The Cousins Process in High Ester Rums by Richard Seale

[OtisT]

You must have a clear liquid to boil it down.

OK please explain why?

I believe it is clear because of the process says to use lees (content of a retort/thumper after a first run), which will be clear. Your short summary of the process lists using the contents of the 1st boiler (dunder), which is not clear.

That’s just how I read this. Otis.

[kiwi Bruce]

Here's why I think it's dunder (besides the fact I've not seen the residue left over from a thumper called lees) there would be no fatty acids in the residue left over from the thumper as the vapor point of fatty acids is too low to distill, they would have to be left in the pot of the beer run. "Lees" is what the Scots single Malt distillers call the residue left from a beer run. Cousins may have used "Lees" in his paper because the term "dunder" may not have been familiar to his readers. Just saying...I think he's talking about dunder.

[WeegieDistiller]

Spent lees is the residue or effluent from a spirit distillation of single malt, not a wash distillation. The leftovers from the wash distillation is called the pot ale or in the rum world, dunder.

The reason why I think it's liquid from the 1st thumper is because it has already been through one distillation, in the pot, and the double retort set up is technically triple distilling a spirit.

[SaltyStaves]

(did I read this here? pH 3)

Unless its in that thesis der wo posted, I have not read that.

[NZChris]

Here's why I think it's dunder (besides the fact I've not seen the residue left over from a thumper called lees) there would be no fatty acids in the residue left over from the thumper as the vapor point of fatty acids is too low to distill, they would have to be left in the pot of the beer run. "Lees" is what the Scots single Malt distillers call the residue left from a beer run. Cousins may have used "Lees" in his paper because the term "dunder" may not have been familiar to his readers. Just saying...I think he's talking about dunder.

The ‘lees’ in the retort at the end of distillation...

cannot indicate dunder as the main boiler isn't called a retort.

With a simple pot still, the lees from the spirit run would do, with a single thumper it would be the lees from the thumper.

[SaltyStaves]

https://www.bostonapothecary.com/wp-con ... uction.pdf" onclick="window.open(this.href);return false;" rel="nofollow

The majority of these acids are to be found in traces in rum, and in view of their high boiling points (78 C.) are probably distilled in steam towards the end of the distillation. They should, therefore, be more concentrated in the retort lees, a fact which is borne out by the use of these lees for the preparation of "lime salts" used in the preparation of "high ether" rums.

There is further required reading in this same document.

[NZChris]

The majority of these acids are to be found in traces in rum, and in view of their high boiling points (78 C.) are probably distilled in steam towards the end of the distillation. They should, therefore, be more concentrated in the retort lees, a fact which is borne out by the use of these lees for the preparation of "lime salts" used in the preparation of "high ether" rums.

Something doesn't ring true to me about that quote, Salty. 78 C isn't high.

[der wo]

You must have a clear liquid to boil it down.

OK please explain why?

Because otherwise you get mainly a thick sludge from ash, gums and yeast. It's all molasses washes. Probably gums produce off flavors.

Here's why I think it's dunder (besides the fact I've not seen the residue left over from a thumper called lees) there would be no fatty acids in the residue left over from the thumper as the vapor point of fatty acids is too low to distill, they would have to be left in the pot of the beer run.

The boiling points of the pure substances are high. But this doesn't mean that they are not volatile. Butyric acid has a boiling point of 164°C, but once you get your nose near a bottle with it you will never forget the smell.

(did I read this here? pH 3)

Unless its in that thesis der wo posted, I have not read that.

If I wrote this somewhere, it was only what I would try out, not what I have read somewhere (Arroyo for example).

The majority of these acids are to be found in traces in rum, and in view of their high boiling points (78 C.) are probably distilled in steam towards the end of the distillation. They should, therefore, be more concentrated in the retort lees, a fact which is borne out by the use of these lees for the preparation of "lime salts" used in the preparation of "high ether" rums.

Something doesn't ring true to me about that quote, Salty. 78 C isn't high.

Incomplete quoting. It's "and in view of their high boiling points as compared with alcohol (78 C.)"

[SaltyStaves]

The majority of these acids are to be found in traces in rum, and in view of their high boiling points (78 C.) are probably distilled in steam towards the end of the distillation. They should, therefore, be more concentrated in the retort lees, a fact which is borne out by the use of these lees for the preparation of "lime salts" used in the preparation of "high ether" rums.

Something doesn't ring true to me about that quote, Salty. 78 C isn't high.

Damn. Serves me right for trying to transcribe while keeping one eye on the collection jar.

[NZChris]

BTW, the original Cousins report is also available in the Kingston Daily Gleaner, September 27, 1907, Page 9

[WeegieDistiller]

Would anybody be willing to haphazard a guess at volumes and amounts of lime and sulfuric acid to use for a given quantity.

I haven't jumped down the rabit hole this far to date. Might be worth ready through Arroyos notes again to see it anything jumps out of the pages.

I think sourcing Sulfuric Acid in the UK is going to be a bit difficult for personal use as there's been a rise in acid attacks unfortunately stupid humans!! Will try and source via "company" instead as well as the lime.

[der wo]

Search for "instant drain cleaner". This should be sulfuric acid somewhere over 90%. No guarantee, you have to find out yourself if there is something els in it, besides water of course. Or battery acid. This is around 30% sulfuric acid, nothing else, besides water.
Sorry, I can't give you clear amounts. But because a distillate is not strong acidic and has no buffers, a very small amount lime will be enough. And then, the less lime you need, the less acid you will need. 1l battery acid or drain cleaner will be enough for many many experiments... Lime, perhaps something like four or ten times more than (pure) sulphuric acid?

[kiwi Bruce]

Would anybody be willing to haphazard a guess at volumes and amounts of lime and sulfuric acid to use for a given quantity.
I think sourcing Sulfuric Acid in the UK is going to be a bit difficult for personal use as there's been a rise in acid attacks unfortunately stupid humans!! Will try and source via "company" instead as well as the lime.

Go to your local Homebrew supplier and get you hands on brewers pH papers. These are used in the Homebrew Hobby to get the water in the right range for mashing malt in an all grain brew. A pH of 7 is neutral...pickling lime (Calcium Hydroxide) will take the solution into the "Basic" range...so Plus pH. I think you'll only need to go to a pH reading of 10 (about as strong as Milk of Magnesia) to capture the fatty Acids your after with your lime. This pH movement is quantitative... meaning - the more fatty acids there are the more lime that will be required to bring the pH up to 10. Likewise when you want to take the solution back in the "Acid" direction...so Negative pH...with Sulfuric Acid. You'll need to take the pH to around pH 3 (about as strong as Lemon Juice) Again this pH movement is quantitative... meaning that if there is a little more lime in the solution it will "Buffer" the liquid at around pH 7 until enough acid has been added to bring the pH down. The second reason for using Sulfuric Acid is that it is the Catalyst in the esterification reaction...Fatty Acids + Alcohol + H2SO4 = Esters.

The pH ranges I've given are an educated guess (I know I've read this - can't remember where...Anyone else know?)
I don't drink to forget...it just happens that why!

Now getting the acid in the UK...You CAN use used battery acid, it will have dissolved lead salts but these will not distill over. You can make it...look on YouTube...but only if you can't find it anywhere else...your time is far better spent making some spirits than chasing Sulfuric Acid.

[der wo]

I think you'll only need to go to a pH reading of 10 (about as strong as Milk of Magnesia) to capture the fatty Acids your after with your lime.

In theory pH 7 should be enough. I would target 7.5.
And then you will mix the boiled down powder into the fermented wash? Then it will be acidic enough even without adding an acid. So you need sulphuric acid mainly as a catalyst, not for dropping the pH.

Edit: Why I only want small pH corrections? Because I am unsure. And the only data I have is how Arroyo thinks about pH. He only makes small corrections. For example when clarifying an unfermented wash by boiling, he rises the pH from 5.5 to only 6.0. This small correction seems to be enough to keep the acids and esters. But he doesn't say, what would happen with pH 8 for example. If it would be only a waste of lime (and later acid) or perhaps if it would have negative consequences.
I think there are many possible experiments with pH correction and Rum. But without side by side comparision it doesn't make much sense.

[WeegieDistiller]

Thanks for the alternative sources for acids.

I was going to attempt two separate trials when giving it a bash. First one at lime till the ph is neutral or slightly above and the second at lime so it is a higher ph value about 8 or 9. Add the acid to bring the ph level down and react with the calcium to form the calcium sulphate.


I'm thinking that any excess or left over sulfuric acid will act as a catalyst in the thumper as you say.

I've also read on cocktail wonks blog from his trip to Hampden Distillery that they do the same with their muck for "long term storage" of the acids between production cycles.

W

[der wo]

I was going to attempt two separate trials when giving it a bash. First one at lime till the ph is neutral or slightly above and the second at lime so it is a higher ph value about 8 or 9. Add the acid to bring the ph level down and react with the calcium to form the calcium sulphate. You mean you split something like spirit run stillage and experiment with different pH levels, and boil them down to powder? And then?

I've also read on cocktail wonks blog from his trip to Hampden Distillery that they do the same with their muck for "long term storage" of the acids between production cycles. But this is to keep the bacteria happy. They use lime to hold the pH at 5.8. without lime the pH would drop very fast (because of the acids the bacteria produce) and the bacteria would stop working.

[SaltyStaves]

Aroma analysis should be a straightforward way to qualify your essence prior to running it.
A small amount of it in a test tube, with ethanol and gentle heat, will give you an indication as to what the potential is.

[WeegieDistiller]

"You mean you split something like spirit run stillage and experiment with different pH levels, and boil them down to powder? And then?."
Yes I want to split the lees into two batches to try different routes by increasing with lime and reducing to the salts then add the sulfuric acid afterwards to hopefully precipitate calcium sulfate. The original guide mentions to add this to high proof spirit and put in the 1st retort and carry out another run to produce the "flavoured " run concentrate

"But this is to keep the bacteria happy. They use lime to hold the pH at 5.8. without lime the pH would drop very fast (because of the acids the bacteria produce) and the bacteria would stop working."
The article I read says at Hampden Distillery they adjust the ph to make the bacteria dormant or stable for long term storage in the ground. It doesn't mention anything about raising or lowering in this part just that if they are left to themselves they would create undesirable forms of the acids.

[kiwi Bruce]

In theory pH 7 should be enough. I would target 7.5.

Not so much...pH 7 is neutral :- tap water (sea water is pH 8 )...believe me on this one, neutral won't do shi#...the still residue should be acid, like a sour mash setback---pH 5 or 4...so you'll have to go further than that.

[der wo]

In theory pH 7 should be enough. I would target 7.5.

Not so much...pH 7 is neutral :- tap water (sea water is pH 8 )...believe me on this one, neutral won't do shi#...the still residue should be acid, like a sour mash setback---pH 5 or 4...so you'll have to go further than that.

Neutral means all acidity is neutralized. No H+ ions are left. and this means no way for the acids to evaporate.
For example hydrochloric acid (HCl) is in solution Cl- and H+ ions. If all H+ ions have reacted with the OH- ions of a base to water (H²O), and this is the case at pH 7 or higher, the Cl- won't find a H+ ion to connect and evaporate.
Of course it depends on the acid content how much lime is needed for pH 7.
Perhaps you understood me wrong? Of course you cannot add something with pH 7 and this will bring something with pH 5 to pH 7. Of course you have to add something stronger. But when the pH is 7, the solution is neutral, no matter how acidic it was before adding lime.

[der wo]

"But this is to keep the bacteria happy. They use lime to hold the pH at 5.8. without lime the pH would drop very fast (because of the acids the bacteria produce) and the bacteria would stop working."
The article I read says at Hampden Distillery they adjust the ph to make the bacteria dormant or stable for long term storage in the ground. It doesn't mention anything about raising or lowering in this part just that if they are left to themselves they would create undesirable forms of the acids.

Yes. I feared you would mention this... Because IMO there must be something wrong:
It may be possible to make the bacterias dormant by high pH. But this would kill them and it would kill the muck, because other bacterias would take over (rotten meat smell probably). The best way to keep a bacterial culture alive is to let it work under proper circumstances. Or perhaps a low pH is meant, this would indeed stop the bacterial work and also hinder other infections. But this would also cause acids and esters to evaporate...

[Shine0n]

If my ph drops to blow 4.2ish my pellicle falls off the top, I believe this stage is dormant.
When I add lime to raise the ph, the pellicle returns.

I've tossed all the muck except the potatoes and soil pit, I've not looked at it in 2 weeks because of work but the pellicle is very thick/deep probably 2.5"-3" and looks like it moving underneath it.

This will most likely my last stance with adding to low wines for a spirit run. Instead I will be adding 4 days into fermentation and going 3 weeks long instead, with a double retort potstill.

I love the excitement of this but I'm not really wanting DOC, I'd rather have something along the 200-500 ppm range without blending with 1600 Ppm

[SaltyStaves]

Left to their own devices and not given a source of food, bacteria will reduce their environment to water and ammonia.
My own outdoor pit is dormant for the winter. I acidified it to pH 4.5. There are no signs of activity. When the warmer months return, I'll be adding lime to it to restart it.

This is how it is done with distilleries that have the outdoor 'Graves'. They have seasonal shutdown periods and they stop and start the graves accordingly.

[der wo]

If my ph drops to blow 4.2ish my pellicle falls off the top, I believe this stage is dormant.
When I add lime to raise the ph, the pellicle returns. Yes. But this makes the acids and esters volatile. You are loosing many of them.

I love the excitement of this but I'm not really wanting DOC, I'd rather have something along the 200-500 ppm range without blending with 1600 Ppm And where do you know what 200-500 ppm tastes like?

[der wo]

Left to their own devices and not given a source of food, bacteria will reduce their environment to water and ammonia.
My own outdoor pit is dormant for the winter. I acidified it to pH 4.5. There are no signs of activity. When the warmer months return, I'll be adding lime to it to restart it. But this would make the acids volatile. Less a problem in winter where you live perhaps. But in the tropics?

This is how it is done with distilleries that have the outdoor 'Graves'. They have seasonal shutdown periods and they stop and start the graves accordingly. You mean in winter when no molasses is growing on the trees and all Jamaikans are skiing on the hills, two people go to the earthen muck grave and one of them throws lime or sulphuric acid into it and the other one stirs with a large spoon?

I think, the grave runs more or less on its own and from time to time someone throws whatever food in there and takes out a few canister muck for the distillery. And then when the muck is in use in the muck pit (with a stirrer), they of course take care of the pH.

There are muck graves and muck pits. It's not the same.[/color]

[SaltyStaves]

There are muck graves and muck pits. It's not the same.[/color]

Then we agree on that at least.
The graves are not bioreactors. The pits (vats) are. The graves are long term storage. I'm am not convinced that they are perpetually maintained.

[kiwi Bruce]

Cousins wasn't writing about Dunder pits though...He's talking about reusing the Liquid leftover from the still itself and adjusting that.

[WeegieDistiller]

Too far down the rabbit hole haha

Sometimes it can't be helped

[kiwi Bruce]

Neutral means all acidity is neutralized. No H+ ions are left.

I'm not A Chemistry teacher, however I did work as an inorganic chemist in another life.
"Neutral means all acidity is neutralized" Yes, but Neutral also means all bases are neutralized.
pH (potential hydrogen) is a measure using a 10 logarithm scale, of the molar concentration of hydrogen ions, in moles per liter. pH 4 is ten times more acid than pH 5 but a hundred times more acid than pH 6. So even a neutral solution has Hydrogen anions but they are in a balance with the cations in the solution.
The concentration of the hydrogen ions is 10−7 gram-equivalents per liter, which corresponds to a pH of 7.

and this means no way for the acids to evaporate.

Don't take me wrong, not a knock-down...Acids and Bases, like there salts, don't evaporate, they decompose.

[Single Malt Yinzer]

More background on HH Cousins: - From Boston Apothecary because of course he's a few years ahead of us.
https://www.bostonapothecary.com/jamaic ... h-cousins/" onclick="window.open(this.href);return false;" rel="nofollow