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Freebasing harmalas from syrian rue with sodium carbonate - not all falling to bottom of jar Options
 
DesykaLamgeenie
#1 Posted : 10/17/2013 2:38:10 AM
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Hello everyone,

I did a simple extraction of syrian rue following this tek: https://wiki.dmt-nexus.m...Y_Harmaloid_Freebase_TEK

I've done this tek before and it went well, but I left it in salt form.

This time I decided to freebase it using sodium carbonate. So I dissolved the crystals in just enough water to completely dissolve them, and added a sodium carbonate-saturated solution. It quickly changed color, and I realized after the fact that I'd probably added more than necessary. (added all of the solution I'd made instead of stopping after the color stopped changing) The sodium-carbonate solution was probably 4 or 5 times the volume of the harmala solution.

Now, 24 hours later, a lot of the harmalas have dropped to the bottom of the jar, but a lot is still floating - suspended in the solution. And what's on the bottom isn't totally settled, either - when I gently rotate the jar, they swirl a bit.

Everything has separated, that's visibly clear - it's just not falling out completely.

Is it maybe just too thick? In which case I could add a little water to thin it out? (since I added probably 2 times more sodium carbonate solution than necessary?)

Or is that totally off...

Thanks in advance
 

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endlessness
#2 Posted : 10/17/2013 9:34:09 AM

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You can just filter it as-is to retrieve your alkaloids.

Decanting saves time on filtering but sometimes alkaloids just dont settle so you can go ahead and filter.

Investing in a vacuum filtering set up is not very heavy on the budget and VERY recommended. You can get the full set up in ebay or similar, or you can get the separate parts (You need a 500ml or bigger vacuum filtering flask, a buchner funnel, a stopcock of right size, filter papers and a vaccuum pump like the mityvac silverline )
 
Randomness
#3 Posted : 10/17/2013 10:20:52 AM

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Have you tried popping it in the freezer for a bit? I usually try this if something won't resolve. Can work wonders
 
DesykaLamgeenie
#4 Posted : 10/17/2013 5:20:15 PM
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Excellent, thank you both -

I didn't try the freezer, but I had stored the sodium carbonate solution in the fridge before using it and it froze rather quickly just at that temperature, so I think this situation may be an exception to how the freezer sometimes helps with precipitation.

That gets me thinking, though - if the sodium carbonate raises the freezing point of water, then it should stand that at room temperature, the solution would be thicker and more difficult for things to precipitate out of than, say, distilled water at room temperature - and that maybe if I warm the contents up, that would bring the viscosity closer to distilled water and the harmalas would be able to drop out a little easier...? Thus allowing me to decant and skip the filtering...I really dislike the idea of getting some of the harmalas stuck in the coffee filter. Not that I wouldn't be able to wash them out with water, but it's just a step I'd love to skip. Smile

I think I'll experiment with that first, and if it gets me nowhere then I'll go ahead and filter.

And thank you for the walkthrough on the vacuum setup - I know of them, but it's helpful to know exactly what parts go in to the process. It's something I definitely plan on acquiring in the future.

Much appreciated
 
 
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