Equalizing a column or getting everything in the boiler upto temp.

[drmiller100]

.

-Fletching

Viscosity is a thing. The hotter the water the easier the molecules bounce around.

Also if you heat the top of the water amd don't stir the bottom can stay cold.

This has nothing to do with distillation as distillation can't start until the wash is boiling.

Above, you said:

“ The fluid in the boiler is all the same temperature. It is either below boiling temperature, at boiling temperature, or it is boiling. If it isn't boiling nothing is going on.”

So I heated up the water, showing that temps were different before boiling, at boiling, and while boiling. Also noted that water started boiling directly above the element first.

So please tell me how my post is irrelevant if it addresses the very things you were talking about.

Then, in this post, you said:
“Also if you heat the top of the water and don't stir the bottom can stay cold.”

One post you say that temp in the boiler is always the same and in another post you say that it will be different if you don’t stir.

Maybe I misunderstood what the discussion was about, but I thought it was about finding whether varying boiler temps while heating the still with an electric element played a larger part in waiting to pull fores/heads than charging the column did.

Was this not the original question in this thread?

So, are we in agreement distillation doesn't start until the wash starts boiling and vapor heads up the column?
And we are in agreement the wash is homogeneous and the alcohols and water are completely mixed?
Are we in agreement that once it starts boiling the wash Temps are uniform?

If the answer is yes to those questions then we agree how long we putter about slowly warming the wash up to boiling is wasted time??....

Maybe there is value in cooking the wash to get a Carmel taste or some other scent or something. I know nothing about flavors.

I think we aren't understanding each other.

I'll drop it.

[kimbodious]

My experience is that if I heat up slowly that it takes less time after reaching boiling point for the column to stabilise in total reflux. I get the tightest cuts this way. What I mean by “heating up slowly” is operating the boiler at the heating power setting that I use for hearts and not at full power. No doubt the nett period will be similar but the quality of the product is my measure of success.

I use the same principle for heating up for spirit runs on my pot still.

[shadylane]

Methanol will generally tend to come out of the wash quicker than ethanol,

I used to believe that. But it's not true.

[LWTCS]

Methanol will generally tend to come out of the wash quicker than ethanol,

I used to believe that. But it's not true.

100%

[drmiller100]

Methanol will generally tend to come out of the wash quicker than ethanol,

I used to believe that. But it's not true.

100%

Link?

[shadylane]

The search button is in the upper right-hand corner.

As too methanol, there's only a tiny amount made when fermenting a sugar wash.
I've been told that some fruit juice has more methanol than a sugar wash.
That's why I prefer chasing a shot with water instead of orange juice.

[LWTCS]

Methanol will generally tend to come out of the wash quicker than ethanol,

I used to believe that. But it's not true.

100%

Link?

Pretty good write up here:

[drmiller100]

>>>**On small scale reflux columns, there will be a small spike of methanol in the heads if the column is left in equilibrium (100% reflux) for a long while, <<<<<<

Great article!!! Thank you for sharing it!!

[shadylane]

>>>**On small scale reflux columns, there will be a small spike of methanol in the heads if the column is left in equilibrium (100% reflux) for a long while, <<<<<<

Great article!!! Thank you for sharing it!!

"if there is methanol present, it will be present throughout the run, with a higher occurrence in the tails as ethanol is depleted and water concentration increases. Its distillation is more dependent on how much water is present rather than simply comparing boiling points between ethanol and methanol."

[Saltbush Bill]

Excellent easy to understand write up Larry.......should be read by every Newb.

[Ben]

Ok, some measurements are in order, I haven't done this math in a while so if something is wrong someone should correct me.

Assuming a 3" column with a 60" height that is 424 cubic inches, or 6.95 liters.

Lets assume that what's in the column is pure methanol, it probably
So no... Can't fit that tablespoon of fores in your column. Not even close.

In that packed column is also liquid. How much liquid?

Have you personally run a reflux column?

Yes, as mentioned above 2 plate 4", pretty much exclusively these days. Which has nothing to do with what the column holds. The liquid volume is small enough to call negligible, but even if it wasn't it would be math beyond my level.

If you don't believe boiler temps vary wildly think about your hot water heater. As you draw hot water what is coming off of it doesn't automatically get colder as the boiler fills with cold water, it stays about the same. Strange, my tap water is about 58°, but my hot water will come out at 130 until the heater is empty... then it gets real cold real fast. It is not strange its just fluid mechanics. The same holds true in your boiler, until you actually hit boiling; then it takes a little time to stir up and the gradient becomes much smaller.

2 plates in a column does not equate to reflux. Does your still send some liquid back down the column? How much fluid do both of those plates hold?

In a real reflux column the amount of liquid is significant and is what I was discussing.

Yes, i will agree a pot still run in reflux will not consolidate heads.

Hot water heater are pretty simple. Google!!!!

Again if the wash ain't boiling you are not distilling yet!

Are you intentionally wasting peoples time or are you just very stuck on yourself?

One of the side effects of my large tube dephlegmator on my two plate setup is I dont achieve full reflux if I am boiling at more than about 40%n.

[Setsumi]

Methanol will generally tend to come out of the wash quicker than ethanol,

I used to believe that. But it's not true.

100%

Link?

Distillation Techniques in the Fruit Spirits Production
By Nermina Spaho

Good text to understand the 2 azetropes that methanol foms. In a high alc environment it forms azetrope with ethanol in a low alc environment it forms azetrope with water.
Edit, high alc as in reflux still vs potstill. But present throughout the run as said.
Page 16, if i remember correct. Sorry, not page 16, look for fig 5 and 6 and read around there.

[EricTheRed]

That article should be in required reading

[shadylane]

Long story short.
It's not because of methanol that we dispose of foreshots.
It's to get rid of all the other nasties.

[Hügelwilli]

Only because firewater shows one paper that support his opinion doesn't mean that everything he writes is true.

For example that he mentions acetone at the first place when writing about foreshot compounds shows that he doesn't have much knowledge about the subject. Acetone is not a major congener in spirits.

And some conclusions are arbitrarily: First he writes how the demethylizer column works. Now he could come to two different conclusions:
1. This is the only way to remove methanol and cannot be done by homedistillers.
2. This is the most economic way to remove methanol. Other ways can be done by homedistillers.

He decides for No.1 without giving us any reason.

Fact is that methanol is more volatile than ethanol above around 50%abv. This means every plate or theoretical plate at over 50%abv concentrates methanol. When you have a reflux column it needs only a few plates to get over 90%abv. Then the absolute volatility of methanol is around 1.5 or 1.6. This means that for example ten plates at over 90%abv will result in a total absolute volatility of around 60 (ten times 1.5 multiplicated by itself). This means, you have 60 times more methanol in one gramm distillate than 10 plates further down.
This calculation is valid only if the total methanol concentration is low. The higher it is the worse is the concentration of methanol. So in practice it is probably a bit less than 60 times.

I posted many resources about the volatilities of all kinds of congeners here: https://homedistiller.org/forum/viewtop ... 8#p7623540 In five of them you can find volatility data of methanol.

[Sporacle]

So from all this I'm figuring that I heat gently, stabilise till I think I've got it stable, run it to where it performs how I like it and then make my cuts so the stuff I drink I like

[Dancing4dan]

Distillation Techniques in the Fruit Spirits Production
By Nermina Spaho

Good text to understand the 2 azetropes that methanol foms. In a high alc environment it forms azetrope with ethanol in a low alc environment it forms azetrope with water.
Edit, high alc as in reflux still vs potstill. But present throughout the run as said.
Page 16, if i remember correct. Sorry, not page 16, look for fig 5 and 6 and read around there.

Interesting article. It supports what others here have said about the variables involved in distilling off methanol. Pot still vs column still makes a difference in what part of the run methanol is removed. And how each still is run will have a big impact as well.

People like to speak in absolutes. “Methanol is in the heads” or “Methanol is in the tails”. From reading the articles sited in this thread…. There are no absolutes!

After reading this I have a better understanding of my reflux column and what is going on inside of it. I will be stabilizing the column for a bit longer before initial production and perhaps again toward the onset of tails.

Time at temperature must an impact on distillation.

[Hügelwilli]

Distillation Techniques in the Fruit Spirits Production
By Nermina Spaho

Good text to understand the 2 azetropes that methanol foms. In a high alc environment it forms azetrope with ethanol in a low alc environment it forms azetrope with water.
Edit, high alc as in reflux still vs potstill. But present throughout the run as said.
Page 16, if i remember correct. Sorry, not page 16, look for fig 5 and 6 and read around there.

I don't find terms like "azeotrope" or "azeotropic" in this pdf. Also I don't see a high abv reflux distillation. This pdf doesn't say anything about high abv distillation like the OP does. And even if ethanol, methanol and water would be able to form two different azeotropes, what would this mean for distilling spirits? Nothing I think, because we never would have a such high methanol concentration to reach those azeotropes.

[Setsumi]

Distillation Techniques in the Fruit Spirits Production
By Nermina Spaho

Good text to understand the 2 azetropes that methanol foms. In a high alc environment it forms azetrope with ethanol in a low alc environment it forms azetrope with water.
Edit, high alc as in reflux still vs potstill. But present throughout the run as said.
Page 16, if i remember correct. Sorry, not page 16, look for fig 5 and 6 and read around there.

I don't find terms like "azeotrope" or "azeotropic" in this pdf. Also I don't see a high abv reflux distillation. This pdf doesn't say anything about high abv distillation like the OP does. And even if ethanol, methanol and water would be able to form two different azeotropes, what would this mean for distilling spirits? Nothing I think, because we never would have a such high methanol concentration to reach those azeotropes.

From the Spaho article...

"Methanol appears in almost equal concentration in all fractions of distillation due to the formation of azeotropic mixtures [39, 40]. It is really difficult to separate the methanol from the ethanol-water mixture. When low alcohol mixture (like fruit-fermented mash) is distilled in simple pot still, methanol will go out following his solubility in water rather than his boiling point. Methanol is highly soluble in water, therefore, methanol will distill more at the end of distillations, when vapours are richer in water. That means that methanol will accumulate more in the tail fraction [7, 32],during distillation in alembic pot still as it showed in Figure 6."

"When high alcohol mixture distills, methanol will evaporate following his boiling point and will be present in the first fraction of the distillation in higher concentration. It appears mainly in the head fractions when distillation column was used [21]. Results of Cortes et al. [32] showed the concentration of the methanol was seven times higher in the case of industrial distillation (means higher concentrates and cleanses of ethanol) than the concentration of methanol in the distillates obtained by simple pot still."

To me both azetrope and reflux is addressed in the portions of text copied. I will agree that the reflux discussed is a plated still that will in all probability not produce 96% but it is presented as a still capable of much higher % than a potstill.

This study relates to fruit distillation, a commercial enterprise that research methanol in spirits because it impacts on safety of product and it is regulated.

My reference to this was to 1) show that a stabilizing period as hobby stillers use in reflux stills are benefitial to product and within academic reason. And 2) to show that fractions does not vaporize one by one but in a changing continuum.

[Hügelwilli]

I am sorry setsumi, I looked at the wrong pdf. I thought you mean the pdf firewater linked. My fault.

The quote refers to two other studies "[39, 40]". One from the author himself, I downloaded it and there is nothing to find about methanol. And the other one states the same thing but refers to another study, that I don't find online: Orriols, I. (1994). Tecnologı´a de la destilacio´n en los aguardientes de orujo. Proceedings I Congreso Internacional de la Vitivinicultura Atla´ntica.

My problem is, that it makes no sense. And here they say there is no such azeotrope: http://www.ddbst.de/en/EED/AZD/AZD%20Et ... BWater.php

Whatever, azeotrope is defined as a mixture that cannot be concentrated further by simple distillation. And because there is such a thing like a demethylizer we know, that it is possible to concentrate it further, at least when the methanol concentration is as low like in normal spirits production.


That a stabilizing period at 100% reflux helps to separate the compounds better, I think, is obvious when you look at the thermometer at a LM- or VM-reflux column: When the vapor arrives the temperature shoots upwards an then slowly drops down again a bit. So at least while the temperature drops, the 100% reflux helps to concentrate the foreshots. If longer, we don't know.

[drmiller100]

Yeah, the article can be read to support any argument.

With 36 inches of marbles I've got a lot more plates than the guy running a 4 inch column with 2 shelves which don't hold any fluid.

Another thing is it doesn't matter how slow or fast you heat the wash. Nothing magic happens if you take 2 hours to bring the wash up to boiling.
Further, I believe you are better to boil the wash as hard as you run it normally as you concentrate the heads.
The heads come out of the boiler because of boiling. Not evaporation.


s

[Saltbush Bill]

The heads come out of the boiler because of boiling. Not evaporation.

Can anything really go up a column because its boiling? As I see it, it cant go anywhere until it evaporates.
In short if the heads don't evaporate they stay in the boiling wash.

Evaporation
/ɪˌvapəˈreɪʃ(ə)n/
Learn to pronounce
noun
noun: evaporation; plural noun: evaporations
the process of turning from liquid into vapour.
"snow cover prevents evaporation of water from the soil"
the process of something abstract ceasing to exist.
"thousands of employees witnessed the rapid evaporation of their retirement plans"

[drmiller100]

The heads come out of the boiler because of boiling. Not evaporation.

Can anything really go up a column because its boiling? As I see it, it cant go anywhere until it evaporates.
In short if the heads don't evaporate they stay in the boiling wash.

Evaporation
/ɪˌvapəˈreɪʃ(ə)n/
Learn to pronounce
noun
noun: evaporation; plural noun: evaporations
the process of turning from liquid into vapour.
"snow cover prevents evaporation of water from the soil"
the process of something abstract ceasing to exist.
"thousands of employees witnessed the rapid evaporation of their retirement plans"

Yeah, terminology is tough. Years ago many people on this site thought you didn't have to boil to distill. They thought if you got the wash hot the steam coming off was all you needed.

To me, boiling is the rapid conversion from liquid to vapor. Further, to me you can boil agiven pot at say 1000 watts or 2000 watts, and there will be twice as much vapor at 2000 watts as there is at 1000 watts.

My word choice is distillation does not start until the wash is boiling.
To me, evaporation is setting the pot outside in a warm afternoon.

I understand different communities use words differently. If everyone else uses evaporation differently I will happily adjust

On edit.
https://byjus.com/chemistry/difference- ... d-boiling/

Part of my background are degrees in math and physics. I think of a pot full of wash starting to wash. Chaos theory and probability state that the lighter components tend to boil off (evaporate?) Faster than water. They are also less likely to turn back into liquid.
Various things influence this vaporization rate.
Temperature
Percentages. If you have .2 percent etoh in 5 gallons you are going to have a lot of boiling to drive that last bit out. How much boiling? Well, if you want it all, you have to boil the pot dry.
The limit as 1/x approaches infinity.
But the reality is that way sucks.

Anyway.....

[drmiller100]

I have a question on my continuous fuel still.

The top of my column is 170 and etoh and heads come out the top.
My boiler is 212 and my column drains down to the boiler. Let's say I run 20 gallons through. Where do the tails go?
Well, they have to come out the boiler.
Which means the temp drops a degree or so.
So now I'm at 211.
Does that lower temp mean a tiny bit of ethanol is making it out?

[drmiller100]

Common practice is to hold a column @ 100% reflux for awhile before taking off any alcohol.
Here's something I've wondered about.
How much of the advantage of doing it that way, is due to "stacking the column"
And/or how much is from entire boiler charge getting up to temp?

I don't think im making sense on evaporation.
Shadyside seems to be asking if he is concentrating the heads in the column as the wash comes up to boiling temp. To me, this is completely untrue.
As rhe pot is below boiling temp distillation is not occurring. Are there a few evaporation vapors coming off? Sure. But they don't matter. Nothing matters until the pot is boiling.

It doesn't matter if the wash used to be 40 degrees. It only matters once it starts boiling and significant vapor comes off

[Yummyrum]

Of cause the pot must be boiling during equalisation . There is a fuck ton of reflux pouring off the Reflux condenser .

[Saltbush Bill]

Years ago many people on this site thought you didn't have to boil to distill. They thought if you got the wash hot the steam coming off was all you needed.

Ive been here a fair while, I've never seen anyone claim that to be the case, on this forum or any others that Ive frequented.
Do you have a link to any such discussions?

[drmiller100]

Years ago many people on this site thought you didn't have to boil to distill. They thought if you got the wash hot the steam coming off was all you needed.

Ive been here a fair while, I've never seen anyone claim that to be the case, on this forum or any others that Ive frequented.
Do you have a link to any such discussions?

Well, the first post in this thread for instance.
Maybe I misunderstood it????

[Dancing4dan]

How much of the advantage of doing it that way, is due to "stacking the column"
And/or how much is from entire boiler charge getting up to temp?

How do you answer "How much of the advantage...?"

Stacking the column includes having the boiler charge and column up to stable temperatures so that a "fuck ton" of reflux occurs!

Kinda like the chicken or the egg...no one cares!

[drmiller100]

How much of the advantage of doing it that way, is due to "stacking the column"
And/or how much is from entire boiler charge getting up to temp?

How do you answer "How much of the advantage...?"

Stacking the column includes having the boiler charge and column up to stable temperatures so that a "fuck ton" of reflux occurs!

Kinda like the chicken or the egg...no one cares!

What does shadylanes second sentence mean? I HAVE to be reading it wrong.
And a guy above says if he slowly brings the wash up to temp he gets better cuts???? Why?
I'm sorry I'm not understanding.