“Synthetic” dunder.

[Bolverk]

There's a thread over on SD where Cotherman says he gets his sulfuric 35% from a pool supply place... I don't know if that helps you at all?

Just a thought, if storage is a problem buy in the quantity for a single use. 30ml of 98% is like $10 and is enough to treat 30g of what you have there.

Sounds like a solid plan.

Yeah thumpers, while an old technology they are really pretty special when it comes to exploiting certain inefficiencies and processes. 

Lemons are like 3.2, I think you could reasonably drop it to at least that to promote that higher acid environment after fermentation is complete. For safety sake i would test the ph of the distillate before you try tasting it thought lol

Cool, looking forward to updates

 

[Al The Chemist]

Good point! I'll check out Cotherman's thread. Apprecaite all the insight! (Update) Found 30ml of 50% Sulfuric. Will add that in. 
Haha, and I'll definitly test the Ph  

[SlickFloss]

This is 100% the best thread and conversation on this forum in the last 3 years. Thank you all. 

[Al The Chemist]

Happy to share the pains!
I'll post progress once fermentation completes. 

[Florida Cracker]

On 1/15/2024 at 11:32 AM, Bolverk said:

FC, I've read that thread at least a dozen times when I was trying to wrap my head around the whole muck pit concept. Your experiments and the comments of the others on that thread were invaluable to my current understanding.

 

On 1/15/2024 at 1:37 PM, Al The Chemist said:

FC, I recall that thread well. I was following it as it was forming. It was one of my inspirations to start this “artificial pit” as I was researching the likely bacterial infections and attempting to “cut out the middle man”. Thank you for starting that thread!
 

 

Thanks guys. Those experiments were rudimentary at best but in searching the internet now on the subject, it comes up frequently. Really glad that you both got something out of it and are now upping the game.

 

FC

[Bolverk]

Hey Al, do you have any of the butyric left?

 

Here's a really cool experiment... take like 50l of some high proof alcohol (higher the better), add like 3ml of if butyric, and slowly (carefully) add a few drops of sulfuric, and give her a stir.... keep doing that until it goes from smelling like blue cheese to fruit. Eventually it'll start to smell like a nondescript fruit candy.... it's crazy!

[Al The Chemist]

I unfortunately don’t. Though if you've added the acids to ethyl alcohol (which is likely the case) what you have there is Ethyl-Butyrate, which is a candy-like pineapple ester. Its one of the esters i hope to collect with this experiment. It's extremely volatile (vapor at 78f in its pure form) so it should be easy to collect, My worry is to maintain it and not lose it post condensation. If you have some isopropyl at hand and repeat that experiment, you'll get iso-butyrate, which is what gives the "funky Caribbean rums" their funk. 

I have to have enough iso in my wash from the backset and deep tails to get some of that in the distillate as well.
I’m a bit more doubtful I’ll be able to grab any of that though as it has a really high evaporation temp. My suspicion is that some would make it through in a very hot running pot still through pure thermos kinetics. I’m going to be running in a semi reflux configuration. So I don’t have high hopes there.

[Bolverk]

The esters "should" stick as long as you keep your proof above 95. I haven't seen the results at 2+ years though...

[Silk City Distillers]

Also keep in mind, heads cut is more of a state of mind than a manifestation of physical activity, if you get my drift.

[Al The Chemist]

For sure and noted on the heads. I'll also keep the proofing in mind. 

My current dilemma is do I use a direct pot to try and collet the heavier elements or do I do a 4 plated column to more accurately focus on the volatiles. 

[Al The Chemist]

Just added 30ml of 50% sulfuric to the wash. That would be 1.5ml sulfuric acid (at 100%) per gallon. an hour in I am not smelling any noticeable ester formation. I will check again tomorrow. 

[Bolverk]

Of the methods above, I still think the 4 plate is the way to go

You probably won't notice much until you get the acids and alcohol out of the water.

[Al The Chemist]

Thinking the same thing. Too much water to catalyze. Might do a 3-4 phase column. Though still considering putting a copper helmet in the center instead of one of the plates for more copper contact. Likely right above the first "stripping" plate.

[Bolverk]

If you're talking plate, plate, helmet, plate, plate? I don't see how it could hurt.

I don't have any experience running it that way, but it makes sense to have some sort of copper reaction chamber.

[Al The Chemist]

Yup. Exactly what I’m thinking. 

[Bolverk]

You run it yet?

[Al The Chemist]

Finishing up the run as we speak. Collecting tails. going to stop collecting at 10-15%, then combine it back with backset. 

Long Story short. It worked! Esters came out essentially in the order I expected. First cocoanut and candied pineapple, then deeper funky cheese notes. All the while a good buttery layer that really shined through as clear butterscotch in one of the cuts (I added 3ml per gallon of Lactic acid before running). 

Now that I have the general idea of how this works. There are things I would do differently. I'll post a more detailed reply shortly.

[Bolverk]

Nice! Glad to hear it worked for you too!

Good call on the lactic 

Cool, looking forward to reading it

[Al The Chemist]

OK!

So as I mentioned above, this method is 100% functional. At the end of the day, it boils down to what flavor profile you are looking for in your Rum, add the acids that create the esters you are looking for. No need to roll the dice with an open, infected fermentation that contains an unknown amount of unknown bacteria (though it does take some of the magic away  ). 

Take aways:
 

1. The Rum overall came out far too light for my liking (just a hair above neutral). After reading some old notes and doing some research I actually went for a 3 (1/2)  phase reflux. From the boiler up; Plate, Helmet, Plate, Dephleg, Condenser. This was also my first time using just Panela for my fermentation. 

Conclusion: Will try a; plate, helmet, dephleg, configuration next time. Hopefully this results in a slightly heavier product. first pate traps the initial stripping, then regulating the dephleg should churn the catalyzation in the helmet. I will also go back to either full Molasses or a Molasses Panela mix.

2. There is no need to add the acids during fermentation. All it results in is a potential for a mess and severe stink (if you use Butyric). The fermentation does not contain nearly the right conditions to start any form of serious esterification. The acidity is not low enough and the water levels are too high. I also think I might have not added enough sulfuric acid. 

conclusion: Add acids directly to the charged boiler. Even if you do add Sulfuric acid I don't think letting it sit will help any as the water levels are still too high. I added 1.5ml per gallon of sulfuric, I'd try 3ml per gallon next time. 

3. A little Butyric acid goes a LONG way.

Conclusion: I would aim for something around 6ml per gallon (I ended up with 12ml per gallon). Once the cuts rest a bit and my nose rests, I have a feeling I will get some serious ripe cheese funk in this rum (which is not all bad).

4. Ethyl-Butyrate is quite tricky to capture. I lost a bunch of it in the foreshots and it vanished almost immediately when I took a distillate sample to test for cuts. This might go back to not using enough Sulfuric acid and not forming as much Ethyl-Butyrate as I'd hoped.

5. The dephleg is super useful. At first I considered just letting everything run free, though the Dephleg really helped me balance the collection, especially as the hearts started going into the tails. That border between the 2 is where I found most of the heavier Rum notes I was looking for.

I am still looking forward to going though these cuts and seeing what I came up with.

Cheers, and thank you for all the feedback along the way!

[Bolverk]

1. Ive never been a fan of all panela rum, even double pot stilled is still way to light for my taste. The only way I've gotten the kind of heavy profile I wanted was using 40% dunder (clean stillage) in place of the water.

The 1 plate and helmet is good but I don't think that it will be enough reaction time in the column for the Fischers to really do anything. I would seriously consider a thumper if you can find a way to swing it. The esterification will be so much more intense, the product is like concentrated ester that you can then use to blend into your other rums (this was one of the real reasons for the super high ester rums in the first place). 

2. No, definitely add them after primary fermentation is complete.  I was honestly surprised your fermentation finished at all. All those acids add a tremendous amount of VA to the wash that will hinder a healthy fermentation... ask me how I know 😂

3. Haha yes it does 

4. By running a thumper with bypass valves it would allow you to take of your fores/heads before installing the vapor into the thumper so you maximize the amount of butyric esters carrying over into your desired cuts

5. Can't speak to the use of the dephleg,  I'm glad it worked though. 

Looking forward to your tasting notes.

 

[Al The Chemist]

Yeah, the issue might be the Panela. Fermentation went off without a hitch. 1.098 to 0.997 in 8 days.

My concern about this process though is its effect on the dunder. My dudner is now acid loaded (the butyric is definitely still in there). So unless you start this process fresh every time, there will always be the issue of acid transfer through added dunder. At that point it will be hard to judge how much there is of what in there.

The more I tinker with Rum the more I’m getting the feeling that a thumper is the way to go. I initially thought the plates would do the same general job if all the source material is already in the boiler, but that does not seem to be the case.
I did get some strong esterification to make a spirit with a very distinct flavor. But I would by no means say that It’s so strong I can use it as a flavor blender for “softer” Rums.

A traditional thumper (sitting on the side) would be tricky for me to adopt considering how I have things configured. I’ve been playing with a design for a thumper that sits vertically on a column stack. I haven’t seen anything like that commercially available, which makes me think there is something about a thumper that I just don’t understand, or this would be more widely available. Maybe sonething to do with the more direct heat transfer? 

I’d be curious to hear your thoughts.

The way I see it, It can be a single “over gown”, tall, single bubbler setup, encased in a Xgallon container, with a port to charge it and a valve to clear it. Maybe an overflow line that at a specific charge height funnels the liquid back to the stack under it. 

[Bolverk]

Wow surprising it went completely dry..

Yeah, you're almost going to need new dunder and you can slowly feed this back into the boiler when you do your runs to recover some of the flavor. 

My understanding of the Hampden process is that they add 10% of their wash volume in muck right before distillation, but of that 10%, I can't imagine it being more than 3-4% acid.

Smaug (Larry w/stilldragon) can probably get you a vertical thumper. Go search HD and/or SD for mention of the vertical thumper and the "humper thumper". I've seen some of his cad drawings of the professional ones floating around, i just don't know if its OK to repost them.

Yes, it's definitely more heat efficient to go vertical, it's talked about a bit in some of the 3 chamber threads (basically 3 thumpers stacked on top of each other).

Oh, if you start digging into the 3 chamber still... let me apologize now, it will become an addiction/new habit hole... that thing is fascinating.

[Al The Chemist]

I'm psyched to hear this has been discussed. I've wanted to have one made for a few years now. Thank you for the new rabbit hole!

[Al The Chemist]

Yup, from what I'm reading, thats essentially the same design I had in mind. @Bolverk, what are your thoughts on using 1 vs 2 thumpers? 

[Bolverk]

If you want to go all in on rum and make traditional high ester, then yes its a no brainer... you need them both.

(You could do a small pilot sized double retort because if done to its extreme, you can make a 6000 g/hl aa ester rum for blending, this is so concentrated you won't need much of it to blend back to your normal stock)

It requires some fanagling, but you can get something resembling a Caribbean rum with a single thumper/retort though.