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Recrystalization question (with pic)

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ghostman

ghostman

Rising Star
I dissolved 2.5g spice in a shot glass with a little naphtha. There is a clear darker layer with some white chunks underneath. I use a sep funnel and never let any soup into the solvent when pulling.

What exactly is in the darker layer and underneath and should I store it for a future extraction or dump it?

re-x.jpg
 
how much naphtha in ml you think that is? you need maybe 30ml per g of dmt so you should have at least 75ml naphtha otherwise there's gonna be plenty of dmt in that bottom layer

SWIM would decant the top layer (and that into the freezer), add more warm naphtha to that bottom layer and it should pick up more dmt...
 
Depending on what steps you used previously, it's likely a mixture of oils, fats, tannins and n-oxide. Could be, if you weren't careful along the way, that it even contains some lye (but you say that you were, so probably not). Regardless, I definitely wouldn't dump it. Oxides are plenty active and can either be used as is, or collected and converted back into DMT with zinc.

Your top layer will yield a much purer product with a better defined melting point, and it ought to pack all of the punch with considerably less of a body load.

BTW, heptane is a much better option for this than naptha, but you can always recrystallize repeatedly. Try a freeze precip for the first and slow evap for the second - 20 mls per gram.
 
This was about 30ml solvent. It set almost immediately and started forming crystals within minutes. I skimmed the top layer and did another 2 dissolves. There was no residue left, except for a tiny lump of ear-waxy stuff.

I did an AB extraction and have a large sep funnel. I am always very careful not to get ANY soup into my solvent pulls. The first set of precipitated crystals were chunky white with a slight trace of dark yellow in parts, hence the re-exing.

Art, sadly heptane is nigh on impossible to get in my neck of the woods... hence the naphtha.

Thanks for the feedback guys, I'll post results.

You guys rock!
 
Some of that is n-oxide (orange/yellow), some of that is undissolved spice (white) because swiy used a tiny amount of solvent.
 
I am now facing a challenge...

I did 3 x re-crystalizations of 30ml on 2.5g of what actually pretty clean spice. Each batch went into a shot glass (see pic above). I put the three glasses into a cabinet for 24 hours, they evaporated to about half. I took the first 2 glasses (the cleanest) which had little pure white crystal formations all around the sides of the glass and put them into the freezer to finish off with a precip.

24 hours later nothing has precipitated out!

There are crystals in the glass, but nowhere near the 2.5g that originally went in.

The naphtha was quite hot when it went in. Have I lost spice by somehow destroying it?

We live, we learn...
 
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