Esters from Lime salts - using sulfuric acid; process

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distiller_dresden
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Re: Esters from Lime salts - using sulfuric acid; process

Post by distiller_dresden » Thu Nov 07, 2019 12:04 pm

Been a while. So this is my current high ester Jamaican rum production process. Several objective tasters have told me these 'heavy rums' from my 'heavy process' are indistinguishable from god Jamaican commercials.

I feel really good about my current bill for contents and process, it centers on dunder infected with specific things, like butyricum, lactic and propionic acid producing bacteria. Then fancy molasses to an abv between 9-11%, added in steps - basically 2lbs to start in 1.5 gal volume at temp. After 6 hours in that, I then add half my remaining molasses needed, bring volume to 5.5g, and then after 30 hours the remaining half of molasses. This gives me nice longer ferments. I'm also doping the wash at the first half full volume add with 2g each of heptanoic, benzoic, caprylic, propionic, malic, formic, and butyric acids. I get formic acid by figuring out what amount is in raspberries, then I keep 6oz bags in the freezer for one pitch dosing.

I bring, at the full volume point, PH up to 7.5 with garden lime, or calcium oxide (this is my basic PH giver), then drop it to 5.3 (or max for yeast I'm using; I am trying Lallemands cachaca yeast today in a new ferment beginning, in fact) with sulfuric acid (my acidic PH giver) and let her rip. I check PH each morning and try to keep it over 5 for the first, most active, part of the ferment. Have learned (via extensive reading all of the old rum studies) esters form more readily in ferment above 5.0. 48 hours after my last sugar add, I stop checking PH. Then I typically let it rest at least 3 days before distillation.

Just prior to distillation, 36 hours ahead, I add sulfuric to bring PH down to 3.4-3.7, usually gauging how low I go based on how well the beer responds to the sulfuric. Even formulaic as this is, some ferments resist dropping harder than others, these I get to 3.7 and stay, lest I make copper sulfate from too much sulfuric. Then day of, I fill the first thumper with low wines to 30%, the second with high wines to 75%. This has the added benefit of super esterification in them, and the heads will move nicely from 1, but the carryover heat cant quite get tails out efficiently. Then in 2 the heads have a harder time because theres even more heat loss, since only steam is carrying heat from 1 to 2 and 2 to spout.

I try to keep ice on hand to hold my cooling water around 70 so the exit is perfect temp and the top is around 100-110, this seems to get the best version of distillate, and I culled that from the studies. This results in a white that is SUPER fruity and flavorful, with even a hint of reproducible funk, that's delicious and drinkable after a few days rest in glass.

Boiling this all down: for infecting dunder get a good 'norse' yogurt like siggis, some real block parmesan, I had to get butyricum tabs from Japan on Amazon, I also get 'dosing' fatty acids (which form esters) from Amazon like those I listed - if you can get pure versions it's good, but salt versions like 'sodium propionate' are fine too, they'll drop the salt side and turn to the acids in wash.
Dunder is 20% of wash
5.5 gals volume at 9.5% potential ABV is ~5600g sugar, I'll use a gallon fancy mol and some turbinado sugar. Gordon's food svc has good, cheap fancy mol gals.
Get a good yeast from Lallemand in MI, their RM or Cannamax are great.
Garden lime for raising PH, sulfuric acid (dudadiesel) for lowering. When wash is ready, before adding dunder, get PH to 7.4, then add dunder, and if you still need it lower (bring to 5.3-5.5, the high max for yeast) use sulfuric acid.
Esters form better over 5.0, and around 85F for ferment. Check the wash once or twice a day to keep at or over 4.9.
After 4 days stop worrying/checking PH and let it go. Let the wash rest at least 3 days following ferment finish. 36-48hr before distillation, drop PH to 3.5 area with sulfuric and a good strong stir.

This is my current process and makes a very suitable, genuine Jamaican style rum. It will have strong flavors, nose, and even some funk. It ages gorgeously, and should consume wood, like a gal of my last 60% took 6 5" staves and 1/2c chips, no oakiness after a year! Just be sure to boil or add boiling water to your wood, and let it sit maybe 5 min, then empty, before adding/filling. This pulls the harsher tannins out; if the wood is previously used, no need to do this, just start aging. Or age in glass, giving a shake once a day to oxygenate, because that helps form esters.

This is reproducible, but better results once limed dunder gets going with infections. Dominant flavors change somewhat batch to batch. My latest is really apple forward, like Fuji apple and skin flavors, with pineapple background and more mysterious sweetness, caramel, spices, and funk beneath. Before that I got a more pineapple dominant one. One came out like berries and apples. But the background/supporting flavors are always there and the same. Change up the wood for different results of flavor long-chain esters being formed.
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"I don't know half of you half as well as I should like; and I like less than half of you half as well as you deserve."

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WeegieDistiller
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Re: Esters from Lime salts - using sulfuric acid; process

Post by WeegieDistiller » Sat Nov 09, 2019 5:45 am

Great wee write up and glad to see you're embracing the infected dunder too!

You must get a fair amount of gypsum precipitating when changing the ph levels from calcium and sulfuric acid?

Have you tried stripping the infected dunder by itself so the water and the fatty acids come through and leave the solids behind? That's the method I've been giving a bash for reproducibility (without the single acid additions) and easier to handle too.

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Single Malt Yinzer
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Re: Esters from Lime salts - using sulfuric acid; process

Post by Single Malt Yinzer » Sat Nov 09, 2019 11:49 am

Great write up and great results. Good job on all the research & experimentation. This is really cool you got the results you wanted.

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Re: Esters from Lime salts - using sulfuric acid; process

Post by pope » Sat Nov 09, 2019 2:16 pm

Wow! Phenomenal write up, I’m really glad to see your persistence paid off. I’m very interested in culturing a dunder pit one of these days and will have to also come give your process some trials of my own. Sounds like you’ve created a reliable process!
"A little learning is a dang'rous thing; Drink deep, or taste not the Pierian spring: There shallow draughts intoxicate the brain, And drinking largely sobers us again." - Alexander Pope

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Re: Esters from Lime salts - using sulfuric acid; process

Post by distiller_dresden » Thu Nov 21, 2019 10:07 am

Thanks for feedback everyone; to answer the few questions, I haven't noticed much gypsum precipitate, but it's likely a component of the lees/muck at the bottom of my fermenter post distillation (and ferment). I usually distill it 'clean' which it always rests about 5-6 days post ferment prior to my 36-48 hr pre-treatment with sulfuric to drop PH and form some last minute esters. I give it a good stir, and then it stands clearing. It's usually as 'cleared' as it will be when I take off the top/over lees for distillation, the sulfuric drop usually causes it to settle quite well. Then I grab 1c of the lees/sludge to add to the pot and stir in before sealing and heating up; lots of esters/flavor in the lees, but don't use so much it causes build up in my still. Haven't tried clearing the dunder either, since it's infected I don't want to cook it, I worked hard to get all the right infections to establish well! Especially the butyric, which you can smell like sweaty toes or not quite 'poop', but like a wet butt lol.

I've tried so many different methods, and not until I incorporated sulfuric and lime with the infected dunder, and my dunder stock had begun to be majority from washes using sulfuric and lime, did I start really noticing the super charging of esters. This is NOT a rum for someone unassociated with funky or Jamaican rums, so to them it may seem 'bad' or 'off taste', but if you are into them or have tried a funked up rum, you'll immediately notice the profile. Mine skews more vegetal/apple peel than olive brine or other flavors like petrol, but I suspect a change in the addition of various fatty acids or the balance of the dunder infection would yield those results.

If I could get my hands on longer-fermenting top ferment yeast, or even a sound schizosaccromyces pombe, I'm sure I'd get even nearer.

For now, the Lallemand (MI) CM and RM, or their cachaca and rum yeasts (RM is the grand daddy 493 EDV), are doing very well. I have seen internal diagrams and tests on the ester profile of each, RM is heaviest in floral aromas, with CM ticking above (very high) RM in tropical/banana/red apple esters, but lower in floral and 'malty' esters. I'm not sure the correlate to rum that 'malty' flavors have, the charts were unfinished and used existing 'whiskey' or bourbon flavor profile descriptors. Perhaps 'molasses/buttery/caramel/brown sugar' would be the equivalent for rum.

Aside, their cachaca yeast makes a TREMENDOUSLY JUICY FRUIT rum when you follow the weird, specific hydrate and pitching directions for the yeast, in a wash of 'raw' cane sugar, the more yellow crystalized sugar you can buy. I used a wash of 1gal coconut sugar dunder (from prior washes for my coconut flower rum) to 30% turbinado sugar and 70% raw or 'organic' sugar and the distillate was amazingly fruity and vanillan, like a piece of juicy fruit gum with a slight vanilla sugar kind of flavor. Doing my first 'heavy' process all molasses rum now with the CM, and cooking this weekend.
I read, I write, I still.
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"I don't know half of you half as well as I should like; and I like less than half of you half as well as you deserve."

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Re: Esters from Lime salts - using sulfuric acid; process

Post by pope » Thu Nov 21, 2019 10:11 am

First I've heard of the CM yeast, where do you source yours? I've only been able to find lallemand's tq and rm (haven't looked for any whiskey yeasts yet).
"A little learning is a dang'rous thing; Drink deep, or taste not the Pierian spring: There shallow draughts intoxicate the brain, And drinking largely sobers us again." - Alexander Pope

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Re: Esters from Lime salts - using sulfuric acid; process

Post by distiller_dresden » Thu Nov 21, 2019 8:36 pm

Looks like they've named it CN for US; there is a location in MI you can call, setup a craft distiller account and order all kinds.
I read, I write, I still.
The must interstitial man no Earth.
"I don't know half of you half as well as I should like; and I like less than half of you half as well as you deserve."

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