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Harmala extraction help Options
 
Xtal
#1 Posted : 3/16/2010 5:48:03 PM
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"Time is a river winding steadily through the landscape of tomorrow. There are those who would steal a glimpse around the next bend and those who would fight the current. But the wisest are those who turn their eyes from the waters and seek out a fellow traveler to share in the journey."

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endlessness
Moderator
#2 Posted : 3/16/2010 6:19:24 PM
first thing: You should definitely filter the liquid many times before saturating with salt, it will make your life much easier later on.

As for the precipitation, are you sure the water was really saturated with salt? How much salt did you add?

I wouldnt use NaOH, its such a strong base, im not sure how stable harmalas are if the solution gets too basic.. Plus its unnecessarily risky to work with NaOH in terms of personal safety if you can perfectly work with sodium carbonate

Anyways, without exact measures one cannot know the pH you got there with your NaOH , so its hard to say what that is.. It could be just a bit of harmine precipitated, it could be all of harmine+harmaline, who knows.. maybe raising the pH could precipitate the rest, but I would use sodium carbonate instead

And to recover the precipitated harmalas you HAVE to use a filter as thin as a coffee filter otherwise they will pass through (in something like a cotton funnel).. Thats why you have to filter a few times in progressively finer filters before the first precipitation, so that most filter clogging stuff is gone before you really need to use the coffee filter...

So you can try to decant most if the precipitation is on the bottom, but at least the last bit you will have to filter (or, get rid of most liquid, redissolve precipitation in acidified liquid, filter many times, and then precipitate again with sodium carbonate)
 
Xtal
#3 Posted : 3/16/2010 11:23:16 PM
.
Everything this user types is a lie.

"Time is a river winding steadily through the landscape of tomorrow. There are those who would steal a glimpse around the next bend and those who would fight the current. But the wisest are those who turn their eyes from the waters and seek out a fellow traveler to share in the journey."

Any first person pronouns refer to SWIM.
 
endlessness
Moderator
#4 Posted : 3/17/2010 12:00:05 AM
it could be vasicine and vasicinone, the unwanted alkaloids from rue.. Im not sure at what pH they precipitate, but seems too low pH for harmine/harmaline, if the reading is correct.. if you raise it up to 9 or 10 then the other alks should precipitate also, then you could redissolve, filter, and I would recommend saturating with salt and precipitating that successfully at least once because its this step that gets rid of vasicine/vasicinone.. What you do is have your harmala solution in a pot, boiling, and keep adding salt and mixing until no more dissolves.. add some more just in case, and then just pour this solution into another container for precipitating in the fridge, leaving the undissolved salt behind..

then redissolving that precipitation and filtering once more and then precipitating with the base at the end will yield you a nice quite pure product

good luck and tell us how it went. dont throw anything away, because if anything goes unexpected it can mostly always be recovered
 
Xtal
#5 Posted : 3/17/2010 1:30:56 AM
.
Everything this user types is a lie.

"Time is a river winding steadily through the landscape of tomorrow. There are those who would steal a glimpse around the next bend and those who would fight the current. But the wisest are those who turn their eyes from the waters and seek out a fellow traveler to share in the journey."

Any first person pronouns refer to SWIM.
 
 
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