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quick question about recrystalization Options
 
DMTer
#1 Posted : 4/9/2010 12:52:08 AM
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SWIM preformed a STB extraction using 100 g's of MHRB, NaOH and DCM as the solvent. unfortunately, SWIM was left with an awful yellow oil which refuses to evaporate fully. SWIM just wants to know if the procedure to recrystallize is correct as follows:

1. mix pH 3ish distilled H2O + acetic acid into gooey oil.
2. collect pH 3 water and basify to pH 13.
3. mix in clean DCM to basic water, separate DCM and evaporate the DCM.

 

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endlessness
#2 Posted : 4/9/2010 12:57:00 AM

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DCM pulls too much plant oils and so on.. you wont get clean crystals like this.. you'll either need to extensively defat, but even so I suspect you'll still not get clean crystals.. The other solution is to get some naphta/heptane/hexane, which is what people use to recrystalize dmt. So you dissolve your product in a minimal amount of warm naphtha/co, decant this solvent away from the bottom layer of undissolved goo that will remain and into a clean container, and stick it into the freezer..
 
lyserge
#3 Posted : 4/9/2010 1:05:45 AM

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OK endlessness and others, SWIM tried to recrystallize some white/off-white crystals that were very harsh when smoked, and after the recrystallization there's a large amount of yellow goo stuck in the bottom of the glass container. The goo is rock hard after maybe 3-4 different washes with hot naphtha, and there is some definite nasty lye stuff in it (brown and red spots), but the yellow goo has also formed crystalline shapes that indicate the presence of tryptamines in the goo. SWIM has been unable to get any more of the rock-hard goo to dissolve into hot or cold naphtha, but she doesn't want to throw the entire goo away. She's had this problem before with yellow crystals left in a vial in the car; when she returned they had melted down into a very hard goo that was impossible to redissolve in naphtha. How does SWIM get the rest of the Spice out of the rock hard goo while leaving the brown and red impurities in the container?
"...I didn't know that Cheshire cats always grinned; in fact, I didn't know that cats could grin..." - Alice's Adventures in Wonderland
 
DMTer
#4 Posted : 4/9/2010 1:07:27 AM
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Thanks for the info about Naptha. SWIM used it in previous extractions with the same results but also could have been caused by fanning the evaporating solvent. Unfortunately, SWIM has access to only DCM at the moment and as you have pointed out, a clean extract using it is impossible. I still have the all the remaining goo but I don't know what to do with it. SWIM can't scrape it, SWIM can't clean it, all SWIM can do is stare at it. Is there anything SWIM can do to recover the DMT from the oil into some sort of smokable state? SWIM has given up all hopes of a pure extract at this point.
 
endlessness
#5 Posted : 4/9/2010 1:07:42 AM

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well if its dmt, then very warm naphtha and mixing it up should pick it up! just leave it all in a water bath (no fires near) and mix it up a few times and leave it for some minutes, it should dissolve the actives
 
Samadhi-Sukha-Upekkha
#6 Posted : 4/9/2010 4:16:54 AM
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Wait, if SWIY wants to do a defat during the recrystallization and only has access to DCM as a solvent, then SWIY needs to do pulls with DCM on the acidified solution to try and get the oils out. That DCM can be removed, and then the water can be basified and alkaloids pulled with fresh DCM.

Access to acetone and fumaric acid would allow SWIY to do a FASA tek to get just the alkaloids to salt out of solution, leaving oils and waxes behind. But then SWIY has to deal with the fumarate.
 
lyserge
#7 Posted : 4/9/2010 12:00:16 PM

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endlessness wrote:
well if its dmt, then very warm naphtha and mixing it up should pick it up! just leave it all in a water bath (no fires near) and mix it up a few times and leave it for some minutes, it should dissolve the actives


No this isn't working, and SWIM knows there's a significant amount of Spice in there due to the hyper-fractali-crystallization in the goo. The goo is ROCK HARD, and after three or four hot naphtha baths it's still in there. When this happened previously SWIM scraped it out with a knife and just vaporized the goo, and a very small amount of goo (maybe 1/2 cm deep in a small gold vial) lasted for at least 30 solid sessions, must've been close to a gram condensed into a very dense goo. Anyone had this happen?

Sorry if I hijacked your question, DMTer, our questions seemed similar but now I realize they're different since you don't have access to naphtha.
"...I didn't know that Cheshire cats always grinned; in fact, I didn't know that cats could grin..." - Alice's Adventures in Wonderland
 
 
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