Thank you for the experiment :thumb_up:
Elrik said:
... Supposedly the bicarbonate stage would precipitate only harmine and some of any DHH that might remain...When I came back at 40 minutes it looked like milk.
Don't forget the Zn salts, these are typical to form "milk" effects. Harmalas never gave me much of milk appearance but rather dust looking.
Elrik said:
...Is it the case that fully driving the carbon dioxide off from a bicarbonate basing will freebase all three alkaloids? If so how do we know when to filter to separate the alkaloids?...
It would have been more indicating if you had pH checks between the stages, we're kind of blind now. A pH meter is quite cheap, and even if the absolute calibration is a tad off, they are good for indicating pH-differences.
Especially working with carbonates, it has shown before that close sticking to VDS is important, but you are right that he did not mention much about stirring times.
I have a fair trust in the reduction process.
To free your products from Zn-salts, redissolve them both separately in vinegar, base firm with ammonia only this time. Filter. You can wash them with a weak carbonate flush.
About bicarbonate taking out the THH, this is surprising indeed.
Microscopic checking of the crystals formed (best in situ) could reveal something. But if we have no pH-data nor these images nor any other kind of identification then it's hard to say something. The VDS protocols surely would not expect us to take out THH on bicarbonate, only partly DHH as you mentioned.
If bicarbonate would take out THH, then it surely would take out DHH fully, which is not the case as we know so far.
The only thing you did in particular is the long precipitations times, as you mention that might be a factor not included so far.
For me this is just another reason to stick to ammonia only (+ pH meter), carbonates only added fuzz. But I understand the no pH meter style of things. But if so, we should have a reliable workflow and we find us a bit uncomfy now isn't it.
Hope An1cca jumps in on his thoughts.
*
On another note, I'd never pharma further with Harmine-THH combo only, something is missing imho. Last time was 150 harmine + 50 DHH + 50 THH and that was much more wholesome blend. So I would always keep some DHH un-reacted.
:thumb_up: