I have decided to purify DMT extract using mini A/B procedure described in "SWIM's Psychedelic Cookbook", here is the outline:

- dissolve DMT in NPS (naphtha, heptane)
- pull with water (add enough acid to keed the water acidic)
- basify the water with sodium carbonate to pH 9.5
- pull with fresh NPS
- freeze precipitate

Unfortunately, there is a huge loss of product (over 80% !!) so I evaporated the aqueous phase (see picture).

This should be a mix of DMT acetate, sodium acetate and acetic acid.

How can I salvage the DMT?

My best guess is to redissolve this in minimum amount of water, basify, evaporate the water and pull with NPS.

However, maybe using acetone will be more efficient as it evaporates more easily and sodium carbonate is insoluble in it. I am however not sure about the sodium acetate.

According to table, sodium acetate is almost insoluble in acetone (0.5 g/kg) so it seems acetone will easily wash this residue once it's basic.

Are you sure you basified enough with the sodium carbonate?
Was there pH check on that 9.5?

Yes, I am sure. I have used a calibrated pH meter (which correctly checked pH 7 in distilled water as well as correct pH values in control buffer solutions).

I have even done three pulls with fresh heptane (20 + 20 + 15 ml). Both water and heptane were heated to 40 degrees centigrade.

I've used 250 ml separatory funnel and shook it quite vigorously for two minutes each time.

When initially moving DMT from NPS to water, the water turned basic several times indicating more freebase is moving into the water. I had to repeatedly add several drops of 50% acetic acid until the water stayed acidic.

Maybe salting the water will help shifting the equilibrium. Or maybe pushing pH up even more.

I cannot see an error.
I've never really worked with vinegar and sodcarb in those stages though. I'm using muriatic acid and lye instead.

Did you have success before doing that tek?

So far I always did a solvent wash (basic sodium carbonate) and then dissolved the impure DMT in warm heptane, separated from brown oily residue and recrystallized.

This also caused significant loss of yield though, like 60% or more, lowering the total yield from 1.1% to 0.4% or so.

I followed recipe from Swim's Psychedelic Cookbook to the letter, using analytical techniques but still it doesn't seem to work.

I expect losses like up to 20% from purification (the initial product is already pretty clear as I do DCM defatting and lots of filtration), but 60-90% loss is way too much...