Yield vs EtOH Extraction Temperature

  • Thread starter Eskander
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Eskander

Eskander

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I'm looking for numbers on how much is being extracted with ethanol washing at different temperatures and if doing secondary washes is worth the effort. My current line of thinking is to do a fairly rapid anhydrous ethanol extraction on freeze dried material at -40F and then do a soak at higher temp to pull anything left. If you have measured it, please specify your conditions for EtOH%, bud fresh or dry, extraction time and how you are measuring concentrations before and after.

Better living though chemistry no?

-Eskander
 
Moe.Red

Moe.Red

5,044
313
Interesting question.

While I do not have the data to share that you ask, this is a process I have done a ton. I have a bunch I want to get thru the rotovap this weekend. I'll try to collect some data points for you as I go along.

I doubt you will get too many other responses, there are not a lot of folks out there that do not make money off this type of process that would be willing to freely share information. These types of threads do not gain much traction in my experience. People that know, don't share because it impacts them financially. It is what it is.
 
Eskander

Eskander

149
43
I guess I just assumed that with all the commercial extractors people are trying to sell, it would more or less be in a manual somewhere. I can't even find a solubility in ethanol vs temp curve which seems like it should be basic stuff. Looking for process details seems to get things more at the level of recipes rather than protocols but there has always been a stark divide between chemist/manufacturer and well... dirty hippie interested in this stuff. I did find this article that is interesting to consider the implications of. Realistically you would be forced to do a water wash after rotavaping off the methanol, but that might not be a terrible thing to do anyway and sep funnels are cheap enough. Might be able to just freeze the washed extract and then peal off the organic layer though. That or diethyl-ether to keep the organic layer fluid...

-Eskander

Download full-text PDF
 
Moshmen

Moshmen

8,218
313
Sounds like ur gonna be a busy guy this weekend moe ! Lol make no mistake about it I appreciate all the info you share ! Guys like you bring the chemistry side of things that is layman don’t really understand - but I’ve learned a lot from you already just how to treat different symptoms with different things - and geez so much from you already you don’t even know ! Thanks again
 
Moe.Red

Moe.Red

5,044
313
Cant read the full text on this tiny screen but in the abstract they are talking about using menthol and acetic acid to perform the extraction vs organic solvents.

I see no benefit to methanol over ethanol if you are going to use solvents, only drawbacks.
 
Moe.Red

Moe.Red

5,044
313
Sounds like ur gonna be a busy guy this weekend moe ! Lol make no mistake about it I appreciate all the info you share ! Guys like you bring the chemistry side of things that is layman don’t really understand - but I’ve learned a lot from you already just how to treat different symptoms with different things - and geez so much from you already you don’t even know ! Thanks again
Dude I’m blushing.

I have a crew coming over this weekend it’s gonna be all hands on deck. I’ve got 2 nice 4x8 tent harvests to get thru. I’m gonna press some and use part of that in the short path. Then a bunch of ETH extracting. We’ll see if I get it all done.
 
Eskander

Eskander

149
43
Cant read the full text on this tiny screen but in the abstract they are talking about using menthol and acetic acid to perform the extraction vs organic solvents.

I see no benefit to methanol over ethanol if you are going to use solvents, only drawbacks.
21% increase in yield with methanol:AA over ethanol seems non-trivial. Methanol will be faster to evaporate off but with the additional steps to remove and then recover the acetic acid, you are definitely at a loss in terms of time. Since you have some loss at every step in handling, that has to be considered too. It comes down to cost/benefit but most everything does.

-Eskander
 
Moe.Red

Moe.Red

5,044
313
Are they not talking about menthol not methanol? You gonna make me go to the basement so I can read the whole thing? Cant I just pretend I did? That’s what you do on the internet, right?
 
Eskander

Eskander

149
43
Are they not talking about menthol not methanol? You gonna make me go to the basement so I can read the whole thing? Cant I just pretend I did? That’s what you do on the internet, right?
Oh god... you are right. Menthol would be a shit show to remove. I'm not even sure at a glance how you'd do it other than a chiral binding ligand column and I say this with all my heart, fuck that. It also looks like the acetic acid would need to be reacted out and then washed out because its would solubilize cannabinoids in an aqueous solution...

Oh well lol...

-Eskander
 
extractoilminussixty

extractoilminussixty

270
93
I'm looking for numbers on how much is being extracted with ethanol washing at different temperatures and if doing secondary washes is worth the effort. My current line of thinking is to do a fairly rapid anhydrous ethanol extraction on freeze dried material at -40F and then do a soak at higher temp to pull anything left. If you have measured it, please specify your conditions for EtOH%, bud fresh or dry, extraction time and how you are measuring concentrations before and after.

Better living though chemistry no?

-Eskander

I’ve done my own testing, here r results:
(because I want to know how much of the waxes, fats, chlorophyll and other lipids, & undesirables are in room temperature oil VS super low temperature extraction used in CCell vape cart).

Same strain GSC Auto (Girl scout cookies) , 22% Thc Garden of Green breeder
two batch runs different temperatures…

Batch #1 Room Temperature 74f
GSC 74f , one OZ very dry & ground in hand crank nut grinder slightly larger than joint material !)
Everclear generic 74f 14OZs
Mix together in mason jar, shake several times over 25 min time period.
Result after “ALL” Micro bubbles disappear from ethanol & residual water evaporation on hot plate is…
6.6–7 grams black oil.
Net Yield ~ 24–25%

Batch #2 Using 10lbs dry ice inside of a food cooler placed above (on a metal screen) herb & ethanol filled Mason jars
for 3Hrs.
Cooler temperature minus -60f
Herb & Ethanol temperature -60f
Mix mason jars in cooler & leave in cooler for 25 minutes, stir 3 times.
Drain extract “ASAP” using 75u micron
bubble bag then 25u filter.
Result after “ALL” Micro bubbles disappear from ethanol & residual water evaporation on hot plate is…
4–4.3 grams golden oil
Net yield ~ 15.4%
Conclusion: So I’ve removed about 36% of undesirables mentioned above.
I have run this test using GSC, Tangiematic & Northern Lights with similar results ~ 34-36% of undesirables removed using Super Cooled QWET
Vapes great, even without emulsions or Terps added. Pic below
((Sorry I was so wordy, but I think the path is important))
 
2D706DA4 D261 44A9 B7A8 B403BC263E55
Dank.in.Donuts

Dank.in.Donuts

139
43
Interesting question.

While I do not have the data to share that you ask, this is a process I have done a ton. I have a bunch I want to get thru the rotovap this weekend. I'll try to collect some data points for you as I go along.

I doubt you will get too many other responses, there are not a lot of folks out there that do not make money off this type of process that would be willing to freely share information. These types of threads do not gain much traction in my experience. People that know, don't share because it impacts them financially. It is what it is.
can I use 70% Grain Alchohol for extraction or is that too low?
 
extractoilminussixty

extractoilminussixty

270
93
4.6 out of 5 stars 214Reviews


I have never used it, I only use 190 proof ethanol generic Everclear or Everclear.
It takes me a long time just to get the residual water out of 190 proof sitting in a small glass jar on my coffee plate warmer about 2 hrs min. , and this is after 95% of the alcohol has been evaporated off using electric skillet, fan and Pyrex square dish…
70% I believe would strip cannabinoids
(see article below using iso 70) , but it would take some time and a long long time to get all water residual evaporated out. (but I am positive it can be done)
The water appears as very very very small micro bubbles that you only see when stirring with a small toothpick or something like that, when you think you have it all out “you don’t” , keep going until all micro bubbles are gone.
Alternative is to cover it with a tissue but high up on a shelf and let it evaporate over several days then check on coffee warmer for any micro bubbles of water left.
Also unless you’re doing this in very sub chilled dry ice temperature -40 —-60f in a cooler you will pick up all kinds of fats waxes lipids and such. These will have to be removed by Winterization, which again requires a very high alcohol like 190 proof or more !!! (that is if you were going to Vape)
I’m just not an iso 91 guy, but from everything I read it will evaporate out 100% naturally or heat induced, but I would still put it on a hot plate or a coffee warmer until all micro bubbles do not appear anymore! It also has a low flashpoint another reason I don’t use it.
Everclear is food grade iso 91 is not. :(

Article:
3 minute QWISO extraction
A quick note on Isopropyl Alcohol: The higher purity of alcohol that is used, the lower amount of water-soluble materials will be pulled into your product. 70% Isopropyl Alcohol, available at the grocery store, is 30% water so you will pull much more water solubles using this strength versus a 99.9% ISO. Also, properly cured and stored cannabis will have between 10-15% water content as well.
Using a low strength 70% ISO will absorb way more unwanted impurities, making your final product far “dirtier” because of the water solubles that were pulled into the mix. More water also means a longer evaporation process. For the absolute best results, spring for the 99.9% Isopropyl Alcohol – your final product will be night and day better.”

Article: 190proof extraction
“Super Cooled QWET Wash For
Cannabis extraction”

I don’t use the ichibancrafter, I don’t reclaim. Alcohol and dry ice treated as expense!!! Don’t make enough of it, last me a long time vape in CCell cartridges.
 
Dank.in.Donuts

Dank.in.Donuts

139
43
4.6 out of 5 stars 214Reviews


I have never used it, I only use 190 proof ethanol generic Everclear or Everclear.
It takes me a long time just to get the residual water out of 190 proof sitting in a small glass jar on my coffee plate warmer about 2 hrs min. , and this is after 95% of the alcohol has been evaporated off using electric skillet, fan and Pyrex square dish…
70% I believe would strip cannabinoids
(see article below using iso 70) , but it would take some time and a long long time to get all water residual evaporated out. (but I am positive it can be done)
The water appears as very very very small micro bubbles that you only see when stirring with a small toothpick or something like that, when you think you have it all out “you don’t” , keep going until all micro bubbles are gone.
Alternative is to cover it with a tissue but high up on a shelf and let it evaporate over several days then check on coffee warmer for any micro bubbles of water left.
Also unless you’re doing this in very sub chilled dry ice temperature -40 —-60f in a cooler you will pick up all kinds of fats waxes lipids and such. These will have to be removed by Winterization, which again requires a very high alcohol like 190 proof or more !!! (that is if you were going to Vape)
I’m just not an iso 91 guy, but from everything I read it will evaporate out 100% naturally or heat induced, but I would still put it on a hot plate or a coffee warmer until all micro bubbles do not appear anymore! It also has a low flashpoint another reason I don’t use it.
Everclear is food grade iso 91 is not. :(

Article:
3 minute QWISO extraction

Excerpt—“A note on Purity​

A quick note on Isopropyl Alcohol: The higher purity of alcohol that is used, the lower amount of water-soluble materials will be pulled into your product. 70% Isopropyl Alcohol, available at the grocery store, is 30% water so you will pull much more water solubles using this strength versus a 99.9% ISO. Also, properly cured and stored cannabis will have between 10-15% water content as well.
Using a low strength 70% ISO will absorb way more unwanted impurities, making your final product far “dirtier” because of the water solubles that were pulled into the mix. More water also means a longer evaporation process. For the absolute best results, spring for the 99.9% Isopropyl Alcohol – your final product will be night and day better.”

Article: 190proof extraction
“Super Cooled QWET Wash For
Cannabis extraction”

I don’t use the ichibancrafter, I don’t reclaim. Alcohol and dry ice treated as expense!!! Don’t make enough of it, last me a long time vape in CCell cartridges.
What do you think about this product ?
It looks good but I thoight I would ask
I mean for $600-1000 is great I think considering the bastards were selling CO2 at 75k 5years ago now they are down to a few thou
 
Dank.in.Donuts

Dank.in.Donuts

139
43
what about extractohol has anyone used it for consumables?
anyone have directions on making a homemade CO2 extractor?
 
Dank.in.Donuts

Dank.in.Donuts

139
43
can I use 190 proof with 5% denatured and then wash again to clean out any chemical for comsumables?
 

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