Nitric Acid Synthesis
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- Опубліковано 2 лип 2024
- Here, I make nitric acid using ammonium nitrate and concentrated sulfuric acid. They react together via this equation:
2NH4NO3 + H2SO4 == 2HNO3 + (NH4)2SO4
This must be done in an all-glass setup, because nitric acid will eat away rubber stoppers. It actually attacked my black plastic thermometer adapter a bit!
This method produces what is known as RFNA, or Red Fuming Nitric Acid. The red color comes from dissolved nitrogen dioxide gas, and the fuming characteristic arises from the acid's concentration - when you blow air at the acid, it fumes! This is because the acid readily reacts with moisture in the air to form little droplets of acid.
In the end, I collected 38mL of 70% (or 16M) nitric acid, determined by titration against NaOH solution. There was significant loss due to over-heating the system, which decomposed much of the nitric acid into various nitrogen oxides. Nitric acid decomposes when exposed to heat and light, so I'm keeping mine in a big rubbermaid tub in an amber glass, plastic safety coated bottle. - Наука та технологія
I'm glad that you shared this even though you ran across some complications because it helps us all learn from your mistakes as well as fostering community as we discuss solutions.
Glad to see another upload, keep um coming!
Keep them coming please, they're very informative !
Well done! That was a nice video.. helped me a lot.
Great reaction !
Hey! Nice video! a few constructive critics :)
1- always try to use potassium or sodium nitrate, since ammonium nitrate will generate some ammonia gas and neutralize part of your product and contaminate it.(lowering your HNO3 conc.)
2- altho fuming nitric acid is a therm used for +85% nitric acid concentration, i think is better to talk about FNA (red) from 94% to 98,5% and white from 99% to 99,9%.
3- Instead of using Al foil to isolate, is better to use an oil bath (or water, but oil is better) to get an even heat distribution and prevent crackin or overheating of the flask among other things.
4- If you don't want to get those NO2 gases out of the distill. setup and into your house, environment, or lungs, make a NaOH (sodium hydroxide) or NaHCO3 (sodium bicarbonate) aqueous solution trap.
Sorry if I misspelled something, regards from Argentina!
A good and classic way to determinate you have around +90% FNA is to react a piece of copper into the FNA and seeing very little to no NO2 gas production, and a dark green HNO3/CuNO3 solution.
not your hot plate dude. its because you are putting a roundbottom on a hotplate. was never intended to be used like that. contact patch is tiny. use a water bath or oil etc.
or a heating mantle. ice bath under the receiving flask is also helpful
I think it's the best and cheaper way! top video man!
Yes to all your points! Vacuum distillation is really good here because it runs at a lower temperature and thus you get less decomposition of the acid, leading to better yields. That's actually the only way to produce white fuming nitric acid (here I made red fuming). I just don't have a good vacuum source at the moment.
Yep! I tend to go through spurts of activity, it seems. This acid will be used in a top secret experiment I've got coming up, and if it works I'll have a really interesting video for everybody. :)
Hmm, will you consider nitrating some glycerol?
That's actually a really great question, I'll have to look into that. It's probably dependent on the reaction you are doing, but I've never seen NaNO3 been referred to as an "oxidizing salt," for example. Lots of sites say it's because it is the nitrate ion that is being reduced, rather than the hydrogen ion as in other acids, but NaNO3 doesn't react in the same way and it too has nitrate! That's very interesting, I'll have to get back to you on this one...
I like watching these:)!
very cool!
That's definitely a possibility - some people prefer to use other nitrate salts because of that. I had forgotten about that, thanks for the reminder. As for the heating setup, the flask actually wasn't touching the hot plate, it was sitting just above it. The hot air heats it from all sides (somewhat) evenly. Really I just wanted to try out a different heating method!
Consider using a sand bath between your hot plate and the round bottom flask, it'll allow the heat to be spread more evenly along the bottom as apposed to a single point.
The shiny side of the foil works better at reflecting the heat back to were you want to keep hot.
I've heard lots of stories like that from Australia. It's a real shame how bad things have gotten over there. In the US, Texas is particularly bad too. They're all pointless laws anyway, really. If you're determined to make illegal things, you'll find a way to do it without using official glassware.
Dang! Its been a while since you put out a video!
That reaction would be hard to separate your products, since both sodium sulfate and ammonium bicarbonate are very close in solubility. You could make ammonia with it by adding a base (possibly, haven't tried it myself), use it as a fertilizer, or use it to make double salts like ammonium alum or ferric ammonium sulfate!
I'd think it would, as bisulfate is a common substitute for sulfuric acid. The problem with that, though, might be that there is too much water. I tried this synthesis with dilute sulfuric acid and only got an incredibly dilute nitric product. Lots of water comes over in the distillation - that's why I used concentrated sulfuric. You could maybe try dissolving in an absolute minimum of water and carefully distilling at nitric acid's boiling point.
I store all my acids in plastic safety-coated glass bottles with plastic phenolic caps, and these are placed inside a rubbermaid tub with a layer of baking soda on the bottom. This absorbs any leaking fumes and will neutralize any spills. Acid fumes easily corrode metal caps. What do you mean your acid neutralized though? It won't do that unless a base is around, or a lot of metal to react with. I hadn't heard of any problem storing nitric in plastic bottles, but it's always best to use glass.
Not that I know of, what do you mean by weird? Bromine and nitric acid were always the two I heard the most about avoiding rubber stoppers. Most of my kit was from Dr. Bob on Science Madness, but they sometimes have pretty good deals on whole kits on eBay.
If it was anhydrous it would be a dry distillation, and I think that would have trouble since here you have two solids reacting. Trying to use a tiny amount of water wouldn't work because it would just evaporate off immediately during the distillation. You can certainly try it, but I think conc. sulfuric is the way to go.
you should convert the amonium nitrate into Na or K nitrate because the ammonia degrades the acid. just use no salt or just KCL or Sodium bicarbonate.
i think you were right about the orange haze btw my question is do you reckon if u used ur vacum outlet to rid the system of oxygen would this occur i have a similar set up n im considering not putting a full vaccum but using an aspirator to just remove any oxygen but totally unsure on the results is it that the oxygen works as an oxidiser and removing it would mess the whole experiment up ? either way the nitric is contaminated which im trying to avoid not that its necessary
Would this also work with sodium bisulfate substituting for sulfuric acid? I know it can be used to make hydrochloric acid, and HCl is a stronger acid than nitric acid so it would make sense.
Oxygen doesn't really play a part here. The purpose of using reduced pressure is that you can carry out the distillation at a lower temperature, which prevents the nitric acid from decomposing into NO2. This yields white fuming nitric acid (WFNA) instead of red fuming (RFNA) like I got. Having some dissolved NO2 has never really been a problem for me, since most reactions I use it for produce the gas anyway!
Here's what I found: the oxidizing power of the acid comes mainly from the fact that in concentrated solutions, a lot of HNO3 remains undissociated. This molecule is much more oxidizing than just the NO3(-) ion, which is found in nitrate salts and dilute acid. The salts do become good oxidizers at high temperature, which is why they find use in pyrotechnics. I've sent you a message with more info since I'm limited here.
I don't think so - the only way I've ever heard of to remove the NO2 is to put the acid under reduced pressure. Distilling it under somewhat of a vacuum gives you WFNA (white fuming nitric acid) instead, which doesn't have the dissolved gases. You might get rid of some of it by heating, or perhaps by bubbling air through the acid to carry it away, but that's just a bit of guesswork on my part.
Not all acids are equal. Nitric acid is an oxidizing acid that will dissolve many things sulfuric won't, like copper. It's also used in nitration reactions, which as you might have guessed from the name require the nitrate ions from nitric acid!
oh yeah and use stir rods or boiling stones to prevent bumping
Strong acids dissociate fully in dilute solution, but in concentrated solutions dissociation is incomplete, because there simply aren't enough water molecules around to protonate. Also, nitric acid is not entirely a strong acid, as its acid dissociation constant is lower than that for [H3O+].
Could this have been done at a lower temperature using vacuum distillation? And if so, you think that process might produce less nitrogen dioxide, leaving your end product clearer?
Epic
Please, tell me where can I store nitric acid at home?! I had a glass container, but with metal cap, and my acid neutralised overnight. Maybe due to fumes from acid reacting with cap? I don't have a propper equipment, but please tell me what should I do. I think it cannot be stored in plastic, but if it can, please tell me. Thanx!
I am assuming you're talking about the nitrate NO3- that does the oxidizing? If this is the case, couldn't you use something like NaNO3(aq) for the oxidizing properties? (just curious)
I saw a method where you use nitric acid, KNO3 (or other nitrate salt) and copper, i'd imagine you don't get a very high concentration though.
what method i seen thats use h2so4+nano3+65%hno3 for the mixture is it better?
What is this I hear about a run away reaction when you use Ammonium Nitrate as a Nitrate Salt...
e the glass and cause the RBF to shatter on cooling. it'll make a cake of salts in the bottle that differ due to the impurities in fertiliser and the bisulphate. what i do is boil some parrafin oil alongside my dry distillation and pour in the parrafin oil IMMEDIATELY after the dry distillation stops.
then i clean the reaction vessel with concentrated HCl and finish washing with acetone or methanol. whichever is cheaper for you
It is not the best to use ammonium nitrate because there is a bit of ammonia in the end product.
I was using ammonium nitrate and after a day or two there would be a white substance at the bottom and I am assuming this to be ammonium nitrate I think.
I switched to potassium nitrate because of this.
I think it should be:
NH4NO3 + H2SO4 ----> NH4HSO4 + HNO3 (as bisulfate is formed here)
i dont quite understand why your product was not more pure?
even simple distillation should yield a product too pure to react with copper that vigorously.
did you dilute it for the copper test???
Interesting, definitely sounds like it was attacked. Might be time to upgrade to all glass! Mine was somewhere around $100, but I bought it in a bunch of pieces so not sure what exactly it was. Check on eBay for some good deals.
No, HCl is too volatile. It would come over along with any nitric formed when you distilled. A mixture of a nitrate salt and HCl can act like nitric acid, but I don't think you can isolate much of it.
When you made yours did you use lab grease on the joints? I have done it both ways and it seams to make the acid a little more yellow.
I did grease the joints, yes. I have heard you can grease with sulfuric acid in some cases, which could be a good idea if you don't mind a little possible sulfate contamination.
:) thanks for getting back 2 me.
I am just slightly confused, it sounds like they're saying that the oxidizing comes from "disassociated HNO3"(but nitric acid is a strong acid which fully disassociates from my understanding." I also don't understand how a compound (no charge HNO3(unassociated) has oxidizing ability) I'll ask my chem professor see what she says.
That drain cleaner is only around 90 to 93% sulfuric acid it is not 98% there's a lot of water and organic impurities. You should always distill it first and get nice clean acid from it I know it's a pain in the ass but it's worth it. Even if you just boil the sulfuric acid in a beaker it will drive off the water and at least it'll be stronger. Another tip would be to always use at least 10% excess sulfuric acid over the about dictated by stoichiometry
Hmm, so it couldn't be done anhydrous? Would you really have to dissolve it in water, or could you not use just a really small amount of water to initiate the reaction and act as a catalyst? Perhaps that would just make 68% acid, in which case hydrochloric acid is probably a better bet.
I want to resolve the question about if it is safe or not to manipulate nitric acid with nitrile gloves. I saw a few days ago your comments in this video, so i said to my inorganic teacher (im studying chemistry at the university) if it it's dangerous or not. We decided to try this experiment, and today we have done it. The conclusion is: they don't react.
To sum up, you can manipulate nitrile gloves with nitric acid safely, even if it's concentrated (we use HNO3 10M to test the experiment)
I've also tried this, and found out that it's only certain types of nitric acid that cause bad things to happen with nitrile gloves. Red or white fuming nitric acid is what you need to watch out for. I tried this experiment with what I made here and it didn't react, so that means I didn't actually make red fuming acid like I say in the video. Later I tried this with reagent grade white fuming acid and the glove caught fire almost immediately! Scary stuff.
Also my white fuming acid was 17M, so there must be some threshold concentration where the danger really starts.
Um doesn't hydrofluoric acid also dissolve copper?
Kind of. It is not the action of acid that will go after the rubber it's the fluorine
nope, NO2 was formed from decomposition of the ammonium nitrate i expect. also i would have gone for a water bath, heating a flask from one point of contact just doesnt seem right...
سيكون حمضا ضعيفا وغير مركز.هل صحيح؟
I don't need conc. Nitric Acid, so is it possible to use Cheaper low Concentratet Sulfuric Acid? (37.5%)
No, concentrated acid is required in this particular reaction. You can always make concentrated nitric then dilute down to whatever strength you require, though. There are other ways to make the acid that don't require sulfuric, if that's your problem. Look into ways of creating NOx gases and leading these into hydrogen peroxide solution.
ok thanks!
you can make it with hydrochloric acid,copper,nitrate salt and hydrogen peroxide.
Should have placed a large beaker of water on the hot plate, and than submerged the round flask into the hot water.
MrLol333 is right - it's been particularly hard for me to find anyone that sells this acid. And if they do, few want to ship it or will charge exorbitant hazmat fees to do so. Sure, I could just buy almost everything I need, but half the fun of the science is being able to make the stuff myself!
Ive been told that the ammonia that gets released when using ammonium nitrate can contaminate the nitric acid - is that not the case?
It's not really a great compound to use, no. It ties up hydrogens in ammonium bisulfate, and can indeed decompose into ammonia which neutralizes your target acid back into the starting materials. It's also said to be dangerous to hear, although the quantities used here should be fine. Really you'd be better off using potassium nitrate.
@@mrhomescientist yeah, im told that it works better if you convert the ammonium nitrate to sodium nitrate using sodium hydroxide
@@jhyland87 Yep that would also work. I find that potassium nitrate is easier to make than sodium nitrate, but work with what you've got!
@@mrhomescientist yeah i just ordered potassium nitrate. I just have a bunch of ammonium nitrate, but no sodium hydroxide either, lol
Isn't it a bad idea to use NH4NO3? Some of the NH4+ might decompose you might get some NH3 comming over with the HNO3 and reform NH4NO3.
It is probably better to use a alkali nitrate instead.
plus it can overheat till the point of detonation once the reaction is initiated
Ya mon, plus the ammonia will neutralize the acid product
Okay so I'm not trying to be mr. Know it all cuz God knows I am not I have trouble with Stoichiometry I'll admit it. But think of it this way the reaction once it gets hot drives heat on its own so I always approach heating this very very low temperature I might crank my mantle up to about 5 to get it started but once it starts emitting a little bit of nitrogen dioxide gas I turn it way down almost off and it'll continue to Bubble because of the reaction is exothermic this way you do not not overshoot your temperature range
Use a sandbath. You will develop spider cracks in your round bottoms.
Could the ammonium nitrate being used neutralize the acid very much because it makes ammonia gas?
yeah
Cody Smith Hardly, think about it, what would that produce? Ammonia + Nitric acid would make ammonium nitrate again so no problem.
Instead of using a round bottomed reaction flask, why not just use an erlenmeyer to increase the surface area, making it heat more efficiently?
+John Van Vynck
The trick is to find an erlenmeyer flask with a ground glass joint. I
+John Van Vynck
But a water bath in a pot could have helped
ebay
You can buy 1 liter erlenmeyers with 24/40 female joints all day long on eBay.
couldnt you just buy it from ebay?
Wait why wouldn't you use an excess of sulfuric acid? Its boiling point is waaay higher than nitric acid, so you wouldn't lose any of the reaction to lack of reactants. Also why not grind the ammonium nitrate into powder for greatest surface area? Great informative video though, thank you!
Both great ideas! I also did my stoichiometry wrong because one of the products is actually KHSO4, not K2SO4.
+mrhomescientist ok cool, gotcha.
as I understand the RFNA should be above 90% and you state in your description that your conc was 70% , do I miss something here?
It was my impression that RFNA was concentrated nitric acid with lots of nitrogen dioxide dissolved in it. Looking around a bit, you may be right. The acid I produced is very similar to it, but apparently technically isn't RFNA. My mistake.
I tried this experience with something I thought was Amonium Nitrate from an instant cold pack..
first try: too much heat it exploded and made a big white fume.
second try: I reached 100°C.. I tried to control it at 83°C.. I failed.. no red fume and bang at 101°C it did the same thing.. exploded and made a big white fume. (exploded, my joint poped out)
If it wasn't amonium nitrate.. what was it? it was small white pearl.
BIGGY Girl Urea is another common chemical for cold packs. Check the label or look for an SDS online.
mrhomescientist damn.. it's urea.
well.. now you know what it do haha I will try the stochemetric to see what was the fume. Thanks! Now I need to find amonium nitrate to retry your technique.
mrhomescientist ok, after the stoichimetric calcul.. I made CH4N2S.. thiourea.. it means that I will have thyroid problem.
lesson of the day : always make sure of what I use before experimenting.
dry distill it mate.
it's SOOOOOO CHEAP to do it that way. a few years ago, that's how i always made my Nitric Acid when i couldn't find most things. impure Ammonium nitrate fertiliser mixed with impure sodium bisulphate. Heat it up to around 350 centigrade and it produces a great red fuming nitric acid.
if you add water, you'll actually get a less concentrated nitric acid so keep your apparatus as dry as possible.
the ONLY problem.. however.. is that when the final thing cools, it CAN fractur
Because obviously, all you can use cheap chemical glassware from China for is making not just drugs, but specifically amphetamines. It's theoretically relatively simple, an acetoacetic ester synthesis with chlorobenzene followed by reductive amination with methylamine will yield methamphetamine, but it's not like ethyl acetoacetate is exactly cheap.
The only way you can get the NO2 out of the nitric acid is to vacuum distill it i believe.
You can also bubble DRY air from a long glass tube through the red fuming acid for a couple of hours to produce water clear WFNA. I use an aquarium pump followed by a 200 x 30 mm glass column packed with anhydrous calcium chloride. This is available at Home Depot and just about any grocery store under the name "Damp Rid". Just pick up the refill kit and you will have nearly a kilo of white flaked anhydrous CaCl2. Once opened, be sure to store the excess dessicant in a resealable airtight container or it will soak up enough water from the air to turn into a puddle of snot. Also, be sure to buy the unscented Damp Rid refills. The scented stuff works fine, but there's just something creepy about WFNA that smells like a breath of Spring.
way easyier just to brew some benzal up then reduce it to phenylacetone and reduce again with methylamine and if ur going to the trouble of make methylamine you already have your adol cat just need some nitroethane which u can make with available stuffs or u can just not go to the hassle n stick to pyro.
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Breaking Bad gone wild...
How much was your yield?
It's in the description.
U should say that ammonium is the last source to look at i always use sodium
potassium nitrate has always worked the best for me.
Yeah most people seem to prefer it. Ammonium nitrate is what I had on hand so it's what I used. I think there's some concern that ammonia will be produced and neutralize some of your product.
the final prooduct can be cleaned by bubbling air through. u can also make it anhydrous by distilling with equal parts 98% h2so4
No it would cause nitric acid to decompose, producing more NO2
I've never heard of it being used that way - I don't believe the proportions of nitric and hydrochloric are right. My sulfuric acid is "Liquid Fire" brand drain opener, so it's either some sort of dye or suspended carbon particles. Drain cleaner acid is sometimes industrial waste acid that they don't bother cleaning up.
can 50% H2SO4 work?
No, very high concentration sulfuric acid is required for high concentration nitric acid. Otherwise you're just distilling a lot of water.
alphachem.ca is a good site and they do ship to individuals its who I use but this is only good if you live in Canada and Ontario to be more specific.
plus u have to pay the $69 hazzmatt fee
Anything that has a reasonable chance of breaking relatively expensive glass equipment is probably not such a good idea.
Try using a sand bath next time
If you want to wait an hour for it to warm up...
I don't understand why you'd make nitric acid if you already have an asic H2SO4...
asmcriminaL nitrations, aqua regia
Different acids do different things. Some will do things others won't. It's best to have a few different kinds.
Hey mrhomescientist, my condenser is longer than yours ;D be envious
haha
300mm
didn't mention a fractionation column
thats ridiculous anyone with determination doesn't need glass ware to make amphetamines we are all well versed in chemistry and i dont know about you but if i needed to make some amphetamine i would be able to bodge a condenser thats literally all you need and a reaction vessel not hard ^_^
I have that same hot plate. Its crap haha
But it can boil a whole liter of water in JUST 30 minutes!
Wouldhave been much smarter to use a pot of water, set the flask in the water and heat the pot. Either that, or get yourself a heating mantle, or a flat bottom flask Waste of Energy and good way to burn out your heating element
Even worse, nitric acid reacts with hydrochloric acid to make nitrosyl chloride. Not a good chemical to have belch out of your reaction mixture.
I understood nothing of what you said.......cool as hell though haha
Do not use nitrle gloves when handling concentrated nitric acid, they will catch fire on your hands if you spill it. Use noeprene instead.
Nitric acid vs. Nitrile gloves
I actually tried that experiment using my acid, and got no reaction. I think I was mistaken in calling this "fuming nitric acid" - it's not potent enough to destroy nitrile gloves like that. This type of glove still probably isn't ideal for nitric acid of any concentration. I have a glove compatibility chart in my lab that goes into detail on this topic.
mrhomescientist I found this out the hard way after making vacuum distilled
WFNA. I spilled a little on the gloves and managed to get them off before they started to smolder. I then replicated the experiment in the video.
why arent you a science profeser
no one should be a profeser!