Most interesting distillation

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tommysb
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Most interesting distillation

Post by tommysb »

Not an absinthe, but was distilling with some friends a herbal 'bitters' recipe. Unfortunately, I don't remember everything that was in the recipe (I didn't create the base infusion), but it contained amongst various things:
Olive leaves
Peppermint
Spearmint
Linden
(+10 other herbs)
The sort of things that one would put into a Vermouth (actually it was based on vermouth recipe)


Now, the most interesting thing was the fractions that came off the still.

First, around 60-70c, we got a lot of cloudy oils. It caught me by surprise, as I was not expecting anything from the still as it was still warming up, as far as i knew!

Then a small pause, and less activity at the spout.
Then the first running started to come . First clear, then we started to get GREEN liquid. I haven't seen this before. colour coming over, and was kind of surprised. I am pretty sure it's not a puke, as it was a small still, running on low power, and loaded with about 40% ABV.

A couple more jars of green stuff (with bubble gum aroma, in the first part of the run), and then the distillate cleared out.
IMG_20230201_191238.jpg
The beaker on the left shows the first super cloudy part. This reminded me a lot of Pastis, a lot of annis or fennel notes.
IMG_20230201_202853.jpg
Here we can see the various cuts and the colour progression in Jars 1-4. On the furthest left, to the left of jar 0, was a sample of the original infusion which was distilled which is a very dark greeny brown.

For discussion: Is it normal to get colours coming over in the distillate? This was a maceration LOADED with botanicals, so in a way i'm not surprised, but I've never seen this before.
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Dancing4dan
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Re: Most interesting distillation

Post by Dancing4dan »

Interesting.

Post a picture of the still used. What volume of herbs to liquid volume?

Not sure the method used can be compared to a “normal” run. Seems like a high potential for essential oils to come over.
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Re: Most interesting distillation

Post by StillerBoy »

tommysb wrote: Thu Feb 02, 2023 2:36 pm I am pretty sure it's not a puke, as it was a small still, running on low power, and loaded with about 40% ABV.
I do Pastis, and have never encounter discoloration or cloudiness while doing the run.. but the load is reduced to 30% and run really slow.. so maybe your power usage was still to high for the size and amount in the boiler.. getting cloudy first then followed by coloring distillate plus how fast it was brought up to temp..

Mars
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Re: Most interesting distillation

Post by tommysb »

Hi - unfortunately, since I didn't make the recipe, I couldn't tell you exactly what in there - but there was 57g of botanicals in 750ml 77% grape origin spirit/aguardente (the same thing that Port Wine is diluted with). That was then strained, and diluted with 50% water. SO a still charge of 1.5 litres

The still was exactly this model:
4195_1e.png
Our working hypothosis is that the first cloudy part was almost certainly from essential oils.

I don't mind that the colour came over, but it was just very unexpected. I wouldn't even really have bothered making cuts, but was demonstrating the idea of different flavours coming over in different fractions .

I will have to redo a run of the same recipe again and see if we get the same result (when time allows).
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Re: Most interesting distillation

Post by StillerBoy »

tommysb wrote: Fri Feb 03, 2023 12:02 pm The still was exactly this model:
What size is the still, and what source of power was used..

Mars
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NZChris
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Re: Most interesting distillation

Post by NZChris »

If it walks like a duck and talks like a duck, it's a duck.

It puked.

Also, you should not get any color until very close to the end of the hearts, preferably after them. If you do, you are running too much power. Slow down, or get a taller still head, or add a slobber box.
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Re: Most interesting distillation

Post by Saltbush Bill »

NZChris wrote: Fri Feb 03, 2023 12:49 pmIt puked.
:thumbup: There is no other possible reason IMO.
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Re: Most interesting distillation

Post by LordL »

Saltbush Bill wrote: Sat Feb 04, 2023 2:24 am
NZChris wrote: Fri Feb 03, 2023 12:49 pmIt puked.
:thumbup: There is no other possible reason IMO.
Feels weird to have a spirit run go puking though?
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Re: Most interesting distillation

Post by StillerBoy »

LordL wrote: Sat Feb 04, 2023 7:17 am Feels weird to have a spirit run go puking though?
But it wasn't a spirit run.. it was a botanical run similar to making gin or pastis..

But the principal of operating a still applied, but without the cuts, as they were done previous in the making of the neutral used..

Mars
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Re: Most interesting distillation

Post by tommysb »

On reflection, it makes sense that the simplest explanation is the most likely.

I will probably do a repeat run and dial the power back, and see if we still get the colour coming over. The hotplate was on almost full power as it has a very slow duty cycle on lower settings (e.g. on for 20 seconds, off for 10 seconds) which leads to variations in output rate.

The only evidence against a puke, and why i thought it wasn't, was that there was green residue inside the lower part of the still, but nothing higher up in the riser. I would assume that in a puke, the green residue would also have been deposited on the inside of the riser.

The still volume is 2.5L, and it was loaded with 1.5L charge. I think the hotplate is 400w but don't have it with me to check.
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Re: Most interesting distillation

Post by StillerBoy »

tommysb wrote: Sat Feb 04, 2023 9:37 am I will probably do a repeat run and dial the power back, and see if we still get the colour coming over.
To assist in resolving your hot plate issue, use a 1/4" plate between the element and the pot, this will reduce the cycling greatly.. one can be made by cutting out the bottom of an old heavy duty frying pan..

A 1.5 is a small amount thereby requires very little heat input to move the temp of the batch..

A puke is carry over of the water by using to much power, first in the form of foaming, then condense back to colored liquid, not the residue of the ingredients in the pot.. the pot used what 2.5L and the load what 1.5L.. that provided little head space.. no different than if one is stripping, head space is required..

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Re: Most interesting distillation

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tommysb wrote: Sat Feb 04, 2023 9:37 am On reflection, it makes sense that the simplest explanation is the most likely… The hotplate was on almost full power as it has a very slow duty cycle on lower settings (e.g. on for 20 seconds, off for 10 seconds) which leads to variations in output rate.

:::especially because…. The still volume is 2.5L, and it was loaded with 1.5L charge.
I ALWAYS use my unaltered hotplate…to negate that ‘slow duty cycle’ nonsense, I have a small bag of Aquarium grade pebbles that are in the bottom of my tiny pot still. It reaches temperature, and when the hot plate cycles, the heat dissipates into the cooking mash, and the output stays relatively stable…

Very useful for full on Spirit runs….especially.
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Re: Most interesting distillation

Post by NZChris »

Try using a cheap power controller with the plate turned to max.
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Re: Most interesting distillation

Post by SouthwestAl »

tommysb wrote: Fri Feb 03, 2023 12:02 pm Hi - unfortunately, since I didn't make the recipe, I couldn't tell you exactly what in there - but there was 57g of botanicals in 750ml 77% grape origin spirit/aguardente (the same thing that Port Wine is diluted with). That was then strained, and diluted with 50% water. SO a still charge of 1.5 litres

The still was exactly this model:
4195_1e.png

Our working hypothosis is that the first cloudy part was almost certainly from essential oils.

I don't mind that the colour came over, but it was just very unexpected. I wouldn't even really have bothered making cuts, but was demonstrating the idea of different flavours coming over in different fractions .

I will have to redo a run of the same recipe again and see if we get the same result (when time allows).
I've got a bunch of these exact 2,5L stills from Iberian Coppers, and I am pretty sure it puked or 'frothed' too. I think you are right about the first part being essential oils though.

I use the same 2,5L models with a max. charge of 1 litre, and heat them fast - power setting 6 on those German heaters they come with, and as soon as the first drip appears, drop them down to 4,5 to 5. The one time I have had a puke with one of them was when I tried using a 2 litre charge, and the thing just bubbled over. Depending on what you are using, and how much it might froth when being heated, it could have bubbled over perhaps?

I just double-checked. The model sold as the 2,5 L Distilling Column Alembic Premium, Thermometer & Electric Plate, actually holds 2,25L if you fill it up the very brim of the pot, and a further 750ml in the head. So the 2,5L is the total volume of the alambic still, not the usable volume. So on this basis, your 1,5L charge is pretty close to the top of the pot, so would have to be heated really, really slowly - like setting 3 on the heater (they go from 0, off to 6, Max). Did you seal the pot with tape or paste, and if not, did you notice and leakage in the join as it started?
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Re: Most interesting distillation

Post by BoomTown »

SouthwestAl wrote: Sun Feb 05, 2023 9:20 am
tommysb wrote: Fri Feb 03, 2023 12:02 pm Hi - unfortunately, since I didn't make the recipe, I couldn't tell you exactly what in there - but there was 57g of botanicals in 750ml 77% grape origin spirit/aguardente (the same thing that Port Wine is diluted with). That was then strained, and diluted with 50% water. SO a still charge of 1.5 litres

The still was exactly this model:
4195_1e.png

Our working hypothosis is that the first cloudy part was almost certainly from essential oils.

I don't mind that the colour came over, but it was just very unexpected. I wouldn't even really have bothered making cuts, but was demonstrating the idea of different flavours coming over in different fractions .

I will have to redo a run of the same recipe again and see if we get the same result (when time allows).
I've got a bunch of these exact 2,5L stills from Iberian Coppers, and I am pretty sure it puked or 'frothed' too. I think you are right about the first part being essential oils though.

I use the same 2,5L models with a max. charge of 1 litre, and heat them fast - power setting 6 on those German heaters they come with, and as soon as the first drip appears, drop them down to 4,5 to 5. The one time I have had a puke with one of them was when I tried using a 2 litre charge, and the thing just bubbled over. Depending on what you are using, and how much it might froth when being heated, it could have bubbled over perhaps?

I just double-checked. The model sold as the 2,5 L Distilling Column Alembic Premium, Thermometer & Electric Plate, actually holds 2,25L if you fill it up the very brim of the pot, and a further 750ml in the head. So the 2,5L is the total volume of the alambic still, not the usable volume. So on this basis, your 1,5L charge is pretty close to the top of the pot, so would have to be heated really, really slowly - like setting 3 on the heater (they go from 0, off to 6, Max). Did you seal the pot with tape or paste, and if not, did you notice and leakage in the join as it started?
I agree with not filling the pot to the max…gotta let a still have room to ‘breathe’…
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Re: Most interesting distillation

Post by tommysb »

Thanks everyone for chiming in. Sincerely. Yes, I am pretty sure it must have been a puke, and feel kind of silly for having made a whole thread about it now!

I thought the high ABV in the pot would mean that I wouldn't get a puke, and the riser part making it even less likely.

SouthwestAl - it was sealed with tape. I was filled to around the join line just above the handle. I think we were close to the limit of a sensible fill level, but certainly not past it. Total capacity would be 3l if we have 2.25+.75 in the riser.

The good news is that the product out was very fine, (since imo it was very fine going in already).

Again, hearty thanks for helping out with a simple/obvious problem and providing a sounding board :thumbup:
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Re: Most interesting distillation

Post by NZChris »

An early puke is caused by the surface tension caused by the ingredients in the boiler, coupled with too much heat applied due to the impatience, or inexperience, of the distiller. When you have it charged with ingredients that you've never used before, be especially careful.

If it does puke and that is going to be a real problem, shut down, take the head off and add it back to the pot. It's a PITA, but it doesn't take long.
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Re: Most interesting distillation

Post by Dougmatt »

tommysb wrote: Mon Feb 06, 2023 12:34 am Thanks everyone for chiming in. Sincerely. Yes, I am pretty sure it must have been a puke, and feel kind of silly for having made a whole thread about it now!
Don’t feel silly. It’s not the first one, and someone else may learn from this. It’s good to have these posts out there.
I just read an article about the dangers of drinking that scared the crap out of me.

That’s it. No more reading!
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