Elementary Productions: Concentrating Nitric acid

[floortrader60]

During the second distillation under a vacuum, where is the dissolved nitrogen dioxide after it is taken out of the nitric acid?

[floortrader60]

Why couldn't you distill under a vacuum during the first distillation? Lower temps would decrease the decomposition of the nitric acid.

[4johnybravo]

yeah what is the ratio of nitric to sulfuric you used?

[MrBaadpyro]

hvor mye vann tar 100ml H2SO4 opp ?

Jeg skal destillere fra 62 % HNO3

Takk for svar

[nickalisse1]

It's been a while since we talked! N vids are great as I remembered. As for this one, could u remind us the ratios, for a good distillation rate??

[crapbag1997]

could i use this method to further concentrate 90% nitric acid and would ther be any changes or could i just do the same thing

[g3ov4n12]

You need to add boiling chips.

[giorulesallofu]

@mabakken How did you know how much H2SO4 to add?

[membola]

nice video! i just got 25% nitric (highest i seem to be able to get) and want to make aqua regia to dissolve gold, i will try this, only thing is my sulphuric is only about 20%, do you think that would work or would there be too much water for it to suck out the water from the hno3 and give it a desired azeotropic phase?

[CHEMIST674]

Hie mabakken! I just wanted to ask u a question-what r the ratios which i can use for H2SO4 and HNO3?

[334683171014]

@CHEMIST674 This is my guess, say you have 70% nitric acid and you have 500ml of it that you are wanting to distill. Just add 1000 ml of 98% sulfuric acid. So just add twice as much sulfuric acid as the nitric acid.

[dd3121]

Great Video! I hope people would start appreciating this series of videos for the science behind it. Mabakken is a great chemist who knows what he is doing and he demonstrates all these important reactions. reactions we would not see otherwise, and we start talking about bombs or try to make ourselves look smart by pointing out our misunderstanding from Chem 100 in college.

As for me, I am grateful to see all these reactions I know from theory actually occurring, and it is a great pleasure.

[knackersau]

Hi mabakken, thank you for sharing your expertise with us, could you please inform me as to, "during the first distilation is the apparatus sealed ? and secondly is the vaccum tube plastic ? Thanks again

[starshock01]

i dont know why...but i find this video very relaxing...despite the fact its a very toxic and strong acid...

[imzeinternet]

* tries breathing nitrogen dioxide* *dies*

[hkparker]

Thanks for the guide, I recently bought 70% nitric acid and ill probably be using this method to make some 99% like what I made by the distillation of sodium nitrate and sulfuric acid.

[Bilbo940]

What is the percentage yield of this ^^?

Sorry if this question has been asked b4.

[vitorix24]

100% ?? are you fool? its 99.999999999999999999999999999­99999% 

[TheGeorges123]

Awesome man ! but I have a question.When we r making Nitric acid by adding a nitrate salt to concentrated sulfuric acid and distilling the solution what's the concentration(%) of Nitric acid ? isn't 95 % ?

[elbsenk]

where did you buy your distilling apparatus and for about how much?

[hobomnky]

that was great!

i wish u put a penny in there would have love to see how 99% reacts with copper

[ervali9]

@hobomnky watch nurdrages video to see..

[endimion17]

Great video, I'm planning to repeat the same stuff, as I have some old but reagent grade nitric acid lying around.

What was the efficiency of the whole procedure? Is the thermometer really necessary? I've got one for the whole setup, but it has no glass joint. I have to use plastic screw with silicone-teflon seal, and I have no idea what will happen. Teflon coating is ok, but the rest, and especially the plastic, could be damaged if anything this hot and reactive leaks beyond the thin coating.

[KrimeMater]

This solution if on your skin can easily melt you right?

[TheMaDMAli]

you can not obtain 100% nitric acid with fractional distillation let alone simple distillation, nitric acid froms a very strong azeotrope with water, and the yellow you see is disolved nitrogen dioxide from when the nitric acid decomposed from distiallation.

[Viking0fNorway]

Mener å huske at om du tilsetter ett gram eller to mer ureanitrat i tillegg til HNO3 og H2SO4, vil du få mye renere produkt (tenker på NOx) ved første dest.

Flotte videoer!

Peace Out!

[darrylportelli]

nice apparatus!!!!

to determine purity, its better to titrate against a standard solution (this takes time!!! but you will know the exact molarity of the acid)

10x for the synthesis...all of them are good....

can you try the extraction of white phosphorous from urine....I know its not exactly sanitary but for white phosphorous I think its worth it...If you do a vid of and it works it I will definately give it a go!!!

[starshock01]

because 65% wasnt dangerous enough...you had to have fuming lol

[blueduderanch]

in your second distillation your clamp stand bases were facing the wrong way. you also didnt add antibumping granuels so it didnt bubble continuously.

[magget16]

What do you have to do with the water aspirator, just attatch? or release/close any valves, keep it dipped in water etc..

[kmncztms]

Sry, i dont know the name of chimical stuffs in english, but this nitric acid is HNO3, isn't it?

[surplusdriller]

da er det bare å koke svovelsyren å bruke den igjenn??

[TinyCoconut]

Nice analytical scale.

Fuck yea, 4 decimal places

[lithiumw]

this is not analytical :)

[TinyCoconut]

A scale (or balance) that can read to 4 gram decimals is called an analytical balance.

They tend to be among of the most expensive pieces of standard equipment in a lab.

[lithiumw]

ok

In my lab, this is not called an analytical scale ^^

the analytical scales: 0.0001g

to 0.0000001g

[lewisvz]

thanks this video had some cool sound effects that i can use to make video games :)

[CarnalDiafragma]

Have you ever made concentrated nitric acid by dissolving dilute nitric acid in dichloromethane? I don't know exactly how this works :P Great video!

[hiperion421]

nice ty

[pbbehv]

HCl = gas in pure form..

[antiswattt2]

what about concentrated HCl, H2SO4 and HNO3? :D

[Mensch135]

I already made nitric acid from potassium nitrate and sulphuric acid. Now I want to concentrate my 53% nitric acid.

What ratio of HNO3/H2SO4 did you use?

Your videos are great!

[liquidgrain]

Are you using a fractionating column? I would like to reproduce this however I don't have one myself and I am wondering if it is neccecery for the separation. Additionaly I'm not sure if there is a reaction here, the HNO3 and H2SO4 do not react under regular cercumstances(not sure about elevated tempertures though).

[donnelrj01]

You've probably already had a reply.

However, a fractionating column is not needed for this. That's because you want the vapor to leave the flask as soon as possible to avoid further decomposition.

With a column, the acid will condense and reflux back into the flask meaning you'll only obtain a small amount of the acid. H2SO4 breaks the azeotrope between HNO3 and water.

[itsumonihon]

in fact if i remember right that may have been how mercury fulminate was discovered. the miners used mercury to help trap small particles of gold, then would introduce some nitric acid which would dissolve the mercury but leave the gold. depending on the conditions (i.e. if he screwed up) the miner would be left with fulminate of mercury or fulminate of gold.

[hardhitman69]

Making mercury fulminate is a little bit more complex than just adding nitric acid to mercury

[felizgar]

What other uses has nitric acid besides making bombs? Everytime I ask, everyone wants to look cool or someting and brags about bombs. In what was used before bombs?

[isthisnameavailable]

Rocket fuel. Check out the BI-1 Rocket built by the Russians during WWII. It used Nitric Acid and tractor Kerosene as it's propellant.

[itsumonihon]

gold mining uses nitric acid

[thesinner85]

For hobbyist's, there's probably not much else use for it, aside from clandestine methods of making bombs and drugs.

It' has a lot of use in the metal finishing industry. If your silverware (stainless steel) starts to rust, dipping in nitric will clean it in a matter of seconds.

[RicardoGarciaPino]

i would gess nitrogen dioxide would not precipitate from the distill, but this will make less nitric acid from the total absolute weigth of nitric acid in the first mix?

[zcuttlefish]

It would be pretty easy to confirm with a titration using phenolphthalein (and a bit of NaOH). lol how much did your setup cost? My guess $200-250 for condenser setup. Am i close?

[TheFluorineMartyr]

Mabakken.... you are a genius - I'm sure you're aware.

So you've done it! WFNA. So? Have you tried RDX yet? ^^

[46Palladium106]

What's the ratio between the added nitric and sulfuric acid?

[thejanitor99]

As many moles H2SO4 as there are H2O perhaps?

[badgoodtalker]

WOW! also were do I get muriatic acid hydrochloric acid ( 10-12% pecent acid) I also found out that the skin is strong enough to withstand hydrochloric acid (muriatic) because of the proteins

[starshock01]

muriatic acid can be picked up at any hardware store for 6-8 usd's a gallon, but the concentration is usually around 31-40% for safety reasons

[Peterditaa]

hydrochloric acid cant have more than 37,6 % cause its the maximal volume of HCL gas dissolving in water.

the low concentrated hcl is like 24-25 percent you can get it at any good hardwarestore

[starshock01]

thats just what's labelled on the bottle...but im sure the bottle i have now says 31 percent...

[hardhitman69]

I got 35% from a hardware store, its used for pools and cleaning concrete.

[donnelrj01]

You mean HCL.

[siliciumsilicium]

yap nitric acid react with plastic. I had some silicon on the glass and it turnd brown-red. What is it? Silicon polinitrat? is it an explosive-energetic material?

[xXKentoXx]

Where do you buy all these item

[Sebbass69]

wouldn't the NO2 gases released, and even some of the HNO3 ruin the vacuum pump?

[sockpuppetsfromhell]

You should do a video showing people how to make fuming nitric acid from the distillation of sulfuric acid in the presence of potassium nitrate. It's an easy and quite useful synthesis.

[AlchemistShaman]

Why did you set the heating mantle to max when nitric acid begins to decompose at just 140°F?

[AlchemistShaman]

How come you didn't just make the nitric acid from potassium nitrate by dissolving it in the sulfuric acid and condensing the gas released?

[sockpuppetsfromhell]

That's what I was thinking. It's a simple reaction and I got fuming grade nitric directly from it.

[MariusSemeonOrtiz]

Really good video - 5 starts. Shame i can't even hope to ever get all that sophisticated equipment....

[endr117]

bravo. my only criticism is that none of the text shows up for very long.

[mabakken]

Thank you, and I know =)

I based the duration of the text on how fast I read it. =)

[AlchemistShaman]

Windows movie maker automatically sets the length of the time the text remains on screen based on the average reading speed, computed with how many words are in the message

[darrylportelli]

@mabakken so you are using H2SO4 as a drying agent?? usually P4O10 is used to dry the azeotrope

[bfesser]

@endr117 Use the pause option!

[peterzembeik]

I was made nitric acid by melting sulfuric acid with potassium nitrate but I don't know the concentration of nitric acid.can you tell me the concentration of nitric acid.can i concetrate nitric acid without vakum pump.

[tkurtis20111]

i don't think you need a vakum pump to concentrate it. if you have a distilling kit that would work just fine, just reheat and reheat and it shuld become more concentrated.

[peterzembeik]

But what did you think?Can i make white nitric acid when i melt potassium nitrate and sulfuric acid without wakum pump.I only get red nitric acid full with NO2 gases.

[evsonjunior]

I would like to know how do I do to concentrate the sulfuric acid, as a azeotrope can not be distilled, What can I use to break this azeotrope, or if you have another method of concentration is just tell me. please reply. thanks

[reza360]

Hi again,

let me know about the pressure of vacuum pump and the temperature of mixture when you used vacuum pump

[HumanNitrate]

oh OK thanks. for some reason i thought the ammonia gas would cause a problem. I'm going to try it with a retort (for convenience). :)

[HumanNitrate]

would ammonium nitrate work?

[mabakken]

What do you mean?

Ammonium Nitrate by itself will form Nitrous Oxide gas and water. If you mix the ammonium nitrate with sulfuric acid and then do the distillation, it will form Nitric acid =)

[reza360]

Hi mate,

thanks for your clip:)

I have two question:

1- let me know about the pressure of vacume pump

2- the temperature of the mixture when you used the vacume pump

cheers

[salut151]

Are you aware that your thermometer is not positioned properly ? I just want to let you know. Good video.

[mabakken]

Yes I know, but only by a couple of centimetres. Also, It reads a temperature higher than that of the actual one, which is a good thing when one wants to limit thermal decomposition.

But yes, you are absolutely right!! =)

[nixrate]

heard u can use small amounts of urea and dried air to remove nitrous oxides.

[b43e65f77]

Can I use NaNO3 react with sulfuric acid to make nearly 100% Nitric acid?

[mabakken]

First of all: very sorry for late reply!

Yes you can use Sodium Nitrate...any nitrate works (as long as it's soluble) :)

[b43e65f77]

thx,I will do that later.I have no vacuum device,so I will add a little hydrogen peroxide or potassium persulfate to prevent NOx formation,do you think it is work or not?

[jmrdelorean]

Though I think it would work for Gunpoweder better.

[johancs7]

Nice Vid!

[mabakken]

No worries =)

The round- bottomed flask is 250 ml, yes.

The Liebig condenser is 35 cm long (I think) =)

[mabakken]

The disclaimer is implied in all of my videos, as I do not include any specifics.

If one were to replicate the experiment, I could not be held responsible if anything goes wrong, because the specifics are not the same as mine.

Almost every chemical known are becoming illegal or controlled in the US. As for where I am from, Norway, all of the chemicals used in this video can be bought at the local hardware- store.

Besides...SOMEONE needs to post the videos that others cant't =)

[darkcurrent]

I'm amazed/surprised at your lax chemical laws in norway. Isn't the norway gov. afraid of homemade bombs or drugs? Liquid ecstasy (GHB) and barbiturates and methamphetamine (huge problem in the states) are easily made with precursors.

Anyways, good luck in making more vids.

[mabakken]

The way I see it, every other country than the US have laxed laws concerning chemicals and drugs. I like to call it an understandable shame!

[FP791]

Did you put any boiling stones in?

[zasx20]

could you do the same with other acids? such as sulphuric acid or hydrochlorine?

[FP791]

stop trying to make explosives.

amateur.

[waketlanceewdew]

What ratio of HNO3 65% and H2SO4 did you use?

[zasx20]

could you do the same with other acids? such as sulphuric acid or hydrochlorine?

[mabakken]

A long time...in the range of hours! =)

[Fentanyl3]

why not distill it the first time under vacuum?

also, how corrosive are the vapors being pulled though the pump? I have a rotary vane vacuum pump very similar to yours, but it's actually meant for evacuating auto AC's which HCL can and is created in wet AC systems it's not nearly as strong as whats being condensed here, i'm just wondering if I am going to seriously shorten my pumps life

[zasx20]

hey i have a quick question could you condence other acids in the same way like hydrochoric acid or sulphuric acid?

[CarefaceProduction]

Hei

Hva er forskjellen på å bruke en vigreuxkolonne og et reduksjonsadapter??

Brukte du forresten sånn "voks" når du monterte opp settet for å forhindre "frysning"??

Veldig interessant video forresten:P

[mabakken]

Heisann.

En vigreux- kolonne brukes som regel under reflux distillering, og er en slags condenser.

En reduksjonsadapter er bare en del av et distillerings utstyr som brukes til å sette delene sammen. Ikke alle delene har samme størrelse, og ved hjelp av adapteren, kan utstyret kobles sammen.

Jeg bruker en silikon- basert smøring for å forsikre at utstyret er tett. =)

[Loeffelstiel90]

i thought, royal water is HCl and H2SO4 not HNO3 and HClO4

[mabakken]

Royal water is HCl and HNO3 =)

[v3user810]

Royal water= 1part HNO3  + 3parts HCl

[Pyrotrons]

How did you weigh the acid with enough resolution to determine that you had a concentration of 99%?

[flach99]

Is it possible to clean the NOx with dry ice? I saw that 'bublers are used to clean, so i thought it could be possible.

[mabakken]

I'm sorry, I don't see how that can be done. Could you elaborate, please?

[flach99]

i read that NOx is cleaned out by letting bubbles trough the acid. somehow (i do not really know that part) the NOx escapes trough (or with) the bubbles as gas. So, is it posssible to use dry ice for such a bubbling?

in an industrial rate the nitric is falling trough a tower and it is cleaned by the same! nitric acid! going (fuming maybe) the opposite way.

[mabakken]

Oh I see! It sounds plausible, as NOx are very soluble in both water and Nitric acid. Only thing with Dry Ice is that you will have carbonate ions floating around. As some carbonates are insoluble, this could inhibit the Nitric acid's use in a synthesis, for example.

[mabakken]

Again, use goggles and gloves. Do not get any on your skin. If you do, do not rinse with water: sprinkle Sodium Bicarbonate on it. (small spills on skin can be rinsed with water). Generally: be very careful, and take the precautions you find necessary.

[mabakken]

Use goggles and gloves. One piece at a time. Avoid any spills, especially on skin. Wash thoroughly.

[smiles76239]

Could you please tell me the name of the company that you got your distillation apparatus from, or did you buy it piece by piece.

[y2k042000]

my quickfit just can't completely air-tight..what shall I do? Grease will react with nitric acid..

[mabakken]

Depends on what type of grease. Get yourself some purely Silicone based grease, and you should be OK. Also, Teflon tape works wonders. :)

[adyzal]

where do you buy those chemical..?

[mabakken]

From a norwegian supplier of chemicals.

[cyanide444]

Would you mind telling me thse companies?

[FideliBomBom]

Bra video:)

Kjøpte du forresten dette settet på kptnaturfag?

Så at de selgte et sett som lignet veldig på ditt...

[mabakken]

Jo tusen takk :)

Jeg tror jeg kjøpte dette settet fra KPT, ja.

[slither888]

To clarify, I mean do you think that because I use water to generate the vacuum that somehow the acid will absorb this through the air?

[mabakken]

To create a vacuum, the distillation equipment needs to be airtight anyway, so no moisture will enter.

[slither888]

Excellent video, I'm glad someone finally demonstrated the right way to do a NA distillation and concentration. Did you work in a professional lab to do this because it sure looked like it with the heating mantle and vacuum pump. Do you think it will work with a hydro-aspirator?

[mabakken]

Thank you very much :)

No, I don't work in a lab; I did this at home.

It will most certainly work with an aspirator, but the pressure does not get quite as low, so I would heat the Nitric acid very carefully.

[cyanide444]

Where do you buy the respirator and the apparautus...isn't it expensive?

[mabakken]

I'm sorry, I don't know what you mean by "respirator".

The rest of the apparatus is bought off of a norwegian supplier of laboratory glassware. It's not extremely expensive, but it's not cheap either ;)

[cyanide444]

The gas mask...I don't know what else to call it. Do these suppliers ship to the states or india?

[Marcooftw]

I'd say concentration of nitric acid could be done much easier. The problem with this method is, that water is formed, which is hard to separate from the nitric acid.

Instead nitric acid could be made by pouring concentrated sulfuric over for instance KNO3.

The the following reaction would occur:

H2SO4(aq) + 2 KNO3(s) -> 2 HNO3(g) + K2SO4(s)

Benefit of this method is of course, that no water is produced.

[mabakken]

I agree on what you're saying, although what you're saying is not completely correct.

In my video I purify Nitric acid. In your suggested procedure, Nitric acid is synthesized. Also, no water is formed as there is no chemical reaction occuring, not taking into consideration the decomposition of the Nitric acid. In the second stage of the purification (under vacuum), virtually no decomposition takes place.

Also, potassium bisulfate is formed, not Potassium sulfate :)

[y2k0420000]

Isn't the experment can be done by distialling

the mix-acid under vacuum?

[mabakken]

Yes, it can be done, but then the distillate will become much less pure due to Sulfur compounds.

[y2k042000]

what pressure is need?

[y2k042000]

and no granules is need?

[mabakken]

I am uncertain what pressure is needed. It all depends on how pure you want the Nitric acid, and I didn't have a pressure- gauge at that time.

What do you mean "granules"? Do you mean activated carbon?

[y2k042000]

oh.I mean the anti-bumping granules. And it's necessary to clean the nitric acid steam before it enters the vacuum pump?

[mabakken]

Anti- bumping granules is not very necessary, but could be added to ensure a more even boiling.

The distillation apparatus is evacuated before the heat is turned on, so there is not much Nitric Acid vapor going through the vacuum pump. One could add a gas- wash- bottle to the apparatues to minimize Nitric Acid steam to reach the vacuum pump, but this is also not necessary! If you don't have fume hood or a source for the exhaust air from the vacuum pump to be removed, this should be done! :)

[floke5]

AWESOME! dude this was like the coolest video i have ever seen! i just wish i was alot smarter to understand Chemistry lol

[mabakken]

hehe. Very good to hear!! You know, it's never too late to learn ;)

[Basco36]

what is the ratio of nitric to sulfuric?

[mabakken]

Sulfuric acid: Nitric acid -- 2:1

[Basco36]

Do you know what compound of gold is formed when you dissolve gold in aqua regia?

[mabakken]

That would be Gold Chloride (Auric chloride AuCl3)

[Basco36]

but what happend to the nitric acid? it wouldn't be gold nitrate?

[mabakken]

The Nitric acid oxidises the gold, but in extremely low amounts. It is here the chloride ions come in, because they take the place of the Nitrate ions, allowing for further oxidation of the Nitrate ions. The chloride and nitrate ions work together, which is why neither acid will dissolve gold on its own! =)

Respective equations:

Au (s) + 3 NO3- (aq) + 6 H+ (aq) → Au3+ (aq) + 3 NO2 (g) + 3 H2O (l)

Au3+ (aq) + 4 Cl- (aq) → AuCl4- (aq).

[Basco36]

I like the glass set up, very cool.

[davidkoster]

You're the best chemist onn youtube;)

I will try this experiment tomorow

[mabakken]

Thank you! I really appreciate it =)

It's a pleasure by the way ;)

[mabakken]

Thanks, crazyboy :)

[crazyboy0602]

Nice job! Good video. i have heard the best temp is 85C but i barely saw any decomp with your setup. BTW it's nitric not bitric acid as it says in the description.