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.

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.

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.

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.

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

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

Appreciate the link! At this point I dont have the facilities to safely handle or store sulfuric acid at those concentrations. I’m going to go out on a theoretical limb. Reading more it seems like the main contribution of the Sulfuric acid is to create a more hydrophobic environment for the esters to form in a high water content wash. Considering I can't currently use sulfuric. I’m going to experiment with this as follows (and will let you know how it goes): @Bolverk, I’ll use your still configuration only to replace the 2nd form the bottom plate with a helmet. The first plate interaction should already bring the “low wines” on that plate to 45-60% abv. I’ll rely on the hope that the sheer thermo-kinetic energy coming out of the boiler pushes though some of the heavier desired compounds into the column. Once they are there, the environment is already going to be lower in water and will hopefully promote some esterification. As you recommended, I will run hard with little reflux to pull out heads, then let the system churn in full reflux (again, hoping the desired, heavier compounds are lifted, at least, into the first plate). From there the large copper surface contact and the lower water environment should help esterification in the column, rather than the wash. I can see how esterification in the wash/thumper is a lot more effective as the esters are very volatile and I’d likely be pulling a lot more of them into the system during the boil. My wash was at 3.8 Ph before buffering to 4.75 with Calcium Carbonate, so the acid potential is high. I’ll probably do an additional acid add once fermentation is complete. Open to any other ideas. Wish me luck! 😀

What concentration of sulfuric do you use? I can source roughly 5%. But that’s still technically considered hazmat and I’d like to save the backset as dunder. With any significant concentration of sulfuric that worries me. I’ll try the single run. That makes sense.

The plan was to indeed strip then do a pot configuration cuts run. It’s a lot of added work I’d be happy to avoid. You believe a 4 plate run should be more successful? I was planning on trying on copper contact as a partial catalyst (the plates would provide some, the helmet was new at to be the main contact point). Would be great to avoid using sulfuric (it’s a nasty acid, storage song would be a worry), though if you guys haven’t had much luck with copper as a main catalyst. I might give it a go.

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! As it stands. I’m at about 12ml of Butyric per gallon. I am already starting to smell the iso-butyrate in the ferment. Still no ethyl-butyrate, though fermentation is really early. The wash also has additions of lactic, acetic, and malic. If I can detect any of the butyrates I’ll assume the other are also catalyzing. I looked loosely into the chemistry of sulfuric as a catalyzer and it looks like the acidity itself is a pretty significant factor. I’ll dig in a bit more. as for the stripping configuration. You guys recommend running the stripping in a full 6 plated reflux? I worry that will strip things down too much even if I run it hard to tails. that’s why I landed more on the helmet + 2 plate + dephleg to push for Fischer esterification after I dispose of foreshore. The bottom plate (pre helmet) should help with water reduction and the plate above the helmet plus the dephleg should add a “capture chamber” and control reflux. the helmet itself should provide a good catalyst chamber. what do you think?

I hear ya. I'll give it a go and post how things turn out. Appreciate all teh advice! the "right to left" factor of the equasion might indeed be an issue. after some adjustmetns. I'm at about 80ml Butyric per 5 gal (X2).

That makes sense. Also, 1.5ml of Byteric acid to 2.5g makes a lot more sense than what I did. The puke smell is still quite rough on a 10 gal wash. I unfortunately don't have a thumper. I plan on running a stripping run deep into the tails using a freshly passivated copper helmet with one copper plate in it. on top of that nother chamber with a copper plate (replacing the traditional copper lentil) then a dephleg to push for longer churn and contact times with the catalyzing elements. I'm going to throw a passivated copper mesh into the boiler itself as well. I'm hoping that the heat along with the reactive copper will provide enough of a catalyzing element to constitute the esters. I am actually not super interested in Isopropyl-butyrate rather more going for the ethyl-butyrate. I'm hoping some of that forms during fermentation as the ethyl alcohols are formed. Once the stripping run is done, I plan to run a helmet + plate on the stripped run to make cuts. I do have a test still, though its unfortunately not copper. Do you find sulfuric acid reduces the puke factor?

I mixed the acids with deep tails and backset (my attempt to make a non-infected muck pit). Running a test run with this at 2 gallons "muck" in a 10 gallon wash. The Butyric acid is still very dominant in the smell, hence my concern about going overboard. I couldn't find any reference to ratio so I just took a stab. Wash Ph was 3.8 (whcih is odd because it was the Ph of my "muck") having a hard time adjusting to 5.0 with Calcium Carbonate. Sugar source is Panela.

@Bolverk, you were not kidding! 3 drops of this stuff can take down a squre block! Dealing with it felt like handling explosives. I ended up with 20ml Butyric acid per gallon in my wash, I have a feeling I've over done it. Any thoughts?

I'll considering trying the bacterial route again. Appreciate the info and the warnings!

I hear you on the cost. I was pretty floored as I was looking around. I can definitely produce them myself. Though I’ve found that bacterial infections can quickly get out of hand and I’ve had some mishaps with unintended cross contaminations even with pretty strict hygiene protocols. That’s why I’m trying to skip the troublesome middle man. It’s good to hear I’m not missing anything by not finding food grade products. Appreciate the info!

I’m experimenting with making a dunder that contains backsets and a balanced/controlled introduction of selected acids. My hope is to remove the more chaotic bacterial infection factor from the dunder acid production process. This should also help control Ph and flavor profile as I know exactly which acids are going to potentially transform into which esters during esterification. I was wondering if anyone has experience sourcing and handling Butyric acid. I'd like to add it to my dunder to create ethyl butyrate (that funky pineapple note). Though I can only find products that are not rated as food grade (even though they are pure Butyric acid). Any thoughts about the safety and risk of using them?

Figured out the issue. The internal tight spaces of the bubbler cups were retaining gunk and spilling it out after cleaning when the plates were drying (even after a thorough wash). Disassembling the plates and acid washing the parts did the trick.

I can't for the life of me get my copper plates clean. This is after 2 x 30 minute soaks in citric acid. First soaking the plates looked pretty good (not shiny all the way, but at least not darkened). I rinsed off with hot water and let it air dry. It darkened like the picture above. Plates have a mixed-nuts-like metallic stink that sticks to your fingers. Second soaking I left for 30 minutes then pasisvated with sodium carbonate (just in case the copper was left to reactive and was reacting with the air). Still no go, the result was the pic above. (funny to see I started this thread and still having the same issues 6 years later! :D) Any ideas?

Hey Denver Distiller, I'm planning on using a citric acid rinse to passivate my copper helmet. Would you think it will suffice to give it a good warm tap water rinse without running a sacrificial run? Cheers.

@DrDistillation Thanks for the tips. I did bring the spirit down to 80 proof and let is rest. It did improve the issue somewhat, but not to the extent I would hope. Question about the glycerin. Is the goal added body (mouth feel viscosity) or to add sweetness? The spirit has quite a bit of body from the tannin in the barrel. @bluestar, apologies for the lack of terminology accuracy. I'd be happy to dial in on the difference for future. What are you referring to by heat? From what you're saying, I'm referring to alcohol burn. As for proof, I tried it at both 110 and 80 proof. The 80 proof was more palatable. Though the rum was FAR less "notably alcoholic" going into the barrel. And there was very little difference in abv.

My reference to hotter is the feel of alcohol burn in the mouth and throat. Adds to the opposite of smooth :) oddly this is exactly the profile I was expecting the barrel to mellow out. The oak has to be quite dense. Flavor on the rum is great. Like an good aged whisky with rum overtones. Nice and heavy, full of flavor. Wish it was more palatable. Blending is definitely an option.

@kleclerc77 I am as well, there was surprisingly little loss. @DrDistillation, I've only considered the blending option. I'll give the others a go. Very helpful, thanks! On the bright side, there is so much caramel/vanilla in this batch, it will likely make a great blender. Do you by any chance know what compound creates the "heat"?

Barrel was a 4 out of 10 (1 being neutral 10 being charred to a crisp). Rum went in at ~55% and is now 57%. Odd, I was expecting the alcohol level to go down.

The ambient temperature of the room I store the barrel is a bit warm. Around a pretty stable 70, which I understand is not ideal. That sux to hear. I was hoping that more time will result in a better aging, smoother pallet. How are the longer aged Rums done, X.O.s and the likes? A more depleted barrel, less charring? Is there anything I can do to save it? Or am I looking at a 2 Y.O. neutral spirit in the making.