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Butanol-FASA TEK Options
 
Ruffles
#1 Posted : 6/24/2021 3:04:29 AM
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Very new here, posting in the wrong section, if this can be moved to advanced chemistry I believe it should. This is only a humble contribution to the combined efforts on the NEXUS.

This is a report on a friend`s attempt to extract spice using Butanol. Report is necessary because there is no info here on Butanol use for Spice extraction. All of this was inspired by Rossi et al. 2019 (Internet method for the extraction of N,N-dimethyltryptamine from Mimosa hostilis roots: Does it really extract dimethyltryptamine?). On that paper they described Butanol as grabbing 20x more spice compared with Hexane. They just Lazy Man tekked and pulled into the solvents then mass spec, no other considerations regarding overall purity, solvent usage details or bioassays.

Notes on butanol: it stinks oily s@#$, it doesn`t dry as easily as any other common NPS, it mixes too well with water (sometimes it mixes completely) and it is more viscous.


Acid Base extraction using MAX ion TEK with NPS N-Butanol, with or without defatting (made no difference because of later FASA), but the volumes were different. Basically 50 g powder MHRB to 400 ml distilled water for acid warm baths, then the 400 ml were filtered and reduced to 100 ml, add NaCl then NaOH up to 13... volume went up to 150 ml. Then at least 50 ml of Butanol was used for the pull. Three shakes. Butanol turns into a very strong yellow tinge. NPS was collected.

Now the FASA step. Adding FASA at room temp turns butanol cloudy as expected, but nothing drops out. After clouds dissipate (again room temp), if dropwise FASA again no clouds form! Strange! You can shake, add a LOT more, but nothing drops out! Here comes the trick: PUT IT IN THE FRIDGE AND WAIT. It will drop out of solution after 12 hours or so.

And that`s it! What`s new here? One: butanol can be used. Two: FASA works ONLY at cold temperatures for precipitating the spice within butanol. Why that is so? I am not fully sure, but butanol has low apolarity (or maybe I should say it is relatively more polar than other solvents, such as hexane or xylene) and it is able to hold DMT-fumarate at room temperature, unlike xylene, but at cold temperatures butanol can`t form hydration shells well enough around the salty spice, which has no option but to bind to itself and precipitate out of solution. The good side of its polarity issue is that it able to grab more stuff from the alkalinized bark, bad side of it is that it may grab more impurities, but we have options for cleanup, right? So, cold temperature is the key to crash out the spice from butanol.

NOTE2: There is a possibility that what precipitates in the fridge is freebase spice.

If anyone is able to reproduce this, please give it a shot and let us all know if it works, I might just be crazy. Herein is a picture of 50 ml butanol on the fridge. Not that good of a picture, but that`s it.

Ruffles attached the following image(s):
thedrop.jpg (2,954kb) downloaded 111 time(s).
 

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downwardsfromzero
#2 Posted : 6/24/2021 7:50:06 PM

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Welcome, and thanks for posting.

Interesting experiment. The next thing to do is separate off the solvent and rinse the crystals with a little ice-cold acetone, prior to steps towards characterization and bioassay.

Have you tried putting the butanol pulls in the fridge/freezer before adding any FASA? I doubt freebase DMT would chill/freeze precipitate from butanol, tbh. Once you've added the FASA it's pretty much guaranteed to be DMT fumarate that crashes.

What do you plan to do next?




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Ruffles
#3 Posted : 6/25/2021 5:23:25 PM
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Indeed. Next step was to filter crystals from solvent, however, leaving it out of the fridge to see if it remains solid in solution (like in XyleneFASA) and it didn`t, throwing it back into the fridge did not produce crystals anymore (this is the reason that it maybe freebase crashing out but it clashes with the following).

Pulled more into butanol and restarted the thing, this time two batches of 50 ml, both went into the fridge, after 12 h or so both went cloudy, no precipitation whatsoever, one tube got 1 ml of FASA, other didn`t, 1 h later back into fridge the FASAd-butanol had beautiful and fast precipitation coming out of it, unFASAd didn`t. Seems reproducible to me.

Tricky questions: could precipitation be FumaricDMT that only crashes out of butanol on cold temps? Or adding FASA (or just plain acetone (no test that yet)) somehow makes freebase crash out (shouldn`t because FASA would spend freebase into salt, counterintuitive to say the least)? Dilemmas all around.

Quote:
Have you tried putting the butanol pulls in the fridge/freezer before adding any FASA? I doubt freebase DMT would chill/freeze precipitate from butanol, tbh. Once you've added the FASA it's pretty much guaranteed to be DMT fumarate that crashes.


Yes, the tek actually works better (or maybe faster) when you `freeze` butanol prior to adding FASA. How would you test whether its fumarate or freebase? (add hexane-naphta and dissolves = freebase?)

FASI drops something else, weirder, smaller concentration, transparent cuboid crystals with a sweet taste that remain insoluble at room temp (reminder to never do taste tests ever on unknown shit, tachycardia 2 h after, slightly altered OEV).

Friend says she`s interested in trying solvent mixes, but has no idea where to begin. Something that keeps butanol ability to grab stuff but would help forcing it out of solution after FASA at room temp. Maybe grabbing with butanol then mixing with something else that steals butanol from solutes, some chaotrope or such, then FASA to crash it out?
 
downwardsfromzero
#4 Posted : 6/25/2021 9:08:52 PM

Boundary condition

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You need to do a freeze test on the FASA and butanol only (without pulling any MHRB, so no dissolved DMT) to see if it's just fumaric acid that's crashing out in the freezer.

Quote:
How would you test whether its fumarate or freebase? (add hexane-naphta and dissolves = freebase?)
That would be one way of doing it. DMT fumarate would dissolve in water instead of naphtha.

Quote:
chaotrope
You could try doping the butanol with acetone after pulling and before adding the FASA. I don't think the term 'chaotrope' applies here, however.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Ruffles
#5 Posted : 6/25/2021 10:40:22 PM
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Quote:
You need to do a freeze test on the FASA and butanol only (without pulling any MHRB, so no dissolved DMT) to see if it's just fumaric acid that's crashing out in the freezer.


It is not. Room temp or freezer, fumaric acid does not crash out. Plus, what crashes out after the tek and drying smells `tryptamines` but it has a pinkish hue to it.

Quote:
You could try doping the butanol with acetone after pulling and before adding the FASA. I don't think the term 'chaotrope' applies here, however.


Just meant as some additive that would reduce butanol affinity for the magic at room temp, analogy-wise, but guess chaotropes should stick with water and breaking hydrogen bonds. Just acetone is on the to do list.
 
downwardsfromzero
#6 Posted : 6/27/2021 1:31:19 PM

Boundary condition

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Quote:
FASI drops something else, weirder, smaller concentration, transparent cuboid crystals with a sweet taste that remain insoluble at room temp (reminder to never do taste tests ever on unknown shit, tachycardia 2 h after, slightly altered OEV).
Didn't address this particular comment yet. Have you looked into whether butanol can pull saccharides? And does the usual fumarate precipitate as the same time as these cuboids with FASI?




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Ruffles
#7 Posted : 7/30/2021 7:01:05 PM
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Nope, SWIM didn`t look at its ability to grab saccharides it would make sense though since butanol apparently keeps some water (which would explain why spice does not crash out after FASA), but then why would them sugars FASI precipitate?

Butanol does not separate completely from the black solution, it requires a much longer time in rest to separate but SWIM now thinks that it doesn`t ever fully separate from the polar fraction. Why? Because the butanol fraction had a smaller volume after a too aggressive shaking, meaning some of it stays into polar fraction.

Anyways, Butanol may be used for FASA tek with low temps to precipitate spice since converting precipatates to freebase with carbonate and bioassays proved that, this was the main report goal, now adding the caveat that it just needs to keep temperatures low and shake a little bit less than usual to avoid having to wait too much for good phase separation.
 
downwardsfromzero
#8 Posted : 7/31/2021 12:55:54 PM

Boundary condition

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Butanol is partially miscible with water. Adding salt will reduce its solubility in the water, as well as helping pull a bit of water back out of the butanol.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
 
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