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Anyone familiar with toluene pull? Please check the image Options
 
teadock
#1 Posted : 11/10/2014 10:02:13 AM
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Hi. I am embarrased for making this mistake - A/B extraction: I was trying to get fast results and that's the reason why I used naphta from gasoline station (I believe I can't yet understand the full depth of stupidity that those with experience will see in this). It does not dry clean, there must be some oil residue or something.
I got virtually nothing usable from the first pull (room teperature precip) so when I was searching for the mistake in the process, I couldn't fing anything else that the usage of wrong solvent - but that might not be the ONLY mistake I made, please review:
1. Removed by Moderator.
2. Acid cook - 4x 105min, for every cook 1800ml distilled water + 200ml 5% vinegar acid.
3. Basification - adding 125g NaOH.
4. Extraction - while heating, adding 500ml of naphta, shaking 10x, removing naphta from the surface.
5. Precip - 12h left in room teperature (17-18°C).

So then I found something viscous at the bottom of the jar, filtered it, but couldn't dry it or get it near crystallic appearance - so I tried dissolving it in naphta again and put it back in the mixture.
My amateur deduction is, that the oily content of my wrong solvent are attaching to DMT preventing it from forming crystals. My idea is to make the whole content acidic again, shake it, boil it and try to get the DMT water soluble again. Then change the solvent and try again. But that could also be a bad idea, I am no chemist so I would be grateful for any insight.

Thanks in advance.
 

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endlessness
#2 Posted : 11/10/2014 10:04:57 AM

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Did you do an evap test on the solvent by itself to see if it leaves the residue or if its maybe just DMT in oil form that isnt crystallizing?
 
teadock
#3 Posted : 11/10/2014 10:32:03 AM
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Yes - I tried it on white napkin and even with hairdryer it leaves a stain with oily feeling to it but it doesn't smell so strongly at that point.
 
endlessness
#4 Posted : 11/10/2014 10:52:23 AM

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Dont evap on a napkin, evap on a glass surface.

As for how to clean it up, there are several ways. I'd redissolve in clean naphtha, salt out the naphtha using vinegar, re-base the vinegar, re-extract using fresh clean naphtha, and freeze precipitate. And if you want to be extra careful, you could also redissolve in acetone, add FASA to precipitate fumarates, wait couple of days and collect your fumarates , wash your fumarates with cold acetone, then reconvert them to freebase (check the wiki, use either type 3 or type 1).

Good luck, and keep us updated!
 
teadock
#5 Posted : 11/10/2014 11:01:16 AM
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Ok, thank you. Will post the results.
 
teadock
#6 Posted : 11/19/2014 1:43:38 PM
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It seems it's impossible to get clean naphta where I'm from, so I used toluene as described in Shaggy's Jungle Tek.
First I added vinegar to the original mixture with naphta until pH was around 3. Then shaking and cooking, removing naphta + basification. Added toluene and continued with the procedure from Shaggy's Tek, also did the acetone wash and this is what I got - .
The result has honey-like consistency and you can spot kind of yellowish fluid in the top right corner of the image - is this anywhere near what you should expect?
 
steppa
#7 Posted : 11/19/2014 2:58:13 PM

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You need to remove the "." from your link to make it work.

You could also use the button and paste the link to your pic to embed it directly into your post.

Sorry . I don't know how a toulene pull should look like.
Everything is always okay in the end, if it's not, then it's not the end.
 
teadock
#8 Posted : 11/19/2014 6:47:06 PM
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Ok thanks for that, steppa
 
boogerz
#9 Posted : 11/19/2014 7:35:44 PM

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Just don't throw anything away. I think toulene has been used for getting jungle spice. So what you probably have there is DMT plus some other goodies
 
SnozzleBerry
#10 Posted : 11/19/2014 7:58:15 PM

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It looks normal to me, for a toluene pull. If you scrape it around with a razor blade (referred to as a "manual re-x" by some) it will turn waxy and eventually solidify even more. If you do this until it is a crumbly/waxy consistency and then leave for an extended period of time, it may even harden significantly.

burnt's analysis of so-called "jungle spice" showed that his samples were ~95% DMT and ~5% 2-MTHBC.

Enjoy!
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teadock
#11 Posted : 11/20/2014 2:39:51 PM
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Thank you guys, I'll give it a try then.
PS: I've never thrown anything away during the whole procedure, so there's plenty of jars filled with stuff here Smile.
 
 
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