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No smell quick and easy purification help needed

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M

monkeyboy

Rising Star
Can someone please explain to swim just when he should be pulling from the solvent mix when at the final purification stage?

swim did not see distinct layers- though he did pull mostly clear looking stuff from the top which did produce a rip-roaring fantastic (side effect free) experience.

Swim read elsewhere that one should pull as soon as they see something clear on top- but swim saw that and the volume of mostly clear solution didnt seem to swim like all the good stuff would be there.

Other than a xylene boil (which goes against the whole premise of the 'no smell' tek), swim is hoping to get a better understanding of whats going on. So far, according to swims limited understanding, it appears as if there are impurities in the basified extract (duh!) and that bufo should be the first to crash out once the proper dipole moment is reached by combining solvents?????? Is this correct?

If so, then one adds Naphta to the acetone dropwise until clear stuff crashes out, and then once that ratio is noted, one may possibly continue to add that mix/ratio in order to allow for more volume of solution to get all of the bufo out.???

Swim noted what looked like a top, mostly clear phase, then a gradiation all the way down to the darker waste layer that ended up yielding sludge after everything was evaporated- he was frustrated that there wasnt a clean separation because he feels he was likely leaving alot of good stuff behind (aprox 600 mg of impure fumerate salt only yielded 20 someodd mgs of off white goodness.
 
What 'crashes out' are the unwanted compounds. With just the right polarity of solvent the bufotenine stays solved and the noxious unwanted compounds stick to the bottom and sides of your vessel or may even be as a thick liquid blob at the bottom of the solvent containing vessel. Probably both...

Your suspicion that you are not getting all of the bufo when decanting a clear layer is not unfounded!
One of the factors that makes understanding solubility difficult is that there is a range between the polarity at which a substance begins to solve and the polarity at which it begins to cuagulate. Other compounds with a similar polarity profile have a soluability range that is partualy within the soluability range of the desired compound that is targeted for extraction.
When a substance is desolved in a solvent that has (precisely) matching polarity value we could say that it is perfectly solved and observe that (in this case with 5-HO-DMT and a solvent of approximately one part acetone and four parts naphtha) the solution is transparent and not at all cloudy.

When a solution consists of a solvent and a substance with polarity propertys that are nearly the same but not exactly we can observe that the solution will be cloudy. For another example of this look at naphtha solution from a DMT extraction that is being freeze percipitated. As the naphtha gets colder and colder it gets cloudy untill most of the DMT finally crashes-out and forms on the surface of the container it's in. At which point the naphtha becomes clear again...

Note that in the case of DMT extraction with naphtha we can extract some(most) of the DMT in MHRB with naphtha but not all. In order to get all of the DMT in MHRB one has to use a solvent with a higher pka value.
Ofcourse doing so results in a wider range 'spectrum' of DMT being pulled and this extraction will include a few diffrent extras that are not 100% n-nDMT. They give this extraction it's different qualitys...

Note that a solvent is also cloudy when it becomes super-saturated with a particular compound, to the limit of what its' quantity can hold.

:!: 'Nuff said?!:idea:
It really comes down to quality vs. quanity, or, purity vs. quanity for that matter...Remember; Bufos' two cousins, 5Meo and n-n, are living next door to each other right up polarity street on the same block!
In trace amounts at least,
but so do some of the NAUSEA NASTYIES:evil: :twisted: :evil: :twisted:
 
youre speaking of dipole moment, correct?

I was a little confused, because a search for this doesnt provide alot of info, and I imagine theres some misinfo around here as well because I saw another post somewhere on this site where someone is stating the precipitate is the good stuff. Im quite certain this isnt the case, because of the gunk and other stuff that accompanies the sediment.

Its a good thing too, my friend tried this and when adding sodium carbonate to the formic salt, he added an excess of carbonate, and that stuff mechanically follows over when pooring out the acetone (when adding acetone to pull goodies before final purification). Besides, previous attempts involved only pulling the clear layer on top, and has yielded very active, CLEAN stuff, though in minute quantities.


Very frustrated, using tons of bufo-fumeric salt to get such crappy yields.

Im not sure what my friend should be looking for when adding naphta dropwise. Other than for a clear layer on top and to stop at that point.

Next question is how far into the shady areas does one pull? As previously stated, its a question of quality vs quantity. By pulling only clear layer, havent noticed ANY nausia! Itching and all that, yes. Nausia or big pressure in the head, no.
 
Today I watched in amazment as if looking through the eyes of a stranger....(lol)...

and saw; two extractions where done in the final phase of the no-smell tek.

In the first one, the solvent was brought to a polarity where nothing was cloudy, there was bits of sticky but solid tar/sludge on the sides and bottom of the flask and a thick, dark goo that was liquid but thick enuf in consistency that it flowed veary slowly (like honey) on the bottom. The rest was crystal clear solvent. This was pulled and saved for evaporation.

Then acetone was added to the flask again and everything remaining in the flask desolved. Next naphtha was added untill there where solid, gooy bits of tar coating the bottom and the solvent was cloudy OFF-WHITE (almost yellow but not green). It was translucent, nearly transparent but not crystal clear. Everything in the flask was either sticky, solid tar/goo or the cloudy solvent. Again, the solvent was pulled and saved for evaporation.

I'll let you know how the bioessays go. Usually someone just does one extraction, on the bufo jam, twice, for purity.
This time two extractions on the bufo jam will only be done once.

I myself am curious about the crystals growing around the sides of the top of the acetone that was initially used for the extraction from the seeds and then saved after the fumerates where removed. It had been split into two containers. One was the bulk of it and had fumeric acid added but the second was just about 30ml in a shot glass and had citric acid added instead to observe the difference. They where both recombined after the salts where removed and set to the side uncovered where it evaporated a little overnight. Now there are crystals around the edge that have a diamond shape resembeling n-nDMT freebase crystal structure.
 
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