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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.

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.

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

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!

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.

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).

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.

This had been my favorite thread for a while now. I wouldn't mind resurrecting it.
Dresden, thanks for getting me onto doing acid base reactions!

At work I was trying to get the taste of a blueberry (bb) into a blueberry fermented vodka which isn't easy since the bb flavour is acidity first, and a subtle glycoside second. Not much aroma or volatile odor to speak of.

I figured out the sugar part and tried simulating the acidity profile of the bb by combining citric, malic and tartaric acids but the acidity was so rough and didn't taste natural.

So I took the stillage of the first distillation (continuous distillation so there were no carmelized sugars and heat degraded molecules) and cleared the proteins and crap with bentonite. Then I dumped in CaOH (Calcium hydroxide) and all the organic acids crystalized and settled quickly. Stillage is nearly always acidic so I use enough CaOH to bring the ph to 7. If I overshoot there will be unreacted CaOH, which is no big deal. 7.5ph is fine as mentioned earlier in this thread.

I racked the Calcium citrate, calcium malate and calcium tartrate crystals and washed several times using cold tap water (tap is cheaper but RO or distilled may be better). Ethanol might be better in terms of solubility but its too wasteful. Once the water is clearish and tastes less of fusels and minerals and crap I decant a last time.

Then sometimes I will dry the crystals so I can weigh them. They are not pure white, there are organics (tannins and pigments?) that get caught up in the process. Then I use a distilled water diluted acid (stronger than citric/malic/tartaric) to grab the calcium which puts the organic acids back into solution. I've tried this with Phosphoric acid and "Formul-a-cid" a combo of Phosphoric and Nitric acid. I just found some sulphuric acid but havent tried yet. When I check the "solubility rules" it looks like phosphoric and sulphuric are better as their calcium salts are less soluble than Calcium nitrate, allowing a cleaner "handoff" of the calcium unto the solids.

The salts turned reddish once acidified and I titrate down to 1ph This part is difficult to manage mathematically (help from chemists would be great). I go by taste here, titrating and tasting less and less calcium, more and more citric acid but stopping before I can taste nitric/phosphoric acid which signifies that acid is in excess.

Then I settle out the precipitate and rack nd keep the liquid. It may be possible here to use activated carbon to decolor the liquid and dry it to achieve white crystals but generally I just add the liquid to my liquor. as long my acid is diluted the same percentage, the organic acids should be the same percentage of the liquid, allowing consistent blending.

When I taste the organic acid liquid, my brain identifies blueberry, and that is the truest test.

Thanks again Dresden. I'm super into doping for ester generation, working on a rum, which is how I found this thread.

Have you looked at trying to degrade carotenoids to produce rose ketones (damascenones etc) aka rum oil?

So I'm curious, are you guys actually using sulphuric acid, and if so where are you getting it?

From my understanding it can be extracted from drain cleaner by distillation, or reaction with peroxide. Neither easy.

Expat wrote: ↑Tue Oct 27, 2020 6:16 pm So I'm curious, are you guys actually using sulphuric acid, and if so where are you getting it?

Here’s one source: https://www.coleparmer.com/i/reagents-s ... Y7EALw_wcB

Larger quantities are available at chemical supply companies.
ss

Or here: https://www.dudadiesel.com/choose_item.php?id=sa950

For some uses I've used straight drain cleaner, check your MDS/MSDS, the ones that only have sulfuric and "buffers" are generally useful enough, but certainly not anything remotely like "food grade". But for general playing with chemistry, no need to distill it.

If you just need a little bit dilute, every car part store in the world sells sulfuric acid for batteries, 15% I think? Again, check the MDS/MSDS to make sure it's just sulfuric, but it probably is just straight tech grade diluted sulfuric. It's dilute, but much cleaner than drain cleaner.

I wouldn’t use battery acid or drain cleaner. Lab grade recommended:
Hach 93153 Sulfuric Acid Standard Solution, 10 N, 1 L

That's cool, I respect that. But having worked in labs, just "lab grade" literally means "not pure enough for food, drugs or analytical chemistry". ACS is probably a reasonable standardized grade often used as an entry level "food grade" and is readily available in the states. Now that you've pressed me it is hard to defend anything less for people that can obtain it, it's available from www.carolina.com for as little as $6!

But many people live in places where pure chemicals are difficult to obtain. I'm personally spoiled living in the states, but my global friends shake their head in wonder (and envy?) at all the things we can just buy anonymously for no good reason. That is the main reason I mentioned battery acid. The stuff I have used is amazingly clean compared to drain cleaner, none of the oxidized organic char, MDS lists only sulfuric and distilled water FWIW. It's perfectly capable of making beautiful textbook crystals of various sulfate salts, and is likely just a diluted version of a random no analysis, non-standardized "lab grade". And it's available around the world. Without an analysis sheet it may or may not be safe. It may or may not also be from the exact same source that a commercial rum distillery would buy from. After all, not even their molasses is food grade

In Aussie I’ve had no trouble just getting a small 1litre bottle from the local chemical supply shop in town .

I would caution against suggesting battery acid . I know we are generally a smart bunch here , but I would hate to think of Dick heads thinking its OK to pour a bit out their car battery , Lead loaded and all .

I’d also add caution when using Sulphuric acid . In its concentrated form ( what you would get from a Chem supplier) , it is 98% ( around 18mol/L ) .

It is much more dangerous than concentrated Hydrochloric acid which is generally sold @ around 32% strength .

Always remember when dilution to Add Acid . Never the other way as it will explode in your face .

Also be aware that a damp cloth used to wipe up a concentrated H2SO4 spill will likely spontaneously catch fire .

Safety rant over .... as you were.

+1 ; Yummyrum safety is not a rant. I would like to add that much earlier in this thread

it is instructed to sniff your concoction after adding acid. DO NOT just stick your nose in

the jug and take a whiff. if you made some miscalculation you could permanently damage

your nose. Use extreme caution and safety protocols with concentrated acids and catch

your whiffs form a safe distance.

Sooner or later this whole thing will end with some fool getting hurt imo.

Saltbush Bill wrote: ↑Wed Oct 28, 2020 1:14 pm Sooner or later this whole thing will end with some fool getting hurt imo.

Likely, but ya can't fix all of the stupid, just look at the "nuclear whisky" thread....

Sometimes We just have cross our fingers and listen for the explosion in the distance

Lol. I’ll experiment with some sulphuric acid in the low wines with infected backset but forget about nuking a jar full of barrel strength! Gotta draw the line somewhere....

The 10 N solution is about 40% so be safe!

Cheers,
Jonny

I have sourced sulfuric acid from garages that do batteries, particularly motorcycle garages, I hear swimming pool supply houses are another option. I found a full plastic container here at work recently - definitely pro chemical supply. The thing weighed half again as much as water!

I've used H2SO4 for rum for over thirty years. It's dangerous if it's miss-handled, so do your research and wear the recommended PPE when using it.

Just because it is also used for lead acid batteries, doesn't mean that what you bought was used in a battery

Yea this stuff is super dangerous if you don't handle it right; make sure you handle it right! Besides PPE, proper storage should be in a chemical cabinet with non-reactive coinhabitants.

That said I got mine in the US from Duda Diesel/Duda Energy. 98% pure, add it to water to dilute to a useful strength so you can measure out what you need to add to your batch. Even a small quantity should last a hobbyist a lifetime. I've spent way more money on way less useful stuff.