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Cleaning M-acetate residue Options
 
AlbertKLloyd
#1 Posted : 4/12/2012 3:14:04 AM

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mew
#2 Posted : 4/13/2012 12:11:27 AM

huachumancer


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pix please, as this cat knows of m-acetate enthusiasts that would love to see this result for novelty purposes
 
mew
#3 Posted : 4/13/2012 2:07:28 AM

huachumancer


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dry ipa dissolved m-acetate with much agitation, a brief stint in the freezer yielded a pile of amber/tan precipitates settled under some dark brown ice cold ipa. more studies are underway
 
mew
#4 Posted : 4/13/2012 7:11:53 PM

huachumancer


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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
 
mew
#5 Posted : 4/14/2012 4:31:17 AM

huachumancer


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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
 
mew
#6 Posted : 4/14/2012 8:28:26 PM

huachumancer


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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 Day Tripper
#7 Posted : 4/15/2012 3:46:05 AM

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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.

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