distillation apparatus

[Comandante]

I've been wanting for a while to try out extracting different scents from different plants but I'm lacking one crucial piece of apparatus, namely distillation set (or more precisely, the condenser part). They are available for purchase at very expensive prices so I was wondering if anyone has any ideas on how to make one that would work for my purpose...

 

Considering other equipment, I have beakers, flasks, round bottom flasks, funnels, tubes, I have water and heat source etc... I was thinking of using polystyrene test tubes and then cutting and melting them such to make something that resembles a condenser, but before I go on with that I just wanted to see if anyone has any other ideas.

 

I've looked around and found some interesting setups, this being one of them: http://orgchem.colorado.edu/hndbksupport/dist/distsetup/distsetmain.html

 

and these being many of them; http://images.google.com.au/images?q=distillation+apparatus&hl=en&um=1&sa=X&oi=images&ct=title

 

Wiki also has a nice diagram of how everything should look like. Basically I need to extract some of these; http://en.wikipedia.org/wiki/Essential_oils using http://en.wikipedia.org/wiki/Distill .

 

And one other question, rather noobish, am I heading in the right direction here? Is this how scents are usually extracted in perfumery? I have a notion that a lot of scents are lab synthesized these days...

[YT2095]

this: http://myweb.tiscali.co.uk/yt2095/experiments/still.jpg

although crude serves me quite well, from alcohols to bromine or acids.

the vapor gets chance to cool a little in the glass pipe but since the end of the tube is in a receiver vessel that IS kept cool, all the real condensing takes place in there

 

that`s certainly One way you could do it, and the glass tubing I bought in 500mm lengths and are quite easy to shape when heated over a bunsen flame.

[Comandante]

Nice setup. Simple too. The thing is I don't have any glass tubing and it might prove tricky to get some.

 

The place where you say "real condensing" apparently takes place you seem to have a large glass .. is that a glass stand or something... and water in it, with another flask in it used to collect the liquid? That's pretty cool anyhow, can I use a bucket of water instead?

 

One other thing I found tricky in distillation is that there are no holes anywhere... Doesn't the internal pressure increase due to heat? Does the condensation counter-act it by decreasing the pressure?

 

If that what you got is all that's needed, distillation doesn't look too hard then.

 

Would it be feasible to use rubber or some other tubing instead of the glass tubing?

[YT2095]

yeah, the receiver is a 250ml graduated volumetric cylinder floating in a gas jar full of ice water.

 

I wouldn`t use rubber or anything that could A) React and B) go soft at temperatures

[Comandante]

Ah I see, I'll try and get some glass tubing, something cheap pops up on ebay every now and then.

 

Ah cool. I was wondering if you also put ice in there

Just an idea, would it help if you added ammonium nitrate to that icey water there since that would result in a nice endothermic reaction?

[YT2095]

sure you could, it makes a great freezing mixture, and it`s easily recoverable too, esp since the summer`s getting closer, a few days out in the sun and it should recrystalize again quite nicely

[Comandante]

Nice. I didn't realize it's reusable! In my case winter's getting closer so would it be feasible to dry it in the oven or on a hot plate ?

 

I'll report back when (and if) I find cheap glass tubing

Thanks.

[YT2095]

No, don`t use direct heat to dry AN, the oven on low with the door open a little would be the safest of the 2 you mentioned, it doesn`t need to be Bone dry either, just nice and crystalised.

[Comandante]

Ah I see. No probs, will do, thanks.

[Comandante]

I received my glass tubing today, 4 tubes around 50cm each, but I can't seem to be able to bend a piece as required using the best heat source I have available at home - gas stove. I'm assuming it can't provide the necessary temperature? As I haven't had any experience with glassworks, is there a method to this? Is the borosilicate glass supposed to turn 'orange hot' for me to be able to bend it?

 

I don't think I'm in the mood to buy propane torch right now, so just a question, will I be able to do what I want using Bunsen burner at uni lab?

[YT2095]

Borosilicate is Very hard to work with using ordinary Methane and or Propane, yes it need to glow orange/yellow and also only Very gentle pressure, Soda Glass tubing is what I use.

[Comandante]

Ah ok. I'm not entirely sure if it's borosilicate. Actually this is the one can you tell me what it is? http://cgi.ebay.com/SIMIX-12-MIL-PYREX-TYPE-GLASS-TUBING-24-24-feet_W0QQitemZ250101770739QQihZ015QQcategoryZ11812QQrdZ1QQcmdZViewItem

 

The seller claims its easily workable with propane torch...

[YT2095]

it is yeah, not too bad a deal either.

all you need is Blowtorch really, you don`t need anything fancy or special like he has on his site, even a Cooks blowtorch works well (Butane gas).

 

it is workable, but I don`t like working boro-glass personally.

[Comandante]

Awesome. Well it's the only thing I've got available so I'll try to work it out. I might buy one of those cooking torches since they're not too expensive but I'll first check if they'll let me use uni's lab - which I doubt, but remain hopeful. Thanks YT, I'll report again when I make progress

[Comandante]

Aight. As an update, lab staff said they don't have anything to work with boro glass (equipment on other campus ), Bunsen flame is too weak they say, so I have to come up with a blowtorch... Where do you think I can find one suitable... cooking supplies? I'll hunt around..

 

I also recently realised that I can't use flat bottom flask for distillation (lol), so.. as I haven't got any round bottom ones, I thought this seller has some good stuff; http://stores.ebay.com.au/UNITED-GLASS-TECHNOLOGIES_FLASKS_Round-Bottom-Flasks_W0QQcolZ4QQdirZ1QQfsubZ9395357QQftidZ2QQtZkm however these are fairly expensive.. what's their value in retail shops?

[Comandante]

Just to add a few notes to this thread; I've managed to bend the glass with propane torch, make the cooler/condenser from a 2L coke bottle and some tubing attached to it (letting the water through it very slowly) and that's as much as I'll say about that (that's the part that worked out ok ) because I soon realized that the setup was not very efficient at all, though it did work (this was a couple of months back, forgot to update ).

 

I then decided to get proper condenser and few other things and I was delighted at the workings of the new setup which was test-run to produce some lavander oil. As I said, worked very well and got me some very nice oil with greenish tint. Will do many distillations in the coming weeks

I recycled water for cooling and used good old alcohol burner as heat source

Here's photo

[grndpndr]

Ammonium nitrates getting pricey and difficult to find so I tend to use all my AN in experiments but a good cheap substitute for an ice bath is UREA available as fertilizer (45-0-0) at ace hardware and others also available in handy 4lb sacks IIRC at around $5-$8.If they dont have it in stock they can order it if your local stores friendly o google 'Mastergardener'.Good thread ive put together some pretty crude distillation apparatus that neeed rebuilt nearly every run.Some handy ideas for an all glass/PVC/teflon imp. distillation apparatus,

 

Given the cost of maintaining an imp set-up ive seen e-bay of all places has all glass dstillation kits with a teflon thermometer adapter and thermometer complete 2000ml distillation kit (all glass/teflon) complete kit only no stand etc. for less than or a little more than $100.If nescessary the stand is far easier to imp than the distillation set-up and far safer depending on distillate.

 

Besides having a limited $ supply for this one of many $$ hobbys I do enjoy improvsing what I can safely.At the momet im rigging an 'agitator' hotplate using a $12 hotplate and the 2 vibrator motor assemblys from a massaging recliner attached to the hotplate base.Not a magnetic stirrer but it does heck of a job mixing w/the agitation saving much elbow grease although not in the league of a $300

magnetic stirrer but recall its total cost was $12.00 plus a piece of scrap plywood and 79cent L brackets to secure the hotplate

Edited September 21, 2008 by grndpndr

[Comandante]

I found that by using large volume of water the heat generated in such small setup would just not lift the temperature of the water by much at all. Just let the water come through the condenser and more than half of it would feel cold to the touch. On the other hand if you had a large condenser in a barrel or something then you could use the AN if you wanted.

 

Also, I've made some improvements to the setup in the picture. For distillation of raw plant material I used steam distillation by boiling water in another flask and letting it through into the main flask (one with plant material) via rubber tubing. Main flask is enclosed by some aluminium foil to keep the heat inside and prevent condensation. Additional heat source can also be used for the main flask. Steam+oil molecules then move into the condenser as usual.

 

With that $12 hotplate of yours, maybe you can implement a little motor below the plate and maybe make a magnetic stirrer similar to the one I described in the other thread.

 

I need to get some larger round bottom flasks too, at least 2L. I hear they're going to get illegal pretty soon, which is a damn shame.