ijahdan said:
Thought Id try reducing some mixed alks while I wait for the harmaline to settle after reprecipitation. Dissolved in vinegar, added zinc, left for 24 hours, filtered. When I started adding ammonia, at first, white clouds formed and disappeared. I added more ammonia, stirring continuously until the precipitate stayed. Then a strange thing happened. The brown goo started to form and stick to the sides of my container and the stirring spoon.
Managed to scrape it off and get it all floating again. Added some more ammonia for luck and left to settle overnight. Ill try to attach a picture. Looks like big brown crystally goo. The alks I started with were an off white fine powder.
I had similar looking gooey crystals forming in alks which were dissolved in vinegar and left in a cold place for a few days. This happened without any addition of base.
Could it be something to do with the low temperatures in my secret lab? Close to zero at night. Anyway, Ill redissolve, reprecipitate at room temperature and try adding the ammonia more slowly this time.
Will definitely try and get hold of a microscope.
This batch you had it precipitated before with ammonia without a problem, the only difference now is that there was a reduction step in between.
First white that disappears is normal and should be like that exactly, that is a good sign that your ZnSalts go to soluble Zincate :thumb_up:
Then the white that stays is the alkaloids precipitating, also very good.
If I look at that pictures it looks like brown yes, but not sticky? It looks non sticky brown, is it?
I've had some brown too before (not that much like yours) that was not sticky, I could easily remove it from the pH probe. I would consider this not a disaster.
But the real stricky-spook you just cant remove it easily because it is actually like glue, it formed a hard layer almost, now that was something else.
I'd like to know what kind of brown yours was please.
You said before that there was a lot of sodbicarb/sodcarb contamination that you removed with an acid/base (vinegar/ammonia) treatment, do you believe that all the sodbicarb/sodcarb was out? If there were still remains these might have added to the brown syndrome.
If I were you I'd just redissolve the brown in vinegar and re base with ammonia. Hopefully you get white THH because there are (quite) no zincate in the equation this time.
VDS added water in the cases that could lead to (sticky) brown syndrome, so perhaps making the solution less concentrated might help, worth trying I guess.
Keep us updated pls :thumb_up:
As for now, we don't know the exact reason why it sometimes appears and at other times it doens't. What we did find out was that when you stick to the experimental details in chapter 2 of VDS's paper, it stays away. So adding the ammonia slowly under stirring might be a good idea indeed. Yieldwise as well, it will surely help. Also, you could try keeping the concentrations of the reagents as similar as possible to the ones in the paper. You're so close, Ijahdan, good luck:thumb_up: !
