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glad to be back! Got some crystals pics but I need help with id Options
 
MomentOfTruth
#1 Posted : 12/21/2015 1:13:19 PM

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So I did a very extensive extract of 114 g of Syrian rue and initially had problems getting precipitate using lye as a base. I kept all the liquids, reduced, filtered 25 time-ish until the basic liquid was just pouring straight through 5-6 coffee filters at a time. I spent hours doing it to make sure it was cleaner than clean! Then I baked some sodium carbonate and rebased with that and left it in the fridge overnight. I filtered it off today and this is what I found. Keep in mind that I originally did a manske with no results so there was already salt in the mixture. , anyways I added some more vinegar, reduced and rebased with sodium carbonate. I'm not sure what exactly I have here but it is absolutely beautiful regardless! Is this just crystallized carbonate or do the look like harmala crystals? Or even salt contamination?

Any input would be appreciated!!

Nice to be back everyone! Hope all is well and happy holidays!



MomentOfTruth attached the following image(s):
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image.png (1,039kb) downloaded 129 time(s).
image.png (1,015kb) downloaded 126 time(s).
Coinci-Transcendentalism
 

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endlessness
#2 Posted : 12/21/2015 5:39:12 PM

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What did you do with what stayed on top of the filters when you filtered after adding lye? Thats where most if not all of your harmalas should be.

I've never seen harmalas form visible crystals as a freebase, more like fine precipitation. I don't think those pictures show harmalas, probably some inactive salt. You can always try dissolving it in acidified water, seeing if it shines under UV, or use a TLC kit to test.
 
rOm
#3 Posted : 12/21/2015 10:12:26 PM

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This crystals remind me more also of salts recrystallisation too than harmalas who tend to do brown powder which wet simply is some brown clay like apparence. The HCL makes very tiny needle like crystles.. no huge cluster as far as seen. Now I never did the exact same extraction as you did ( using lye as well as carbonate, with sodium chlorides ).
Nice stalagmites nonetheless.

A few tests could settle this down.
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MomentOfTruth
#4 Posted : 12/23/2015 7:58:50 PM

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I dissolved the sryatalw all back into hot vinegar and filter and filtere. I also saved all the filters and I ended up retrieving all of the alkaloids.It appears the crystals that appeared in the jar were actually definitely salt crystals or something similar.) thanks guys!!!!
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