Cologne - high alcohol

[AlexandreDumars]

Hi everyone. So today I did my first run using the still (column alembic 10 litre) - I did an initial clean with rye flour and water and following that there was still a distinct smell of linseed from the interior sealant. I then ran a batch of just plain water through the system collecting another 100ml of liquid. The scent persists though it is fading so I have now done a third - but this time with a cup of vinegar added. Anyway - once there is absolutely no odour I will continue with my labours. There are two things I want to do:

1. Make cologne in the traditional way, distilling a blend of citrus oils, 95% alcohol and distilled water. The total alcohol volume comes to around 70% I believe. 600g of this blend is meant to be distilled with the first 500g being captured for use and the rest discarded. It is then blended with essential oils and that's it.

2. Make a special tincture. I tincture in the normal manner vanilla beans with a drinking spirit (40% alcohol) and grain ethanol (96%) blended to make around 70% alcohol if you also take in to account the 25% water content of the vanilla beans which may exude during the tincturing process. This I then wish to distill to make the finished product. I am considering stuffing botanicals in the column of the still to add a little further intensity to the finished product.

My questions are thus:

1. Is it especially dangerous to be running this level of alcohol through the still (I use an electric hotplate in an airy environment). This is, I believe, the traditional way colognes were made and the alcohol amounts match with history so I presume it was considered safe enough to do in the past.

2. Should I remove the vanilla beans from the alcohol / water tincture before I distill it?

3. Is it a bad idea to stuff the column with some added material due to issues with reflux?

I am rather eager to learn and have been watching videos to understand the general principles of what is happening inside the still but as these are slightly different uses than the norm (making drinks) I am not finding info quite so easily.

[still_stirrin]

My questions are thus:

1. Is it especially dangerous to be running this level of alcohol through the still (I use an electric hotplate in an airy environment). This is, I believe, the traditional way colognes were made and the alcohol amounts match with history so I presume it was considered safe enough to do in the past.

Yes. Alcohol has a low flash point, meaning higher purity alcohol in the boiler will not only boil a lower temperature, but the temperature that the vapors can explode is also low. A vapor leak can auto-ignite if exposed to the other components of the “fire triangle” (oxygen and an ignition source) at the appropriate concentrations. This means, keep the system contained (no leaks) from the boiler to the product condenser and make sure your condenser can fully condense the vapors.

When I make absinthe, the boiler charge is usually around 65%ABV (higher the our usually recommended upper limit of 40%ABV) because the higher purity will boil at a lower temperature which is critical to the essence extraction of the botanicals. And when the boiler is heating (at a slower than usual rate, ie - low heat input), I often can hear “thumps” inside the boiler as large bubbles break out of the liquid charge to the surface. These “pressure bumps” could cause vapors to leak out of seals, especially the lid-to-stockpot seal, if not properly secured.

Also, I use a potstill, not a reflux still for the absinthe spirit run, so the vapor path is closed from the boiler to the product condenser. With a reflux still, you have an atmospheric vent in the vapor path that could leak explosive vapors, so be very careful.

So indeed, it is dangerous to run your boiler at these elevated boiler charge %ABVs. Use caution…NO OPEN FLAMES. And keep a fire extinguisher handy.

2. Should I remove the vanilla beans from the alcohol / water tincture before I distill it?

You’ll get significantly greater vanilla extraction at elevated temperatures, so I’d leave the beans in the boiler. However, you may need to adjust the amount of vanilla used. But, I would make those adjustments to the recipe after the first run, or possibly the third or fourth run. I doubt you’ll have “too much vanilla” character in the product.

3. Is it a bad idea to stuff the column with some added material due to issues with reflux?

If you’re running the still in reflux, just make sure the column is not packed too tight. And if putting additional botanicals into the column, put them above the packing (below the reflux condenser) so the falling condensate drips back through the botanicals.

This is parallel to the way we make gin with a “gin basket” where the hot alcohol vapors push through the botanical load out towards the product condenser. In the case of the gin basket, the extraction of the essence will be more delicate because only alcohol vapors effect the botanicals, not the condensate.

… I am rather eager to learn and have been watching videos to understand the general principles of what is happening inside the still but as these are slightly different uses than the norm (making drinks) I am not finding info quite so easily.

Yes, our hobby indeed focuses on ethanol for consumption, not really perfume making. But after all, “alcohol is alcohol”, right? I’m not going to address other opportunities of alcohol distillation because of our focus, OK?
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[jonnys_spirit]

A small’ish vacuum lab still might be useful for lowering boiling points and reducing heat on botanicals.

Cheers,
Jonny

[AlexandreDumars]

Also, I use a potstill, not a reflux still for the absinthe spirit run, so the vapor path is closed from the boiler to the product condenser. With a reflux still, you have an atmospheric vent in the vapor path that could leak explosive vapors, so be very careful.

This is enormously helpful thank you! It seems the key to keep this as safe as possible is sealing the still up tight.

I should mention, in case it makes a difference, that my still doesn't have any reflux equipment - it is a regular still with a detachable central column - it was into that column that I planned to put the additional botanicals.



Initially I shall try working on colognes as there is less time involved - the materials are blended and rested for 24 hours, rather than three months for the vanilla!

Your help has given me the confidence to continue on so thank you!

[AlexandreDumars]

A small’ish vacuum lab still might be useful for lowering boiling points and reducing heat on botanicals.

Cheers,
Jonny

Thanks for this suggestion - I will look into those.

[NZChris]

What you have done so far won't have removed all of the toxic flux and machine oils from the build. You need to do a sacrificial alcohol run to remove them before you put product through it.

[AlexandreDumars]

What you have done so far won't have removed all of the toxic flux and machine oils from the build. You need to do a sacrificial alcohol run to remove them before you put product through it.

Thanks Chris - I am going to do that today. Finger's crossed!

[AlexandreDumars]

Thank you to everyone for the advice given.

I did a sacrificial alcohol run and it completely removed the malodours that were plaguing me.

I then went on to do a first attempt distilling a cologne from a blended 70% pure starting material (citrus oils, grain alcohol, other botanical oils). The result was beyond my expectations. The liquid is intense, elegant and explosive (in the good sense!)

So again, thanks for the hand holding through this first step. I foresee many more distillations in my immediate future.