Workflow for neutral or flavored spirit and liqueur

[spot]

I'd be grateful for as much critical comment as can be made to correct and improve the post, this is only one of the many possible ways of getting a result and obviously imperfect



Abbreviations and terms used

alcohol: wherever this word occurs it means exactly ethanol and nothing else

%abv: an alcohol/water mix showing the percentage of alcohol by volume. This pecentage is a higher figure than the percentage of alcohol by mass, %abw, because (roughly) a litre (which is a volume, a cube with side 10cm) of alcohol has a mass of 800g and a litre of water has a mass of 1000g and mixing the two gives you slightly less than 2 litres as the molecules pack more tightly in a mixture.

T500, SmartStill: commercial tools, the first a fractionating still and the second a still without a fractionating effect


Background

This workflow uses both a T500 and a SmartStill, two 30 litre lidded containers, a bucket to catch distillate and a waste solvent bottle

The T500 creates 90-93%abv of neutral (unflavored) spirit from a boiler containing 14-93%abv.

The SmartStill distills out more than 50%abv with volatile flavors from a boiler containing 14%abv, or about 65%abv from a boiler containing 40%abv. There's a graph describing this concentrating effect at https://en.wikipedia.org/wiki/Ethanol_% ... _Water.png

I'm using the SmartStill to retain volatile flavors while holding back less volatile oils and solids, and the T500 to create neutral unflavored overproof spirit from a fermented wash.


Sterilizing

Immediately before use, sterilize everything which will touch the wash before and during fermentation. Once all the sugar has fermented out there is no reason to sterilize anything, washed-clean is sufficient.

Some people would boil the tapwater ingredient too, which both sterilizes it and removes chlorine


Eliminating chlorine and minerals

The only stage where tapwater is inappropriate is when diluting the final product to a drinkable strength, where distilled (or possibly fresh or bottled spring) water should be used


Eliminating everything which isn't ethanol or water

When distilling from the wash, discard the first 50ml which will contain all of the organic product more volatile than ethanol (including whatever potentially-lethal methanol might have been made if an unlikely contamination of the yeast has happened)

Every other non-ethanol contaminant will be removed by a week soaking over activated carbon, to whatever extent soaking over activated carbon can remove non-ethanol contaminants


One-time preparation

Mark one washed 30 litre container "the fermenting tub"

Mark the other washed 30 litre container "the carbon-filtering tub"

Wash a kilo of activated carbon pellets until the tapwater runs clear and place the pellets in the carbon-filtering tub with sufficient tapwater to completely submerge them. Most people would keep these pellets in a loose-mesh bag or basket. Annually replace the activated carbon pellets with fresh washed replacements


Procedure for creating intermediate carbon-filtered 40%abv

Sterilize a whisk, stirrer, the fermenting tub, bubbler if used

Make up a 25 litre neutral sugar wash including sugar, nutrient and tapwater, in the fermenting tub. Thoroughly whisk to aerate, then stir in the yeast

Wash the whisk and stirrer clean

[A]: Allow the wash to fully ferment under a loose lid, or tight lid with bubbler if preferred

Sterilize a hydrometer and graduated cylinder and check the SG

Wash the hydrometer and graduated cylinder clean

If the SG is above 1, restart the fermenting and go to [A]

Allow the fermented wash to clear, with fining if that's preferred

After a day or more, siphon the cleared liquid into the T500 boiler and add coins or boiling stones

Wash the siphon, fermenting tub, bubbler if used

Distill with an outflow water temperature between 50-65°C, immediately discarding the first 50ml of distillate into a waste solvent bottle, until the output stops

Turn off and wash the boiler clean

Add 4-5 litres of tapwater to the carbon-filtering tub (less the 2 litres already in the tub if this is the first time it's being used)

Add the 3-4 litres of distillate to the tub, put the tight lid back and give it a swirl or two. The ratio of tapwater to distillate should make roughly 40%abv.

Wait a week for non-ethanol volatile organics to adhere to the carbon filter pellets if they're going to


Procedure for creating 40%abv final product

Fill the SmartStill with 4 litres from the carbon-filtering tub (which will have a carbon dust suspension) but don't leave the activated carbon pellets uncovered

If you intend flavoring the product, add essential oils to the SmartStill

Run the SmartStill until 2.5 litres of distillate has been extracted - this will be 65%abv and have no oil or suspended carbon but with flavor if you used it

Wash the SmartStill boiler

Dilute using distilled water with an alcometer to 40%abv or to taste

Bottle for use as a spirit or with sugar to taste for use as a liqueur

[Curmudgeon]

I'm still a newbie and I've never used carbon, but I confess I'm struggling to work out the logic behind filtering after stripping run rather than spirit run?

Surely you go through at least twice as much carbon?

Other than that, making no cuts other than taking off fores seems a big step backwards from most current thinking. ie your process is stripping run, remove fores, filter, spirit run whereas most do stripping run, spirit run,remove fores, make cuts (and then maybe filter).

[spot]

It's good of you to raise issues, thank you.

Regarding the activated carbon, what I've done is put as much as anyone would use in a year into one tub and left it there for the duration. I'm sure a year's worth of fermented sugar wash distillate will not overload an entire kilo's ability to absorb complex organic molecules. The other advantage is that there's no directional flow across the activated carbon to flush out older captured content. Finally, the carbon never sees any alcohol at more than 40%abv.

The T500 will remove everything that's solid, and everything that's not volatile, and it will concentrate all of the alcohol from the wash into a 90-93%abv distillate. So the only things that can be in the distillate are (1) things more volatile than ethanol, and (2) ethanol and water, and (3) every other volatile which is none of the above.

Removing (1) by chucking the first 50ml of the run means there will never be any things more volatile than ethanol at any stage further down the line. Top of the list is any methanol, but we all agree the first 50ml smells undrinkable whatever's in it.

Removing (3) with the activated charcoal is the only way anyone seems to have to get rid of those other less volatile organics. What else does anyone do which might achieve that?

Speaking solely for myself I don't believe a sugar wash ferment will contain "heads" in a fractionated distillation. I think heads are something you get with a non-fractionating still and a mash designed to take lots of complex molecules as flavor through a simple still which has no plates to force them back down into the boiler. If anyone would like to correct me I would be delighted to hear their reason.

The reason I do the two runs in this order is so that the flavoring only goes through the SmartStill, which won't hold it back. I'm quite sure a fractionating head would interfere with any flavoring, so I do the fractionating before I add any essential oils. If you look at viewtopic.php?f=1&t=4361&p=39433#p39388 the Adams gin process uses the same order, fractionating followed by a pot still, for the same reason.

I'd be happy to throw 100ml instead of just 50ml, it makes little difference and it might placate onlookers.

When I do a workflow which has flavoring from the beginning - rum and whisky - I'll not use the T500 at all and I'll definitely focus on heads. This workflow is the really really simple one by comparison.

[Anavrin]

Hi Spot

I think you need to take a step back and have a little think about what goes on when you boil a wash, a wash is a volume of fermented liquid that contains water, ethanol and everything in between, including methanol, ethel acetate, acetone and fusel oils, i.e. Every wash contains fores, heads, heart and tails.

You cannot say that the type of Still can affect how these compounds come through, your boiling a liquid, and regardless of what type of Still it is, there will always be fores, heads, hearts and tails coming through the Still in that order, also flavour will still come though, even in a reflux column or plated still.

The only difference between a pot still and a packed column/plated Still, is the way in which the various compounds are compressed, a pot still will produce ethanol continuously, but initially there will be a high concentration of heads that slowly tapers away before the tails start to come though, they will start coming through slowly at first and increase towards the end of the run.

A reflux column or plated still works in a similar way, only the heads are compressed and concentrated into the first part of the output, allowing a window of opportunity where clean hearts can be collected before the tails start to come though, these are also compressed into the very end of the the run, making a packed column ideal for neutral spirits but you will still have to make a significant heads cut before you find the clean hearts.

Flavour works in a similar way, the flavour is in the late heads and early tails, therefore so far as a pot still is concerned, will be mixed with the middle hearts cut, it will contain some heads and tails giving it flavour, the same can also be achieved with a plated or packed column, however because of the cleaner hearts cut, you would need to carefully add some late heads and early tails to you hearts collection to get the flavour back.

On the point you made about carbon filtering, don't bother until you have finished your second spirit run, and then only if you after a neutral spirit.

[Anavrin]

And a sugar wash contains lots of heads, probably no methanol but lots of heads for sure.

[Curmudgeon]

Fair play to you Spot, you are zigging when the rest of the world is zagging.

There's probably good reasons why almost everyone else does it different to you and has done for a 1000 years and more, but I don't know what they are.

Do me one favour Please? and tell me you aren't using plastic containers? I'm more relaxed than most about the non tefal o ring in my T500 pot head and the food safe but not alcohol safe other bits my booze may briefly come into contact with, but when you talk about storing for a week, I have to ask.

It's like the old thing about dropped food being OK on the floor for so many seconds. No way high proof for a week is OK in plastic. I've seen 23 litre glass carboys, but not 30 litre.

[Mash]

Can I ask what the purpose of your original post was please?
I ask because sometimes I think you are a chemist, and understand where you are coming from because I have experience with that mindset.
Then other times your approach and what you write to seem to be a little bit out of balance, and demonstrate some fundamental misunderstandings.

In your post of Sun Oct 30, 2016 you wrote...
"I bought a SS a couple of weeks ago and I've been triple-distilling water to get a feel for it."

So as an amateur you have come an awful long way in 6 weeks or so - or you had a head start.

[spot]

I'm grateful for the effort that has gone into those posts, they bring out very relevant points.

You're quite right Mash, this is purely from a chemist's view and I've little recent experience in distillation and no prior history of distilling alcohol. What I'm doing is preparation for putting detailed snapshot samples through this gas chromatograph I picked up, to explore the identity and location of all these volatile organic components we're discussing, adding some figures to the thread and modifying my ideas as I do so.

Now, to these fundamental misunderstandings. I regard this thread as part of my education and I certainly intend to modify my workflow once we settle to some form of consensus here. I would not have come to this gathering of experts had I not intended to learn from you.

I agree entirely with Anavrin that every volatile organic will come over regardless of whether it's with a fractionating column or with a pot still, and that the time each component comes over is the sole variable. I must agree this has to happen for flavors too as he says, which changes my thinking in that regard. If flavors could in fact be held back by a column then they'd not get over a pot head either. Is "pot head" acceptable terminology or is it exclusively a 60s hippy?

I also think it likely that "a sugar wash contains lots of heads, probably no methanol but lots of heads for sure" and I suggest a fractionating head will focus these more volatile organics into that first 50ml (or 100ml, as you will) more than a pot would, I don't think that's contentious. Regarding tails, anything that might qualify as a tail compound is removed by the first fractionation - my understanding is that there are no tails from a fractionating still.

The elephant in the room is this activated carbon, and what it's supposed to do. Either it will scavenge a large proportion of the volatile organics (the ethyl acetate, acetone and fusel oils mentioned) and lock them up from a 40%abv spirit, or it won't. If it will, why are the heads collected after fractionation? Note I am not arguing against the collection and evaluation of heads from a pot or alembic, that's obviously an important process, I'm solely considering what comes off a fractionating head here. And if activated carbon won't lock these organic components up, what on earth is the activated carbon supposed to be doing? There's nothing else there for it to take hold of.

Curmudgeon's note on leaching from plastics is also helpful and something I hope to be able to check later. I would hope we agree that people routinely ferment to 10-20%abv in plastic containers, so the question is more about what happens after than whether leaching is a worry. In the case of the workflow I outline, nothing stored in plastic is considered drinkable and nothing leached has a low enough molecular weight to be distilled into a product. Everything I collect from the second distillation goes into glass and stays in glass and is bottled into glass. I think this is precautionary rather than essential, I'd have no problem drinking spirits stored in, say, recyclable HDPE plastic containers (the sort milk's sold in) but I don't in fact do that. If anyone thinks a leached compound can arrive in a distillate could they tell me what compound it is please?

[Easydrinker]

To answer a few of your points,starting from the bottom.

Plastics.
This is something that I looked at in detail a while back.
Many HDPE and PET bottles are spray lined at maufacture with another compound, matched to the proposed contents.The 'plastic' spirit bottles that you buy at airline duty free are an example, designed for 40% alcohol. Plastic bottle maufacture is complex.

Activated Carbon.
You are probably correct,use enough of this and you could filter heads.
This is what big players try.
For us it is easier and cheaper to seperate the heads out.

Tails and a fractionating still.
Run the still hard enough,to leave less alcohol in the boiler,and you WILL get tails.
Most stop before this point is reached.

Heads and a fractionating still.
You cannot condense the heads into the small volume that you describe.
My own experience is that a boiler charge of around 18-20 litres @28-30% will produce around 700ml of Fores/heads running at around 94%.
Of course this is subjective,the line between heads and hearts is not fixed,

Robert.

[spot]

That's invaluable Robert, thank you.

[Brewhunter]

Good post Robert