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Build a Lab Quality (ish) Distillation Apparatus.

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lab fractional distillation.jpg

There are a few Instructables out there on how to create stills for various purposes. Usually these include a large amount of small diameter, flexible copper refrigerator tubing. While these stills can be quite effective, there is just something a little hokey about them. Especially the part where you run a large amount of expensive copper tubing through a bucket of standing water to cool the condensate. Then there's the issue of a high surface area on the interior of the tubing, which makes small volume distillations difficult to impossible. Plus they're bulky, unwieldy, and they look like a meth lab. I do have to give the authors of these projects some credit however, since DIY is typically about getting the job done, form follows function, etc etc. BUT...

I say there is a better way.

By using a small amount of 1/2" and 3/4" copper pipe, it is possible to build a lightweight, compact, collapsible, interchangeable, universal distillation apparatus for anything you could possibly hope to distill. The apparatus featured here is capable of efficient low to medium volume distillations and could in principle be scaled for use in high volume applications. It is constructed from relatively inexpensive parts which are available at any hardware store.

UPDATE 10/27/2011: If you find the start-up costs for this project to be prohibitive, I recommend this instructable.

I was inspired to build a distillation apparatus during an organic chemistry lab where we were required to identify an unknown organic solvent by IR spectroscopy. The samples they gave use weren't pure and we had to distill them first so the IR machine could get a good spectrum. This apparatus is modeled after the one I used in that lab. In the lab the apparatus was made of lab quality glassware. Since I don't know how to work with glass, and I DO have experience remodeling houses, I decided to combine my experiences to make an affordable, clean, safe, glass alternative distillation apparatus.

So. Now I've got your attention. Read on, my friend.

 
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sfranger made it!5 months ago

I made mine last summer with an old aluminum pressure cooker. It works pretty well. I need to get better seals for the cooker because there is a good amount of losses. the way I joined the copper fitting to the lid of the cooker was by drilling out a hole and tapping it with pipe thread and joining it with a fitting. It worked really well.

IMAG0202.jpg
laserjocky (author)  sfranger4 days ago

Hey, that looks great! I had to do a double take because it looks so much like mine. Nice work, and I'll keep the tapped hole idea around for the next project.

jtucker1410 months ago
web site http://homedistiller.org/forum/viewtopic.php?f=3&t=5041
is this good enough or should i keep going i found these sights in 5 min do your research before you brew 'PLEASE'
sorry you can do it if you want to i will not make my spirits in it and personally wouldn't drink it but go ahead not trying to sound rude it just isn't for me
I just don't want anyone to 'DIE'
laserjocky (author)  jtucker1410 months ago
I understand your concern but I disagree. From a scientific standpoint I wouldn't exactly call answerbag.com or yahoo answers references. There is one linked paper from India that looks reasonably legitimate which states,

"Therefore, it can be suggested that general neurotoxicity produced by aluminum is not modified by ethanol. However, the aluminum load caused by aluminum exposure, may be influenced by ethanol co-exposure."

In other words, ethanol MAY help your body absorb more aluminum, but doesn't convert aluminum into poison. The same could be said of having a beer with the meal you cooked in an aluminum pot.

The methodology of the paper included dissolving large amounts of aluminum in "nitric acid, sulphuric acid and perchloric acid in the ratio of 6:1:1" and feeding it to rats. Wort is slightly acidic, nowhere near H2SO4 and HNO3.

Aluminum metal is highly reactive. It reacts with oxygen to form Al2O3, which is one of the most stable compounds known. It's sapphire. It's sandpaper. Any aluminum exposed to air will immediately form a coating of Al2O3. Al2O3 has a boiling point of 2,977°C, which is a little hotter than a pot still can get. Other aluminum compounds tend to have extremely high boiling points or undergo decomposition at high temperatures before being able to boil. That means aluminum in a pot still is very unlikely to make it out of the pot still, since that requires the aluminum compounds to boil.

You might run into a few more problems if the condenser was made of aluminum. Or if the container used to store the spirit was made of aluminum. But I very much doubt an aluminum pot still could do anything worse than if your grandmother cooked you some spaghetti sauce in an aluminum pot.

I understand the "better safe than sorry" mentality. Aluminum is kind of a touchy topic. There is a lot of pseudoscience surrounding relatively mundane things like aluminum, copper, magnets, vaccines, etc. But there is a big difference between informed caution and fear mongering. Given the evidence considered here I hardly think warnings of death are warranted.
http://www.answerbag.com/q_view/2253999
http://answers.yahoo.com/question/index?qid=20070330162444AAjZosw
jtucker1410 months ago
DO NOT EVER USE aluminum to distill spirits you will poison your self or someone else aluminum poisons spirits use copper or stainless PLEASE
laserjocky (author)  jtucker1410 months ago
That's an important claim if it's true. I haven't found any good documentation of that. Can you please provide a reference?
skwoorl1 year ago
I like the way this instructable is laid out, very easy to follow. I have heard that crushed glass works great as copper pot scrubbers are somewhat hard to find. If accessible, well sanitized auto glass breaks into nice small pieces, just right for this application.
skwoorl1 year ago
To be certain that you get the most efficient flow of coolant and also more surface area inside the condenser, could one step up the dia. of the tubes used for the condenser chamber? Say inner tube 3/4" and outer at 1.25 or 1.5" even?
wanabepro1 year ago
thank you
good post clears up my problem.
wanabepro1 year ago
Hello sir
I understand most of your design but am having trouble with the thermometer. were is the sensor located.is it in the column above the packing. I'm just not sure.
laserjocky (author)  wanabepro1 year ago
The sensor (thermocouple) is the silver probe which is stuck all the way through the rubber stopper at the very top of the vertical column. You can use a regular thermometer if you wish, but digital thermocouples are not hard to come by, and they are much more accurate. Just be sure to get one that has a rigid metal probe. This one or anything similar would work:

http://www.ebay.com/itm/LCD-Type-K-Digital-Thermometer-TM-902C-2-Thermocouple-Probe-/190579208001?pt=LH_DefaultDomain_0&hash=item2c5f67ef41

The probe should be positioned to read the temperature of the vapor right where the vapor travels through the T section on its way to the condenser. Don't let the probe touch the column packing or the side of the column, and be sure the probe is sticking through the stopper, not with the tip inside the rubber. It should be measuring the vapor temperature only.
Does anyone appreciate the irony that there are 12 steps in this project?
logicrules1 year ago
Vaary nicshe, a'll drink to thish, hic
Sergei-2 years ago
Hi

Nice looking fractional pot still, I would have tried to find 304 or 316 stainless for it because of the pain in the ass cleaning of copper after each run or you get opper sulphate in it and then you go blind, but keep the copper scrubbers because if theres no copper at all there will be an unpleasant rotten egg smell

Looks like your running it a bit to fast, to get a purer spirit it should be about 80 deg c - for a pot still might be a bit higher but not to close to 100c

Nice job in the soldering make sure it's lead free solder or you will get led poisoning without a gun involved hahahaha but seriously it's no laugthing matter

Heres my setup
All glassware and fits to a modified 50 litre keg
IMG0125A.jpg
http://www.labdepotinc.com/Product_Details~id~761~pid~59709.aspx


I found this from a chemestry supply store for $250... do you mean that glasss would be safer to use... and are you saying coppy plays a role in filtration?


Broom2 years ago
Thank you for this tip:
"If you want a clean-looking joint (no solder blobs), quickly (before the solder solidifies) brush the exterior of the joint with the flux brush AWAY FROM YOUR FACE. This will remove the majority of the exterior solder drippage."

I'll try it next time I plumb, for whatever reason!
dacuna012 years ago
This pressure fitting is gas tight? Does the lid just jam tight against the edges of the copper female adapter?
laserjocky (author)  dacuna012 years ago
Sorry for the slow reply. There is a very small amount of leakage when using the fractionating column, about as much as what escapes from the emergency pressure release thingy (to use the technical term). I may seal this with epoxy at some point but it hasn't been a big problem so far.
A very old school way of sealing small gaps in a still was to mix a dough of just flour and water and use the paste to seal any small holes- the advantage to this is that it is non-toxic- when you are done wash it of and reapply next time- no risk of hot liquids/ gasses/ being affecting the epoxy or the epoxy contaminating your process.
laserjocky (author)  shantinath10002 years ago
Actually I tried this method. I must not have done it right because it didn't work very well. I was probably supposed to let it dry. I get a little frantic and impatient at the end of a project. I'll have to try it again next time.
sschoemann2 years ago
The best thing about the "green energy movement in the US, is that they have lifted the prohibition on nome distilling alcohol, as long as it us used for fuel purposes mind you...
Actually I believe you still have to register with the ATF and pay fees to do any distillation of alcohol. Before going ahead with distilling anything, even if you are just using it for fuel, I'd double check with the ATF because there is no difference between a rig for making fuel and one for making drinking alcohol.
I've done some research into the distillation subject because of my son's
interest. It is illegal to do any distillation at home for any purpose
unless you buy a distillation permit from the government to
"distill fuel." The information that I gathered was, In Illinois it cost
$3600.00 for a permit for fuel distillation for one (1) year. No
individual is allowed to distill spirits for their personal or any other
use. You can make beer and wine to your hearts content, but distillation
will end in trouble. The main reasoning that was given was the government
claims that you will get lead poising. They think the public is still
using car radiator to use as a condenser.
The main reason would be ... tax money. If people really were free and they acted so freely as to actually do something that man has been doing for thousands of years then they gov't types wouldn't have the power to tell them what to do and what not to do and to have a nice cushy gov't job and benefits because there wouldn't be tax dollars enough to go around.
I believe that to be very true, and the real reason we can't distill our own.

There is too much profit from the taxes collected from the sale of the spirits.
A great portion of that revenue would be lost, So the government spreads the
false story about getting lead poisoning if you distill your own.

We have come a great distance since prohibition and World War II, but the
government wants to keep us there. Locked in that period's frame of mindset.
You also can distill.. essences. Dunno if there it's illegal or not. But these things usually are illegal to avoid people
Lead poisoning could happen, if you use lead xDDD

Prohibition in distilling is only for money, gov money, big companies money. As many other things, they are not interested in you know the procedures but as information flows then it's better forbidden some activities.

There is a risk in distilling but i think it's not much more than cooking with the pressure pot (a real one with the valve).

I'm interested in this instructable just for essences (herbal essences).

Nice job :D
You can make 15 gallons of hard liquor a year back in 1991, I don't know if they chanced the law, but back when you could brew up 195 poof and then mixed down to 60 poof as according to state law.
Sorry, not any more. Not without that license form the state. They are pretty
adamant about no one distilling. Home breweries for beer and wine are okay
because you are fermenting, zero tolerance on distilling.
laserjocky (author) 2 years ago
A BIG Thank You to everyone who voted for me in the Mad Scientist Fair! You guys rock!!
DavidKaine2 years ago
Here's my setup.  It's almost identical to yours, except for a few modifications. My coolant is a closed loop using an aquarium pump I had from an old computer water-cooling setup.  I found some great 3-way fittings at Home Depot that were like 1/2" - 3/4" reducing couplings but with a 1/2" fitting coming off one side. I drilled out the retaining lip inside, put the fittings on either end of the 3/4" tube, then passed the 1/2" tube through it.  soldering was interesting, but not terribly difficult.  I also forewent the screw fittings to save a bit on cost, and just slip-fit the pieces.  I was able to tap 3/8 NPT threads into the pressure relief valve without even affecting the valve seat, so I can even still use it as a pressure cooker.  Let me know if you see something you're curious about.
columnating.jpg
laserjocky (author)  DavidKaine2 years ago
I thought about trying to use the threads that were already in the cooker. I'll have to try that out next time I make one of these.
Light_Lab2 years ago
I am sorry aeturnusjunk but a metal still is not "laboratory quality". Glass is used in laboratory stills to minimise metal ion contamination. Also hot copper is sufficient to catalyse reactions with ethanol.

http://www.sciencemadness.org/talk/viewthread.php?tid=8709

People do get away with copper stills all the time by avoiding hotspots, even commercially, but it is risky.
Sorry, I didn't mean to discourage you. You don't have to be a glass blower though, in the lab we use QuickFit glassware
http://en.wikipedia.org/wiki/Quickfit_apparatus
- expensive but very good and lasts. Before quickfit we used to use glass tubing and corks.
In industry potable liquids including wine, beer and spirits are processed through stainless steel. When I was a teenager I made a water purification still from aluminium. The tank eventually corroded but it provided many years of service. 
In the alcohol industry they use copper because during fermentation the yeast puts out sulfides. Using copper will remove these from your distillates as it works.

At least that is what I have been lead to believe.
Yes some commercial stills like the Coffey Patent still are made from copper and often hillbilly stills had a copper cooling coil. But these stills are not Lab quality; the small traces of copper ions introduced would be unacceptable. Keep in mind that the most significant use of stills in the lab is for the production of highly purity distilled water.
When copper is used in alcoholic beverage industrial stills care is taken to ensure that no hot spots occur that could cause the reduction of alcohol to aldehyde. The small trace of copper introduced into alcohol during contact at low temperature is usually low enough that drinkers are not at much risk.
Yeast doesn't produce significant sulfides during fermentation, though often H2S is used to destroy wild yeasts in the ingredients before the introduction of the yeast culture. Sulfides are pretty toxic to yeasts. The low pH of the must would make the formation of copper / sulphide compounds unlikely, most trace sulfides end up as gaseous H2S and leave the system.
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