So I'm posting in the STB section because that's how the extraction began. After lots of troubles with pulling other stuff along with the desired alkaloid, all of the combined sticky brown goo from lots of pulls was mixed with an acid solution. This ended up being ~600 ml of liquid @ a PH of 3-4.
This was strained twice through coffee filters to mitigate the wicked emulsion problems that had been plaguing this project. Theoretically this 600 ml of solution contained the majority of the desired alkaloid from 450 grams of MHRB. Through an unintentional process of distilling, all but 650 mg (the total yield of pure alkaloid so far) has been dissolved into this solution.
The PH was raised to 13 with the addition of a lye/water mix. After thorough mixing, the solution (now ~1200 ml) looked very much like coffee with a little cream.
There was a small amount of non polar solvent in the mix from all of the previous work done with this material.
So here's the weird thing- after sitting overnight, the solution was pretty clear (slight reddish tint) and there was a really thin layer of tan emulsion. Floating on and in the emulsion layer were lots of clear shards! These were removed with a spoon and allowed to dry. What are they? They sure look like beautiful, shiny, delicious crystals, but is that possible?
If the solution contained LOTS of alkaloids, could they precipitate at room temperature in the little bit of solvent that was in the mix? If not, than what are they? Whatever they are, they formed overnight as the solution was carefully strained.
Any advice will be greatly appreciated
Pokey the Perplexed