We've Moved! Visit our NEW FORUM to join the latest discussions. This is an archive of our previous conversations...

You can find the login page for the old forum here.
CHATPRIVACYDONATELOGINREGISTER
DMT-Nexus
FAQWIKIHEALTH & SAFETYARTATTITUDEACTIVE TOPICS
Soxhlet Question Options
 
Nathanial.Dread
#1 Posted : 4/1/2016 1:24:00 AM

DMT-Nexus member


Posts: 2151
Joined: 23-Nov-2012
Last visit: 07-Mar-2017
If I had a soxhlet, could I extract with a mixture of ddH2O and acetic acid (pH ~ 4)? I looked at some older topics, but couldn't find any kind of confirmation.

The acid should travel with the solvent, meaning that the bark/leaves/whatever was getting extracted directly into acidified water.

Then do usual A/B.

Blessings
~ND
"There are many paths up the same mountain."

 

Live plants. Sustainable, ethically sourced, native American owned.
 
Mindlusion
#2 Posted : 4/1/2016 1:42:46 AM

Chairman of the Celestial Divison

Extreme Chemical expertChemical expertSenior Member

Posts: 1393
Joined: 21-Jul-2010
Last visit: 19-Jan-2024
Location: the ancient cluster
You could.

Typically you wouldn't want to use a mixture like that (5% acetic acid). Even though it doesn't form an azeotrope, acetic acid is volatile enough and close enough to the b.p. of water that it will still work. (its hard to concentrate acetic acid by boiling or distillation, you need a very tall column).

Though, It would be much easier to use something like ethanol in the soxhlet. Make a crude alcoholic extract which you can distill off the ethanol, then do the A/B on that crude extract.

It is extremely effective in reducing the material you have to work with, and alcoholic extracts of natural products in a soxhlet will almost always give you quantitative yields.

I don't know about acetic acid, it may work just as well but could take a lot longer.
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."
 
Nathanial.Dread
#3 Posted : 4/1/2016 2:27:45 AM

DMT-Nexus member


Posts: 2151
Joined: 23-Nov-2012
Last visit: 07-Mar-2017
Thanks for the insight.

Do you have any off-the-cuff guesstimates as to what the minimum usable %EtOH would be? Everclear would be much easier to get a hold of than trying to track down anhydrous EtOH or distilling my own.

Would you acidify the EtOH solution in the soxhlet? If you could, it would basically save a step, you could treat the product like you were going STB (if I'm understanding this right).

Blessings
~ND
"There are many paths up the same mountain."

 
Mindlusion
#4 Posted : 4/1/2016 2:54:49 AM

Chairman of the Celestial Divison

Extreme Chemical expertChemical expertSenior Member

Posts: 1393
Joined: 21-Jul-2010
Last visit: 19-Jan-2024
Location: the ancient cluster
You don't want to use anhydrous in a soxhlet, its better used for other applications. Its going to absorb a bit of water anyway.
you want to use azeotropic. (about 95%) <-- that is everclear i believe.

No need to acidify, the ethanol will extract everything by itself. You are going to need to remove the ethanol by distillation or evaporation after the soxhlet extract. You can't treat it like water and add base, either. The freebase is soluble in ethanol anyway.
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."
 
blue.magic
#5 Posted : 12/24/2017 7:48:50 PM

DMT-Nexus member


Posts: 1104
Joined: 11-Feb-2017
Last visit: 18-Jan-2021
I think you have to use some other acid then acetic in your EtOH solution as acetic acid and EtOH form ethyl acetate (?).

I found some people don't even use acid at all for initial extraction. It may not be necessary for alcoholic extract as DMT freebase is soluble in ethanol. Ethanol will therefore pull both DMT salt and freebase. If you really want/need an acid step (e.g. for de-fatting), then you can mix your alcohol extract with acidic water, distill off the ethanol and continue with A/B extraction as usual.

I never tried that, but this method is described in one cactus analysis thread and works very well for mescaline.
 
downwardsfromzero
#6 Posted : 12/24/2017 10:20:53 PM

Boundary condition

ModeratorChemical expert

Posts: 8617
Joined: 30-Aug-2008
Last visit: 16-Mar-2024
Location: square root of minus one
blue.magic wrote:
I think you have to use some other acid then acetic in your EtOH solution as acetic acid and EtOH form ethyl acetate (?).

Very little ethyl acetate will be formed from mixing just ethanol and acetic acid without adding a strong mineral acid catalyst or a suitable reagent system to absorb the water which is also formed in the esterification reaction.

Quote:
I found some people don't even use acid at all for initial extraction. It may not be necessary for alcoholic extract as DMT freebase is soluble in ethanol. Ethanol will therefore pull both DMT salt and freebase. If you really want/need an acid step (e.g. for de-fatting), then you can mix your alcohol extract with acidic water, distill off the ethanol and continue with A/B extraction as usual.

I never tried that, but this method is described in one cactus analysis thread and works very well for mescaline.


From what I read in the posts preceding yours, the choice would be either/or, rather than both, with the greatly preferred choice being 95% ethanol. Do you have a link for the acidified ethanol cactus extraction? Is it any better than using plain ethanol?




“There 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."
― Jacques Bergier, quoting Fulcanelli
 
blue.magic
#7 Posted : 12/25/2017 12:25:15 AM

DMT-Nexus member


Posts: 1104
Joined: 11-Feb-2017
Last visit: 18-Jan-2021
downwardsfromzero wrote:
From what I read in the posts preceding yours, the choice would be either/or, rather than both, with the greatly preferred choice being 95% ethanol. Do you have a link for the acidified ethanol cactus extraction? Is it any better than using plain ethanol


Here: Mescaline quantification in live cacti using TLC.

See the attached PDF file, step 9). The actual tek is in the second half of the document.

The initial extraction is actually done in basified ethanol (since freebase mescaline is said to be more soluble in ethanol), then transferred to acidified water and then filtered.

I guess the water phase is added to remove water-insoluble impurities (there is quite a lot of them depicted).

So the benefit of using two solvents (EtOH, H20) is the opportunity to remove more impurities. I am not sure how that applies to DMT-containing plant material used by OP.
 
downwardsfromzero
#8 Posted : 12/25/2017 2:17:46 AM

Boundary condition

ModeratorChemical expert

Posts: 8617
Joined: 30-Aug-2008
Last visit: 16-Mar-2024
Location: square root of minus one
Thanks. The document is describing development of a tlc plate, though.
Quote:
9) After spotting, the plates are eluted with Bunk Police’s eluens. I think it’s 100/2
methanol/ammonia (24,5%).

That's rather different from a primary extraction in a soxhlet. Ammoniacal ethanol might be a way to go for cactus extraction but you'd need really good containment to prevent all the ammonia escaping during the several hours of reflux. Ditto for DMT extraction.




“There 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."
― Jacques Bergier, quoting Fulcanelli
 
blue.magic
#9 Posted : 12/25/2017 6:07:02 AM

DMT-Nexus member


Posts: 1104
Joined: 11-Feb-2017
Last visit: 18-Jan-2021
downwardsfromzero wrote:
Thanks. The document is describing development of a tlc plate, though.
Quote:
9) After spotting, the plates are eluted with Bunk Police’s eluens. I think it’s 100/2
methanol/ammonia (24,5%).

That's rather different from a primary extraction in a soxhlet. Ammoniacal ethanol might be a way to go for cactus extraction but you'd need really good containment to prevent all the ammonia escaping during the several hours of reflux. Ditto for DMT extraction.


No, that's the TLC part - look at the second part of the document, where is the actual extraction tek.

It's the second half of the PDF.
 
Ulim
#10 Posted : 12/25/2017 1:56:10 PM

DMT-Nexus member


Posts: 1023
Joined: 19-Mar-2016
Last visit: 31-May-2023
downwardsfromzero wrote:
blue.magic wrote:
I think you have to use some other acid then acetic in your EtOH solution as acetic acid and EtOH form ethyl acetate (?).

Very little ethyl acetate will be formed from mixing just ethanol and acetic acid without adding a strong mineral acid catalyst or a suitable reagent system to absorb the water which is also formed in the esterification reaction.

Thats true. If you have high water content the equilibrium will be shifted towards EtOH and acetic acid.

Iirc its like 60% ethyl acetate at room temp if you just mix 99% acetic and 99% EtOH.
The acetic will catalyze itself but rather slowly.
Also i dont expect that to even be bad. Ethyl acetate is a good solvent too.
 
downwardsfromzero
#11 Posted : 1/3/2018 1:43:13 AM

Boundary condition

ModeratorChemical expert

Posts: 8617
Joined: 30-Aug-2008
Last visit: 16-Mar-2024
Location: square root of minus one
blue.magic wrote:

No, that's the TLC part - look at the second part of the document, where is the actual extraction tek.

It's the second half of the PDF.

Oh, so it is - I've no idea why last time I looked only the first half of the document was visible.

It's a lovely piece of work that document. The crude extraction should work as a general method but the workup would have to be tuned to whatever the target compound might happen to be.




“There 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."
― Jacques Bergier, quoting Fulcanelli
 
blue.magic
#12 Posted : 1/3/2018 4:07:00 AM

DMT-Nexus member


Posts: 1104
Joined: 11-Feb-2017
Last visit: 18-Jan-2021
downwardsfromzero wrote:
blue.magic wrote:

No, that's the TLC part - look at the second part of the document, where is the actual extraction tek.

It's the second half of the PDF.

Oh, so it is - I've no idea why last time I looked only the first half of the document was visible.

It's a lovely piece of work that document. The crude extraction should work as a general method but the workup would have to be tuned to whatever the target compound might happen to be.


Yes I plan to reproduce the extraction for mescaline, but now researching how to employ similar process for MHRB.

Some say to use just ethanol, some basic ethanol and some acidic ethanol.

Why not to use say ammonia + EtOH for extraction. After Soxhletation, one need to just pull with nonpolar and then either freeze precipitate or backsalt.

Alternatively, one may soak the root bark in minimal amout of basic water, dry and transfer to Soxhlet for alcoholic extraction.

I guess the whoel point of acidic extraction is the opportunity to defat, right?
 
 
Users browsing this forum
Guest

DMT-Nexus theme created by The Traveler
This page was generated in 0.030 seconds.