In this video, I make acetic anhydride using the ketene lamp I built in part 1. Support my channel with Patreon! / dougslab
Пікірлер: 255
@adrianhenle8 жыл бұрын
I would never have the balls to switch that heating element on without running the apparatus under positive pressure of inert gas. Kudos on your immense testicular fortitude.
@Oli-jm9fc6 жыл бұрын
balls of steel indeed
@cravenmoorehead70993 жыл бұрын
Saculus in latin
@bobsinclair39933 жыл бұрын
Please explain this for me Adrian im fascinated
@bobsinclair39933 жыл бұрын
Couldn't you just use a ventilator on a separate oxygen line from the room?
@getmeoutofsanfrancisco99173 жыл бұрын
@@bobsinclair3993 He means purging the apparatus via vacuum and reintroducing an inert gas (nitrogen for example) in order to remove/replace all oxygen which could potentially lead to fatal consequences (combustion/a bomb). Bomb = bad.
@samhood79868 жыл бұрын
I always thought ketene lamps were stories chemists use to scare their children!
@DitchChipsNsourCream2 жыл бұрын
That's the best way to stop children turning into self righteous imbeciles.. the invisible danger. Covid. I mean. Yeah.
@freon5008 жыл бұрын
Doug, you're suggestion to use a smoke bomb to test the ventilation in the smoke hood and lab area is well taken. If there are problems evacuating the smoke out of these areas you need cross ventilation, what is known as "make up air". Particularly and most commonly if you are in a basement in the winter you will have negative air pressure the indoors relative to the outdoors, this negative air pressure must be dealt with. Cross ventilation will make the space colder but it will provide you with the essential fresh air. The way to test for negative air pressure in the lab area is to open a window or door to the outdoors or turn off the fan in the fume hood and see if air rushes in through the openning, if it does you have negative air pressure. Hood fans, which are exhaust fans, can't overcome negative air pressure because the more air they pump out of the room the more negative the air pressure, the vacuum, becomes. By the way, sometimes you don't need a second fan, all you need is to leave a window or door open to the outdoors across the room to let the air in. We love our chemists and we want them safe.
@DutchPhlogiston8 жыл бұрын
Well done, brave man, and a great account of the synthesis, thanks. I would recommended using a second bubbler to eliminate residual ketene in the exhaust though.
@_arthurski13378 жыл бұрын
Maybe fork out $1000 to encase the apparatus in a nifty acrylic enclosure, with water sprinklers on top, to douse the mess when the whole shebang blows out. That might save a chemist life, and his cat Schlipsi's too.
@_arthurski13378 жыл бұрын
*pumped to negative pressure.
@jonross3773 жыл бұрын
@@_arthurski1337 It wont blow if you know what you are doing. Dont attempt it if you dont fully understand what you are doing.
@bdot028 жыл бұрын
Couldn't help but wear my safety squints while watching.
@bensons9998 жыл бұрын
+bdot02 "safety squints" I love it! Hahaha.
@Len_M.8 жыл бұрын
AVE. :)
@chemistryscuriosities5 жыл бұрын
Safety squints ingaged
@russellhamner48982 ай бұрын
A little ketene never hurt anyone, other than all of those people it hurt and killed.
@xeigen28 жыл бұрын
Well I don't think I'd do it myself, but it was great to see it done! Very interesting process.
@blairlattimer77352 жыл бұрын
Absolute mad-lad; this is great chemistry content.
@minipac28 жыл бұрын
I've been looking forward to this!
@emanuelnemec7 жыл бұрын
Dude you're smart. Thanks for the video !
@elliotwilliams75234 жыл бұрын
One of your best videos!
@flaplaya7 жыл бұрын
Wow this looks dangerous.. I seem to remember him talking about an inert atmosphere. Heating a NiCr wire in the presence of acetone.. Not for the faint hearted. Really cool video and I've honestly never heard of Ketene. Learn something everyday.
@mehdituran19187 жыл бұрын
Excellent, I really enjoyed this
@MrEbenezer137 жыл бұрын
Awesome stuff man! SO glad I started subscribing to your channel!
@philipstowers4741 Жыл бұрын
Absolutely inspiring.
@charlesthomas79707 жыл бұрын
I might have missed it, but it looks as if the reaction and work-up were done without an inerting gas. Granted, the volume of the system is fairly small but best practice would be to inert the system prior to introduction of reagents. This is something that I have to do often at work (chemical plant operator) for safety reasons. Great video, I really enjoyed it.
@zuthalsoraniz67645 жыл бұрын
It probably feels more acceptable to be a bit more "cavalier" about the safety procedures if a) doing them might not be so easily available to you as an amateur and b) it's just your own life that you're putting on the line, as opposed to the lives of everyone working in the plant and potentially people living nearby.
@chemprofdave5 жыл бұрын
I think a tank of arc-welding gas (argon/CO2) would be a good cheap way to get the oxygen purged out.
@EddieTheH Жыл бұрын
@@chemprofdave That's what I use but it does require a lot of drying first. I'd bubble it through H2SO4 (actually piranha to be overkill) then through a drying line of anhydrous Mgso4.
@AugustusOakstar4 жыл бұрын
Very Impressive, you have given me great impetus and making my own Ketene lamp. I’m just waiting for a 500 mill chromatography reservoir and then I’m going to get busy too. Vogel shows a ketene lamp but it varies a bit from your design, you showed me that it doesn’t have to be 100% equivalence. And my design certainly is not like yours, I’ll let you know how my first acidic anhydride turns out. Thanks Doug, you are quite the chemist. I have always been drawn to physics, but of course had taken my share of chemistry courses. Most of them had been in organic let’s face it most of the interesting things are in the realm of organic chemistry. The fact that a Nobel laureate described the blue color of an alkali metal dissolving in anhydrous ammonia as the solvated electrons from the metal just blows me away. Everybody had seen it, but the person who secured it out that’s figured it out, won the Nobel prize.
@AugustusOakstar3 жыл бұрын
@@NerdyNEET hi, I have refined my ketene lamp several times and would be happy to get back to you with some photos.
@bruse87788 жыл бұрын
Awesome video. A proper walkthrough of the safety precautions you had in place would be neat.
@bjthinks8 жыл бұрын
I, too, am curious about this. Were the ground glass joints well greased? Did you provide secondary support in case one of the orange clips snapped? How far back into the fan alcove did the exhaust tube go? Etc.
@JRScience8 жыл бұрын
Great video! Out of curiosity, what was your PPE for this video? Given that you were dealing with such toxic substances were you using any form of respirator? If you were, what canister did you select? Cheers! keep up the great work!
@stanwashighski35533 жыл бұрын
Hoods good you good🤓
@quickminutetv41705 жыл бұрын
I like the idea
@mimoshwarring14326 жыл бұрын
Xcellent very nice stuff
@kerrycollins9597 Жыл бұрын
A very useful compound indeed
@ATLTraveler4 жыл бұрын
Careful. I made one of these when I was 16 and the DEA came to my house (not joking). Turns out acedic anhydride is exactly what you use to convert morphine to heroin and i had googled so much stuff about it they came knocking. Because my parents are rich and we had a really nice house they thought we were heroin kingpins. I just explained to them i was interested in chemistry and they were actually really cool, i cant remember if they told me officially it was illegal to make or not but basically told me i would be fine as long as I didnt sell it or, of course, start making heroin. One of the guys left a coffee mug that says DEA on it so I have proof.
@elsdiv39332 жыл бұрын
Post mug
@FeR-kt1jt2 ай бұрын
That’s why you use glacial acetic acid to reflux with morphine to get 6monoacetylmorphine which is stronger than heroin or just as strong 😎
@lagrangiankid3782 ай бұрын
It's impossible they came just because you googled it. Maybe a neighbor or someone snitched on you, otherwise they don't just arrive like that.
@kieranodea7716 жыл бұрын
Smoke bomb is a good tip, I use the big 6 inch ones you can pick up at any fireworks stand. I had to use that trick to make sure my hood is good enough for me to safely work with phosgene. I still used a respirator though
@AtlasReburdened6 жыл бұрын
You can make a useful smoke pen out of nothing but tightly rolled paper towels. It doesn't exactly plume huge quantities of smoke but it naturally smells terrible, being burning cellulose, and you can use the scent as an indicator of fume hood failure while still getting the benefit of being able to accurately test small cross sections of the flow path.
@jvanasselberg6 жыл бұрын
Amazing! BTW, I hope to never live downwind of you... Ever!!! LOL
@UC2358 жыл бұрын
You're mad. Absolutely fantastic, though. Have you considered deliberately producing diketene? Ethanolysis gives ethyl acetoacetate which otherwise needs to be made through the low-yielding and laborious Claisen condensation.
@bruse87788 жыл бұрын
+UC235 You're still around? :O New videos from you would be awesome. Any plans of doing that?
@DougsLab8 жыл бұрын
+UC235 I'll have to write this one down for a rainy day. The catalyst tube would be the hardest part, but I have an idea already about a type of apparatus with a liquid-only return path... hmm.
@jonhoyles7148 жыл бұрын
+UC235 wave @ UC235 hi buddy hope to see more vids soon :)
@gogear1318 жыл бұрын
your big words confuse me
@bensons9998 жыл бұрын
+UC235 Wow! I thik I subbed to your channel a _loooooong_ long time ago! :)
@psycronizer8 жыл бұрын
" to show that this is really acetic anhydride, I've got some morphine mono-hydrate here and we'll just reflux that in just enough anhydride to cover it...mmmm thats a tasty little treat mama....the final product is so good that it was used to stop babies crying, to treat alcoholism, oh and just about any other pain you could think of, not to mention being used as a CURE for morphine addiction..hahaha..yes it's true....that's the crazy crazy world around the 1900's..ever get the feeling we are deprived from having the freedom to try new and different things?
@bcubed727 жыл бұрын
+psycronizer Considering that plain ol' benzoic acid has all the same lipo-solubility bennies of AA, it's peculiar that folks hold AA as some sort of Holy Grail...I've heard (second-hand only) that dibenzoyl morphine is every bit as life-destroyingly wonderful as, well...
@psycronizer7 жыл бұрын
....to us chemists's out there, we all know that both the benzyl and acetyl derivs of morphine are of course just esters, both of the OH groups on the Heroin are esterified, of course one of those OH groups is alcoholic and the other phenolic, which naturally means that there is a different rate at which the esterification reaction occurs for both groups, with the more acidic phenol group reacting a lot faster than the alcohol group. But here's my point, it is STILL just an esterification reaction, between and carboxylic acid and hydroxy group, these are traditionally catalyzed by a small amount of strong mineral acid, so, I would bet my left testicle that it could be achieved with either acetic or benzoic acid with say one percent dry HCl as a catalyst dissolved in some methanol as the solvent...it might take 24 hours of refluxing to be absolutely sure to push the reaction all the way, but I see no reason why it wouldn't work.
@chemistryscuriosities5 жыл бұрын
psycronizer how would you get "Dry" hydrogen chloride as its just chlorine desolved in water?
@chemistryscuriosities5 жыл бұрын
@@11Rastafari11 yes I know. Oh I get it now it just dawned on me you bubble the HCL through sulfuric acid or pass the gas through a disaacant like CaCl or P2O5 right?
@11Rastafari115 жыл бұрын
@@chemistryscuriosities yes that's right. You can add suf.acid to NaCl to produce HCL and Na2SO4. The Hcl is then dryied through CaCl.
@p.f.30147 жыл бұрын
I admire your courage. Would the cyclohexane to 1,3-butadiene reaction be any safer to try?
@shonkysidewayssam61346 жыл бұрын
I can’t wait until the day I can have my own lab, that is not under threat from raids.
@leenolan23392 жыл бұрын
The simple way to make this is 50ml of acetone and 1ml of hydrochloric acid hope you have a good lab
@Finnnicus8 жыл бұрын
Also is this purely to show how to produce ac2o or do you have further plans for a compound using the anhydride you made.
@squirreleyy8 жыл бұрын
Great video Doug. It's hard to see the layers of acetic anhydride and water on the video. Do you think you could add a small amount of dye to the water? Maybe it would help with the visualization of the two layers? I'm not sure.
@BackYardScience20004 жыл бұрын
A black background would be great too.
@TheBookDoctor8 жыл бұрын
Ok. So if you suddenly stop producing new videos, we'll know why...
@DougsLab8 жыл бұрын
+TheBookDoctor Bah, I filmed this three days ago. Safe and sound. :) Also, as you probably saw, I usually buy my Ac2O. I just wanted to prove it could be made at home.
@JoeHeiserA8 жыл бұрын
+Doug's Lab Where do you get your commercial Ac2O from?
@blackirish7814 жыл бұрын
I'd like to know too
@SuperAngelofglory4 жыл бұрын
@@DougsLab there are other ways to make Ac2O at home
@Andrew-my1cp4 жыл бұрын
@@SuperAngelofglory how?
@David-fh6rr6 жыл бұрын
Can you use this aperatus to produce acrolein from glycerin?
@Finnnicus8 жыл бұрын
If you used larger ketones would it work just as well? Say propanoic anhydride from methyl ethyl ketone. Also do you plan to use this apparatus for other pyrolysis reactions? There are a lot of interesting synthesises (sorry) around pyrolysis but proper apparatus, particularly apparatus that gives good yield, is hard to make/come by.
@scowell7 жыл бұрын
Bhopal, baby!
@wubblybubbly55588 жыл бұрын
What gasmask filter type are you using?
@bensons9998 жыл бұрын
Just stumbled on your channel by accident- great video!(I subbed instantly!!!) You've got a fantastic setup there dude! It puts most of my lab equipment to shame! Have you purchased all your lab aparatus and chems yourself?(Privately, I mean?) Do you hold any kind of licence that enables you to purchace labware, chems, etc? Appart from just being interested,(nosey!) I'm curious because I've found it quite difficult to buy (even very common) chemicals from chem supply places here in the UK, more often than not having to resort to finding substitute chems/chems that are used for other purposes... It's a *huge* pain in bum,(!) so much so that I often end up having to give up on a project before I even start it! :'( Really looking forward to having a look through some of your videos! Cheers!
@allenrowe67783 жыл бұрын
Try buying chems in New Zealand, what a nightmare. All the anti Meth laws have made it ridiculously hard. Hydrochloric, Sulphuric, Acetone, Toluene are all on Precursor list. What will be next Water?
@rockinbobokkin78317 жыл бұрын
New subscriber. Great stuff! I've read that taking essential oils or aromatics from roses is challenging. Do you care to tackle that?
@homesynthesis6 жыл бұрын
Amazing. I've been designing my own but alas it likely will stay just a design as I have no fume hood currently. Where did you get the acetic anhydride? I've been trying to get my hands on some for a video on acetylsalicylic acid but the only way it seems possible is to go all the way from urea and acetic acid through acetonitrile (thanks to Chem Player's fantastic video on the subject), but it would be super nice to just be able to buy some (I don't have a business or company i.d. so, unfortunately, that doesn't work entirely).
@erikshaw15118 жыл бұрын
Hey Doug, I have a few questions, if you would be so kind to take the time to answer them, it would be greatly appreciated.. What type of respirator cartridge do you suggest using on a full face respirator when generating ketene? What gauge nichrome wire did you utilize for the filament? Can this be used with other species of ketones for example, Methyl Ethyl Ketone, to generate propionic anhydride? I think it's great that you've utilized standard apparatus to assemble a ketene lamp, I have contemplated doing the same but have yet to have the chance to set it up and work out the kinks myself. I look forward to your insight, thanks
@tolyan9756 Жыл бұрын
This comment is 6 years old, but I'll respond for the curious. To generate propionic anhydride you would need to pass ketene into propionic acid, obtaining mixed acetic-propionic anhydride, and then to slowly distill mixed anhydride with second molar proportion of propionic acid. Also works with any other carboxylic acid. That's from Vogel's Practical Org. Chem. p. 694.
@shainemaine12683 жыл бұрын
Hey if you can find a way to get your percolation to form smaller bubbles, and used a taller/thinner collection vessel, you'd likely increase the ketene absorbtion
@shainemaine12683 жыл бұрын
@@NerdyNEET thanks, you taught me about a piece of equipment I'd never heard of before!
@erikshaw15118 жыл бұрын
Hey Doug, One more important question I forgot to ask, what glass tubing " borosilicate, flint?" and size " inner diameter, wall thickness, outer diameter?" did you use to insulate the "12 gauge??" copper lead wires...
@SuperAngelofglory4 жыл бұрын
If I ever try this (which I doubt), I am pretty sure I will use flame to burn the methane and traces of unreacted ketene and als will flush the setup, when the reaction is done, with some butane, which I will also burn. Ketene is no joke.
@cappnzak7 жыл бұрын
Correction: it looks to be a Friedrichs-type condenser you're using at the first stage reflux? In short, I'm asking are they better performers than the regular,(read cheaper;) )kinds one could use? Thanks.
@noncustomcarsbikes94905 жыл бұрын
Please mention about the quantity of the chemical to be used for producing acetic anhydride will be waiting for reply thank
@christopherblanchart84012 жыл бұрын
Hi Doug, a quick question: what was the temperature of the acetic acid before going up to the reflux?
@rareearth74668 жыл бұрын
wouldn't this synthesis be a lot safer under argon or nitrogen flush ?
@jhyland873 жыл бұрын
I was thinking the same thing.
@jonross3773 жыл бұрын
How exactly would you do that? The atmosphere will become acetone and then ketene regardless of how you start the lamp.
@rareearth74663 жыл бұрын
@@jonross377 it removes the excess oxygen and does not react with anything
@jonross3773 жыл бұрын
@@rareearth7466 I said how, not why.
@EdwardTriesToScience3 жыл бұрын
Pull a vacuum, then fill it with an inert gas, repeat for a few times, or leave the acetone refluxing without the coil on, and the acetone vapors would displace the oxygen anyway
@st4ble8698 жыл бұрын
From which book did u get the set up? What sort of metal is the wire?You said NiCr or Chromel i think. Kanthal should also work?
@wubblybubbly55588 жыл бұрын
What are the side products when making acetic acid via this method?
@hughiemac7 жыл бұрын
where does the exhaust of the fan go? Is there a filter on it? Or is 5 ppm no too important when released outside?
@cravenmoorehead70993 жыл бұрын
Giant sacculence...respect
@brannonmcclure27864 жыл бұрын
Thanks.
@user-rd6pg3rz4q6 жыл бұрын
How isolation mix a acetic acid and acetic anhydride? And whate is test acetic anhydride in laboratory? Thanks for this video
@wubblybubbly55588 жыл бұрын
If you want to make glacial acetic acid vie this method, what temperature would you distill at, and would it have to be fractional? Also, would it be possible to make the generator out of steel pipes that would be welded together for minimal gas escape?
@chrishill42658 жыл бұрын
I'm looking into this as well
@0x73V145 жыл бұрын
you can buy inert welding gas from any welding shop that way you can fire it up without the step of "turn it on and hope the acetone displaced enough oxygen
@_arthurski13378 жыл бұрын
Doug, is a "lamp" the only way to achieve thermolysis? If you used a steel tube heated by a flame or electric resistance to pyrolyse the acetone vapor, could it be made to work as well ?
@DougsLab8 жыл бұрын
+_Arthur Ski There is nothing special about the lamp other than it exposes acetone to high temperatures. Glass tubes would also work just fine if you could get them hot enough. A steel tube would not work very well since traces of acetic acid that form in the refluxing mixture would slowly dissolve the tube. Even my NiCr wire is corroded so badly it cannot be used after 30 or 40 hours of operation, and must be replaced. Many ordinary metals would not last very long.
@_arthurski13378 жыл бұрын
Yes, the iron would both corrode and mess up the reaction, and the fittings between steel and glassware might be tricky. And nobody can afford a platinum tube just for that reaction. Oh well.
@SuperAngelofglory6 жыл бұрын
is adition of ketene to hypochlorous acid resulting in chloroacetic acid ?
@_arthurski13378 жыл бұрын
I read that carbon disulfide is normally used as a catalyst for the thermolysis of acetone into kethene/ethenone. How come you're getting decent yields without using a catalyst ?
@DougsLab8 жыл бұрын
+_Arthur Ski A catalyst is often unnecessary. It simply lowers the activation energy required to make the reaction happen. In some cases, getting the molecules hot enough to react without a catalyst destroys them in the process, so those reactions require catalysts. This one doesn't need a catalyst, but a catalyst would reduce the energy required and improve yield. I don't have CS2 though, so I ran without.
@SolarSeeker452 жыл бұрын
So it makes water into 70% acetic acid but stops at some point and if you start with high concentration it makes glacial acetic acid into the anhydride. It seems to me you could combine the high purity product with the low purity product and bring it all the way to anhydrous. You could probably use a separatory funnel and a claisen adapter to gradually dilute the product dropwise as you're bubbling the ketene into it.
@sabz44597 жыл бұрын
Good work sir the system is totally close.methane and other products like methylene and CO may generate pressure within the system
@mishmash69912 жыл бұрын
To: Doug's lab At the very end how cold or warm is the distilled water in the 3 tubes ? I'm curious cuz I'm wondering if it matters like if it was hot would that mess it up the same with cold or warm,its probably room temperature.
@rezasahab63518 жыл бұрын
Hi, I just got this system for the production of acetic anhydride repeatedly tried but ultimately failed. Please guide me and tell more details.How much acetone and acetic acid is used?
@WeebRemover4500 Жыл бұрын
it seems this method either works, or it simply doesnt. other variations using a copper tube have also been used but people report either success or nothing at all variation in wire temperature etc seems to make zero difference in my world i cant even get the acid to gain weight, its supposed to go from 120g to 200g at 100% vinyl acetate may be another route catalysed with palladium chloride or copper chloride
@brandonross6083 Жыл бұрын
You got some cahones brother. Geez! Would love to have a chat with you tho. Obviously you know a few things
@thrdel6 жыл бұрын
Bro , you have a very detailed warning about how dangerous Ketene is . Now, I've seen quite a few videos about Copper Catalytic Pyrolysis of Acetone done at home , in schools , shows / presentations , etc. Didn't see anyone dropping down dead yet. Is it possible that they are all morons ? And if so, how come no one died inhaling that stuff ? Don't get me wrong, we can all see that you've done your homework and the quality of your videos is top class . The question is just out of curiosity and not a critique of the video.
@user21XXL5 жыл бұрын
the catalitic reaction of acetone is carried out in oxygen atmosphere - this should limit ketene production,
@zodd00017 жыл бұрын
how do you purify the product ?
@skidderjohn8 жыл бұрын
very nice Doug this is amazing! chemistry is very awesome i would love to chat with you an pick your brain some day please
@bpark100015 жыл бұрын
Whenever you have electric heaters with exposed connections, it is safer to use an isolation transformer between the Variac and the load. Even better would be a 120 to 48 volt transformer. Wouldn't moisture in the air quickly destroy escaping ketene as fast as it escapes?
@jonross3772 жыл бұрын
Wish he were around to answer this question.
@HyunAYuchi8 жыл бұрын
Any chance you're going other to make other crazy chemicals in the future? Like SO3 and reacting with HCl to make ClSO3H :D
@hes-labhcm66047 жыл бұрын
Hello Doug - this video is awesome, more than great :)) I'm trying to buy some commercial Anhydride Acetic like the one in your video (wiki says it is low cost) but it is hard to find an online shop, can you tell me where to buy that cool liquid?
@DavidL-qb8cl4 жыл бұрын
Lmao you can't. It's a controlled substance in most countries
@SweMateo4 жыл бұрын
@@DavidL-qb8cl Avaliable on ebay right now if you look.
@fmdj3 ай бұрын
1:00 no worries even though I like doing dangerous stuff I'm really not planning on attempting this (especially with my chemistry lab being my kitchen at the moment), but I find the "ppm" unit absolutely non intuitive. I have no idea what "1 ppm" represents in practice. I know it is very little but how much so? I guess the point I'm trying to make is that I think it could be useful to express these thresholds in a way we can relate to, like (just an example, dunno if it is the correct order of magnitude at all) "this is the equivalent of 1ml uniformly spread inside of a football stadium" or something like that. Imho it would help convey the danger level better cuz I'm not sure if many people have an intuitive representation of what "1 ppm" is. I know I don't.
@lagrangiankid3782 ай бұрын
1 ppm, or one part per million by volume, is just one ml of gas per cubic meter of air. Considering that a football stadium has a volume of as much as 1 million cubic meters, one ml per football stadium would be 10^-6=0.000001 ppm. Personally, to get a better idea of the toxicity, I like to use the LCt50 reported in the literature to calculate the total lethal dose you'd have to inhale (assuming a respiration rate of 6.5 liters per minute). For example, ~130 mg of chlorine gas are the average human lethal dose, compared with ~20 mg of phosgene, 12 mg of hydrogen cyanide, 500 μg of sarin and 200 μg of VX nerve agent.
@mikechambers91296 жыл бұрын
FYI, Doug, the Patreon link from this particular video is broken.
@hsnizdkh95354 жыл бұрын
Dear sir.I did that process carefully and step by step as you did.but the result liquid solved easily in the water.The question: Should I purefy it by distillation?
@alexakennedy6704 жыл бұрын
I’m imagining you filming this in a scuba suit
@psycronizer8 жыл бұрын
yeah, I've seen the Vogel set up, and I suppose as long as the reaction tube is rated to handle those high temps, and you expell the oxygen from the atmosphere, is should,nt go kaboom. Personally...I'd be using a stainless setup for something that, err lively..and not starting with glacial acetic is just madness.
@Oli-jm9fc6 жыл бұрын
I was thinking the same, shouldn't you use a quartz reaction chamber for this? If that shit cracks it can mean your death. Also, I'd feel safer to purge everything with nitrogen or argon first.
@bromisovalum84173 жыл бұрын
doesn't the flask that holds the hot wire have to be quartz for safety?
@MostFolkCallMeOrangeJoe8 жыл бұрын
I would be shitting myself turning on that nichrome in case it ignites the acetone vapor.The upper flammability limit of acetone is about 13% so it's not a problem but it would still be on my mind. This is a very cool video, I love seeing big glassware setups like this. What can acetic anhydride be used for?
@NatureHacker8 жыл бұрын
acetylating things.
@DougsLab8 жыл бұрын
+Adam Harrington Yes, I have to admit that's a bit of a clench moment. :) Ac2O is used in a ton of stuff. Fabric fibers, plastics, pharmaceuticals, explosives. It's a very useful thing to have.
@Marwie948 жыл бұрын
+Doug's Lab Isnt it better to run quick vacuum on the setup before refluxing?
@danawold45478 жыл бұрын
+Doug's Lab : So, are you saying you could make fibers to turn into yarn, then weave into airbag cushions and then use the other half to make propellant for inflators?
@adrianhenle8 жыл бұрын
It's best to do the whole thing under inert gas pressure, but that's pretty tough if you don't have some special equipment. Standard stuff for a modern lab, but outrageously expensive. Vacuum wouldn't work all that well, especially in this exact setup, because when the vacuum is relieved, the system would back-fill with atmosphere and you'd have to start exactly like Doug did anyway (purging the air from the system with acetone vapor).
@NatureHacker8 жыл бұрын
What is the immediately dangerous level of nitrogen dioxide? Because that you can readily sense and unless you are locked in a lab you wouldn't let yourself get poisoned by it because it burns.
@DougsLab8 жыл бұрын
+NatureHacker NO2 was 68ppm but was revised to 20ppm conservatively. See here: www.cdc.gov/niosh/idlh/10102440.html
@dmartinster12 жыл бұрын
I live in Australia and have tried this experiment many times as per this video's instructions precisely, with locally purchased ACS grade acetone, but unfortunately could not get any gas production, could anyone offer any suggestions as to why no ketene was produced?
@WeebRemover4500 Жыл бұрын
im trying too, i do get gas formed. you might wanna increase wire temperature, ive seen 650-750*C as ideal, if no gas is produced you have leaky glassware, glue all joints up or grind them together with Cr2O3 i do get gas and some ketone formed, but zero anhydride- it seems that either this works or it doesnt, im doing a run out of frustration now where im having acetone AND glacial acetic acid in same vessel, supposing the ketone will be absorbed into the acetic acid- its plausible that acetone+water would form acetic acid in this kind of setup i found some hints on acetic acid used for ketene generation as well, supposedly filaments can last a bit with acetic acid vapors acetone+ketene yields isopropenyl acetate which can also be used for forming acetic anhydride by glacial acetic, a bit of conc H2SO4 and isopropenyl acetate
@christopherleubner6633 Жыл бұрын
I made ketene by utter mistake when i was a kid. I used air over acetone as a bunsen burner and it had some steel wool as a flame arrester, well it didnt work like that, the iron worked as a catylist and oxidized the acetone to ketene and formaldehyde ☹😵😵😵
@surplusdriller17 жыл бұрын
its toxic, but will it not be quicly hydrolysed in air to acetic acid? as long as the hydrolysys isent in your lungs ur fine
@chrisfromnz30385 жыл бұрын
Are those weight figures correct? 30.9gms to 52.5gms? Shouldnt it be 32.5gms? Gaa is 1.03gm/ml and a.a. is 1.05gm/ml
@nnamrehck Жыл бұрын
Cool video but you are crazy to make such a toxic compound in a home lab!
@WeebRemover4500 Жыл бұрын
its not that bad, some sources cite that its about 1/5 as toxic as chlorine gas
@jean-yvesboilard62287 жыл бұрын
Would like tout se you synthesis acetylacetone with your lamp.
@MarshalDavid7 жыл бұрын
Why in the flask is a golden color ?
@cappnzak7 жыл бұрын
"Degradation products",David. I believe I heard him mention it somewhere during the vid.i e breakdown material from the copper wire and the nichrome wire. It looks like the nichrome discolors and suffers a little from the high temp and may shed a little of it's material as the discoloration in the flask.Just a thought.
@russellhamner48982 ай бұрын
So before turning on the filament / heating element, you can be assured that there is no more oxygen in the lamp (or at least not enough for an ignition event) just by the flowing acetone vapor? That part scares me more than the muffkin' ketene as I can shield myself from the ketene gas with a proper vent hood and respirator, but an exploding ketene lamp is harder to shield from. For educational purposes only; m0rphin3 is bad enough WITHOUT being tampered with.
@MrTheboffin Жыл бұрын
For safety I'd have bubbled what was coming out though a large container of water with a pH indicator. Provided the reaction with ketene is 100% or close to that then when the water colour changes, I know the reaction has fiinished.
@emmepombar33283 жыл бұрын
Could you use a similar setup to make Formaldehyde from Methanol?
@WeebRemover4500 Жыл бұрын
that requires airflow, silver or platinum can be used for that iirc without needing to be heated
@emmepombar3328 Жыл бұрын
@@WeebRemover4500 Do you have a source or a paper?
@WeebRemover4500 Жыл бұрын
@@emmepombar3328 nope, but it can be done using copper where its heated redhot and then an air-input is directed into the alcohol, and an air-outlet pulls out the formaldehyde fumes, it has been done in glass jars with metal lids by a fellow chemist the methanol variant has tendencies to blow up however so you want decent airflow control to prevent, and some safety measures to prevent a massive fire as well.
@emmepombar3328 Жыл бұрын
@@WeebRemover4500 Have I understood that correctly? I let air bubble through MeOH, catching some MeOH fumes, which then stream over red hot copper catalyst forming formaldehyde? tbh, that sounds like boom. Really air?
@bobweiram63213 жыл бұрын
Can you just use acetylene?
@luiseduardogonzalezgranado30282 жыл бұрын
Is there a way to contact you by email? what voltage did you use on the resistor
@raju99505007 жыл бұрын
Sir 70 % ch3cooh & 30% c3h6o = 100% c4h6o3. Possible????? Please reply me sir
@wubblybubbly55588 жыл бұрын
God damn it doug, what are the sideproducts. If you are trying to not get me killed by not giving me info, I tell you that I have already run the generator to produce acetic acid, none died, but I still need to know the sideproducts if I want to get the acid glacial.
@josephstalin34508 жыл бұрын
i think you got the chemical formula of keten wrong its H2C2O not C2O,besides that great video keep up the good work
@DougsLab8 жыл бұрын
+Joseph stalin It's common in org. chem to use shorthand notation which assumes hydrogen saturation. The 2 hydrogen atoms are implied.
@Thebarnardfactor8 жыл бұрын
+Doug's Lab NEVER QUESTION THE GREAT LEADER
@jhyland876 жыл бұрын
Interesting how Wikipedia doesn't have squat on the toxicity of ketene, such as its IDLH value you mentioned.
@jhyland873 жыл бұрын
@@NerdyNEET Yep, I did after posting the above comment (and I just deleted my last reply to you. I replied to the wrong thread, stupid me).
@forestdenizen64974 жыл бұрын
So if one filled a vape tank with acetone, then inhaled helium and blew through the vape while holding the fire button, one would expel deadly gases into the atmosphere?
@zippy37116 жыл бұрын
I thought my hobbies were all over the map.
@MisterLove9996 жыл бұрын
Good job, absolutely brilliant :) Such a beautifully simple and useful process (notwithstanding it's dangerous nature). Have you tried the red hot Cu catalyzed pyrolysis of acetone instead of heating with a glowing wire ? It doesn't (AFAIK) require additional heating past the initiation, since it's exothermic enough to keep the Cu glowing. The difficulty is of course in designing it as a closed system... How to heat your Cu catalyst to glowing red inside a closed apparatus. A worthy challenge perhaps ? Thank you.
@ddawnvit4 жыл бұрын
It's pyrolysis and broken chinaware pieces can be used instead of copper wire coil. Heating is done externally. Industrially, stainless steel equipment is used.
@melody37415 жыл бұрын
Does ketene feel like phosgene? I inhaled phosgene once, it was rough LMAO.
@tracnemaker1234 жыл бұрын
A lucky nigga you are
@timecode374 жыл бұрын
Are you sure it was phosgene?
@GlossKarin5 жыл бұрын
Great video! But there is a mistake in ethenone structure, one of the carbons lack two hydrogen atoms :c
@kingkarlito2 жыл бұрын
when chemists draw organic molecules all carbon atoms are understood to be fully saturated with hydrogen atoms, unless they are otherwise noted. a molecule like propane would be drawn like /\, which tells us the structure is H3C-CH2-CH3.
@GlossKarin2 жыл бұрын
@@kingkarlito Yeah, I know what you mean. But when you use that type of notation ( /\ ) you do not use the symbol C. For ketene you either put =C=O (like here pubchem.ncbi.nlm.nih.gov/compound/ketene#section=Structures ) or =•=O (like you can sometimes see for allenes etc.) I think putting a C=C=O is incorrect. Hope this helps.
@edwardarruda72152 жыл бұрын
I'm retired chemist and agree never do this at home...so you should do it? BTW, is this your mom's home?
@marcingoawski93058 жыл бұрын
Now, let's make heroine! Oh, you need morphine too? :-( So why is acetic anhydride restricted here where I live?...
@chrisfromnz30386 жыл бұрын
All you need to make a heroine is a brave lady....heroin on the other hand.....
@SuperAngelofglory6 жыл бұрын
yes, this is why (CH3CO)2O is a controlled chemical in most countries (and I so hope heroin drugg lords will try to make it from ketene)
@Astaldoath5 жыл бұрын
if you think they cant hire corrupt chemists who know how to do this you are an acetic asshole XD
@forestdenizen64974 жыл бұрын
@@Astaldoath is a chemist who works on chemical weapons for the govt also corrupt?
@BackYardScience20004 жыл бұрын
@@forestdenizen6497 we're talking about drug lords and drugs. Not chemical weapons. Stay on track.