Chemistry Peeps: Help my distillation please.

January 23, 2008 5:52 PM

I'm doing research in prep for some small batch distillation of corn liquor/moonshine. (For educational purposes only.) Very specific question inside.

From what I've been reading, my mash will produce some methanol before prior to producing the consumable ethanol. I understand the methanol arrives first with the lower distillation temp.

How do I determine which is which? Do they burn with different colors, for example? Any advice or ideas are greatly appreciated.

This is just for fun, but I don't want to hurt anyone (myself) in the process.

Best Answer gets a quart jar!

posted by snsranch to science & nature (28 comments total)

I am not a chemist, but knowing the s.g. of the two chemicals involved you could use a hydrometer to determine which is which.

http://en.wikipedia.org/wiki/Hydrometer
(I hope one of the above appears a link).
posted by lungtaworld at 6:05 PM on January 23, 2008

Dude, there's a reason the feds regulate production of booze. Screw it up and you could end up blind or dead. Might want to anonymize this at least.
posted by cosmicbandito at 6:08 PM on January 23, 2008

"A simple (but effective) rule of thumb for this is to throw away the first 50 mL you collect (per 20 L mash used) for a reflux still. If using a potstill, make it more like 100-200 mL. Do this, and you have removed all the hazardous foreshots, including the methanol. "

From http://homedistiller.org/.

I'm jealous. I just recently found my old copies of Foxfire and it has very detailed plans for a still, but it looks like more work than I can commit to. Good luck!
posted by dirtdirt at 6:11 PM on January 23, 2008

I think the specific gravities of the two chemicals are too similar to use a hydrometer you could buy at a homebrew store. If you can get a more accurate one, that might work.

Otherwise, their boiling points are significantly different. Methanol is about 65 degrees C, ethanol about 78.5. So, you can actually distill out the methanol first by heating the whole mixture to slightly higher than 65, and I imagine use the same process that you would to distill out the ethanol.

Through cursory research, it seems a bigger fear would be lead contamination from using lead-soldered pipes and other bits. So, I'd worry about that more than the methanol.
posted by backseatpilot at 6:20 PM on January 23, 2008

(Fed-wise, I think you are OK if it's for personal consumption. I'm not your fake lawyer, etc.)

I made some of that stuff once. It was REALLY potent and tasted like kerosene, but I did not go blind. We did try backseatpilot's method of boiling to 65 but under 78.5. If I was going to do it again, I would use a more fool proof method.
posted by gjc at 6:30 PM on January 23, 2008

I am not a chemist. I do have a laptop, internet access, and some time. I can only point you to this web page that claims that methanol is not and cannot be a by product of distilling when making moonshine. This other page suggests that if any forms, it is in very small amounts unless you are distilling alcohol that comes from fruits containing pectin, so with corn the amount is negligible. Finally, this page discusses making moonshine and has lots of stuff in the comments. So I would suspect that with corn you would be ok. Probably tossing the first 50ml to be sure.

Good luck!
posted by procrastination at 6:36 PM on January 23, 2008

gjc: Fed-wise, it's not OK.

I once observed a friend of mine working a column still, however. As I recall, he just arbitrarily discarded the initial 50 or 100 ml of product as heads. Wasn't much. Identifying when the tails began was trickier - he was sniffing and tasting the output towards the end of the run. It's apparently a detectable change in quality, but I don't know how to describe its onset.
posted by mumkin at 6:47 PM on January 23, 2008

Oh, also, Foxfire is unclear on the point of methanol. They do say to filter through hickory coals, to remove impurities and the, um, "bardy grease". You dxon't want to have bardy grease in your ruckus juice, do you?
posted by dirtdirt at 6:51 PM on January 23, 2008

Methanol is about 65 degrees C, ethanol about 78.5. So, you can actually distill out the methanol first by heating the whole mixture to slightly higher than 65, and I imagine use the same process that you would to distill out the ethanol.

That's not how it works. Though methanol boils at 65 ºC, a mixture of water and methanol does not boil at 65 ºC, so heating the mixture to 65 won't really boil off anything.

Others are right that if the concentration of methanol is small, it should all come out near the beginning of the distillation.

I'm pretty sure there's no easy at-home assay for the presence of methanol. The only way I can think to do it is to send samples away for GC/MS analysis. An analysis service should be easy to find (here's one to try), but it might be more expensive than you like.

They do say to filter through hickory coals, to remove impurities and the, um, "bardy grease".

I don't think charcoal filtration will remove methanol any better than it removes ethanol....
posted by mr_roboto at 7:00 PM on January 23, 2008

@gjc: no, I'm pretty sure distilling any amount of drinkable ethanol without a license is a crime in the US.
posted by ArgentCorvid at 7:05 PM on January 23, 2008

Bardy grease is not methanol, I did not phrase things clearly enough. According to this article it is an actual oily residue that floats on top of the corn beer, before it is distilled into whiskey. According to this book, anyway.
posted by dirtdirt at 7:07 PM on January 23, 2008

It is legal in many states. I never really wanted to do this, especially after the pillsbury dough boy, my high school chem teacher, had us distill some rum type stuff and let us try it, OMG, Dave's Insanity Sauce is easier to stomach, even drop for drop. If our technique were better, we might have had better results. Make wine, make beer, buy hard liquor from the pros.
posted by caddis at 7:11 PM on January 23, 2008

Nuts, you're right mr_roboto. And to think my alma mater gave me a technical degree. The fools!
posted by backseatpilot at 7:21 PM on January 23, 2008

to clarify, It may be legal by state law, but federal law prohibits any distillation of ethanol without a license. the BATF would like to have a word with your HS teacher, caddis...
posted by ArgentCorvid at 7:22 PM on January 23, 2008

Wow, color me educated. Sorry for the misinformation!
posted by gjc at 7:24 PM on January 23, 2008

Thanks everyone, for the input. I'm determined to do this even if just to see if I can pick up an old family skill and tradition. Sadly, I've waited until now to begin to care about such things, because any family member who could have helped me with this is gone. I'm hoping that this will be less nasty and more like a top shelf vodka.

Yee Hoo! If this really works well, you'll be able to check it out on Projects.
posted by snsranch at 7:36 PM on January 23, 2008

Speaking hypothetically, if I was going to do something like that, I would make the firewater as strong as possible, and then filter it through a Brita about 10 times, and then water it down to 80 proof-ish with the best tasting spring water I could find.

I'm just guessing there, but the good vodkas and gins I've had always had sort of that smooth flavor that a good spring water has.
posted by gjc at 8:25 PM on January 23, 2008

I had never heard the term "ruckus juice" before. Thank you dirtdirt. I will use that often.
posted by JohnnyGunn at 8:55 PM on January 23, 2008

I can't speak for straight distilling, but a word of warning, if you plan to filter. I freeze-distilled a few gallons of hard cider, and then ran some of what I got through a brita, just for kicks.

Big mistake. I'm not exactly clear on what happened, but my Applejack went in looking like apple juice, and came out looking like iced tea. Needless to say, I didn't drink it. Nor will I be filtering my next batch.
posted by god hates math at 9:05 PM on January 23, 2008

Otherwise, their boiling points are significantly different. Methanol is about 65 degrees C, ethanol about 78.5. So, you can actually distill out the methanol first by heating the whole mixture to slightly higher than 65

No. Go back and learn about azeotropes and try again.
posted by ikkyu2 at 9:20 PM on January 23, 2008

backseatpilot writes "Through cursory research, it seems a bigger fear would be lead contamination from using lead-soldered pipes and other bits."

This is a lot easier to avoid now that you can easily buy lead free solder (Actually it's getting kind of hard to buy leaded solder, at least around here). However you can avoid the problem entirely by skipping the very expensive copper (with the exception of the condensing heat exchanger) and going with glass, silicone/rubber, and stainless for your still. A good source for a vessel to hold the mash is a large stainless pressure cooker (avoid the aluminum type). It's a bit more expensive to buy fittings to connect everything up but most people don't have the skills or equipment to make stuff from scratch by soldering sheet copper anyways.
posted by Mitheral at 10:32 PM on January 23, 2008

No. Go back and learn about azeotropes and try again.

Are you claiming that the methanol will for a tertiary azeotrope with the water and ethanol? I don't think that's right.
posted by mr_roboto at 10:53 PM on January 23, 2008

Back in the mists of time, I came into a very fine glass still. A little like a Liebig's condenser, but with an open bottom that you could place over a suitable sized boiler. I fermented a heap of sugar using some yeast that would be stable up to about 14% alcohol by volume. I let it rip for a few weeks until it was evident that fermentation had ceased. The fermented liquid was still very sweet to taste, so I assume it had reached a high enough concentration of alcohol to have killed the yeast and stopped fermentation.

Anyway, I batch-distilled this in 3 liters batches. The first half-cup or so of distillate from each batch was discarded, and the rest carefully collected. To this day I don't know how strong the product was, but somewhere between 'very strong' and 'heroic' sounds about right. I ended up with about 2.5 liters of the stuff.

That was the easy part. The hard part was drinking it. It tasted like someone had steeped old gym socks in it, and it burned like the fires of hell. Eventually a friend and I hit on the idea of mixing it with lime juice cordial and diluting it with mineral water - both of which I had handy at the time. We drank some and we drank some more. I don't remember how the evening ended, but I woke up the next morning feeling surprisingly chipper. A large plastic bucket and a jug of water was beside my bed. I marvelled at how considerate my housemate must have been to have put them there. I later found out that I had in fact been seen last staggering down the hall with said bucket and jug, but alas that memory remains lost to me.

I toddled off to work feeling as though I had dodged a bullet, as my wonder-liquor apparently did not produce hangovers. About midday, I started to feel a little off-colour. By 1pm, I was sitting under my desk in my office with the lights off. My kidneys ached. I had hot and cold flushes. I thought I had poisoned myself. Which, quite possibly I had done.

Anyway, I've been there and done that and lived to tell the tale. It's not too difficult, and by my reckoning there is enough information in this thread to do it relatively safely. Whilst I wouldn't dissuade anyone from trying this - provided they have some basic chemistry knowledge and common sense - I'm never going to do it again. There are wonderful spirits in the world, each blessed with its own subtle taste, heady aroma and any other number of good qualities. Perhaps in time I would have gotten better at distilling, but I reason that since I only have the one liver I'd rather spend it drinking Laphroaig or Tanqueray #10 than trying to work out just where I went wrong again in my latest batch of gutrot hooch. But good luck to you.
posted by tim_in_oz at 11:16 PM on January 23, 2008 [1 favorite]

federal law prohibits any distillation of ethanol without a license

a little research shows that this is in fact correct. I think I was misremembering old discussions from some home brew blogs on this subject. anyway, it is illegal and if you make a noise about it they will chase you down, or perhaps not be inclined to bother, but don't go do something dumb like make a web page with all your distilling exploits exposed
posted by caddis at 12:02 AM on January 24, 2008

I perhaps should have said that I came into possession of a very nice glass still. I make this amendment before anyone can suggest that I was responsible for the hooch smelling like old socks.
posted by tim_in_oz at 1:07 AM on January 24, 2008

If your educational purposes are performed within the confines of a university, federal law might not be an issue. The US Code has an exemption for experimental research conducted at colleges and universities. It looks like the Treasury has implemented some pretty strict regulatory hurdles, however.


no, I'm pretty sure distilling any amount of drinkable ethanol without a license is a crime in the US.
If you want to get technical, and I suspect the sorts of people who build stills for fun like to get technical, it's possible that the laws AgentCorvid are talking about might be overbroad when it comes to personal usage. During the Warren era, the Supreme Court gave Congress great leeway in exercising it's Commerce Clause authority. The more modern courts started to roll back this authority in with Lopez in 1995.

So you could make the argument that if no part of your production (and perhaps personal production in general) had a sufficient nexus with interstate commerce, that Congress had exceeded it's authority and ask for those provisions to be struck down. How do you feel about being a test case, snsranch?
posted by averyoldworld at 9:08 AM on January 24, 2008

Actually, please don't be a test case - the Commerce Clause is important to a lot of civil rights statutes. We need those.
posted by averyoldworld at 9:12 AM on January 24, 2008

Hey, thanks everybody! This is fun and interesting stuff. It's time to pour some yeast into a can of creamed corn;)
posted by snsranch at 4:19 PM on January 24, 2008