Sciencemadness Discussion Board

Beginner Distillation Projects

kt5000 - 7-8-2014 at 20:04

I'm fairly new to Chemistry, studing Chem 1 and Intro to Organic Chemistry. I have a basic distillation set at home. Have distilled ethanol from Vodka with decent success and fun.

Can anyone suggest some other safe, beginner-level distillations with easy-to-find chemicals?

Thx!

Crowfjord - 7-8-2014 at 20:30

Try a steam distillation. It's super simple - take an herb or spice of your choosing (cloves and cinnamon are really good ones), grind to a powder and add to your distillation flask/pot. The spice volume should probably be no more than about a fifth the volume of the flask. Then add water - no more than about half the flask's capacity. Set up for distillation and carefully heat. The water and essential oil will distill over. Don't distill until the stuff in the pot is dry, it might hurt the flask. Depending on the herb or spice you choose, the oil may rise to the top or sink to the bottom.

Happy tinkering!

Texium - 7-8-2014 at 20:32

If you're able to convert your setup to a steam distillation setup, many interesting organic distillations could be done using various common substances, like cinnamon. I haven't done any myself, but it's something I've been wanting to start playing with. Fellow member arkoma has done a lot of steam distillation and will probably chime in on this thread too. :)

My first distillation was bromine :o... which I would not recommend. It was a success and I have a few mLs of bromine (with about a mL of water floating on it) to show for it, but it was also very scary and not something that I probably should have tried with limited equipment and only a month of chemistry experience.

Edit: Well, it looks like Crowfjord beat me to it about steam distillation while I was typing my reply!

[Edited on 8-8-2014 by zts16]

kt5000 - 7-8-2014 at 20:57

Sounds like my setup would work.. So the hot water drives the oil out of the herb, but what causes the oil to distill over? Does it have a lower BP than water?

Texium - 7-8-2014 at 21:07

http://en.wikipedia.org/wiki/Steam_distillation

kt5000 - 7-8-2014 at 21:21

Unrelated, but I made the mistake of storing my 80+% ethanol in a PETE water bottle. It sat for a couple days and I distilled it again. I ended up with a cloudy white solution and a green oil left in the distillation flask. All I can think is that was crap leeched out of the plastic container by the ethanol. Nasty!

[Edited on 8-8-2014 by kt5000]

kt5000 - 7-8-2014 at 21:24

Quote: Originally posted by zts16  
http://en.wikipedia.org/wiki/Steam_distillation


Wikipedia is my friend :D

arkoma - 8-8-2014 at 06:30

*officially chiming in* LOL

My BEST results steam distilling have been with cloves. However, remember that cloves attack plastic--I learned this the hard way when I ground them in my nephews brand new Ninja blender. I got "banned" from that particular appliance..........

For "dry" steam disty's, I ran a small piece of copper tubing in through the thermometer inlet of the disty head to bottom of flask, other end in a bored cork stuck in a tea kettle. Bend carefully!





Another good beginning distillation is Isopropyl Alcohol. I buy the cheap 70%, toss in a half inch or so of plain salt, wait for it to layer out, then distill the top. It is believed that IPA can/does form explosive peroxides so:

DON'T BOIL IT DRY, EVER

The "weak" water/alcohol "waste" after distilling I keep in a squirt bottle for rinsing off glassware when I wash it.

Zyklon-A - 8-8-2014 at 09:07

Quote: Originally posted by zts16  


My first distillation was bromine :o... which I would not recommend.

Haha, mine was fuming nitric acid!
If you know what you're doing, you'd be surprised how how simple distillations can be. I should've done something less dangerous, but everything went fine.
Acetone is something that should be distilled if bought at a hardware store, mind the very flammable vapors and use a hot plate or similar rather than an open flame.

arkoma - 8-8-2014 at 09:48

D'oh--should have mentioned acetone. water from a teakettle is hot enough to vigorously boil it.

Brain&Force - 8-8-2014 at 10:08

You could try making nitric acid, 68% or even fuming nitric acid with nitrates and sulfuric acid.

aga - 8-8-2014 at 11:02

Distilling concentrated sulphuric acid with a nitrate salt is an awesome distillation, although it may not meet the OP's requirement : "safe, beginner-level distillations with easy-to-find chemicals".

Much safer - mix table salt and water.
If you distill it perfectly, the distillate will not be salty at all.

kt5000 - 8-8-2014 at 13:43

Quote: Originally posted by Zyklon-A  
Quote: Originally posted by zts16  


My first distillation was bromine :o... which I would not recommend.

Haha, mine was fuming nitric acid!
If you know what you're doing, you'd be surprised how how simple distillations can be. I should've done something less dangerous, but everything went fine.
Acetone is something that should be distilled if bought at a hardware store, mind the very flammable vapors and use a hot plate or similar rather than an open flame.


I use a hot plate whenever possible. I was heating an acetone mixture once, forgot to add boiling chips, and ended up with quite a mess. It would have been quite a FIRE if I had an open flame :P Lesson learned.

kt5000 - 8-8-2014 at 13:46

Quote: Originally posted by Brain&Force  
You could try making nitric acid, 68% or even fuming nitric acid with nitrates and sulfuric acid.


I read about that process and am considering doing it at some point. What kind of a nitrate would be suitable and readily available?

TheChemiKid - 8-8-2014 at 14:04

It depends where you are. Probably sodium, potassium, ammonium, or an ammonium-calcium mixture

Brain&Force - 8-8-2014 at 14:36

Quote: Originally posted by aga  
Distilling concentrated sulphuric acid with a nitrate salt is an awesome distillation, although it may not meet the OP's requirement : "safe, beginner-level distillations with easy-to-find chemicals".

Much safer - mix table salt and water.
If you distill it perfectly, the distillate will not be salty at all.


Why not distill seawater?

kt5000 - 8-8-2014 at 14:38

Quote: Originally posted by Brain&Force  

Why not distill seawater?


I have no sea :P

Texium - 8-8-2014 at 14:38

Not much seawater in the southwest US, unless he's in California or Salt Lake City
Edit: Ah yes, you beat me to the point. I actually just remembered that you can buy genuine sea water at the pet store for saltwater fish, so if you really wanted to you could get some of that, lol

[Edited on 8-8-2014 by zts16]

TheChemiKid - 8-8-2014 at 14:43

But at that point, its probably easier buying a bunch of cheap salt at the supermarket, and dissolving it in water.
If you want to, add some grass as a seaweed substitute. :P

Artemus Gordon - 8-8-2014 at 16:10

It's not distillation, but I had fun recrystallizing copper sulphate. I bought 10 lbs. of root killer CuSO4 from Amazon. After dissolving some of it in hot water and filtering, I caught an interesting olive-green solid in the filter paper. I then put the CuSO4 solution in the freezer to crystallize it and then filtered out my higher-purity CuSO4. The stuff that stayed in solution I put in a beaker with a watchglass cover to slowly evaporate. I got lovely large deep blue crystals of CuSO4 and some cool brown needle crystals of some other contaminant.

Texium - 8-8-2014 at 16:29

Yeah, that is a fun one to do. I did it with root killer also, but mine seemed to have almost no contamination. Only a light dusting of grayish powder was filtered out and nothing else crystallized.

subsecret - 10-8-2014 at 10:43

You could buy some paint stripper and distill dichloromethane. It's very volatile, as it only boils at 39 degrees or so.

Magpie - 10-8-2014 at 10:56

Quote: Originally posted by kt5000  
I'm fairly new to Chemistry, studing Chem 1 and Intro to Organic Chemistry. I have a basic distillation set at home. Have distilled ethanol from Vodka with decent success and fun.


Are you using a fractionation column? The boiling point difference between water (100°C) and the 95% ethanol azeotrope (78°C) is only 22°C. The rule of thumb is that the component bps should be >80°C (Brewster) for just simple distillation.

[Edited on 11-8-2014 by Magpie]

kt5000 - 20-8-2014 at 19:47

Quote: Originally posted by Awesomeness  
You could buy some paint stripper and distill dichloromethane. It's very volatile, as it only boils at 39 degrees or so.


I've looked at paint thinners before, as a simple source of solvents. Everything seems to be a solution of at least three solvents (DCM, acetone, xylene, methanol, etc.) I think I considered separation via distillation at one time and decided I didn't have the equipment or skill to separate liquids with such close boiling points. I think the low autoignition temp of some of those substances was a concern as well.

kt5000 - 20-8-2014 at 19:50

Quote: Originally posted by Magpie  
Are you using a fractionation column? The boiling point difference between water (100°C) and the 95% ethanol azeotrope (78°C) is only 22°C. The rule of thumb is that the component bps should be >80°C (Brewster) for just simple distillation.


Not yet.. A Vigreux fractionating column is on my glassware wishlist :)

Magpie - 21-8-2014 at 15:30

I don't know if a Vigreux column has enough "stages" to separate water and azeotropic ethanol. I was able to do this with an 8" long Hempel column packed with a ss scrub pad, however. I supposed it depends on the length of the Viqreux

aga - 22-8-2014 at 15:39

Quote: Originally posted by Magpie  
I don't know if a Vigreux column has enough "stages" to separate water and azeotropic ethanol. I was able to do this with an 8" long Hempel column packed with a ss scrub pad, however. I supposed it depends on the length of the Viqreux

wooo. Hempel Column.
more glassware to acquire ...

blogfast25 - 23-8-2014 at 04:47

Quote: Originally posted by Magpie  
I supposed it depends on the length of the Viqreux


Well, exactly. Column height, operating conditions like reflux ratio (ratio of reflux stream to product stream), internal surface area of the column and feedstock composition in terms of EtOH are the main variables that affect product composition.

There is no a priori reason to believe that in suitable conditions azeotropic EtOH cannot be achieved with a good Vigreux set up.

Hempel columns (packed columns) have their own set of problematics like potential column flooding for instance, which can limit the amount of reflux achievable.

[Edited on 23-8-2014 by blogfast25]

Magpie - 23-8-2014 at 14:13

Kt5000 seemed to be a beginner at distillation who was looking for advice. I assumed that he would not know what length of Vigreux that is necessary for this separation (I don't). My post was only meant as a warning that not just any fractionating set-up will separate azeotropic ethanol from water. I then gave the conditions that I used which provided a successful result. It's a data point for him to consider.

I know Vigreux columns have their place. I don't own one and admit a prejudice against using one for any challenging distillation, which I consider the above case to be as the boiling point difference is only 22°C (100-78). My college lab manual (Pavia et al) says the following regarding the Vigreux:

"Vigreux columns are popular in cases where only a small number of theoretical plates are required. They are not very efficient (a 20-cm column might have only 2.5 theoretical plates), but they allow for rapid distillation and have a small holdup (the amount of liquid retained by the column). A column packed with stainless steel sponge is a more effective fractionating column than a Vigreux, but not by a large margin."

[Edited on 23-8-2014 by Magpie]

aga - 23-8-2014 at 14:30

Chill Mags.
No attack going on.

Bloggers is just a bit blunt and grumpy cos a student sterilised the pet hampster ...
... in an autoclave.

Magpie - 23-8-2014 at 14:40

Shame on him...everyone knows that for a hampster you use a microwave oven.

aga - 23-8-2014 at 15:04

Some recipies are better than others.
Personally i favour Turnip Surprise.
Surprised everyone, including the hampster.

Fantasma4500 - 24-8-2014 at 03:51

orange skin!
then pour the destillate into some tall thin glass container and add some food colouring, it should only colour the water making it relatively easy to seperate out the limonene, it should float on top
otherwise i recall some interesting compound was extracted from tomato paste

confused - 24-8-2014 at 04:26

is there any way to test the water content after ethanol distillation?

blogfast25 - 24-8-2014 at 04:38

Quote: Originally posted by confused  
is there any way to test the water content after ethanol distillation?


Density of the ethanol goes up with water content, as the density of pure EtOH is 0.789 and that of water 1.000. Towards the high end of EtOH content that method becomes fairly insensitive though.

EtOH content in EtOH/water mixtures can be chemically determined by iodometry. Standardised acidified potassium dichromate is reduced by EtOH to Cr (III). The remaining potassium dichromate is used to oxidise iodide to iodine and the iodine titrated with standardised sodium thiosulphate. Quite laborious...

For very low levels of water Karl Fisher titrations would be called for.

[Edited on 24-8-2014 by blogfast25]

kt5000 - 3-9-2014 at 19:09

Quote: Originally posted by aga  

Bloggers is just a bit blunt and grumpy cos a student sterilised the pet hampster ...
... in an autoclave.


I don't have an autoclave.. Microwave will have to do.

Texium - 3-9-2014 at 19:21

Quote: Originally posted by Antiswat  
otherwise i recall some interesting compound was extracted from tomato paste
I believe that this was the thread you were thinking of: Extraction of Lycopene
It does look interesting. It has a very nice color to it.