Love touur videos man you, nilered, explosionsandfire, extractionsandire, nurdrage, codys lab, so many orhers, mrgeenguy or w.e, jaylaser. I have zero chemistry chemistry experience. I taught myself everything myself but without you guys and your hard work makingg these. Videos i couldnt have. Been able to do thechemistry I love so. Much thank you all!!!
6:10 , slow distillation also ensures that your acid won't break down into as much nitrogen dioxide as it would if you cranked the heat. Leading to more product and slightly better yields. Thanks for sharing! Not many know that HNO3 can be made this way, so it's good to see you (and others) showing this method, which really helps those who either can't get or have a really hard time finding sulfuric acid that isn't extremely diluted. Great job! 😃
I can get virgin sulfuric acid at around 93%-97% at Walmart for $15 a gallon as professional strength drain opener. I remember checking out with a gallon of hydrochloric acid (muriatic acid) and a half gallon of sulfuric acid (drain opener) in the girl put them both in the same bag and when I looked the handles and started to load it in the bucket they both fell out the bottom and hit the concrete floor (I cringed) and said man we don't want those two busting at the same time, that would make a big damn mess, and the girl just looked at me like I had two heads. She had no idea
I didn't properly dry my potassium nitrate on my first attempt making nitric acid and it wouldn't start gloves on fire. I was a little disappointed. I dried it in an oven for 4 hours on very low heat and put it in a dessicator for a day. The sulfuric I used was also almost pure.(on my second attempt) Much better results.
I hope I caught you to tell you 2 important things 1st if your acid is concentrate enough you must store it In brown glass because nitric acid tends to be decomposed from UV radiation(thats why your distillation apparatus got full of red fumes (nitrogen dioxide) because the sun decompose your product) and 2 you may be careful because sealed fuming nitric acid botle tends to builds up pressure and maybe it explodes on your face when you trying to open or even touch it ! I personal be lucky 1 month ago by the same accident.. i was in my homemade lab ☺️ and searching for some glass apparatus to find when i heard a Sharp pop sound from the sample cabinet. When i open it i find the bottle in pieces and fumes everywhere.... Imagine to open the cabinet that time what would happen to me!! I clean up my mess and Search it ... And now i tell you to be careful!!! Thumbs up for your videos! also this bottle problems i think all fuming acids have it i am not sure but i search for it!!!
Another good video. Like Mike Hanley mentioned, I'd suggest measuring the density to figure out the acid content. I'm not sure exactly how concentrated you're needing it but if you do have a bit of sulfuric acid and need it stronger you can always mix it in and distill from the mixed acid for a quick upgrade. I can see a yellow glow in your acid but did it look greenish in person to you? I've done this method with sodium bisulfate and sodium nitrate and when I ran just the salts together the acid I was collecting was greenish. Teflon tape for sealing the joints was an interesting idea I might try if I do it again. I was using sulfuric acid as a joint grease.
I'll definitely be measuring the concentration at some point, and thanks for the idea for drying it! I'll be sure to do that if I ever need RFNA specifically. At this stage, I don't have any use for concentrated (or even azeotropic) nitric acid, but I'll keep it around just in case. The colour of the nitric acid is an interesting property of the nitric acid/nitrogen dioxide mixture. Under most circumstances and concentrations, the acid appears yellow due to a small quantity of dissolved NO2. However, under the right conditions, the equilibrium which holds NO2 in solution will shift towards making N2O4, which also stays dissolved in the acid to give a green colour instead. I'm not sure exactly which conditions favour the formation of N2O4 instead of NO2 (it's likely to be temperature I suppose), but it's nothing to worry about since the chemistry of NO2 and N2O4 are extremely similar.
Safety steps not shown or mentioned to viewer: * Hose nearby. * Bicarb nearby. * Dog on leash. * Snakes chased away from work area. * Friends (And self) limited to one bottle of cider/beer. * Pants.
I'm going to do this pretty soon myself. Nitric acid is nearly impossible for me to find in any concentration and the prices online are kind of insulting. So I've stocked up on potassium nitrate and sulfuric acid and am just waiting on a day where it isn't raining or snowing to do it haha. I have the opposite issue you have with the sulfuric acid, I have a choice of like 5 different kinds where I'm from for drain cleaner, but I cannot find sodium bisulfate anywhere.
I've been subscribed for a while now and am waiting with anticipation for that video! 😃 But I wanted to point out that the cost of the acid itself isn't that high. It's the costs of shipping it that make the price go high, though most sellers combine all the costs and say that shipping is "free", which is absurd and makes the price seem very high. The requirements for legally shipping nitric acid are insane and cost a lot to implement. If you ever order any and there isn't a large amount of packaging, containment and safety steps implemented in the packaging, then the seller is pocketing that money and putting others at risk by shipping it in a hazardous manner, which is illegal as well. If you ever order nitric acid, always order from a reputable company with great reviews. Otherwise the simple act of just ordering it could put people at risk unnecessarily. It's generally easy to tell who these companies are as they have somewhat crappy and suspect listings online. It's not hard to find what I mean. But yeah, it's the costs of shipping that make it high, not the acid itself. Just wanted to clarify that for those who don't have experience in chemical distribution and sales. 🙂
@@BackYardScience2000 I remember an old UA-camr, myst32yt or something like that, purified concrete cleaner he got from the hardware store which contained nitric acid. I think that video was from like 2012, and ever since then I've been on the lookout for it at all my local hardware stores. But I've given up on ever finding it and just decided to make my own. I guess you can't really blame companies for not being too excited about shipping nitric acid, and therefore charging quite a bit more to ship it. Oh well, I guess if nothing else, having to make your own is a good learning opportunity. (:
@@randomergy683 Nitric acid can't be sold as such to private individuals anymore since 2014 or so withing the EU (because >muh terrorism). But you can still buy it mixed with phosphoric acid, sold as pipe descaler, from which the azeotrope can be distilled out. Not ideal, but good for the home chemistry or noble metal scrap refiner hobbyist.
@@bromisovalum8417 ahhhh that makes sense. I live in the US and even here it's impossible to find even in pipe descaler, concrete etchant, etc. At least where I live. All I need is azetropic. Not even fuming lol. All I want it for is to make some silver nitrate and a few other nitrate compounds. Oh well, like I said, at least it forces you to learn more about the chemistry if you have to synthesize your own lol.
@@randomergy683 it's the same here. They don't sell it in any concentration in stores anymore, which sucks. So online is the only place left to buy it these days. Which really sucks due to the high hazmat fees associated with shipping it. That's the majority of the costs. Much, much easier and cheaper to just make it yourself these days.
The sodium bisulfate is the hydrated form of the salt, so there's a bit of water that distils over while the acid is produced. This is enough water to make the product about 15-20% water overall.
I managed to buy some potassium nitrate online a while ago (it was a lot easier to get hold of than I thought), so obtaining nitrate is not generally a problem for me these days. However, easily making large quantities of nitrate is a goal that I'll be visiting in many future videos. I've got plans to try some electrochemical and electric discharge processes for synthesising lots of nitrate, so stay tuned!
@@murkyseb Nitrate (KNO3) can also be made DIY by using urine (or urea) and soil in a big pot, combined with potash [or chalk if you don't mind about getting Ca(NO3)2 ] - and let some microbes do their jobs for some weeks. Later you can extract the Nitrate from the soil. It's a method everyone should know about, at least and if done in the right dimension, it can be much more efficient, than this electric discharge process. For gunpowder that was the anxient process, to produce nitrate, used by several nations.
Could you make the sodium bisulphate anhydrous before going this? If you answer this could you also help me understand the ratios. 1.5 molar equivalence, I don't know how to calculate. Would 3 parts NaHSO₄ to 2 parts KNO3 by weight be close enough to what you mean?
You could make the sodium bisulfate anhydrous if you wanted, but the main mechanism by which the reaction occurs requires the reactants to melt. The melting point of the hydrated form of sodium bisulfate is around 50 C (which makes it very easy to use in this reaction with modest temperatures), but the anhydrous form melts at above 300 C. While it would work to some degree, running a reaction at over 300 C is generally very difficult, and likely would decompose the nitric acid considerably. The ratio of NaHSO4:KNO3 I refer to in the video is not based on mass, but is instead based on the stoichiometry of the reaction. It's not possible to explain the fundamentals of this in a single youtube comment, so you'll need to do some research here. As a starting point, you'll need to look up topics such as the 'mole' and the 'molar mass'. Once you've understood these ideas, maybe search for 'stoichiometry basics'. There are plenty of textbooks online which can explain the ideas much better than I can. As a final note, if you are planning on doing this yourself (I mean, I don't know if you actually are, so this paragraph might not be relevant). I don't want to be rude here, but based on the fact that 'molar equivalence' is an unfamiliar term, please don't try this without extensive research. I'm not sure about your experience with chemistry, hazardous materials, or PPE, but this really isn't the project to do without an extensive understanding of the fundamental chemistry of the reaction and the substances involved.
@@ScrapScience thanks for replying and you're right, I don't have formal training however I'm cautious. I have experience making azeotropic nitric acid several times and sulfuric acid as well as things like chloroform and hydrazine sulphate for copper mirror and a lot of metal salts and complexes, tollens reagent. I use suitable ventilation and ppe. I'm not breathing in stuff in and I've not blown anything up yet. Most of it has been careful following of set procedures and looking things up online I've just got this far without having to calculate stociometry. I'll learn about it. Again thanks 😊
If I am only interested in azeotropic nitric acid, would adding a small amount of water helps with the distillation/foaming/dry potassium sulfate mass that will break the distillation flask? Using hydrogen peroxide in the trap would generate (dilute) nitric acid better?
Adding a little bit of water is a good idea if you don't mind a slightly lower concentration. It's still important to use an excess of bisulfate for the reaction though. Hydrogen peroxide won't help with NO2 absorption, the gas is extremely soluble in water anyway, and I don't think there's any real benefit to doing this, but I could be wrong.
Can you still use the inverted funnel and tube in the speaker for the process which involves the potassium nitrate and the sulfuric acid? Or is it just for that particular process?
Yes! The inverted funnel trap is effective for any reaction that generates nitrogen dioxide as a by-product (in fact, it works for other soluble gasses too). The reaction involving sulfuric acid and potassium nitrate makes much less nitrogen dioxide to begin with, but the inverted funnel setup is still a good way to deal with the gas.
@@ScrapScience I used it yesterday. But I don't think I much nitrogen dioxide because I didn't see any go in and it seemed like the water in the cup was just water. But it was a plastic funnel maybe that that escape? Either way I think it's now a mandatory part of my distillation process thank you!
3:59 I heard somewhere that bubbling nitrogen dioxide gas through 35% hydrogen peroxide would make an even higher potency nitric acid than using distilled water and I was wondering if you could confirm that
Yes that works. In this case you'd add the peroxide to the funnel trap at the end which wouldn't get you much more acid ,but if you're just making a small amount by bubbling NO2 through peroxide it's better than using water. For making any reasonable amount distillation is necessary.
Another question. If you heat up calcium nitrate you get NOx. Is there any benefit of using NaHSO4 like better yield or something? I can get calcium nitrate very cheaply.
Decomposition of calcium nitrate requires at least 500 C, which is generally beyond one's capabilities in a home setting (at least in a controlled fashion). The bisulfate reaction is much easier, only requiring around 100 C to perform.
@@ScrapScience I don't know about beyond one's capability. It is much simpler with a bunsen burner and a test tube. Drop calcium nitrate in the test tube and heat it. However, it might be more impractical if you do larger batches?
That's true, but a test tube scale reaction won't give you much nitric acid. I'd much rather do the bisulfate method a few times instead of hundreds of test tube reactions for calcium nitrate. As you've said, it's a much less practical method for making the acid. The bisulfate reaction also has the benefit of making highly concentrated acid, as opposed to a dilute solution.
Interesting thing before 1900 they used for concentrated (destiny 1,42 not high concentratet 1,52) heating nitrate of sodium or potasium with MnCl2 ,MnSO4, SiO2 from water glas acid reaction and sometimes MgSO4. They condenst most of the no2 but for an lab methode i think its to nasty.For ammo manufacturing they used the classic H2SO4 nitrate methode but only to hydrogensulfate never 1 mol H2SO4 on 2 nitrate mols.The MnCl reaction starts at 240C.
In that case, I'm afraid it won't generate nitric acid at any reasonable yield. HCl is more volatile than HNO3, so the distillation will just boil over the hydrochloric acid instead.
Interesting, maybe the sodium salt is a better choice then, and has the additional benefit of containing more nitrate per unit of mass. Ultimately, I suppose it comes down to whichever salt is easier to obtain for the individual. For me, that's definitely the potassium salt, but for someone who has the choice, sodium nitrate might be the way to go.
Thats a nice motorhome water pump you got there lol, I would use something like that for a water pump but I need it for my motorhome, if that's not from a motorhome just know that i have one that looks just like it that is from my RV
If I lived in a large city with access to a proper sewage system, I would just pour the waste down the drain, since everything I'm using in this particular experiment are actually common components in drain cleaners, and none of the ions I'm dealing with are remotely toxic. Since I don't live in a large city, I just bottled it and I'll eventually take it in and pour it down a sewage-system-connected drain. Of course, this is only for this particular experiment. Many other experiments require different procedures and the waste definitely cannot go down the drain.
@@ScrapScienceYou’re profile picture looks like the regular show home with rigby nd Mordecai on the couch and benson is there with 2 other guys actually plus there’s maybe a few benson relatives too also as well BTW .Just letting Y’k ,Lmk
Nice demonstration, as always :) If you protect your apparatus from UV-light (with aluminium foil for example), less nitric acid can decompose into nitrogen dioxode, and the yield of your highly concentrated nitric acid will be (slightly) better at the end. Would it be possilbe for you to messure the concentration of the highly nitric acid, would be really interested in it. I always used to use sulfuric acid, but it would be a blessing for me to be able to use sodium bisulfate when still getting the same (or at least similar) results. Btw, is the perchlorate cell video already in plan? ;)
Yep, thanks for the tip! Protecting the apparatus from UV light is generally a good idea here (I'm not exactly sure how much it helps, but it should reduce the decomposition somewhat). Sadly, protecting the setup from UV with aluminium foil also protects it from being filmed properly, so it's a tricky decision to make. Sadly, I won't be able to measure the concentration until we get around to using it (maybe two videos away at most). Until then, if you want an in-depth analysis of the efficiency and yield of this method (including the effect of running it with different ratios of reactants), you should check out Nurdrage's video on the topic. The link is in the description. The perchlorate cell is still a long while away I'm afraid. Since it's a relatively popular topic without much relevant information on UA-cam, I want to make sure I do it well. As such, I'm still in the research stage for that one. So far, its about 10th-15th in my list of video ideas that I've got lined up for the future. With my current upload rate, it's going to be quite a while before it's finished.
That'd work. In my opinion, it's not really worth it on this scale due to the high solubility of NO2 in general. Good thing to remember for large batches though, thanks!
Would you consider your water circulation pump to be overkill? I've always used smaller aquarium pumps for similar work and have never noticed any issues. That being said I'm by no means an expert and would appreciate any advice.
Have you got anything on line about your cooling water pump? I tend to spend more time "unnecessarily" fiddling with apparatus than do doing actual experiments.
Have you ever tried to extract salts and other minerals acids from urine? I would like to know if there is anything good we could extract from our pee, if there is any.
I'm not really a fan of doing chemistry with urine. As far as I know, the only thing of reasonable quantity for extraction is probably urea, which is cheaply available anyway.
@@ScrapScience you're right. Very little can come from urine other than urea. Which is far cheaper to just buy and the smell of extracting it is insanely horrid. It's worth buying just to not have to put up with the smell. Hahaha! 😂🤮
There's the niter bed method where you biochemically convert urea to nitrates, and where using urine is actually the preferred way, since it has micronutrients that help the bacteria grow and do their work. Plus it is incredibly low tech. Cody's Lab had a video on this (he used the nitrates to make gunpowder) but sadly that's no longer on UA-cam.
Great video! Can you tell me if it's possible to make 99% nitric acid with this Method? Or you still need to dehydrate with sulfuric acid or magnesium nitrate to obtain 99%?
It will depend on how dry your starting materials are. It's very likely that you'll need to do a drying step at the end since most sources of bisulfate salts will have at least a little bit of water (which carries over into the product).
It probably didn't make a big difference, you're right. But it's generally a good idea to insulate the distillation head in a lot of cases, even for a marginal increase in the efficiency. It's just the way it seems to be done by a lot of people.
The foil also protects the acid vapors from decomposing due to light breaking it down. It helps in 2 ways, not just one. It helps hold heat which makes it distill easier and protects the vapors from light, which can cause it to decompose. Doing this will help the yield some, but it's not a huge amount. Still very worth doing.
Nice work! Can red fuming nitric acid be stored easily for long amounts of time? Also here I've seen sodium bisulfate crystals sold as toilet cleaner/declogger.
I've been storing it in a glass reagent bottle with no issues for a couple of months now. Since it's said to build up a little bit of pressure in a sealed container, it's also important to vent the bottle every week or so (not that I've noticed any pressure build-up with this particular sample). Perfectly possible to store I'd say.
Yeah pressure will build over time, so you have to open the bottle to let the pressure vent occasionally, but it's not too bad. I've stored nitric acid for years before and it was fine. Just gotta be sure that you have a bottle that can hold up good to it and not leak. If it does leak, everything around it will be rusted or reacted making it brittle. Use PTFE tape around the threads of your container and make sure the lid is on tight and keep it away from light do it doesn't break the acid down over time. Also, store it in a cool, dry and dark place to ensure it is stored correctly.
Impossible not- You can collect nitrates from your own and any animal's urine and dung. It's not practiced anymore, but it was the source of gunpowder oxidizer, other than mining bird and bat colony excrement deposits ... If you are serious, I recommend assembling an ammonia to nitric acid apparatus..
I have looked every local fertilizers and pharmacy and hardware store there is nothing that contain nitrates I'm guessing it's some old restrictions when terrorist used to roam north africa I have a niter bed going and I'm working on birkeland eyed reactor thing so it's not that bad
The H2SO4 + KNO3 method yields higher concentration….also have you checked auto supply for your acid ? I believe it comes in at 50%. Just boil the water off .
Auto stores don't sell sulfuric acid anywhere near where I live (I've asked around a bunch of stores). I'm able to get hold of sulfuric acid these days, but the price of the bisulfate product is so much lower - hence why I'm using this reaction even with its lower yield.
Yep... or at least, it would be if I didn't get these gloves for free. I've got a friend in the fire service, and they have to basically throw out gloves with any degree of damage. Very convenient on my end.
Since dimethylmercury has a high permeability in latex and plastic laboratory equipment, the risk of doing this is high and assume permanent health damage.
You could run either reaction (i.e. generate potassium sulfate or bisulfate) if you wanted. They just require different temperatures and stoichiometric conditions.
Some gnarly stuff haha... but GREAT vid. I also liked the method of production! Those elements or the elements to make them a caveman had access to (dirt, wood ash, S acid, and salt water) instead of ice packs, ammonia, or something (lame). Cheers! #ScrapIt
There's a product called Rooto professional drain cleaner it's cleaner than most technical grade sulfuric acids on the market I don't know what country you're in however. They're manufacturing facilities about 10 now maybe 20 miles from me. 48 or $10 you can get 500 ml a very very very clean sulfuric acid
You need to control your heat better 78c-83c no hotter and you will produce better nitric acid we do it on the farm in a half gallon Jack Daniels bottle with a cork wrapped in Teflon tape and a glass tube running over to our collection bottle wrapped in a paper towel and kept misted with a fan blowing on it and produce 98% and way cleaner nitric. (Stay below the temperature of water vapor. to improve yield heat to 121c to get asiatrope at 68%)
If you're scared of hot sulfuric acid, molten sodium bisulfate should definitely scare you too. This process also runs a lot hotter than the sulfuric acid version, generates much more NO2, and runs a much higher risk of foaming over. Most people actually consider this method to be the more dangerous route.
Mmh Is not pure that acid. Mine is more strong and there is not more nitrogen dioxide inside the receiving flask. My receiving flask is just with a yellow nitric acid, maybe because I put aluminium foil around the tube too. And maybe the temperature is too hot and water is going into the nytric acid. The distillation process have to to go up 80°C or water will ruin the purity grade. And be carefully with the tube that go into the water. Because a bit of water will return into the little flask cause the pressure. Enjoy :)
It is strange that sulfuric acid is expensive in your country. In Iran, I buy 20 liters of 98% sulfuric acid for less than 5 dollars. It is cheaper than mineral water 😄
درود بر شما هم وطن عزیز من اسید سولفرویک 98% رو که به عنوان کود شیمیایی میفروشند اینجا تا قبل عید 20 لیتری رو میخریدم 170 تومان که جدیدا شده 220 تومان خلوصش هم روش نوشته و من باهاش خیلی چیزا درست کردم که جواب داده از اسید نیتریک بالای 93% تا نیتروگلیرسیرین و این آخری پتن 😄 خیلی تعجب کردم دیدم اسید سولفوریک 93% به عنوان چاه بازکن اینقدر گرونه اونجا@@explosivepo
Your warning at the start of the video missed a couple of vital elements, in the UK at least. You MUST have an appropriate licence in the UK (and probably some other countries) to possess, manufacture, utilise and combine certain liquids and materials above an allowable concentration. You must ALSO be able to demonstrate and declare your knowledge and capabilities for such usage, storage and possession including the necessary facilities for the same. Anyone ignoring the law on this is liable to SEVERE penalties including being placed on international terrorist watch lists. Of all the restricted materials nitric acid and hydrogen peroxide are at or very near the top of the list due to their extreme oxidisation capabilities. Consider yourselves warned!
Love touur videos man you, nilered, explosionsandfire, extractionsandire, nurdrage, codys lab, so many orhers, mrgeenguy or w.e, jaylaser. I have zero chemistry chemistry experience. I taught myself everything myself but without you guys and your hard work makingg these. Videos i couldnt have. Been able to do thechemistry I love so. Much thank you all!!!
6:10 , slow distillation also ensures that your acid won't break down into as much nitrogen dioxide as it would if you cranked the heat. Leading to more product and slightly better yields. Thanks for sharing! Not many know that HNO3 can be made this way, so it's good to see you (and others) showing this method, which really helps those who either can't get or have a really hard time finding sulfuric acid that isn't extremely diluted. Great job! 😃
I can get virgin sulfuric acid at around 93%-97% at Walmart for $15 a gallon as professional strength drain opener. I remember checking out with a gallon of hydrochloric acid (muriatic acid) and a half gallon of sulfuric acid (drain opener) in the girl put them both in the same bag and when I looked the handles and started to load it in the bucket they both fell out the bottom and hit the concrete floor (I cringed) and said man we don't want those two busting at the same time, that would make a big damn mess, and the girl just looked at me like I had two heads. She had no idea
Would the whole process work the same with Ammonium nitrate or is the ammonia causing problems ?
2NaHSO4=H2SO4+Na2SO4
@Rob337_aka_CancelProof in the USA? IN CANADA i can for 10 or maybe 12 bucks forn1 liter of H2SO4!
Nice workaround for the lack of sulfuric. Great video.
I didn't properly dry my potassium nitrate on my first attempt making nitric acid and it wouldn't start gloves on fire. I was a little disappointed.
I dried it in an oven for 4 hours on very low heat and put it in a dessicator for a day. The sulfuric I used was also almost pure.(on my second attempt)
Much better results.
Measure the density of your acid, i'm guessing it will be around 80% given the water content in your bisulfate.
you are absolutely right...
Dehydrate it in a oven
Magnificent. Love watching acid videos.
I hope I caught you to tell you 2 important things 1st if your acid is concentrate enough you must store it In brown glass because nitric acid tends to be decomposed from UV radiation(thats why your distillation apparatus got full of red fumes (nitrogen dioxide) because the sun decompose your product) and 2 you may be careful because sealed fuming nitric acid botle tends to builds up pressure and maybe it explodes on your face when you trying to open or even touch it ! I personal be lucky 1 month ago by the same accident.. i was in my homemade lab ☺️ and searching for some glass apparatus to find when i heard a Sharp pop sound from the sample cabinet. When i open it i find the bottle in pieces and fumes everywhere.... Imagine to open the cabinet that time what would happen to me!! I clean up my mess and Search it ... And now i tell you to be careful!!! Thumbs up for your videos! also this bottle problems i think all fuming acids have it i am not sure but i search for it!!!
Another good video. Like Mike Hanley mentioned, I'd suggest measuring the density to figure out the acid content. I'm not sure exactly how concentrated you're needing it but if you do have a bit of sulfuric acid and need it stronger you can always mix it in and distill from the mixed acid for a quick upgrade.
I can see a yellow glow in your acid but did it look greenish in person to you? I've done this method with sodium bisulfate and sodium nitrate and when I ran just the salts together the acid I was collecting was greenish. Teflon tape for sealing the joints was an interesting idea I might try if I do it again. I was using sulfuric acid as a joint grease.
I'll definitely be measuring the concentration at some point, and thanks for the idea for drying it! I'll be sure to do that if I ever need RFNA specifically. At this stage, I don't have any use for concentrated (or even azeotropic) nitric acid, but I'll keep it around just in case.
The colour of the nitric acid is an interesting property of the nitric acid/nitrogen dioxide mixture. Under most circumstances and concentrations, the acid appears yellow due to a small quantity of dissolved NO2. However, under the right conditions, the equilibrium which holds NO2 in solution will shift towards making N2O4, which also stays dissolved in the acid to give a green colour instead. I'm not sure exactly which conditions favour the formation of N2O4 instead of NO2 (it's likely to be temperature I suppose), but it's nothing to worry about since the chemistry of NO2 and N2O4 are extremely similar.
Safety steps not shown or mentioned to viewer:
* Hose nearby.
* Bicarb nearby.
* Dog on leash.
* Snakes chased away from work area.
* Friends (And self) limited to one bottle of cider/beer.
* Pants.
Haha, the last three are the most important, of course.
I'm going to do this pretty soon myself. Nitric acid is nearly impossible for me to find in any concentration and the prices online are kind of insulting. So I've stocked up on potassium nitrate and sulfuric acid and am just waiting on a day where it isn't raining or snowing to do it haha. I have the opposite issue you have with the sulfuric acid, I have a choice of like 5 different kinds where I'm from for drain cleaner, but I cannot find sodium bisulfate anywhere.
I've been subscribed for a while now and am waiting with anticipation for that video! 😃
But I wanted to point out that the cost of the acid itself isn't that high. It's the costs of shipping it that make the price go high, though most sellers combine all the costs and say that shipping is "free", which is absurd and makes the price seem very high. The requirements for legally shipping nitric acid are insane and cost a lot to implement. If you ever order any and there isn't a large amount of packaging, containment and safety steps implemented in the packaging, then the seller is pocketing that money and putting others at risk by shipping it in a hazardous manner, which is illegal as well. If you ever order nitric acid, always order from a reputable company with great reviews. Otherwise the simple act of just ordering it could put people at risk unnecessarily. It's generally easy to tell who these companies are as they have somewhat crappy and suspect listings online. It's not hard to find what I mean. But yeah, it's the costs of shipping that make it high, not the acid itself. Just wanted to clarify that for those who don't have experience in chemical distribution and sales. 🙂
@@BackYardScience2000 I remember an old UA-camr, myst32yt or something like that, purified concrete cleaner he got from the hardware store which contained nitric acid. I think that video was from like 2012, and ever since then I've been on the lookout for it at all my local hardware stores. But I've given up on ever finding it and just decided to make my own. I guess you can't really blame companies for not being too excited about shipping nitric acid, and therefore charging quite a bit more to ship it. Oh well, I guess if nothing else, having to make your own is a good learning opportunity. (:
@@randomergy683 Nitric acid can't be sold as such to private individuals anymore since 2014 or so withing the EU (because >muh terrorism). But you can still buy it mixed with phosphoric acid, sold as pipe descaler, from which the azeotrope can be distilled out. Not ideal, but good for the home chemistry or noble metal scrap refiner hobbyist.
@@bromisovalum8417 ahhhh that makes sense. I live in the US and even here it's impossible to find even in pipe descaler, concrete etchant, etc. At least where I live. All I need is azetropic. Not even fuming lol. All I want it for is to make some silver nitrate and a few other nitrate compounds. Oh well, like I said, at least it forces you to learn more about the chemistry if you have to synthesize your own lol.
@@randomergy683 it's the same here. They don't sell it in any concentration in stores anymore, which sucks. So online is the only place left to buy it these days. Which really sucks due to the high hazmat fees associated with shipping it. That's the majority of the costs. Much, much easier and cheaper to just make it yourself these days.
How is there water with it I didn't see you add any water wooden contain enough residual moisture to dilute that process
The sodium bisulfate is the hydrated form of the salt, so there's a bit of water that distils over while the acid is produced. This is enough water to make the product about 15-20% water overall.
You might want to use a thermometer to avoid overheating the nitric acid vapors which will lower your yield.
That was very interesting, excellent video as always :) do you have to make your nitrate ? If so that would make an interesting video
I managed to buy some potassium nitrate online a while ago (it was a lot easier to get hold of than I thought), so obtaining nitrate is not generally a problem for me these days.
However, easily making large quantities of nitrate is a goal that I'll be visiting in many future videos. I've got plans to try some electrochemical and electric discharge processes for synthesising lots of nitrate, so stay tuned!
Scrap Science interesting I’m surprised it was easy to buy but that’s good to know. That sounds awesome I’m looking forward to seeing that!
@@murkyseb Nitrate (KNO3) can also be made DIY by using urine (or urea) and soil in a big pot, combined with potash [or chalk if you don't mind about getting Ca(NO3)2 ] - and let some microbes do their jobs for some weeks. Later you can extract the Nitrate from the soil. It's a method everyone should know about, at least and if done in the right dimension, it can be much more efficient, than this electric discharge process. For gunpowder that was the anxient process, to produce nitrate, used by several nations.
What if you run oxygen through salt with little pump
Pump oxygen through which salt? To produce what?
Could you make the sodium bisulphate anhydrous before going this?
If you answer this could you also help me understand the ratios. 1.5 molar equivalence, I don't know how to calculate. Would 3 parts NaHSO₄ to 2 parts KNO3 by weight be close enough to what you mean?
You could make the sodium bisulfate anhydrous if you wanted, but the main mechanism by which the reaction occurs requires the reactants to melt.
The melting point of the hydrated form of sodium bisulfate is around 50 C (which makes it very easy to use in this reaction with modest temperatures), but the anhydrous form melts at above 300 C. While it would work to some degree, running a reaction at over 300 C is generally very difficult, and likely would decompose the nitric acid considerably.
The ratio of NaHSO4:KNO3 I refer to in the video is not based on mass, but is instead based on the stoichiometry of the reaction. It's not possible to explain the fundamentals of this in a single youtube comment, so you'll need to do some research here.
As a starting point, you'll need to look up topics such as the 'mole' and the 'molar mass'. Once you've understood these ideas, maybe search for 'stoichiometry basics'. There are plenty of textbooks online which can explain the ideas much better than I can.
As a final note, if you are planning on doing this yourself (I mean, I don't know if you actually are, so this paragraph might not be relevant). I don't want to be rude here, but based on the fact that 'molar equivalence' is an unfamiliar term, please don't try this without extensive research. I'm not sure about your experience with chemistry, hazardous materials, or PPE, but this really isn't the project to do without an extensive understanding of the fundamental chemistry of the reaction and the substances involved.
@@ScrapScience thanks for replying and you're right, I don't have formal training however I'm cautious. I have experience making azeotropic nitric acid several times and sulfuric acid as well as things like chloroform and hydrazine sulphate for copper mirror and a lot of metal salts and complexes, tollens reagent. I use suitable ventilation and ppe. I'm not breathing in stuff in and I've not blown anything up yet. Most of it has been careful following of set procedures and looking things up online I've just got this far without having to calculate stociometry. I'll learn about it. Again thanks 😊
@@ScrapScience I should add the term is not unfamiliar
Great procedure!
If I am only interested in azeotropic nitric acid, would adding a small amount of water helps with the distillation/foaming/dry potassium sulfate mass that will break the distillation flask? Using hydrogen peroxide in the trap would generate (dilute) nitric acid better?
Adding a little bit of water is a good idea if you don't mind a slightly lower concentration. It's still important to use an excess of bisulfate for the reaction though.
Hydrogen peroxide won't help with NO2 absorption, the gas is extremely soluble in water anyway, and I don't think there's any real benefit to doing this, but I could be wrong.
Can you still use the inverted funnel and tube in the speaker for the process which involves the potassium nitrate and the sulfuric acid? Or is it just for that particular process?
Yes! The inverted funnel trap is effective for any reaction that generates nitrogen dioxide as a by-product (in fact, it works for other soluble gasses too). The reaction involving sulfuric acid and potassium nitrate makes much less nitrogen dioxide to begin with, but the inverted funnel setup is still a good way to deal with the gas.
@@ScrapScience I used it yesterday. But I don't think I much nitrogen dioxide because I didn't see any go in and it seemed like the water in the cup was just water. But it was a plastic funnel maybe that that escape? Either way I think it's now a mandatory part of my distillation process thank you!
Can't you do this same process with HCl?
With HCl as the reactant or product?
@@ScrapScience He meant Conc.HCl and KNO3 as reactant
3:59 I heard somewhere that bubbling nitrogen dioxide gas through 35% hydrogen peroxide would make an even higher potency nitric acid than using distilled water and I was wondering if you could confirm that
Yes that works. In this case you'd add the peroxide to the funnel trap at the end which wouldn't get you much more acid ,but if you're just making a small amount by bubbling NO2 through peroxide it's better than using water. For making any reasonable amount distillation is necessary.
Another question. If you heat up calcium nitrate you get NOx. Is there any benefit of using NaHSO4 like better yield or something? I can get calcium nitrate very cheaply.
Decomposition of calcium nitrate requires at least 500 C, which is generally beyond one's capabilities in a home setting (at least in a controlled fashion). The bisulfate reaction is much easier, only requiring around 100 C to perform.
@@ScrapScience I don't know about beyond one's capability. It is much simpler with a bunsen burner and a test tube. Drop calcium nitrate in the test tube and heat it. However, it might be more impractical if you do larger batches?
That's true, but a test tube scale reaction won't give you much nitric acid. I'd much rather do the bisulfate method a few times instead of hundreds of test tube reactions for calcium nitrate. As you've said, it's a much less practical method for making the acid.
The bisulfate reaction also has the benefit of making highly concentrated acid, as opposed to a dilute solution.
Interesting thing before 1900 they used for concentrated (destiny 1,42 not high concentratet 1,52) heating nitrate of sodium or potasium with MnCl2 ,MnSO4, SiO2 from water glas acid reaction and sometimes MgSO4. They condenst most of the no2 but for an lab methode i think its to nasty.For ammo manufacturing they used the classic H2SO4 nitrate methode but only to hydrogensulfate never 1 mol H2SO4 on 2 nitrate mols.The MnCl reaction starts at 240C.
This method is work with household hydrochloric acid as well, right?
As in, using hydrochloric acid as a replacement for a bisulfate salt?
@@ScrapScience yes
In that case, I'm afraid it won't generate nitric acid at any reasonable yield. HCl is more volatile than HNO3, so the distillation will just boil over the hydrochloric acid instead.
@@ScrapScience I see..
Cool video.
Never even think of quiting UA-cam
Never :)
There might be a few long periods without any videos, but I'll be here for a very long time yet.
Harry is there any tubing that WILL survive the nitro dioxide?
PTFE and viton tubing will both survive direct contact with the gas indefinitely. There may be others as well.
I heard that if you use sodium nitrate the foaming isn't very intense
Interesting, maybe the sodium salt is a better choice then, and has the additional benefit of containing more nitrate per unit of mass.
Ultimately, I suppose it comes down to whichever salt is easier to obtain for the individual. For me, that's definitely the potassium salt, but for someone who has the choice, sodium nitrate might be the way to go.
I've used both and never really saw a difference. I think another factor in foaming is the use of anticaking agents.
Thats a nice motorhome water pump you got there lol, I would use something like that for a water pump but I need it for my motorhome, if that's not from a motorhome just know that i have one that looks just like it that is from my RV
Maybe a silly question, but how do you treat the waste for disposal? Great video, by the way!
If I lived in a large city with access to a proper sewage system, I would just pour the waste down the drain, since everything I'm using in this particular experiment are actually common components in drain cleaners, and none of the ions I'm dealing with are remotely toxic. Since I don't live in a large city, I just bottled it and I'll eventually take it in and pour it down a sewage-system-connected drain.
Of course, this is only for this particular experiment. Many other experiments require different procedures and the waste definitely cannot go down the drain.
@@ScrapScienceYou’re profile picture looks like the regular show home with rigby nd Mordecai on the couch and benson is there with 2 other guys actually plus there’s maybe a few benson relatives too also as well BTW .Just letting Y’k ,Lmk
Nice demonstration, as always :)
If you protect your apparatus from UV-light (with aluminium foil for example), less nitric acid can decompose into nitrogen dioxode, and the yield of your highly concentrated nitric acid will be (slightly) better at the end.
Would it be possilbe for you to messure the concentration of the highly nitric acid, would be really interested in it. I always used to use sulfuric acid, but it would be a blessing for me to be able to use sodium bisulfate when still getting the same (or at least similar) results.
Btw, is the perchlorate cell video already in plan?
;)
Yeah, this is great advice.
Another simple way to prevent UV exposure is just using amber bottles.
Yep, thanks for the tip! Protecting the apparatus from UV light is generally a good idea here (I'm not exactly sure how much it helps, but it should reduce the decomposition somewhat). Sadly, protecting the setup from UV with aluminium foil also protects it from being filmed properly, so it's a tricky decision to make.
Sadly, I won't be able to measure the concentration until we get around to using it (maybe two videos away at most). Until then, if you want an in-depth analysis of the efficiency and yield of this method (including the effect of running it with different ratios of reactants), you should check out Nurdrage's video on the topic. The link is in the description.
The perchlorate cell is still a long while away I'm afraid. Since it's a relatively popular topic without much relevant information on UA-cam, I want to make sure I do it well. As such, I'm still in the research stage for that one.
So far, its about 10th-15th in my list of video ideas that I've got lined up for the future. With my current upload rate, it's going to be quite a while before it's finished.
Borosilicate glass isn't all that transparent to UV light, so decomposition by UV isn't that great of a concern.
You can make 95% white fuming nitric acid from household items, as shown here: ua-cam.com/video/NHBDXtn7pjA/v-deo.html
Add ice to your water bath..... make recovery more efficient
That'd work. In my opinion, it's not really worth it on this scale due to the high solubility of NO2 in general.
Good thing to remember for large batches though, thanks!
I want the REFFERANCE that you used ... Please it's argent 😢
Would you consider your water circulation pump to be overkill? I've always used smaller aquarium pumps for similar work and have never noticed any issues. That being said I'm by no means an expert and would appreciate any advice.
Yeah definitely. I only use this pump because I have it on hand anyway. Anything capable of moving water through the condenser will do the trick.
@@ScrapScience Why not pull a vacuum using your cooling water with a aspirator ?
Have you got anything on line about your cooling water pump? I tend to spend more time "unnecessarily" fiddling with apparatus than do doing actual experiments.
you could make some NaNO3 with your trap-water to dry your RFNA
Thanks for the idea! I don't need the acid to be properly dry at this stage, but if I ever do, I'll keep that in mind.
Have you ever tried to extract salts and other minerals acids from urine? I would like to know if there is anything good we could extract from our pee, if there is any.
I'm not really a fan of doing chemistry with urine. As far as I know, the only thing of reasonable quantity for extraction is probably urea, which is cheaply available anyway.
@@ScrapScience you're right. Very little can come from urine other than urea. Which is far cheaper to just buy and the smell of extracting it is insanely horrid. It's worth buying just to not have to put up with the smell. Hahaha! 😂🤮
There's the niter bed method where you biochemically convert urea to nitrates, and where using urine is actually the preferred way, since it has micronutrients that help the bacteria grow and do their work. Plus it is incredibly low tech. Cody's Lab had a video on this (he used the nitrates to make gunpowder) but sadly that's no longer on UA-cam.
Great video! Can you tell me if it's possible to make 99% nitric acid with this Method? Or you still need to dehydrate with sulfuric acid or magnesium nitrate to obtain 99%?
It will depend on how dry your starting materials are. It's very likely that you'll need to do a drying step at the end since most sources of bisulfate salts will have at least a little bit of water (which carries over into the product).
Have you tried it without the foil? I don't think it makes such a big difference.
It probably didn't make a big difference, you're right. But it's generally a good idea to insulate the distillation head in a lot of cases, even for a marginal increase in the efficiency. It's just the way it seems to be done by a lot of people.
The foil also protects the acid vapors from decomposing due to light breaking it down. It helps in 2 ways, not just one. It helps hold heat which makes it distill easier and protects the vapors from light, which can cause it to decompose. Doing this will help the yield some, but it's not a huge amount. Still very worth doing.
@@ScrapScience Ok
That is very impressive ❤
Nice work! Can red fuming nitric acid be stored easily for long amounts of time? Also here I've seen sodium bisulfate crystals sold as toilet cleaner/declogger.
I've been storing it in a glass reagent bottle with no issues for a couple of months now. Since it's said to build up a little bit of pressure in a sealed container, it's also important to vent the bottle every week or so (not that I've noticed any pressure build-up with this particular sample). Perfectly possible to store I'd say.
Yeah pressure will build over time, so you have to open the bottle to let the pressure vent occasionally, but it's not too bad. I've stored nitric acid for years before and it was fine. Just gotta be sure that you have a bottle that can hold up good to it and not leak. If it does leak, everything around it will be rusted or reacted making it brittle. Use PTFE tape around the threads of your container and make sure the lid is on tight and keep it away from light do it doesn't break the acid down over time. Also, store it in a cool, dry and dark place to ensure it is stored correctly.
Nitrates are impossible to find where I live
Currently I'm working on a birkeland eyed thing
You should try it it's fun
He has a video on how to make nitrates from ammonia!
Yes I watched them
I'm waiting for it to snow here so I dont have to use huge amounts of ice
Impossible not- You can collect nitrates from your own and any animal's urine and dung. It's not practiced anymore, but it was the source of gunpowder oxidizer, other than mining bird and bat colony excrement deposits ... If you are serious, I recommend assembling an ammonia to nitric acid apparatus..
@@koukouzee2923 Don't they sell instant cold pack where you live? They should contain ammonium nitrate
I have looked every local fertilizers and pharmacy and hardware store there is nothing that contain nitrates
I'm guessing it's some old restrictions when terrorist used to roam north africa
I have a niter bed going and I'm working on birkeland eyed reactor thing so it's not that bad
The H2SO4 + KNO3 method yields higher concentration….also have you checked auto supply for your acid ? I believe it comes in at 50%. Just boil the water off .
Auto stores don't sell sulfuric acid anywhere near where I live (I've asked around a bunch of stores). I'm able to get hold of sulfuric acid these days, but the price of the bisulfate product is so much lower - hence why I'm using this reaction even with its lower yield.
Structural gloves.... Expensive choice!
Yep... or at least, it would be if I didn't get these gloves for free. I've got a friend in the fire service, and they have to basically throw out gloves with any degree of damage. Very convenient on my end.
Fantastic!
Sir plz make video on dimethilemircury = hgna + ch3i
Well, thanks for the suggestion, but no... I prefer staying alive.
Suggesting such a video shows that you have absolutely no regard for his well being and life.
Since dimethylmercury has a high permeability in latex and plastic laboratory equipment, the risk of doing this is high and assume permanent health damage.
Your first equation is incorrect:the products formed are nitric acid and potassium bisulfate not potassium sulfate
You could run either reaction (i.e. generate potassium sulfate or bisulfate) if you wanted. They just require different temperatures and stoichiometric conditions.
Douwe Egberts make some of my lab apparatus too
Some gnarly stuff haha... but GREAT vid. I also liked the method of production! Those elements or the elements to make them a caveman had access to (dirt, wood ash, S acid, and salt water) instead of ice packs, ammonia, or something (lame). Cheers!
#ScrapIt
There's a product called Rooto professional drain cleaner it's cleaner than most technical grade sulfuric acids on the market I don't know what country you're in however. They're manufacturing facilities about 10 now maybe 20 miles from me. 48 or $10 you can get 500 ml a very very very clean sulfuric acid
I read this and didn't even remember leaving it and I said oh this guy's near me and then I looked and it was me
Yasss
You need to control your heat better 78c-83c no hotter and you will produce better nitric acid we do it on the farm in a half gallon Jack Daniels bottle with a cork wrapped in Teflon tape and a glass tube running over to our collection bottle wrapped in a paper towel and kept misted with a fan blowing on it and produce 98% and way cleaner nitric. (Stay below the temperature of water vapor. to improve yield heat to 121c to get asiatrope at 68%)
Much, much safer doing it this way. Hot sulfuric acid scares the hell out of me.
If you're scared of hot sulfuric acid, molten sodium bisulfate should definitely scare you too. This process also runs a lot hotter than the sulfuric acid version, generates much more NO2, and runs a much higher risk of foaming over.
Most people actually consider this method to be the more dangerous route.
cool !!!
Mmh Is not pure that acid. Mine is more strong and there is not more nitrogen dioxide inside the receiving flask.
My receiving flask is just with a yellow nitric acid, maybe because I put aluminium foil around the tube too. And maybe the temperature is too hot and water is going into the nytric acid. The distillation process have to to go up 80°C or water will ruin the purity grade.
And be carefully with the tube that go into the water. Because a bit of water will return into the little flask cause the pressure.
Enjoy :)
I've never met an American named Harry.
my throat hurts just watching this
cool
It is strange that sulfuric acid is expensive in your country. In Iran, I buy 20 liters of 98% sulfuric acid for less than 5 dollars. It is cheaper than mineral water 😄
درود بر شما هم وطن عزیز
من اسید سولفرویک 98% رو که به عنوان کود شیمیایی میفروشند اینجا تا قبل عید 20 لیتری رو میخریدم 170 تومان که جدیدا شده 220 تومان خلوصش هم روش نوشته و من باهاش خیلی چیزا درست کردم که جواب داده از اسید نیتریک بالای 93% تا نیتروگلیرسیرین و این آخری پتن 😄
خیلی تعجب کردم دیدم اسید سولفوریک 93% به عنوان چاه بازکن اینقدر گرونه اونجا@@explosivepo
زن زندگی ازادی😅
Hmm, interesting video.
o i ruv doing this efvery thuwday night!@!
ur pump is over powered
yeah, it is
Your warning at the start of the video missed a couple of vital elements, in the UK at least. You MUST have an appropriate licence in the UK (and probably some other countries) to possess, manufacture, utilise and combine certain liquids and materials above an allowable concentration.
You must ALSO be able to demonstrate and declare your knowledge and capabilities for such usage, storage and possession including the necessary facilities for the same.
Anyone ignoring the law on this is liable to SEVERE penalties including being placed on international terrorist watch lists.
Of all the restricted materials nitric acid and hydrogen peroxide are at or very near the top of the list due to their extreme oxidisation capabilities.
Consider yourselves warned!