Distillation Setup

[Oh-Hungee]

I've been contemplating getting into distillation. This is something I would be a complete beginner at, and I was hoping to get some advise on the best equipment to get. My initial interest would in distilling DCM out of paint stripper, and possibly recovering other solvents used in older extractions. I'm also interested in steam distilling essential oils, but this will take extra parts and it'll probably be something I'd try later.

A local store sells distillation kits, and the options I have are between a 300mm liebig or graham condencer, and between rubber or ground glass joints. My concern with the rubber joints is they might react with the solvents and contaminate the final product. I was thinking maybe I could use cork or some other alternate material joints. The main issue with the ground glass joints is that it would be more expensive, and this would mean that I would have to show multiple forms of ID and fill out special paper work. This is something feel a bit leery about.

My best guess would be ground glass, especially for the non-polar solvents. Maybe a graham condenser, but I'm less clear about all the pros and cons between these types. Thanks for any suggestions.

 

[Oh-Hungee]

In the setup that they're selling, rubber stoppers are used to connect the boiling flask to the kjeldahl bulb, and then to the condenser. From the reading I've done so far, some people say the rubber stopper will not be problem with non-polar solvents, while other say it's a big no no. There are two methods I read about people using to deal with rubber reacting. One is to wrap the rubber stoppers with teflon tape, and another is to use cork stoppers that have been soaked in waterglass.

I've been extra conscious of material compatibility after seeing how effectively limonene dissolves nitril gloves.

 

[Oh-Hungee]

I think that glass joints will be the way to go. I suspect the rubber stoppers maybe made out of neoprene. From all my searches, this seems to be the most common material rubber stoppers are made out of. Looking over a material compatibility chart its not recommended for a number of solvents, such as: xylene, toluene, heptane, dcm.

The main drawback for me is going to be the price. For all the glass adapters for a steam distillation setup, the cost is really going to add up. I guess I'll just get a few of the parts at a time.

Thanks for the help.

 

[downwardsfromzero]

In my part of the world there's a healthy market for second hand lab glassware, but then there's no daft law about showing ID for glassware purchases!

I hope your project is proceeding nicely - give me a shout if you need any help, I absolutely adore distillation!

 

[downwardsfromzero]

Here's a pic of a distillation setup I once had:

Some of it is wrapped in foil but it's all ground glass joints: 3-necked flask with thermometer adapter, fractionating column, 'swan neck' anti-splash head, Thorpe condenser, straight vacuum receiver adapter, receiver flask. A pleasure to use with a good heating mantle.

 

[Tranzcentral]

Glass ground joints 100%.

Make sure you buy lab grade grease also.
Invest in a magnetic stirrer also, you'll always use it.

Wow an old school set up. In that pic, your flask is way too full.:shock:

 

[benzyme]

[YOUTUBE]

 

[Tranzcentral]

[YOUTUBE]

O.M.G!!!!!

Did i just see a rotovap?:shock:

I could play that over, and over, and over again....

Just when i thought i had a good set up, you have blown me away...beautiful energy in that room.

If you have more youtube videos like that, i would really enjoy watching...such a sexy video.

I know i'm smitten..