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Conducting 3 FASA experiments, some questions first. Options
 
SuperRad
#1 Posted : 9/17/2009 3:50:26 PM
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I will be doing 3 100g extracts attempting to determine which FASA teks have the best yield to effort ratio.

I will be performing:

1) CASA -> FASA

2) A citric acid water extraction on the bark, followed by evaporating the water completely. Then pull with acetone and FASA.

3) STB, pull with Xylene or Toluene then FASA

Questions:

Xylene or Toluene? I'm leaning towards Toluene. Also I really NEED a good description of the best way to FASA from xylene or toluene.

Should I do a citric acid wash, or should I do a vinegar wash, and then just add a bunch of citric acid to the solution once the initial extraction is done and ready to be reduced?

And finally, I'm looking for any and all help with the CASA -> FASA method.

Thank you, the results will be posted as soon as they're available, but I'm still waiting on some bark.
 

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Infundibulum
#2 Posted : 9/18/2009 10:42:57 AM

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All sound good.

Re #1,
SWIM would normally say do not really bother with CASA->FASA, but what the heck, give it a try if you have time. What SWIM didn't like with this tek is that it takes a long time. Even though it sounds simple in theory, in practise he finds it more cumbersome.


and #2, That sounds fine, but it is only slightly different from CASA->FASA. You can do something different though; do your acidic boils with citric acid or whatever acid you love, evaporrate down to syrupy consistency, mix in calcium hyddroxide or sodium carbonate and let it dry. The latter freebases the alkaloids. Then pull with acetone (which will pull the freebases and all sorts of crap and then do FASA to precipitate the fumarates and leave behind all the crap.

Finally #3. SWIM has been using xylene for FASA, others have been using toluene, basically go with whatever is cheaper. Toluene smells a bit better than xylene though. A fair (but possibly outdated) tek is this one.

Hope that helps!


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
SuperRad
#3 Posted : 9/19/2009 1:59:06 AM
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Infundibulum wrote:
All sound good.

and #2, That sounds fine, but it is only slightly different from CASA->FASA. You can do something different though; do your acidic boils with citric acid or whatever acid you love, evaporrate down to syrupy consistency, mix in calcium hyddroxide or sodium carbonate and let it dry. The latter freebases the alkaloids. Then pull with acetone (which will pull the freebases and all sorts of crap and then do FASA to precipitate the fumarates and leave behind all the crap.



That's not a bad idea at all!

Here's a question: everyone's says that you have to dry the freebase paste completely before doing the acetone wash. That's what I've been doing myself... SEEMS logical enough right? Certainly no water should go into the FASA, but in fact. in order to do that it's best to make sure the acetone itself is dry. SO: why not just wash the still moist freebase paste, THEN dry the acetone with gypsum (or epsom).
 
soulfood
#4 Posted : 9/19/2009 2:03:13 AM

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Well you could but you'd need more epsom.

You can dry water with heat, but obviously heating acetone is a bad idea unless you have the correct setup/ventilation etc.
 
SuperRad
#5 Posted : 9/27/2009 6:22:20 PM
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Alrighty the experiments aren't 100% complete, but here are some preliminary results:

#1 CASA -> FASA: The very first CASA batch crashed out some very purple crystals after being mixed with FASA, abeleit a very small amount. The next to yielded next to nothing. These purple crystals were dissolved in water and then basified. The water went from a clear purple to an opaque black (good sign). Then I mixed with naphtha and separated. The naphtha has been sitting in the freezer almost 24hrs and NOTHING NADA ZIP. Dunno what precipped out of the FASA, but the freebase doesn't seem to be soluble in naphtha.

#2 I just haven't done this one yet... I'll just do it on the 56g I tried to CASA as most of the dmt should still be in there

#3 Worked very well, I have some DMT crystals in naphtha in the freezer, and some ISO evaporating that the naphtha wouldn't get but the Toluene did.
 
 
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