Sciencemadness Discussion Board

Questions about Distillation Apparatus...es (Apparati?)

xeneficus - 23-7-2016 at 18:36

I'd like to try some organic chemistry, and as I understand it a distillation/reflux setup is almost impossible to do without. I'm looking at this one. Yes, it's Chinese, I know, but I think it should do the job (correct me if I'm about to make a huge mistake).

I do have some questions about distillation apparatuses/i, though. For the water source, is there a specific pump I should use and recirculate water? I could get an aquarium pump pretty cheaply I think. Secondly, the joints on this particular setup are 24/29. Would that be compatible with 24/40's when I eventually get them? I imagine they fit together since they have the same starting diameter and 1:10 taper, but is it ok to put them together?

Texium - 23-7-2016 at 20:39

An aquarium pump works great for recirculating condenser water. I got the second cheapest one available at Lowe's and it's been serving me well for a couple years now. I think it was like $20.

24/29 and 24/40 joints will fit together alright, but not perfectly. It's better to stick with one size, and personally, I'm partial to 24/40. How about this one that's 24/40 for $5 more? It's also from Deschem, a seller (also Chinese) that many people myself included have ordered from before and could recommend.

You could also go ahead and buy a larger kit that includes a sep funnel, a Vigreux column, and a few different flasks (including a two necked and a three necked) for just over $100. They make fancier kits that include more flasks, more adapters, and different types of condensers, too. If you get one of those, you'll have pretty much all the glassware that you'll need for most organic synths, and then you can add specialty pieces over time as needed.

j_sum1 - 23-7-2016 at 22:17

Remember, you will break a flask. Probably when you are being really careful. Having a reserve is always a good idea. No one ever regretted having a few extra items of glass.
Remember also that you need a good way of heating also. My 1L flask gets very little use because my mantle is designed for 500mL. You do need to think of your glass, heating and stands as an integrated set. This means working our what you need, biting the bullet and buying it as a kit. It hurts the pocket but you will not regret it.

xeneficus - 24-7-2016 at 00:14

Quote: Originally posted by j_sum1  
Remember, you will break a flask. Probably when you are being really careful. Having a reserve is always a good idea. No one ever regretted having a few extra items of glass.
Remember also that you need a good way of heating also. My 1L flask gets very little use because my mantle is designed for 500mL. You do need to think of your glass, heating and stands as an integrated set. This means working our what you need, biting the bullet and buying it as a kit. It hurts the pocket but you will not regret it.


I'm getting 1 replacement each for the boiling flasks. For heat I think I'm going to use a hotplate like this one with a sand bath. I'm a little concerned about the auto-shutoff function, though. I'm not sure if it will be an issue. As for stands, since I'm only going to have one distillation setup, hence only one set height, I think I'll just have a stack of plywood or something to hold up the hotplate/sand bath to that height. Things will be pretty DIY at the beginning, but I kind of like the feeling of it, there's a kind of charm to jury-rigging up my first setup instead of getting something that works out of the box. :D

j_sum1 - 24-7-2016 at 00:48

My hotplate is similar. Only it is rusted and has lots of interesting chemical splashes all over it. :)
It is annoying that I cannot stir using it but it will suffice until I get a replacement.
The auto shut off is ok -- especially if you are using a sand bath or oil bath. A thermometer in the bath lets you know what temperature you are hitting and you can adjust accordingly. Mine generally gets used for beakers and erlenmeyers and so I have to baby it a bit more.

I recommend getting a stand and some clamps for holding stuff. I got some steel mesh that is normally used to reinforce concrete. I attached it to my workbench at the bottom and also to the beam above. It had a bit of a wobble but worked reasonably well (and was cheap.) I used it for holding beakers, funnels, flasks, distillation columns and -- well everything. It was like an extra set of hands. Don't skimp on boss heads and clamps. I have some rings as well which were very cheap and are rather useful. When I build my lab at my new place I will do something similar. But I also now have a good stand.

Bits of ply will suffice for getting things at the right height. But it will not be long before you are hankering for a lab jack. Mine is a converted car jack (and can hold 1000kg.) It is really useful to have your heat source elevated and your flask fixed. Then when you want to remove the heat you can simply lower the heat source. Ditto for ice baths etc.

I hope this helps.

Sulaiman - 24-7-2016 at 03:55

xeneficus
My first distillation kit was a B10 (10/14) for which I used plywood and terry clips
https://www.google.co.uk/search?q=terry+clip&ie=&oe=

The setup was so rigid that I broke my distillation column when dis-assembling :(

I recently bought a "500ml distillation kit" ... I now own two stands and four clamps :D

I too use one of the cheap hotplates, I wish I had some heating + stirring facility.







Herr Haber - 24-7-2016 at 12:25

Everything has been said already. As recommended I'd get a kit with a Vigreux column. The first set I got also had a vacuum adapter.
I finally got a real PTFE membrane pump instead of the "pumps" that you attache to the faucet.

About PTFE: I use PTFE joints every single time I set up the distillation apparatus now. I got them in the first place to distill nitric acid but they make your life a lot easier when you have to dissasemble your kit. Never broke anything that was stuck so far.
If you can find some at a decent price, get them !