Nitric Acid Concentration and Purification (Azeotropic and Fuming)
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- เผยแพร่เมื่อ 11 ก.ย. 2024
- 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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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
Your patients, devotion to science, and willingness to share your experience with us is truely priceless. I wholeheartedly thank you.
thanks for watching!
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 ....
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
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
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!
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.
"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.
"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?_
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!
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.
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.
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.
I use climbing chalk to make Mg(NO3)2 since it is MgCO3 or sometimes a double salt with Mg(OH)2.
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
That's the clearest and most comprehensive video on working with nitric acid I've seen. Thanks
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
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.
"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.
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!
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.
Wow! After a long time! Love ur videos! Love chem! ☺️❤️
11:31
The Forbidden Sprite.
Old school 7up if you add lithium carbonate.
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
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.
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.
As so often, a very thorough and clear video. Great stuff; well done, and thank you.
Nice! Chemistry rocks!
Science and chemistry is awesome. Learning and experimenting is good for us
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
*Thanks again* .I like to see every tip about nitric acid! Keep good 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).
Thank God for you!
"Do not attempt to handle boiling hot sulfuric acid" - Nobody should have to be told this, but here we are.
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.
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
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!
One of the true Scientist
Your videos really are some of my favorite in the ametueur chemistry area.
TY for your time and the share!
KNO3 and H2SO4 was the only otc way I knew. Na2S04 and N03 salt dry is an awesome idea. Thanks Dr t-Butyllithium
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
so to get artound the dirty filtrate i put one filter a top another and put it on a stand and yeah worked great 2 filtering steps and its clear as anything this was the calcium nitrate method is viable for me at least its very pure NaNO3 from this process of dissolving it the calcium form and then adding sodium carbonate which produces the same chalk like white paste of just calcium carbonate (i think) im not a chemist by any means just an amateur with a hobby and a love for the science!
Would love to see Anhydrous Magnesium Sulfate used as the drying agent!
Always a treat to watch one of your awesome videos, thanks for sharing :D
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.
You can also use ozone to covert it from red fuming to white fuming. This of course requires a good ozone source.
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.
Best videos on youtube
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.
Very cool video. Thank you NurdRage.
Great video my friend glad to see you again can't wait to see the next video god bless
Regarding magnesium carbonate, I have used climbers chalk which claims to be 100% MgCO3.
That was very impressive!
as always, a very interesting and informative video 👍
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
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 have been using Teflon tape for ever!
11:42 forbidden soda
god damn it you made this comment first
@@kiro9291 it does look very refreshing.
I needed this!
Nurd! Come back! Please!
Magnesium carbonate is often sold as hand chalk for very cheap
it's not necessarily pure though. That's why i said "trustworthy". Now they're not deliberately lying, they think they really are selling the 100% pure stuff. But really what they're selling some of the time is crushed dolomite, which contains calcium carbonate as well.
I really love my masters nurd rage and nile red
Interesting, thanks for the lesson. Best to you Cheers!
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
Rage, you should do a series about setting up an amateur lab from scratch. S.V.P. What is involved in establishing a safe and capable lab? Doing some chemistry interests me, but how deep to I need to get to be sensible about it $1000? $3000? Not sure I should begin if I may never get there. Cheers
A question I have about this topic is whether it's cost-efficient to buy second-hand glassware. It tends to be much cheaper than new glassware, but does it last as long?
Sorry if my english isn't that good.
@@stefaniesieveking7698 that will depend on the brand and how it was used. but borosilicate glass is pretty durable. even the thin wall cheap chinese stuff is pretty durable.
I did this experiment by using my $1300 covid-19 relief check on chemistry supplies. you can do it on 1000 but it's very tight and you'll be spending a lot of time scouring the internet for cheap stuff. 3000 would definitely be more comfortable. nurdrage has a video on this topic i believe. this is a spontaneous list and definitely incomplete, and i haven't been in the same state as my chemistry equipment for 3 months, but approximately:
glassware for storing things (reagent bottles, etc),
glassware for holding things while you use them (beakers, flasks. ideally at least two of each type of flask (erlenmeyer, round bottom, florence), and at least 4 of each size of beaker),
glassware for distillation: condensers (probably liebig and/or allihn, graham condensers are common but restrictive), a three neck flask and some glass stoppers, a vigreux column, various connectors, at least two stands and a lab jack
hot plate stirrer: there are a lot of cheaper chinese ones out there with iffy temperature control, but you can also buy old used ones. these can get expensive. $100 is a very good deal. you could spend your entire budget on just this, the hot plate stirrer will probably be a bottleneck.
various stir bars and a ptfe stir bar retriever
a heating mantle stirrer if you're feeling like blowing cash, but you can use fluid baths on the hot plate as a decent substitute
a nice large separatory funnel
a set of grad cylinders
equipment to pull a vacuum (either an aspirator connected to a sink or a pump, aspirator is cheaper but pump is more straightforward to use)
flexible tubing
fish tank pump to flow water through condensers
glass stir rods, metal powder scoops, etc
a butane lighter with a large flame or a proper blowtorch
I'm almost certainly missing obvious things, but take that as you will. you want to avoid the temptation to use a room in your house that has a sink, unless there's a decent size bathroom you can turn into a mini lab. don't work in the kitchen unless you're only using materials you could find in a kitchen. DIY fume hoods are a huge topic, but it's generally a large plywood box with a venting system to the outside, like you'd find on top of a stove in a new house. you can add filters and multiple pumps and all kinds of things but like I said, that's a whole topic.
Sulphuric acid can be obtained almost anywhere in the world much more cheaply than drain cleaner (and generally more pure) as battery acid. Almost any automotive supply or battery specialist store will sell bottles of it for only a few dollars per litre. Since it is used extremely commonly to recharge the electrolyte in lead acid batteries almost no questions are ever asked; and if there are, well, there is at least one simple answer.
Right on!
would vacuum distillation lend itself to making aziotropic
is that counts per sceond on the device? roetegens of radiation?
Great video.
The remark about hot sulfuric acid instantly dissolving flesh, yes that is the absolute fact. I recommend having a large container of iced saturated sodium bicarbonate solution, just in case. 😸
When I read the title and description all I could think of was
"Did patreon get him to test Dr.Stone"?
Great.
Thanks.
Banging video ! Nice one Nurdy !
why thank!
@@NurdRage you're welco !
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.
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?
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... :)
Do you wear a cape? Not all heroes wear capes
Yep, urea. you need very littlr to clarify.
No lie, I got kinda lost many times during this video. Its ok though, it was still awesome! TY!!
You can get sulfuric acid from oxalic acid and epsom salt
You should look up pirana solution. I just seen it on a Facebook video.
Its a solution that eats and eats
How to use magnesium nitrate to concentrate nitric acid with only simple distillation?
And now I'm on a list
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?
At 18:54, rather than letting the fractional still cool down and then reassemble into the simple distillation apparatus, could you just insulate the reflux column and run simple distillation straight through it? That would reduce the labor needed and save time that would be used for the cooldown, reassembly, and restart.
Really risky moving and handling it while hot. Trust me best just let it cool down then reconfigure.
@@sgtbrown4273 No, what I'm suggesting is _not_ to reconfigure significantly, just to add insulation around the reflux column to defeat the reflux function, and carry out the simple distillation without any rebuilding. No joints broken and no exposure of the contents to the air.
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%
What was your reason for not just using anhydrous magnesium sulfate?
Make delta 8 thc oil.
Could somebody be so kind as to tell me if its possible to use nitric acid to first dissolve gold in this acid, then use it for brush plating? Ive been looking at plating solutions but the cost is quite high for the actual amount of gold in it. Where I live, obtaining these chemicals is not easy, and am looking for the simplest solution.. no pun intended....🍺
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 ?
When you mentioned breaking the azeotrope with Toluene I kind of just heard AC/DC in my head.^^ "cause it's TNT" I know it will probably not react fully but still^^ yeah organic solvents and nitric acid means asking for trouble
That's right, you need concentrated nitric acid to produce TNT
@@kelvinpino4065 its usually done with a mix of concentrated nitric acid and sulfuric acid in if memory serves dry ice and acetone as a cold bath. that actually might already be too hot. (well you cool it that strongly if you DON'T want to nitrate it multiple times)
That ice bath is so cold that you can even licuefy ammonia at -33° C, but if you want a powerful explosive you can just make nitroglycerin that doesn't require that cold temperatures
I already made a nitrating solution and made some flash paper, was very satisfying
@@Metalhammer1993 To turn dinitro to trinitro toluene you need to raise temperature over 60 C (dont remember exactly). The last nitration is hard to do so you need the temperature.
Hi- I’m not sure if you’ll read this but if someone could answer me it would be great- it’s actually about the toning coins with anodizing- I am making the solution exactly like you said- HOWEVER I DONT HAVE A STIRRIR LIKE YOU- 1st I tried a mason jar and covered it, it got really hot and never turned orange even shaking it forever - next I did the 1/2 cup water with 2 tablespoons and 1 tablespoon meathod also in glass mason jar- I did a circular motion for about 12 min and NO ORANGE COLOR AGAIN!!!! Why? It was covered so I took the cover off after about 12 minutes thinking that covering it was the problem, stirred a little more but never turns orange- what am I missing? Help please!? Next I’m going to try uncovered with the 1/2 cup and 2Tb&1Tb method in circular tornado motion (I don’t have the magnet yet, maybe that’s the issue? But I’m stirring it similarly) - please help.