Cloudy Vodka

This issue has occurred in multiple batches in various recipes. I am using a stainless steel 8 gallon milk jug boiler, 2” OD sanitary SS column, 30 inches of copper mesh packing, in a vapor management still configuration with electric heating element. This configuration will consistently generate crystal clear spirits at 96% ABV. However, when I dilute the ethanol to 40% ABV with distilled water it becomes cloudy at around 50% ABV.

The last time I was making vodka I was going to see friends the next day and wanted to bring them a bottle. I calculated the DI water to ethanol coming off the still, added the correct amount of water, and allow the distillate to drip in to the bottle straight from the parrot. This bottle came out clear vodka at 40% ABV. This sample was taken from the middle of the run (jar 10 of 21). Later I went to dilute the other jars and they were cloudy.

Attempting to unravel this mystery, I simulated the bottle I produced mid run. I added the correct amount of water to the bottle, placed the ethanol in a plastic bag, poked a hole in the bag, and slowly dripped the ethanol in to the water, as the parrot had done. I was so excited when all the ethanol had been added to the bottle and it was clear, I grabbed the bottle off the counter to show my wife. Upon jerking it off the counter in my excitement and swinging it around to show her the attached picture was the result. The ethanol being less dense had formed a layer on top of the water and when the interface mixed… alas still cloudy. It stayed that way for many days, finally I shook it up and it was still cloudy.

Can someone explain what is happening here and how it is clear vodka is produce? Only the hardest core alcoholics in my life will consider drinking this vodka, which I have attempted to market as “partly cloudy” or “greyer goose” both of which are clearly not going to make it. Its flavor is good, ingredients are pure, but its presentation is unacceptable, as vodka is clear.

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Comments

  • Call it halo vodka. Problem solved.

  • Look up louching

  • You can re-assure your less than hard core friends it's fine.

    Though not the cure for the cause, stick it in the fridge and see if you can cold crash some of that haze out of suspension.

    If you have any glassware that is sort of test tube narrow (and straight) with a wide mouth, it'll make it easier to pour off the clear and leave the jelly fish at the bottom relatively undisturbed.

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  • Thank you for the thought and ideas!! I truly appreciate the expert opinions, and I'll add "Halo Vodka" to my ongoing list of failed attempts to market non-clear vodka. :D

    I have read multiple threads on louching, but everything I have read thus far is referring to the gin, and the interaction of high botanical impurities with the spirit. Without the botanical addition could this still be louching?

    I have attempt the refrigerator and freezer to clarify the vodka, to no avail. I have not attempt "cold filtering"

    I am not sure I understand "the jelly?" Does this imply the cloudiness is some sort of gel suspended solids? I have attempted filtering (albeit just coffee filters) and carbon filtering, but still cloudy? However, I am certain decanting the top off of the cloud would just return high proof ethanol from the top, as it is floating on the water. "The ethanol being less dense had formed a layer on top of the water and when the interface mixed." The picture is not 40% ABV vodka with a cloud in the middle, it is 97 % AVB floating on water, with a cloud at the interface where they mix. Once shaken it is homogeneous cloudy 40% ABV vodka, and does not settle even after months of sitting undisturbed.

    This is the third batch a vodka that has done this. Clear ethanol, at virtually the azeotrope, mixed with DI water from various different manufacturers yields cloudy 80 proof vodka? Changing to different water sources would indicate that the "cloudy" is inherent from the spirits. I don't seem to be able to remove the cloudiness after distillation. Therefore, I think I need to change something in my process, I am just not sure what I could be producing that would carry through the column distillation process.

    I apologize for the lengthy explanations, but feel it is import to provide as much accurate information as possible. I have made multiple attempts to clarify the end product, and once or twice have produced a clear product, but I am baffled as to what the different was.

    Thank you again for any and all thoughts and ideas. Though this is the first time I have posted to the StillDragon community, I have been reading the treads for quite some time, and you all have been instrumental in accelerating my learning... and laughing my way through my mistakes.

    Cheers!

  • Sounds like we are wasting our time marketing distillation units when you have figured out how to seperate the ethanol from the water by just leaving it sit.

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  • Jellyfish being more or less a comical way to refer to the solids that do settle out. Once settled at the bottom the structure of solids resembles a slimy like jelly mass.

    StillDragon North America - Your StillDragon® Distributor for North America

  • I thought ethanol and water mixed nearly instantly. It certainly does when I add water to dilute.

  • Seems like you are getting some oils during distillation. Are you stripping first? When you mention ABV, is this corrected (60F) ABV at 95+ ABV? Are you making conservative cuts and not going deep into tails?

  • @lamanzo. I just hooked up the cooling piping on my vodka still and in the next couple of days I will see if I can make something decent. If not I will call mine Halo Vodka if you havent already taken the name.

  • Slightly off the current direction, but what about trace oils within the still i.e. do you do a CIP prior to your spirit runs ??

  • Thanks for all the thoughts!

    In order:

    @punkin / @Glenndog: Read the first tread third paragraph again, water's density is 1.0 g/ml and ethanol's is 0.789 g/ml. So Ethanol will definitely flow on water, just like you can make a black and tan, or my personal favorite example a dark and stormy (see attached picture, ice excluded for affect)... Normally I cut my spirits by pouring the water and ethanol together with the goal being to "get the job done," but as stated in the third paragraph I was attempting to simulate the clear bottle I produced off the still: water first and than slowly dripping the ethanol in to the jar of water. It was clear when I had dripped the last of the ethanol in completely, or at least I did not notice the thin ring that may have been there. Once complete, I excitedly (thinking the solution had mixed and made clear vodka!) grabbed the bottle off the counter and spun around to triumphantly show my wife. As if to mock me, the motion caused enough mixing in the bottle to yield the result in the picture (very cool, but depressing). I sat it on the shelf for a few days and it did not change substantially. I eventually shook it up, the entire mixture became cloudy and stayed that way.

    @Smaug: Is a "jelly fish" a solid? Would it get hung up in a coffee filter, like a vinegar mother, or the culture in Kombucha? The "cloudy" will not filter, at least not in a simple coffee filter. It passes through.

    @Mtr_Distiller: I do perform a stripping run first. My fermenter is 16 gal and my still is 8gal. So I strip the 16 gal of beer in a batch still configuration (2x), and then combine the two runs and set up the still configuration with the column for vodka. My ABV numbers are off my alcometer and not temperature compensated, so there is a little error in that, but it is at "room temp" so it should be close. I did not cut run and mix the jars together, as I would normally because I have been attempting to understand this problem. I have been experimenting to see if I can get clear vodka at 80 proof.... and, honestly, I have been using some of the jars to increase the yield on my early all grain bourbon runs.

    @DonMateo: I am excite to hear about your results. The name is yours! I am still putting my money on "greyer goose," as I see no feasible way to maintain the "halo" in transit, though a very cool result.

    @richard: You have called me to the carpet on this one. I rinse my still components but I do not "CIP" them, or COP them as my still is easily broken down, or sanitize them like I do the fermenter and things that touch the beer. I rinse with hot water and dry before the next use. Is there a chemical treatment I should be using?

    I feel like I am writing a thesis, but I greatly appreciate all the thoughts and comments, and I don't want to leave anything out that might prove to be important.

  • Dark and Stormy.
    Cheers

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  • edited May 30

    When proofing, you slowly add water to the alcohol, you don't add alcohol to the water.

    The reason for this is that the first alcohol added to water will face extreme dilution, very low ABV. The low alcohol content, and high water content, will cause a number of reactions to take place - the most obvious is hydrolyzing esters that may exist in the alcohol into their constituent acids and alcohols. Many of these long-chain carboxylic acids can cause haze when they clump, and it's not likely they will esterify again at a lower ABV.

    If you are simply mixing the two together in one shot, it's not really relevant. But slowly dripping in alcohol is without a doubt the worst way to dilute.

    If you are talking pure azeo ethanol, it shouldn't matter either. However, you aren't quite there.

  • edited May 30

    Ahh i see. Slowly dripping stops it from diluting at all.

    12 years later and i'm still learning something as basic as that.

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  • Sure, stirring larger volumes stored in cylindrical tanks is common prior to bottling to insure uniform ABV as stratification is a thing.

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  • edited May 30

    Yes i was aware of that, but this is a claim that pure ethanol is sitting on top of pure water. One would expect that a single drop dripping into a volume of water would instantly mix to a very large degree.

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  • @punkin, with only one trial to base results on, I appreciate your challenge of my method and assumptions. Fortunately I have about 5 more pints to experiment with before I have to begin at fermentation again. Attached are picture of trail# 2, same method, but I had to use filtered water instead of DI, as I did not have any in house. This time I capture a bunch a pictures as I swirled and mix it. # 1 shows the etol water interface as almost a line, though the difference in refractive index is apparent. Then I continued slowly getting more vigorous until it was fully mixed. ...and alas, still cloudy... :(

    @grim, thank you for the clear explanation on how I should be mixing and why. Please don't take the recreation of "without a doubt the worst way to dilute" as an indication that I did not understand your thoughts, instructions, and reasoning. I understand and will slowly add water to ethanol in the future!

    After all this discussion, I am not sure this experiment has any true value, but maybe it will help someone else starting out. If nothing else, it is really interesting to observe!

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  • Now sip[hon off some from the bottom and some from the top before you mix, test with an alcometer and tell me if you have a sample with 0% abv and one with 96% abv as claimed.

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  • @Lamanzo's bottle's clear bottom is interesting as I would have expected it to be all haze at the bottom. The picture I've attached is somewhat similar to what was described, but there was no water in this jar to start.

    Basically what you are seeing in my pic is the result of the tails from the previous distillation coming out (low ABV) and the foreshots of the current distillation "floating" on the top (high ABV). This wasn't a drip drip drip either since I poured in about a quarter gallon at a time into this jug. So you can see that things don't mix as readily as you might think.

    Once shaken, this jug was all cloudy as you would expect.

    @Lamanzo, I don't think you are as close to azeotrope as you think. You are getting quite a bit of oil. Where that is coming from, I don't know. You're probably running too fast, but there could be oil in your still too.

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  • I have no doubt that the ethanol can stratify on top of the water in layers (i've seen it many times), just the claim that it's pure ethanol and pure water, if we could do that by settling then we wouldn't have distillation equipment.

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  • Unless I missed something, he says it has NOT settled out. Which as we both know is absolutely correct with the exception of "jelly fish" phenomenon.

    I bet the top is pretty close to pure ethanol. I don't think its inconceivable that the bottom is pretty close to pure water too.

  • @punkin, I thought the idea of the forum was to help one another. My purpose is to blend the solution homogeneously to 80 proof without the cloudiness. To this end, this discussion is proving pointless. Your input is welcome, but not helpful. @jbierling is correct, I never said it settles, I said alcohol was floating on the water due to the way I mixed it, an error on my part. I recreated the results, therefore, I have proven to myself the alcohol IS floating on the water. You have seen it many time, so just what exactly are you looking to prove? I have no reason to continue down this path, as it does not assist in achieving my goal. If you would like to be right, conduct the experiment, decant the liquids, and let us know what you find. We are looking forward to your results.

  • edited June 2

    @Lamanzo said: The picture is not 40% ABV vodka with a cloud in the middle, it is 97 % AVB floating on water, with a cloud at the interface where they mix. Once shaken it is homogeneous cloudy 40% ABV vodka, and does not settle even after months of sitting undisturbed.

    Not exactly true that you didn't say it but i take your point, it is not germane.

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  • @jbierling, you read correctly, understood what I wrote, and I appreciated your help. The only way I have to measure the %ABV is an alcometer. It reads right at 95%, though not temperature compensated (the temp is 65°F). The positive azeotrope is 95.63% ethanol and 4.37% water (by mass). In truth, I was surprised I could get this close with the setup I have. The run took 16 hours to allow the column to stabilize in full reflux, and then slowly draw off the ethanol. So I do not believe I was getting oils carrying over from the boiler, though it is possible. If the oil is coming from my still, could you recommend a cleaning method and/or chemical(s)? As stated above, I rinse and scrub the parts, but that is all. I assumed, a bad idea I realize, that between the heat and the alcohol the still was the cleanest part of the process.

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  • You refluxed for 16 hours before you began to take off product?

    Interesting.

  • edited June 2

    @grim said: You refluxed for 16 hours before you began to take off product?

    Interesting.

    Notwithstanding alcohol enrichment,,,pulled all kinds of spunk up on to the plates...

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  • Just a WAG, but I'd guess the proof is closer to 180 than 190. Temp and little hydrometers make for a wide margin of error. For 190+, at most normal distilling temperatures, you want that hydrometer sunk. Still doesn't explain all the oil though.

    Just as the others have noted, full refluxing for 16 hours is overkill. Really what you want is the temperature at the bottom of the column to stabilize. Then you can be reasonably be sure the column is in a good place. Really shouldn't take much more than 20-45 minutes.

    As for cleaning, up doesn't matter so much, but you want the down (condenser) to be clean. I don't know where you are, but PBW followed by citric acid works well.

  • We need to start a new thread:

    "Show us your jellyfish"

    FC

  • I've got a bottle of pawpaw at the shop that has a hilarious amount of sediment that has settled out.

    There is nothing really special about pawpaw imo. And so the outfit producing this is not really doing themselves any favors by putting this spirit in the bottle so prematurely.

    If presentation is a contributing positive on a shelf overrun with choices, they more or less really screw'd up their opportunity to make a good first impression to so many that would otherwise be potential customers.

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