It's been a while I'm interested in this extraction method, and without any chemistry background, I tried it with a mix of 75 HBWR and 500 MG.
For sure I tried to study a little bit the procedure before, in order to understand the logic of it.
I definitively did the best I could, strictly following the method but I first had some strange issue after acetone pulls. The dry extract was like a brown gooey sludge at the bottom of my mason jar. Maybe it is because of that I encountered a biggest problem with the ending of the procedure.
I made it aqueous lsa citrate, filtered it, wash it 2 times with naphta but the water layer stills a little bit cloudy and grey/tan.
Remark: Removing the whole naphta with the syringe was difficult, cause a very thin naphta layer (1mm) was still at the top of the solution and despite all my effort to remove it, it was still there so I decide to let it float.
Then I add a pinch of ammonia having in my solution a ph between 9-10. 1 min later (maybe it was too much time because it is say to be fast) I took a 25 mL syringe and put 50 mL (25*2) of DCM and mixed the whole solution with a magnetic stirrer during 20 min. When I add the DCM the solution became very milky (same colour as a mix of coffe with a lot of milk). I let it sit a little bit, but there was no visible layer in it. I let it sit more (2-3 hrs) and it does not change... At this point I don't know what to do and how I could deal with this situation...
Maybe it's an emulsion problem? It seems that there is little transparent bubbles of DCM floating in the milky and cloudy solution but it is hard to make difference and I don't think it will be easy to grab these...
Some enlightened advice from someone experienced in extraction and/or chemical fields would be a great help!

Maybe it could help to put it into freezer and let it thaw again

If the worst comes to the worst, DCM evaporates pretty easily. It's somewhat toxic though, so that's best avoided.

Mixing DCM (heavier than water) with naphtha (lighter than water) may have produced a non polar phase that has approximately the same density as the aqueous phase, hence the difficulty in separation. If Twilight Person's suggestion of freezing hasn't helped, you may be able to pull everything out by adding either more DCM or more naphtha, to bring the density of the NPS into a range where it separates more easily.

Seeing as halogenated solvents like DCM are notorious for going into emulsion, I would be tempted to try adding naphtha. The DCM should keep any lysergamides in solution, even when mixed with a fair amount of naphtha (this works for mescaline, at least).

Thanks for the help Thwilight Person!

downwardsfromzero,I thank you too but it's too late cause I tried something just before reading your answer.
I did what you're saying about adding a little more solvent (DCM in my case) and it didn't seem to change anything...!
I searched a little bit more on the net and maybe it is not only because of emulsion that I couldn't see any layer but maybe it's due to the opacity of the whole solution (even with a torch I couldn't see beyond).
As I've red that the frozen point of DCM was -96° C, I decided to put the whole mix into a plastic bottle putted upside down into my freezer (-20°C). I logically thought that when the water will freeze I just need to open the bottle and collect my DCM bottom extract but it wasn't simple as that...
When I opened the freezer after more or less ten hours freezing, I could now see a distinct layer in my bottle (dark grey/green at the top, and my cloudy white at the bottom) but everything was frozen... ( maybe my dcm that is claimed to be 99.5 pure isn't or maybe it's due to the 10 hours freeze because water only need 4h?)
So I cut the bottle where the layer was and I keep the white and cloudy frozen bottom section which is normally my non polar-solvent. Now it melted totally (there still a very thin grey/green layer which I suppose is water and I can't remove it with my syringe) and I'm waiting for a total evaporation. After that I will add distilled water, tartaric acid and pure ethanol on it and I will see if it's shining blue under UV light...

Are you sure it's pure DCM? Sounds very odd... The emulsion microparticles may have become encased in ice I suppose. They would act as nucleation points for ice crystal formation.

The evaporation might lead to oxidation of your product - it's also best to avoid exposure to light.

Pure DCM is what I paid for but I can't be sure what I get is pure DCM... It doesn't seems to dissolve in casual tap water, it makes bubbles, and the taste is kind of sweet, so I think this is at least an apolar solvent. It's the only way I had to test the product!
Now it's not totally evaporated, there is a grey liquid layer that appeared on top of a white substance that look like cream in the bottom. I think this is a part of the extract. I'm wating for the total evap but I don't think I will consume it as the operation was a bit chaotic...!

You can check whether you solvent evaporates cleanly, and you can roughly determine its boiling point with a fairly straightforward experiment.


e.g., this link here. Scroll down to the bit that says "Thiele Tube Theory".


chem.libretexts.org seems overall to be a great resource for bolstering knowledge of practical chemistry techniques.

PS Please don't get into the habit of tasting your solvents!