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Cleaning M-acetate residue
- Thread starter AlbertKLloyd
- Start date
like other freeze precipitations the solution must be highly saturated
upon diluting the solution with more dry ipa and freezing nothing precipitated
the solution was evaporated and redissolved in more dry ipa and set in the freezer, minutes later, tan amber precipitates formed
the above solution was decanted carefully, just a few mls, then more dry ipa was added to the freezer vessel and mixed then set back in the freezer in hopes of removing more and more of the dark colored solution the amber tan precipitates fell out of
results soon
upon diluting the solution with more dry ipa and freezing nothing precipitated
the solution was evaporated and redissolved in more dry ipa and set in the freezer, minutes later, tan amber precipitates formed
the above solution was decanted carefully, just a few mls, then more dry ipa was added to the freezer vessel and mixed then set back in the freezer in hopes of removing more and more of the dark colored solution the amber tan precipitates fell out of
results soon
out of 300 mg dirty black acetate (never have i seen this before) only 30 mg of this flowing tan powder was recovered (and it is gorgeous and bulky for such a light weight, i doubted the scale for a minute) , however there is still more to evap and evaluate so this is an incomplete report at best
i also notice that when the dissolved m-acetate is evapped (even in hot dry ipa) there is still this tan amber solid settling at the bottom, perhaps this is excess acetic acid?
more information and pictures following shortly
the tan powder will be bioassayed alone
then will the evaped dark ipa to compare
i also notice that when the dissolved m-acetate is evapped (even in hot dry ipa) there is still this tan amber solid settling at the bottom, perhaps this is excess acetic acid?
more information and pictures following shortly
the tan powder will be bioassayed alone
then will the evaped dark ipa to compare
the powder is tasteless O.O
the remaining solution was microwaved yielding a blackish goo
the goo was assumed to be freebased mesc alks and was rehydrated with vinegar to give it a salt form
some of the goo stayed as tiny black specks that were adhered to the evaporation dish, they were collected and removed
the vinegar solution was evaporated yielding an odd tasting reddish brown goo that seems to be hardening
still nothing is like the amber orange waxy mesc acetate this cat knew before. what gives? perhaps the m-acetate in this trial is infact contaminated with a strong bass...
the remaining solution was microwaved yielding a blackish goo
the goo was assumed to be freebased mesc alks and was rehydrated with vinegar to give it a salt form
some of the goo stayed as tiny black specks that were adhered to the evaporation dish, they were collected and removed
the vinegar solution was evaporated yielding an odd tasting reddish brown goo that seems to be hardening
still nothing is like the amber orange waxy mesc acetate this cat knew before. what gives? perhaps the m-acetate in this trial is infact contaminated with a strong bass...
The Day Tripper
Rennasauce Man
If you have acess to dry acetone, it works damn well for helping precipitation of mesc hcl from dryish isopropyl (prob 95-97% in my case). Mesc hcl behaved the same was as you describe the acetates do, they'll precipitate and have to evap to get most/all of the xtyals, but still get the goo.
If you add dry acetone to your hot iso saturated with your mesc salt, it will start to precipitate without cooling. Mesc salts are not very soluble at all in acetone, at it makes them less soluble in the binary solvent as a mix.
I still had to evap, but i never froze, just heat/cool with evaps along the way. Collected most of the crystals, then evapped the last little bit of solvent, to get some crystals and goo/crap. Wash that and the xtyals separately with dry acetone (prob minimal amounts and cold if your using mesc acetate, not so big of a deal w/ hcl), then evap and save the washes, should be the crap/impurities/other alkaloids soluble in acetone.
Combine the crystals, crush lightly to not quite a powder, but sandy texture, then wash once more with dry cold acetone.
Took almost all the color/smell out of my mescaline hcl i thought was clean, after washing with dry acetone, and water re-xing, but i think precipitation out of alcohols gives cleaner crystals with less impurities caught up. At least while theres still a good bit of solvent, one thing to keep in mind is as you evap and concentrate the alcohols, the dirtier the precipitates will be.
I've also had ideas about using limo/heptane instead of acetone to force the mesc hcl to crystalize out of the saturated iso. But have not tried it as of yet.
Just take all this with a grain of salt as its ime with the hcl, acetates could have different solubility in iso/acetone.
If you add dry acetone to your hot iso saturated with your mesc salt, it will start to precipitate without cooling. Mesc salts are not very soluble at all in acetone, at it makes them less soluble in the binary solvent as a mix.
I still had to evap, but i never froze, just heat/cool with evaps along the way. Collected most of the crystals, then evapped the last little bit of solvent, to get some crystals and goo/crap. Wash that and the xtyals separately with dry acetone (prob minimal amounts and cold if your using mesc acetate, not so big of a deal w/ hcl), then evap and save the washes, should be the crap/impurities/other alkaloids soluble in acetone.
Combine the crystals, crush lightly to not quite a powder, but sandy texture, then wash once more with dry cold acetone.
Took almost all the color/smell out of my mescaline hcl i thought was clean, after washing with dry acetone, and water re-xing, but i think precipitation out of alcohols gives cleaner crystals with less impurities caught up. At least while theres still a good bit of solvent, one thing to keep in mind is as you evap and concentrate the alcohols, the dirtier the precipitates will be.
I've also had ideas about using limo/heptane instead of acetone to force the mesc hcl to crystalize out of the saturated iso. But have not tried it as of yet.
Just take all this with a grain of salt as its ime with the hcl, acetates could have different solubility in iso/acetone.
