Mead Fractional Freezing Distillation Advice Needed

[Tim Dinger]

Hello; I've brewed some mead, and have gotten it to around 10-12%. I tried to complete the process of freezing the water out of it, which would allow me to take that ice out and have a higher concentration of alchohol/flavour. However my issue is that instead of separating, the entire jug freezes solid, and I am unable to extract the water. Any advice is appreciated.

Edit: I am curious if once it starts to thaw, will the alcohol unfreeze before the water does? If so, could I just pour it off as it thaws and would that leave mostly ice behind, or just frozen mead?

 

[Brett_Bellmore]

The key, as I understand it, is to remove the ice while the contents are only partially frozen. Also, I think it needs to be frozen slowly. I think if it reaches a slushy state you can use a salad spinner on it...

I'm considering giving this a try, if I ever accumulate enough undrank mead. So far my friends and I seem to be drinking the stuff as fast as I can make it.

 

[bernardsmith]

This is not about how to remove water from alcoholic drinks (which may or may not be legal) but is simply to argue that if water thaws at 32 F and pure alcohol at -173 F, it really makes no difference whether you freeze a wine or mead slowly or quickly the ethanol will thaw before the water does although (and I don't know enough about the chemistry) some of the water and ethanol will have formed what is called (I think) an azeotrope and so their boiling point is somewhere between the BP of water and that of ethanol so their freezing point may also be somewhere between the freezing point of the two liquids too, which means that there is a limit to how alcoholic you can "jack" this mead by thawing the frozen solution.

 

[Brett_Bellmore]

For what it's worth, you're not going to get past 92.4% alcohol, at minus 123C. Which is, btw, colder than dry ice will get you.

Dry ice would, in theory, get you to about 80%. You might reach 25%, 50 proof, in your average home deep freeze.

Per some references I looked up, the key is actually dropping the temperature *really* slowly, so that very large ice crystals form, making it easier to separate the liquid.

What does the graph looks like when you include a significant amount of sugar? Haven't a clue, though the fact that sugar doesn't dissolve in alcohol suggests that it shouldn't have much influence.

Ah, correction, I failed to note that the above graph is in weight percentage, while brewers use volume percentage. The volume percentage numbers would be substantially higher, of course, since alcohol has a lower density than water.

 

[JP Smajda]

The alcohol will freeze last/ thaw first. What you are seeing here is an apple jack being made.Take the thawed liquid, put it back into a container and freeze and repeat until it won't freeze anymore. (PS this is an apple jack)

 

[cmac62]

JP is that all you will get out of those two 2 ltrs?

 

[JP Smajda]

The flash is a bit deceptive, but yeah, they are almost done. When it is a solid block of ice, I only let about 50% thaw. The rest is basically a flavored water.

 

[JP Smajda]

This is my work from today. This is a high gravity mead (16ish%) I have a chest freeze that apparently goes down to -20ºF. The bottles froze to a slightly firm slush. I let each 2 litter bottle thaw about 5 cups out, saved that stuff to rebottle and refreeze. I doubt its going to (refreeze) but I just want to make sure.
Then I let each bottle Thaw out another 6ish oz. I hate any waste and that last part was pretty tasty. Not sure what Im going to do with it, but it tastes great and its slightly stronger than a kombucha in alcohol. (2-3%?) Might be something to give a lightweight or something.
The last pic is the remaining ice.

 

[bernardsmith]

The one problem with fractional freezing that I see is that you keep the most volatile alcohols - the acetones, acetaldehydes and the methanol that distillation with a still enables you to remove. I am certain that the quantities are likely to be small (so I am going to ignore their potential toxicity) but those compounds can give you terrible headaches and what's perhaps worse, taste like crap.

 

[rex clingan]

Methanol in wine comes from the pectin, which is why is doesn't appear in beer. I know pollen and pectin start with the same letter, but I don't think methanol is a concern in mead or its freeze concentrates.

 

[bernardsmith]

and acetones? and acetaldehydes? and fusels? I am not talking toxins. I am talking taste but cysers would have lots of pectins and pyments lots of tannins

 

[McHop]

The one problem with fractional freezing that I see is that you keep the most volatile alcohols - the acetones, acetaldehydes and the methanol that distillation with a still enables you to remove. I am certain that the quantities are likely to be small (so I am going to ignore their potential toxicity) but those compounds can give you terrible headaches and what's perhaps worse, taste like crap.

When I made apple jack, I could feel the headache setting in as I was drinking it. If I were to try it again I'd run it through a Brita filter to strip some of the toxins out of it.

 

[Brett_Bellmore]

The one problem with fractional freezing that I see is that you keep the most volatile alcohols - the acetones, acetaldehydes and the methanol that distillation with a still enables you to remove. I am certain that the quantities are likely to be small (so I am going to ignore their potential toxicity) but those compounds can give you terrible headaches and what's perhaps worse, taste like crap.

While it's true that freezing doesn't remove these things, it doesn't add them, either. And it doesn't remove alcohol, either.

So the liter that would get you drunk and not give you a headache turns into 250ml, it still gets you drunk and doesn't give you a headache. Only in a smaller glass you sip at instead of gulping. At least that's my take on it: The amount you're drinking is probably normalized to a particular total amount of alcohol, and thus other constituents.

At least it is for me; I never drink past "happy" anyway.

 

[rex clingan]

and acetones? and acetaldehydes? and fusels? I am not talking toxins. I am talking taste but cysers would have lots of pectins and pyments lots of tannins

Well, Tim's question was about mead. Clearly, any fruit used will have pectin associated with it. I tend to add fruit after fermentation is complete, and expect the yeast activity on components of the fruit to be limited as compared with primary fermentation. I don't recall reading anything about what yeast do with tannin, interesting question.
As Brett noted, the congeners are concentrated with respect to water, and total volume, but not with respect to ethanol, or non-volatiles. Taste profile should be more concentrated, but similar to the starting mead.

 

[Brett_Bellmore]

I put fruit in most of my mead, both initially and on racking, and I've never noticed any particular problem with methanol or fusels.

A quick literature search says that methanol is a product of the action of pectic enzymes on pectin. That could be why I haven't noticed an issue; I hadn't been using it until recently, and my first batch trying it is still aging. I'll know in a few months whether I'm now getting noticeable methanol. If so I'll discontinue using it, since I don't really care if my mead is a little cloudy.

 

[bernardsmith]

I wonder what percentage of a mead (or wine) is likely to be methanol. By all accounts it would seem to be about 5% so if you make a gallon of mead you can assume that about 200 cc is methanol. If a glass of mead is about 150 cc and there are about 5 glasses/ bottle then there is about 8 cc of methanol in every glass (because 25 glasses/gallon) . No expert but given the fact that the treatment for methanol poisoning is ethanol and for every 8cc of methanol you are drinking you are also drinking - what? 17 cc of pure ethanol (assuming 12% ABV) I am not sure that there is a serious problem drinking wine or mead...

 

[Brett_Bellmore]

Well, there isn't a serious problem in terms of toxicity. As a practical matter it's more a question of taste and headaches, which becomes a problem long before you'd get sick from it.

 

[TGFV]

This is my work from today. This is a high gravity mead (16ish%) I have a chest freeze that apparently goes down to -20ºF. The bottles froze to a slightly firm slush. I let each 2 litter bottle thaw about 5 cups out, saved that stuff to rebottle and refreeze. I doubt its going to (refreeze) but I just want to make sure.
Then I let each bottle Thaw out another 6ish oz. I hate any waste and that last part was pretty tasty. Not sure what Im going to do with it, but it tastes great and its slightly stronger than a kombucha in alcohol. (2-3%?) Might be something to give a lightweight or something.
The last pic is the remaining ice.

View attachment 645570 View attachment 645571 View attachment 645572 View attachment 645573

Love the method for doing this!!

Whenever I have done a jack for cider it Mead I usually have it in a bucket in a deep freeze, and then open the lid every 2 hours once freezing starts to kick off (once it starts it's a chain reaction) and use a thin holes strainer to seive the ice out and shake the liquid out.

Usually can bring a jack to 15-20%. I could easily go higher, but the taste is great at this point as the flavours heavily concentrate.

 

[JP Smajda]

Love the method for doing this!!

Whenever I have done a jack for cider it Mead I usually have it in a bucket in a deep freeze, and then open the lid every 2 hours once freezing starts to kick off (once it starts it's a chain reaction) and use a thin holes strainer to seive the ice out and shake the liquid out.

Usually can bring a jack to 15-20%. I could easily go higher, but the taste is great at this point as the flavours heavily concentrate.

I've been surprised at how much this has been freezing. I've gotten those 8 two liter bottles down to about 3 and they are still freezing to a slushy state.
This stuff is DANGEROUSLY smooth.

 

[Bombo80]

JP, I use this freezing method to concentrate fresh cider, to collect the apple essence and sugars, while removing some of the water. That way I don't have to add any granulated sugar to my hard cider, which I then turn into brandy.

 

[cmac62]

Is there any issues with oxidation with jacking cider? I know there would be with beer because of the hops, but if there are no hops does it still oxidize the alcohol?

 

[Brett_Bellmore]

Is there any issues with oxidation with jacking cider? I know there would be with beer because of the hops, but if there are no hops does it still oxidize the alcohol?

Not very rapidly or easily. Oxidation seems to be much less of an issue with mead. Probably precisely because there aren't any hops.

 

[Miraculix]

I wonder what percentage of a mead (or wine) is likely to be methanol. By all accounts it would seem to be about 5% so if you make a gallon of mead you can assume that about 200 cc is methanol. If a glass of mead is about 150 cc and there are about 5 glasses/ bottle then there is about 8 cc of methanol in every glass (because 25 glasses/gallon) . No expert but given the fact that the treatment for methanol poisoning is ethanol and for every 8cc of methanol you are drinking you are also drinking - what? 17 cc of pure ethanol (assuming 12% ABV) I am not sure that there is a serious problem drinking wine or mead...

I'll doubt that any normal wine or mead has 5% methanol. That would be a big problem!!!

And just to explain the treatment of methanol poisoning with ethanol, it is actually not the methanol itself that is the big issue, it's the products from metabolizing it within the liver that are really toxic. So the trick is to keep the liver from metabolising methanol by keeping it busy with ethanol metabolism by ingesting ethanol regularly in significant amounts for a prolonged time period, until the methanol has completely left the system (I guess you pee it out slowly).

So you literal are kept drunk all the time until the methanol is gone without getting metabolised.

 

[Toxxyc]

I'm actually doing this at home right now (perfectly legal here). It's disappointing to see so much being lost, so I'm strongly considering a nice still to distill a bunch of mead, then blend back to 40% ABV using a dry mead for taste, and then backsweeten as needed to make a liqueur from it. Still in starting phase, but so far my 11% mead has frozen 3 times. Will see how far it goes.

 

[Miraculix]

I'm actually doing this at home right now (perfectly legal here). It's disappointing to see so much being lost, so I'm strongly considering a nice still to distill a bunch of mead, then blend back to 40% ABV using a dry mead for taste, and then backsweeten as needed to make a liqueur from it. Still in starting phase, but so far my 11% mead has frozen 3 times. Will see how far it goes.

I also wouldn't be able to throw away the leftovers.

Btw. How did your calcium chloride experiment turn out? Did it clear well?

 

[Toxxyc]

I also wouldn't be able to throw away the leftovers.

Btw. How did your calcium chloride experiment turn out? Did it clear well?

Still waiting on that. I added Zeolite to that batch to check how it's clearing, but from the quick checks, it's not clearing.

PS: I tossed the leftovers. I tasted it, but it just tasted like watered down mead, with little flavour and colour. Not very nice.

 

[Toxxyc]

OK so this batch is bottled and shipped off. Zeolite and water adjustments did zip to the clarity in the end with the same time as the previous batch. I'm not sure how it would compare to an unadjusted water profile with no fining, but that's my next batch's goal. This one was more cloudy and murky than the previous batch. Taste was spot on though.

 

[Toxxyc]

Wait wait the above post was on the wrong thread. My freeze distilled mead got damn strong, full of flavour and turned out great. It's less dry and less abrasive on the tongue than I expected. Probably came in at around 30% ABV. Not bad, but a waste. I'm going to push for a proper still.

 

[Miraculix]

Wait wait the above post was on the wrong thread. My freeze distilled mead got damn strong, full of flavour and turned out great. It's less dry and less abrasive on the tongue than I expected. Probably came in at around 30% ABV. Not bad, but a waste. I'm going to push for a proper still.

I thought so

 

[TGFV]

Wait wait the above post was on the wrong thread. My freeze distilled mead got damn strong, full of flavour and turned out great. It's less dry and less abrasive on the tongue than I expected. Probably came in at around 30% ABV. Not bad, but a waste. I'm going to push for a proper still.

You could always do the freeze distill as a stripping run, and then a proper run in a still for a final product?

 

[Desvio]

You could always do the freeze distill as a stripping run, and then a proper run in a still for a final product?

Thinking about the various freezing and boiling points of the range of alcohols, it almost seems plausible, but I think there is too much "good" product left behind through freeze distillation. If you have a still, think you get better chance of fractioning through heat distillation.

 

[bernardsmith]

e

Thinking about the various freezing and boiling points of the range of alcohols, it almost seems plausible, but I think there is too much "good" product left behind through freeze distillation. If you have a still, think you get better chance of fractioning through heat distillation.

Are you sure anything is "left behind" when you freeze the mead or wine? What you leave behind is ice and if your mead was say, 12% alcohol, almost all the 100 % of that 12% is in the liquid that did not freeze - assuming you can extract all the unfrozen liquid from the ice. Which is why if you begin with a gallon you are likely to get about a quart of liquid of which about 1 pint is ethanol (and other congeners). That said, I don't know that you can fraction anything using freezing since water presumably freezes long, long before ethanol (the latter at minus 173.5 while methanol freezes at minus 143.7 (and presumably both freeze at higher temperatures in the presence of water but still no where nearly as high as the coldest of freezers most folk will have access to)).

 

[Toxxyc]

You could always do the freeze distill as a stripping run, and then a proper run in a still for a final product?

Still too much waste, if you ask me. I would much rather do the stripping run in the still, actually, because you'll distill off the volatile compounds first, which is what you want.

IMO, freeze distilling is nice for playing once, or maybe doing it with cheaper spirits, but for mead it's just not worth it. I ended up using around 4.5l of mead to just get a quart (750ml) of the stronger stuff, and it wasn't even clear enough to look good.

 

[Brett_Bellmore]

IMO, freeze distilling is nice for playing once, or maybe doing it with cheaper spirits, but for mead it's just not worth it. I ended up using around 4.5l of mead to just get a quart (750ml) of the stronger stuff, and it wasn't even clear enough to look good.

I suppose it's a matter of taste: Freeze distilling and actual distilling aren't interchangeable. They produce radically different products. Freeze "distilling" removes water, and that's pretty much that. Actual distilling goes on to change the taste profile, rather than just concentrating it. And it's certainly not going to clarify anything, since it doesn't remove particles.

 

[Toxxyc]

Indeed. I found that the freeze distilling is more "forgiving" on flavour, but it does lose a lot of volume. I've discussed this with some other okes as well, and I think what would be great is a very cheap mead distillate (in other words, make a high-ABV mead, quickly but cleanly, but with cheaper honey or sugars to get the distillate out of it), and then to blend it with a good mead after distillation to get to your target ABV, like whisky makers do with water. That should drastically increase the "mead" flavour, but with a much higher yield. My idea is simple, but I don't have a still yet, so I can't try it:

1. Make a high-ABV mead, around the 16~18% ABV, using 50/50 honey and dextrose for cheap alcohol. You're doing to distill it, so the flavours aren't THAT important. Yes, some will come through, but most will be lost.
2. Distill slowly to get a clean distillate using a pot still for maximum flavour.
3. Test the ABV of the distillate and dilute it back to 40% ABV using a standard traditional, made with high-quality honey for maximum flavour. Keep in mind the traditional I'm making sits with full flavour at 11% ABV already.
4. Backsweeten slightly with raw honey. This should put a very nice sweet hit on the liqueur, making it a nice honey-ish drink, I think more closely resembling what people THINK mead should taste like.

And that's my idea. Just need to find a pot still, or someone with a pot still. I'm lucky that it's pretty legal in South Africa, it's just expensive to buy one

 

[bernardsmith]

Still too much waste, if you ask me. I would much rather do the stripping run in the still, actually, because you'll distill off the volatile compounds first, which is what you want.

IMO, freeze distilling is nice for playing once, or maybe doing it with cheaper spirits, but for mead it's just not worth it. I ended up using around 4.5l of mead to just get a quart (750ml) of the stronger stuff, and it wasn't even clear enough to look good.

I am not sure I see the problem. You got 750 ml of a spirit made from 4500 ml of mead - That's about 16.7% of the total volume and that would be 100% ethanol (AKA 200 proof) if the ABV of your mead was around 17%. I am guessing that you obtained about 80 proof from a mead that was around 12%. What do you think you would obtain if you used a pot still to distill for flavor? and if you were looking for vodka (no flavor) , why is it "worth it" to strip all the flavor and aroma from a honey mead to obtain 98% pure alcohol when you could achieve exactly the same result using table sugar at about 1/5 the cost.

 

[cmac62]

I suppose it's a matter of taste: Freeze distilling and actual distilling aren't interchangeable. They produce radically different products. Freeze "distilling" removes water, and that's pretty much that. Actual distilling goes on to change the taste profile, rather than just concentrating it. And it's certainly not going to clarify anything, since it doesn't remove particles.

I would say heat distilling absolutely does remove all particles because you are only collecting the alcohol as it cools in the worm. It wont have any color either. What you get is basically honey moonshine.

 

[Toxxyc]

I am not sure I see the problem. You got 750 ml of a spirit made from 4500 ml of mead - That's about 16.7% of the total volume and that would be 100% ethanol (AKA 200 proof) if the ABV of your mead was around 17%. I am guessing that you obtained about 80 proof from a mead that was around 12%. What do you think you would obtain if you used a pot still to distill for flavor? and if you were looking for vodka (no flavor) , why is it "worth it" to strip all the flavor and aroma from a honey mead to obtain 98% pure alcohol when you could achieve exactly the same result using table sugar at about 1/5 the cost.

Well, the mead I used was at 11% ABV (22 proof). 4,500ml of that mead contains 495ml of pure ethanol (I won't do stripping runs, as I ferment very clean). From the freeze distilling, I got 750ml of drink at around 25~30% ABV, if I'm to trust my taste. That is only 225ml of ethanol extracted if I work on the high end of that scale. It's more than half the ethanol lost.

Yes, I know in distilling you won't get 100% ethanol on the run. I'll get around 75% ABV instead, more if the still is treated well, but I don't want to lose THAT much flavour. 75% is a realistic run. That then gets cut back to the desired ABV with flavourful mixes - mead and honey. That's my point - freeze distilling makes a killing on the mead.

On the flavours - a pot still doesn't strip all the flavours. Vodka is usually distilled in a column or reflex still, stripping all the flavours. Something like Scotch whisky is distilled in a pot still, and it's obvious from peated whiskies that the flavours definitely isn't all lost.

 

[bernardsmith]

I would use a proof and tralle hydrometer rather than your taste to determine the proof or ABV of your freeze distillation. That it may or may not taste "hot" may have very little to do with the proof of your final product and whether anything was lost or you simply had all 11% ABV in your bottle just diluted with some H2O is the real question. (11% of 4500 is about 495 ml and you got you say 750 ml.) My bet is just about 100 percent of the alcohol was captured PLUS another 250 ml of water. So you loss hardly a drop, you just diluted the ethanol with water.

 

[Brett_Bellmore]

I would say heat distilling absolutely does remove all particles because you are only collecting the alcohol as it cools in the worm. It wont have any color either. What you get is basically honey moonshine.

Yeah, I could have worded that better. I meant freezing won't remove particles.