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Which Solvent to Max Yield Options
 
DudeMeetTyler
#1 Posted : 12/4/2010 10:15:21 PM

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An A/B using vovins tek was performed with naphtha as the solvent. Which yielded .8% of nice some white fluffy stuff via freeze precip and roughly the same of some yellow x's that were obtained when the naphtha solution was left to evap.

The powdered bark (100g before the initial extraction) and the base solution (~800ml) were saved, mixed together and pH'ed to over 12 to perform a STB. This was left for some time (several weeks in fact, as there was no time to tend to it) and then extracted using 3 X 200 ml warm naphtha. Results still pending on evap but even upon slight volume reduction of the solvent solution, freeze precip yielded nothing. But will update with the evap yield in the next few days

A few things
- would using xylene or toluene as the initial solvent (instead of naphtha) increase the yield of the n,n? (It would obviously increase over all yield as it pulls other alks/fat/oils etc, assuming a defat was NOT performed before basifying). To seperate the two a Wash of the evapped goo would then be preformed to seperate the n,n from the "other"...

- can the STB described above on the "scraps" be improved upon?

Thanks in advance for any replies

Edit: Also, which is perfered xylene or toluene? And Why?
Thanks again
"If people let the government decide what foods they eat and what medicines they take, their bodies will soon be a sorry state as are the souls of those who live under tyranny"

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DudeMeetTyler
#2 Posted : 12/5/2010 8:28:24 PM

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Well the solvent evapped from the STB.

Both the bark (100g) and the lye solution (~800ml) were saved from a previous A/B tek. They were then combined and let to sit for probably over a month. 3 X 200 ml warmish naphtha was then used to extract any extra goodies from the solution and left to evap.

Once everything evapped it left some oily orangey-white or tan powder (the colour was consistent through out) that was scraped up from the evap dish and transferred to another dish and left to let the rest of the solventy smell disipate.. it is still sitting now..

it hasnt been weighed but it shows that one should never throw out anything from an A/B tek.
the "spent bark" and lye solution can be combined and left to sit ala an STB and if one freeze precips their goodies outta their solvent it too can be reused to pull from this STB solution.

I'm sure most experienced with this sort of thing already knew about this but for anyone just starting out now you know....
"If people let the government decide what foods they eat and what medicines they take, their bodies will soon be a sorry state as are the souls of those who live under tyranny"

"My orders were to test the drug...It works" Bass Association by Far Too Loud

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DudeMeetTyler
#3 Posted : 12/12/2010 3:33:15 AM

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Hate to keep posting on the same thread but thought an update was in order..

A fresh batch hasnt been started but the thought is that xylene will be used as the solvent on an A/B and the resulting evaporates washed with naphtha (or bestine if it can be found in the area) a few times in an attempt to the remove all the n,n leaving the "jungle" in the remaining goo... any comments on the suitability of such a practice would be muchly appreciated...


As far as the STB on the "scraps" (as i like to call them)... the naphtha was left to evaporate which left a tan powder which smelled slightly of solvent.

This tan powder was them combined with other yellow crystal evaporates (which also smelled slightly of solvent) and enough naphtha was added to dissolve all the solids. This solution was warmed causing a brown gooey residue on the bottom that stuck there once cooled. This was then washed with a sodium carb solution, the water was pipetted off (into a clean container, just in case) and another wash was done with just plain water (again pippetting off the water into the other container).

The Naphtha was then reheated so all the goo would stick together, it was then cooled slightly to allow the goo to again stick to the bottom. The naphtha was then poured into another clean shot glass and the original shot glass was rinsed with warm naphtha and then put into the shot glass with the washed naphtha. The shot glass containing the cleaned naphtha was left to evap for 3 hours (to slightly reduce the volume) before placing in the freezer.

After freezing the naphtha was poured off and the remaining goodies collected...

I guess what I'm trying to say is THANK YOU to the Nexus and all those who made this possible
"If people let the government decide what foods they eat and what medicines they take, their bodies will soon be a sorry state as are the souls of those who live under tyranny"

"My orders were to test the drug...It works" Bass Association by Far Too Loud

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endlessness
#4 Posted : 12/12/2010 10:10:39 AM

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Good work Smile Thanks for sharing!

What was the final yield?

As for the original question, yes using both xylene or toluene will increase yields as they dissolve dmt better (but also other impurities as you said). I dont know if anybody ever tested for differences in xylene or toluene. I already used both (though in different extractions) and they both worked perfectly fine.

Do note that they smell horrible though, specially xylene imo (toluene smells more 'sweet' but also the kind of sweet that feels like its destrying the brain cells Razz ). If you use any of them, rather salt out (with FASA, FASW or vinegar), evap/dry that and later freebase, instead of evaporating the solvents. This way you can reuse the solvent and its not so nasty with all that evapped solvent.

Or, as I prefer, use limonene, which is also a pretty good solvent and smells great, and then salt also (FASI, FASW or vinegar).

By the way, how many and how big pulls had you originally done on the A/B before mixing with the 'spent' bark?
 
DudeMeetTyler
#5 Posted : 12/15/2010 9:15:21 PM

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3 x 200 ml warmed naphtha pulls were performed on the A/B originally to yield just over 1 % from the freeze precip and about the same from evaporating (though alot of weight was lost upon re-x'ing and one wonders now if it is really worth it to evap solvents)

The STB on the spent bark and the left over lye solution only yielded 0.4%... But the naphtha wasnt really warm (infact it was far from it), someone got lazy haha, and didnt think it would produce much in the way of results... next time it'll definately be warmed thoroughly, imaginably giving better results

And thanks, one of either xylene or toluene will be used on the next pulls
"If people let the government decide what foods they eat and what medicines they take, their bodies will soon be a sorry state as are the souls of those who live under tyranny"

"My orders were to test the drug...It works" Bass Association by Far Too Loud

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