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200 Proof Ethanol and Extractions...

Douglas.Curtis

Autistic Diplomat in Training
What's the longest you've found extractions to stretch before quality issues begin. What materials would someone expect to find extracted, from an extra long soak time? Personally, I'm a huge fan of qweth and my soak times are very short. This is research information for someone else.

I greatly appreciate any informative replies on this. Thank You!

:tiphat:Save
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
What's the longest you've found extractions to stretch before quality issues begin. What materials would someone expect to find extracted, from an extra long soak time? Personally, I'm a huge fan of qweth and my soak times are very short. This is research information for someone else.

I greatly appreciate any informative replies on this. Thank You!

:tiphat:Save

Good question! Pharmer Joe has run some really extended soak times below -50C, so I just asked him that same question via email and will report back.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Awesome! Greatly appreciated. :DSave

Joe says he doesn't know what the limits are at -50C to -70C, but he's done it as long as two hours without issues and that there was no reason to go longer, because they had a full extraction.
 

Douglas.Curtis

Autistic Diplomat in Training
Joe says he doesn't know what the limits are at -50C to -70C, but he's done it as long as two hours without issues and that there was no reason to go longer, because they had a full extraction.
:tiphat: This is exactly what I was looking for, without knowing it. Thank Joe for me, you both rock! :D :woohoo:
 

WaterFarmFan

Active member
Veteran
Joe says he doesn't know what the limits are at -50C to -70C, but he's done it as long as two hours without issues and that there was no reason to go longer, because they had a full extraction.

Hey GW. Might you ask Joe if he has a seen any water soluble or other nasties being picked up when using material with a higher moisture content and 200 ethanol at <= -50C? An example would be ground flower material at 25% moisture versus 5%. Thanks!
 

WaterFarmFan

Active member
Veteran
I have a few questions about distilling with 95% vs 100% alcohol. When 190 proof is cold boiled, does the alcohol vapor retain the percentage level of water? Or is alcohol vapor (before condensing) pure but then combines with water vapor that is separately condensed? Logic seems to dictate that the alcohol would boil first, leaving the water and concentrate behind, but that does seem to be the case (from my observations).

An example would be using 2L of 190 proof ethanol, which contains 100ml of water. If solution contains 50 grams of concentrate, and is allowed to cold boil down to "bumpy syrupy" stage of ~100ml, would the residual water and alcohol still be in the same ratio (19:1)? I ask because I see a difference when using 190 vs 200. 190 seems to always have a bit more residual water content (but no where near 100ml).

I understand that 190 proof is the natural level with interaction with moisture in atmosphere, and that steps must be taken with Extractohol to minimize water pickup. But how fast does this reaction really happen? Is this process (200 to 190) accelerated under vacuum? Would 200 proof still be 200 after -50c extraction and reclamation?

Thanks!

WFF
 

troutman

Seed Whore
Alcohol over 96% will grab moisture from the air if left exposed and dilute itself due to it being hygroscopic.

https://en.wikipedia.org/wiki/Hygroscopy

The easiest way to get 100% ethanol is to add a drying agent and distilling with a drying tube
attached to the exit vent of the still to prevent moisture from entering and ruining the final product.

The dry alcohol should be stored immediately in a closed bottle and only opened when needed.
 

WaterFarmFan

Active member
Veteran
Alcohol over 96% will grab moisture from the air if left exposed and dilute itself due to it being hygroscopic.

https://en.wikipedia.org/wiki/Hygroscopy

The easiest way to get 100% ethanol is to add a drying agent and distilling with a drying tube
attached to the exit vent of the still to prevent moisture from entering and ruining the final product.

The dry alcohol should be stored immediately in a closed bottle and only opened when needed.

Thanks Troutman. Did not know the term. I don't want to dry the alcohol myself, but was more curious about the properties. I think that 200 proof Extractohol is made with molecular sieve. I did a bit more reading and found this:

Molecular sieve for Ethanol Dehydration Process requires high level of purity in the range of industrial and food applications. Type 3A molecular sieves are considered as the most effective type to dry ethanol. In the ethanol dehydration process, the hydrated ethanol vapors are passed through the molecular sieve bed. As the vapors pass the sieve bed, in the very first step water gets adsorbed by the pores of the adsorbent structure. The process of adsorption continues until the possible water adsorption from these vapors gets completed or molecular sieve gets saturated.

The process of transferring the water from hydrated ethanol vapors to the activated molecular sieve occurs through an area or a zone where the reduction of water content carries from its inlet to outlet concentration. This master transfer zone provides one active bed for transporting the dehydration while another bed for regeneration. The movement from one bed to another is handled and controlled using the powerful valves and automation. The pure ethanol after the dehydration process using molecular sieves can be used as a fuel in automobiles and other useful applications.
 

G.O. Joe

Active member
Veteran
Does pot dry alcohol or does alcohol dry pot? What does cold boiling mean? If it's vacuum then you'd have to look up the vapor composition for that vacuum. Or vaporizing below boiling should obviously favor removing the alcohol.
 

WaterFarmFan

Active member
Veteran
Does pot dry alcohol or does alcohol dry pot?

Hey Joe. I would say that alcohol drys out pot. "Hygroscopy... is achieved through either absorption or adsorption with the absorbing or adsorbing substance becoming physically changed somewhat... as water molecules can become suspended between the substance's molecules in the process."

What does cold boiling mean? If it's vacuum then you'd have to look up the vapor composition for that vacuum. Or vaporizing below boiling should obviously favor removing the alcohol.

I think that I phrased it poorly. I was asking if the water content in 190 proof acts independently of the alcohol when under vacuum distillation. I do not want to separate water from alcohol, just trying to understand why some but not all of the water evaporates from my concentrate solution prior to purge. I use a mantle and glassware (@ ~200 micron) to vacuum distill down to a thin syrup consistency.
 

WaterFarmFan

Active member
Veteran
I think what I am asking about is the chemical attraction of water to alcohol under different conditions. If you boil 190 ethanol on a hot plate, does water & alcohol evaporate at the same ratio throughout the process? Is this different under vacuum?
 

zif

Well-known member
Veteran
~190 proof is the azeotrope, so yes, alcohol and water will boil off in that ratio. It looks like vacuum breaks the azeotrope. You can pull nearly pure ethanol around 100 mm Hg @ 33° C. So at that point you’d leave all of the water in your extract.

Looks best to start with dry solvent and material....
 

WaterFarmFan

Active member
Veteran
~190 proof is the azeotrope, so yes, alcohol and water will boil off in that ratio. It looks like vacuum breaks the azeotrope. You can pull nearly pure ethanol around 100 mm Hg @ 33° C. So at that point you’d leave all of the water in your extract.

Looks best to start with dry solvent and material....

Do you think that the concentrate ratio to alcohol/water can break the azeotrope? I have decarbed (190 alcohol) extract in a double boiler and watched temps with a thermocouple. It first rises to 190s F and then rapidly to low 210s F as it works through the boiling points. It will then shoot up, but I have removed at this stage and the extract is still a bit runny at room temp, which to me indicated there was still some water content, even after going over the boiling point. Just trying to square my observations with some hard science. Thanks!
 

zif

Well-known member
Veteran
^ This is almost certainly practically the case.

Azeotropes are tricky and may depend on the other compounds (e.g., terpenes). I suppose adding more dry alcohol should allow you to drive water down to any arbitrary level, though, by taking advantage of the azeotrope?

Take that with a grain of salt because although I like the theory, I haven't distilled spirits for a decade or more. And then it was for the spirits!
 

WaterFarmFan

Active member
Veteran
Thanks for the info. I use cured flowers that have ~10-15% moisture, but I freeze flowers to -70C and soak with -50C ethanol. I might get a bit of condensation during my vacuum filtering. Do alcohol and water maintain the azeotrope at different proof levels below 190? So, if 95% alcohol picks up a bit of water, which I assumed was the case every time that you reclaim and then reuse alcohol, and becomes 94%, does it behave differently?
 

WaterFarmFan

Active member
Veteran
More water = More chlorophyll pickup. :tiphat:

I totally get that, and it is why I take significant steps to keep temps in -50C range during extraction, but I am talking about tiny amount of residual water in concentrate after purge. After I started freezing flowers to -70C prior to extraction, I do not see one slight hint of green in my post-filtered solution, and this includes both 190 and 200.

I ran out of 200 proof and have used quite a few gallons of Everclear. Everclear extracts are a bit less stable at room temp vs 200, and I was just guessing that it was water content from the 190. Any other ideas? Thanks.
 

troutman

Seed Whore
Ordered some Calcium oxide (CaO) (aka quicklime) today to help me make 100% ethanol (C2H5OH). :)

Calcium oxide will react with water to create calcium hydroxide which is insoluble in pure ethanol and will
precipitate as a solid. Calcium hydroxide can be converted back into calcium oxide with about 580C heat.

C2H5OH = ethanol
H2O = water
CaO = calcium oxide
Ca(OH)2 = calcium hydroxide

Reaction:

C2H5OH (l) + H2O (l) + CaO (s) = C2H5OH (l) + Ca(OH)2 (s)

Simple distillation with a drying tube to keep water out will then afford me pure ethanol without any water. :woohoo:
 
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