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Having Troubles With Our Vodka

We are having trouble getting the 190 proof that we need to produce our vodka. I am new to using a column still and I am wondering if I am just thinking a little too much into it, or do I need to add more to the setup.

The setup:

  • 100 gal Pot Belly
  • 6-8" columns
  • 4 Bubble Caps
  • 2 Perforated Plates
  • One of those is packed with parasmatic packing about 2" deep
  • The other is completely filled with Lava Rock

The best we have ever gotten is about 189.4 proof.

Please help! I am going nuts here.

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Comments

  • I think you need more plates

  • We are limited on height. That's why we are trying the packing and lava rock. I guess we could start looking at going sideways.

  • Most people have a short packed section on top of the plated section when going for neutral. Usually about 500mm. Maybe you could even try taking a plate or two off to allow more packing?

    StillDragon Australia & New Zealand - Your StillDragon® Distributor for Australia & New Zealand

  • How many runs are you doing? With 6 plate, 2 runs should get you there no problemif you run slow, 3 if you run faster. In the future you're probably gonna want to go sideways if all you can fit is 6 plate (about 10ft total?) and want to save time/energy

  • @toledowhiskeyman said: We are having trouble getting the 190 proof that we need to produce our vodka. I am new to using a column still and I am wondering if I am just thinking a little too much into it, or do I need to add more to the setup.

    The setup:

    • 100 gal Pot Belly
    • 6-8" columns
    • 4 Bubble Caps
    • 2 Perforated Plates
    • One of those is packed with parasmatic packing about 2" deep
    • The other is completely filled with Lava Rock

    The best we have ever gotten is about 189.4 proof.

    Please help! I am going nuts here.

    I am having difficulty with 24 procap plates... (edit: 8" crystal dragon on 380L, running 11kw during run) so don't assume 8-10 plates will completely eliminate your issues... I can go over 190 as measured with certifired and calibrated TTB approved hydrometer and thermometer, but only at a very slow rate... I now have the Anton-Paar DMA35 and i get the same information just a lot faster... easy-peasy to get 20l/hr of 189 proof.. lucky to get 5l/hr of true 190...

  • Also, what wash %age are you starting out with?

  • me, 30%, highest recommended for electric elements...

  • We are starting with 30%. 60 proof.

  • @CothermanDistilling, have you tried/considered changing your still charge configuration from say a 30%abv charge to a 40%abv charge? Just wondering what it's going to take to pull-off 20L/h @ 190/190+.

  • We did try at 35% but still got the same results.

  • I've been in the 40-50% range plenty of times and never had issues or scares. I've also been over that and obviously lived to tell the tale. I've yet to read any definitive article concerning the max and never actually read of an element igniting the charge, only tales that it COULD happen. What I can tell you that cuts are super easy with higher proof, like turning a hearts switch on. It was great.

  • @CothermanDistilling is there a reference to the 30% recommendation? I'd like to know the reasoning behind not going higher.

    @toledowhiskeyman you are correct in your observations, the "same results" can easily be explained by the following graph. As we are now operating at the high end of diminishing returns the measurement accuracy starts to come into it.

    image

    Looking at the above graph I don't have the resolution to show the number of theoretical plates that would be needed to get from the ~155proof first step all the way to 190proof but there's enough literature out there pointing to 30 plates that I'm happy to accept their word for it.

    temp_abv.jpg
    800 x 511 - 79K
  • @Kill_Devil_Spirit_Co said: What I can tell you that cuts are super easy with higher proof, like turning a hearts switch on. It was great.

    Another myth busted?

  • edited November 2015

    I don't see what the safety issue is of 30% vs 40% vs 50% vs 80%, etc etc etc. There is no way that 30% is any safer than 50%, for example...

    image

    Just look at the difference in the critical temps. This doesn't include autoignition temperature, but those numbers are equally as close as these.

    The only factor I can imagine is geometry, keeping the elements covered through the run. This is going to have more to do with your vessel shape really.

    In the case of a failure of the kettle wall or a spill, even 20% is going to be bad, as it's going to be well above the fire point if it spills at run temperatures. You are in every case guaranteed a vapor cloud. Even 10% will be sufficient to flash and do some serious damage. You could argue that a spill of 80% ABV is dangerous, as it would require a significant amount of water to dilute than 30%, perhaps I could buy that as well. Say you have a hose that can spray 10 gallons a minute. Let's say you dump 100 gallons of 30% on the floor. It's going to take 60 minutes to dilute the spill to 5% with that little hose. It's going to take almost 3 hours to dilute the 80%, and it's dangerous pretty much that whole time.

    table.jpg
    464 x 227 - 36K
  • By the way, if you really dump 100 gallons of 30% on the floor, it's probably better to run out the door.

  • Harry has a post on artisan explain the reason for a 30% boiler charge, I think it has to do with leaving esters in the boiler

  • edited November 2015

    Sure, percentage of water in the boiler is going to directly impact esterification/hydrolysis. However, in a plated still, you also have esterification taking place on the plates, in reflux, where the water concentration is significantly lower. Organic acids do make it through distillation, and will exist on the plates. If you have ester precursors in the boiler, you'll form esters on the plates, regardless of the lower boiler charge. We're not talking about a pot still distillation here.

    We've also talked about plenty of ester precursor reduction strategies (and ways to increase esters in the case of heavier rums). Run your ferments at a lower SG, cooler temperatures, good yeast husbandry and nutrients, impeccable sanitation, filter the yeast from the wash, or at least rack it, pH of the boiler charge, antibiotics, etc etc.

    Actually in the process of running a bunch of trials using my lab still with combinations of different alcohols and carboxylic acids from the lab supply. Got inspired to try it in the thread with the discussion about wash pH and esterification.

    The other factor here is the legality issue of hitting the specific take-off minimums. Law is pretty clear, esterification and reactive distillation not so clear.

  • As previously pointed out, I have found 2 things that have improved my neutral;

    1. Make damn sure that the wash going into the boiler is as close to clear as possible. If mine isn't crystal clear I will rack the day before. Splashing from one 5 gallon bucket to the other to remove any CO2 makes a big difference. I do this with rum as well. I realize this isn't feasible for large operations but the process could be adapted to larger scales.

    2. By running at 30% or lower. I once read that water is the best sponge for holding flavor producing compounds and I believe it. Makes a difference in my runs. I obviously don't do this for rum or whiskey.

    I am running a 5" column with 4 ProCap plates. 6" of packed space right under the defleg. One stripping run, and then 2 slow spirit runs leaves me with a neutral that is almost void of any detectable smells or flavors. I also make pretty tight cuts and air out the spirit between runs.

  • Anyone experimented with the procap riser extension pieces yet? Wondering if liquid level is a bigger factor here than we think.

  • @grim said: Anyone experimented with the procap riser extension pieces yet? Wondering if liquid level is a bigger factor here than we think.

    I think that may indeed be a help... and they would also reduce the size of the inlet that a splashed drop can hit...

    now, I am not going to start with all 288 procaps having them, do you think they would be best on the highest caps?

  • Oh, and the 30%... think about this.... by the time it hits the first plate, it is 77%...

    So now I have 77% with 23 plates... IMHO, the low charge theory falls away...

    I can run straight beer through the 24 plates and get the exact same results.. I just don't like the nasties and the foam in the plates...

  • edited November 2015

    Re running till the spent kettle charge is clear (not cloudy) makes for clean distillate.

    Vodka is also made in a pot still by calculating the combined distillation needed to achieve the cumulative degree of cleanliness.

    We all know that high abv does not always equate to a clean spirit.

    StillDragon North America - Your StillDragon® Distributor for North America

  • edited November 2015

    I think I have enough extension tubes here for 5 or 6 8" plates. If someone in the states wants to try it, let me know and we can work something out. No way I'm taking the 12" apart to try it, it would take me all day to disassemble. Besides, with 4 plates, we're finding we need to run pretty fast to keep the proof low enough on a single pass whiskey run (3hr run times on a 1000 liter charge).

  • @CothermanDistilling said: So now I have 77% with 23 plates... IMHO, the low charge theory falls away...

    Maybe, but the idea is that the crap has less of a chance to get to the first plate if it is in more water. Maybe scientifically it falls away, I don't know.

  • We are getting clean tastes and aroma. That isn't our problem. We need to hit the TTB mark for ABV.

  • @grim it's a night and day difference between heads and hearts. At around 172F vapour temp the distillate lost all scent and taste, the transition was very quick. I always figured the watering down was more for easing in so you didn't lose any hearts but anyone paying attention to vape temps can figure out when you are gonna hit hearts (at least in a column)

    So basically we are back to run slow for high proof and fast for 189 and below? Or add more plates and hope? Seems about right haha

  • @FloridaCracker said: Maybe, but the idea is that the crap has less of a chance to get to the first plate if it is in more water. Maybe scientifically it falls away, I don't know.

    also, when your 40% kettle charge was 25% done, it would be 30% stuff in the kettle...

  • Oh, and some of you may remember this, LOTS of great insight from @captainshooch in this experiment he did:
    An experiment with CM/LM and a DASH-2

  • edited November 2015

    @Kill_Devil_Spirit_Co - My brain is having an easier time accepting your description as being more correct than the running theory that a lower boiler charge provides more "purity".

    Honestly, if that was the case, you should be able to get a cleaner spirit out of a single pass run, after all, there is even more water in the boiler to "lock-up" those impurities. Contradiction.

    If you believe a pot still provides very rough cuts (which it absolutely does), than anything you do to increase the output proof is going to provide you with tighter cuts. Safety aside, if increasing the boiler charge increases output abv, than the cuts have to be sharper, not duller. Another contradiction.

    I tried to find that old thread mentioned above, all I found was 7 years of horrible misinformation and an almost religious belief that 30% alcohol is somehow not flammable, so it's safe (which is complete and utter rubbish).

    If you haven't noticed, anyone tells me something is the gospel truth, I'm going to question the hell out of it until I find out why.

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