DMT-Nexus member
Posts: 329 Joined: 05-Jan-2013 Last visit: 02-Apr-2024 Location: tingüindolandia
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I have access to 96% etOH and distilling apparatus and I was wondering if running alcohol instead of water in THP would pull the goods with less volume. The alcohol can be then distilled off to make a very concentrated liquid that would be basified then pulled with NP solvent.
Has anyone tried this?
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Boundary condition
 
Posts: 8617 Joined: 30-Aug-2008 Last visit: 07-Nov-2024 Location: square root of minus one
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How do you plan to do this? Will you be adding base to your material to be extracted, and will this entail an acidic pre-soak? Or do you plan to make an alcohol pull to yield a concentrated extract which you will further process in some way? Either way you could use a soxhlet extractor. βThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work." β Jacques Bergier, quoting Fulcanelli
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Chairman of the Celestial Divison
 
Posts: 1393 Joined: 21-Jul-2010 Last visit: 11-Aug-2024 Location: the ancient cluster
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i do this procedure in a soxhlet, to get a crude extract, which is easier to work up in A/B. If you already have a distillation apparatus you might as well buy one Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
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DMT-Nexus member
Posts: 329 Joined: 05-Jan-2013 Last visit: 02-Apr-2024 Location: tingüindolandia
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Mindlusion wrote:i do this procedure in a soxhlet, to get a crude extract, which is easier to work up in A/B. If you already have a distillation apparatus you might as well buy one Great this is exactly the kind of response I was hoping. Can you please give more details? what's the alcohol to bark ratio, after getting the crude extract how do you process it?. I was thinking about reducing the alcohol extract via distillation to about 1/10 of the volume used for extraction, then let it air evaporate and dissolve the remaining solids in acidic water and then proceed like a normal A/B.
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Chairman of the Celestial Divison
Posts: 1393 Joined: 21-Jul-2010 Last visit: 11-Aug-2024 Location: the ancient cluster
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ymer wrote:Mindlusion wrote:i do this procedure in a soxhlet, to get a crude extract, which is easier to work up in A/B. If you already have a distillation apparatus you might as well buy one Great this is exactly the kind of response I was hoping. Can you please give more details? what's the alcohol to bark ratio, after getting the crude extract how do you process it?. I was thinking about reducing the alcohol extract via distillation to about 1/10 of the volume used for extraction, then let it air evaporate and dissolve the remaining solids in acidic water and then proceed like a normal A/B. well in a soxhlet you can use a very small amount of ethanol to extract a very large amount of bark. a 500mL soxhlet can fit 200-250g of bark and can extract with only 300mL of ethanol. the soxhlet cycles fresh ethanol each time through reflux, its also quantitative. I usually run it over night so its equivalent of running 50-70 times fresh solvent through the bark. outside of this you will probably only do 3-4 extraction cycles, and more solvent is necessary, i start with at least twice the volume to the bark. - for a/b i just reflux the tar in dilute HCl, or acetic acid with strong stirring. Sometimes it can be a bit tough to break up. Alcohol can also extract a lot of coloured components, so I usually defat too before basifying. This is my general technique not limited to MHRB Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
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DMT-Nexus member
Posts: 329 Joined: 05-Jan-2013 Last visit: 02-Apr-2024 Location: tingüindolandia
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Mindlusion wrote:well in a soxhlet you can use a very small amount of ethanol to extract a very large amount of bark. a 500mL soxhlet can fit 200-250g of bark and can extract with only 300mL of ethanol.
the soxhlet cycles fresh ethanol each time through reflux, its also quantitative. I usually run it over night so its equivalent of running 50-70 times fresh solvent through the bark.
outside of this you will probably only do 3-4 extraction cycles, and more solvent is necessary, i start with at least twice the volume to the bark.
Sounds easy enough. However I'd be worried about leaving it overnight because of possible bumping and things getting out of control when I'm not there, but I have never used a soxhlet so maybe that's not something to be worried about? Mindlusion wrote:
for a/b i just reflux the tar in dilute HCl, or acetic acid with strong stirring. Sometimes it can be a bit tough to break up. Alcohol can also extract a lot of coloured components, so I usually defat too before basifying. This is my general technique not limited to MHRB
About the tar, do you let the alcohol evaporate to leave a thick paste or completely dry?
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Chairman of the Celestial Divison
Posts: 1393 Joined: 21-Jul-2010 Last visit: 11-Aug-2024 Location: the ancient cluster
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ymer wrote:
However I'd be worried about leaving it overnight because of possible bumping and things getting out of control when I'm not there, but I have never used a soxhlet so maybe that's not something to be worried about?
Use magnetic stirring when refluxing ALWAYS. that should be commonly understood. At least boiling stone, Stirring is much better. Without it WILL bump and could cause a fire, especially if whatever your extracting thickens up the alcohol. a bit of alcohol is fine, you want to keep a little. helps the acid dissolve it. Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
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DMT-Nexus member
Posts: 329 Joined: 05-Jan-2013 Last visit: 02-Apr-2024 Location: tingüindolandia
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Mindlusion wrote:ymer wrote:
However I'd be worried about leaving it overnight because of possible bumping and things getting out of control when I'm not there, but I have never used a soxhlet so maybe that's not something to be worried about?
Use magnetic stirring when refluxing ALWAYS. that should be commonly understood. At least boiling stone, Stirring is much better. Without it WILL bump and could cause a fire, especially if whatever your extracting thickens up the alcohol. a bit of alcohol is fine, you want to keep a little. helps the acid dissolve it. Yup, my heating mantle has no way to adapt a magnetic stirrer and I don't trust boiling stones. I'll try to adapt a temperature controlled oil bath and do some tests for bumping before getting the soxhlet, getting a new heating mantle with magnetic stirring is outside of my budget. Thanks a lot for the advice 
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