Freezing / Jacking

NOTE:
this fake-still design is NOT recommended. It is much better to design and produce and use a REAL still

Freezing

Another technique is to freeze the wash, and separate the ice (water) from the alcohol. Freezing appears to fall somewhere in-between the legal issues for many areas (eg can you really stop your Applejack from freezing if its left outside ?). Sort it out with your own authorities (or just keep your freezer contents personal).

One thing to be aware of is the the more alcohol that is in the wash, the cooler it will need to be before it freezes ... Disolving (or mixing) something into a liquid will make the freezing point go lower than when it is pure (see the full theory at http://www.chem.vt.edu/chem-dept/dillard/1074Lecture27.pdf)

dT = Kf m where Kf(water) = 1.86

Adding ethanol to water will therefore depress the freezing point by 1.86 C per molar conc present. Doing the translation between molar and regular % by volume gives ...
5% abv 1.6 mol% 3 C lower
10% abv 3.3 mol% 6 C lower
20% abv 7.2 mol% 13 C lower
30% abv 11.7 mol% 22 C lower
40% abv 17.1 mol% 32 C lower
50% abv 23.6 mol% 44 C lower

This explains why beer (at 5% abv) will freeze for ya in the freezer, wine will need it to be a bit colder, but frozen schnapps or vodka won't normally be possible.

Scott adds more details ...
    from http://users.stargate.net/~mshapiro/cfoot.html .. Another method, known as fractional crystalization, is done by inverting the process and freezing the beverage instead of boiling it. This works for very similar reasons to that of normal heat distillation, namely, the differential in freezing points of the two liquids involved. Water freezes at a temperature of 0 C, while ethyl alcohol does not freeze until reaching -114 C.

    This allows the water to be frozen out of the liquid, leaving behind the ethyl alcohol, as well as the other alcohols and esters. This produces a drink of a rather different character from heat distillation, as it contains everything except water, while heat distilled beverages leave everything behind except alcohol. Note also that simply lowering the temperature to 0 C will not produce an increase in alcoholic strength. The temperature required for this process is in the range of -15 C and below, but must vary, much as the diurnal cycle naturally does.

    This allows crystals of ice to form as the temperature drops. As the temperature rises slightly the alcohol will drain out of the crystals so that when the temperature again goes down and more crystals of ice re-form they are purer crystals of water, containing less alcohol. As this process repeats itself the solution will gradually work its way toward the alcohol concentrations listed in the following table which is adapted from a chart on page 102 of the book, Wines & Beers of Old New England:

    Temperature (F/C)% Alc.
    10 / -12.28
    5 / -15.011
    0 / -17.814
    10 / -12.28
    -5 / -20.617
    -10 / -23.320
    -15 / -26.124
    -20 / -28.927
    -25 / -31.730
    -30 / -34.433

There is an excellent account of the history of using freezing at http://www.celticmalts.com/Edge.htm (Whisky on the Edge) by Alex Kraaijeveld.

I've just tried making some myself, with no success. Poured 1.5L of beer into a plastic container, and put it in the freezer. When frozen, I broke it open. The trouble was though that it appears that it all froze too fast - any alcohol there is trapped within the ice matrix - there was no clean "core" of alcohol. I think that if this is to work, you will have to freeze it VERY slowly, so that the alcohol has time to diffuse its way ahead of the freezing ice front.

Raj tells me though that to get a good clean separation ...
    The trick with freezing is to partially thaw and refreeze a few times to promote larger pieces of ice--the frozen cylinder with a heart of alcohol is the consequence of diurnal cycling in a barrel over weeks.

Jack tells me though ..
    Don't bother trying to get a frozen heart of alcohol- it's not really needed. Just fill a gallon (4liter) milk jug half full of your beer/wine, let it freeze solid in the freezer, then get a one quart (1liter) wide mouth jar, and stand the milk jug upside down in it. It will take about four hours or so, but eventually as the ice slowly melts (don't apply any heat), the jar will fill up, and you will have just about doubled the alcohol (by cutting the volume in half). using a 10% wine this method will turn a half gallon into a 17% quarter gallon. I have not tried sticking this 17% wine back in the freezer to see if I can get any more ice out of it, but it's worth a try. It also seems to be the easy way to get "distiller's yeast" performance without fooling about with yeast starters and the like.

There's an excellent book by James Hay called "Homespun Spirits", explaining how to "spin" the alcohol out. Basically what is done is ...

Standard wash is prepared as for distillation - resulting in a liquor of 12-20% alcohol. This is then poured into 1.25 - 2L PET soft-drink bottles. Fill the bottles with little headspace. Shake the bottle to aerate them, so that plenty of air bubbles will form during freezing. Freeze solid (may take several days). Cut V shaped slits into the side of the bottles. so that the points face away from direction of rotation. Approx five rows of four slits, each with sides & base approx 10mm long. Make a couple of air holes above the solid surface. Modify a bottle cap so that it fits into a power-drill - eg thread a long bolt through it, with a couple of washers, and a nut to hold it all in place. Tighten the drill chuck around the length of bolt that extends. With the bottle attached to the drill, spin the bottle inside a tall container (rubbish bin). Use a variable speed drill, so that you can control the speed. The slits create an aerodynamic drag, forming a vacuum. This causes the air bubbles to expand, breaking up the ice, and releasing the non-frozen alcohol. Keep at full revs until no more alcohol is seen running down the side of the bucket, or ice starts coming out the slits. Slow the speed down slowly. Store the spirit for a couple of weeks to let it clear, then polish as for distilled spirit.

However, Ups474 writes :
    More correctly known as "fractional crystillization", the practice of freezing an alcoholic mash then removing the (concentrated)alcohol was used in ancient times before distilling was known. The problems with trying to purify alcohol this way was that not only did the ethanol come out of the block of ice, but so did all the nasty higher and lower alcohols that cause painfull hangovers, and there is no way to separate them from the ethanol by freezing.

    The other reason you may have already seen: if you have ever put a bottle of vodka in the freezer (a traditional method of serving), you will notice that no matter how long it is in there, it never does anything but turn slightly thick, like syrup- no water freezes out once the alcohol gets up to 40%. Unless you have easy access to a source of liquid nitrogen, etc. so you can "super cool" the mash, then bring it's temp back up in a controlled enviroment so as to melt off various alcohols at various times, it's not worth bothering. Even then, it ain't worth it-the energy needed to keep the mash that cold would exceed the energy requirements needed to distill it.

    Home winemakers use this technique to make fortified wines without using distilled spirits- Put the mash in a plastic jug, leaving enough room for expansion, then put this in the freezer until it's a solid block of ice, then invert the container over a collection jar and gather everything that melts out until you have collected half of what is in the jug. With a 10% mash, this will come out to about 17% ABV.

AppleJack



Here's what I've found on making Applejack. Its from a 1957 book "Home-made wines" by Mary Aylett, you may find similar in other wine-making books at your local library.
  • Apple-jack.
      Make a good strong cider, as described in the recipe given, then put it in a sealed cask. Place the cask in some place where it can freeze through very slowly. In Canada this is doen by digging a large hole in the ground and covering the cask about three inches deep. When the thaw comes, the cask is at once dug up, and the contents will be found to have separated into apple water and to pure spirit. The spirit will be in the centre of the cask. The ice must be broken with great care, and the liquid spirit in the centre carefully run off. This is the apple-jack. It should nver be drunk undiluted.
  • Cider.
      Any apples will make good cider, but cider apples are best. If sweet apples are used a mixture of bitter apples or crabs is to be advised. Put the apples into a wooden tub, and smash them roughly with a wooden balk until they are a crude pulp. Cover the tub and leave for twenty four hours. Then put the pulp through a press or crush it in a strong hessian bag. As the juice runs, put it in a cask, and see that it is quite full. Keep the cask in a warm place and allow it to ferment spontaneously which as a rule it does very quickly. At a normal autumn temperature, the apples will ferment within 48 hours. Top up the cask with apple juice until the first violence of the ferment has subsided, then put the cask in a cool place to finish. Do not bung down hard until all sounds of fermenta tion has ceased. It will be ready to drink in three months, but will be better if left for six. It will improve if well racked. For sweet cider add sugar at the rate of a pound to a gallon, or more to taste. (Through the book, Mary is a firm believer in natural fermentation. I'd play on the side of caution, and direct the fermentation by adding a suitable yeast.)


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