Methanol concentrate in the tails according an EC study

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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Fri Apr 14, 2017 12:14 am

LWTCS wrote:Here is a little insight to whiskey run results with three separate systems.
A pot still is R1.
A two plate hybrid is R2.
And a six plate column is R3.

Note R3 how the Active Amyl Alcohols (esters) have increased in spite of more distillation cycles.
And R2 is a slight reduction on the Active Amyl Alcohols compared to pot stilling.

One might assume that the 6 plate system would eliminate even more of the Active Amyl Alcohols.
But it seems clear that the plates will ultimately entrain some compounds to the point where some of these compounds are actually more concentrated on a plated column. This is why plated columns do indeed make a flavored spirit even though abv can be quite high. And protracted refluxing can further promote esterfication and entrainment of esters on the plates even though the extra refluxing can enrich the abv.

For me R3 looks like a later tails cut, that's all. Not like a special plates thing. With all respect, I think it should be noted here, that LWTCS is selling plated columns.
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Re: Methanol concentrate in the tails according an EC study

Postby droo1966 » Fri Apr 14, 2017 12:28 am

Edwin, most people who want to separate different boiling point liquids by distillation use modified petroleum still design like the big companies do.


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Re: Methanol concentrate in the tails according an EC study

Postby LWTCS » Fri Apr 14, 2017 11:08 am

der wo wrote:
LWTCS wrote:Here is a little insight to whiskey run results with three separate systems.
A pot still is R1.
A two plate hybrid is R2.
And a six plate column is R3.

Note R3 how the Active Amyl Alcohols (esters) have increased in spite of more distillation cycles.
And R2 is a slight reduction on the Active Amyl Alcohols compared to pot stilling.

One might assume that the 6 plate system would eliminate even more of the Active Amyl Alcohols.
But it seems clear that the plates will ultimately entrain some compounds to the point where some of these compounds are actually more concentrated on a plated column. This is why plated columns do indeed make a flavored spirit even though abv can be quite high. And protracted refluxing can further promote esterfication and entrainment of esters on the plates even though the extra refluxing can enrich the abv.

For me R3 looks like a later tails cut, that's all. Not like a special plates thing. With all respect, I think it should be noted here, that LWTCS is selling plated columns.



I do sell plated columns.......
I also sell pot stills, and hybrid stills for that matter.

The data that I posted is a specific, and controlled experiment performed by a distillery that is not at all running any distilling equipment sold by me.
To the best of my knowledge the volumes, run speed, and heat applied for all three runs are the same.

The data shared is for the benefit of those interested.
I am not at all implying a "special plates thing". I am implying more specifically that most plate designs are inefficient to the point that congeners (good and bad ) do indeed get trapped on the plate. And some of those very same congeners do also get reinfused with forthcoming vapor.
My assertion is that 95 % ABV is not at all the same thing from a 10 plate (theoretical or otherwise) column compared to 95% from a 22 plate (theoretical or otherwise) column.

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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Sat Apr 15, 2017 12:02 am

But you don't sell packed columns or packing.
I thought the space between the notes is, that you want to point out, what plates can and packing not. Something like "why you can make whisky with plates but not with packing".
Sorry, if I misunderstood you.
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Re: Methanol concentrate in the tails according an EC study

Postby LWTCS » Sat Apr 15, 2017 5:53 am

der wo wrote:But you don't sell packed columns or packing.
I thought the space between the notes is, that you want to point out, what plates can and packing not. Something like "why you can make whisky with plates but not with packing".
Sorry, if I misunderstood you.


We do have many customers that utilize structured packing with our various sizes pipe sections.


My intention is more like,,,we have to often times exploit the inefficiency of our chosen system in order to express the best possible interpretation of the intended finished product.

And also in this example to illustrate that methanol doesn't really seem to be an issue in spite of the plated columns ability to accumulate/concentrate some constituents into the finish product. Nor does it seem to be an issue in spite of the pot still's antiquated ability to efficiently concentrate constituents.
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Re: Methanol concentrate in the tails according an EC study

Postby engunear » Mon Oct 09, 2017 5:16 pm

I finally scored some methanol. Only 25ml, but enough to do a test.

It is indistinguishable from ethanol using an eyeball and a nose.

Chucked it into a still with 1.5l headsy crap, and 5 liters or so of H20. 2m 1.5 inch (american) column, 650W heater. Full reflux to stabilize, then opened it up to about 2 mil per minute. This graph starts when the vapour first hit the top of the column. So temperature comes down as it separates the methanol from ethanol and water. To get a better graph, I probably should have left it to stabilize there a bit longer. It starts to rise when the needle valve was opened. Since there was only 25ml of methanol, it would not have filled more than the top few inches of the column, which is why the temperature does not get all the way down to 64.7C (bp methanol), which I think it would if I had 500ml of methanol. And it took 100ml or so to clear the methanol, as judged by the temperature slowly coming back to 77.8C (bp ethanol).

BTW, the headsy crap never gives full-reflux depression less than 0.5C, usually -0.2 or something not measurable.

The graph seems to show that the methanol has concentrated in the heads. If I left this running, it would sit on 77.8 until the ethanol ran out, then it steps up to 100C as it should, and we'd get a nice stepped graph.

I also scored some ethyl acetate, and am wondering if I can be bothered making a three-way mix. Maybe add some acetone for four. The ethyl acetate can be used to check some ethyl acetate hypotheses, but thats another thread.

Yes, I know that the paper is about pot stills, but a fractionating column is just a succession of pot stills. But short of getting a gas chromatograph, I can't see how else we could check the results & conclusion of that paper.

So I'm back to being confused.
Attachments
methanol-ethanol.png
Fractional distillation of methanol-ethanol mix
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Re: Methanol concentrate in the tails according an EC study

Postby thecroweater » Mon Oct 09, 2017 7:17 pm

doesn't get all the way down to the bp because once you mixed it its not pure methanol anymore but what you observed is very normal and where the great majority of that fraction will come off. A tiny percentage won't as compounds are compounds and stills will smear. :thumbup:
PS you a damn right about it being very difficult to differentiate between methanol and ethanol, takes a carful side by side to tell. Stories of bad taste and smell exist because folks mistake other compounds for methanol like acetone and acetate and other methyl alcohols.
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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Tue Oct 10, 2017 3:02 am

Down to 73.4°C. This is really interesting. There is still a great distance to 64.7°C. You say it's because it's only 25ml methanol. Possible, but not proven. But in any case it looks like a reflux column concentrates the methanol in the heads. For me the great difference of the lowest temp (73.4°C) to 77.8°C is a proof. So it's possible to reduce the methanol content of a spirit with a reflux concentrated fores cut.
Yes, the pdf is about potstills. Anyway, we distill with potstills and reflux stills. So your experiment is very valuable, even if your result is not valid for potstills. Could it be the opposite with potstills? Yes, it could. Looking again at the "Relative volatility of congeners and ethanol"-graph:
download/file.php?id=48559&mode=view
Methanol in under 40%abv is less volatile than ethanol, in over 40%abv it is more volatile. A potstill normally has under 40%abv in the boiler. A reflux still too, but the liquids in the packing are over 40% always, especially at the top of the column.

Thanks engunear. Again a great post.
An experiment with ethyl acetate would be interesting, because you can check it with your nose, not only by temp. But on the other hand we all know the glue smell and we all know from practice, that it is concentrated in the fores. And AFAIK there are no studies claiming the opposite.
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Re: Methanol concentrate in the tails according an EC study

Postby engunear » Tue Oct 10, 2017 6:25 pm

Thinking what to do next by way of experiments. To do the multi-liquid run properly really needs a data logger ... or a person with the patience to take a reading every 5 mins for 4 hours or so ... and that is not me. Maybe a Raspberry Pi + thermocouple setup one day.

But although you (der Wo) claim "everyone knows the smell of ethyl acetate", I wonder if thats true, as there are a bunch of stinky things that (perhaps) create our view of what ethyl acetate is, and it may be wrong. So next experiment is probably ethyl acetate plus base, but thats another thread.
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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Wed Oct 11, 2017 1:11 am

engunear wrote:But although you (der Wo) claim "everyone knows the smell of ethyl acetate", I wonder if thats true, as there are a bunch of stinky things that (perhaps) create our view of what ethyl acetate is, and it may be wrong.

Here I produced pure ethyl acetate:
viewtopic.php?f=1&t=67010
20ml acetic acid (20%) + 20ml ethanol (95%)
Smells like vinegar and ethanol. Adding 10 drops sulphuric acid doesn't change something. But after a while the vinegar smell disappears and more and more a glue/foreshots smell comes up. Nothing fruity. Exactly like the first jar coming from a reflux still after refluxing a while. Very nasty.
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Re: Methanol concentrate in the tails according an EC study

Postby Bagasso » Wed Oct 11, 2017 7:03 am

der wo wrote:But after a while the vinegar smell disappears and more and more a glue/foreshots smell comes up.

But, what kind of glue?
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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Wed Oct 11, 2017 7:17 am

All purpose adhesives for example. Like "Uhu" or "Pattex". But probably you have other brands in your country. Wood glue, glue sticks for kids and superglue smell different.
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Re: Methanol concentrate in the tails according an EC study

Postby Bagasso » Wed Oct 11, 2017 8:32 am

der wo wrote:All purpose adhesives for example. Like "Uhu" or "Pattex". But probably you have other brands in your country. Wood glue, glue sticks for kids and superglue smell different.

So you mean the white glue used by students for paper products?

I used some the other day and noticed that it doesn't seem like the same stuff I used when in school. The one my daughter has seems to be s little more like slime. It also smells different.

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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Wed Oct 11, 2017 8:45 am

Bagasso wrote:So you mean the white glue used by students for paper products?

I mean transparent liquid glue. Like UHU all purpose adhesive.
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Re: Methanol concentrate in the tails according an EC study

Postby Bagasso » Wed Oct 11, 2017 9:26 am

der wo wrote:I mean transparent liquid glue. Like UHU all purpose adhesive.

Just looked up the msds and it says "dangerous compounds: methyl acetate, ethanol and acetone". Seems to fit the description of heads pretty good.

And here I was sniffing school glue.
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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Wed Oct 11, 2017 11:26 am

Bagasso wrote:
der wo wrote:I mean transparent liquid glue. Like UHU all purpose adhesive.

Just looked up the msds and it says "dangerous compounds: methyl acetate, ethanol and acetone".

Probably methyl and ethyl acetate smell similar.
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Re: Methanol concentrate in the tails according an EC study

Postby Bagasso » Wed Oct 11, 2017 11:37 am

der wo wrote:Probably methyl and ethyl acetate smell similar.

Wiki says methyl acetate smells like glue and ethyl acetate smells like pears.

I'm just gonna keep dropping sodium hydroxide in everything and not worry about it.
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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Wed Oct 11, 2017 12:15 pm

Bagasso wrote:
der wo wrote:Probably methyl and ethyl acetate smell similar.

Wiki says methyl acetate smells like glue and ethyl acetate smells like pears.

German Wiki says both smell fruity. And that both is used in glue production. But other sources say ethyl acetate smells like glue:
http://www.toxipedia.org/display/toxipe ... yl+Acetate
Ethyl Acetate is a colorless liquid with a smell similar to glue or nail polish that is used as an industrial solvent.
But when you scroll down a bit:
Ethyl acetate is a flammable colorless liquid with a fruity odor.
Strange, isn't it?
Whatever, I have let react ethanol with vinegar. Of course what I got was ethyl acetate. And smelled definetely not fruity.
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Re: Methanol concentrate in the tails according an EC study

Postby Bagasso » Wed Oct 11, 2017 1:12 pm

der wo wrote:Whatever, I have let react ethanol with vinegar. Of course what I got was ethyl acetate. And smelled definetely not fruity.

I think it has to do with the concentration. Maybe fruity and pleasant in small amounts and solvent-like in higher concentrations.

I was just curious because I have seen you make reference to the glue smell and was wondering which one you were talking about. I found a bottle of something called "liquid silicone" but it has no methyl acetate, just ethanol and acetone. Smelled it before looking up the msds and thought, "this doesn't smell bad". I guess the nose knows.
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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Thu Oct 12, 2017 2:45 am

Bagasso wrote:
der wo wrote:Whatever, I have let react ethanol with vinegar. Of course what I got was ethyl acetate. And smelled definetely not fruity.

I think it has to do with the concentration. Maybe fruity and pleasant in small amounts and solvent-like in higher concentrations.

I don't think. Glue is glue. Dilute a fores jar with alcohol and water. It doesn't get fruity. And in Borurbon or Rum (it is hopefully a low concentration) it also doesn't smell fruity. For me it's really strange, all the sources claiming it smells fruity, but obviously it's not.
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Re: Methanol concentrate in the tails according an EC study

Postby thecroweater » Thu Oct 12, 2017 7:12 am

the smell of pipe glue (PVC glue) is acetone, there will be other compound but that smell is acetone.
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Re: Methanol concentrate in the tails according an EC study

Postby der wo » Thu Oct 12, 2017 7:42 am

I just looked at the ingredients list of UHU. It's a mix from Ethanol, acetone and ethyl acetate. The base is polyvinylacetate.
Probably acetone and ethyl acetate is very similar in smell?
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Re: Methanol concentrate in the tails according an EC study

Postby Bagasso » Thu Oct 12, 2017 11:01 am

der wo wrote:For me it's really strange, all the sources claiming it smells fruity, but obviously it's not.

I think the answer is that not everyone senses things the same. There is a study out there that says that some people have a gene that makes alcoholic drinks taste bitter and those without that gene taste it sweet. Then there are those people that say cilantro tastes like soap when the rest of the world finds it palatable.

Of course this is a home distillers' site and nobody here (with two exceptions) is running lab tests on stuff.
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