Evaporating Acetic Acid Solution

[DudeMeetTyler]

After reading here about never evapping solvents. One decided to salt out remaining goodies from naphtha (after the initial freeze precip) using acetic acid, rather then evap off.

This acetic acid solution was then evapped using the method found here .. However the solution never got to 100 C, max ~80 C... And once fully evaporated it still smelled of vinegar (still does actually, even after allowing to sit for about a week) and left a brown/tan goo on the bottom of the bowl, presumably dmt acetate?

Any thoughts on what went wrong? (the method for evapping acetic acid as mentioned above was followed to a T...)
-should more water be added and then continue to evap?

or - should one convert to freebase using sodium carbonate and water, then pull with naphtha?

Any help would be appreciated

 

[endlessness]

I neither had luck with this acetate evaporation when I tried it. I would say make a paste with sodium carb and a bit of water, dry, powder, and pull with pure IPA/Acetone/Ethanol, and evap that instead (maybe infusing some herbs with it). Or pull with small amounts of warm naphtha and freeze precipitate

Personally I dont agree with what q21 says in that post, I think it is no problem at all evaporating your solvent, and the impurities which he misleadingly calls "nasties" and says should be avoided are harmless. IMO the most problematic impurity would be solvent traces, so regardless if you evaporated or freeze-precipitated your naphtha, I suggest redissolving your crystals in IPA/Acetone/Ethanol and re-evapping that, which will help getting rid of the solvent traces

By the way, why didnt you simply freeze precipitate your naphtha instead of salting?

Salting is very necessary when extracting with limonene (which neither evaps clean and neither freeze-precipitates) or xylene (which smells like hell when evapping and doesnt freeze precipitate). For naphtha its not really necessary because you can freeze precip if you dont want to evap

 

[DudeMeetTyler]

Sounds good, thank you...will update with results

And initially a freeze precip was done.

Salting was done afterward for a couple of reasons;

1 - capture anything that still remained after the freeze precip, without losing any solvent to evaporating

2 - allow for re-use of solvent (after salting was done x 3, naphtha was rinsed with small amount of water ( x 3) to remove any remaining acetic acid solution)

 

[endlessness]

if you freeze precipitated and the naphtha was saturated enough, there shouldnt be any (or very little) dmt in it so salting would yield you mostly plant oils and very little dmt

you could reuse the solvent anyways just after freezing, no need to salt it afterwards.