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kt5000
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Beginner Distillation Projects
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!
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Crowfjord
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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!
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Texium
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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  ... 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]
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kt5000
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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?
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Texium
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http://en.wikipedia.org/wiki/Steam_distillation
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kt5000
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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]
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kt5000
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Wikipedia is my friend 
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arkoma
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*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.
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Zyklon-A
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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.
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arkoma
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D'oh--should have mentioned acetone. water from a teakettle is hot enough to vigorously boil it.
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
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Brain&Force
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You could try making nitric acid, 68% or even fuming nitric acid with nitrates and sulfuric acid.
At the end of the day, simulating atoms doesn't beat working with the real things...
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aga
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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.
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kt5000
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Quote: Originally posted by Zyklon-A  |
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  Lesson learned.
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kt5000
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I read about that process and am considering doing it at some point. What kind of a nitrate would be suitable and readily available?
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TheChemiKid
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It depends where you are. Probably sodium, potassium, ammonium, or an ammonium-calcium mixture
When the police come
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Brain&Force
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| 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.
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Why not distill seawater?
At the end of the day, simulating atoms doesn't beat working with the real things...
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kt5000
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I have no sea
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Texium
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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]
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TheChemiKid
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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.
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Artemus Gordon
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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.
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Texium
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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.
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subsecret
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You could buy some paint stripper and distill dichloromethane. It's very volatile, as it only boils at 39 degrees or so.
Fear is what you get when caution wasn't enough.
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Magpie
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| 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.
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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]
The single most important condition for a successful synthesis is good mixing - Nicodem
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kt5000
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| 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.
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kt5000
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| 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.
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Not yet.. A Vigreux fractionating column is on my glassware wishlist
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