Freeze Distillation- Estimating Final ABV%

I just finished up some freeze distillation and was wondering if anyone had a good way to estimate the finished ABV of a freeze distilled drink.

I started with a hard limeade cooler I made that was 12% and then freeze concentrated it twice and ended up with around 1/4 the original volume.

The finished drink doesn't freeze in my freezer that is set around 0F which tells me its fairly high ABV and should tell me its minimum percentage but I don't know the formula to figure that out. Another estimate I was using was if I got 80% of the alcohol out it should be around 38% ABV. So any simple tests anyone knows of to test a solutions ABV? Its supposed to get to about -25c (-13F) in the next few days so I might use those temperatures as another freeze test.

EDIT: some basic google research is telling me that it's approximately 35% to not freeze at 0F.

Are you sure your on the right site?

If you want to know the alcohol content specifically you need a hydrometer that reads below 1.000. Fairly common in chemistry labs.

Sorry Veinman, but that is not something that we discuss here.

EDIT** I am wrong and have learned something myself. Carry on.

Technically it wouldn't be considered "distillation" so much as "concentration", and contrary to a popular believe IS legal. This is the same process used to make an eisbier, so i think this thread's presence here could be useful given the appropriate info and if it can be applied to the creation of eisbier.

Nothing wrong with what he is doing (the mods won't lock). It is, in fact, one of the BJCP recognized beer styles (eisbock - 5D). It's been discussed ad nauseum on this site.

My attempt at it in pic below. More info at Basic Brewing audio podcast.

Thanks for the correction cactusgarrett and passedpawn. I stand corrected and have have edited my previous post to reflect the same.

Just an added note to the OP and any others interested:

The problems with trying to purify alcohol this way was that not only does the ethanol come out of the ice, but so does 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 method, however, is to put the beer/wine 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. (as shown in passedpawn's post above) Starting with a 10% beverage, this will come out to about 17% ABV.
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.
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.
Temperature (F/C).......% Alc.
............10 / -12.2.........8
.............5 / -15.0.........11
.............0 / -17.8.........14
...........10 / -12.2..........8
...........-5 / -20.6.........17
.........-10 / -23.3..........20
.........-15 / -26.1..........24
.........-20 / -28.9..........27
.........-25 / -31.7..........30
.........-30 / -34.4..........33

To be at 35%, you would to have had to have a very cold freezer. So, getting a hydrometer would be the best solution to answering your question with any surety.

No worries - that's why we're all here. I'm glad you're open to adjusting your beliefs - what frustrates me is the huge amount of info that's passed down here by means of at *least* second hand information, and some people aren't open to the possibility that something they've been doing or told isn't optimum (or wrong).


garrett

Well I'll be darned - learned something. Carry on...

(Previous post deleted )

I'm relatively new here. I also am learning a bunch of new knowledge regarding the entire "distillation" conversation. There is a rather interesting and heated conversation going on in the Cider Forum regarding this topic even as we speak. Wow, apparently there is a lot of misinformation out there even though as you say, this has been discussed here "ad nauseum".

cactusgarrett said:

No worries - that's why we're all here. I'm glad you're open to adjusting your beliefs - what frustrates me is the huge amount of info that's passed down here by means of at *least* second hand information, and some people aren't open to the possibility that something they've been doing or told isn't optimum (or wrong).


garrett

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That seems to be more of an issue with the newer folk that wander in. I have been here long enough to know that I don't know crap compared to many others here and am always open to correction.
Of course, being wrong is something that very rarely happens with me.

If you removed only water and all the alcohol was left behind (not likely) the equation would be very simple:

12%ABV original/0.25 = 48%ABV final

The 0.25 in the equation is the factor of difference in volume from start (you said it was approximately 1/4 the volume you started with).

OK, easy answer is find a Proof & Traille like this one. Basically a hydrometer with a substantially lower range.

I do not think a hydro would be very accurate. The problem is that you are concentrating the entire liquid not just the booze. You are getting the sugars as well.

I have also noticed that said sugars tend to "clump" in a freeze concentrated drink (looks like sand) and they will fall out. I also think it depends on where the drink started at as to where you end up. If you concentrate a bunch of 4% beer vs. 12% the final product will be effected. The reason I say this is because the solution gets more difficult to concentrate after the 1st round, It will be more like a slushy vs. an ice block. Unless you have a freeze paddle or other high end custom built contraption and if so I demand pics!

This can be done to wine as well. When done to Apfelwein it is commonly called apple jack, because it is like apple whiskey.

I have done this to a Merlot as well. It makes the best Gluwein EVER! I can heat up some water, spices and fruit then add the "ice wine" in to each glass and it is nice and strong and hot.

If you try freeze concentrating repeatedly you will increase the alcohol content with each pass up to a limit. Eventually you start locking ethanol in the ice crystals (ethanol attaches to water molecules -- that is why liquor is never 100% alcohol) and you stop going any lower.

It is possible with two passes you got in the upper teens, maybe the lower 20s but as others said, a hydrometer will be the only way to know for sure.

Thanks for all the help guys. I realized reading the responses that "freeze distillation" was the wrong term for a number of reasons especially since "distillation" is a no-no and that "freeze concentration" is much more appropriate and correct. Thanks for corrections. I particularly appreciate the knowledgable members correcting the mis-information about why this is legal and not a forum issue etc. I did get the idea from other threads after all.

Also I should say this wasn't neccesarily about making super strength hooch but another pushing the envelope and trying new things idea that we all love about homebrewing.

Thanks to bull for the chart showing the freezing temperature to ABV ratio I couldn't find anything like this. I know that an alcoholic beverage will not freeze at 0C, my freezer is 0F or about -17C so your chart says that it's at least 14%.

I did a hydrometer reading and the liquid is reading .90. BrewSmith tells me that an OG of 1.100 (which it was) to 0.90 is an ABV of 26.27%. Is there any reason to assume the freeze concentration messed with the standard OG:FG calculations?

I just put a small glass of it out on my back porch where its currently -26C so if its liquid in a few hours I'll know its at least 24% by bulls chart.

Veinman said:

I did a hydrometer reading and the liquid is reading .90. BrewSmith tells me that an OG of 1.100 (which it was) to 0.90 is an ABV of 26.27%. Is there any reason to assume the freeze concentration messed with the standard OG:FG calculations?

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For the reasons that Zamial listed, a hydrometer won't give you an accurate reading. The sugar has concentrated too, and will throw off the reading. You also can't do an og-fg x 131 calculation since the volume has changed and the proportion of water is now different.

The equation I posted above should give you an approximate value for ABV%. It won't be 100% since you have of course removed a little alcohol with the ice but it should be close.

(12% ABV starting) / 0.25 = 48%ABV Final

Let's say you started with 1 liter. I know you probably did more but bear with me. The 1 liter starts off as 12% ethanol. Thus, there is 120 mL of ethanol in your solution. You removed 75% of the volume, which should have been mostly water. You now have 250 mL of solution, and if all the ethanol is still there, 120 mL of the 250 mL is alcohol. Therefore, 120 mL / 250 mL = 0.48 or 48%. Your final solution is 48% Alcohol By Volume.

KingBrianI said:

For the reasons that Zamial listed, a hydrometer won't give you an accurate reading. The sugar has concentrated too, and will throw off the reading. You also can't do an og-fg x 131 calculation since the volume has changed and the proportion of water is now different.

The equation I posted above should give you an approximate value for ABV%. It won't be 100% since you have of course removed a little alcohol with the ice but it should be close.

(12% ABV starting) / 0.25 = 48%ABV Final

Let's say you started with 1 liter. I know you probably did more but bear with me. The 1 liter starts off as 12% ethanol. Thus, there is 120 mL of ethanol in your solution. You removed 75% of the volume, which should have been mostly water. You now have 250 mL of solution, and if all the ethanol is still there, 120 mL of the 250 mL is alcohol. Therefore, 120 mL / 250 mL = 0.48 or 48%. Your final solution is 48% Alcohol By Volume.

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I am not so sure that there is a really good way to figure this out without having a way to actually test the resulting solution. Your equation is correct, but doesn't account for any alcohol trapped in the ice structure itself.
As an extreme/unlikely example, if I froze the beverage quickly and I was only able to get 100 mL out of a 1 L original volume, then obviously the result of the formula would be grossly incorrect. Unless you could extract nearly 100% of the liquid that didn't freeze, which would require a centrifuge-like action, then there is just no accurate way to calculate it. And I think this is primarily due to entrapment in the ice.
I am sure this is as clear as mud.

bull8042 said:

I am not so sure that there is a really good way to figure this out without having a way to actually test the resulting solution. Your equation is correct, but doesn't account for any alcohol trapped in the ice structure itself.
As an extreme/unlikely example, if I froze the beverage quickly and I was only able to get 100 mL out of a 1 L original volume, then obviously the result of the formula would be grossly incorrect. Unless you could extract nearly 100% of the liquid that didn't freeze, which would require a centrifuge-like action, then there is just no accurate way to calculate it. And I think this is primarily due to entrapment in the ice.
I am sure this is as clear as mud.

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I agree with this. It's easy to see that if you go from 4L to 1L and extract 100% of the alcohol the new drink is 4x as strong however in reality there is no way I extracted 100%, the leftover watery mixture still had a little alcohol in it when I tasted it. Determining the exact "extraction efficiency" is the tricky question and impossible to do with 100% certainty. I'm thinking something like a 70-80% number would be about right.
at 70% it seems the final liquid would be:
12*2*.7 = 16.8
16.8 * 2 * .7 = 23.52%

12*2*.8= 19.2
19.2*2*.8= 30.72%

I left an ounce out on the back deck in a shot glass and after a few hours it's not frozen at all and shows no signs of freezing at -24C so from bull's chart I can say it's at least 20%. I'm going to call it an even 25% until I come up with a better way to measure it.

bull do you happen to know what these hydrometers look like or how they work, the website mentions it measures proof but doesn't show a picture or any instructions, is it as simple as dropping it in the liquid and it has a scale? Probably gonna pick one up for 6 bucks if its that simple.

Veinman said:

...........

bull do you happen to know what these hydrometers look like or how they work, the website mentions it measures proof but doesn't show a picture or any instructions, is it as simple as dropping it in the liquid and it has a scale? Probably gonna pick one up for 6 bucks if its that simple.

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Well you obviously understand the point I was trying to make, even with my mediocre explanation. I think your estimates should be pretty close.
As for the proof & traille, I have never seen one that I know of. I would suggest sending Yooper a PM and asking her. She also does a lot of wine and more than likely knows how they work.
I can guess and speculate, but that won't do you much good.

My understanding is that in order for any hydrometer (alcoholometer) to work, you have to do pre- and post fermentation measurements and subtract. That won't work with concentration- as was explained earlier. A hydrometer measures suspended sugars, and doesn't really measure the alcohol. Certain assumptions are made to guess at the ABV%, but the hydrometer itself doesn't measure the ABV.

KingBrianI said:

For the reasons that Zamial listed, a hydrometer won't give you an accurate reading. The sugar has concentrated too, and will throw off the reading. You also can't do an og-fg x 131 calculation since the volume has changed and the proportion of water is now different.

The equation I posted above should give you an approximate value for ABV%. It won't be 100% since you have of course removed a little alcohol with the ice but it should be close.

(12% ABV starting) / 0.25 = 48%ABV Final

Let's say you started with 1 liter. I know you probably did more but bear with me. The 1 liter starts off as 12% ethanol. Thus, there is 120 mL of ethanol in your solution. You removed 75% of the volume, which should have been mostly water. You now have 250 mL of solution, and if all the ethanol is still there, 120 mL of the 250 mL is alcohol. Therefore, 120 mL / 250 mL = 0.48 or 48%. Your final solution is 48% Alcohol By Volume.

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48%? Not even close mate,& here's the reasons why:
The liquid extracted contains disolved water. Alcohol & water form weird mixtures & although you can concentrate them by freeze seperation, the concentration obtainable is dependant entirely on final freeze temp ( a table is there in earlier post) work on neg 25-27C to get 30% product. More than that would require specialist freezing techniques, I don't think home freezers are capable.
If you introduced 40% alcohol into the neck of your bottle at neg25C all that would happen is it will act as an antifreeze & dilute until freezing slush ( 30%ish) occurs.

The best way to do freeze concentration, is to use carbonated ( beer) brewed to a good start alcohol % freeze solid, invert & then put in a fridge to get a partial melt ( encorages pure ice at the top & concentrate at the neck) then refreeze as cold as you can go. Opening the cap carefully ( gas pressure present) will force out the good stuff. Gas is your friend here so carefully release in 3 or 4 stages. What's left in the bottle should look like pretty drained ice with little worth left in it.

Here's a good article with information on temperature vs. alcohol concentration obtained:
http://www.popsci.com/science/article/2013-01/beersci-how-make-strong-beer-stronger

cactusgarrett said:

Technically it wouldn't be considered "distillation" so much as "concentration", and contrary to a popular believe IS legal. This is the same process used to make an eisbier, so i think this thread's presence here could be useful given the appropriate info and if it can be applied to the creation of eisbier.

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Sorry to necro this thread, but when somebody googles freeze distillation, this thread comes up... and this legit offers dangerous advice.

1) Fractional freezing is scientifically considered concentration.
2) Scientific definitions have no weight in regards to legal definitions. That's why Cyanide is an organic compound, but veggies sprayed with cyanide can't be labelled and sold as organic.
3) An Eisbier produced outside of the US can be imported as "beer", and be sold anywhere beer of that alcohol content can be legally sold.
4) Commercial Eisbiers brewed INSIDE the united states require one of two things. A- the beer must have all removed water replaced, so as to not artificially increase alcohol. This concentrates alcohol while lightening body. B- A distillation license. This is PRECISELY why you only see imported eisbiers, the occasional American beer such as NATTY ICE (Look it up, they add the water back and use ICE for marketing)... and why you do not see ANY craft eisbocks. Higher alcohol beer is RIGHT up the American consumer's alley. If it were legal for breweries to do, it would be done with some level of frequency. Especially considering that a 30% fractionally frozen cider could compete with apple liqueurs.

Sorry, but your information is wrong. Fractional freezing is legally considered distillation, even though it isn't considered distillation scientifically.

I am not claiming to be 100% correct, but I am certain that I am correct when I refer to what is considered distillation on the commercial scale.

On the home brewing scale you, may be confusing the Federal Government's complete unwillingness to prosecute people who fractionally freeze or distill for personal use with legality. Just cuz they don't or can't do anything about it doesn't mean its legal. Advising that it is legal is simply NOT a good idea.

Fractional Freezing or Freeze Distillation, to my knowledge, has not been legal anywhere in the US since before prohibition.

marcownz747, I have that same picture on my FB profile

In US to the best of my knowledge distillation is illegal. This includes Freeze Distillation.

There are many ways to distill, you can setup an aquarium air-pump with a diffuser stone, an aquarium air bubblier. The bubbles will evaporate alcohol, just collect it as a condensate.

The problem is that, the only more or less safe way is normal distillation using heat. When a heat distillation runs you discard first few shots, and only collect at certain temperature range after which you would run it through charcoal for chemical filtration.

See the distillation laws we have in US are here for a reason. Without them many Darwin Award winners would die form acute pancreatitis from alcohol poisoning.

In freeze distillation you are not only concentrating alcohol, but also harmful impurities that can poison you.

Exactly.

Also, to my knowledge, the TTB defines distillation as the separation of Ethyl Alcohol from a solution. They do not care if it is a biproduct (IE, if alcohol is distilled by mistake while distilling essential oils via solvent method), or if the alcohol is pure or comes with a bunch of other chemicals. They only care that you're removing alcohol from a solution. Because you're being left with higher concentrations of ethanol in your solution solution when you freeze the water and separate ice from booze, the TTB still sees you as distilling, even though you're technically concentrating.

So Fractional Freezing, while SCIENTIFICALLY being concentration and not distillation... is LEGALLY distillation.

There's a lot of places where rules like this are the case. Pumpkins, peppers, and eggplant are botanically fruit (ripened ovaries of a plant. Technically, they're berries as well). Yet due to their nutritional content and the ways we tend to eat them, the government classifies them as vegetables for the purpose of deciding whether a school is creating school meals with enough veggies.

I am making apple brandy, which usually requires 2 distillations - 1st (the fast stripping run) to increase the alcohol content to the 30-40 abv range, and the 2nd (the slow spirit run) to extract the final product at cask strength(around 60-65 abv).

Instead, I have freeze concentrated 25 gallons of cider down to roughly 5 gallons of product that is around 30%. I'll then run this on one slow spirit run.

The advantage of this approach is that with freeze concentration, the flavors are also concentrated, which carry over into the distillate. The more distillations you do, the less flavors that are carried over.

With freeze concentration, unwanted chemicals like methanol and acetone are also concentrated. But because these have different boiling temperatures, I can collect the distillate into a bunch of small jars, and discard the early ones that I can detect through smell and taste contain too much of these poisons.

Veinman said:

I just finished up some freeze distillation and was wondering if anyone had a good way to estimate the finished ABV of a freeze distilled drink.

I started with a hard limeade cooler I made that was 12% and then freeze concentrated it twice and ended up with around 1/4 the original volume.

The finished drink doesn't freeze in my freezer that is set around 0F which tells me its fairly high ABV and should tell me its minimum percentage but I don't know the formula to figure that out. Another estimate I was using was if I got 80% of the alcohol out it should be around 38% ABV. So any simple tests anyone knows of to test a solutions ABV? Its supposed to get to about -25c (-13F) in the next few days so I might use those temperatures as another freeze test.

EDIT: some basic google research is telling me that it's approximately 35% to not freeze at 0F.

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To answer the OP, yes I tend to use the final volume as a rough guide based on my knowledge of the alcohol percentage of the product going in.

There is going to be some wastage because some of your product will stay in the ice, but I've noticed that it isn't a lot (less than 5 %).

You could use a proof and tralle hydrometer, but because any residual sugars will also be concentrated (you can make maple syrup by freeze concentrating the sap) it will throw off the readings.