Home distillation

Sepulchritude Forum: The Absinthe Forum Archives Thru July 2001: Home distillation
By Don_Walsh on Friday, July 06, 2001 - 09:02 am: Edit

A 1.14 liter (what's that? A quart?) of cheapest vodka $25 Canadian? I reckon that, converting to 75 cl and US$, that's about $7, so not too much more than the $4.50 or so for swill New Jersey vodka sold retail in Thailand ('Petrov' and 'Sasha').

By Wolfgang on Friday, July 06, 2001 - 07:47 am: Edit

Just a side note...

"I go through 3 to 6 metric tons of sucrose a month"

...So he's realy doing thousand of bottles of absinthe and don't sell it yet so it means there's a large vault somewhere where tons of emerald elixir is slowly aging...

Wolf...Dreaming...;-)

By Wolfgang on Friday, July 06, 2001 - 07:34 am: Edit

In Quebec, about 50% of alcohol price is tax...

The cheapest vodka is about 25 CAN$ for 1.14 L. and Stolichnaya is 31 Can$. A cheap brandy is about 28 Can$ in the same qty. (1US$ = 1.51 Can$).

A bottle of Deva delivered to my home cost about 45 Can$ so it wont be cost effective (unless I manage to brew something far supperior to Deva, witch shouldn't be difficult after some adjustments).

By Zman7 on Friday, July 06, 2001 - 06:12 am: Edit

Outstanding treatise for the home distiller Don! I have used the Christian Brothers/Cheap Vodka method for distilling high proof ethanol for awhile now and the results have been great. I run my through a "reflux" system and have been averaging about 90-93% ethanol after one pass through. Thanks again.

By Don_Walsh on Friday, July 06, 2001 - 05:35 am: Edit

Yes, caution is a good idea, but I doubt that Wolfgang is of a mind to combine his ethanol with red fuming nitric acid like old Werner.

I hope Wolfgang knows not to do this in an apartment building; even a house is a little chancy, an outbuilding dedicated to the purpose is best and emergency equipment ought to be on hand. You must plan for contingencies. Coolant supply failure? Glassware fracture? Within the still/apparatus the vapor will have displaced any air but it it leaks or breaks...then you have a rich fuel air mixture and any spark or static could ignite it.

BTW, once you have 'enriched' ethanol, if you fermented it yourself, you always cut it back to 40-50% at most for redistillation and/or carbon treatment. For redistillation, if you don't cut it back you'd be distilling down to a small pot volume and that's a bad idea, the heating mantle makers will tell you what the minimum safe volume left in a given glask size ought to be. For carbon treatment, 40-45% works better. So ideally:

-- Ferment
-- Strip the wash/mash to 40-60% (depends how much % abv was in there, you can tell by hydrometer but accuracy will be poor till you purify. You can also tell by initial vapor temperature and predict the initial product concentration from that, but remember, that's going to decline as you are constantly going to be taking off less alcohol as it is depleted and more water as it is enriched. This describes a simple still, not a fractionating still.

-- Carbon treat, in one or more steps

-- Concentrate again, more carefully.

-- See if it is pure enough. You can do this instrumentally or by wet lab methods.

-- If not pure enough, cut back to 40-45% and repeat the carbon treatment. Then concentrate the alcohol and test it again.

Activated carbon works wonders if you know what grades to buy, how to prepare them, how to use them, and how to store them and sometimes reprocess them so they can be used further, after they get saturated with the fusels etc. Don't try to reuse powdered AC; and not all types of granular AC are suitable for recovery. Don't use household water filters! AC is cheap and efficient.

By Wormwood on Friday, July 06, 2001 - 04:01 am: Edit

Just remember, when Dr. Von Braun was looking for rocket fuel to power his V-2 rockets he picked ethanol for a good reason.

Don't blow yourself up.

By Don_Walsh on Thursday, July 05, 2001 - 09:19 pm: Edit

Whoops, I addressed that one to Andy when it ought to have been to Wolfgang

By Don_Walsh on Thursday, July 05, 2001 - 09:16 pm: Edit

Andy, if you can't find neutral spirits, but want to proceed in modest quantities but not with the tedium of fermentation and distillation/purification, there is a better option. Buy cheap vodka or brandy (cheaper the better), and simple-distill (pot still) this to strip out the ethanol. 40% will get you 80% in one pass with no reflux, just collect 50% of the pot volume and I think your hydrometer will tell you it is now 80% abv. (160 proof). Another pass and it might not be 96% but it will be strong enough for steeping herbs. And you won't have to worry about heads, tails, purification, activated carbon etc, at all. Here, there are cheap American vodkas on sale for $4.50 US per 750 ml. Christian Brothers brandy is only a little more. Each bottle will get you 400 ml of 95% or 500 ml of something useable for steeping. This is fast and easy, and <$10 gets you a liter, enough to make about the same volume of absinthe. (Maybe Canadian liquor taxes are higher than Thailand's but I doubt it.) I did this myself until the quantity I needed was large enough to justify making my own. All you will need is a flask, a still head (Claisen head), a thermometer, a condenser, a receiving adapter and a receiving flask, a heating mantle and controller or variac, a water supply, some tubing, some supports and clamps, and some nerve. The good news is that simple distillation is much faster than fractionating which is about as exciting as watching paint dry -- until something goes wrong and then it is the sort of excitement you want to avoid. I recommend a 5 liter setup with 29/42 standard taper joints. The same setup can be used to strip ethanol from vodka/brandy, and then to distill the steep liquor you make from the results. A 5 liter setup will handle enough steep liquor and herbs to get you 750-1000 ml of absinthe. Bear in mind that you can't put 5 liters in a 5 liter boiling flask, you should not charge it more than 55-60% full at most, and 50% is better. Be GENTLE with the heating by mantle or you will char your herbs. A water bath, or oil bath, would be better. If a water bath, you will have to run it at a boil; if an oil bath, use a non flammable silicone oil, or pure (non smoking) peanut oil, at 100-110 C and put a shield between yourself and the bath in case of a splatter.

I suppose you know this but NEVER even think about distilling alcohol or absinthe by an open flame. Would you distill gasoline that way? Duh! Ethanol and petrol have similar vapor pressures and flash points, and ethanol forms explosive mixtures with air in a wider range than petrol. That's why you can run an older car on 160-180 proof ethanol (not gasohol, straight ethanol) if you just pull out a little on the choke. RESPECT ethanol becasue if you disrespect its flammability it may disrespect your life and property.

By Wolfgang on Thursday, July 05, 2001 - 08:19 pm: Edit

Thank you guys. So my intuitions where not too far away... The reason I was thinking of doing my own pure alcohol was to reduce cost (and also for the scientific pleasure of building and ajusting my own still). After rethinking the whole cost isue, I figured I would have to make absinthe in quantity and sell some of it to make it cost effective.

For the only pleasure of doing absinthe for my own consuption, I better buy the neutral spirit. I'm just not sure if neutral spirit can be fond in Quebec... I doubt SAQ sell it.

Anyway, if I build it, I will just design it in a way that I will have the choice to use the reflux or not... For the electronic control and TC, It will be the easy part for the little electrical engineer I am. I'm more affraid about the chemical side of the job ;-).

Anyway, even if I never build it, it`s still interresting to do some research...

By Don_Walsh on Thursday, July 05, 2001 - 07:29 pm: Edit

Wolf, while fermenting and distilling your own neutral spirits is possible, it is an awful lot of work for what results are usually obtained. It is the purification of the ethanol that is tricky, and if not done correctly, will result in bad tasting hangover producing contaiminated ethanol. The purification is best done by a combination of careful distillation, preferably by a well set up and SLOW fractionating setup, run at a high reflux ratio, and then a fixed bed of activated carbon, possibly multiple beds, until the desired purity is obtained.

The equipment investment can be high, the time and labor are definitely high.

ANYONE who can do so, is far better off buying (usually taxed) 95-96% potable neutral spirits, in my humble opinion.

I make ethanol every day and on a substantial scale. I go through 3 to 6 metric tons of sucrose a month, deal with half a dozen yeast vendors, and have a huge electricity bill, to prove it. I do this because I can't get the alcohol I want any other way, to the quality that I need. The moment that that situation changes, I will have seen my last fermentation.

Fermentation is fairly easy, if you are meticulous about hygiene. But there are a lot of ways to mess this up.

Distillation is relatively easy, if you know what you are doing, and have anticipated a variety of potentially catastrophic failure modes.

Rigorously purifying the ethanol you make is NOT easy, you will spend more time RE-distilling the ethanol than you spent originally stripping it from wort, and a high r.r. column, in order to have the right boil up rate to achieve a reasonable throughput, is a LARGE EXPENSIVE column. When I say large I mean 1 meter long or more and 3-4 inches in diameter. Preferably, vacuum jacketed and silvered. Such a column might be coaxed into producing say half a liter to a liter an hour of 95%, without flooding. It will take hours to get such a column to equilibrate, and all the while you will be expending the energy to maintain a boilup of 10 liters an hour or more (reflux ration = 10). This is not a lab bench scale setup, it is a pilot plant scale setup, and it isn't cheap. The column alone is several thousand dollars.

A temperature controller and thermocouple sensor is a good idea. Placing the tc on the good side of the column can be done but it is trucky as until the boilup has reached top of column you will get nothing on the tc and until the column equilibrates you will get erratic readings, neither of which do you much good in controlling your heating mantle. Also, temperature controllers vary widely in design, price, and quality of engineering. I have half a dozen of them, and have ome pretty firm opinions about what goes into a good one. A temp controller is no substitute for human monitoring.

NONE OF THIS APPLIES TO ABSINTHE. As Artemis points out, absinthe is always distiller in a simple, pot still with NO reflux head or column. Any sort of such will strip out all the herbal oils and return them to the pot.

By Zman7 on Thursday, July 05, 2001 - 05:39 pm: Edit

Wolfgang,
If your'e looking for a decent page with information try Tony's site
www.geocities.com/kiwi_distiller/
It has many types of stills and information for the starting home distiller.

By Artemis on Thursday, July 05, 2001 - 02:35 pm: Edit

Absinthe was made with pot stills, not reflux stills. Refluxing is the opposite of what you want to do to carry over herbal tastiness, I would think.

By Wolfgang on Thursday, July 05, 2001 - 01:53 pm: Edit

I finally found some nice information on how to build what looks like an efficient ''Home distillation apparatus'' involving reflux distillation. I would appreciate some comments from experimented forumites.

I think this still can be usefull to distill the pure alcohol used as a base for making absinthe (when setting the column at a high reflux ratio).

Once you get this alcohol and mix it with the herbs to make absinthe, you then have to distill this mess again to get a palatable absinthe.

I just wonder if this last distillation should be done with a lower reflux ratio to keep some taste in the final product... Maybe a simple pot still would be better at this last stage ?

Anyway, with this apparatus, you can control the reflux ratio, witch may be usefull to make absinthe if my humble intuition is good...

http://members.nbci.com/mtoal/books/home-distillation-apparatus/

Personal note : I would add some thermometers along the column and maybe a temperature controler linked to a column output thermo couple...


Wolf (who may eventualy give it a try if he can find the necessary money to build this tool and buy all the nessesary test equipment...)

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