Purifying commercial wine spirit

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JJF63
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Purifying commercial wine spirit

Post by JJF63 »

This is my first post (besides the introduction).

I searched about the following issue but could not find a satisfactory discussion/explanation.

So, I have access to some commercial wine spirit 95 or 96%. This saves me the hassle of brewing, stripping and rectifying.
But, despite it reads 95%, the fact is this spirit is still full of heads and tails.
I made 2 batches of absinthe + 1 small one of gin. The amount of heads and tails were quite significant despite there was no additional fermentation (only maceration in 85% spirit), although I have not really a way to compare with the outcome of a more traditional rectifying process.
My objectives are doing just absinthe, liquers and other herb based distilled concotions. So, a fairly neutral starting basis is fine (although the light scent and taste of wine spirit is preferable to the rum spirit I rectified before).

Now, how do I get rid of these heads and/or tails without wasting too much of the raw spirit ? (In some cases I want to keep some tails, to become a repository of oils/essences and reuse them in subsequent batches, as is the norm with absinthe).

I don't have (yet) my variable condenser rectifying column ready (I still have to get the fillings, I thought about those wire spirals, forgot the name), because when I found the wine spirit source I forgot about making my own base spirit.
All my setups are in glass (I did before some hobby chemistry, and thought on following the same path), it's clean, nice to observe the process, and I don't need large quantities. My largest flask is 5 liters, which is plenty to make 1 batch of 1,5L 72% absinthe.
Besides the pot-still configuration, I can do also a rectification using a Vigreux column (or rather a Snyder one, those with several glass "ballons" at each stage. https://assets.fishersci.com/TFS-Assets ... PG-650.jpg). Mine has 8 stages. It's far from the efficiency of a good condenser reflux column with fillings but much better than simple pot still.

Returning to my question I see 2 options:
1- Distilling right from undiluted 95% spirit. Safety is not an issue. I have done before much more hazardous distillations (diethyl ether, etc). I don't have ignition points, no flame at all, the setup is quite contained. And the most important: never leave things unattended as long the process is not stabilised.
2- Distilling from diluted spirit. I don't mind getting back just 85% spirit, it's quite enough as a starting base. But not below that. Is there any real advantage with this 2nd option, regarding quality of product output and ease of process ?
What should be my dilution limit ? I probably have to make some tests, to know more precisely about my column rectification capacity ?

Waiting for some advice...
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Salt Must Flow
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Re: Purifying commercial wine spirit

Post by Salt Must Flow »

You would want a good reflux column. Dilute the high % alcohol well below 40% ABV in your boiler. I often dilute down to 15% ABV with water. Diluting a lot with water really aids in cleaning it up. Do a spirit run slow and a good reflux rig should give you very clean product at 97% ABV. Collect product in many glass jars, let it air out for a day or so then make your cuts. I think the tails cut is very easy because tails smells & tastes horrible. Decide where to make the cut for the heads, keep the hearts and dilute the hearts to whatever proof or % ABV you like. I like to toss the heads and the not too nasty tails into a container to do an all feints run when I have collected enough to do so.

You asked what the dilution limit is. There really isn't one. They say to dilute at least to 40% ABV because it's more dangerous at higher % in your boiler. I used to be concerned with 'over diluting' because I feared I would be leaving alcohol in the boiler the more I diluted. This is NOT the case at all. If you let the boiler cool down and test it, you'll find that what's left is less than 1% ABV. You're going to recover all of your alcohol and diluting more helps trap the nasties in your boiler.

You say you have access to commercial wine spirit. Do you have to pay for it? Hopefully not much if you do. I mostly do sugar washes which consists of just sugar, DAP, boiled yeast, pinch of Epsom salt and B vitamin for nutrients. I add a little citric acid and crushed oyster shell to buffer the ph. This makes even 45 gal fementations pretty inexpensive.
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Re: Purifying commercial wine spirit

Post by still_stirrin »

JJF63 wrote: Sat May 14, 2022 2:47 pm… Now, how do I get rid of these heads and/or tails without wasting too much of the raw spirit ?
You won’t. You’ve got to make good cuts if you don’t want “scraps” in your macerated spirit. “Garbage in —> garbage out”.
JJF63 wrote: Sat May 14, 2022 2:47 pm… Returning to my question I see 2 options:
1- Distilling right from undiluted 95% spirit. Safety is not an issue. I have done before much more hazardous distillations (diethyl ether, etc). I don't have ignition points, no flame at all, the setup is quite contained. And the most important: never leave things unattended as long the process is not stabilised. <— Not a safe proposal!

2- Distilling from diluted spirit. I don't mind getting back just 85% spirit, it's quite enough as a starting base. But not below that. Is there any real advantage with this 2nd option, regarding quality of product output and ease of process ? <— Also, not a safe proposal.

Waiting for some advice...
Clean up your base spirit before you macerate with botanicals. And then, I wouldn’t use a spirit more than 45 to 50%ABV for macerating in. Otherwise, you’ll extract a lot of really bad flavors from the botanicals.

A wine-base neutral can be nice to start. But don’t get “greedy” when you make your cuts (for the base spirit).
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NZChris
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Re: Purifying commercial wine spirit

Post by NZChris »

I would dilute it to 40%, put it through a pot still and choose a cut suitable for Absinthe. You should easily get a cut at around 80%, which is more than enough for steeping the botanicals.
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Re: Purifying commercial wine spirit

Post by JJF63 »

Salt Must Flow wrote: Sat May 14, 2022 3:19 pm You would want a good reflux column. Dilute the high % alcohol well below 40% ABV in your boiler. I often dilute down to 15% ABV with water. Diluting a lot with water really aids in cleaning it up. Do a spirit run slow and a good reflux rig should give you very clean product at 97% ABV.
As I said, I am limited because I don't have a very good rectification column. Although from what I read in the alcohol vapor chart, from 40% ABV I can get around 77% ABV with simple pot-still distillation (but this applies just to the start of distillation, average for all process will be lower. So, with this Snyder column, maybe I can get 85% ABV in the end, starting with 35 or 40% ABV. But not from lower ABV.
Salt Must Flow wrote: Sat May 14, 2022 3:19 pm and diluting more helps trap the nasties in your boiler.
That's what I suspected. Thanks.
But I don't know how to overcome the rectification column limitation, with the model I have now.
Salt Must Flow wrote: Sat May 14, 2022 3:19 pm You say you have access to commercial wine spirit. Do you have to pay for it? Hopefully not much if you do. I mostly do sugar washes which consists of just sugar, DAP, boiled yeast, pinch of Epsom salt and B vitamin for nutrients. I add a little citric acid and crushed oyster shell to buffer the ph. This makes even 45 gal fementations pretty inexpensive.
I pay not much. Maybe I would spend a little less doing sugar washes, but sparing me all the hassle and the extra equipment is quite advantageous.
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Re: Purifying commercial wine spirit

Post by JJF63 »

still_stirrin wrote: Sat May 14, 2022 3:32 pm
JJF63 wrote: Sat May 14, 2022 2:47 pm 2- Distilling from diluted spirit. I don't mind getting back just 85% spirit, it's quite enough as a starting base. But not below that. Is there any real advantage with this 2nd option, regarding quality of product output and ease of process ? <— Also, not a safe proposal.
I could not understand why this 2nd option is also unsafe. In order to get an output of 85% ABV, I have maybe to start from 40% ABV diluted base spirit (with the help of my Snyder column).
still_stirrin wrote: Sat May 14, 2022 3:32 pm Clean up your base spirit before you macerate with botanicals.
Yes, that's my idea. Except for absinthe (and probably other liqueur and distilled herbal drinks) some tails are required, because a good part of heavier oils and essences only pass with higher temperatures, and those aromatic oils are necessary to add strength and aroma in subsequent batches. Some experimentation may be required.
still_stirrin wrote: Sat May 14, 2022 3:32 pm And then, I wouldn’t use a spirit more than 45 to 50%ABV for macerating in. Otherwise, you’ll extract a lot of really bad flavors from the botanicals.
All old recipe books I saw (Duplais, Brevan, Bonot-Petit, Fritsch) require maceration with 80 or 85% ABV spirit. Distillation is then carried on after dilution to 40%ABV (with the herbs in).
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Re: Purifying commercial wine spirit

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NZChris wrote: Sat May 14, 2022 3:48 pm I would dilute it to 40%, put it through a pot still and choose a cut suitable for Absinthe. You should easily get a cut at around 80%, which is more than enough for steeping the botanicals.
Yes. For absinthe I need too some of the tails, because they get to concentrate the heavier oils and essences, which add strength and aroma in subsequent batches. These tails are cut during the distillation with the herbs, and kept apart to add to next batch maceration volume.
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Salt Must Flow
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Re: Purifying commercial wine spirit

Post by Salt Must Flow »

NZChris is probably right. A single distillation should give you the heads and tails cut you are looking for considering that the product you're working with is already pretty high % ABV. I just have it stuck in my head to get it as pure as I possibly can. That was my misunderstanding.

JJF63 like you said, if your still can get approximately 85% ABV of total collected product then it would also be much cleaner than what you started out with only more water. Maybe try it both ways. Start with a simple pot still distillation and compare it with doing a run using your rectification column and see if the extra time it takes is worth the results it provides. Anything you do will make it better than it already is.
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jonnys_spirit
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Re: Purifying commercial wine spirit

Post by jonnys_spirit »

Redistill your brandy to fraction it out. Collect in 20-30 jars and select your heart cut. When you re-distill it into fractions proof your boiler charge down to 40%abv or less like others have recommended.

With your new hearts cut test it white and proofed to -40%abv. Ince happy with your brandt hearts go from there.

The brandy you purchased sounds luke it wasn’t cut so maybe that’s why it’s inexpensive?

Cheers!
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Re: Purifying commercial wine spirit

Post by JJF63 »

Thanks for the advices.
I shall do as you say, try 2 short runs starting with 40%ABV (after dilution of original 95%ABV product), both ways, and compare quality and quantities of cuts obtained.
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Re: Purifying commercial wine spirit

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Yes, that sounds the way, thanks.
jonnys_spirit wrote: Sat May 14, 2022 6:18 pm Collect in 20-30 jars and select your heart cut.
That looks quite a lot of jars...
What I have done before, for a trial with shop bought rum, and for the absinthe and gin runs, I used about 5 or 6 small jars. First for the heads cut: I collect around 30-40ml (from a distilling batch of 2.5-3L of 40-50% ABV product) fractions in those small jars, then taste them (after diluting to 40%), and decide where my hearts start. Then let it run for a while, and repeat the process to decide where I cut for the tails.
Salt Must Flow recommended to let the fractions air for a day before tasting and deciding where to cut. Is that a must, or I can rely on tasting on spot ?
jonnys_spirit wrote: Sat May 14, 2022 6:18 pm The brandy you purchased sounds luke it wasn’t cut so maybe that’s why it’s inexpensive?
It surely isn't cut, despite it is used for specialty wine treatment (enriching ABV).
I wonder if the treated wines wouldn't get much better if the alcohol was first cut. But maybe the heads and tails play a part in the bouquet formation, with the subsequent aging process...
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Re: Purifying commercial wine spirit

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The VOCs that you don't like in the heads are easy to get rid of. You don't even need to re-distil the whole batch, just run until the nail varnish is gone, then shut the still down.

Tails are more difficult to remove. Don't confuse tails from an Absinthe run with the tails from cleaning up a spirit ready for making Absinthe. If you want to recycle the tails from an Absinthe run, you must remove most of the fusels from the base spirit before steeping the botanicals. Any still can do this, some are more efficient than others, but the heart cut is selected by you and your senses, not by the still or it's thermometers etc..

I've done several very nice Absinthe runs using grape based spirit and don't believe internet advice that you need a very neutral base spirit.
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Re: Purifying commercial wine spirit

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Thanks for the explanation. Some questions:
NZChris wrote: Sat May 14, 2022 10:35 pm The VOCs that you don't like in the heads are easy to get rid of. You don't even need to re-distil the whole batch, just run until the nail varnish is gone, then shut the still down.
Yes, that was my initial idea. But then, all tails (fusels, etc) will remain in my base spirit for steeping the botanicals.
NZChris wrote: Sat May 14, 2022 10:35 pmTails are more difficult to remove. Don't confuse tails from an Absinthe run with the tails from cleaning up a spirit ready for making Absinthe. If you want to recycle the tails from an Absinthe run, you must remove most of the fusels from the base spirit before steeping the botanicals.
I don't want to question your knowledge, you certainly have much more experience than me. But if the purpose of tails from an Absinthe run is just to impart more flavour (and louche, etc) in subsequent batches, and somehow I have to make a cut (for tails), based on taste, what is the problem of having there fusels and other non-wanted substances (from the original base spirit) ? They will always remain in the tails part and not pass into my hearts part, isn't so ?
Or those fusels may nevertheless impart some bad characteristics to the good cut ?

Also, does it makes sense to save tails from other herb based distilled products, for reuse in next batches ? From Gin, etc ?
NZChris wrote: Sat May 14, 2022 10:35 pmAny still can do this, some are more efficient than others, but the heart cut is selected by you and your senses, not by the still or it's thermometers etc..
Yes, sure, I have seen a lot of videos and posts explaining that. My previous question was: is it necessary to let the cuts rest and air some time before tasting and deciding where to cut ? How long ?
NZChris wrote: Sat May 14, 2022 10:35 pmI've done several very nice Absinthe runs using grape based spirit and don't believe internet advice that you need a very neutral base spirit.
Probably not. But for heads, it's a waste to get rid of first cuts when they carry a lot of good initial aromas from your herbs.

BTW, any suggestions about making similar herb based drinks ?
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Re: Purifying commercial wine spirit

Post by jonnys_spirit »

5960D5FF-1615-4868-BCB2-04297CEBC751.jpeg
JJF63 wrote: Sat May 14, 2022 6:45 pm Yes, that sounds the way, thanks.
jonnys_spirit wrote: Sat May 14, 2022 6:18 pm Collect in 20-30 jars and select your heart cut.
That looks quite a lot of jars...
I did a spirit run yesterday from low wines & feints. Collected into 22jars. This is my hearts cut with preliminary transition heads/tails top/bottom. Prolly average 160proof from the pot still but I haven’t measured anything yet. Figure i’ll take approx 1.5 -1.7 gallons barrel cut around 120proof on this just under 2g @ -160pf. I’m going to keep a middle white-cut jar then finish blending the barrel cut with what’s left. The rest into feints for next run and i’ve still got late tails and rum oils for the feints carboy. I did a three jar fores/early heads cut for the fores jug.

This is pot still not reflux.

20’Ish jars is a good number but you can do less too if you like.
I usually take five cuts - fores, feints, barrel, white, weed-killer - so i appreciate the resolution and every once in a while on the fly?

Cheers!
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Re: Purifying commercial wine spirit

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jonnys_spirit wrote: Sun May 15, 2022 8:21 am The rest into feints for next run and i’ve still got late tails and rum oils for the feints carboy.
So, you keep your feints (tails) of every batch and add them to next one. I suppose this increases your product taste progressively.
One question: at some point you haven't to get rid of some of the feints ? Its volume might keep increasing, I suppose.
jonnys_spirit wrote: Sun May 15, 2022 8:21 am I usually take five cuts - fores, feints, barrel, white, weed-killer - so i appreciate the resolution and every once in a while on the fly?
Looks great ! What are those 3 categories: barrel, white, weed-killer ?

I'm in the middle of my first test (pot-still). 1.500ml 96.4% base spirit, diluted to 50% (I did not opt for the 40% because I really wanted a final spirit with at least 80%).
Used 9 small flasks for collecting the heads, 10-12 ml each. First 3 were tasted and discarded immediately. Next 4 I'm waiting for tomorrow to decide. Last 2 are OK. Now shall start doing the same for feints. Maybe after collecting 700-800 ml. But with larger fractions, maybe of 30-40ml each.
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Re: Purifying commercial wine spirit

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JJF63 wrote: Sun May 15, 2022 5:45 am
NZChris wrote: Sat May 14, 2022 10:35 pmTails are more difficult to remove. Don't confuse tails from an Absinthe run with the tails from cleaning up a spirit ready for making Absinthe. If you want to recycle the tails from an Absinthe run, you must remove most of the fusels from the base spirit before steeping the botanicals.
I don't want to question your knowledge, you certainly have much more experience than me. But if the purpose of tails from an Absinthe run is just to impart more flavour (and louche, etc) in subsequent batches, and somehow I have to make a cut (for tails), based on taste, what is the problem of having there fusels and other non-wanted substances (from the original base spirit) ? They will always remain in the tails part and not pass into my hearts part, isn't so ?
Or those fusels may nevertheless impart some bad characteristics to the good cut ?

Also, does it makes sense to save tails from other herb based distilled products, for reuse in next batches ? From Gin, etc ?
Fusel oils taste bad to me, that is why I remove them the the spirit I'm going to make Absinthe and gin with. If you want to leave them in and then concentrate them in your future Absinthes by recycling them in your tails, go right ahead, but it's not something you'll catch me doing.

I put my spent Absinthe coloration herbs in the tails.

I'm not commercial and am only interested in making high quality products for my own consumption, so I haven't experimented with recycling tails in any other herbal products.
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Re: Purifying commercial wine spirit

Post by JJF63 »

Hi,
Just to make an update about the tests on rectifying my 96% wine base spirit.
I made one pot-still run and 2 runs using the Snyder column. Pot still run and 1st column run used 1.500ml base spirit 96,4% ABV, diluted to 50% (I did not opt for the 40% because I really wanted a final spirit with at least 80%).
Here are the results:

Pot still
---------------volume ------ ABV ------- EtOH total ---- % EtOH initial
Heads -------- 51 ----------- 88% ------- 44,9 ------------ 3,1%
Hearts 1 ---- 705 ----------- 87% -------- 613,4 ---------- 42,4%
Hearts 2 -----515 ----------- 83% -------- 427,5 ---------- 29,6%
Tails --------- 404 --------- 61,7% ------- 249,3 ---------- 17,2%

Total --------1675 ------------------------ 1334,9 --------- 92,3%
Losses -------------------------------------- 111,1 ---------- 7,7%

Snyder column
------------------ volume ---- ABV ------ EtOH total ------ % EtOH initial
Heads ------------ 35-------- 91,5% --------- 32,0 --------------- 2,2%
Hearts 1 ------- 766 ------ 91,2% -------- 698,6 -------------- 48,3%
Hearts 2 --------- 572 ------ 86,6% -------- 495,4 -------------- 34,3%
Tails -------------- 170 ------ 43,0% ---------- 73,1 --------------- 5,1%

Total ------------ 1543 ----------------------- 1299,1-------------- 89,8%
Losses ------------------------------------------ 146,9 -------------- 10,2%

There are 2 significant differences.
First is the big narrowing of tails. Instead of throwing out 17% of all alcohol in a pot still separation, I just throw out 5% with the column rectification. Heads are also a bit reduced but it's not significant.
Another difference is the clearly higher ABV obtained with the column rectification, from 83-87% to 86-91%.

I was also a bit surprised on getting more than 87% from a 50% ABV diluted liquor (and going down along the distillation), in pot still, when the theoretical output is not more than 81-82%. Which means there is some "plate effect" on the top of boiling vessel-distilling head.

The losses in the column run are a bit high, but I suspect it's due to a not well sealed joint, letting some vapour to escape.
I made a 2nd run (column) taking care of that joint, and losses lowered to 6,4%. I think this can still be improved.

Now, are these figures similar to what you get with your pot still- packed column distillations ?
Maybe it's not comparable, because I don't start with low wines directly from a fermentation, but from an already distilled product.

Any feedback would be much appreciated.
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