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Author: Subject: Help with my first distillation, ever.
nannah
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[*] posted on 14-10-2014 at 09:48
Help with my first distillation, ever.


Hi, guys. Today i decided to take the bull by the horns and for the first time ever do a simple distillation.
About a week ago i mixed sugar, yeast and half a liter of water together. Today the fermentation was ready.
I also tested the alcohol level, and it ranged between 5-10 %

I have a basic distillation setup, but no fume hood. I plan to measure up 50 ml of mash.

Do you think i can do the distillation without a fume hood? I will place a fan next to the setup and have it blow all the fumes away, diluting it a little bit. :)

Thanks in advance. :)
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DutchChemistryBox
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[*] posted on 14-10-2014 at 09:56


Assuming that you have a suitable condensor, it shouldn't be a big problem. Provided that you ventilate enough to make sure that you're not accumulating flammable vapors.





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aga
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[*] posted on 14-10-2014 at 10:45


If it's not a naked flame, you'll be fine with ethanol distillation.

If it is, then be very careful to ensure that the glass joints are sealed, and Cannot come apart half-way through, releasing hot ethanol vapour near your flame.




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DutchChemistryBox
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[*] posted on 14-10-2014 at 11:25


I agree with what aga says. If you only have a naked flame, than maybe it is better to wait and spend some money on a heat plate.
Better safe than sorry




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nannah
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[*] posted on 14-10-2014 at 22:44


Im sorry i didnt write that right away. I have a 300 mm 24/40 Liebig, and also a 400 mm 24/29 Liebig condenser. I can use either of those right?

I will heat with a water bath, on a hot plate with magnetic stirrer.

Im goind to grease and clamp the joints before i start.

Have to go. Thanks guys! :)
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blogfast25
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[*] posted on 15-10-2014 at 04:58


400 mm would be overkill: ethanol condenses easily.

Water bath would take a long time to get the mash boiling. Small hot plate preferred.

Grease but only lightly.

[Edited on 15-10-2014 by blogfast25]




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Amos
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[*] posted on 15-10-2014 at 05:29


I would assume you've probably already done the distillation by now, but if you didn't already know, when using a hotplate, take a long sheet of aluminum foil and create a skirt around the boiling flask(narrow at the top, and about the width of the hotplate at the bottom) to trap heat and promote more even heating throughout. It will considerably speed up the process, just be careful not to boil it too strongly.



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nannah
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[*] posted on 15-10-2014 at 06:25


Thanks for the advice, guys. I am using plumbers grease that i bought from the local hardware store.

Also i have a Dean-Stark moisture trap. Can i add it to the apparatus to dry it even further?

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Loptr
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[*] posted on 15-10-2014 at 07:13


Quote: Originally posted by nannah  
Thanks for the advice, guys. I am using plumbers grease that i bought from the local hardware store.

Also i have a Dean-Stark moisture trap. Can i add it to the apparatus to dry it even further?



Dean-Stark is for liquids that aren't miscible. Ethanol and water are miscible, and therefore, do not form layers that would provide the ability to return one of them to the boiling flask.

You would further dry the ethanol by redistilling it with anhydrous calcium chloride, or some other similar drying agent. Molecular Sieves will also work, such as the Zeolite 3A that are shown here: http://www.imakemygas.com/

[Edited on 15-10-2014 by Loptr]

[Edited on 15-10-2014 by Loptr]
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CuReUS
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[*] posted on 15-10-2014 at 08:07


you can also read bromic acid's book,he provides many tips for a good distillation
http://www.bromicacid.com/bookprogress.htm
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nannah
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[*] posted on 15-10-2014 at 12:38


This is why i love this place. I learn new stuff everyday. Thanks Loptr.

No, im not done yet. In fact, i havent even started. :)
I cant seem to keep the hose in place on my water pump, so i couldnt get any water to my condenser. It keeps falling out each time i get it in place. Its a small submersible aquarium pump.
What can i do about that, any ideas? I was thinking that i would use electrical tape.

Cereus. I will check it out. :)

Thanks guys so very much. :)
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aga
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[*] posted on 15-10-2014 at 13:11


If the Pipe is too big, it won't grab onto the glass pipe.
Getting electrical tape to work would be an Advanced Lab Practical (it can actually be done).

Easier to get a few cm of the next sized pipe down from the one you got, and shove a 5~7cm piece into the end of your pipe as far as it will go.
As you shove the smaller pipe onto the Glass pipe, the smaller pipe will seal onto the glass, and the bigger Outside pipe, making a watertight (ish) Seal.

Be sure to have the Pump going to the Lowest part of your condenser - it should fill from the Bottom Up, not trickle from the Top Down.

If you want to try electrical tape, carefully wrap loads of it around the Glass pipe on the condenser.
If you get lucky, the plastic pipe will eventually fit with just a few drops of leak.

Unlikely to last a long time, but might work for long enough before spraying water everywhere.
But then, water is Fun !

Edit:

Oh. I remember now.
No, water is definitely Not Fun when it knackers your laptop keyboard.
OSK is HELL.

[Edited on 15-10-2014 by aga]




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hyfalcon
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[*] posted on 15-10-2014 at 13:21


I use wire ties myself to hold the tubing onto the nibs of my pump and condenser.
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Actinium
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[*] posted on 15-10-2014 at 22:03


distill till you get the Azeotrope to where alcohol is at a max 96% then either use molecular Sieves or Distill with Calcium Oxide and for ultra dry use the Sieves after the Calcium Oxide Distill.
Another way to dry it is to do Azeotropic distillation.
If you are trying to tape anything up that needs a good seal and needs to be water proof, just my suggestion but I would forfeit the electrical tape in favor of pond liner tape. Its hardy, heavy duty, its meant to hold under tremendous stress and guess what????? ITS WATER PROOF....:D
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nannah
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[*] posted on 16-10-2014 at 01:52


I have a pump with sort of like a dolphine blow hole that you have to put the tube into, but it keeps falling out. The tubing is going perfectly onto the nipple of the condenser.

I am going to distill with CaO the second time. What difference of procentage will it be at if i choose to only dry with sieves? My goal is to get it to 96%.
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hyfalcon
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[*] posted on 16-10-2014 at 04:45


I would try to find a piece of tubing that would fit into your blow hole and still allow your tubing to also fit onto said tubing. Once I had dry fit that and found the right size, I would try gluing it into your outlet on the pump.
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Chemosynthesis
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[*] posted on 16-10-2014 at 07:48


There is probably no appreciable difference in sieves vs. CaO for your purposes. To get technical, it can vary depending on amount per solvent and time dried. Check J. Org. sachem 2010, 75, 8351-8354 or similar for more detail.

Also, while there would be no real benefit from a Dean Stark trap in your circumstances here, it can be helpful with miscible liquids when you are removing an azeotrope while formed. An example would be using dried ethanol in a condensation reaction; your newly formed water/ethanol azeotrope could distill out from the dried ethanol reaction flask under the proper circumstances.
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CuReUS
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[*] posted on 16-10-2014 at 07:56


are your pumps like these
https://www.customaquatic.com/estore/control/subctg/~ctg=s_w...
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