Sciencemadness Discussion Board - distillation apparatus

zts16 wouldnt the vapors/liquid come out of the hole that sticks out to the side at the bottom of the condenser?

That hole is for cold water to go in, so that the condenser can condense the vapours.

Texium - 24-3-2014 at 16:47

No, that hole is the output for the cooling water. I just didn't have anything attached there in that picture.
The condenser that it uses is a Graham condenser, so the distillate runs through the coil, and the cooling water flows around it. The distillate drips out of the bottom, into the flask.
So far the only thing that I've distilled with it is store bought ammonia, to remove the surfactants. I plan on doing much more with it in the upcoming weekends though!

copperastic - 24-3-2014 at 16:50

oh ok. Also could i use a adapter to close it off at the end so that i can distill dangerous chemicals like bromine?And does that site have tubing to connect to the condenser? I might buy that (asking my parents for a early b-day right now).

[Edited on 25-3-2014 by copperastic]

copperastic - 24-3-2014 at 16:54

Does it fit with a thermometer adapter?
Sorry for asking so many questions..

DraconicAcid - 24-3-2014 at 16:56

No, that hole is the output for the cooling water. I just didn't have anything attached there in that picture.

The cooling water always goes in the bottom and out the top, so that the condenser is full of cold water.

copperastic - 24-3-2014 at 16:58

Wait how would i run water through it?

DraconicAcid - 24-3-2014 at 17:00

Wait how would i run water through it?

A thin rubber hose will connect to the glass inlet/outlet.

copperastic - 24-3-2014 at 17:02

i know but will i connect it to a faucet?

TheChemiKid - 24-3-2014 at 17:03

You may also want to buy a longer liebig, especially for lower boiling distillations, such as bromine, DCM, etc.

DraconicAcid - 24-3-2014 at 17:11

i know but will i connect it to a faucet?

The hose probably won't attach to a faucet unless you've got a very thin one. You might be able to jam a funnel into the hose and keep it topped up, or you might be able to get an adaptor for it.

[Edited on 25-3-2014 by DraconicAcid]

Texium - 24-3-2014 at 17:11

Quote: Originally posted by DraconicAcid

No, that hole is the output for the cooling water. I just didn't have anything attached there in that picture.

The cooling water always goes in the bottom and out the top, so that the condenser is full of cold water.

Oh… oops, yeah, that makes sense… I was doing some weird thing in which I was letting off water from the bottom occasionally and letting more flow in from the top, now I realize how counter-productive that is.
Thanks!

Also, since I work outside on my patio and don't have access to a faucet other than the garden hose which is usually rather warm, I have a plan to attach a large funnel (improvised from a milk jug) to the arbor and pour ice water in there, letting it gravity feed into the condenser.

[Edited on 3-25-2014 by zts16]

copperastic - 24-3-2014 at 17:13

Zts16 how do i get water into the tubing? (I know to use amber or any kind of tubing connected to the condenser) but how do i get it in? faucet? never mind just the the post above.

[Edited on 25-3-2014 by copperastic]

DraconicAcid - 24-3-2014 at 17:15

Oh… oops, yeah, that makes sense… Thanks!

It's obvious once it's pointed out- I received a sound mocking in my first year of organic chemistry for not seeing it the first time.

Texium - 24-3-2014 at 17:18

Yeah, a faucet works great if you have close access to it and the water is nice and cold. If the tubing won't connect, you might be able to buy an adapter that will fit. In the classrooms at my school, the sinks have little threaded pointy adapters so you can work a piece of tubing onto them. Otherwise, gravity feeding is the only thing that I can think of. Or if you're really desperate, spraying it in with a wash bottle! (:

Demosthenes - 24-3-2014 at 17:20

Copperastic, if you don't have lab faucets you can go to your larger hardware store and purchase a small fountain pump for <$20. Just google "fountain pump" to see what they look like. You just place the pump in a gallon bucket with your cooling fluid, plug it in and your good to go!

This is my first post, but I have been a (creepy?) lurker here for some time now.

copperastic - 24-3-2014 at 17:26

ok demosthenes thanks.

copperastic - 24-3-2014 at 17:33

lol zts a spray bottle...

Dr.Bob - 24-3-2014 at 18:12

Many faucets are threaded at the end, and you can screw in an adapter which is threaded at one end and has a hose barb at the other - I likely have some of them somewhere around here. But the simple fountain or fish pump and a bucket of water (with ice if needed) works fine also and saves some water.

Do be careful, I would advise people working with anything flammable who are new to organic or distillations to start outside or somewhere where starting a fire is not as bad. I have read about, heard of and created enough fires to know what I speak of, trust me. If you have a stirring hotplate and use a water or oil bath, it might work OK in a garage or workshop, but if you are trying to boil methanol with a flame, then outside is really a good idea. Once you have tried things, you will get the hang of what is safe and what is not. I would maybe even try ethyl acetate first, as it is more useful (does not boil way so fast) and ethanol is a great chemical. Just finding or making acetic acid will be a good first step. It is very useful and might be a good trial distillation.

The Volatile Chemist - 24-3-2014 at 18:19

For a good, friendly supplier, try http://www.hometrainingtools.com/ They've always had some of the less complex stuff at great prices, organic glassware, chemicals in small amounts, etc.

thesmug - 24-3-2014 at 18:21

As Dr.Bob said, many faucets are threaded. I faced this issue since I don't have any threaded faucets in my home. If you don't have any threaded faucets, you might actually find that you can remove the end piece which is held on by, you guessed it, threads. Homesciencetools sells a condenser faucet kit which is sized to accept both British (common even in the US) sink/hose threads and regular threads. It also comes with tubing to run the water with!

copperastic - 25-3-2014 at 03:16

Ok dr. bob. Thanks for warning me.

copperastic - 25-3-2014 at 12:20

Dr.Bob in making ethyl acetate ( i just watched a video) they say set up a reflux. Do i have to do that?

thesmug - 25-3-2014 at 15:36

Dr.Bob in making ethyl acetate ( i just watched a video) they say set up a reflux. Do i have to do that?

Yes, you do. The reason is that in order for enough energy to be supplied to run the reaction efficiently you need to conduct it at temperatures above the B.P. of the solvent. Of course you don't want to distill off your solvent, so you use a reflux setup to recondense the solvent.

copperastic - 25-3-2014 at 16:18

How could i set up a reflux? I might get that distillation setup that Zts got So could i somehow set that up?

Mailinmypocket - 25-3-2014 at 16:49

You can't really do a reflux with a graham condenser. You will flood the coils. A Liebig, reflux condenser, alihn, freidrich are all better suited for refluxing. Read a few manuals in the forum library on basic laboratory techniques. The answers will come faster than bombarding everyone with one liner questions that can easily be answered with google or reading books.

http://www.chem.ucalgary.ca/courses/351/laboratory/reflux.pd...

macckone - 25-3-2014 at 17:26

You can't really do a reflux with a graham condenser. You will flood the coils. A Liebig, reflux condenser, alihn, freidrich are all better suited for refluxing. Read a few manuals in the forum library on basic laboratory techniques. The answers will come faster than bombarding everyone with one liner questions that can easily be answered with google or reading books.

http://www.chem.ucalgary.ca/courses/351/laboratory/reflux.pd...

That link suggests cooling water should enter at the bottom but my personal experience is that entering at the top is better for reflux.
Ie. The bottom part of the column will be hotter than the top and it prevents vapor from escaping.

The Handbook of Petroleum Processing, Jones and Puhado 2006 has
a good diagram of how this is done industrially where the vapor is
condensed at the top of the tower and feed back via a reflux drum.

Mailinmypocket - 25-3-2014 at 17:34

Well that would be the first time I have heard of somebody refluxing with the water running in the opposite direction than it should for a reflux (or distillation).

By going from bottom to top you create a uniform jacket of cold water, when it runs in the top is just sloshes all over the place inside, but hey, if that's how you feel it works best.

[Edited on 26-3-2014 by Mailinmypocket]

thesmug - 25-3-2014 at 17:44

Well that would be the first time I have heard of somebody refluxing with the water running in the opposite direction than it should for a reflux (or distillation).

By going from bottom to top you create a uniform jacket of cold water, when it runs in the top is just sloshes all over the place inside, but hey, if that's how you feel it works best.

[Edited on 26-3-2014 by Mailinmypocket]

You're very funny (I'm not being sarcastic). If you do it on an angle will it work?

macckone - 25-3-2014 at 18:26

You have to restrict the outflow. It would not make sense to partially fill the column.
You also do not want the water to flow very fast.

TheAlchemistPirate - 25-3-2014 at 19:28

I bought a distillation apparatus last week. I got it in on Friday, and I've only used it once. It's not Pyrex, but seems perfectly acceptable, especially for a beginner level one.
Also, it's a great deal and comes with all of the hardware required to support it, including an extremely heavy duty ring stand that I am very impressed with. You can buy the exact same kit here:
http://www.cynmar.com/ProductDetail/11K21640_Distillation-Ap...

Also, the picture on there is kind of bad, so here's a better one that I took:

I wish I had seen this before spending 200$ and weeks of searching for a graham condenser distillation setup

Mailinmypocket - 26-3-2014 at 03:27

Is there anyone else who runs their condenser water from top to bottom? Well, either way that's not how it is done- working in professional laboratories past and present, I have yet to see a colleague do it that way. In school the teachers would actually tell people they were doing it wrong when they made that mistake.
Wiki

Quote: Originally posted by macckone

You have to restrict the outflow. It would not make sense to partially fill the column.
You also do not want the water to flow very fast.

[Edited on 26-3-2014 by Mailinmypocket]

[Edited on 26-3-2014 by Mailinmypocket]

macckone - 26-3-2014 at 04:21

Is there anyone else who runs their condenser water from top to bottom? Well, either way that's not how it is done- working in professional laboratories past and present, I have yet to see a colleague do it that way. In school the teachers would actually tell people they were doing it wrong when they made that mistake.
Wiki

Quote: Originally posted by macckone

You have to restrict the outflow. It would not make sense to partially fill the column.
You also do not want the water to flow very fast.

[Edited on 26-3-2014 by Mailinmypocket]

[Edited on 26-3-2014 by Mailinmypocket]

If you are refluxing like your picture it is definitely wrong.
That is distillation not reflux.

Mailinmypocket - 26-3-2014 at 05:13

No it's to demonstrate that water is supposed to always to in the bottom out the top. Regardless, I'm not going to continue disputing over a basic lab skill that had been discussed a bunch of times on the forum and is demonstrated in textbooks. Do it how you like though.

Dr.Bob - 26-3-2014 at 05:13

If you using a liebig or west condenser, you will always want to tun the water from lower to higher, whether rfluxing or not, as the water will not fill the condenser otherwise. For MOST other condensers, that is also true, but there are a few coil type condensers that the water could run either direction, especially the type with two coils in opposite directions, as the water will run both up and down no matter what. But they have a small diameter coil, so the air in the line will get pushed out by the water.

In industrial systems, the water is rarely in a large space like a liebig, it is usually in a copper type line, which is wrapped around the reactor, or in a very thin space around it, so the chance of building up air spaces is reduced, and typically the reactor is engineered/designed to avoid air spaces in the water that way, so you can make the flow go what ever way you design it to work with.

And that is the key to using glassware, use it for what it was designed for. A Graham condenser is designed for condensing small volumes of vapor into a small flow of liquid, typically in a vertical orientation. It is NOT designed for other uses, but many people want to use them since they look cool. A Liebig is the simplest condenser and works well in many cases, and can be use for condensing, refluxing, or as a distillation column. But some other condensers are best only for reflux, Allihn ones are ideal for vertical reflux, but pool liquid in them if used sideways. So use Google or other sources and look at the item and see why it was designed the way it was, if you are not sure. The internet has made it easy to do that now.

Ax165Xj - 3-4-2014 at 09:24

Quote: Originally posted by DraconicAcid