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Thread: Vinegar distillation

  1. #31
    Whilst sadly there are people who do sell oils (elixir mixer bought some), these derived from work with metals, perhaps you are correct JDP.
    Last edited by Axismundi000; 03-19-2017 at 10:44 PM. Reason: Edited

  2. #32
    So if we prudently estimate twice frozen vinegar is say 20% acetic acid concentration I make that about 90grams of powdered mineral carbonate/oxide to a 1 gallon (4.55litre) demijohn.

    Using demijohns and putting them on a pet warming pad, giving them a shake daily sounds doable to me. It allows for a steady stream of production without going into some kind of expensive large scale production with vats of wine and vinegar filling the whole garage. Looking on Facebook homebrew pages there are plenty of people who do exactly that though with lots of expensive gear. I am brewing 15-20 demijohns of wine a month so a relatively small scale operation compared to what I have seen some homebrew enthusiasts produce.

  3. #33
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    Quote Originally Posted by JDP View Post
    I don't think it is possible to reach such concentrations by freezing alone under normal atmospheric conditions:

    https://books.google.com/books?id=ax...ntrate&f=false

    "The highest concentration attained in practice by freezing vinegar under atmospheric conditions is 26% of acetic acid." (page 210)

    Another problem to consider is that even distilled vinegar nowadays is contaminated with solid additives (not sure why do manufacturers feel the need to do this, it's not like vinegar "spoils", there should be no need to add preservatives to it):

    http://forum.alchemyforums.com/showt...4721#post34721

    Getting rid of these solid additives would help to dispense with the need to re-distill the distilled vinegar. Soluble lead salts (like lead acetate, for example), which readily combines with these additives and forms a white precipitate, are one possible solution. If you intend to use the vinegar for experiments involving lead, or where the presence of small amounts of lead salts are not a problem, then no further work is needed on the commercial distilled vinegar. You can simply concentrate it up to about 26% by freezing and then treat it with a solution of a soluble lead salt until no more precipitate forms and then filter the resulting vinegar.

    But if you want to get rid of the remaining lead salt, I've been thinking that maybe it should be possible to do this by treating the lead-contaminated vinegar with hydrogen sulfide gas, until no more black lead sulfide precipitate forms. Then you filter the vinegar and get rid of whatever traces of hydrogen sulfide gas might remain dissolved in the vinegar by warming it for an hour or two. Needs to be tested. If it works, it would give you a more concentrated vinegar (about 26%, as opposed to the usual 5 to 9% concentration of commercial distilled vinegars) without any solid additives, and no re-distillation would be involved.
    The above method has now been tested. Seems to work very well. I tested a sample of the treated commercial distilled vinegar with sulfuric acid and not white precipitate formed, meaning that no lead was present after the excess of lead acetate was precipitated by the hydrogen sulfide gas. This method allows one to get rid of whatever is that bothersome crap they put in distilled vinegar (and who knows why, because, as already stated, distilled vinegar DOES NOT "SPOIL", there is no need to add anything to it!) without having to tediously distill it again.

  4. #34
    Thanks for sharing your practical findings JDP. I look forward to hearing more about your work as time goes by.

  5. #35
    Improvised Alembic using glass teapot, silicone rubber soft funnel and 2ltr erhlenmeyer flask.



    Hopefully the gradually narrowing outlet will encourage the acetic acid to reflux more than the water does and water will primarily come out of the spout. If it dribbles down the side of the flask as well the saucepan will catch it. The stains on the PVC tubing are mildew as this piece of tubing was previously used for coolant water flow to Liebig condenser. The water might not evaporate but I'd don't want to heat the vinegar above 90C so I can always try a smaller 1 litre flask maybe.

    If this works I will be delighted because vacuum distilling requires more supervision.
    Last edited by Axismundi000; 09-23-2017 at 06:40 PM. Reason: Added a bit

  6. #36
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    Good effort Axis!
    Join me; on a voyage of stupidity, and self discovery: https://www.youtube.com/watch?time_c...&v=vccZSHroTG4

  7. #37


    It works kind of with no funnel so a larger outlet. I'm hoping that the vinegar mainly drops back down into the liquid and the water vapour escapes. We shall see, I can use PH papers and test with some eggshells because I have already tested the diluted vinegar in this way. It is slow but you can just let it run unlike with vacuum distillation which I find needs supervision especially of the cold trap.

  8. #38
    It didn't really work I'm getting about 25% of the vinegar coming over with the water. Vacuum distilling saves virtually all the vinegar but it needs much more supervision. I have a new wacky plan for another try of sweating water out of vinegar which I will probably try tomorrow.

    Edit: waiting for a part ordered. I know I could just see if I can get an alembic for this but it would be nice to find another solution because Alembic's are not commonly available. Also I have a fair bit of push to fit lab glass so I'm trying to stick with that because different pieces have several uses.
    Last edited by Axismundi000; 09-26-2017 at 11:34 AM. Reason: Waiting for a part.

  9. #39
    None of my wacky plans have worked here. Vacuum distillation is the only way I have found to separate acetic acid and water with the temperature below 90 centigrade. I suspect sweating off the water with an alembic would work but I can’t justify the expense besides I suspect that I can get a run completed faster with the modern approach. It must have taken the medieval Alchemist’s so much time to sweat water out of vinegar. Also the acetic acid itself correctly produced and concentrated is the point here. It’s fun to tinker with stuff but an objective needs to exist and be achieved I have spent enough time on this now.

  10. #40
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    Quote Originally Posted by Axismundi000 View Post
    None of my wacky plans have worked here. Vacuum distillation is the only way I have found to separate acetic acid and water with the temperature below 90 centigrade. I suspect sweating off the water with an alembic would work but I can’t justify the expense besides I suspect that I can get a run completed faster with the modern approach. It must have taken the medieval Alchemist’s so much time to sweat water out of vinegar. Also the acetic acid itself correctly produced and concentrated is the point here. It’s fun to tinker with stuff but an objective needs to exist and be achieved I have spent enough time on this now.
    Did you do these distillations after sufficient distillation by freezing? I assume? Acetic is definitely a PITA to separate and from what I've read, always needs to be done in fractions, over and over. If you start with 5-10% in the boiling flask, you will catch hell trying to distill it to a more concentrated solution. You already know this Axis, I'm sure, but just for reference to anyone perusing the thread.

    It's interesting that vacuum distillation is working. Does the vapor pressure of acetic not rise as quickly as water at lower pressures? I never thought to dig through Google for a graph of that.

    I'm also not sure that the toil is worth much. The Hermes book I have contains an experiment "of many jars" where different solvents are used on various metals to extract the oil. The methods are slightly different per method, but the solvent is always pulled off. I'm not convinced that (for regular solvents) it needs to be prepped by making all of that wine vinegar, but I commend your efforts. We might consider that those trying the acetate path simply recycled their strong vinegar over and over to extract more oil, but that is more toil too. JDP might be right in saying that this is something good to put in an alchemy book to waste the time and energy of seekers.

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