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stb extraction/ water crystallization Options
 
doodlekid
#1 Posted : 4/25/2015 6:26:26 PM
Hi,

I've just weighed the result of my extraction of 200 grams of MHRB and it is more than 20 grams. So I figured something gone wrong...

Now I did a STB extraction with sodium hydroxide and naphta. Following one of the teks posted here, the one in dutch actually.

Anyway after I separated the naphta from the solution I went for a extra step in order the crystallize in water.

So I put some vinegar and the naphta together and shook it for a while. Then separated both liquids and started to add sodium carbonate to the vinegar until it didn't react anymore and then continued, gradually, till it became a milky/ cloudy solution. I used a small spoon and added the undissolved stuff...

This I put in the fridge for about a week and saw that crystals had formed in clear liquid.

So I filtered and dried the crystals. But they weighed over 20 grams, where I used 200 grams of MHRB. That's way too much...

Now my guess is that the result is partly DMT and partly sodium carbonate. That I may have added to much soda and that it crystallized together the DMT. Because it does smell like DMT and it's very white, rocky crystals.

Maybe it would have been better to use a saturated soda solution and gradually added that, instead of directly adding soda from a spoon.

Anyway, what would the best way of getting it pure? I figured to put it all back into a jar with water and make sure to not saturate it and then put the whole thing back in the fridge and wait again, but will that work for sure?

I will post a pic tomorrow if neccesary, but I just took my jar from the freezer and saw some more crystals formed and now my dish needs to dry again from this extra addition.
 
1ce
#2 Posted : 4/25/2015 7:53:17 PM
Dissolve 10g lye with 100ml water, pull into solvent, and set basic water aside for now. Wash solvent with water, sucking off the water layer. It is fine to leave a tiny layer of water with the solvent. Do this a total of 3 times to the solvent, the final time removing as much water as possible.

Repeat this process from the basic water 2 more times to be certain you got all your DMT. Evaporate 2/3 of your solvent, seal your dish, and precipitate your DMT freebase in the freezer overnight.

 
doodlekid
#3 Posted : 4/26/2015 4:43:15 PM
1ce, thanks for the reply. I hope I've described well enough what I've done, cause I don't get your reply fully. So I added a pic of what I've got right now. Also I kept the solvent and base water I've used.

Anyway, you advise to dissolve the material in the picture in water along with lye and wash this with solvent 3x and precipitate it in this? Is there a way to do this without the solvent, I would prefer this.
doodlekid attached the following image(s):
result.JPG (46kb) downloaded 92 time(s).
 
 
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