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Making Vodka

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  • So the baking soda plain is the one that works fastest? Could have sworn it was the other way around but obviously I fuked something up. Thanks. It changed the smell of the strip immediately.

  • edited August 2015

    Sodium Carbonate = soda ash Na2CO3.

    Sodium bicarbonate (sodium hydrogen carbonate) = baking soda NaHCO3

    Baking powder is a blend of NaHCO3 and crystalline acids (monocalcium phosphate and sodium aluminum sulfate). When heated the mixture reacts and the acid-base reaction evolves carbon dioxide, providing a non-yeast leavening agent.

    I'm more like I am now than I was before.

  • I guess I will let this strip calm down for a while and then try and run it again.

  • edited August 2015

    General Chemistry Online: FAQ: Introduction to inorganic chemistry: What happens when sodium bicarbonate is heated?

    So you baked the strong arm (NaHCO3) to try convert it to Na2CO3?
    I think it needs water too, it starts breaking down at around 80°.
    You should get a copy of Riku's ARC book. The why's and how's are all spelled out in there in appendix 4.
    You also need to make sure the original wash was quite acidic (below 6pH) when you stripped it.
    The impression I got was that it was purely for increased yield and if your still isn't good enough to strip out the ethyl acetate out.
    He's done the work and its a good reference book to have on the shelf if you're after a bit more than just the basics.

  • @jacksonbrown said: General Chemistry Online: FAQ: Introduction to inorganic chemistry: What happens when sodium bicarbonate is heated?

    So you baked the strong arm (NaHCO3) to try convert it to Na2CO3?
    I think it needs water too, it starts breaking down at around 80° .
    You should get a copy of Riku's ARC book. The why's and how's are all spelled out in there in appendix 4. You also need to make sure the original wash was quite acidic (below 6pH) when you stripped it.
    The impression I got was that it was purely for increased yield and if your still isn't good enough to strip out the ethyl acetate out.
    He's done the work and its a good reference book to have on the shelf if you're after a bit more than just the basics.

    I never do anything to increase yield. If anything I strive to DECREASE it if I think it will improve the spirit. I pitch spirit that is way into the hearts to make sure that all heads are gone and on neutrals I stop collecting as soon as the abv starts dropping. Earlier in this thread it was posted that the addition of (fill in the blank) helped bind up some nasties and keep them from coming through the still. I immediately noticed that after adding the (whatever the fuck I had made) the strip had lost any smell which I considered to be a good thing.

    Oh, and the problem wasn't with the still at all; it was totally the guy operating it. The still is quite qualified.

    The guy? Up for debate.

  • I didn't read the whole thread just then so sorry if I missed some important info.
    If it made a big difference it kinda sounds like you used to have a lot of ethyl acetate coming through, even with your brutal cuts (its' BP is only 1° off ethanol's so you need a lot of plates to separate them).
    From what I remember the procedure works by converting the high levels of ethyl acetate into ethanol. It could be the operator like you suggest but in my experience, when you have enough plates (theoretical or actual) it's really quite hard to stuff up neutral.
    Just reflux for an hour and take off slow. Do those two things through enough plates and the cuts will be so obvious that literally anyone can do it.
    This is why the tool I use for neutral is a packed column. Flutes are fantastic as a consistent, de-tuned column for flavored spirit but for making small scale neutral there are much better options IMO.
    Are you running 30+ plates? I can easily do that in under a meter of packed column. Not SD bashing, just suggesting a few more plates or some quality packing might make all the difference.

    You need an efficient column to make neutral and under ten plates just doesn't cut it IMO.
    With enough plates there won't be much point saving heads and tails either because they're already so concentrated and there's also no issue using turbo's either because the nastys are where they're meant to be, in the heads and tails.

    The reason to do the NaHCO3 thing is convert some of the heads into hearts.
    I could well be off the mark with all that but it's the conclusion I came to after many years testing and reading.

  • still seems easier to just raise the pH with food grade lye instead.

  • edited August 2015

    I save my NaOH for making pretzels and bagels and soap. I use 8N KOH for pH control.

    +1 What JB said about neutral production. It's hard to beat a packed column for nice sharp cuts. My VM column runs itself over in the corner of the shed while I brew and/or grill on the other side of the shed. It really has become an automatic azeotrope machine. Once you get the routine down you can make the cuts pretty much by volume. (although I still use my thermometers as a backup) I don't bother with a parrot on my column. It's so boringly steady, spiders build webs on it during the run.

    P.S.
    NaOH and KOH are extra nasty stuff. PPE is a must when working with them. One boo boo and your eyes are fucked for good.

    I'm more like I am now than I was before.

  • I use just limewater for raising pH. It's strong enough to work but not so strong that I feel I'm working with nuclear waste.
    Make up a saturated solution of slaked lime and water in a drum then just take from the top and top up as necessary.

    Just adding on from the ethyl acetate thing.
    I think it was Edwin that dug up some interesting info a while back about removing it with distillation.

    I think it had to do with its boiling point changing at different concentrations with ethanol and strange azeotropes forming in specific areas of the column.
    I didn’t fully understand it at the time but the gist was that under certain conditions it could get trapped in the column and build up there , possibly over flowing out the take off later in the run, instead of coming off with the heads.

    At the time I couldn’t think of a decent way of dealing with it so I didn’t worry about it.
    Maybe converting it in the low wines is the key there?

  • edited August 2015

    This impacts all esterification. It's the opposite of the recommendation in the Arroyo patent (adding a mineral acid to increase the production of heavier rum esters).

  • edited August 2015

    I see no reason why this would work only with low wines and not a wash, the chemistry is applicable to both, heck, you could do it in both if you really wanted to (would you hit diminishing returns? who knows).

    If you believe that the mechanism driving the esterification during distillation is the Fischer Spier reaction:

    Fischer esterification or Fischer–Speier esterification is a special type of esterification by refluxing a carboxylic acid and an alcohol in the presence of an acid catalyst.

    As applicable to distillation, I'll reference back to the oldest case I can find that references this particular reaction, the Arroyo heavy rum patent. Remember, Arroyo wanted to INCREASE, as much as possible, the esters in the final product, unlike this scenario, where we wish to REDUCE as much as possible:

    At the beginning of the evaporation, the ascending alcoholic vapors are totally refluxed back to the column, for a time which is determined largely by the particular characteristics which it is desired to impart to the end product; it has been found that 1 to 2 hours of refluxing is appropriate in most cases. This refluxing increases the esterification...

    Or just watch this:

    https://www.youtube.com/watch?v=ewnJXhPO26k

  • edited August 2015

    If you are wondering where the reactants are coming from in the reaction described in the video.

    The carboxylic acids come from the yeast and bacteria (Acetic Acid, Propionic Acid).

    The alcohols described in the video are common fusels, byproduct of fermentation: Isopentyl Alcohol (aka Isoamyl) and Isobutyl alcohol.

    They are essentially replicating the conditions under which the primary rum esters could be generated during distillation.

    At 2:00 you'll see them describe what happens when Sodium Bicarbonate is added.

  • edited August 2015

    The last piece is, if you believe the above, extended/long reflux periods for neutral could potentially be a negative, and not a positive, since you would be creating an environment that favors increased esterification.

  • @grim said: I see no reason why this would work only with low wines and not a wash, the chemistry is applicable to both, heck, you could do it in both if you really wanted to (would you hit diminishing returns? who knows).

    If you believe that the mechanism driving the esterification during distillation is the Fischer Spier reaction:

    Fischer esterification or Fischer–Speier esterification is a special type of esterification by refluxing a carboxylic acid and an alcohol in the presence of an acid catalyst.

    As applicable to distillation, I'll reference back to the oldest case I can find that references this particular reaction, the Arroyo heavy rum patent. Remember, Arroyo wanted to INCREASE, as much as possible, the esters in the final product, unlike this scenario, where we wish to REDUCE as much as possible:

    At the beginning of the evaporation, the ascending alcoholic vapors are totally refluxed back to the column, for a time which is determined largely by the particular characteristics which it is desired to impart to the end product; it has been found that 1 to 2 hours of refluxing is appropriate in most cases. This refluxing increases the esterification...

    Or just watch this:

    https://www.youtube.com/watch?v=ewnJXhPO26k

    I haven't ever had a problem with my neutrals, but I am always looking for ways to improve what I am making. After the stripping run, the low wines had a slight yeast smell because the wash hadn't completely cleared . I added the "sodium carbonate" and after stirring it in I could not smell the yeast anymore. It definitely did _ something._

    For a neutral I am running 4 plates with 4 procaps and a 5" bubble tee about 3/4 full of packing. If I could find a fucking source for the correct SPP I would load up a tee with those but I can't seem to find any. Guess I will have to make my own. I am using the bubble tee because SD didn't have any 5" straight pipe.

    Grim, I had heard that adding this stuff to the WASH could have a bad reaction with the copper and cause a blue spirit. Also, I thought that I should avoid a long reflux to avoid esterfication in the column. Just the opposite of Arroyo=less flavor.

    The puzzling part about this is that I didn't have any bubbles until about half way through the run and then it was not possible to continue. I haven't ever had a problem with a spirit run and had no idea that pH was a consideration. What is a perfect pH for a spirit run?

  • edited August 2015

    Reaction of a carboxylic acid and sodium hydroxide (lye):

    RCOOH + NaOH(aq) → RCOO−Na+(aq) + H2O

    Reaction of a carboxylic acid and sodium bicarbonate (baking soda):

    RCOOH + Na2CO3(aq) → 2RCOO-Na(aq) + H2O + CO2(g)

    Reaction of a carboxylic acid and sodium carbonate (washing soda):

    RCOOH + NaHCO3(aq) → RCOO-Na(aq) + H2O + CO2(g)

    (Florida - the third equation may show your bubbles - was your sodium carbonate added as a liquid solution and thoroughly mixed in, or was it added as powder).

  • As powder and then stirred. Might have been some residue or un dissolved stuff at the bottom

  • edited August 2015

    @FloridaCracker said: What is a perfect pH for a spirit run?

    No clue, but it's a continuum, and any prescribed additions are going to need to be based on the specific wash/wines being treated. I don't posit to know what the right amount is, but if someone tells you one and a half tablespoons is always the correct number, I'd be a skeptic. It might work just fine, it might not, but the amount required is always going to differ.

    I suggested pH because it's measurable and repeatable. If you find that using NaOH or Bicarb to adjust the pH up to 6.1 makes a nice drink, you can repeat that every time.

  • edited August 2015

    There was an old recommendation from @Harry to not go over pH 7, and I recall something from Pint saying approximately the same. Keep in mind the other side of the blue distillate problem, overabundance of nutrient.

  • OK thanks a bunch. I have a pH tester on the way and will wait until it arrives before I run this again. I haven't had much luck with strips as I am colorblind.

  • Yeah, me too.

  • Using it in the wash/mash ... reacts with the copper if i remember correctly and blue distillate is an issue

    Happy Stillin, FS

  • edited August 2015

    Shrug, never had a problem, but I've never gone over 5.5 or so. I used sodium bicarb quite a bit to maintain specific fermentation pH ranges. I'm talking about tiny additions, less than a gram per gallon.

    Wouldn't even wager a bet at where a tablespoon per gallon would get you, probably way over to the other side of the pH chart.

  • Fixed it for you.

    Reaction of a carboxylic acid and sodium carbonate (washing soda):
    RCOOH + Na2CO3(aq) → 2RCOO-Na(aq) + H2O + CO2(g)

    Reaction of a carboxylic acid and sodium bicarbonate (baking soda):
    RCOOH + NaHCO3(aq) → RCOO-Na(aq) + H2O + CO2(g)

    I'm more like I am now than I was before.

  • edited August 2015

    @grim said: The last piece is, if you believe the above, extended/long reflux periods for neutral could potentially be a negative, and not a positive, since you would be creating an environment that favors increased esterification.

    Are you refluxing in a basic environment or an acid one?
    That's makes all the difference. You need to reflux for a long time if your making neutral, to collect and concentrate all the heads out of the boiler. Just make sure it's in not in an acidic environment. Riku recons strip in an acid one (between 5 and 6 pH) to loose the ammonia compounds (the blue spirit) then get your low wines to 8 or 9 pH.
    This reverses the esterification process and any acids that form from the reversal are immediately converted to salts in the basic environment. Standard acid base reaction.
    You'll still need to remove the resulting alcohols with a decent column but the perception threshold of esters mean they stand out a lot more, even in trace amounts. Like I said, it's a good book worth having.

    With regards to SPP, it's not worth the effort IMO.
    It is a serious PITA to work with. It gets tangled with itself, ends up with dust bunnys and all sorts of crap incorporated into it. It gets into everything from one end of the house to the other and is a bit temperamental to distill with too.
    You need an extremely open retainer to use it or they clog and flood (and don't get me started on the 'aquatic environment' rubbish).
    Get some amphora packing. You might not get as low HETP as SPP but it'll just work and it is soooo much easier to handle gives heaps of copper contact. 1 to 1.5 meters of that stuff.
    I've tried 3 or for different types of copper packing. Some I got of Ebay was rubbish. The weave was in the wrong direction and the gauge was to thin so it rolled up way to dense and flooded like crazy.
    The amphora stuff is the dux nutz, nice and open. They've done the testing and selected the best.

    Sure SPP has the lowest HETP but there's a lot of baggage that comes with it.

    It's just the latest reinvention of the wheel.

  • edited August 2015

    Four words regarding column packing: stainless steel pot scrubbers

    (says the man who can pick scoria up off of the ground all around for free)

    I'm more like I am now than I was before.

  • They run a close second for me after the amphora stuff.
    The SS is a nice and cheap option and they work great but if I went with them I would have no copper in the system at all and with the rubbish I run I need some. At the moment I strip through a 0.5 m column of copper mesh. For spirit runs I'm doing neutral through SPP and flavored through 3 or four plates.

  • edited August 2015

    @Kapea said: Fixed it for you.

    Damn, I edited the post to add the carbonate based on Florida's comment and I went and mucked it all up.

    @jacksonbrown said: Are you refluxing in a basic environment or an acid one?

    Always acidic. How I understand it is that the esterification reactions are equilibrium reactions, they don't run to completion, they are reversible (esterification<->hydrolysis) , and they will change in real-time based on the environment they are in. The balance of the equilibrium is going to be determined by a number of factors, ethanol/water concentrations, acidity, concentration of carboxylic acids, etc. You don't need to take the wash to neutral or basic pH to get an impact. Simply reducing the acidity from 3.5 to 5.5, for example, is going to swing the equilibrium point to favor fewer esters. If you then re-acidified back to 3.5, balance would favor a greater amount of esters, as the reactions would reverse. Likewise, in the still, I wouldn't be surprised if you saw different ester concentrations on each individual plate, as ethanol increases, water decreases, esterification is going to be favored.

  • Reviving an old topic...

    Has anyone been able to nail down a general formula for sodium carbonate addition to low wines? X grams per gallon?

  • I know that it has worked for some but my last attempt at adding the sodium carbonate to the low wines was a complete failure. I definitely fucked something up because I had to re-run about 3 times and still didn't get the odd taste out. Also had a BUNCH of bubbles and foam during the boil which is something that I never had with a spirit run before. Hope you have better luck. I will say this; it did make the low wine smell disappear before it went into the boiler so something happened.

  • Did you use a box of washing soda from the grocery?

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