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My extraction method Options
 
dread
#1 Posted : 7/28/2009 10:11:36 PM
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I've been trying a new(?) extraction method which is kind of a "reverse a/b" extraction. It starts with an STB though, so I decided to post it here. If someone has already posted a similar method, then I apologize, but I actually did figure this out by myself.

Here it is in a nutshell:

--

1. basify the bark with NaOH. Extract with a large amount of heavy aliphatic naphtha to get max. amount of alkaloids out.

2. Mix 1g citric acid per 100g of bark into 100ml water. Add the citric acid solution to the extracted heavy naphtha, shake and let separate a few times until the water/acid solution turns yellow. Separate the layers into 2 jars.

3. Now take the same amount of NaOH, maybe a few grams extra to be sure, as you used citric acid, and dissolve it in 100ml water. Then mix this with the jar with the water and DMT citrate to basify the spice again. Then extract again with a light naphtha and freeze precipitate.

--

The idea here is, that the heavy aliphatic naphtha is good for pulling the spice from the bark, but it's worthless for precipitation, and even evaporating takes a long time (also evaporation of it tends to result in a sort of goo, with plant fats and whatnot).

Now a light aliph. naphtha is good for precipitation, but it tends to pull less spice. So I devised this method of first pulling with heavy naphtha, then extracting the alkaloids from the heavy naphtha (and exluding plant fats) by citric acid/water solution, then basifying again and extracting the alkaloids from it with light naphtha. The last step might be unnecessary though, since the spice should in theory precipitate out from the water as soon as you basify it again. I have yet to try it that way though.

A result of this method is now in the final phase, that is, in the freezer. So far it seems to be working, and by the looks of it, I've never had so much spice in so little amount of naphtha with a standard STB. (Of course, the amount of heavier naphtha I used was larger, this is due to heavy naphtha being cheaper and easier to get than the light one, around here).

I might be able to post some pictures later.
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
noothgrush
#2 Posted : 7/29/2009 12:19:02 AM

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Sounds veryy interesting, I'm in the middle of a STB extraction now, but with disappointing yields. I've been thinking of doing an A/B next time, but this seems easier. Looking forward to some input from the experts on the board.
 
soulfood
#3 Posted : 7/29/2009 12:23:28 AM

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Yup... that's the best way to get goods out of strong solvents like xylene's and what not.

Best to use fumaric acid instead of citric and then evap the water.

It's quite similar to the classic cactus teks and jorkests fumaric acid on D-limonene approach.
 
dread
#4 Posted : 7/29/2009 12:43:17 AM
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I'll be posting some pics soon. Just got the spice out from the freezer, and the crystals look awesome. There's also some yellow oil, some yellow crystal and some white crystal. I believe there's quite a lot of N-oxide, but that's probably because I had to leave for a week-long vacation while the bark and the lye had already been mixed together... so it sat doing nothing for a good time (well, at least the heavy naphtha got to soak up the spice thoroughly).

And let me say, I did get a really nice amount of spice considering it was done in one pull.

This might become my favorite extraction method, if the good results stay consistent.

@ soulfood: why fumaric instead of citric?
 
dread
#5 Posted : 7/29/2009 1:15:46 AM
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Hmm... something funny. The spice looks nice, but it has a very strong earthy smell to it. Strong enough to almost completely hide the plasticky smell. The smell somehow reminds me of potatos, only, not quite.

What does this indicate?
 
DoingKermit
#6 Posted : 7/29/2009 1:55:40 PM

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Haha! Potatos?! Never heard of that before Smile
 
dread
#7 Posted : 7/29/2009 8:13:47 PM
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Well... I'm probably thinking about the underground cellars they used to store potatoes in. That's what the smell most reminds me of.

I've read that N-oxide supposedly has a musty smell. Could it be that the spice I pulled has so much N-oxide that the smell overwhelms the usual spice smell?

Anyone with experience of pure N-oxide, I would like to hear from you..
 
soulfood
#8 Posted : 7/29/2009 9:02:34 PM

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dread wrote:


@ soulfood: why fumaric instead of citric?


I suppose it's only worth it if you want to evap the water once you've migrated it out of the heavy naphtha as DMT is a very solid crystal and DMT citrate is all gooey.
 
dread
#9 Posted : 7/29/2009 10:52:39 PM
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^ yeah well, since I convert it back to freebase anyway it doesn't much matter what acid I use, eh?

 
dread
#10 Posted : 7/30/2009 6:30:52 PM
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Well anyway, here's pics of the stuff taken just after extraction:





The spice still smells funny, but I had a friend sample it (really) and he tells me it tastes right when vaporized, and works as it's supposed to. I'll let you know more when I get to sample it myself.
 
dread
#11 Posted : 8/2/2009 10:57:42 AM
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Quick report: I tried the spice myself yesterday, and it's amazing. Great. One small toke from the vape...
 
 
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