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Author: Subject: Boiling off organic solvents
Rich_Insane
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[*] posted on 23-1-2013 at 21:39
Boiling off organic solvents


Hey everyone:

I have a product which was reacted in a little too much xylene, and it is slightly soluble in xylene, so there is likely a lot of product dissolved in the solvent. Now, I know I have to boil off xylene, but I am afraid to do so. I cannot go outdoors to do this because it is very cold (around the freezing point of water) and I am using a cheap cooking stove as a hotplate. I have qualms about boiling a volatile, highly flammable solvent inside my house -- I also get a lot of lung irritation from the vapor at STP , let alone a cloud of vapor from boiling solvent.

Is xylene volatile enough to evaporate rapidly in air? Can I just boil it down in small (~20 ml --> 10 ml with about 160 ml total, final volume intended at 80 ml) aliquots? Suggestions?
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Sedit
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[*] posted on 23-1-2013 at 21:46


Why not make a getto distillation of sorts to either recover your Xylene or at the very least dispose of your vapors.




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Rich_Insane
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[*] posted on 23-1-2013 at 22:02


What do you reccomend? I have a distillation apparatus, but no ring-stand, no thermometer adapter and no pump to cycle water through the jacket.
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Tsjerk
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[*] posted on 24-1-2013 at 05:13


For the pump part, you can hook it up on your water supply directly. It sounds like a waste of water, but if you hook up the water supply on the bottom you only have to run a very little amount of water to keep your condenser cool, If you really don't want to waste water you can probably turn it on for a couple of seconds once in a while, depending on the rate you're distilling with and the size of your condenser.

A thermometer isn't necessary in your case as you just want to boil down, just put something in the hole to close it.

A ring-stand you should just buy.
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smaerd
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[*] posted on 24-1-2013 at 06:24


Xylene will evaporate in air no so much in the winter time. Not a good idea to evaporate the stuff inside your house.

Maybe boiling it off through a plug of dry activated carbon could help to remove some of the vapors. Ultimately though you should really invest in a distillation apparatus + ring-stand & clamps which recycles the pump water(pond pump).

Might be able to do a short path-distillation(flask, thermometer adapter, vacuum take off, flask) with no condenser(depending on how much solvent you want to boil of and how well your compound can handle heat), run a hose from the vacuum take-off out a window or something.




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