greenyppols
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Distill Chloroform...
I also acquired a 14/20 glassware set...learned the hard way the difference between that and 24/40..oh,well..the smaller unit is probably better as a
beginner set-up for me anyway...
So I followed the forum recipe with bleach and acetone..several times!!! and I believe I have somewhere around 100ml...and being kinda picky about
purity, I wanna distill in a...warm water bath, right? As the bp of chloroform is 62c, a water bath would be easiest 1st time for me to attempt,
right?
I have read these forums some..I bought some glindemann sealing rings..I read somewhere about acid going through grease..
I dont even know how much chlorobutanol I made from instructions here..but Im not sure about a mixed solvent recrystallization yet..I dont have
ethanol yet..my mash should be clearing up soon and hopefully will have..ethanol by Friday..
Yeah, seems like a lot at once, but I've been reading the books from your servers here also. Many thanks!
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runlabrun
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You want to be very careful about vapours leaking from your distillation set, do this disto outside preferably.
But yes a warm water bath and increse temp very slowly so you dont alot of bumping in such a volitile distillate as chloroform this would be not a
favourable thing to happen.
Just take it slowly and do it outside with plenty of air flow, chloroform will knock you on your ass at a low enough conc to not be realised easily.
-rlr
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neutrino
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A water bath should be fine. Bumping can be easily avoided by adding some boiling stones (unglazed porcelain).
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greenyppols
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outside, next time
ah, live n learn.
runlabun - Hot water bath on stove (darned cold outside last night) thought all sealed nicely. Nope. Kinda stinky. In a nice way I guess. The 100ml or
so is now less than 50. I'd guess 40 since this container isnt graduated.
Afterwards I thought, thats probably why I can run a line from the vacuum port to vent any smells? doh.
Not anhydrous, I can see droplets of water. Is this where a dessicant dryer?(saw one on ebay) would work? Or soak with calcium chloride(i think) thats
been baked and re-distill?
Seems I lost a lot? Probably crummy yield because I essentially dont know what Im doing, what would normally be expected to be "lost" in a
any purification, of anything? Or is it a real-wide swath of possibilities depending on ability?
I used a vigruex on top of a small rb flask and another condensor after the thermometer adapter, but didnt run water through the condenser..should I
have? I didnt because I thought I read because of the low BP it wasnt necessary, really, but now I think that I should have to cool it even
more..might that have been it?
I dont really intend to make more, just was messin' around, but might try to dry it much better if I do, next time.
neutrino- I didnt use a stone. I remember now having read somewhere to always use one..but I didnt..I will remember next time
Thanks
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neutrino
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Sorry, but adding calcium chloride won’t help. The hydrated form is slightly soluble in chloroform, so you can’t filter it out. Redistilling will
invariable carry over a good deal of the water, as you’re basically steam distilling the water with chloroform. If you just want something decently
dry, though, it should work. If you really want something dry, add concentrated sulfuric acid and separate the layers later.
You have to run water through the condenser <b>especially</b> is it’s a low-boiling substance. You can only neglect water with very high
boiling substances, using an unjacketed leibig condenser.
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runlabrun
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oh please say you used a condenser....
Without this most of your chloroform would have been away with the vapours of air....
To avoid moisture will be hard... you made your chloroform from acetone and bleach which both contain shit loads of water...
As neutrino said, distill your crude chloroform next time and add conc sulphuric acid (very slowly) to the distillate flask, run it down the side,
dont drip it in to the distillate... dont want chloroform splashing up at you do you??
Agitate and keep adding cycles, then seperate the layers in a sep funnel. Wahlah, dry chloroform.
-rlr
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greenyppols
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runlabrun - yeah, I did use a condensor but I didnt run water through as I said. I used two actually. A vigreux on top of a 250ml rb flask, to
claisen and another condensor..which is the one I didnt have water running through..or anything else to cool, for that matter. I see the posts here
now with a PVC cooling tower.
neutrino - Im going to check on adding concentrated sulphuric acid, which I have now after boiling battery acid a few days ago. thanks
I did and do expect to make more than my fair share of goofs. I counted on doing any of this to have a sharp learning curve. Live n Learn, I always
said.
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