Making Concentrated (68%) Nitric Acid

Hello! In this video we will be making 68% (azeotropic) nitric acid. This is standard lab grade stuff to do things like nitrations.
I am making the nitric acid because i need it to make mercury (II) thiocyanate (aka the Pharaoh's Serpent).
Doug's Lab video: • Nitric Acid Day!
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Nile talks about lab safety: • Chemistry is dangerous.

[@Incubansoul]

"it's also useful for making explosives" *marks off another spot on my FBI watchlist bingo card*

[@the_inquisitive_inquisitor]

*ASLO useful for?* That's like the main thing it does!

[@mathewrabchuk2500]

He definitely already has 60 bingos

[@kibukaj2956]

Totally not the reason I searched for it

[@aldenconsolver3428]

Just remember next time you buy online chemicals to take a couple cups of coffee out to that unmarked van in front of the neighbours.

[@big_oil]

Combine with Aniline for a special surprise

[@maddieshalaby3482]

watching niles older videos and comparing them to his newer videos is fun, he’s gotten so much more comfortable with us. love you nile

[@dudetapedtoafridge3073]

​@@ithecasticdon't worry thats just his crippling caffeine addiction taking over

[@SirJeff]

0:49 "I don't really plan on making any videos on explosives" Ex&F: Mmmm yes, it's free real estate

[@placeholerwav]

The funny thing is that he made picric acid

[@sobbe07]

Can someone please explain why Nile's videos are so calming? ha

[@NileRed]

+sobbe07 haha i never thought they would be calming

[@sobbe07]

+Nile Red Maybe it's just me hah

[@Agustx0]

It's a very calm voice.

[@JamesHartleyri]

+Nile Red If you had an ASMR channel you would probably have a million Subs. Perfect ASMR Voice! Meant as a compliment of course, not sarcasm etc. You have a really great voice

[@origamigek]

Because his video's have a calm formal instructional vibe to them.

[@NicolasBana]

Who thinks the round bottom flask looks a bit like Jupiter at 2:34 ?

[@a3xccy379]

Same pinch

[@196Stefan2]

yes, there is even a "Big Red Spot" (of NO2).

[@ccleake1]

196Stefan2 Of nitrogen dioxide?

[@196Stefan2]

In the round flask of course, not on Jupiter. It's upper atmoshere consists of many different compounds, but NO2 isn't there in a remarkable concentration.

[@Tornado5871]

I was about to say that.

[@jafddfea3979]

Hey, I'm from Germany and love your videos because they are still understandable although I'm not the best in english. Also you promoted my interest in chemistry because now I'm able to understand more of the processes during a reaction especialy because in school we aren't allowed to do almost all experiments which may be funny ( Germany... ) :). I like too that you speak clear and not to slow or fast, that you put pictures of the reactions to the top (or somewhere else) is good. So go on, please!!!

[@NileRed]

+Jafd Dfea I am very glad that you enjoy it. I am happy to know that they are easy to understand :)

[@hamoudi_d]

its weri gud juh faund gugl translätor 😂

[@Creed590]

@@NileRed Hey, im a great Fan of your Channel, also from Germany and have a simple question, hope you can help me with it: I liked to make some nitration acid and read about it from mixing sulfuric acid with nitric acid (in ratio 2:1 - 1:2). I got sulfiric acid (94-96%) and nitric acid (60%), is it possible to mix this to make nitration acid in a good concentraition? in what ratio should i mix it? Hope you can help me, i realy Like to Support you in the future, only of cause your cannel i manneged to isolate a bit Bromine :D Thanks and go on, you make a really good job!

[@Creed590]

Hope you know waht i mean, the translation is not that easy for me, in german: nitric acid is Salpetersäure. But i need the spesific nititon acid for nitrations in german: Nitrirsäure and i do not know the english synonyme...

[@yasyasmarangoz3577]

Hallo, auch Deutsch :D?

[@Dingomush]

I’m so glad that you do chemistry and post videos. I’d love to be able to do reactions, reductions,and distillations but I’m bad enough at cooking! Let alone something that I or someone else could get hurt with! Thank you, Sir.

[@Sentinalh]

Your videos really make me want to get into chemistry.

[@1HeartCell]

+Sentinalh Do it, its worth it.

[@LadyBas666]

+1HeartCell True!

[@chemistryscuriosities]

they got me into it! got two distalation sets with the vigruex columns and a Graham condenser and of course the Liebig condensers with 500ml round bottom flasks and 250ml also it's only 24/29 and I think the 24/40 is stronger. what do you think?

[@Nickalaich]

+Cannagorilla Canna In Russia we don't have 24/29 and 24/40 at all. 14/23 and 29/32 are common, lol, and we don't bother with chossing the right one. It depends mostly on the size of your setup.

[@chemistryscuriosities]

Well, ebay or a good connect in the states can help you. What are you looking for?

[@BWIceSoldier]

When you did the last distillation, i started to look up what the fractional column did since i'd seen it in other (later) videos as well. I laughed when i came back to the video and you actually explained it immediately after i unpaused! Love your videos!

[@stevetobias4890]

You inspire me to learn more about chemistry. The way you explain everything as well as the way you demonstrate each procedure. Job well done and worth watching every minute.

[@the_inquisitive_inquisitor]

Nitric Acid be looking like Jupiter. Fun stuff, I like how it turns basically anything into explosives.

[@geomadened6201]

I watch these videos because they’re informal and calming, and half the time at the middle of the night when I can’t sleep, like a lullaby

[@something8886]

After taking an organic chem lab course as well as 2 organic chem courses i find these videos a lot more understandable and i can even go with the reaction :D

[@josephberto5106]

the copper looked amazing! with the gas wow!

[@maryudomah4387]

The thumbnail looked like Saturn or Jupiter... Cooooooooool

[@annelieseocallaghan801]

Wow, I agree!

[@BanilyaGorilya]

We use it in lithography to etch stones and in Intaglio to etch copper plates.

[@annelieseocallaghan801]

Interesting, thanks!

[@williamjemeyson6983]

I play your videos every morning drive to work. It’s how I ease my nerves.

[@iv3game]

The revival petrifition fluid!!!!

[@praspurgh]

in the end, I was expecting "again, here's a list of videos that I'm currently editing and list of videos that I plan to film..."

[@xd1712]

man the glassmakers making all these different flasks/jars/distillators in one continous glass piece amaze me.

[@animebloodkurenai1997]

Yup Dr. Stone😂

[@robertgaudet7407]

Been experimenting with ammonium nitrate, as far as I can tell it doesn't react with high concentration sulphuric acid at low temperatures ~0 C, while potassium nitrate does.

[@prinzeugenvansovoyen732]

How abaut TNT?

[@fudes587]

@@prinzeugenvansovoyen732 tnt is overrated

[@chemistryofquestionablequa6252]

@@fudes587yep, awkward to make in small amounts and the nitration is long and can be dangerous. Good for melt casting with nitroguanidine compounds to increase density though.

[@tomlutman2041]

After doing this last night, I can add one thing. Run a vacuum. I used a cheap vacuum into a trap with some hydrogen peroxide in it expecting some NO2 gas. I had none. My initial reaction came out crystal clear, and the temp required was lower (of course). I got a 37% HNO3 out of the reaction. I started to distill (fractional) again using vacuum getting a bunch of water around 72c. I didn't get to finish it out before I had to pack it up, but again, no NO2 and I'm up to 47%.

[@jhyland87]

The flask in the thumbnail kinda looks like a picture of Jupiter, with the multiple phases in Juputer-ish colors.

[@somerandomhuman1234]

1 experiment is better than 100 theoretical explainations, I missed these in my childhood.

[@hellon203]

If you are doing this without lab equipment simply take your weak nitric acid and run it again perhaps again after that. Not the most efficient way to do it but each time the nitric acid will get more concentrated. It is about maximizing the contact between the nitric oxide and hydrogen peroxide. It will be less as effective each time though. Use a narrow pvc tube perhaps 1/4”. This will cause more bubbles agitating the hydrogen peroxide causing more contact. Use a narrow container too. The more narrow and tall the better. This will allow the nitric oxide to travel further before reaching the top releasing into the air. Plug the top of your container loosely to to semi vent it. This will allow a reaction to occur on the surface with the nitric dioxide that has been released. For some reason an ice bath also creates a better reaction.

[@ayshamelia4145]

pls make more content, i literally can't sleep without listening to a nile red video and i almost know them off by heart 😂 love your content!!!!!!

[@XXXXXXVIVI]

I dig that higher mic quality lately.

[@Mohamm3dAlObaidi]

When I saw the thumbnail, I thought he made Jupiter in a flask.

[@angusfulton1622]

Important about fractional distillation with a vigreux column! Only insulate if your desired product is the final known component and aluminum foil is not efficient insulation. Always use a combination of wool wrapped in foil

[@LaHayeSaint]

Use mineral wool ONLY and not cotton wool, which could lead to explosion.

[@scottnation5685]

I think it's his voice, it's calming.

[@Peaserist]

If you have Sodium Nitrate, NaNO3, aka Chilean Saltpeter, you can use 339g of it in place of 404g KNO3 or 320g NH4NO3, because each of these have almost exactly 247.5g of NO3 Ions by weight

[@ajingolk7716]

NH4NO3 + H2SO4 =🎉

[@RobinMartensson]

Love these videos. Inspiring me for my job as science teacher. I wonder, why did you not just end the final fractional destillation once the water had come over? Where there not only aesotrophic HNO3 left? Greetings from Robin, Sweden.

[@PaulSteMarie]

I'm surprised that you aren't getting sulfuric acid from a car parts store. NAPA carries it for car batteries.

[@edisonkelly2729]

Senku's guide to making revival fluid

[@aiden4163]

Not many dr stone comments

[@Methylenedream]

Thank you Nitric Acid for my yellow fingers.

[@akhilthechemist]

MDMA4LIFE ya that sucks nitric acid had stained my thumb yellow for almost a weak . When I put a moist thumb on a test tube evolving HNO3 vapours . That is a very bad test for NO3- ions😢😢

[@LaHayeSaint]

You should be wearing protective gloves when handling concentrated nitric acid. It is dangerous to nitrate your skin.

[@Methylenedream]

@@LaHayeSaint Thank you master of 5 years late and probably never worked in a lab in your entire life.

[@LaHayeSaint]

@@Methylenedream Are you attempting to be facetious? Please do not presume to know my academic background. What is your explanation?

[@Methylenedream]

@@LaHayeSaint You are a loser who replies to 5 year old threads, that is my 'explanation'.

[@NvrchFotia]

The acid i buy is bright pink. It looks exactly like pink gatorade. I'm suprised they color it that way.

[@jonasstrzyz2469]

I like the NO3- group, but Cu beats you in its beautiful complexes, Schweitzer's reagent. =D

[@NvrchFotia]

Jonas Strzyz Why not both? Copper nitrate is pretty, and it's used in the synthesis of RDX.

[@jonasstrzyz2469]

Both, but Copper(II)acetate is like blue/green permanganate... so in terms of beauty and not to forget Schweitzer's reagent, (dissolve cotton) good prank. I general, nitrogen is an amazing element, but Copper is a very aesthetically element and forms beautiful complexes, CuSO4 + 4 NH3. I do fancy the nitrate group in terms of its explosive potential, absolutely amazing how it blows you away and then liquid nitrogen, nice stuff.

[@IIHawkGamingII]

You can also just use battery acid, no organic inhibitors and generally cheeper at hardware stores. Typically 80% and up too.

[@uslph.]

that's sulfuric acid

[@brianrigsby7900]

I have a request that I bet others will enjoy. Can u slowmo the stirring when something gets added in flasks? I don’t know y, but watching whirlpools is so satisfying 2 me

[@BlueMoonshine]

Why do you add water to the potassium nitrate and sulfuric acid? If you don't, you will produce nitric acid that has a concentration near 95%, with a simple distillation. You can dilute it after, if you need to.

[@applepie6470]

YESSS NEW VID!!

[@eternallag]

When doing a distillation up to an azeotrope, why do you switch to a collection flask once you think you've hit the azeotrope? Wouldn't the boiler and every stage of the column be your product at that point? Other than that: great video. I know this is pretty old but I've been binging your videos and your channel is great. Keep it up.

[@LiborTinka]

Purity. There would be a small amount of sulfuric acid and other reagents if you keep product at that stage. But depending on application that might be sufficient. Once the flask is heated up it does not take that much energy to just let it to distill. It costs mostly time.

[@spicychickennuggett1763]

you should do this using the Ostwald Process

[@floppa24]

8:41 *angry Explosions & Fire noises*

[@belrestro]

every nileRed is masterpiece

[@wyldeman0O7]

Thumbnail looks like Jupiter :P

[@muathi6928]

thank you so much. Your videos really make me want to get into chemistry.

[@BruceBoppoTiemann]

8:18 "Once only a very small amount of distillate is left" - I think you mean still residue here, i.e. in the originating flask, rather than in the receiving flask.

[@tylertaylor7237]

I know somewhere he talks about helping put kits together. Im mostly interested in nitriting and recover

[@nancypagan6878]

It can also be used as plant fertilizer.

[@Citizen-of-theworld]

You should get a pycnometer for measuring density. They are pretty cheap and can be very accurate.

[@joeestes8114]

its great to revisit this!

[@burntorangeak]

Could be noted that nitrogen dioxide is one of the principal compounds that give photochemical smog over large cities it's reddish hazy color.

[@ZaphiraK]

these videos always makes me curious if these things happen naturally on some other planets

[@137bob3d]

williamson's book on 'organic experiments' , 3'd ed. in Chap. 5 mentions a distillation packing material for a column called 'copper sponge (Chore Boy is its commercial name ). its surface area adds many many more equilibrium stages to the distilling process for more refined separation and your demo with the penny woke me up to the fact that distilling azeo' HNO3 would not be a suitable application for any of this copper sponge material.

[@prinzeugenvansovoyen732]

apparently this makes nitroglycerine if you mix it with hand sanetizer, also interesting, if yo uget that ieven in traces on your skin and go to a airport within 4 days of that mishap you can very well end on a no fly list and get the Men in Black to visit your home

[@dudeistpriest787]

I have a funny feeling that winding up on a no fly list is one of the least unfortunate outcomes of accidentally making nitroglycerin.

[@ta6576]

Do you ever make stuff that is destructive to the glassware, stir bar, or other equipment that you use?

[@Lunchpacked180]

9:37 Nice!

[@bormisha]

This is the reaction performed by Jules Verne in his "Mysterious island"! There, Cyrus Smith turned sulfuric acid and a nitrate into the nitric acid.

[@formdoggie5]

Wouldn't the yellow be from sulfur contamination? Nitrogen contamination would be blue, wouldn't it?

[@dROcITYkING11]

Another top notch vid 👨🏻‍🔬👨🏻‍🏫👍👍

[@fullsolutionslab]

Hi Nile! Why do you dont tell them how to make 99.9% Nitric acid? It's simple: Just take your obtained 68% Nitric acid and mix it with 98% Sulphuric acid (2:1) and do a simple destilation as shon in your movie. Then repeat this step and tadaaaa...: 99.9% Nitric acid. To explain it in a (very) simple way: the sulphuric acid "steal" and keeps the water from the nitric acid while the nitric acid distill's off. But nice movie and perfectly explained! :-) Kind regards and have a nice day

[@NileRed]

+swim hive Very true. The reason I didnt make 99% is because I needed to make 68% for my nitration of mercury. The super high concentration would actually make the reaction a little more dangerous.

[@amidfallen]

What about adding CaCl2 or some drying agent to the 68% acid in order to obtain higher concentration, will it work?

[@shoutitallloud]

@@amidfallen I guess it won't

[@summeronio9751]

Glanced at the thumbnail, thought it was Jupiter. Clicked, pleasant surprise

[@Commodore1702]

According to page 14 of US TM 31-210 you can get sulfuric acid by boiling the electrolyte from a car battery until white fumes appear as well. This is definitely a much cleaner and probably better way though, as the manual focuses on improvised means, not lab methods.

[@leyre4439]

You're right. You could do that. The problem is cost. Hardware store sulfuric acid drain cleaner comes at azeotrope in my neck of the woods and I pay about 20 USD per gallon. A battery costs about 1-200 USD and yields much less at much less concentration. But in a pinch you could do that.

[@Rhodanide]

YO 300g MERCURY THIOCYANATE??! IM PUMPED!!! :D

[@mattibboss]

it's overkill....he had a lot of fun cleaning up... but we'll have fun watching that video :D

[@Rhodanide]

mattibboss Hell yeah lol

[@rafaelpatriciodasilva2187]

Nilered,por favor dá um video ensinando a sintetizar ácido sulfônico,amida 60 e lauril éter sulfato de sódio

[@joshborchardt5050]

I cuss like a sailor and I very much appreciate the cleanliness of language that Nilered always attains.

[@scubadave4220]

How to get a meeting with homeland security.

[@iamzid]

man the more i look into making ammonia nitrate the more i'm starting to think that it'd be easier to buy bags of fertilizer and try washing it out with methanol. it seems like only half of the ingredients used to make it from scratch are easy to get.

[@alish5417]

Im obsessed with SOX SO2 SO3 GASSES THESE DAYS.

[@coraliacries4209]

ah yes DR.Stone research here i come

[@liamcg2521]

this might be a dumb question but why not just use the vigreux collumn in the first distillation instead of doing a second one

[@backtrack5pro]

you should make a video about your home lab. I'm thinking of making one myself. Love the vids btw

[@akhilthechemist]

backtrack5_pro I have made on my channel

[@stephenjacks8196]

Anhydrous Barium Nitrate (Calcium Nitrate works) and xs Sulfuric Acid. HNO3 in H2SO4.

[@Prototype5151]

Fantastic video man!! I'd love to see the new Pharaoh's serpent on a large scale.

[@keithmorrison6176]

I like your videos, well explained and not like some that rambles on. keep up the good work.

[@edwhitson9873]

I've always heard there I concentration of gold in quartz that can be easily and effectively extracted with nitric acid

[@christopherbutler8176]

Is it possible to omit the water in order to purify the nitrate acid without fractional distillation

[@mattm3492]

It's weird, I've watched almost all your videos and this is the only place I don't scan comments while watching. Not sure why but it seems to always be that way

[@ethanrimelman9224]

probably because his videos make you think hard and learn, the opposite of what surrounds youtube comments

[@raymondreyes8046]

Can you make a video of setting up the the chemistry apparatus? What I mean is, where things go, why they are there? Heat? Cold? What are those hoses for? How hot does the solution need to be? Best way to heat it? What kinds of equipment should one upgrade to? Like do some of these pieces not stand up to the acids?

[@spaceyboi6651]

Maybe you should try to make a video about titration? This way we can use more dilute solutions of unknown concentration

[@NileRed]

+Janusz Januszowski I should. I just have kind of an aversion to titrations though for some reason. I find them very boring.

[@spaceyboi6651]

+Nile Red yeah they are boring but pretty useful

[@NileRed]

Janusz Januszowski haha very very useful.

[@spaceyboi6651]

+Nile Red And youre making technique series soo it will fit there

[@levi4979]

Well I'm on a watch list now lol.

[@rhyscentin6399]

“Concentrated” *laughs in red fuming nitric acid*

[@GeneralSulla]

Back in my day, you could go to a scientific glass production company and buy any and all extra glassware/apparatus they had on hand that wasn't selling. Not so today.

[@kevinburns8473]

Yer' a wizard, Nile!

[@kurokaminari4566]

This is the new gen asmr

[@graceofbaal]

Why not just use the Vigreux column with the original reaction mixture? Should work the same, and would save on the second distillation.

[@LiborTinka]

Not really. In the first distillation, I found the vapour temperature is about 120° C all the time, so what comes over is almost azeotropic nitric acid with some water. If fractional column has been used, more and more water would go back to the reaction mixture instead of being removed and this would prolong the whole process, maybe promoting decomposition of the nitric acid and lowering yield. In the two-step process, the near-azeotropic nitric acid is distilled off the reaction mixture first, then the bulk of the water is separated in short time. The product is also much cleaner that way.

[@SuperAngelofglory]

@@LiborTinka plus refluxing water over a boiling mixture that contains concentrated H2SO4 can't be a very good idea

[@um999out6]

Hey Nile!! Huge fan here!! Are you canadian by any chance?? french writing on your sulfuric acid bottle gave it away... where from? quebec city here

[@dtiydr]

If he would have made TNT you can bet it would have been taken down before he even put it up.

[@justcause3844]

I read that the density of 68% Nitric Acid solution is about 1.504g/mL. With that in mind, and your yield of 134mL, you should have 68% of 1.504g*134mL. This would mean you have 201.536g of 68% Nitric acid. Breaking it down further, the solution contains 137.04g of HNO3. The perfect yield, by stoichiometric conversion, is 251.8g. This means that 114.8g of Nitric acid were lost, likely in the weak solution among other things. I am not trying to demean you, just trying to figure out why so much was lost, because I personally don't know. Your yield was 54% of a perfect yield. Do you have an explanation of how that may have happened, or maybe I did something wrong in my calculations? Thanks

[@michaelchauncey6806]

you mentioned making 100 percent h2so4. I would like to see that. though I don't know what to use it for. we have done fuming hno3. so here is a good challenge

[@madmattdigs9518]

Why add the water in the first place? If there’s no water, or very little, you can distill a higher concentration nitric acid. I guess, as you said, you wanted to get azeotropic nitric acid, but I don’t understand the point of adding water in the beginning, then doing the fractional distillation. You can make a concentrated acid, then dilute to the concentration you want.

[@turelish3408]

We need a collab here! Nile red and Doug's lab or Nile red and Nurd rage! It needs to happen! Maybe you could both work on the vanillyl amine and capsaicin reactions ^^

[@NileRed]

+TU Relish Once we finally are able to make vanillylamine we can start thinking of capsaicinoids! The amine is being a pain to make. A collab should happen. The only issue is that we all live pretty far away from each other. So it would all have to be done over the internet, which is not ideal.

[@michaelchauncey6806]

you mentioned making 100 percent h2so4. I would like to see that. though I don't know what to use it for. we have done fuming hno3. so here is a good challenge

[@michaelchauncey6806]

can you dehydrate HCl or hno3 too? like with molecular sieves or reg drying agent and distill?

[@keshavmurali98]

That would be Oleum though.

[@jonasstrzyz2469]

Try dehydrating, HCL with Calcium(II)Chloride.

[@jonhoyles714]

I thought u needed copper for this reaction unless for generating the gas maybe yep most likely :) great vid

[@scienceteam9254]

OHAYOU SEKAI GOOD MORNING WOOOOOOORLD!!!!!!!!

[@moonlight_5836]

HOW LONG HAVE I BEEN WALIKNG

[@BlurredTheLines]

I scrolled down hoping someone made a dr stone reference. I was not disappointed

[@rvlifestylelivin]

curious is water vaporizes at 100c and nitric acid at 120c couldn't you just heat the solution to 100c and distill the water out leaving behind more pure nitric acid?

[@LuckyS4tyr]

0:49 “ i dont plan on making any explosions” Years later…

[@janszreniawski]

Bring it up by one, so it's nice.

[@LA_Viking]

I would like to add a probably unnecessary warning here. The narrator of this video appears to be very good at what he does. As a result, the process looks far easier than it actually is. Add to this the fact that he is employing professional grade laboratory equipment...it’s the first time I’ve seen anyone using a heating mantle on KZbin. This equipment is very expensive and may be hard to locate and procure. Even matching the sizes of the slip fit components can be confusing. As far as manufacturing explosives...well, unless you are very well versed in lab procedures and are accustomed to working in a lab, don’t even consider it. I’m a FBI/US Army-trained Hazardous Devices Technician, worked as a weapons and explosives safety officer for a defense contractor, and formerly held state and federal licenses to manufacture high explosives. I’ve got a lot of training and experience. Having said that, I would be quite reluctant to engage in any such activity without a significant amount of very expensive preparation. Good luck!