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Making Vodka

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  • Back when I was into big reef aquariums, it was common to use over the counter washing soda as part the dosing required to keep the chemistry right. Inevitably someone would pick up a box of washing soda that would contain other "Laundry Boosters" that would be certain doom for the tank. I've seen it with fragrance, surfactants, and other chemicals. I suppose if it contained a surfactant, it would cause it to foam pretty easily.

  • Also. Should I allow it to interact with the low wines for a bit (24hr) then transfer to the kettle and distill, or should I distill with the Na2CO3 added directly to the kettle? Or both?

  • By low wines you guys are talking about first strip runs that have been cut back to 20 to 30abv... Not a wash... only product that has been distilled at least once...?

  • I have read using any of these in a wash prove ineffective or will cause the copper in the column to corrode or scale up at a very high rate... along with green or blue distillate being possible...

    Just making sure all you guys are on the same page...

    Chapter 37 verse 2 Smaug's Rulez and Regulations

  • @FullySilenced said: By low wines you guys are talking about first strip runs that have been cut back to 20 to 30abv... Not a wash... only product that has been distilled at least once...?

    That is correct. The bad interaction with copper is if you add it to the wash, not the strip.

  • @grim said: Did you use a box of washing soda from the grocery?

    Yes. It was a box of baking soda that I heated to 400 degrees for 45 minutes. The process is supposed to convert the sodium bicarbonate into sodium carbonate which is what I understood to be what we want. Arm & Hammer. Don't think there was anything in there other than soda. I know there weren't any fragrances. I just started another neutral wash today and I will not be using the stuff again.

  • edited October 2015

    I did my own test. Did a strip run in June of raw sugar wash, diluted it to 30%ABV and added 1 gram per litre of Arm and Hammer. I left it in the shed until last week, about 4 months all up, then I ran it through the big column. Before I added the soda the strip had the usual strip smell, a mix of heads, fores, hearts and tails, but when I took the lid off the drum after 4 months that strip smell wasn't there, it smelled a lot cleaner. I had less fores and heads, no odd taste in the hearts and I got more than I expected to get and no coloured tinge, but a larger than usual amount of tails. It didn't foam during the run but when I poured it into the boiler it looked like a suds laden washing machine. So something happened some where. I will do this to every neutral strip I do from now on. I have about 160 litres in the shed that I added the soda to about 2 months ago.

    Edit. I will ferment another neutral batch tonight, take a sample, strip it and take a sample, add the soda take a sample after 4 months, distil it and take a sample and get the whole lot put through the HPLC and see what the difference is.

  • Doesn't hurt to try different things but I don't think the reaction takes very long.
    I just did straight bi-carb with no pre-treat. Add few spoons in 30% low wines the night before with lots of agitation then run the next day.
    You won't get more than a few spoons to dissolve anyway.
    Seemed to clean things up a bit for me.

  • edited October 2015

    You guys have pH meters? Test strips? I'm still wondering if the right approach here is to target a specific pH, and not that it's based on a general weight per volume liquid.

  • edited October 2015

    Check the pH of the alcohol you mean? Never done it. What is the pH of alcohol anyway? pH of the stripped run?

  • edited October 2015

    Yah, we're talking esterification of the typical carboxylic acids (or rather in this case, hydrolysis). It's the exact opposite of what Arroyo recommends to increase esters (to keep this thread linked to the rum thread). With rum, add an acid, increase the esters. With neutral, add a base, decrease the esters. The reaction itself is reversible, and runs on a continuum, so theoretically you can increase or decrease the resulting esters.

    You'd probably get similar results using other food grade bases like lime or lye (sodium hydroxide or calcium hydroxide). Probably need to use a whole lot less of it too.

    I know the recommendation somewhere always used to be one teaspoon per liter, but that sounds like an astronomical amount to me. Way more than could possibly be needed. Or, if that much actually is needed, than it makes more sense to use sodium hydroxide, because the change in pH will be much greater with smaller amounts needed.

  • A pH of 8 or 9 pH was recommended on the previous page.
    What pH is a saturated solution of Bicarbonate Soda?
    It's cheap as, just put enough in so that it is a saturated solution (so there's a tiny bit left over that won't dissolve)
    It would be cool to hear about any other methods getting good results too but this one's pretty cheap and simple. No testing needed.

  • I added one tablespoon per gallon of strip. Made a huge difference in smell. Wish I could get this figured out, just don't want to ruin another 6 gallons of strip to do it. I have 1 gallon of neutral from the last run (already cut to 40%) that I will toss into the next run. That spirit STILL has a bad taste/smell and has been run 3 times already. Wife says "You are making awesome rum, why can't you make a decent vodka for me"? She mixes it so a good, clean neutral works for her. I definitely took a step in the wrong direction last run. By all accounts, it should have been a lot better.

    Still not sure where I fucked it up..........

  • More plates will fix everything :D

  • edited October 2015

    Lets get crazy here guys, if we're locked in the embrace of an arms race of plates and chemical warfare, I'll drop the nuclear bomb.

    Antibiotics.

    Kaboom.

    We are screwing with reducing the carboxylic acids and esters that are likely the result of other bacteria in the wash, since we're not in any way near aseptic/sterile.

    Large scale ethanol manufacturers will use antibiotics to sterilize a mash, increase yield, reduce congeners.

    I'm not going to condone it, because personally I believe antibiotic overuse is a huge problem.

    BUT. If we're going with the nuclear option, there is a reason why so many big manufacturers are doing it. It works. No, it really really works.

    Bugs in the System - How the FDA Fails to Regulate Antibiotics in Ethanol Production (PDF)

    Fueling Resistance? Antibiotics in Ethanol Production (PDF)

    Lactoside 247™ @ Lallemand Biofuels & Distilled Spirits

    (Lallemand has a smorgasbord of fermentation antibiotics)

    Just saying... if super clean neutral is your game... We are talking about chemical approaches to addressing a symptom of another problem. Why not address the problem?

  • edited October 2015

    And an approach that used non-antibiotic PAA and Hydrogen Peroxide:

    Controlling Bacteria During Corn Mash Fermentation @ Ethanol Producer Magazine

    Using hop acids as antibacterials (most guys here would probably be OK with this approach, you know, given... BEER):

    Hop acids as natural antibacterials can efficiently replace antibiotics in ethanol production (PDF)

    Optimizing Bioethanol Fermentation by Inhibiting Bacteria without Antibiotics (PDF)

  • Never add it to a wash from what i read.... only to the strips or high wines..... etc.

  • edited October 2015

    I can probably get some isostab if you guys in the states want to try it out. I can see what the minimum is and then subdivide it into smaller quantities.

  • I have a digital pH meter. I'm going to measure the pH before and after. I'll report back with quantities, observations, etc.

    Is 7.0 the target to push the esterification process in the reverse direction?

  • I tried adding arm & hammer to a spirit run, probably about 35 gallons or so after watering it back to 30%, I added about 3oz of the washing powder to the boiler and gave it a good stir. The powder appeared to be fully dissolved and I let it set overnight. Ran it the next day and the consensus by my normal tasters was that it was cleaner and smoother with the arm & hammer addition. One unusual observation was a white foamy lather, coating the inside of the boiler,. I will definitely try this again

  • I read that the longer you let it rest after adding to a low wines or strip the better it seems to work.. i have left mine for up to a week... the longer you are able to let it rest i think the better up to a production point...

    happy stillin,

    FS

  • Interesting thought. Let's throw in some phage too.

  • @bachman said: I tried adding arm & hammer to a spirit run, probably about 35 gallons or so after watering it back to 30%, I added about 3oz of the washing powder to the boiler and gave it a good stir. The powder appeared to be fully dissolved and I let it set overnight. Ran it the next day and the consensus by my normal tasters was that it was cleaner and smoother with the arm & hammer addition. One unusual observation was a white foamy lather, coating the inside of the boiler,. I will definitely try this again

    My observations too. But i let mine sit for 4 months. My best production yet according to the vodka drinkers.

  • edited October 2015

    I use this brand soda wash, 100% sodium carbonate. I don't bother with Bi-Carb anymore. I add one teaspoon per liter of low wines. Cleans up the low wines immediately. I have never had a problem with foam or bad smells. The treated low wines runs thru the still a little differently than un-treated low wines. Ie. It's easier to pick end of heads, the abv remains constant throughout the entire run until tails arrive which is very evident when it happens, there are very little tails and I believe the end product is cleaner.
    I've been doing this since I read FS's post back on page 3 of this thread. Thanks again FS, works great!! My last few runs have definitely been smoother.

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  • Posted two papers in the rum dunder thread that are applicable here. They list some interesting pH ranges, and it seems that one doesn't need to go all the way to pH 7 to reduce potential ester formation. The impact of moving from 3 to 4.5 shows a marked reduction in acids and esters in the distillate.

    I'll run a trial when I get around to it, but there should be ABSOLUTELY POSITIVE BENEFIT in adjusting the final MASH ph to around 5-5.5 or so prior to first distillation if your goal is neutral.

    Yes, mash, first distillation, not low wines. I am not talking about raising the alkalinity to absurd levels, I'm talking about slightly reducing the acidity of the mash.

    Cue blue-tinged screams of heresy.

  • @grim I ferment all my neutral mashes at pH 3.3, and thats where I strip at. I will adjust to ph5 for the next strip. Is there a time that the wash should sit at 5 before stripping?

  • Wouldn't wait at all, by moving it to 5 you are going to create a happy place for other bacteria.

  • Speaking of making Vodka, I just got 2 of these on eBay for $50, "millipore KVGLA04TT3 " 0.22 micron... will circulate the bottling tank using it...can't wait for the next batch to bottle!

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