NurdRage - 2018-01-27
In this video we purify and dry highly contaminated diethyl ether using potassium hydroxide and sodium metal. To a 500mL portion of dethyl ether we add 30g of potassium hydroxide and stir over night. The diethyl ether is then decanted off the aqueous layer of dissolved contaminants. Now 10g of sodium metal are added to the diethyl ether and the mixture stirred while loosely stopped to allow hydrogen escape. After all visible hydrogen evolution ceases (usually about one day) the flask is tightly stopped and allowed to stir vigorously until the sodium metal begins cold welding together into larger and larger aggregates. Alternatively, for professional labs, 0.2g of benzophenone maybe added before sealing and the color change to red or purple is indicated. This takes a couple of days but can take a week. Then the diethyl ether is distilled and used immediately for grignard reactions. Donate to NurdRage! Through Patreon (preferred): https://www.patreon.com/NurdRage Through Bitcoin: 1NurdRAge7PNR4ULrbrpcYvc9RC4LDp9pS Glassware generously provided by http://www.alchemylabsupply.com/ Use the discount code "nurdrage" for a 5% discount. Social media links: Twitter: https://twitter.com/NurdRage Facebook: https://www.facebook.com/NurdRageYoutube/ Instagram: https://www.instagram.com/nurdrageyoutube/
ahh, how you always choose the catchiest titles
yeah, pure clickbait! :)
Apologies for the lateness.
The whole grignard project was about 6 videos worth of work plus failures. I'm currently editing them together into seperate topics. The first one is this video, preparing the solvent, since grignard reactions are so dependent on good solvent that they deserve a special video for purification. The second video will be on performing the grignard reactions theselves, I performed 4 reactions to make 4 different products but i'll be putting them together into one video. The third video will be on testing the products to make sure i performed the reaction correctly.
NurdRage love your videos buddy!
Are you speaking with Hamilton Morris about being on his show? It would get you some exposure to a new demographic of fans.
What’s a grinyard reaction?
Grignards are much easier to initiate when using the Iodide, rather than the Bromide or Chloride. I synthesized benzene from sodium hydroxide and sodium benzoate, cleaned it up and used it to synthesize Iodobenzene and then produced PhMgI with ether fresh out of the bottle. Initiated withing 10 minutes. According to the label, the ether I used was "for photographic purposes". Go figure.
You forgot to shoutout your patreon supporters (but whatever, less clutter in videos is better IMO)
Would liked to have seen you cut open the sodium at the end 😊
I agree, that would have been neat.
I only figured it out long after i had finished the experiment and was cleaning up. But by then i had already squeezed out the lump so could no longer film it. I agree it would have been cool. If it happens again in the future i'll be sure to do it. :)
Ah yes, that old chestnut from Dr Julius Sumner Miller:
"Do What You Oughta, add Potassium Hydroxide to your Ether to Absorb the Wattah"
Ummmm... benzophenone is easy to find now. I remember I looked for some back in 2012 and couldn’t find it so ended up trying to synthesize it (screwed up the synthesis somehow so just ordered it from Fisher). But yeah, it’s out there now.
i haven't been to find it outside of lab suppliers. Where have you been finding it?
NurdRage I bought 500g on Amazon for around $20
interesting! i guess i need to make an update :)
why pay for a degree when you have the whole local library in your bedroom.
3:39 a friend of my mother died in that way
Pietro Tettamanti was it triggered by sodium reacting with the water?
Joey Valladared no, she was just distilling it and added the boiling stones while it was superheated. As nurdrage said, it became a fireball of burning ether.
Joey Valladared Fun little story: At university we were shown the reaction of sodium metal with water on a small patch of grass right outside the building. As we all know it reacted with a nice loud "bang". Immedatly after that a bunch of bunnys ran away in panik and a small bird dropped dead of a branch.
What does the term "amateur" mean in this case? You seem to be pretty experienced, sorry if it's a dumb question, but I'm curious
He means somebody that isn't in a professional laboratory with simple access to chemicals like benzophenone. I doubt he could just buy it off ebay for usage at home for example
Neutralise Music Oohh, makes sense. Thanks :)
amateur = doing it as a hobby, not as a job
professionals do stuff for money, that does not mean they are better at that, just that they do it as a profession
This isn't something I'd do in a home lab. Back in 89, I spent the summer in Chicago helping to synthesize taxol. The lab had an ether still. It was probably the most dangerous thing in the lab. We were next door to Dr. Eaton's cubane lab, so no one worried about us. (Except when the vacuum trap turned blue...oops)
Great video series. As an ex-chemist, I love watching your videos. I really hope they help foster a new generation of chemists for research.
5:38 Isn't it bad to distill it to a flask without an adapter? It maximizes contact with air and moisture.
User THC Exactly what I thought...
Same, usually drying tube attachment on the adapter and then straight into a round bottom
Love watching your videos, chemistry is so amazing to watch like this.
Aww, I wanted to see the ball of sodium up close :p
We need to donate some stir bars to nurdrage. I usually throw mine out when they turn that color.
I love you and your science. I live how your teaching me stuff and don't even know it.
Amazing stuff, I've been a subscriber for a long time and can't wait to see more new content
Awesome. This would sound weird anywhere else, but I love chemistry. I wish I had focused on it in my studies. It’s a subject I’ve gained a lot of interest in, due to my career progression. But I never had the chance to study in a lab, under an experienced person
Everything wrong in chemistry seems to result in explosions or toxic gas... kind of hard to feel comfortable getting into but I love watching the videos.
Lab safety is very important.
8th comment and 300 viewer ;) Luvv ur vids bro <3
just great! I await your Gingiard!!
will this process remove any heptane contamination from starter fluid separation?
no, you'll need fractional distillation for that.
Hey. can you please show the powerful reaction of Chlorine trifluoride oxide (ClF3O)
thank you.
Do you look up things like the NaOH goo formation vs. KOH layer separation or do you just know that from experience? Just seems like a very specific tidbit of information. Very useful.
you either learn it from experience or you have lab assistance while you´re at university telling you. you´d be surprised how many things you learn there already just from talking to your colleagues/profs/TAs. tidbits like that probably are results of experience by some but spread due to people talking about it. you´ll hardly find literature about something like that, but colleagues will tell you or will be grateful if they get a tip like that from you
I come back in my house from my chem lab (Sodium/Potassium cyanide and I see ,, new video from NurdRage"
Nice
I store my ether over potassium hydroxide and frequently check for peroxides.
thanks a lot
Nice science experience for schooling children (thanks)
Could you please do a video on making 4-(N-Ethyl-N-2-hydroxyethyl)-2-methylphenylenediamine sulfate?
Gimmie shoutout
Dr Butyl Lithium, I have some ether that is highly contaminated with visible peroxides (flat white flakes). Can this be salvaged with your method?
if it's that badly contaminated then discard it. That level of danger is not worth working with. To salvage something like that you need to first perform a reduction step. But still, don't bother.
NurdRage dam, I was afraid you'd say that. Thank you
do you think you would be able to make Aluminium oxynitride, a Ceramic glass
You are the best!
Did you see codyslab was taken down again?
What is your way of attaching tubing to a water supply? I had to use glass tubing with a bung. Is there a better way?
Would be funny if it was a way to make perfect sphere of sodium.
So that's how they make Sodium Balls !!
Can you make a video on how to recristalice substances with slightly different solubilities.
Mexi Chemia you must find a solvent in which they have different enough solubilities.
Pietro Tettamanti i mean inorganic salts, like sepairing KCl from NaCl as an example
Mexi Chemia crown ethers is all that I know. Or maybe there is a method that involves the polarity difference of the two ions. Our nerve cells can do this.
A rough method that can more or less work is this, but it'll be really imprecise and I don't even know if it is possible to do. You can just boil it down. The sodium chloride should precipitate first, and when all the sodium ions are gone, the potassium chloride will precipitate. But you must know the exact concentration of the sodium chloride, otherwise you won't be able to tell the difference.
Pietro Tettamanti thats the issue
Although I remember Chem Player did a video on a dirty and wet Grignard and it worked better than you would think.
very easy alkyl halides like ethyl iodide can work in wet solvents. But hard alkyl halides like chlorides require better conditions. Also, even if you have the grignard, water considerably reduces yields. Ultimately, you have to decide if you desire higher yield or reduced work. But just because something can be done badly doesn't mean it should be.
We don't have benzophenon what else we can use?
We're making thf anhydrous
What type if molecular sieves would you store the ether with? 3a?
I wonder what the point of using such a large amount of sodium metal is? There should only be a very small amount of water left after drying with KOH?
I Imagine purifying THF would be ultra similar?.....
Could you make a video on a more efficient essential oil distilling apparatus the amount of oil you get is just so small compared to the amount to hydrosols is just inefficient and time consuming
See all of his Soxhlet Extractor videos - this is one of their main purposes. Especially the first one where he shows how you jerry-rig one from more common glassware (although a proper Soxhlet is better.)
+
Can you do experiments with chlorine plz?
You are an organo metallic compound.
Pressing thin wire from sodium metal is relatively easy and safe. Due to the enlarged surface the drying process is more efficient and goes a lot quicker.
Thank you for the video! Will this method also work for dioxane that has been stored for a long time? I always worry about how to deal with peroxide formation.
yes, it works very well with dioxane. Although i'll make a separate video for dealing with large amounts of peroxides. For exceptionally high levels of contamination you actually use another step first: a reduction step with sodium metabisulfite or iron chloride. Then you do the potassium hydroxide and sodium after. (but i'll make a video on that)
NurdRage Thank you. I appreciate that very much.
Pretty neat how the sodium formed a hollow ball like that... :)
He said it was hollow and my first thought was, 'that would probably make an interesting bang if you tossed it in water.'
I'd say I'd be a bad chemist, but the Klapötke lab exists and actively tries to make things so explosive they can't even get (good) measurements on it (like C2N14. It really doesn't want to exist (*14* nitrogen atoms in one molecule, mostly bound to themselves!), and will express so with all 357 kcal/mole that went into making it).
A couple of points if I may. 1) I would use a ground glass connection on the receiving flask. 2) Locate the receiving flask a little further away from the heat source. 3) Collect the diethyl ether in an ice bath. 4) pH Test Strips. 5) Do not use the molecular sieves because of reuse problems. 6) Use KOH for ether storage in a labeled clear reagent bottle with phenolic screw top secured with plumbers' tape on the inside, and electricians' tape on the outside. 7) Refrigerate ether when not in use. 8) SDS (MSDS) And last, but not least, 9) Peroxide test strips. Have a blessed day.
aetius31 - 2018-01-27
The poor stir bar have gone through some serious shit lol