Just bought a new distillation set. Always wanted one, but never had the money to actually get a decent setup - but taxes solved that.

Got the 1000ml RB distillation flask with 500ml receiving flask, Vigreux fractioning column with thermometer adapter, Liebig condenser, vacuum distillation adapter, and an optional 3-way distilling head with thermometer adapter. Plan on getting a lot more to toy around with, but was wondering about a couple of things...

First off, how do ya'll dry ya'lls flasks out? Every time I try to dry out the 1000ml, water just stays in there. Most of my flasks don't have a problem drying on the inside, but two of these just don't want to... Sep funnel seems to do the same thing. Stupid question, but I can't see how to dry the inside.

Two... I've gotten siphons going on the cooling jacket of the liebig condenser going, but I would prefer being able to leave the distillation running by itself without checking the siphon every 2 minutes. What do ya'll do to keep water flowing?

Also, not that it's that important right now, but what do ya'll suggest for a vacuum? I heard water aspirators would due good, but just don't know.

Been using cooking oil to heat the distilling flask, takes a long time to heat up though. Any suggestions on better heat? I was thinking about a heating mantle, you know the one that wraps around the flask, but am undecided about what to go with so far...

Thanks!

I dry my flasks either by air-drying, or for stubborn ones I toss in a teaspoon of dried MgSO4 , cap it and shake it around for a little while then recover the salt later on. I always get water trapped around the valve on my sep though.

Water aspirator has always worked fine for my vacuum, but I'm not pulling anything too high, mostly just solvents out of solution so heavy pressure isn't an issue. it really depends on what sort of duty you're putting it to.

EDIT: For liquid baths I use DOT 5 silicon brake fluid, sort of an industry standard in these parts. Otherwise, my ghetto mantle (nichrome in a plaster cast on a dimmer switch) or a vermiculite bath.

The proper way to dry a flask is first to properly clean it, and once clean and as dry as possible, shake around a bit of acetone in it, dump all that out, then set it upside down in an electric oven set on the lowest setting for just a bit, with the door slightly open to allow any possible fumes to escape.


As for you water source, I suggest you do some nigger rigging and run that shit to a spigot. A quick trip to the hardware store for some long hose, and a few well chosen adapters and you are in business. Remember, coldest possible source=stronger vac power, if you choose to use a water pressure vac system. Old fridge compressors work well too.


I hope you got a vac takeoff adapter for your receiving flask. You should also make sure to get some kecks, as well as a good reliable heating source, mag stir hot plates are the shit, as well as steam bath, and oil/sand baths. The choice of oil depends on your use. Really, your choice of heating method in general depends on use.

Also, not sure what kind of three way adapter you have, but if the main vertical joint is a ground glass, and not a tapered thermometer slide like on some, then you should get an addition funnel in the size of that ground glass joint there.


Now, with some work, and extra parts for quick conversions, you can perform thousands upon thousands or procedures. Steam distill, reflux, react under inert atmosphere, all kinds of shit.

Cleaning flasks: As Noob said - acetone is the thing to get the flask dry. The acetone is miscible with water, as well as volatile, thus can remove the residual water easily.


Vaccuum source: Just remember that water aspirators go through a LOT of water... something like 10-15 L/min IIRC


Heating source: Get a stirrer hotplate. Silicon oil is good for heating, maybe peanut oil at a pinch...?

I do not have much to add as everyone summed it up nicely

bu yeah heating mantles are the shit! But get different size ones, expensive but worth it! Also always two magnetic stirrers, because if one craps out you can straight away continue.

If you do not mind what size is your glassware? i presume 24/29 (USA standards if i am correct). But yes as Stupid Noob once you have the basic bits, nothing can stop you only time i guess

Oh and while we are into this:

-Most of my glassware is quickfit, also i have some little platsic clips so keep it together (i will put pictures up if you do not understand what i mean), what temps will they get without melting?

- I recently aquired:

1 x 500 ml 3 neck flask
1x 10000 ml 3 neck flask

Both are 29/32 joint size, i can't find any bits of glass to go with this , i looked on ebay and no one has any! Does anyone have a shop in europe where i could buy glassware of this size?

(SN, if this is sourcing just edit the last part of my post out)

As a general rule, the higher quality the oil, the higher the temperature it gets before it starts smoking. Silicon oil is probably best, as it has excellent heat conduction and has to get to9 a very very high temperature before it starts to smoke.

Unfortunately, silicon oil is also pretty expensive, and I, being a cheap bastard, prefer to use a simple sand bath - no worries about it boiling/decomposing/beginning to smoke, and has acceptably good heat conduction.

Obviously a fine grain of sand is preferred, as this will give you a more dense medium, and a closer fit around your flask, resulting in more even heating.

Oh, and do want pics of the setup please

Here are some random set up:

My new "stand" It works pretty well
http://img150.imageshack.us/img150/4134/11022008001sg7.jpg


This set-up doesn't have much use but it looks pretty nice (maybe the addition of two liquids in a solvent to form a precipitate and to remove the solvent ? dunno)
http://img120.imageshack.us/img120/1615/11022008002kt6.jpg

Regular distillation set up:
http://img137.imageshack.us/img137/4628/11022008005bi6.jpg

Yes i know i need some more stands, but i haven't finished make them yet

And some more joint clips, otherwise your lovely glass is going to shatter on the floor...!

I know! But they tend to be expensive! Even on ebay

Those plastic clips are called kecks, I mentioned them in a previous post, and they stand up to extreme temps, not exactly sure how high though. And yes, they are a must. Someone I know was distilling AA and the graham came off the three way and started dripping AA into the oil bath, as well as putting out a shit load of AA gas.


Not fun to fix, and scary as fuck, could have been prevented with 10 bucks worth of plastic.