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Offlineneuro
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Simple Distillation Pictorial
    #3661822 - 01/22/05 04:18 AM (11 years, 10 months ago)


Materials needed: Round bottom boiling flask, distillation arm, thermometer adapter, mercury thermometer, condenser, collecting flask, vaseline, safety goggles, boiling chip (piece of glass or porcelain - it's stuck in the top of the cork, the cork won't be used)

The vaseline is used to lubricate the ground glass joints for ease of fitting and a good semi air-tight fit, note completely air-tight is quite dangerous.

The condenser is connected to my sink through quite an elaborate adapter system and hosing which is connected to the ports on the condenser through rubber hosing, both input and output. The output simnply drains into the sink.




The to be distilled liquid is loaded into the round bottom flask with the boiling chip. The boiling chip is added to ensure we do not super heat the solution and have a sudden explosive episode of boiling.

The still is partially assembled, the distilling arm arm and the thermometer are put in place.

Note the thermember bulb is placed right at the distillation side arm, this was an error on my part, the thermometer bulb should be placed just below the side arm, as to accurately measure the vapor that is to run into the distillation arm (Remember, liquids boil when the vapor pressure equals atmospheric pressure, in our case caused by a temperature increase). We are boiling everclear with wormwood steeped in it. Therefore our liquid consists of 95% EtOH, Water and oils and solubles from the Wormwood.





The still is completely assembled. Notice that I am using 2 rings to hold the boiling flask and distilling arm in place. This is because I had 2 clamps of the type that is holding the condenser in place. But while I was assembling the still I put one of the clamps down somewhere and couldn't find it. The clamp of the type that is holding the condenser should be used instead of the second higher ring. However I looked for at least and hour and couldn't find it, so i substituted it with another ring to ensure some sort of stability.

The condenser has cold water running through it.

The water that runs through the condenser is drained into the sink.





The top of the flask and distilling arm is insulated with some tin foil to keep the heat in.

The heat source is fired (literally) up.

Note the temperature rising on the thermometer (temps are in C not F)





The liquid begins to boil. Note the temperature is at about 78C, this is the boiling point of alcohol since it's component is substantial it's nearly on the mark. As it proceeds to boil, the first distillate beings to drip out.




After several minutes time note the amount that has been recovered. The color is also clear.




As the liquid in the round bottom class distills off, the clear liquid that has been collected has increased substnatially in volume. Notice the darkening of the liquid still left in the round bottom flask.

As the amount of alcohol decreases and the water content as well as oil content from the wormwood increases, the vapor temperature in the distilling arm increases beyond 78C where the temperature was pegged for quite a while, while the volume of the liquid in the round bottom flask decreased.





As the volume decreases more and more the boiling point increases ever higher.





As we're getting to the nitty gritty end, the volume in the flask decreases and the pot residue (what's left over) gets ever so concentrated and dark. I also had to add another flask to collect the distillate.





The whole distillation has come to a completion. The pot-residue was collected in a mason jar and inspected, it smells quite intriguing, almost pleasant, but strong and volatile feeling when inhaled. The distillate is pictured, notice the clear color.



Distillation Precautions:
  • Never distill to dryness. The resulting pot residue is sometimes explosive (in our case that's not really a problem), other times it is hard to get the remaining crud out.
  • Never distill in an airtight system. Pressure can build up and cause explosive results.
  • Do not distill using an open flame. (Yes I know I broke this rule, but this was all I had as a heat source. It is best to use a hot sand bath or a hot plate with a heat transfer element. I had a fire extinguisher around ready to put out any resulting fire that would have resulted from my glassware cracking an burning the eveclear that was being distilled. Don't try this at home, I'm sort of a professional.)
  • Always use a boiling chip. Boiling chips help prevent super heating, especially of pure liquids. (Consider precautions with water, especially distilled water, in the microwave. Super heating can occur then, many people can and do get burned badly ever year from putting a spoon in their coffee cup only to have it erupt in a violent boil and burn them badly.) Boiling chips have irregular surfaces that allow the formation of vapor bubbles that facilitates boiling.

  • Never add a boiling chip to hot liquid, it may over boil.



Other considerations:
  • A constant boiling point on distillation does not guarantee that the disillate is one pure compound.
  • Boiling point changes with pressure. Depending on elevation your boiling point of pure or non-pure liquids is subject to change. For example, some food cook times are adjusted for high altitudes.



Words to know:

Azeotrope: A mixture of liquids of a certain definite composition. Not all liquids form ideal solutions. Because of molecular interaction a mixture of 95.5% (by weight) of ethanol and 4.5% of water boils below (78.15C) the boiling point of pure ethanol (78.3C). Thus no matter how efficient the distilling apparatus, 100% ethanol cannot be obtained by distillation of a mixture of say 75% water and 25% ethanol. A 100% pure sample of ethanol must be prepared chemically.


Hold-up: What's left in the condenser or fractioning column (for fractional distillation) after you have stopped the distillation.


Pot residue: What's left in your boiling flask that did not make it to through the condenser and into your collecting flask.


Edited by neuro (01/22/05 02:32 PM)


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Invisiblespudamore
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Re: Simple Distillation Pictorial [Re: neuro]
    #3661829 - 01/22/05 04:21 AM (11 years, 10 months ago)

thanks for the post neuro, i will post my set-up in just over a week.
cheers again.


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OfflineAuroricDistortions
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Re: Simple Distillation Pictorial [Re: neuro]
    #3662325 - 01/22/05 12:33 PM (11 years, 10 months ago)

Very nice work!  My absinthe is still waiting, since I need a few parts to complete my still.  The b.p. of thujone is around 85C so it looks like you got the goodies in your flask.  Impressive color difference.  Let us know how it tastes :wink:!


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Offlinefelixhigh
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Re: Simple Distillation Pictorial [Re: neuro]
    #3662393 - 01/22/05 12:56 PM (11 years, 10 months ago)

very neat! =b~~~
very useful!


FH


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InvisibleStonehenge
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Re: Simple Distillation Pictorial [Re: AuroricDistortions]
    #3662453 - 01/22/05 01:18 PM (11 years, 10 months ago)

Super, neuro, that's just what is needed for a lot of people. That will probably save someone from burning his place down, seeing how to do it right. Don't forget to take it off the heat before it gets dry or you'll have a very hard time getting it out of the flask.

Now we need to see a soxhlet in operation. Matter of fact, I posted a link to soe MIT lab videos a while back that showed a reflux and soxhlet and how you set them up. Lot's of people doing extractions might be interested in that.

A soxhlet is what you might do just before neuro's distillation above. You can soak your herbs in the solvent, such as alcohol, or you can do a sox which passes pure solvent through the material over and over again using the same solvent over and over. It distills the solvent and puts pure alcohol continually through the herb. It will get out everything that can be gotten with a solvent. It's a little more expensive to set up than a simple distillation. You need a soxhlet, I picked one up for less than $20 including shipping. You need a condenser to go with it, a lab stand or something else to hold things so they don't fall over, a heat source and you're all set.


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Offlineneuro
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Re: Simple Distillation Pictorial [Re: Stonehenge]
    #3662467 - 01/22/05 01:26 PM (11 years, 10 months ago)

>>Super, neuro, that's just what is needed for a lot of people. That will probably save someone from burning his place down, seeing how to do it right. Don't forget to take it off the heat before it gets dry or you'll have a very hard time getting it out of the flask.


Yes! That's a very good point. I was going ot post a list of precautions after this last night but turned in and went to bed, it was 4AM. I will do that in a separate post in this thread in a second.


As for the soxhlet extraction, I need to get a soxhlet thimble and some time to actually do it. For those that will read this, the soxhlet extraction is just what stonehenge says it is. It's purpose would be best served for making an absinthe essence that one would later add to a drink, but NEVER drink it on it's own as it'd be toxic. The essence bottles can be bought online too. Soxhlet serves many other purposes. Soxhlet extractions in the end would circumvent the week one spends macerating the wormwood and herbs in a bottle with heat and reflux as stonehenge has described.

Now for the list of precautions.


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InvisibleShamansPalace
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Re: Simple Distillation Pictorial [Re: neuro]
    #3662516 - 01/22/05 01:42 PM (11 years, 10 months ago)

Frickin awesome !


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Offlineneuro
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Re: Simple Distillation Pictorial [Re: ShamansPalace]
    #3662644 - 01/22/05 02:23 PM (11 years, 10 months ago)

Okay, the precautions and other stuff have been added to the first post for ease of browsing/use for future reference.


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OfflineGr0wer
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Re: Simple Distillation Pictorial [Re: neuro]
    #3662760 - 01/22/05 02:59 PM (11 years, 10 months ago)

Nice work and nice labware.

Heres a cheaper route. http://www.amazingstill.com/Amazingstill.pdf


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OfflinePsilygirl
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Re: Simple Distillation Pictorial [Re: neuro]
    #3663219 - 01/22/05 05:31 PM (11 years, 10 months ago)

very cool!!

maybe Organic chem lab might be useful for something one day :wink:


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Invisiblespudamore
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Re: Simple Distillation Pictorial [Re: neuro]
    #3663368 - 01/22/05 06:13 PM (11 years, 10 months ago)

how do you seperate the rest of the oil from what little is left of the distillate?


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OfflineLegoulash
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Re: Simple Distillation Pictorial [Re: spudamore]
    #3663518 - 01/22/05 06:56 PM (11 years, 10 months ago)

Thank you thank you thank you..

But where do I get all the glassware? Has anyone had luck with buying from universities?


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InvisibleShamansPalace
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Re: Simple Distillation Pictorial [Re: spudamore]
    #3663640 - 01/22/05 07:24 PM (11 years, 10 months ago)

Quote:

spudamore said:
how do you seperate the rest of the oil from what little is left of the distillate?




Evap?


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Invisiblespudamore
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Re: Simple Distillation Pictorial [Re: Legoulash]
    #3663707 - 01/22/05 07:40 PM (11 years, 10 months ago)

gotta look at what would cost more glass ware or making a still
http://www.moonshine-still.com/page2.htm
you can do the same things with a still and more.


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OfflinePsilygirl
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Re: Simple Distillation Pictorial [Re: ShamansPalace]
    #3664149 - 01/22/05 09:24 PM (11 years, 10 months ago)

yeah evaporation by a stream of air and putting the flask in a steam bath (or put your hands around it--anything you can think of to give an input of heat--but not too hot) usually makes it go faster.


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Offlineneuro
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Re: Simple Distillation Pictorial [Re: spudamore]
    #3664867 - 01/23/05 12:05 AM (11 years, 10 months ago)

I'm not sure I'm following you.

The distillate is the large clear liquid that was collected.

What was left in the round bottom flask is the pot residue and that is to be discarded, I got what i wanted out of it in the distillation (namely volatile oils, thujone and the alcohol). What's in the oil are bitters and other things that make the absinthe taste poorly. The oil was just washed down the sink with copious amounts of water.


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Invisiblespudamore
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Re: Simple Distillation Pictorial [Re: neuro]
    #3664880 - 01/23/05 12:06 AM (11 years, 10 months ago)

ok sorry, but if you wanted to seperate to make pure oil? seperate oil from the water or distillate..


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Offlineneuro
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Re: Simple Distillation Pictorial [Re: spudamore]
    #3665049 - 01/23/05 12:33 AM (11 years, 10 months ago)

for the oil you'd do what Stonehenge was talking about with a soxhlet apparatus.


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OfflineBorgFace
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Re: Simple Distillation Pictorial [Re: neuro]
    #3665991 - 01/23/05 03:10 AM (11 years, 10 months ago)

Excellent thread.

It's just what I was looking for.


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OfflineFluxburn
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Re: Simple Distillation Pictorial [Re: BorgFace]
    #4076904 - 04/20/05 02:13 PM (11 years, 7 months ago)

Ok neuro I know you are not moddin anymore but if you do read this. I was planning on making my own ethanol from grain and yeast or yeast and sugar. After allowing the material to ferment, it will have produced ethanol and by product. I was going todo the same procedure with glass lab appartus as well. I was going to more use along the lines of 1000ml or 2000ml boiling flask. I was under the impression a larger fractioning column would be necessary, yet the one you are using is almost no existent, thus I guess a large one is not necessary. The fire danger of course is present, I was also under the impression that the glass seals where quick lock for organic chemistry and do not need any sealing agent. The capillary action of the seals provides a sealing bond that is more then sufficent from what I have read.

You say not to use a flame source, yet either a flame source is used in the lab or a heating mantel in trandition settings. I have also seen the boiling flask attached straight to a hot plate. No offense, but if the boiling flask explodes on a open flame you will have fire, but if the flask explodes on a hot plate it will most likely burst in to flames unless the alcohol content is too high and not enough oxygen is present. I understand your disclaimer for the open flame of course, without a open flame you most likely have more critical seconds to extinguish the area that is about to burst into flames.

About the tin foil? Is this just a precation to avoid splashing of possible materials?

Also you must not have that pure of ethanol in those flasks since the fractioning column is so small. I am just assuming this logically since each still device that has a larger fractioning column has high proof alcohol vs. the pot stills (or just distillation appartus you have created).

So you are performing distillation and not fractional distillation. This is of importance to me because I am trying to make as pure ethanol as possible, i.e. 95% ethanol 5% water.


Ps. the lab glass can be had on ebay for pennies of its oringal cost. I bought 4 500ml pyrex flasks, $15 shipped. I mean I see lienderburg condesors with fractioning columns for $30 shipped. All ones needs is a hot plate ($40 shipped) and a boiling flask, ($20). I guess it adds up but your can use lab appartus for more then one application.

Last, looking at college organic chemistry classes, this is primarily the first lab they perform. I guess it is dangerous in aspects, but if you wish todo any organic chemistry you should be able to complete such a simple task.


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Edited by Fluxburn (04/20/05 03:07 PM)


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