no crystals using "fake" naphta.

[oneistheall]

hi. would kindly appreciate some insight.
my friend did something like the lextek (the video from the guy that dyes his hair during the extraction) for the second time, first time he had 2% yield from mimosa using petroleum ether which is super expensive, second time he used what in his country they call naphta for a tenth of the value but this time he had zero crystals, he did some research and found out that the product could be mixed with xylene so in order to get the spice out he washed 3x the so called naphta with lab vinegar, atm he has 3 dishes on top of the heater to evaporate. He uderstands that IF the problem was the fake naphta now he will obtain spice acetate (the problem could have been an other, for the no cristalization or no extraction) he plans now to dissolve whatever is left after evporation in petroleoum ether and crystallize in the freezer. Will this work and render spice freebase? or spice acetate is not soluble in petroleum ether? what do you guys think? Note: petroleum ether is actually the real naphta (lab grade he think). he saved the solvent to evaporate it also, in case the vinager has zero goodies.
thanks!

 

[downwardsfromzero]

Do you have a MSDS for the specific solvent? Xylene in any significant proportion would certainly screw up a freeze precipitation.

The vinegar washes were trhe right thing to do. Any resulting DMT acetate will need to be freebased again otherwise it will not be soluble in petroleum ether, nor would it be suitable for vaporising as is.

A good way to go here - assuming the vinegar wash yields anything - would be to make the evaporated vinegar goo into a paste with sodium carbonate. The paste can be pulled with warm pet. ether and freeze precipitated. Alternatively one could use 99% isopropanol or 95-99% ethanol for the pull, followed by evaporation.


All-in-all, it sounds like things are on track despite the minor hiccup.

 

[oneistheall]

thank you downwardsfromzero. attached is what he found to remain after evaporation, it fits with what he expected(in looks not in amount), the vinegar was pure (made with acetic acid) and the amount of solvent pulled was minimal so he guesses this is it. he did expect a bit more its true. he has 3 pyrex with that kind of goo. he started with 250gr mimosa so he expected a 1.5/2% yield. now he is wondering if 3 acid pulls(100ml each) where enough...
well now to the next step. he did the paste which at a first glance looked like it wouldnt work, but hot solvent and stirring broke it up into powder eventually. he pulled with the solvent and filtered with coffee filter trying to avoid suspended sodium carbonate. its in the freezer now, in a little while he will now if it worked or the spice remained in the initial caustic soup (that he threw away, argggg).

 

[downwardsfromzero]

Looks about right! Acetic acid wouldn't have yielded anything on evaporation by itself.

in a little while he will now if it worked or the spice remained in the initial caustic soup (that he threw away, argggg).

I once kept some base soup for about three years and eventually found that the residual occluded solvent had floated to the top and evaporated, leaving an appreciable quantity of crystals which could be purified by recrystallisation. So, yeah, never be too hasty with throwing your base soup away - at least if you have somewhere safe to store it.

he is wondering if 3 acid pulls(100ml each) where enough

300mL of 5% acetic acid should be ample to recover 500mg of base.


I hope your friend has enjoyed doing the extra bit of 'science'! :thumb_up:

 

[oneistheall]

Imagine how MY friend is feeling now...amazing results! downwardsfromzero my friend is extremely grateful and told me to send you a hug!

 

[downwardsfromzero]

It really is a pleasure - thanks for the crystal pr0n!

I can almost smell them from the picture :want: