Equilibrium?

[jarheadshiner]

I look at Dad's method as a way of keeping the MAJORITY of the fore/heads from ever contaminating the packing. You may lose a slight bit of product overall but that is a tradeoff that is worthwhile. Some people add a heads trap and other contraptions in an effort to keep the fores/heads out of their column. I look at this no differently.

[humbledore]

I have to say this kept gnawing at me so I tried it with a sac run on a new boiler and a new boka head on my modular setup. I did the head per the standard design so that with the valve open no reflux returns to the column. I kept the valve open as it came up to temp. And I am not saying I'm a convert...but I will say that the fores came out pretty cleanly based on smell only. And I was still getting a pretty clear crossover from fores to heads. I then closed the valve down somewhat to get some reflux going. When it started to smell clean I closed the valve and put it into equilibrium. I didn't want to taste it for obvious reasons. but my experience is that when the heads smell starts to die down there is still some heads "sting" coming out. So after a while I took some more heads off at a drip and then ran the rest as normal. I am interested enough to try it again on a real run.

[DAD300]

Ah...Humbledore, you could smell you got the fores and some heads out...before full reflux...I give you great credit for trying it.

If you were still getting some heads smell, as you went to higher reflux, where do you think the remaining heads went?

As suggested in another post, I'll repeat this weekends run here...

Sugar head with rice for flavor, ~14%, plus two quarts of fients...13.5 gallons into keg boiler

Min reflux as the vapor reached the top of the column, 300ml of fores and a quart of "real" heads, then I added just a bit of reflux to get to my sweet spot of takeoff rate, next quart was weak heads, next three were pure hearts, next two were very light mix of hearts and tails, then tails...best five quarts mixed together make almost three gallons of drink.

Start through quart seven was all 95+. Hearts are just a very little sweet (rice influence). And when I say tails were light, I mean after airing they were undetectable by smell, but still a slight taste.

I will still advise, that the bad stuff comes off first and you should get it out of your still asap!

If you need to reflux heavier to get the abv you're after, at least bleed the fores and half your expected heads before increasing the reflux!

People keep saying the vapors stack themselves in a predestined order. They do! Until you condense them and send them back down the column. If you 100% reflux with fores and heads in the column, you just make it harder to detect them as the ABV rises. You don't concentrate them. You smear them so wide they are hidden.

After a few runs, you should know the quantity of fores and heads that are unusable in you normal charge. Get that amount out before using the amount of reflux your still needs to get the abv you are after.

Never, purposely, use a total or 100% reflux with fores and heads in the column...

I think it's just common sense. And, if nothing else, everyone should be willing to at least try it.

Earlier in this post, we went on about commercial oil refineries and their " tall thin columns" where they segregate the individual products of their distillation. I missed a key word here...segregate. In those tall thin columns they trap and segregate the bi-products such as benzine, butane, acetone and whatever...they don't keep refluxing them back through the other products.

We don't need that storage of the segregated elements, because we don't want to keep them. Get them out. Use them for fire starter. Continue your production of drinkable product without them...

Common wisdom here is that we tell people to save everything from a stripping run. In the realm of safety and better spirit runs, I wish we would start telling them to toss the first x% of product from a stripping run.

I don't do stripping runs as a general practice, but if I did, and I was there attending my still, and the first 8oz's smelled like acetone, I'd surely toss it. There's no way I'd purposely add it to the spirit run.

[DAD300]

I've had another thought on how to present/explain this to make it more logical.

Theorize with me. Let's say you have a still that produced 95% abv, with min reflux of 1:1, 3" VM with 3" takeoff, from fores to tails.

Would you still stop and 100% reflux to "stack" the column?

Or, would you just let the products come off in natural order?

[Cardinalbags]

Earlier in this post, we went on about commercial oil refineries and their " tall thin columns" where they segregate the individual products of their distillation. I missed a key word here...segregate. In those tall thin columns they trap and segregate the bi-products such as benzine, butane, acetone and whatever...they don't keep refluxing them back through the other products.

This will be my last post on this topic as it is starting to bore me that the science behind distillation principles are being ignored or twisted for ones own way of how they run their still.

Refineries use a shitload of reflux to purify the product into segregating the fractions in the columns. They just have multiple levels of reflux and reboil at the base of the column which is just not feasible for home distillers to replicate using our limited technology. how can i state this with any authority? Well just so happens I work in the refining industry and see it in action everyday.

They have much more flexibility in setting the temperature profile in the column to be able to reheat the lighter fraction so they move back to top of the column. They do not smear back through the entire length of the column. If it did, we would never be able to replicate product on spec ( and when we say on spec, it means that 95% of the product is the desired product and the remaining 5% is made up of the next lighter compound and the next heavier compound - check your propane tank.... its got some butane in there as well. in the industry its called giveaway)

The only reason product would smear across fractions is drawing too fast for the efficiency of the packing. We get too impatient waiting for the shit fores and heads to be drawn off in heavy reflux. They need to betaken off very slowly based on the technology available to us.

I would bet the value of my house that when tested on GC equipment, that i would have less fores and heads in my first jar of hearts by refluxing the shit out of it and taking my time pulling them out slowly than running with minimal reflux and taking off as much product as possible on the front end.

I am not arguing that you can't get a great product operating as DAD suggests, I am arguing the distillations principles at play here and how we work with them. I am most happy to take the extra time to draw the fores and heads off slowly before I get into hearts run. It keeps me at the still maybe a bit longer and away from having the wife give me items from her honeydew list... but ultimately allowing the science to work as intended based on the efficiency of my packed column to give me a cleaner product.

[Cardinalbags]

I've had another thought on how to present/explain this to make it more logical.

Theorize with me. Let's say you have a still that produced 95% abv, with min reflux of 1:1, 3" VM with 3" takeoff, from fores to tails.

Would you still stop and 100% reflux to "stack" the column?

Or, would you just let the products come off in natural order?

Products do not boil off in natural order. The mixture boils off based on the make up of the mixture....... That is just hard scientific fact. How many times have we heard newbies on here saying they want to monitor temperature in their pot still so they can boil off the methanol first, then raise the temperature slightly and then boil off the acetones and acetates? This is just wrong.

Maritimer already hit it right on the head with his reference to Raoult's law back on page 3 of this thread.

ok.... i said my last post was going to be my last on this topic.... i'll get off my soapbox now.

[DAD300]

I understand Raoult's Law...and I understand that our "mixture" and it's components are basically the same for every still charge and distillation of ethanol.

Raoult's Law is based on the components reaching thermodynamic equilibrium in a closed environment. When they reach equilibrium, the pressure of each component will "stack" the components in the column relative to the individual vapor pressure of each component(s) or mixture there of.

So, all the nastys, we want rid of, in the fores would be at the top of the column.

If you have a sealed vessel filled with half pure helium and half pure argon by volume, at rest they will stack themselves. Throw it about, they will mix and you have no longer be stacked.

We (by refluxing) disrupt Raoutl's Law by condensing (creating a liquid heavier than vapor) the nastys and sending them back down the column to mix with the vapor components coming up the column. Constantly changing the vapor/liquid mixture and disrupting the closed environment.

I said in my first post, the term equilibrium is misapplied to anything we do. Hobbyist, certainly no one on this board, uses Raoult's Law, to stack vapor components in a fractionating column for the distillation of ethanol!

No matter how nice you try to be...

To tell a noob, he'll get a purer/safer product (ethanol) by refluxing for 15 minutes or hours, while taking product at drops per second is wrong!

He will however, get a higher ABV reading on a simple Alcoholometer.

Alcoholometers have no idea what liquid you just dropped them into. They assume ethanol.

But, an alcoholometer will sink like a stone in fores or acetone...is it good or safe to drink just because it appears as a higher ABV?

Don't confuse refluxing to get a high ABV reading with removing the bad components within a still charge.

Don't confuse a high reading on an alcoholometer with purity of ethanol.

[humbledore]

I'm not a theory guy and I'm not experienced enought to debate it. But it sure seems to me like the idea of reflux is that as the liquid comes back through the packing, the top packing is cooler than at the bottom. Meaning, the lower boiling point components of the liquid will vaporize higher in the packing. They will not make it all the way down to the hotter packing below. And that's how the stacking gets done. now is there some kind of mixing going on due to liquid mixing and not perfectly boiling off at set points in the column? may be. Do I find the idea intriguing (sp?) that fores should just come out and have zero mixing with the other crap? Yes. Because while the vapor coming up does not boil off in perfect order as many have pointed out, it sure seems like the majority of it coming out first is the nasty stuff based off my limited experience.

[wv_cooker]

Boy ask for a simple explanation of equilibrium and get a complete education on distillation principles and personal choices of how to operate a still, lol. I for one apologize to the OP for us hijacking his thread but there is a good education to be had here. True scientific fact of the matter is that fractions come of the still by the order of their specific boiling points.

If you use a pot still for instance the first thing off is Foreshots, next heads, next hearts, tails and so forth. Now depending on your wash there are other compounds involved, for the sake of time and writing a book we know they are there and we know that we only want mostly hearts for our purposes, so we collect in the appropriate containers, do our cuts, and then blend back what pleases our personal tastes. We know using a pot we are going to be leaving compounds and fractions in our product as we don't have the ability to separate them efficiently in a pot still making a pot better suited for flavored drinks.

So now we decide we want a more neutral product with less taste, or even no taste at all. We must now at the hobby level, use a reflux or fractionating column to achieve this goal. How does this work, we fill our column with some type of structured packing and apply some type of condenser that will return liquid back down the column in the form of reflux. Here is where all the confusion and different theories get confused, the fractions heat to their specific temp and start out of the still just as though it were a pot and they head towards the take off. Fores being first will go right on out unless we apply coolant and create reflux, the problem is there will be other compounds that may be very close in boiling point that will start out as well if you let them go they will go right on with the fores and be thrown out as well.

This is why we equalize or stabilize our column and allow them to stack, now Dad says they don't compress but yes they do compress or we will use our new found word segregate in order back down the column. I have seen that some have the misconception that they smear though the packing causing smearing. This is not where smearing occurs, it occurs in the vapor phase when we try to take them off too fast, all of the fractions start to race toward the take off at too fast of vapor speed until they all start to mix and get turned back into liquid at the product condenser. Now depending on the type of still this can also be created at the reflux condenser how ever the returning reflux will be separated again once it reaches the column and packing.

The packing is used to slow the return of the lower temperature liquid returning to the boiler, allowing time for the higher temperature vapor to mix and mingle in the packing separating more of the fractions from the liquid, changing them back into vapor and allowing them to head back up the column. The heavier compounds of the vapor will stop at each temperature gradient in the column that corresponds with it's own temp allowing the lighter compounds to rise on up. That is what we call stacking the column. Now take them off very slowly and each one will rise to the take off in order, get impatient and try to take them off to fast and they will all race to the take off causing smearing.

Is it possible to use Dads method, yes very possible as the fores especially, will start out first just like on a pot still. Are there some stills better suited for this method than others, yes Dads Manu designed CC/VM type still as well as a CM, even an LM with the ability to stop reflux would be able to accomplish this method. At some point the column would stabilize once you turned the reflux back on, until such time you would have smearing until the fractions began to separate again and stack naturally back in the column.

I have a concern that we are confusing the issues for folks trying to learn the processes of distillation by trying to infuse our own concepts of how to properly run a still into a simple discussion of equilibrium. Yes fractions separate at their boiling points even in a pot still, with a reflux column they can be separated and compressed even farther. Some compounds will never leave the still, such as solids that get left in the packing and water along with still other compounds that are left in the boiler.

As a fairly Newb myself it is confusing enough trying to learn the theories and proper practices of safe distillation without trying to prove that our method or particular still is better than everyonelses. My simple suggestion to any one trying to learn is try it both ways, even better experiment with many different ways of running your own still and see what best suites you for what you want to make.

As to the OP equilibrium is as stated in the first few post's of this thread and to you and all others I hope this entire discussion has been enlightening for those wanting to learn. Sorry to all for the book but, all the different components of distillation takes many books to explain and is not answered in a few simple words as most think in the beginning! Happy Stillin!

[humbledore]

Well put wv_cooker. Don't want to confuse people trying to learn. I am enjoying the discussion though.

[Jacksonbrown]

A lot of misinformation in this thread that I don’t really want to buy into but for anyone reading through it all that actually wants to understand what they are doing I would suggest reading through “The Compleat Distiller’ a few times.

[Jacksonbrown]

I would also add that water is just another fraction in the mix. Think about it.

Why use reflux to only take out the water then just put it back again to drink it??? You may as well run a pot if your going to drive it like that (or at lease a packed column with no reflux for the whole run).

Also alcometer readings should be temp adjusted and read from under the meniscus (which is almost imposable using a parrot).

What do people think about parrots smearing.

[jarheadshiner]

Not to question your knowledge Jacksonbrown but maybe at least step over to the welcome center and introduce yourself properly before you continue. You're not gonna make a great first impression this way.

[Maritimer]

Hi Jackson,

Howdy do? and welcome.

I was surprised when you said to read the meniscus at the bottom, because I've always been told to read the top. Such instruments are calibrated to be read at the top of the meniscus for just the reason that reading the bottom is difficult, I would think.

When reading the gradations on a graduated flask, for example, you read at the bottom of the meniscus and the actual contents of the meniscus added to the contents of the flask is a tiny error. If you read at the top of the meniscus in a graduated cylinder, the volume of the missing liquid would be considerable.

M

[wv_cooker]

A lot of misinformation in this thread that I don’t really want to buy into but for anyone reading through it all that actually wants to understand what they are doing I would suggest reading through “The Compleat Distiller’ a few times.

Hi Jacksonbrown, as Jarhead has stated it is customary for all new members to give us a proper introduction at the welcome center. When you have done that I for one am excited to here a more complete explanation of your statements. As for the Compleat Distiller it is a highly recommended reading around these forums. I can also point to at least 2 participants of this thread that not only have read the new version but also have read the original version. I can also point you to a thread where the discrepancies between the versions were discussed and introduce you to a highly respected member of these forums that contacted the author and discussed those discrepancies with him. This leads me to wonder why we should take one book and one authors opinions as the absolute Bible for distilling alcohol.

Next I would agree that water in the wash is just one more compound as you have stated but I think the confusion comes when you state that we are removing the water. If you want say 8 to 10 percent alcohol all you have to do is drink the wash, otherwise we are trying to remove the pure ethanol from all the other compounds or fractions in order to compress it to a higher ABV and more pure product for our enjoyment. Now I wish I could jump right past the lower boiling point alcohols and get right into taking hearts there by leaving fores and heads behind with water and other compounds but as I am sure you are aware that is physically impossible at the hobby level. Or at least I know no method at this point.

As for reading the top or bottom of the meniscus on an alcoholmeter can you please explain what the very minute difference in those readings has to do with equalizing or stabilizing a reflux column, I am just slightly confused on this?

For your last question of how we feel about smearing in a parrot, I for one have a valve in the very bottom of mine that remains open until all fores and heads have been taken and actually allow a small amount of hearts to wash it out before it is closed and hearts are allowed to fill the parrot. By using this method I feel that any minute mixing of the fores and heads back in my product will be so nil as to have no effect on my finished product.

Welcome to the forum and we are looking forward to your expanded discussions!

[Jacksonbrown]

Perhaps it was a bit rude of me to barge in like I did and for that I apologise.
I frequent a lot of various forums and it bugs me when people are laying down the lore when they clearly haven’t done their homework.
It just makes it hard for other people trying to learn as they have to trawl through a lot of fiction to get to the fact.

You had me second guessing myself after your comments RE the Alcolmeter meniscus so I did some reading and tested my gear on 20°C water.
0% in the same plane as the surface and 6% at the top of the meniscus and quite easy to read with minimal parallax in a glass measuring tube.
Granted the graduated measurements are closer together at the bottom of the scale and my equipment might not be the same as everyone else’s.
The comment was in reference to people bragging about their purity. The motives of those people usually aren’t all that pure (excuse the pun)
I tend to work off vapor temp for driving anyway (adjusted for altitude). It might not be as fashionable as parrots but i think it still has merit.


I’ve got a lot of learning to do myself but I have read almost everything I can get my hands on. I work closely with process engineers and chemical engineers and a doctor in heat transfer and evaporation that I call on regularly.
I’ll always take the word of these people over that of the Hillbillies (of which I’m probably a member too )

[wv_cooker]

Just for a little of your enlightenment Mr Jacksonbrown at least 2 of the participants of these discussions in this thread do I believe hold degrees in some type of chemical engineering and one of those just happens to work in the distilling industry at the commercial level every day of his life. Another is a highly respected member not just these forums but most of the forums at the hobby level and as for me it is relatively easy to see by my name that I am one of those Hillbillies of which you speak and very proud of my heritage at that. Again I say welcome to the forums and we still await that introduction at the welcome center!

[Maritimer]

Regarding the meniscus, here is the instruction sheet for my hydrometer. The alcoholometer does not specify where to read the meniscus.

This discussion is taking on the eerie aspect of a Creationist vs. Scientist debate. As such, it is doomed to go nowhere.

Mr Cooker, comparing The Compleat Distiller to the Bible is backwards. It should be compared to Darwin's On the Origin of Species. DAD seems to be writing his own scriptures.

M

[DAD300]

Not scriptures for sure...but there is a huge difference between scientific laws, applied science and the hobbyist realm of alchemy we live in.

Few of use work in a laboratory, a few do have some really nice equipment and most of us can make a great drink.

I worry we use the mask of distillation being so damn scientific, that we scare people from trying anything for themselves.

Take a tour of a huge commercial distillery, and the poor tech's running some very crude 100 year old design stills have very little idea of what's going on. Yet, here we are at the hobby level with no qualms about citing Scientific Laws to validate techniques we are incapable of employing and with little or no applied testing. Then when someone does a little testing, he gets ridiculed for not being scientific enough.

Consider the simple idea of reading above or below the meniscus...even at a low ABV, your talking one percent ABV!!! I'm willing to bet that few of these alcoholometers are manufactured within 1%. None of us need to know + or - one percent.

Some of the papers I've read, say that reaching equilibrium, even in a laboratory setting, where temps can be controlled within half degrees is an "infinite" process. The slightest disturbance mixes the purest of the elements. They are talking about columns controlled within a half degree and with no forced reflux. Think forced reflux is a disturbance? I don't think two days with forced reflux will stack anything but your power bill.

So, I've run with an hour 100% reflux and with no 100% reflux. And I, see no difference in the finished product. In fact my nose and taste buds tell me the shorter the reflux period the easier my cuts.

My point is "try it for yourself." There is always more than one way! There is a multitude of misleading or misinformation. And none of our equipment matches any other.

Why do we use science as a detractor on some subjects and let so much misinformation fly on other subjects.

If the process can be simpler, safer and/or cheaper and achieve the same result (a good, safe drink), everything else is mental masturbation. And distillation forums are often a Glory Hole.

[DAD300]

Making jokes about Hillbillys on a distillation forum is pretty funny...without them prohibition would still be a reality. And I think most of the forums were started by them.

Anyway...Love you guys...just keep thinking...

[wv_cooker]

Now Dad I can agree 100% with everything you say in your last 2 post's. I too believe we try to be too exact with science and theories. Things do work a certain way because of science, and there are many ways of accomplishing the same goals. Can we reach a total and perfect equilibrium in a column at the hobby level, I seriously doubt it as there are too many uncontrollable factors in our equipment and environments. I can also imagine that even if we did as soon as we start taking off product we will disrupt equilibrium to some degree anyway.

Do fractions come from the wash in the order of there boiling points, yes. Can we stack them in a reflux column, yes they do it naturally. How long should we reflux to accomplish our goals, my answer would be however long you feel needed to accomplish your own personal goals.

What should we have learned, that if we are new to distilling we need to learn the basic theories and principles of distilling. That there is stabilization that takes place in a reflux column that is usually referred to as equilibrium. We also need to learn why fractions separate, at what temperatures, temperature gradients within a column and why that is important. We need to learn about smearing and what creates it, like being impatient and trying to push things to happen faster than they want to naturally. I could go on and on and write another book here but I think we see the jest of it.

The biggest thing that I agree with the most is that we all should experiment with different ways of running our equipment if for no other reason than knowing what that equipment is capable of and knowing all the safety factors involved with running it. These discussions to me have been very enlightening for a new distiller to learn from. I believe that everyone that has participated has given true and accurate information. I believe the discrepancies are in methodology and different ways of operating ones still. I don't believe that the science of distillation changes, I do believe there are many ways of accomplishing the same goals.

For those reasons I believe everyone should experiment and try different methods and even report back their findings so that we all continue to learn and become even better at our craft. I have thoroughly enjoyed this thread even though I feel we have totally hijacked the OP's original intent, and for that I apologize to him.

Thanks Dad for making our minds work and thanks to all others for your input!

[woodshed]

wv_cooker has it right. More people need to experiment with their equipment. Dad has made some really good points and comes very close to my own protocol, regardless of the science. Why send it back down if you can get it out ahead of time?

[Hound Dog]

I am apt to try it Dad's way a bit more when I get back up and running. My last runwas actually before this thread. I had a couple gallons of feints mixed in so i took off about a third quart right off the bat just because I was thinking along these lines. Then I did the standard reflux for a bit and took off a bit more. It was a good run. I will try it more because I am not too worried about loosing an extra bit of what I would not be drinking as heads anyway even if it didn't w ork.

But as far as reading your meter..... Really?......... You guys are that frickin' anal? I figure the cheap ass meter I have isn't that accurate to begin with. I use it for consistancy to know I'm in the ballpark of where I want to be. It's just for me and the wife to enjoy and get a little drunk on. Not like I have to pass a guberment regulatory test. Relax a bit yall.

[T-Pee]

First off, quit apologizing. This is an internet discussion forum and thread drift is where great information slides in amongst the answer to the OP. That said...

I'm finding out that there are so many ways I can run this rig of mine. With the plethora (good word, huh) of different builds being used, there's about as many ways to use them to get to the same general end. Everyone's contributions have been most appreciated and I've learned a lot with my one, simple question.

Thanks, all!

tp (don't stop here though)

[DAD300]

Oh...T-Pee, yeah, you started this....glad you got something from it...

[scree]

As a noob,Dad confused me by making perfect sense. I pulled out some rank smelling heads before refluxing. I then shut the valve and concentrated a bit more. The bulk of it was in the first shot however. I'm glad i didn't know any better and wasn't stuck in my thinking.

[humbledore]

Thread revival. I just want to point out that Dad is running a 3" SPP packed column. That's a lot of mass. There has been discussion on other threads that the mass/surface area of the SPP requires a longer heat up time than scrubbies (extra 30 min?), and during that time there is actually internal reflux going on as the vapors hit cooler packing and slowly heat it up and repeat the process. So by the time it gets to the top there actually *has* been some reflux to concentrate fores and even heads somewhat. I am sure this applies somewhat to a SS scrubbie packed column but I'm guessing not to the same degree. Anyway I add this not as a "gotcha" or anything, I found it very interesting and saw it as an extension of this discussion.

[scree]

I have a 5' x 3" column column full of lava rock, so l'm sure
I'm getting a good bit of reflux as well. But isn't that why we have columns?
Regardless, the lower temperatures during warm up will only allow specific vapors to make their way into the first shot.
There is no reason for a noob to at least not try it. I find it works well for me.

I've enjoyed this whole post and actually found agreement with both points of view. It really helped my understanding.

[DAD300]

Finding the best parts of "all" points of view is in itself a great thing. Everyone's equipment is just a little different. There are a lot of compromises in real world application of processes and we should always be learning.

In the past couple of weeks, from these posts and forums, I certainly learned that during the time it takes to heat a packing with more mass, I am refluxing longer than I thought. Unconsciously, the packing is doing it for me. Love SPP!

I also now see throwing a lot of heat at a scrubbie packed column, during heatup, as a bad idea...even with scrubbies I think there would be a benefit to slowing down the heatup.

On the other hand, I pot stilled some left over wash last night...yes pot stilled. And sure enough everything came off in the order I expected.

When I got done, the hearts were very, I mean very, very pure. I mean to say this stuff was GREAT! So much so, that it made me go, "@^%$ why do we even reflux for high abv?"

Well, the answer is to get better cuts, and that allows for a better consistency/repeatability run after run.

Why did this pot still run come out so good. I have to assume that after years of fermenting, my ferments are getting better.

But it served to remind me that fermenting, pot stilling, experimenting are all just aspects of distilling.

[T-Pee]

I guess my question at this point, which may or may not have precluded this whole discussion, is why isn't the term "equilibrium" in the Glossary?
Just about any thread regarding reflux uses the term.

tp