Second run (w/ Fractional Reflux operation instructions)

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Re: Second run (w/ Fractional Reflux operation instructions)

Postby DestructoMutt » Sun Jul 12, 2009 3:24 pm

edbarcik44 wrote:New to the craft and have been somewhat successful except I cannot get above 88% ABV, I have a reflux unit 6' X 2" and does 25l batch. Yesterday I had a power failure during a spirit run and power was off for several hours. When power came back, I started everything up again, took an hour to get boiling but I could not control the temp in the head, kept running at 95+, opened the valve to cool the top of the tower and temp went to below 70, I kept adjusting and it would just go up and down, never settle in the right temp range, I took off about a gallon of spirits before the power failure, is this batch history or can it be salvaged?
I followed the instructions posted in this forum to the letter.
Thanks for your advice.
Ed

sounds like you are not running in equlibrium long enough, thus not separating the foreshots completely from the hearts. you need to let your column run in equilibrium until the head temperature drops of it's own accord (natural action).

to achieve equilibrium you get the boiler up to boiling, then turn the heat down so that you have a slow simmer (still boiling, but slowly). before the boiling begins, you turn on your reflux condensor so that the vapors from the boiler are ALL condensed and returned to the top of your column as liquid. you do not remove any product during this time/period. everything is returned to the top of the column as liquid. during this period the head temperature may jump up to 84C, relax, don't worry, be patient, watch it, it will slowly drop back down to something less than 78C. by slowly, i mean 1 - 4 hours, depending entirely on your system and the wash you are using. after the temp has dropped on it's own (you can not force it to drop before it is ready to without screwing things up), you can start to slowly bleed off the foreshots. watch the thermometer while you are doing this, if it starts to move slowly upwards, you are taking the foreshots off too quickly. if it holds steady for a while (10mins or so), while bleeding off the foreshots, you are taking them off at the correct rate. after 10-15mins, the temperature will make a quick jump, if you have collected the foreshots slowly enough; if not, it will make a slow steady climb - this means you are dragging the foreshots through to the hearts and creating heads (heads are a mixture of foreshots and hearts). the more slowly you bleed off the foreshots, the better your separation from foreshots to hearts will be. [what would you rather have, 500ml of foreshots/heads in 15 minutes or 100 ml of foreshots/heads in 30 minutes?]
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Re: Second run (w/ Fractional Reflux operation instructions)

Postby gbdsl0 » Mon Jul 20, 2009 4:38 pm

Hi, I am currently using a still maker internal reflux still. (In the process of making a valved reflux still) I have used the still quite a few times and managed to get at least 90% ABV. I have only ever done this in a single run by regulating the temperature (79c degrees) at the take off point. I have never done a stripping run.

Now this question relates specifically to temperature control in a stripping run. I want to know if I need to be overly particular about the temperature at the take off point when I'm doing the stripping run. Because of the design of my still I can't switch the reflux off so I need to run the temerature at the take off point around 84/85c degrees to maintain a decent flow rate. This puts the temperature above the boiling point of 2-propanol.

Now if I understand my theory right the different components in the wash will seperate themselves into gradients, those with the lowest boiling point will be at the top. So would it be true to say that prior to any large amounts of 2-propanol coming out, I should be able to extract mostly ethanol even with this higher temperature at the take off point.

I did the calcs on my wash and I should be able to get approx 4.5 litres of ethanol from the wash.

Thanks

gbdsl0 :D
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Re: Second run (w/ Fractional Reflux operation instructions)

Postby Dnderhead » Mon Jul 20, 2009 5:13 pm

""Because of the design of my still I can't switch the reflux off""
I believe that is part of your problem,, do some repluming so you can control both reflux and condenser separately. (a simple Y valve)
stripping run,, just run hard and fast as you can and still knock down the vapor.
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Re: Second run (w/ Fractional Reflux operation instructions)

Postby gbdsl0 » Tue Jul 21, 2009 3:39 am

Thanks for your help Dnderhead. Can anyone advise how long I strip run for. Do I keep going until there is no Ethanol in the distillate or is there an approx ABV I should stop at.

Can anyone advise also if my assumptions in my previous post were correct?

Thanks again.

gbdsl0 :D
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Re: Second run (w/ Fractional Reflux operation instructions)

Postby Mc Shine » Sun Jan 10, 2010 12:42 pm

This is my second run ever ,still usein birdwatchers and the instructions are spot on . thanks for the help. my still is a LM keg boiler 4 foot collom cross flow condencer
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Re: Second run (w/ Fractional Reflux operation instructions)

Postby Jon » Thu Apr 15, 2010 2:16 pm

[what would you rather have, 500ml of foreshots/heads in 15 minutes or 100 ml of foreshots/heads in 30 minutes?]


Doing my first run on my 3 ft reflux column with bokakob head. The 36" column is lightly filled with coppers scrubbers.

I'm distilling 6500ml of 40% abv, the result of a stripping run (in a pot still) of 5.5 gallons of birdwatchers sugar wash. I discarded the foreshot of 100ml and am 400ml into the heads (1 drop / second). It's been 4 hours since the first drop, and 3 hours of heads (100/ml an hour). The temp has been steady at 75.1C to 75.3C since the headshot (74.8C).

Is this normal or are my drops small? :)

It's still coming out smelling like grape koolaid/acetone.
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Re: Second run (w/ Fractional Reflux operation instructions)

Postby Dnderhead » Fri Apr 16, 2010 4:40 am

depends, you doing one or two runs? if your stripping, just run it off in a stream, a stripping run,is just to reduce the amount of wash and clean it up a bit. with no major concerns for purity.
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Re: Second run (w/ Fractional Reflux operation instructions)

Postby Jon » Sun Apr 18, 2010 9:33 am

Well the run worked out just fine. I ended up with about 1100ml of 95% abv. I had 200-300ml of heads and missed the start of the tails so i spoiled about 200ml of good body. I will toss it into the next run. My thermometer must be off by 3 degrees because it read 75 when the temp had to have been 78?

Aired it out for 2 days and mixed it with distilled water to 2300ml of 40% abv. Did a taste test vs. Skyy vodka and wow, this is so much better. Thanks for the instructions.
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Re: Second run (w/ Fractional Reflux operation instructions)

Postby CROW-EATER » Thu May 27, 2010 2:27 am

Great post husker,coppied into my documents for printing as im about to use my offset head fractional still for the first time very soon,
cant wait !
Its people like yourself that make these kind of sites worth thier weight in gold.
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Re: Second run (w/ Fractional Reflux operation instructions

Postby Kiwi-lembic » Mon Feb 14, 2011 11:57 am

Great Stuff Husker ..was there ever a link for pot still instructions made (stripping runs/spirit runs in a pot)..going looking /reading for myself ...after reading this it might help new people....making it easy to find if it was plastered here for ease ..many thanks for you great post
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Re: Second run (w/ Fractional Reflux operation instructions

Postby CH3CH2OH » Mon Oct 24, 2011 3:38 pm

Great instructions
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Re:

Postby yamastill » Wed Apr 04, 2012 8:45 am

Husker wrote:
Bohunk wrote:Husker, what an awesome answer... You have continually provide a lot
of folks with help, there are few folks here willing to take the time to help
like this. Proud of you dude!!! Now if only those other huskers could make me proud again, damm.

The Bohunk


I dont expect the "other" Huskers will make us too proud any time soon. It is a sad time, when the defense is not even up to blackshirt standards, and have to lose them.

H.


This really explains a lot. I was keeping my condenser water wide open figuring it would just knock everything down but I guess you want what is coming down to be warm. Round 2 Friday with playing around with it some more,, Thanks Man!
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Re: Second run (w/ Fractional Reflux operation instructions

Postby john442 » Thu Apr 05, 2012 6:02 am

These are some awesome instructions !...Thanks
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Re: Second run (w/ Fractional Reflux operation instructions

Postby freespirited » Sun Apr 22, 2012 1:08 pm

There are instructions here for every avenue. You just need to read. Stripping runs can be done at full power using a design that allows for condensing only the vapor on the take off port. There are no cuts to be made on a stripping run and you can collect to as far down as 25%.
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Re: Second run (w/ Fractional Reflux operation instructions

Postby XFABCALGARY » Wed Jun 06, 2012 7:07 am

running "as" a reflux system, to build a neutral

bookmarked for post number 4
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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
Rich
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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,

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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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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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