Second run (w/ Fractional Reflux operation instructions)

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Re: Second run (w/ Fractional Reflux operation instructions

Postby monkeyb0y » Wed Jan 09, 2013 2:07 am

Brilliant instructions for new guys like myself...

Many thanks
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Re: Second run (w/ Fractional Reflux operation instructions

Postby Bodhammer » Sat May 25, 2013 3:42 pm

A couple of things I have learned in my first couple of runs -

Altitude affects your boiling points so be sure to take that into account. Chart found here: download/file.php?id=14141&mode=view

Hydrometer temp correction. As my run progressed, my cooling water heating changed the temp of my distillate in the parrot. You need to adjust to the calibration temp of your hydrometer: viewtopic.php?f=2&t=19391

Here is one for the 60° Brewhaus and Widder alcoholmeters: http://www.brewhaus.com/CategoryGrid4.a ... goryId=142
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Re: Second run (w/ Fractional Reflux operation instructions

Postby TheMechwarrior » Thu Jun 27, 2013 9:12 pm

Husker,

Firstly thanks for a great set of instructions!
Secondly, will this apply to a VM still?

After many years of tinkering, moving house, having kids, changing jobs etc I've finally gotten my still to the point it's ready for a leak test and run. Photos to follow.

Cheers,

Mech.
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Re: Second run (w/ Fractional Reflux operation instructions

Postby pounsfos » Mon Nov 04, 2013 4:33 am

can we get these instructions put in the novice reading lounge by some chance....

I for one can vouch that they most certainly helped me and a few of others I've helped.....
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Re: Second run (w/ Fractional Reflux operation instructions

Postby Hound Dog » Mon Nov 04, 2013 4:55 pm

I have to agree with everyone else. I was lucky enough to find these instructions before my first run and they made things more clear than all the other reading that I had done. What I was not quite sure of, I just did on faith and then, BAM! It worked. Thanks Husker!

This should definitley be manditory reading.
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Re: Second run (w/ Fractional Reflux operation instructions

Postby Prairiepiss » Mon Nov 04, 2013 5:28 pm

It's already a sticky. Personaly in my mind. Any sticky thread is a must read thread. On any forum.
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Re: Second run (w/ Fractional Reflux operation instructions

Postby Due51 » Fri Dec 13, 2013 12:56 pm

Thanks from a newb. I am trying to read and comprehend as much as I can. While reading this thread, I found a few other topics I need to learn about and have them opened in another tab. I now have 4 different HD tabs open on my computer and my head is spinning.

Thanks Husker, from a Wolverine.
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Re: Second run (w/ Fractional Reflux operation instructions

Postby sergiolis » Mon Dec 01, 2014 2:11 pm

Hi Husker and others. As a novice I'm a bit disoriented and I would be very grateful if you could help me. I had 2 already stripped runs of 20 liters AllBran washes. I cut the foreshots 150ml for every wash when i did the stripping run. So finally I got 6900 ml at 60% ABV.... So yesterday I decided to reflux that with a Bokakob 2" and 1'20m of copper scrubbers packing. When I put this into the keg I added some water. I don't know how much but I can imagine I had 18 liters at 23% ABV.
It was my first reflux Bokakob run so I follow to the T these instructions. Everything was alright except the lenght of the whole run. It was 15 hours. I was disoriented about how many drops per second or how to adjust the speed of the run.
Husker I read you recommnend to run 3 or 4 mash runs stripped... but if I took 15 hours to run 2 mash I assume I was wrong with the speed...
1. My first question is.... you talk about 4 to 1 Reflux Ratio. Is it equivalent to 75% reflux ratio?
2. How could I figure out how long the run will take?
3.The step 6 of the instructions talks about to collect the heads untill the bad smell has gone at a speed of 1 drop a second. 7th step is to go back to 100%reflux, but 8th step talks about to collect at 2 or 3 drops per second the tails again until 150ml or so. If I don't misunderstand you are collecting heads in 3 steps...

I was collecting the hearts about 6 ml/min. But I dont know if I was right... and If I could i would like to shorten my reflux runs... I'm worried about such long runs because i don't know if i could go a bit faster.
Thanks a lot and sorry about my poor english
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Re: Second run (w/ Fractional Reflux operation instructions

Postby rad14701 » Mon Dec 01, 2014 4:39 pm

sergiolis, most here, including myself, run far faster take off rates when running a spirit run of stripped low wines... I run a 1.25" LM reflux column, packed with marbles, and collect ~1oz/30ml per minute... That's 5x faster than you are running... If you can maintain azeotrope then you aren't running too fast of a take off rate... If the spirits don't taste clean enough just slow the take off rate a bit... I can think of several forms of torture I'd rather endure than watch a reflux column go drip . . . . drip . . . . drip...

As for the reflux ratio, 4:1 means return 4 for every 1 collected... So that's 80%, not 75% returned...

In short, the exact details that Husker posted are for example purposes only... Very few of us follow them verbatim... You have to find out what works for you and your rig... It'll take some practice, but it'll become second nature once you get the hang of your rigs sweet spot... I'd rather do a second decent speed spirit run than become a zombie watching slow drips, and I'd still be done a lot sooner than your 15 hours...
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Re: Second run (w/ Fractional Reflux operation instructions

Postby sergiolis » Mon Dec 01, 2014 5:59 pm

Rad You are always my Savior, hehehheheheh I supose I deserve some novice blunders... you are completely right, I became a zombie because i couldn't sleep watching slow drips all night long. I will remember forever my first fractional run. I read in "The Complete Distiller" about a take off rate of 5ml/min and as a novice I obeyed.
I don't want to be a pain but about the heads...
We need to collect them 2 or 3 drops a second or we could go faster?
Why we have to do 3 steps to collect the heads?

Thanks a lot Rad. If you are using a 1.25" LM with a 30ml per minute rate I supose I could go faster with a 2". So your answer it's really encouraging...... thanks thanks thanks a lot ;-)
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Re: Second run (w/ Fractional Reflux operation instructions

Postby rad14701 » Mon Dec 01, 2014 7:17 pm

I collect foreshots faster as well... I almost never collect at less than 4 drips per second... But, then again, I almost always run low wines through my reflux column... But even when running wash I run at a good clip... Maybe I'm just lucky to be able to get such good performance out of such a relatively small column...
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Re: Second run (w/ Fractional Reflux operation instructions

Postby sergiolis » Wed Dec 03, 2014 3:05 pm

Thanks a lot Rad... I'm not sure if it is the best but I discard the foreshots in the stripped run.... so I start the fractional run just with heads... So definitely I will double my speed next time for both heads and heart.... My allbran are fermenting in 6-7 days (+ 2 days of rest).... next sunday i will try it again... Thanks rad I really appreciate all your comments....
I've seen a post about cuts for pot still... is there any post for fractional cuts?
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Re: Second run (w/ Fractional Reflux operation instructions

Postby rad14701 » Thu Dec 04, 2014 2:31 pm

sergiolis wrote:Thanks a lot Rad... I'm not sure if it is the best but I discard the foreshots in the stripped run.... so I start the fractional run just with heads... So definitely I will double my speed next time for both heads and heart.... My allbran are fermenting in 6-7 days (+ 2 days of rest).... next sunday i will try it again... Thanks rad I really appreciate all your comments....
I've seen a post about cuts for pot still... is there any post for fractional cuts?

You're welcome... There is at least one topic in the New Distiller Reading Lounge, as well as information on the parent site, which cover reflux column operation... Use all of the information as guidelines only because you'll need to adjust for your particular situation...
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Re: Second run (w/ Fractional Reflux operation instructions

Postby madmace » Fri Jan 30, 2015 3:10 pm

Hi all
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If anybody still has ?s about liebig design or double wound coil?s give me a shout have some tried and true results.they worked for me and they might just work for you.
for Example
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used 3/4 steel pipe with 3 eye hooks towards end of pipe
used 1/4 pipe and slid it in the three eyes.wound it down to desired length,,put piece of cardboard around first length of coil,and wound 2nd coil back up.
3/4 pipe,4- 1/4 widths for the 4 turns used in coil
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Re:

Postby baltobrewer » Wed Feb 18, 2015 6:47 am

Hi all, I have been reading every part of this forum that I can for about 5 months now in the hopes that I can avoid a lot of the newbie mistakes and build a still that will serve me well for both neutrals and flavored drinks. I've been an all grain homebrewer for about 19 years, so no newbie to the ferm side, but the distillation side is more complex than i would have ever imagined. I'm leaning heavily toward building a Boka, either 2" or 3" packed (and insulated) column based around a 15.5G keg boiler. Husker's write up is absolute gold. I have a few questions about some points though, and hope others can help in my understanding. Apologies in advance if I sound like an idiot.

Husker wrote:1. Fill your boiler, and do a stripping run (when you have your wash done). When you do this, don't try to reflux anything, just leave the take-off valve wide open, and collect from the beginning, until the EtOH is been fully boiled off.


Does this mean that for a stripping run that the foreshots go in with the rest of the distillate, or do you take these off as you would for a spirit run?

Husker wrote:Reflux run: 1. Bring mash up to boil. When things get to boiling, the temp will rise up the column. At this time, you want to run 100% reflux. 2. When the top of the still head gets hot (say 170°F), turn down your flame.


So the boiler is at full-tilt boil. This would mean (to me) that both EtOH and water vapor are coming off. I had thought from my prior reading that you only want the EtOH part that starts boiling away at 172.5. If we are at 212, then don't you get a weird mix of water and alcohol? Or will this naturally gradient itself out as you reflux?

Husker wrote:4. Reflux 100% like this (equilibrium) for at least 30 minutes (an hour is not out of the question). What you are doing during this time is to build a proper gradient of different products within the column. The most volatile will all be concentrated in the top of the column.


So as you reflux the whole column, the foreshots and then heads will naturally rise to the top?

Husker wrote:5. Now, just barely crack open the output valve. Take off (about a drop per second), and collect 150 to 250 ml of foreshots. Monitor the temp in the still head. It should rise a little.


Temp rises because EtOH is being removed, not because heat input is being increased, correct?

Husker wrote:6. Switch out your foreshot container, with a container for the heads. Slowly collect the heads. Again, watch the temp of the top of the column, watch the temp of the condenser output (so that it is very warm, but that NO vapors are escaping). Keep the output rate at a drop or so a second. Monitor the smell and taste (water down if testing taste, and spit). Run like this, until the off flavor/smell heads are gone.


The smell/flavor of the heads that we are looking to get past is one of solventy/nail polish remover/acetone, correct?

Husker wrote:7. Close off your output valve, increase the water flow rate of the condenser a little, turn up the input heat just a touch (if using propane), and run under 100% for 15 minutes or so.


So after the heads smell dissipates, we close the output and run under full reflux again? Is this so that we can re-establish a gradient within the column?

Husker wrote:9. Now switch to the collection of the body. You can do a lot of this using the thermometer (in the column top).


Since pressure in a still is a no-no, do you just loosely hang the thermometer in the top cap (or however you have it) so that it's open to atmospheric pressure?

Husker wrote:Usually, about a 4 to 1 reflux ratio works pretty good.


A Boka is a closed copper column (meaning you can't see inside). How do you have any idea how much is being returned to the column vs. how much is being taken off?

Husker wrote:11. When you get to the point of about 75-80% of the EtOH being removed (you can pre-compute how much EtOH is in your starting still charge, and you can compute how much has been taken out, by measuring the volumes and ABV of what you have recovered).


This is a big question of mine: Do you use an alcohol hydrometer, and if so, where? Some folks seem to use a parrot, but if you're collecting in small vessels, do you dump from the vessel into a hydrometer jar, measure, and then dump back to the collection jar? Also, does the ABV hydrometer adjust for temp of distillate, or does it not matter? (I use a refractometer for brewing to avoid this temp issue) Or, do you simply just kind of learn when you're running low on EtOH by watching the temp rise in the column?

Husker wrote:At this time, you might have to re-equalize every once in a while to keep the ABV rate consistent.


You mean shut off collection and reflux to equilibrium?


Folks, I APOLOGIZE for what must seem like a barrage of dumba** questions, but these are things that I haven't come across yet in my readings. Thanks in advance to all who may answer.

Jay
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Re: Re:

Postby Husker » Wed Feb 18, 2015 9:23 am

baltobrewer wrote:
Husker wrote:1. Fill your boiler, and do a stripping run (when you have your wash done). When you do this, don't try to reflux anything, just leave the take-off valve wide open, and collect from the beginning, until the EtOH is been fully boiled off.


Does this mean that for a stripping run that the foreshots go in with the rest of the distillate, or do you take these off as you would for a spirit run?

You can remove some of the early stuff. I would remove 250ml or so from a 10 gallon wash charge. I would consider this heads, put it into a 'heads' jug to re-run at some later point. This is no where near as concentrated as you will get with the foreshots. The foreshots are obtained by doing very high reflux, and then dripping off the foreshots very slowly. Depending upon how clean your wash is, the foreshots usually are not 'that' huge an amount, IF you compress it properly, making very stong foreshots.

baltobrewer wrote:
Husker wrote:Reflux run: 1. Bring mash up to boil. When things get to boiling, the temp will rise up the column. At this time, you want to run 100% reflux. 2. When the top of the still head gets hot (say 170°F), turn down your flame.


So the boiler is at full-tilt boil. This would mean (to me) that both EtOH and water vapor are coming off. I had thought from my prior reading that you only want the EtOH part that starts boiling away at 172.5. If we are at 212, then don't you get a weird mix of water and alcohol? Or will this naturally gradient itself out as you reflux?

Ethanol does not boil off water at 172.5. What happens is that the 'mixture' of ethanol and water will boil at a specific temp. Please dig into the parent site on reflux theory section (http://homedistiller.org/theory/theory and just read that entire section). What will happen is you have a boiler that is say 40% (a good ABV from a stripping run from a true pot still). That will boil at about 185F (IIRC). The vapor that is rising off is about 75-80%. Now this vapor rises you your column. It cools off and condenses. But it is 75%, not 40%. This liquid falls back down the column. BUT more vapor is rising up the column right behind it. So this warmer vapor will 'boil' some of this falling liquid. It was 75%, but when it boils, it will be 85% (just a guess). Also, some of that warm vapor cooled, and condensed as 75%. The higher 85% will rise and condense, the 75% liquid will fall and reboil, and more vapor is rising. This happens OVER and over again. The net result is that a gradient will form within the column, where the column is continually reboiling and condensing vapor. The higher you go in the column, the higher ABV (lower boiling point) the vapor/liquid mix will be. Near the bottom of the column, the ABV will be much lower, usually the ABV that the current boiler load will be outputting. Also there will be pure water falling back into to the boiler (it's boiling point being too high for the rising vapors to re-boil). Now as it runs, the boiler itself will have it's ABV reduced, since you are pulling off product.

Now, what that step talks about, is running water to the condenser (ALWAYS DO THIS), and not taking ANY product off. Simply let the column 'live' a while. What will happen is this gradient will form, and the column will equalize. The temp at the bottom of the column may be 185%, the boiling temp may be 190F, and the very top of the column (at the takeoff) may actually be LESS than 172.5, when you are doing early equalizations. The reason it may be cooler, is that the highly concentrated foreshots (acetone, some very volatile alcohols, etc), will be strongly concentrated at the top. Step 4 boils in this equalibrium a while, trying to force the lightest (and nastiest) volatile products to the very top of the column.[/quote]

baltobrewer wrote:
Husker wrote:4. Reflux 100% like this (equilibrium) for at least 30 minutes (an hour is not out of the question). What you are doing during this time is to build a proper gradient of different products within the column. The most volatile will all be concentrated in the top of the column.


So as you reflux the whole column, the foreshots and then heads will naturally rise to the top?

Exactly

baltobrewer wrote:
Husker wrote:5. Now, just barely crack open the output valve. Take off (about a drop per second), and collect 150 to 250 ml of foreshots. Monitor the temp in the still head. It should rise a little.


Temp rises because EtOH is being removed, not because heat input is being increased, correct?

In this case, the temp rises because you are taking away the stuff that boils BELOW the temp of EtOH. You are trying to remove this without removing any EtOH (not possible). Well, you want to remove these while removing as little EtOH as possible. Thus you do it VERY slowly, to try to not change that gradient of product. You will change it over time. You are removing product. At some point, you have remove so much that the temp rises and you start taking off about 90% EtOH and 10% foreshots. At this time, we consider this heads, and we continue to slowly bleed this off (trying to NOT break that gradient), until ALL of the foreshots (heads) have been removed. BUT this part is worth keeping to rerun at a later date. The initial foreshots, NO, never put that back in a still. Burn it in a camp stove, in one of the aluminum can alcohol stoves (viewtopic.php?f=7&t=19823). Also the more concentrated you can get these foreshots, the less of these nasties will be left to have to be removed as heads.

I think some of the other questions may handle themselves once you wrap your head around this part of the process (what is happening).

As for percentage reflux the easiest way to get the take off rate right, is to simply do some runs. Take off in small jars, so you do not screw stuff up. Crack your valve open just a little. Watch the temp at the very TOP of the column (and you can also measure the ABV with a hydrometer, but the temp is better). As long as you can keep that temp rock solid (i.e. it does not start rising), then things are fine (i.e. equilibrium is still being maintained). If the temp rises, then slow down the take off rate, and make sure the temp drops back down to what it should be. If that happens, it probably is good to let it re-equalize (it might happen while still taking off product, it may be that you have to shut the valve down and run 5-10min or so). But once you re-equalize, switch jars, and that jar that got the heads (or tails) in it should be put int he heads jar, or at least marked as a 'questionable' sample. Then when you get things back to equalized, crack the valve open, but not quite as much as you did when the temp rose. ALSO as the run progresses you WILL have to make adjustments, slowly closing the valve, to take off product at a reduced rate. You will have to do this to maintain that temp.
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Re: Second run (w/ Fractional Reflux operation instructions

Postby baltobrewer » Wed Feb 18, 2015 1:27 pm

This is fantastic, thanks. I had read that reflux theory before but the light bulb in my head is only slowly going on (dim as it may be). It takes awhile for what you read and what you understand to meet. I hadn't gotten the whole "compression" theory behind refluxing until now. As for the initial runs, once I get the still built, I'll probably run some of what I have laying about to get the hang of my system. I have about 5 cases of homebrewed red wine that are somewhat oxidized and not very drinkable that I've been loathe to dump (sangria quality). Could these be used for a stripping run? I would guess that I have about 12-13 gallons. I also have 10 gallons of Belgian Tripel that finished way too sweet but is still probably 9% ABV. Very lightly hopped. Viable?
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