Infundibulum said:
OK....I need to apologise for some of the data and assumptions I have made so far. It is so easy to be carried over by experimental enthusiasm and "publish" any observations prematurely. The ultimate tests, such as bioactivities should be our guide and not and vague solubility data published here or there.
So, the white precipitate after ethanol washing of Manske precipitates was tested. To my great disappointment it was not only totally inactive to dose up to 1 gram, it also tasted very salty. In fact it IS pure salt, well done Infundibulum, you managed to separate salt contamination from harmala alkaloids..:lol:. And it makes sense, since the Manske precipitation is bound to have plenty of residual sodium chloride when dried, which is fairly insoluble in ethanol...
That made me laugh. First laugh I had all day.
I can’t stop laughing.
That’s funny.
It’s good you tested it and posted your results.
You know this type of thing happens to all of us. We do some experiment, find some results, and then publish them, and then….oooops….Look at my thread on DMT Fumarate. The very first post in that has a tech from SWIM’s notes that doesn’t even work! I was so embarrassed by that one. Several people tried it and wrote me saying it didn’t work. Then SWIM tried it, and sure enough, it didn’t work! But SWIM tried it before and it worked, so SWIM apparently wrote down something wrong in his notes while doing the test, and then like an idiot I posted the notes without it being tested again. To this day I’m not sure what SWIM wrote down wrong in that tech.
Oh, if you don’t want much salt contamination from the Manske tech here’s what you do:
After extracting add 10% salt to your extraction. Bring it to a boil for about 30 seconds. Do NOT move it. Let it cool without touching it. When it cools down to room temperature, carefully move it to the refrigerator. That way the crystals grow more slowly and are far more pure. The difference can be dramatic. If you add salt and mix and don’t bring it to a boil, the harmaline and harmine start precipitating too quickly and form around pieces of salt and you can have your final product contaminated with as much as 50% salt! But if you follow my guide, salt contamination will go down to about 5% or less, especially if you re-crystallize a few times in salt water.
This works because harmaline HCl and harmine HCl are practically insoluble in cold 10% salt water, are somewhat insoluble in room temperature 10% salt water, but are quite soluble in boiling 10% salt water. If you don’t bring it to a boil after adding salt, some tiny harmala crystals form immediately after adding the salt. That’s a bad thing. When you bring it to a boil, all the salt dissolves, and all the harmaline HCl and harmine HCl dissolve. The boiling solution will have no crystals of salt or harmala alkaloids it in. The salt will stay completely dissolved as it cools, but the harmala alkaloids won’t. If you don’t move it, the molecules slowly navigate towards each other and form nearly perfect large crystals. If you move it, this causes tiny imperfect crystals to form that will have a lot of the solution trapped between them.
Harmaline chloride is insoluble in ethanol and very slightly soluble in hot alcohol. The picture below is harmala alkaloids from Manske precipitation mixed in ethanol, then incubated at 100 C for 10-15 min. One can see the harmaline falling on the bottom (left pic), it is so white one can assume very high purity. The top layer contains the dissolved harmine and other crap. 
