Nitric Acid Concentration and Purification (Azeotropic and Fuming)
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- Опубліковано 27 вер 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!
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!
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
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 ....
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.
@1 2 the glassware doesn't care about the purity of the nitric acid.
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
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.
"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?_
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
"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.
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!
That's the clearest and most comprehensive video on working with nitric acid I've seen. Thanks
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.
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!
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.
11:31
The Forbidden Sprite.
Old school 7up if you add lithium carbonate.
Wow! After a long time! Love ur videos! Love chem! ☺️❤️
Science and chemistry is awesome. Learning and experimenting is good for us
"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.
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!
"Do not attempt to handle boiling hot sulfuric acid" - Nobody should have to be told this, but here we are.
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!
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
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).
*Thanks again* .I like to see every tip about nitric acid! Keep good work
One of the true Scientist
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 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.
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!
KNO3 and H2SO4 was the only otc way I knew. Na2S04 and N03 salt dry is an awesome idea. Thanks Dr t-Butyllithium
Would love to see Anhydrous Magnesium Sulfate used as the drying agent!
TY for your time and the share!
Your videos really are some of my favorite in the ametueur chemistry area.
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
Nurd! Come back! Please!
You can also use ozone to covert it from red fuming to white fuming. This of course requires a good ozone source.
Best videos on youtube
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.
Always a treat to watch one of your awesome videos, thanks for sharing :D
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 have been using Teflon tape for ever!
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.
Very cool video. Thank you NurdRage.
That was very impressive!
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.
I really love my masters nurd rage and nile red
as always, a very interesting and informative video 👍
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.
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.
Do you wear a cape? Not all heroes wear capes
Banging video ! Nice one Nurdy !
why thank!
@@NurdRage you're welco !
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..
Right on!
Great video.
Interesting, thanks for the lesson. Best to you Cheers!
And now I'm on a list
Yep, urea. you need very littlr to clarify.
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. 😸
You can get sulfuric acid from oxalic acid and epsom salt
is that counts per sceond on the device? roetegens of radiation?
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.
Great.
Thanks.
When I read the title and description all I could think of was
"Did patreon get him to test Dr.Stone"?
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.
It does work but remember will slightly dilute your acid 😊
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?
Make delta 8 thc oil.
No lie, I got kinda lost many times during this video. Its ok though, it was still awesome! TY!!
10:20 Making magnesium nitrate for stronger nitric acid. (15:00)
I want to know that the ball point pens contains Polyethylene glycol as the Google says that it also contains polyethylene glycol
What was your reason for not just using anhydrous magnesium sulfate?
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.
happy to be able to see your new video. Hard for a Chinese to cross the government's ban of the internet
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%
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?
Greetings, we provide the Silicon Carbide Heat-Exchanger for Hydrogen fluoride, Nitric acid, phosphoric acid and other complex condition all over the world.
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.
I now really wonder why you don't use magnesium sulfate directly as a desiccating agent. The thing is it is readily available, also very hygroscopic and you can't do anything wrong while regenerating it, as it does not decompose untill 1200 °C.
Or calcium nitrate directly.
I got my PTFE seals for a reasonable price, 2-3 USD per piece I think. I could send you some but I am not sure if I can get the right size. Mines are 29/32. Let me know
Shows there are 396 comments.... but I can only see 46 of them. Whats up here UA-cam??
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.
Glass sculptures that's what I call these dangers
@Whoop!
got your video as a suggestion not in my subscriptions feed... :(
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?
for the life of me, I can't find a decent distillation kit. Either no name brands sketch me out on large vendor websites or fischer scientific/2 more decent places want to sell a very minimal one for too much. Sufficient pieced kit is like 250$ atleast anywhere
What is the difference between using magnesium nitrate and magnesium sulfate as desiccant?
Hi i need Stannous Octoate T9 catalyst making pls