I was following gibran2's caapi tek, found here, but was substituting syrian rue for the caapi with the eventual idea of performing a manske after getting a pure harmala yield. These crystals precipitated from the combined decanted liquid which I got from the prior steps, which was basified with sodium carbonate and placed in the fridge for about 20 hours, and appear to be in excess of 100 grams weight (the container is about 20cm by 20cm ish). So, anyone know what these are composed of/how to purify any harmalas which are in here? I added quite a lot of sodium carbonate to the solution, so I figure these may be crystals of that with some stray harmala/plant matter caught inside, but I'd like to get the input of someone a bit more experienced with this process.
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Syrian rue extraction, what these crystals are/where to go from here?
- Thread starter qwerty310
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That's a really cool looking formation. I really don't know how much of it is harmala or sodium carb or acetic acid or what... how much starting material did you have? rue doesnt usually have more than 6 percent yield, so that puts an educated guess on the upper limit of how much harmala is in there.
looks like a good time to manske - I'd
1)dissolve it all in some vinegar / water mix
2)reduce the liquid to 1L
3)prepare 1L of salt saturated boiling water*
4)mix salt water and harmala liquid
5)leave mixture in the fridge for 24 hours, cooling it slowly in a cupboard first will promote larger crystals to form making the next step easier
6)filter out crystals
Optional:
7) dissolve manske crystals in minimal boiling or nearly boiling water
8) put this liquid back in the fridge for 24 hours to get purer manske xtals
9) repeat 7-8 as much as desired. I clean harmalas until there is no more nasty rue taste, which usually takes only 1-2 recrystallization.
*to prepare salt saturated boiling water, add salt(preferably pure nacl) to fully boiling water and mix until no more salt dissolves.
looks like a good time to manske - I'd
1)dissolve it all in some vinegar / water mix
2)reduce the liquid to 1L
3)prepare 1L of salt saturated boiling water*
4)mix salt water and harmala liquid
5)leave mixture in the fridge for 24 hours, cooling it slowly in a cupboard first will promote larger crystals to form making the next step easier
6)filter out crystals
Optional:
7) dissolve manske crystals in minimal boiling or nearly boiling water
8) put this liquid back in the fridge for 24 hours to get purer manske xtals
9) repeat 7-8 as much as desired. I clean harmalas until there is no more nasty rue taste, which usually takes only 1-2 recrystallization.
*to prepare salt saturated boiling water, add salt(preferably pure nacl) to fully boiling water and mix until no more salt dissolves.
Thanks for the advice:d , I'm going through the process as I type. I only started with about 56 grams of rue, so this definitely was a bunch of contamination from one of the steps, though it's sort of weird because the crystals don't really dissolve/react in either a based solution or vinegar without some additional heat.
If you only started with 56 g rue, I'd do one more base precip before manske actually. That means most of those crystals are actually impurities - Did those all precip? or did you evaporate a solution of sodium carbonate/acetic acid/rue tea?
Anyways, when you get the rue alks into solution, you should be able to recover them in fairly pure form by raising the PH to around 9-10 - probably 2-3 g fluffy stuff will precip, and then you can do the manske I outlined with much less water. Maybe reduce the tea to 200 mL and use 200 mL salt saturated boiling water. I use 1L each when I'm expecting 20-30 g of harmalas
Anyways, when you get the rue alks into solution, you should be able to recover them in fairly pure form by raising the PH to around 9-10 - probably 2-3 g fluffy stuff will precip, and then you can do the manske I outlined with much less water. Maybe reduce the tea to 200 mL and use 200 mL salt saturated boiling water. I use 1L each when I'm expecting 20-30 g of harmalas
All of this precipitated after about a week in the fridge from some sodium carbonate saturated solution. After a taste test (really bad, I know, but I figured since it was all food-safe reagents/solvents involved I'd be okay) hesitantly determined that what was in solution was mainly sodium bicarb/carb with a minute amount of harmala alkaloids/mystery coloring agents. Tried a basing step but nothing seemed to precipitate. The rest of my undertaking of this tek, with the non-discarded active liquid stages, worked out pretty well, though, yielding about 1.6-2 grams of freebase harmalas using ammonia as a basing agent followed by 4 water washes and drying. Thanks again for the advice, though, and now I know what to look for/do when I get to doing this again.
Nice, I'm glad ammonia worked for you and you got some cleanish hamalas. If a saturated solution of sodium carbonate didn't precip anything, my guess is that you tried to convert baking soda to sodium carbonate and it didnt work for some reason. Do any chemists around here know if sodium carbonate will spontaneously convert back to baking soda given enough time in air? Anyways, I have had problems with using sodium carbonate as a harmala basing agent for whatever reason and prefer to just use lye. A tiny amount of lye crashes all the harmala out very quickly so there is no waiting for soda carb to dissolve and wondering if its actually baking soda that didn't convert or whatever. I think using soda carb as base is the cause for the vast majority of failed harmala extractions.
off topic, but I'd like to try TSP to see if it will base harmalas reliably.
off topic, but I'd like to try TSP to see if it will base harmalas reliably.
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