Distilling Sulfuric Acid with Some Mishaps
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- เผยแพร่เมื่อ 24 ม.ค. 2018
- In this video, I distill some sulfuric acid... but run into a few problems along the way!
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Good having you back. I missed you.
love it
NurdRage you too are Epic, love your channel as much as this one......almost.
He never likes NurdRage comments
Then he disappears.. again! hah.
Same for you .... NR
This video reminds me of a story my chem professor told in lecture...
A few years ago, a student (undergrad) was working in the lab and accidentally emptied some organic waste into the acid waste container. Rather than alerting the TA, the student tried to hide his/her mistake by sealing the container (we use giant glass carboys that probably hold about 10 liters or so) and walking away like nothing happened. At the time, my professor was in her office and she heard an explosion next door followed by the sound of falling glass shards. She runs out of her office to find the entire lab group of 30 or so panicked students evacuating the lab followed by a cloud of HCl and NO2 gas. Several students had to be rushed to the hospital for burns and glass cuts and law enforcement was involved as well... just goes to show what happens when you don't properly fix your mistakes in the lab :)
How did they found out?
what would be the appropriate thing to do in that situation tho?
@@nabrialesadramelech3299 leave it open, close the door and open the windows to allow the gas to escape
@@seibtyee637Strong acids or bases must always be neutralized before being placed in the appropriate waste containers.
@@SciDOCMBC yes. but i was referring to what to do after someone causes an explosion like that.
I love when NurdRage includes his mistakes and solutions. I think you managed to 1 up him by actually thinking through solutions in real time with footage to the experiment going awry.
It's not a proper lab bench unless it has acid burn marks on it.
It's not a proper lab bench until it has a big old hole with glowing perimeter. Bonus if the glow is due to radioactive fission byproducts.
@@stamasd8500 it's not a proper lab bench if you never burnt a hole straight into it using a blowtorch because you got impatient
A badge of pride!!!☝️
@@VerbenaIDKit's not a lab bench if it doesn't have a hole going to earths core with a perimeter warping into the fith dimension
@@dudetapedtoafridge3073 back when i did chemistry my "lab bench" had no holes, because it was stone :3
Lovely work as usual, Doug.
Really good to see clean-up of a real spill. Such things are usually left out but they are extremely important. And the simulated situations found in safety videos really don't cut it.
I am enjoying the increased video frequency. Thanks.
OMG - even though you showed your mishaps, you still manage to make that look so easy. I've distilled H2SO4 before to purify it, and that was probably one the scariest days of my life!!!
Thanks for sharing so many useful tips and tricks along the way - Especially about using a hot air gun to stop the water droplets falling back into the boiling acid mixture at the beginning. I must try that next time. Maybe then I'll need less changes of underwear when caring out this prep!
I really like these basic task “how-to” videos. Good choice on your part Doug for showing us stuff to keep us from frying ourselves.
Look children, lets distill sulfuric Acid in the dark... They didn't teach you that in school..!!! ;-)
I love your video's and greetings from the Netherlands...;-))
'Hi Doug. I'm relatively new to chemistry. I had extreme violent bumping recently when I tried to extract HCl (9.5% w/w, active ingredient) from Lysol Power Toilet Bowl Cleaner through distillation. I'd bought this product at the dollar store. A 1 litre bottle of HCl acid costs 73$ on Amazon. I wanted, no needed, to save money. I'd researched all the ingredients to the Lysol product, but for some reason C10-16 Pareth (or C12, or C16) had escaped me. It turns out this ethoxylated alcohol is explosive (or is an explosive) when heated. I'm lucky nothing major happened during my HCl extraction experiment. Today, I attempted to concentrate some sulfuric acid I'd made from Epsom salt through electrolysis. My r.b. boiling flask survived the Lysol HCL extraction experiment, but it finally cracked during the sulfuric acid distillation, and acid leaked onto my homemade heating mantle and work table. It hadn't had time to concentrate, so it caused no major damage to my mantle or work table.
I love these weekday videos. Keep it up.
Holy crap! So many videos!!! Keep up the incredible work!
I found my RB flask dissolved the glass enough to see a ripple around the acid level was!
Had some violent back flashes when acid sucked the water vapor back.
I used activated charcoal to purify our additives and limit splashing so it could have caused interior of flask dissolving!
I would be very reluctant to do this in glassware like this, the thermal stress on the glass is enormous. Given how high the flask was, if it shattered it would have splashed boiling hot concentrated acid everywhere. Also the pinging coming from the condenser is a very bad sign, the condenser was also highly stressed and could have cracked.
I am glad nothing bad happened, but I would not want to stress my glassware like this.
Take an quartz glassware instead and you will be more safe 😊
Thank you for showing your mishaps, it increases the educational value of the videos!
Great video! You're "learning experiences" we're the best parts! Lot's of ppl want their videos perfect. Thanks for showing us!
Nice one Prax !
Great to see Real experiment. Superb to see how you deal with accidents.
You are one of my favorite (if not my favorite) chemistry channels. Your videos are well made, fun, and always interesting. You inspired me to start making my own videos, and have given me many ideas for my own lab. You're awesome.
Thanks, Doug. I'm not a chemist but I love chemistry and these simpler videos are very enjoyable for me.
Good video as always Doug, and good on you for showing the work around to a problem. It's not easy showing people screw ups, but when you do it helps people see the foibles, and know how to get past them.
Details explained in this video was very helpful. Keep it up.
Well done, Doug!
Holy crap, your video is so good and extremely educational, you have my Subscription and likes from now on sir, great work!
One thing to stay aware of is that boiling chips might have enough water in/on them to cause a problem. Baking them or making sure whatever you are adding the chips to is around or below 100c would be a bit safer.
Very cool and informative video! Keep them coming!
awesome video and extremely informative. it really helps us newbies just getting into chemistry with you explaining why certain methods are used and for what specific reasoning. thanks so much.
This is why I love Doug's Lab :)
Very nice result. The mishaps were perfect for learning purposes. :-)
This was very interesting. hope to see more in the future
Thanks for recording and posting this video. Good information about an important process. Much appreciated.
Keep up the excellent work, thank you.
Mishaps with solutions are great to see.
Neat! Distillation of sulfuric is kinda scary, but I intend to do it at some point. Very cool video and well thought out setup.
Perfect timing! Just recently made some cerium sulfate from CeO2 for myself and wanted to recover the extreme excess of Sulfuric Acid I had to use. Definitely not easy to come by for the average home chemist!
WELCOME BACK DOUG!!
Super video Doug, good to see you are human 😀 Everyone makes mistakes, the important thing is that we learn from them.
I have the same thermocouple! Terra cotta pieces are also a good idea for boiling chips; I'll have to try that. I really liked all the real-world problem solving you did too. That's great to show how real chemistry in a real lab is. Good stuff!
Chips from spark plug porcelain work well as boiling chips
Hey bud. I’ve just made some weak h2so4 myself. I worked out 6.25x10-4 mol concentration via titration. This video helped a lot, has inspired me tbh.
Great video. Thanks! Are you going to make some videos on analysis? For example, how would you figure out compounds are left in the undistilled portion?
15:30 were you worried about thermal shock cracking glassware with that boiling occurring inside the condenser column? Those 'clicks' sounded angry xD
Love the vids man. Thank you!
I love this Bunsen burner. Such a neat well-stocked lab, and such a post-apocalyptic, Fallout style burner...
Just heads up, you showed part of your face at 2:25. I'm not sure if you're fine with that or if it was a mistake, but I figured I should mention it
I noticed! Anonymity is not really a concern for me. I usually don't show my face because I want people to stay for the chemistry, not because I'm being a quirky TV personality.
At 4:56 you can see it again ;)
He's not making Dimethylonepentamethamphetahydroxazine here guys. Just a simple, yet ballsy, distillate of H2S04.
love that!
I`ll be honest, I kinda want to see who this person that runs "Doug's Lab" is now. :P
God I would be so scared that the flask might break! Nice video!
great video
Nice video Doug's Lab, keep up the good work! , i am wondering why you didn't do a vacuum distillation thus avoiding these extremely high temperatures..
Very cool. Concentrated sulfuric acid is so cheap and easily available that I don't think I'd ever try this. However, it is good to know how it's done.
glad you're back with gusto. hope nothing depressing happened lol
Great job; combination of preparation, technique, and recovery. Yes, I have a gallon or so of drain cleaner sulfuric acid, and have been holding-off with a bit of trepidation. Having watched a few videos, but now, with caution, I will give it a go.
PS
I have click your channel for sometime (since, 'The Fischer Esterification: Methyl Salicylate', more than a year ago) hoping for an update, Ta-Da!
Charge on and keep breaking bonds!
Cheers, Mark
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Im so glad youre back. Do you have a patreon?
oh nevermind ha you said it at the end
Gas is both elegant and simple at the same time. Saw some other youtuber mess with a heating mantle.
hi Doug when are you back? your channel is the best here and we need you. what are you up to?
its 2021 October and Dougs video "Nitric acid day" has now been deleted by youtube.
Doug, what are your thoughts on a vac distillation in this case instead of the high temps? Great video!
you can prolly do a vac distill...but it will be much more dangerous as the risk of implosion is there...and hot conc sulfuring acid is not a match to hot exploding sulfuric acid
Why would vacuum distillation cause an implosion
It's not this simple, Doug, and you made few errors.
First thing, to turn this type of drain cleaner (not sure why this is used instead of much better NaOH, but who cares if this makes sulfuric acid easily obtainable :) ) into a very pure sulfuric acid, you really need to reflux it a bit with small addition of hydrogen peroxide. That will create weak piranha in situ which will destroy organic compounds and oxidize pretty much everything to CO2, H2O, N2. And it really is something that has to be done because sulfuric acid doesn't render organic compounds (they're listed as "inhibitors") to the very simplest ones, but leaves you with hot fumes that still contain reactive species that distill over.
Weak piranha reflux is simply essential and produces very clean acid.
Second, water condenser and this distillation don't go together. Temperature difference is over the borosilicate glass limit and introduces such stress that there is a plausible chance of glass breaking. Use an air condenser. Those are cheap (it's just a tube, afterall) and do their job well. Of course, it must be angled. If it goes straight down, it heats itself and then overheats.
Third, NEVER EVER heat borosilicate flasks with an open flame. That's an open invitation for a very bad day. Not only it can break and let out boiling corrosive liquid, but it wears the glass down, introduces stress and material aging. If one doesn't have a heating mantle and the heating plate is too weak even with additional insulation, flash has to be wrapped with steel wire mesh. At least two layers. That delivers almost all of the heat, but there isn't a temperature spike of the open flame involved. Steel mesh lets through hot gas and also radiates heat into the flask.
Fourth, use glass shards for the boiling chips. Porcelain is harder than borosilicate glass so each time it touches the glass, it scratches it and gradually erodes the inner surface, making it prone to cracking. Bubbling moves the shards up and down, scratching their way around.
All in all, you did manage this quite well and you have a good sense of solving problems when they occur. Panic is always a stupid thing to do.
I've purified several litres of this tamed beast in my life so I was glad to share some things with you.
for the first method I don't even think distillation is required. add the H2O2 and heat and drive off all the water in an open vessel and you should have clean concentrated acid left over.
No, because inhibitors include insoluble, nonvolatile salts. Distillation is essential.
well if they're insoluble why don't they drop out of solution? would you happen to know the name of these salts?
My mistake. I meant to say nonvolatile only. They are soluble. I think some phosphates are the guilty party.
I do have some on hand prepared in this fashion. I guess the best way to verify is to boil a small amount to dryness and see if any sort of film/particulate is left behind... is this something you have done?
Probably my favourite video demonstration of this task so far. What thermometer/probe do you use to measure the temperature in the flask? I have a surface temp IR one but need to find a cost effective +300°c one. Regards.
Serious question: If super hot h2so4 is so dangerous, why are there no videos of the vacuum distillation of h2so4? Wouldn't that allow for better control of the temperatures? As, if there was a glass failure, the pressure would instantly increase, and boiling would stop.. seems safer. Before saying the gasses would eat your vacuum pump, what about a cold trap with liquid nitrogen innit or even dry ice and isopropyl? Also, why is nobody using a bump trap?
that looks exciting
Greetings Excellent Video I have a question Can you increase the acid concentration using a vacuum pump Or you can decrease the process time by applying a vacuum to the distillation.
Great video.
My two son's and I are getting into doing some home chemistry.
It seems getting hold of chemicals here in the UK is more difficult than in the US.
We live off grid and have about half a ton of dead lead acid batteries so thinking utilising that acid would be good and any bi products can be poured back into the batteries when I recycle them.
I am wondering if your distillation method would be a good route to take to get clean concentrated sulphuric acid from the battery acid? I appreciate starting at such a low concentration would result in a lot of weak distillate to distill off first but wondering if this would be a good way to remove the lead and other battery plate doping materials from the original acid?
Thanks for posting, nice to see a TH-cam video without a cat wandering around in the background, although it probably would increase your subs.
Cat hater. :) Cats always spruce up a video! But a cat in the lab is not a good idea!
This scares the hell out of me. I keep thinking, what happens and what do I do if that thing breaks (the flask)? What does the 320 degree acid (with SO3 fumes) do when it hits the wood? Explode in flames? What if it happens while I'm reaching over to attend the apparatus? What if some of it splashes on me?
Would it be safer to use quarz equipment?
I was wondering why you didn't add boiling stones :)
could you use vacuum distillation to lower the boiling point instead of using flame to get the right temp?
I have a question, i have my concentrated sulfuric acid in a cool dark place but it still turned dark.Will this cause the acid to be weaker than 98% ?
Yeah, I added boiling chips to some extremely concentrated coffee I was boiling down (in an attempt to make a homemade ink). That was...exciting. Extremely exciting.
The main thing I'd recommend doing differently is the use of a metal bath (Wood's metal or Rose's metal*) rather than putting the flask directly in a flame. That's a lot of stress, even for a quality flask, and tiny scratches in an older flask could prove to be weak points.
Along the same lines, blowing air through the condenser instead of water (use a cheap aquarium pump, or an aspirator) would stress the condenser less. Failure is not likely, but would be spectacular (in a bad way) if it happened.
And your distilled acid isn't as pure as it looks - the anticorrosion ingredients in the drain cleaner degrade, but they aren't destroyed, so there are sulfonic acids that distill over, and probably a fair amount of SO2. Adding 30% hydrogen peroxide at the beginning will make a big difference; about 10% of the mass of the acid should do the trick. Distilling the water out won't take all that long. Finally, avoid exposing the distilled acid to air, because it absorbs moisture instantly.
*I prefer Rose's, since it doesn't contain cadmium.
And the award for most dangerous H2SO4 distillation goes to...
What is that piece of glassware that your thermocouple probe sits in called
Doug, can you make the video you always promised on drying concentrated acetic acid to glacial?
Do you think you would have been better off putting a claison adapter in the system to control the boiling and foaming? I liked the vid and love looking at different setups especially with good explanations.
Did you titrate the product? At 17:15 it looks like there is separate layers of liquids and when you pour the produck in the first storage vessel it seems like those layers are mixing and the liquid goes a bit hazy.
Awesome skeleton watch bro! And great video! Taught me something :) could I do this distillation with car battery acid?
Haha thanks, but it's nothing special. It's an Armitron 20/4406BISV, about $85 at Sears. And yes, you can do this with battery acid, except you'll just have to take off a lot more water at the beginning.
I am certain you could. I seem to remember that the solution in car batteries is fairly dilute. You'll have to remove a lot of water, so I wouldn't expect an amazing yield.
Where I can buy a funnel with grindstone for pouring liquids from flasks like you have on 17:20?? What is the name of this glass?
Do you think you could do a video on extracting magnesium metal from Epsom salt?
LOL, I predicted the acid would start spitting out of the side of the flask
It used to happen to me in the kitchen all the time when I'm concentrating the H2SO4 I synthesize.
You can insure no presence of water during distillation by heating at about 80-100c in a glass boro kettle, and drop a cone shaped drinking glass with some water in it, in the opening to keep the acid in and the water escapes. Don't be impatient with the temp because you'll end up with a spitting acid situation again. It takes a while but the distillation goes seamlessly.
I just came up with a synth process and started making my own, that way all I have to do is evaporate the water until it reaches it's azeotrope.
I was making nitric acid with ammonium nitrate from cold packs. The packs said ammonium nitrate, but they must have been Ca Ammonium nitrate, because as soon as I added the acid it started foaming up. Had to disassemble and dunk the flask in a bucket of water, then added baking soda but ran out, and then dumped a whole bottle of 10% ammonia solution into the bucket to ensure neutralization. Lesson learned, test your NH4NO3 before you commit to a large batch.
Ammonium is available over the counter. Also the ammonium sulfate left over is extremely water soluble and easy to wash out. Doug has a video of him using potassium nitrate and he pushes the reaction to form potassium bisulfate instead of sulfate, for the reason that potassium sulfate is much less soluble and harder to clean out. But that reaction requires more sulfuric acid than if you pushed the reaction to get K2SO4. So by using ammonium nitrate I can push the reaction to ammonium sulfate instead of bisulfate, get more nitric acid by using less sulfuric, and its easy to wash out. All that and there weren't many videos on yt showing how to make nitric acid with NH4NO3. My video is here, but I have another one coming out when I get the editing done, bc I have better footage the 2nd time around. th-cam.com/video/dCxs_tlJaIg/w-d-xo.html
I find that simply adding hydrogen peroxide to the rooto brand drain cleaner will oxidize all the organic impurities. It works a lot faster with hot acid but it can also be done at room temperature.
What could be used for containment under the whole aparatus in the event of a catastrophic failure or even minor leakage like demonstrated.
Hey @Doug's Lab could you please tell me what thermocouple you are using at 11:25? I really can't find one good enough to use in an acid destillation environment without it getting all destroyed...
Note that it is placed in the glass protection tube.
What happens with the inhibitors? Are they attacked by the hot acid?
How long you think that condenser is? 200mm? Asking for a friend 😅
17:22 nice watch! What kind?
I was doing this once and needed to add boiling chips. The moment I took the the thermometer adapter off it exploded, luckily it only got on my fingers and arm. I cant think of any reason that would happen though??
hello doug! please upload video "synthesis PCl5"
Did you measure its density?
what is your glassware made of that it can withstand those temperatures? mine is borrosilicate and thus fractures at 165 C. So what is yours and where did you get it?
Pyrex does not fracture at 165C. Note that the fracture temperature depends on the glassware configuration. A round boiling flask for example will take much higher temperature than an erlenmeyer flask. Whatever, it is EXTREMELY DANGEROUS to heat an open flask like that in the video with no catch basin under it in case of a fracture. It is best to have a sand filled box under the setup so if it cracks and all the hot acid splashes down it will be contained instead of splashing all over the place. Half and half sand and baking soda is best.
The temperature of the acid was over 300 degrees and still the glass didn’t crack what sort of glass is this ?
Do you have the Index of Refraction?
and, do you have access maybe to IR or NMR spectroscopy? would love to see the results of said analyses.
Refractometers shouldn't be too expensive.
EDIT: I lied, the one we use in our lab (the cheapest of the cheap) is like, $1000...
I have to extremely need to know how we can sulphonation by sulfuric acid with benzene or any alkyl group...????
Can you make video on sulphonation?
My target is to prepare Sulphonic Acid.
What is the condenser water temperature?
Actually, the azeotrope is 98.2% H2SO4. How long would it take to get azeotropic H2SO4 from bettery acid (40% H2SO4) - asking because H2SO4 based drain cleaners are not easily available here
shouldnt pressure be vented from this system?
Is there a way to distill under reduced pressure? That would help lower the temp needed & hopefully reduce bumping a bit. Anyhow, thank you for uploading!
Sulfuric acid vapor doesn't play nice with vacuum pumps.
True but boiling at such high temperature might increase the chance of an explosion
Question: can you clean up the coloration with hydrogen peroxide? I mean, you dilute the acid, but you create piranha and you avoid having to setup a distillation.
Yes, you can add a little weak hydrogen peroxide which will destroy any organic matter present, oxidizing it to H2O and CO2. This usually clears up the coloration, but will not remove metal salts. It will also need to be boiled to remove the water that comes with the hydrogen peroxide and to destroy remaining peroxide before it is used in a reaction.
Doug's Lab thanks! Glad to have you back
If you don't mind me asking, about how much money did you invest into that lab up to this point? (Including chemicals, glassware and everything else)
Pretty scary video, fortunately nothing bad happened :D. I have my self bad experience with only dehydrating the acid, not distillation, some broken glass, because of that. Is it safe to cool hot H2SO4 with water jacked? I mean I only read about air jacked used for this purpose since its boiling over 300*C and we could see ourselves, that water was boiling in contact with H2SO4 steam. I know that even laboratory glass is save to use only when there are max differences in temperature, about 100*C, then it can crack?
It is not safe at all. Temperature difference is over 150 degrees which is kind of a textbook limit. This simply requires an air condenser.
I didn't hear the customary warning about SO3 gas making its way out and killing you, how big of a concern is this? (I noticed the big sucking fan, I'm not planning to do this without a fume extraction mechanism but I'm still not done building it)
Hey Doug can we use broken glass as boiling chips ??
Broken glass works poorly! You need something that is porous, and never used before (after use and cooling, the pores get filled). The acid must be heated nearly to boiling before the chips are put in, and the heat must not reduced (as when he cools to add more acid). More (just 1 more) chips need adding at that point, after every cooling/reheat. The chips can be reused after washing and drying completely to open the pores. The commercial ones are usually discarded after use.
I'd be well paranoid heating glass like that. Even if it's slowly & evenly heated I'd be waiting for something bad to happen....
Not paranoia, but common sense. This should never ever be done. He was lucky it didn't snap.
Well, if the glassware used is borosilicate there really isn’t nothing to worry about, especially if it is heated slowly
Not true. Ask any laboratory flameworker. It's a bad practice that induces fatigue, lowering expected lifetime of the vessel. And then one day it breaks while there's ether inside. :/
Oh, didnt know that. I guess I will be safer from now on :)
It's certainly better practice to place at least a gauze between the flame and the glass.
9:43 a friend of my mother died in that way distilling diethyl ether (in the university lab, not at home).
Pseudo Memes only a total idiot would distill old ether. She was just recycling a 5L gallon of 2 week old ether used for various purposes. She was distilling 1L of it (in a 2L flask of course). The temperature was well above 37°C when she realized that she forgot to add boiling chips.
Now, forgetting to add boiling chips is quite a bad mistake, specially when distilling ether. But it can happen, it was just a distraction. But the really bad error that she did was not to let the whole thing cool. The ether was like 20 degrees above its boiling point. If there were peroxides, they were really dilute, peroxides in the distillations of ethers are a concern only when the thing comes to an end.
The ether overflowed so violently that it spit hot liquid and vapor all over the fumehood, and then it catched fire. I wasn't born at the time, luckily, but my mother
told me that there was literally a bubble of fire.
Anyways, my mother's friend went to the hospital with 3rd grade burns all over her body (lab coats weren't fire proof, so she literally became a human torch), and then she died because her skin couldn't work. If a person has 3rd grade burns there isn't a cure that you can apply. You can give her only first aid and hope that the surface of the undamaged skin is big enough to allow the body to expell toxins, sweat and things. If it isn't, the person will just die. You can't do anything.
I have been wondering if bits of charcoal can work to stop bumping but would the heat and elemental carbon start a reduction in the hot acid to hydrogen sulfide?
Oop, ment dioxide, lol, that's a delayed notice
Does sulphuric acid also form azeotrope with water just like HCL ?
yes