An undergraduate student working close to me decided to evaporate off some diethyl ether by holding an open round bottom flask (RBF) over a Bunsen Burner. Inevitably the ether ignited. She was hand holding the RBF, which was overflowing flames onto her hands. She held it for a while, not knowing what to do, and then threw the flask resulting in a lab fire. Take care with ether!
Dear god man I was ranting and raving about all the missteps you took along the way but you actually did it in your own haphazard fashion yields be damned. Congrats really
I used to have a collumn with the glass beads in, I wasn't sure how much difference it made til I broke it and switched to a normal vigreux. Turns out they actually do make quite a difference! They're super easy to break when cleaning though.
Question? When I clean my flasks, crystallization dishes, test tubes ex. I usually use piranha solution, but how and what do you use to clean out your columns, safely?
@@MichaelLapore-lk9jz I usually use piranha too, though it depends what I've run through it. Sometimes I'll use various solvents that are suited to the contaminants before a final piranha wash to get stuff sparkling.
Is piranha solution one of those mixtures of acids? (I vaguely recall _aqua regia_ is something like hydrochloric and sulfuric acids, able to dissolve gold.) I'm guessing piranha solution is something that completely evaporates though, yeah?
Cyanoacrylate glue works pretty well to repair broken pestles. Mine broke similarly and glued it with CA glue it lasts many years before you have to re-glue it.
Welcome to wonders of distillation. With something like 6 plates or so you never get close to 95% from 40% in a single go. The key is to adjust temperature to keep the flow not too high ie. column reflux ratio higher. Often it is quicker to make a couple faster distillations at higher flow rate than a single very high reflux rate distillation. Distillation seems so simple in theory but when you look more closely into it, you quicky notice you always get a mixture with the unwanted components.
Maybe if you use Sodium Carbonate to seperate the water from the Ethanol and then distill the Ethanol after seperating. But thats not really the same as distilling it if you first seperate it.
@@TjallieBrrr You probably mean potassium carbonate instead of sodium. It is one well known method to separate water and ethanol. Indeed, those are quite different methods than simple distillation. Many other methods like extractive and azeotropic distillation are also possible and often used industrially.
@@hoggif Potassium Carbonate works better but Sodium Carbonate also works, ive tried it but never distilled it so i dont know if Sodium Carbonate is completely insoluble in Ethanol. It also seems to be fairly dependent on temperature or else the Sodium Carbonate will crash out if too cold. I tried it with Vodka and when its warm/hot it will seperate into 2 nice layers. Just a small expiriment i did a couple years ago
@@TjallieBrrr That was interesting to find out. Everyone seems to use potassium salt due to very low solubility. I have to give that one a try some day. Sodium carbonate is dirt cheap and so readily available. I checked up some data and at 30C it has solubility of 30mg/100g in 95% ethanol, about 1g/100g in 50% ethanol and about 2g/100g in 40% ethanol. Slight solubility is probably not a problem because it will most likely be redistilled anyway.
@@hoggif yeah thats exactly what i was thinking. I have no idea how i got the idea of doing it, i remember scouring the internet and couldnt find anything and at some point just tried it and found what i just reported to you. It would make Ethanol purification st home much easier. If you tried it let me know please
If you want to get 100% ethanol, you should minimise contact with air and store it under argon (better in Schlenk tube). When I tried to get absolute ethanol by triple azeotrope (benzene, water and ethanol), even doing inert distillation I got only 95% ethanol, because it is very hygroscopic
You did mess something up there. 95% can be achieved with good distillation only. I don't know what didn't work out, but something is off there. EthOH is hygroscopic, but it is possible to get it virtually anhydrous.
@@Psychx_ Probably yes, but you need a lot of it. I have never done that. There might be a risk of dissolving some of that in the residual water, which then lingers as contamination of your ethanol. It is mostly used to absorb, what molecular sieves can't or would take very long. Good distillation: >94% Sieves: 99.x% MgSO4/CaCl: 99.9x%
Why not just add some calcium metal pieces to it or calcium oxide? im pretty sure that should make it very dry you just have to distill with a baked apparatus to remove any calcium in it.
Ahh. Devil ether. It makes you behave like the village drunkard in some early Irish novel. Total loss of all basic motor skills. Blurred vision, no balance, numb tongue. The mind recoils in horror... unable to communicate with the spinal column... which is interesting because you can actually watch yourself behaving in this terrible way... but you can't control it.
@vylbird8014 I’ve never tried ether, but after reading tons of anecdotal reports on Erowid back in the day, no. It’s different. Ether is more potent as a GABA-A agonist and has a higher affinity for the N-methyl-D-aspartate receptors as an antagonist, so it’s like drinking combined with taking dextromethorphan (found in NyQuil) except it takes a lot less to get you plastered. Then again, if you drink enough vodka…
Nice, I like the idea and side content. Unfortunately here in Germany it's illegal to concentrate ethanol that isn't denaturated, even if it's already taxed. So we have to use denaturated alcohol for things like this. A few recommendations: - Stonehard material can better be crushed in a plastic bag with a hammer. Don't forget to wear safety goggles when doing this! Commercial boiling stones are still the best choice and not too expensive at all. - Azeotropic ethanol can be dried with calcium oxide, molecular sieves can be used to keep it dry because anhydrous ethanol is hygroscopic. Never heat the dried solvent together with the used drying agent because it might give back the water. Anhydrous sodium sulfate is better suited as a drying agent than calcium chloride because CaCl2 forms adducts with many organic solvents. It should only be used in drying tubes or desiccators, not in the solvent itself. - This way selfmade diethyl ether might also contain traces of highly toxic and carcinogenic diethyl sullfate. Avoid inhaling the fumes! - Never store highly volatile and flammable substances in normal fridges or freezers, because they are not secured against explosions! - Diethyl ether and other peroxide forming solvents have to be tested with acidified iodide starch solution every time before heated. Never rely solely on your stabilizer. - Whereever possible replace diethyl ether by methyltertbutyl ether which is much less volatile and flammable and doesn't form any peroxides at all. - Since conc. sulfuric acid in any form is banned for hobby chemists in the EU, anhydrous zinc chloride can be used here instead.
I am surprised at how obedient you are to your gumment! Here in the USA we have a third finger, plus we have GUNS! Remember, your gumment wants you in a kid's playpen with plastic dolls for entertainment!
Kolumne frakcyjną polecam owijać kawałkiem koca a nie folią aluminiową. Folia sprawia że kolumna nie ma gradientu temperatur (za bardzo się nagrzewa na całej długości) - zwłaszcza te specyficzne „chemland’owe” z kuleczkami. Owinięcie kocem daje perfekcyjną separacje destylowanych frakcji.
For a better yield, use the sieves the ethanol was stored over as the nucleation material for the dehydration step. Zeolite beads nucleate even better than silica quartz. There's no need to separate the dust from the sieves. The drying power of the sieves would itself help drive the equilibrium forward. And you get back the ethanol that would've been lost to adsorbtion into the macro-scale porosity of the beads. (Only water can enter the pores in the zeolite crystal matrix itself, but you do lose some amount of any other material to the larger-scale porosity between different crystal grains.)
What do you think of this, will it also loose alcohol: Adding desiccants like calcium oxide (quicklime) to absorb water from the ethanol. Calcium oxide is also cheap and easy to get and maybe good for a DIY process.
was good to see someone performing this function, as I have been planning on using the function to make ethylene gas for conversion into polyethylene plastic polymer and do some testing to try and insert other atoms like sulfur into it for conductive polymers such as pedot (plan is still to make both N and P charge doped polymers for semiconductive traits so layered we could make things like solar cells that are transparent, experiment with various frequency responses and clear OLEDs and such :)
Pro tip: Store your diethyl ether in an aluminium bottle at room temperature. It will build up a bit of pressure and you'll loose a few microliters every time you open it, but that way you don't have to put it in a freezer/refrigerator and especially don't have to let it warm up to room temperature before using it (to avoid condensation. This is applicable to everything, if you don't let it warm up to RT before opening it, condensation will build up and your product will take up moisture). Of course except if you live somewhere with temperatures much above 30 °C... Then I would put it in a fridge, but only an EX certified one! Don't put flammable substances in non EX certified fridges... It can end badly... With a fridge getting blown through a wall and spreading the chemicals inside it everywhere... You really don't want that to happen... If you're lucky with the climate and your lab AC and heating is bad, your ether boils in the summer and your DMSO freezes in the winter 😂
@@Milkex... iron is better, limits the buildup of explosive peroxide. Add a rusty nail for good measure. Those premixed two cycle chainsaw fuel containers are perfect and people who use them tend to treat them as disposable so easy to get for free and already marked with flammable liquids labels!
@@darnoc4470 I don't have an article , it's just something multiple teachers told me 30-40 years ago .. preferential oxidization of the iron. It's actually something I intend to do an experiment with, since I've had this discussion with other people.
@@petevenuti7355 reactivity sequence of metals? something like that? been the same time since i was at school but seems to stick in my mind from somewhere.
1:30 It looks weird , just watching it bro. I feel ya. I mean, Im just curious about this subject after watching other things, And Ive always know ether existed and some of its uses trying to learn more about it has been a troublsome bother.. Thanks for the video. I leave a Like.
Bro, awesome video as always! Could you perhaps show us how to distill sulfuric acid safely to concentrate it from battery acid ? It's unfindable in Europe in concentrated form, and it's literally one of the most useful reagents ever.
Thanks! I will definitely do a video about concentrating sulfuric acid sometime in the future, I also have to use only the non official sources of sulfuric acid and recently I came arcoss some proffesional drain cleaner which is dirt cheap and consists of pure sulfuric acid, maybe in your county you could get something similar :)
@@Amateur.Chemistry Could you maybe point me to where you find drain cleaner like this ? I'm sure there's a way, I can definitely clean the acid but concentrating it makes me anxious af because heat + sulfuric acid on your skin and you become carbon 😃
I get my drain cleaner from a local online store, I don’t even need to purify it because it is just clean 96% h2so4. Before discovering this method I distilled battery acid but it was a mix of pain and danger and I am still afraid of it
If you think one fractional distillation column is bad, try 3 on top each other with 3 outlets. Only the top needed water cooling, the middle was air cooled, and the lowest was short path.
@evilplaguedoctor5158 I didn't have anything particularly harmful running through it. But I did have the excess gas/vapor run outside through a bubbler first.
6:46 lol 😂 Glas bubbles having a mental breakdown 😅 Very interesting seperating column! I prefer using the good old vigreux column 😊 Or if I really need insane seperation and time, yield and amount isn't a problem, a simple glasstube filled with small pieces of glass tube.
Try putting a good handful of table salt into the ice-water baths, it will significantly bring the liquid water temperature down, closer to the temperature of the ice. I imagine it would stay at a low temperature longer too. Alternatively you could just put a very strong saltwater solution ( not supersaturated, keep adding salt until it stops dissolving) in a freezer for a few days. I found that a chest freezer works best.
where i live, you can buy 195 proof (97.5%) wood grain alcohol without any kind of license. it is actually sold as a drink for some unholy reason. and it is literally just ethanol made from wood (usually pine trees) and then distilled down to 97.5% purity. its actually quite pure because it is meant for human consumption. i once drank a double shot of it straight and its the only time i've ever had a hangover in my life. a lot of chemists where i live will buy this alcohol and use it for experiments because it saves so much time and is WAY cheaper than "lab grade" distilled ethanol
6:39 Do not insulate your distilling column, the whole point of all those steps is to condense water and drip it back into the flask. If the temperature is too high you will not fully get that effect.
I really don't know why all of you amateur chemists have to shake liquids every time they're in bottles. This shaking not only means that the oxygen in the air above the gas space of the liquid diffuses much faster into the liquid. The same also happens with the air humidity. Just as a small example. If you fill sodium-dried diethyl ether from one bottle into another bottle the humidity introduced during decanting is already sufficient to affect very sensitive Grignard reactions, sometimes to completely prevent the formation of the Grignard reagent. So if you have half-full bottles with a liquid that should be anhydrous, don't shake the thing, so as not to speed up the absorption of O2 and H2O. If you want to carry out chemical syntheses, you should get used to the right way of working from the start. This comment is by no means meant to be malicious. It is only intended to make it clear that the correct handling of chemicals is just as important as the entire synthesis route. Chemistry is a wonderful natural science. However, reliable results can only be achieved if you use the same correct working methods as the author of the paper.
90% using a massive fractionating column starting from vodka! I think this column should be returned to sender. I think the boiling flask was not big enough for this setup; more boiling material + more wattage of heat would have meant a better throughput, which would have meant you wouldn't need to insulate your column as well, and you would have collected much more in a small period of time.
Having done quite a few distillations of ethanol myself, this was pretty frustrating to watch. It should take no longer than an hour per run for an entire liter. Also, like someone else stated, even with good reflux, you won't be able to get all the way to your target in one go. So my suggestion is: jack the set temperature much higher and do two or three runs.
When distilling alcohol in general, and ethanol in particular, monitor your temperatures and know your boiling points (watch for when the temperatures stall as comparing with lab pure boiling points are not reliable). In my setup fractioning between methanol, ethanol, water, and impurities stalled around 168F, 184F, and 202F, and nothing useful came over higher than that. The lowest stall is methanol that I save for camp fuel and other experiments (nitromethanol is not nitromethane, but still interesting), the middle stall is ethanol at around 70% At the high stall I was getting around 40% but mostly water (your experiment was here, so you pretty much moved the solution from one flask to the other. ...just watch Moonshiners. It's pretty much exactly the same process). Save each "stall" in a separate flask (Your commercial vodka should only have a speed bump if at all at the low-stall point, or you have a lawsuit to persue) and check periodically on the high-stall to see if it is still flammable. Stop when it doesn't light anymore. You can then re-distill the high-stall end with the same process as many times it takes or as long as you care, and add the mid-stalls to the first run until the high stall is just boiling water or the boiling stops above the high-stall but below boiling water. Re-distill the mids, and you should get between 80-90% (I got 95% on one run (mid of the mids), and seived that part to make a bit of homemade E85 gasoline)
I was hospitalised with tonsilitis in 1969 and remember the nurses waking me up in the middle of the night to give me ether “So you get some sleep” (Nurse logic) It smelt and felt horrible.
That type of fractioning column is easily flooded, which is what you did, thus making it rather ineffective and slowing down your distillation as well. You need to go slower with it
Great video but one thing you need to do when giving long technical names like ingredients is to add some subtitles. Your English is good, but it me a while to realize you were saying " Sulfuric Acid " and I know it wasn't what yt CC said you were saying ( Saturnic Acid ) 🤣
Quick check: If it says 80 Proof or 40%ABV on the bottle, then 40% or 2/5ths of the bottle is Ethanol. Detailed check: Pour your distillate back into the vodka bottle. If it was 80 Proof/40%ABV if your product is 90% it should be Original%ABV+(product%-100%) full or in your case 40%+(90-100)% or 44% of the full bottle. Or take starting volume x %ABV (I'm guessing 750ml Vodka x 40% or 80 Proof) should have netted you about 300ml ethanol + (100-Distillate%) or 330ml@90%ABV. OR knowing that a 750ml@40%ABV will have 300ml Ethanol, fill the empty bottle with 300ml of the original or water, and draw a line on the bottle at that level. Pour your distillate back into the empty bottle, and see how close you get above that line. Divide 300 by total distillate 330, and you get 90% (well...91% by the math, but I will cut a fool who ever uses the term "significant figures" with me)
THANK YOU, I REALLY ENJOYED YOUR HUMOUR -SO I SUBSCRIBED, AWESOME WORK , MUCH APPRECIATED. SORRY FOR *SHOUTING, I JUST STEPPED ON MY NEW GLASSES,,, ((AT LEAST I DIDNT PUT THEM IN THE MICROWAVE ,THIS TIME,,,SO IM HAPPY,,)
Get a pc cooling pump with reservoir and radiator and mount it on a small plate. Then you have a great setup for later distilling that does not need refilling ice all the time.
22:53 It doesn't just evaporate very quickly and accumulates on the ground, it also has a tendency to build peroxides, who are basically tiny spontaneous ignitors. Better test your ether for peroxides before using it. There are cheap indicator strips available.
4:40 Instead of the tedious making glass fragments in order to use them as boiling chips, I'd use little glass spheres, 5-10 mm diametre, with a bore and a "frosted" rough surface. I bought some dozen online. They are offered for the making of decorative, cheap jewelry.
"Ah, devil ether. It makes you behave like the village drunkard in some early Irish novel. Total loss of all basic motor function. Blurred vision, no balance, numb tongue. The mind recoils in horror, unable to communicate with the spinal column. Which is interesting because you can actually watch yourself behaving in this terrible way, but you can't control it."
