Hello all:

SWIM is experiencing a frustrating setback during extraction and would appreciate any assistance.

Problem: The solvent that's being used, toluene, is not separating properly. After adding the toluene, mixing, and allowing time for separation, a thick purple-colored layer formed on top of the plant mixture, presumably toluene (same volume as went in), but also seems to have picked up unwanted materials, as it is difficult to pour off and separate from the top layer, and doesn't look ready to be poured off anyway.

SWIM is following pretty much the same tek as was used successfully and with no hitches last time, only instead of basifying water with NaOH crystals like last time, here a 50% concentrated solution of NaOH was diluted with H20 until pH 12, added to the acidic solution, and pH further adjusted by adding more of the 50% NaOH solution.

Basic Process:
H2O was acidified using glacial acetic acid until pH 3-4 and added into a 2L RB with the MHRB in it.
Next day, basic solution was prepared using the method above and added to the 2L
Afer ~18 hours, toluene was added, mixed, and here is where the problems were noted.

No separation occurred as expected - mixture was foamy, and top layer thick.

SWIM thought that the pH readings of the bark mixture after basifying were off, as the color was rather light, so into the RB was added additional basified water, here using NaOH crystals instead of the viscous 50% solution. The color of the bark mixture turned to the usual dark purple
This was after a hasty attempt to fix this by adding more solvent.

SWIM was working without their stir plate (/hot plate) (lost power cord..), so the RBF didn't get as much mixing in the beginning as would have been desired. SWIM thought that a coagulation of materials on the bottom of the RB might be the issue, and while chunks were found and broken apart, that still did not correct the problem.

Now SWIM is stuck. Thinking proper course of action might be to siphon off the top layer, regret that they used so much toluene already and that it's probably bad, then re-add the solvent, hoping that with only fresh toluene in the flask, no unwanted reactions are taking place.

Can anyone please provide some guidance as to what to do from here?
All help is much appreciated, and thank you

Dont throw anything away, nothing is lost.

I hope this helps:

https://wiki.dmt-nexus.m...eparate.2C_what_to_do.3F
https://wiki.dmt-nexus.m...2FDark.2C_what_to_do_.3F

Doesn't look so bad - at least there are two visible layers!

Definitely syphon off and keep the toluene. Put it into a tall thin container and wait for particulates to settle out.

Good luck!

When I look at the first picture, there seem to be 3 layers - water, emulsion and np. But it is not 100% visible. Is it the case? Or are there only 2 layers - water & something else? If so, the "something else" is containing bubbles of any size? Sometimes I had to use magnifier to ensure.
What others are suggesting depends on what case it is.

No way, there hadn't been any notification of rep[lies,was just going to kindly ask again, but you guys answered -- ah, tremendous amount of thanks!

@endlessness & downwardsfromzero : What a relief to hear. This was discouraging.. SWIM even ordered more bark out of frustration. Thanks for the encouragment and advice. endlessness, the links were very helpful. Thank you ...

@pete666 : good catch. There is an extremely thin layer above what otherwise could be said to be the top layer. It's only around the edges. SWIM would say it looks like how toluene should look after it picks up alkaloids. If SWIM could get to it, it would produce a yield, but it is so thin it would be virtually impossible to isolate.

Again, thank you very much for the help

Actually, pete666, you bring up another question --

SWIM was planning on using their FASA to precipitate out the freebase anyway -- would that still work in this situation?

If I understand, then the two main layers are water layer and emulsion layer? (Emulsion means it consists of bubbles)
Have you then broken up the emulsion to get just toluene? (without bubbles)
Without such toluene, you hardly can do anything else...

You should be able to fasa with toluene containting dmt freebase (I have not done it myself though). But the result is not precipitated freebase, but dmt fumarate.

Yes, there is the bottom aqueous layer and the top layer of emulsions.
SWIM tried breaking up the emulsions with a (small) spatula, turning on their stir plate with newly found cord, as well as adding a little heat. The stir bar wasn't working to break everything up, as after turning the stirring off, the emulsion layer still came back, with just slightly more solvent on top.
Can't even do FASA actually, as this top layer is far too thick to even filter. You're right the result is DMT fumarate. I was referring to the freebase which would be precipitated out as the fumarate.

SWIM will add more basified water, as the flask wasn't the ideal size to begin with. If this doesn't work, a mini A/B with the top layer will probably be the chosen course of action. That or splitting the mixture up into two flasks, then adding more water, and taking it from there.

Again, thanks !

I would separate the emulsion (turkey baster?), so you don't have to work with all when trying to break it up.
Then heating it to about 60C for about an hour could help. If you attach some vibrating device (mobile phone, aquarium pump) to the vessel when heated and gently stir it every few minutes, you can help it a lot.
Time is very important when solving emulsions too. If previous steps don't solve it, just put it aside for few days, with occasional gentle stirring. You may be tempted to solve it quickly and not wait, but this urge is useless when handling entheogens

And remember, it is always much easier to avoid emulsions than to break them up when they appear. If you select/design your tek properly, you can shake like crazy and won't have it