I was growing up! Btw, love your channel Cody.
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.
i really appreciate your vids dude. Much love
& your condenser columns are beautiful
hmmmmm...... as a fellow chemist I have to ask one question very suspiciously...
"What do you need so much Nitric Acid for...?"
@@highlander723 as a fellow viewer of the guy “not your business” because he teaches us loads of info
@@highlander723 he uses it as lube when he performs reactions upon ur butt
Damn, NileRed, NurdRage, ThoiSoi2 and Chemical Force upload a video on the same day, well well, science
More like Saturday...and also higher add buy rates!
@@Wearepricester do you understand transesterification ? You prob could spend your time less complaining and more learning
RIP doug's lab
@@planetsoccer99 ya no1 remembers
Too bad ex&fire didn't. He's taking a break now
these videos are the best one dollars I've ever spent
these videos cost money to watch?
@@okay8632 They cost money to make
@@okay8632 patreon
My friends watch cooking videos for relaxation, and I'm here learning how to distill acid :)
Acid?
It's time to cook!
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
"Do not attempt to handle boiling hot sulfuric acid" - Nobody should have to be told this, but here we are.
Your patients, devotion to science, and willingness to share your experience with us is truely priceless. I wholeheartedly thank you.
thanks for watching!
"because you tend to make explosives" The 10 year old in me perked up at that.
explosions&fire has entered the chat
You just have to search the terrorist manual or the anarchist's cookbook, there is the detailed instructions
exploosives
@@kiro9291 fuck i love the 60s
@@MrDJAK777 good year... _was it?_
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.
@@human_isomer Good catch. God forbid getting silicates in your glassware.
@@user-yb5cn3np5q the glassware doesn't care about the purity of the nitric acid.
@@human_isomer Uh, what?
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.
gas scrubber and a fan does the job
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!
I hope you were running your vacuum line through a gas washing bottle filled with sodium bicarb solution ....
PTFE tape and cable ties are like 50% of my apparatus contructions.
Hahaha me too
Lol
Relatable
@@chemistryofquestionablequa6252 you don’t even know. just yesterday I solved a leaky tank by copious amounts of PTFE tape and 4 cable ties.
NileRed and NurdRage uploading at similar times hummmmm
beat off to nile red talkin bout epsom salt lmfao
Its called a saturday.
@@NurdRage it’s funny of them to draw a comparison due to your videos being much more detailed and providing many useful ideas than a kid making urea from his piss jugs
@@NurdRage and who would’ve thought 💭 uploading a video on the weekend, conspiracy etc., Some viewers have not been using a fume hood while they distill solvents
@@bxnkroll u mad bro
As so often, a very thorough and clear video. Great stuff; well done, and thank you.
That's the clearest and most comprehensive video on working with nitric acid I've seen. Thanks
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!
"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.
Wow! After a long time! Love ur videos! Love chem! ☺️❤️
*Thanks again* .I like to see every tip about nitric acid! Keep good work
I use climbing chalk to make Mg(NO3)2 since it is MgCO3 or sometimes a double salt with Mg(OH)2.
Always a treat to watch one of your awesome videos, thanks for sharing :D
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.
Yeah, wonder what you could end up with.
@@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
@@okay8632 i just pictured that in my head and couldnt stop laughing
You’d also be missing a critical ingredient.
"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.
11:31
The Forbidden Sprite.
Old school 7up if you add lithium carbonate.
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.
There is a good method to deal with precipitate of calcium sulfate: you have to just heat it up to about 40-60°C and leave it like this for several days or even weeks. The precipitate will be aggregated and much more filterable even under vacuum
Your videos really are some of my favorite in the ametueur chemistry area.
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).
TY for your time and the share!
We have new PFA Acid Purifier which could easy to take a look with extremely low bank of metal elements. The model in 2000ML could purify 900ML high purity acid in 12 hours.
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.
Very cool video. Thank you NurdRage.
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.
PTFE tape
as always, a very interesting and informative video 👍
That was very impressive!
I needed this!
Great video my friend glad to see you again can't wait to see the next video god bless
PSA!!!!! Do a video on your repaired hotplates! I was scrolling through your videos as I often do an saw heard your request to remind you. So here you go!
slow and careful heating is absolutely true, always do this during distillation on columns and refluxers, this is essential.
if you have a 1 kW electric stove, and the heating is divided into six divisions, then the distillation can be carried out at the highest heating, but this will be a mistake, you should act sequentially, do an exposure of 20 minutes on the first division, then 20 minutes on the second and so further, so, many people think that acetic acid is poorly concentrated by distillation, but it concentrates quite well.
overheating during distillation spoils everything, so for a stove of one kilowatt with six divisions, ethyl alcohol cannot be distilled at the sixth division, since the required distillation temperature is already reached at the third division, the vapor temperature error is one tenth of a degree, that is, when the temperature changes by two tenths, the distillation is completed.
Nice! Chemistry rocks!
Best videos on youtube
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.
Banging video ! Nice one Nurdy !
why thank!
@@NurdRage you're welco !
KNO3 and H2SO4 was the only otc way I knew. Na2S04 and N03 salt dry is an awesome idea. Thanks Dr t-Butyllithium
One of the true Scientist
Interesting, thanks for the lesson. Best to you Cheers!
i wish i was as smart as you but i sufferd from seizures but i a not going to let it stop me from learning thank you NurdRage i wish you could teach me some of the basics i am going through a very hard time an this is my only outlet to forget my depression
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.
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!
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.
Great video.
I have been using Teflon tape for ever!
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.
You can get H2SO4 relatively easily from copper sulfate electrolysis, see his other video on this topic
Thank God for you!
Right on!
Regarding your comments about molten salts in erlenmeyer flasks: I wish I'd had this knowledge several years ago. I was using a gigantic erlenmeyer (I think it was 25 liters - it was almost a meter tall) for spent acid storage from electronics gold recovery. Copper sulfate crystalized to a layer about 5cm thick on the bottom. I was processing the spent acid and got down to the crystals. I decided to use warm water to speed the dissolution of the crystals. The bottom of the flask blew out as the crystals warmed and expanded. I got it as cheap surplus from a collage lab sale, but I can't even find one to figure out exactly how stupid I was in breaking it, but I figure it would be well into the several hundreds of dollars. Learn from my mistake!
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.
You can also use ozone to covert it from red fuming to white fuming. This of course requires a good ozone source.
Would love to see Anhydrous Magnesium Sulfate used as the drying agent!
I could only get calcium nitrate. Just added water and sodium bicarbonate and crystallized out sodium nitrate. Got some fine fuming nitric when distilling with H2SO4👍 Works like a charm.
Edit: I can get magnesium nitrate too. Might use NaOH to get magnesium hydroxide and sodium nitrate for another reaction. Need the magnesium hydroxide to make different salts and the nitric for nitrations.
Ordering magnesium nitrate will definitely get you on an FBI watch list. I ordered some for my lab because nitric acid for metal etching is expensive, so I was trying to recollect and reuse . The ebay seller reported me and I got a visit lol😂. I fired the supplier and banded them from selling to any of our labs. Then posted there name on all the chemistry pages. They went out of business because of it. Do yourself a favor just make your own.
I really love my masters nurd rage and nile red
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... :)
Thanks.
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.
It's good to mention that is not strictly necessary to use the fractionation column and azeotropic nitric acid to obtain the fuming nitric acid, I just made the experiment and I only needed to add a little bit more dessicat and i used high grade (anhydrous) calcium nitrate fertilizer as dessicat and 55% nitric acid, and a simple distillation apparatus
Yeah, I was also thinking why wouldn't calcium nitrate work directly as desiccant. Apparently calcium nitrate is almost insoluble in nitric acid, so seems it would be great for this purpose.
I do it the calcium nitrate and magnesium sulfate route to make magnesium nitrate.
@Footing Ball555 yes making RDX and PETN but you need 98 + % nitric acid. Here is a link to me making RDX www.bitchute.com/video/6mnKHHEos2c4/
@Footing Ball555 I use magnesium nitrate as a drying agent
Would using a round bottom flask avoid the molten salt problem or make it worse and unavoidable?
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?
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.
Great.
Also I did use the non orange/pale yellow solution on the silver coins and it did seem to work/did work- but I am really wondering why it’s not turning orange like your other videos and if that affects the toning?
I was wondering if instead of using magnesium nitrate to remove the water from the acid, if anhydrous magnesium sulfate can be used instead?
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?
At the end of making fuming Kno3 with con. Kno3 and con. H2so4 how do u regenerate the H2so4?
Could it be done just by boiling the water in it and reused?
as a drying agent would it be possible to use potassium nitrate rather than magnesium nitrate when producing fuming nitric acid? its a bit more available to me and I noticed it tends to absorb water from the air leading me to think it could be a viable drying agent ?
And now I'm on a list
11:42 forbidden soda
god damn it you made this comment first
@@kiro9291 it does look very refreshing.
What was your reason for not just using anhydrous magnesium sulfate?
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!
Pipe insulation as well as wrapped towels are a really greatest thing I've ever used with columns. Until boiling toluene. It just melts down lol. Glass wool followed with foil or something that hang it on the column seems like the best choise for high temperatures
I made a bunch of nitric acid last year in both 99% and 68% so I'm set for a long time.
wow crazy u a hero to us all /s
What purity? Ive been wanting to make some for awhile, i prefer white fuming nitric acid but its hard to purify to that point so i go with rfna instead commonly, but some expiriments i want to try require a certain purity
What Magnesium Nitrate are you using ? the hexahydrate? . I have access to the fertiliser grade that is the hexahydrate
What is the difference between using magnesium nitrate and magnesium sulfate as desiccant?
So... instead of buying PTFE sleeves or tape, (which is Teflon right?) What about using Super Lube? It's supposed to be PTFE grease. Might be easier and cheaper than the other depending of course. Just a thought..
I need nitric acid for silver refining and have managed to make fuming nitric acid however I am concerned about the acid being to strong since I’m not needing a bomb. Lol. Do I distill through fractional distillation?
When I read the title and description all I could think of was
"Did patreon get him to test Dr.Stone"?
Hey I’m here from the DSSC video could you please tell me the name of the electrolyte you synthesised to put between the 2 plates
is that counts per sceond on the device? roetegens of radiation?
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%
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.
Hey have you remembered to repair your hotplates? Also are you still going to make one?
nurdrage where did you get your digi thermometer?
Nurd! Come back! Please!
Can you use liquid fertilizer to produce nitric acid?
Is it possible to use 55% nitric acid(or even a little less) and sulfuric acid directly to get fuming nitric acid?🤔
Would this work with Potassium Nitrate instead of Sodium Nitrate?
Yes, but how does it taste?
Greeting
That's a good video.
Thanks for the explanation!
Where do you measure the temperature? In liquid or in the throat before the distiller?
the throat, you want to see liquid condensing and dripping off the thermometer. The boiling liquid itself is not good because mixtures of liquids will have different temperatures than the fractionated vapor.
@@NurdRage Thanks for the explanation.
What type of liquid would be best used for a heating bath? So I can maintain an accurate and constant temperature.
@@marox3G i don't use heating baths since i find them unnecessary for nitric acid. But if you really have to use one, then mineral oil or silicon oil would likely be best. A sand bath or copper shot bath can also be used.
@@NurdRage Thanks for the reply.
What do you change Wire gauzes, with ceramic when you don't have one? Could I use transformer oil for a bath?