Thanks 😊

I'll earmark a sample of freebase solution for temperature cycling tests. It seems the reversible colour change displayed by my initial test precipitate was a peculiar anomaly.

On further examination of the CASBA-CIBLO precipitation it appears that the primrose-yellow suspension aggregates to form dirty orange masses as the solution settles. Much as one might expect, settling is more rapid with the more concentrated fraction.

Speaking of settling, I just decanted the solution of re-acidified freebase that fell on the floor. Despite slow filtering through a generous cotton plug, there was a couple of milimetres thickness of black 'harmala crud'™ sat at the bottom of the jug. This kind of highlights the value of patience in harmala extractions as this has had over a week's settling time. I'll be leaving the decanted solution to settle for a few more days to help clean that up - something any home winemaker should understand.

PS - thought I'd best mention, the repaired microgram scales turned out to be way off in the calibration tests, not to mention lacking stability. I'm still restricted to centigram resolution until this gets sorted out.

I find when doing the tek the "citric EA" jug will crash out a little more over a few days as does the based harmala jug. (only a small amount)

I usually decant the citric EA and use the harmala citrate goo for the next run. As for the FB harmala that crashes over a few days in the left over base jug, instead of being a nice white-grey harmala it too is a almost black crude harmala. I have no idea how much of it would be usable (could be worth a LC-MS). I always figured it was mostly impurities?

The reason I wrote up the tek to be as quick as it is, is because the end result is very decent purity and color (IMO) and can be done quick with very decent yields. One can always do repeat runs on spent material as well for a better yield. I guess I'm just impatient. The other reason for the quick tek as well, is, if you live in a country where harmala is illegal you can do it in a couple hours rather than having 'manufacturing evidence' sitting around for weeks.

I always figured it was just impurities in the base jug that crashed out when left for a few days or a week. At the very least it looks impure by color. I guess ammonia wash could clean it up and more harmala could be recovered?