MHRB Soxhlet Extraction

[Trickster]

There is more than just dmt acetate and water at this point.
Next step would be a defat with naptha.

This would be your typical A/B but replacing the 3 boils with a more efficient way of removing alks from the plant matter. So at this point it's the normal A/B steps.

So, SWIM proceeded as follows:

1. Diluted the extract with DH2O + vinegar ( pH ~3.3).
2. Defatted twice with heptane.
3. Basified with diluted lye to pH = 12.6.
4. Did 4 pulls with heptane with a sep funnel.
5. Got about 80 ml of yellow reddish opaque heptane.
6. Let it sit at a room temp for a day.

Now she has got around 60 ml of heptane (some of it evaporated) separated into 3 layers. A very thin dark oily looking liquid at the bottom. A layer of heptane with fluffy flakes in the bottom half of the glass. An upper layer of clear yellow reddish transparent heptane. Now what? Decant, filter and discard the precipitate and oils and freeze-precip yellow-reddish heptane?

 

[D_Juggz]

The biggest problem swim was having with the first run was drainage, by packing down the powdered bark too much. Try to put the bark in as loosely as possible, making sure the soxhlet body is dry on the inside when you put the bark in. (otherwise it gets stuck everywhere)
SWIM ran the sox for 9 hours with a full chamber, and the solvent still wasn't completely clear. If you have a large amount (ie. >100g) I'd recommend running it for at least 10 - 12 hours.
Plz correct me if i'm wrong.

Trickster:
so you have 3 layers?
is that heptane/emulsion/water?
I'd say do a freeze percip to see how much product you can filter off that way, then dry out the rest for changa?
Plz let us know how you go.

 

[voidwalker]

can anyone help me ? my extract is sitting here for days and i don't know how to proceed. please.

 

[D_Juggz]

Ok, so you have your solution of black stuff right?
Do what trickster said:
1.water down with distilled water + vinegar to get ~pH=3
2.defat with naptha swirl, decant (do this twice)
3.for the third time, add naptha diluted with lye to get ~pH=12 (which means the DMT will move into the naptha.
4. Do ~4 pulls with the basified naptha

 

[Trickster]

The biggest problem swim was having with the first run was drainage, by packing down the powdered bark too much. Try to put the bark in as loosely as possible, making sure the soxhlet body is dry on the inside when you put the bark in. (otherwise it gets stuck everywhere)
SWIM ran the sox for 9 hours with a full chamber, and the solvent still wasn't completely clear. If you have a large amount (ie. >100g) I'd recommend running it for at least 10 - 12 hours.
Plz correct me if i'm wrong.

SWIM uses a Continuous Solid Liquid Extractor described in another thread here and has no experience with sox. There is no cycling similar to Soxhlet's. The CSLE requires some fine-tuning of the hotplate temp so it is not overflowing but it seems much more efficient. Usually in 2 hours the solvent is completely clear. SWIM runs the CSLE for another 30 min to be on the safe side.

Trickster:
so you have 3 layers?
is that heptane/emulsion/water?
I'd say do a freeze percip to see how much product you can filter off that way, then dry out the rest for changa?
Plz let us know how you go.

SWIM's told me that it was heptane that separated into 3 layers. After 24 hours layers distribution stabilized and she decided to decant and filter it. She's got 60 ml of yellow-reddish transparent heptane and ~1 g (eyeballed) of jelly-like, slimy goo that also contained a few drops of black basified solution. The goo was evapped and now is waiting for further processing. It will be decided whether to do it or not after reducing heptane to ~1/5 of its current volume and freeze-precipitation. If yield ~1% is reached then the goo will be discarded. If not - then the goo will be diluted in vinegar, defatted with heptane, basified and pulled with heptane and so forth.

 

[D_Juggz]

Agh swim has been fucking around with this all night.
After two defats there were still some oils remaining in the naptha once it started to cool.
Swim evapped most of it and then put it in the freezer for a 2 hours until there were some crystals starting to form (was not sure if it was water or oil, but it smelt like dmt)
Swim tried to pour off the naptha and let the crystals dry, but as they heated up they just melted back into an oil...even after the naptha was apparently cone.
What remained was an oily goo.
Swim added a bit more warm naptha to dissolve it all, then added vinegar and dH2O, (which should cause the DMT to move across to the water)
separated the water which looked fairly clear, then added NaOH and naptha.
Agitated well and separated the naptha, then put it back in the freezer (100ml)
hope something comes up but swim thinks its a lost cause.

 

[Trickster]

Swim tried to pour off the naptha and let the crystals dry, but as they heated up they just melted back into an oil...even after the naptha was apparently cone.
What remained was an oily goo.

Did SWIY do that at room temp?

Swim added a bit more warm naptha to dissolve it all, then added vinegar and dH2O, (which should cause the DMT to move across to the water)

I think SWIY should have not used naphta at this stage, but just dried the goo and dissolved it in vinegar and dH2O. Some spice may have been left in naphta.

swim thinks its a lost cause.

Does SWIY still have that naphta around?

SWIM usually keeps all the by-products until the end of extraction process.

 

[endlessness]

Agh swim has been fucking around with this all night.
After two defats there were still some oils remaining in the naptha once it started to cool.
Swim evapped most of it and then put it in the freezer for a 2 hours until there were some crystals starting to form (was not sure if it was water or oil, but it smelt like dmt)
Swim tried to pour off the naptha and let the crystals dry, but as they heated up they just melted back into an oil...even after the naptha was apparently cone.
What remained was an oily goo.
Swim added a bit more warm naptha to dissolve it all, then added vinegar and dH2O, (which should cause the DMT to move across to the water)
separated the water which looked fairly clear, then added NaOH and naptha.
Agitated well and separated the naptha, then put it back in the freezer (100ml)
hope something comes up but swim thinks its a lost cause.

dont throw anythign away, your dmt doesnt just dissapear in mid air, so unless you threw something away its always gonna be there

btw if after this redissolving and pulling again you only did one naphtha pull there is probably alkaloids in your acqueous layer still, make another pull

I would suggest even smaller warm pull. If the one on the freezer yields no or little crystals, evap it some more and stick on freezer again

as for the problem of melting crystals, read this:

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

good luck and report back

 

[D_Juggz]

Haha cheers guys, i know ur right. SWIM evapped some of the naptha and it turned into this brown DMT smelling goo. Looked kinda nasty though so it was all discarded. I think the soxhlet pulled everything ok, but SWIM must have buggered something up after that...maybe not hot enough pulls? I dont know...will give it another try soon. Besides that SWIM kept what he reckoned to be some DMT acetate...will try to pull some from it soon.

 

[Trickster]

Haha cheers guys, i know ur right. SWIM evapped some of the naptha and it turned into this brown DMT smelling goo. Looked kinda nasty though so it was all discarded.

That was a mistake. SWIM carefully stored all the nasty stuff that her experiments produced. She combined all the goo collected at various stages and evapped it. Finally this morning after doing A/B for the second time and a lot of filtering/decanting she collected 410 mg of white snow. This is her cleanest product ever. And not a bad yield too (0.82%). The smell is so faint that at some point she was afraid that it is not spice. But it undoubtedly is.

I think the soxhlet pulled everything ok,

SWIM thinks it is not Soxhlet itself that pulls everything, but alcohols used as solvents.

i thought you guys would have figured this out by now: alcoholic extractions are never selective.
they'll pull anything that can interact in h-bonding

So, next time SWIM is going to use acidified dH2O instead of IPA. Yeah, IPA works, but it takes a lot of time to get to the final product.

but SWIM must have buggered something up after that...maybe not hot enough pulls?

SWIM does not do hot pulls and usually gets decent yields.

It is always better to do many small pulls than a single pull using the same amount of solvent.

 

[oetzi13]

Swim has been intensly beguiled by the sophex posts on this forum, and wants to put together a crisp system very soon. Originally he had a lot questions, but after reading here for weeks now he has answered most them himself. It's now time to get the parts. Often it is recommended to get a CLLE also. As a beginner, what is better to get? the lighter or heavier than water type?

Anyone here ever used one of these?:

http://www.edenlabs.org/home_light_commercial.html

 

[eindreizig]

Swim has been intensly beguiled by the sophex posts on this forum, and wants to put together a crisp system very soon. Originally he had a lot questions, but after reading here for weeks now he has answered most them himself. It's now time to get the parts. Often it is recommended to get a CLLE also. As a beginner, what is better to get? the lighter or heavier than water type?

Anyone here ever used one of these?:

http://www.edenlabs.org/home_light_commercial.html

Depends on the solvent used.

Heavier than water is for solvents heavier than water, like DCM, chloroform, etc.

Lighter than water is for solvents that are lighter, such as naptha.

I prefer DCM.