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First FASA attempt yielding unexpected liquid results

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Hi, I tried the FASA approach with 2 recent Xylene pulls of IPA/basified water mix (ph ~12) and have had some odd results. I took my Xylene pulls (performed after 3 heptane pulls) combining them and making very sure that there was no water layer or drops in the jar before adding FASA. I put in a few pipette droppers of FASA and it did get cloudy, I let it sit overnight, added more FASA in morning & let sit again. Now nothing more precipitates out but what had originally precipitated out is present as a liquid. There is now a thin layer on the bottom of the jar, slightly darker than the Xylene above. I'm sure this is what has resulted from adding the FASA but it is a liquid not a solid. Anyone got any possible explanations or ever experienced the same?
 
I was sure that the acetone had all the water removed. I made a batch of anhydrous acetone with magnesium sulphate, took some of it and added fumaric acid. It's been sitting for a while though and the seal of the bottle was a little loose though I didn't think any moisture could get in. I'm still not sure that it would be sufficient to explain this though.
It looks like it it aqueous contamination, at least I can't think of an alternative, is there any way to recover the spice?
I was using IPA as I extracted the mimosa using a soxhlet and was using IPA as its reportedly the most efficient extraction liquid to use. IPA was diluted, basified and pulled with heptane & xylene.
 
Ah that explains it. Never looked into soxhlet techniques, myself.

One thing SWIY could try to do in order to recover the extraction, is to evap, basify, and recover as freebase. Try this with the liquid on the bottom. Otherwise SWIY could try putting that liquid in the oven at the lowest setting.
 
Last night I put the Xylene and aqueous liquid in the freezer to see what effect this would have & in the hope of easily seperating the layers. The result is interesting in that a large number of decent size thin shard-like crystals/ice emerged, spread fairly evenly through the Xylene not just stuck to the bottom. I don't know what these are - frozen acetone? frozen DMT fumarate salts and acetone? something else?

There is (visually) a lot more volume of ice/crystals than I'd expect from the size of the thin liquid layer on the bottom. I'm going to separate the crystal/ice and evap it though I've just found out that the IPA I used (99.9%) doesn't extract DMT very well & it needs to be more dilute to work effectiely, so it could be that the whole extraction is flawed & there's no spice there to start with. I suppose this'd explain the lack of salts precipitating out. I'll investigate further.

Thanks
 
The crystals have now evaporated down to yield a small quantity of yellow, mostly hard but waxy in places residue which smells of DMT. Presumably this is DMT Fumarate, though how pure I don't know. I'm leaving it to see if it dries out further but I estimate about 50mg, quite a small yield.

I don't know how the yield measures up with what's expected/what others have achieved, but its better than nothing, which is what I'd thought I'd get. I don't know the chemistry, or even if excess water was the problem, but its possible that freezing of FASA'd Xylene which has yielded only liquid is an effective recovery method. Don't know how much was lost of course so it would require further experimentation - hopefully not by me though as I'll be making very sure my acetone/FASA is devoid of all moisture before I try this again. It is also possible that it was due to the fact that the Xylene pull was from IPA rather than base water.

If anyone has an understanding of the chemistry or what has happened here I'd love to hear it.

I've just found out that the IPA I used (99.9%) doesn't extract DMT very well & it needs to be more dilute to work effectively, so it could be that the whole extraction is flawed & there's no spice there to start with. I suppose this'd explain the lack of salts precipitating out.
Click to expand...
This is a very peculiar aspect - as no DMT was present in the heptane pulls I made of the same bark, but some was present in the Xylene- it could be that that n-oxides were pulled out by the 99.9% IPA & then present in the Xylene but not Heptane.
 
I'm currently testing my FASA, I dissolved 10mg DMT freebase in clean Xylene adding FASA from the same bottle as previously used to check if there is excessive moisture in the FASA. Cloudy precipitate formed but it hasn't settled yet.
 
I've ruled out excessive moisture contamination in the FASA - my test precipitated out DMT Fumarate as a solid with no liquid layer forming.
I'm concluding from this that the problem arose not with the FASA but due to the initial use of IPA. The only possible cause for the liquid layer I can see is that the Xylene pull of the IPA pulled out something in addition to the DMT alkaloids which then resulted in a liquid layer forming when FASA was added.
From this I'd say Xylene which has been used to extract from IPA is not suitable for use with FASA.
 
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