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Unexpected results extracting harmalas? Options
 
nigredo
#1 Posted : 5/6/2018 8:24:47 PM
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An extraction of syrian rue went as normal. Cooked 3 times in acidified water. Basified, and precipitate allowed to settle. Said precipitate was then collected and and mansked 4 times.

Then what should have been the harmala salt was dissolved in 200 ml of vinegar. I expected it to go into solution and remain there. Instead, a precipitate formed shortly after mixing the solids with the vinegar. It settled down overnight in flakes.

I wished to oven dry at just under 100 degrees celsius. This was not a problem before as I'd used that same method to dry the precipitate right before attempting to redissolve it in vinegar. But with the new precipitate, heating it up resulted in more fluid. It was as though the solids were melting. I don't know any harmala salt to have a melting point so low, and I dried them with a container of water nearby to be sure that my oven was not heating up to much higher temperatures than stated. Unsure what was going on, I redissolved it all in water and added base to recover harmala freebase. It seemed to be rather potent suggesting to me that I was dealing with at least 80% harmalas there. I am at a loss as to why heating a paste produced so much liquid.

Does anyone know what happened?
 

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Jagube
#2 Posted : 5/7/2018 6:56:59 AM

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I don't know the answer to your questions, but you don't need vinegar to dissolve your Manske crystals. They're very water-soluble and if you use water to dissolve them, you'll subsequently need less base.
 
 
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