First Recrystallization - No separation?

[SoulPioneer]

Hey guys, I had a question for those of you familiar with the recrystallization process. I tried it for the first time last night. Here's what I did:
-Made a hot water bath and warmed some "klean-strip" naphtha to 50 degrees Celsius.
-Poured approximately 8mL of warm naphtha into a small glass containing 250mg of "light yellow" spice.
-Gently swirled, everything dissolved in about 1 minute. Solution is now bright yellow.
-Blowing on it made it cloudy (confirming it's nice and saturated, according to posts I've read from others)
-Let it sit and cool to room temperature

Now here's my question, even after sitting at room temp for 4 hours, there was NO separation, NO gunk or "goo" at the bottom. Crystals did begin forming, and after 4 hours I put in fridge overnight, and into freezer this morning. The crystals are growing nicely, and that was really my only goal, with any purification being an added bonus. (the process, recrystallization, infusing leaf, making changa, or whatever, is almost just as enjoyable to me as smoking it! LOL) But I am still curious... Why no separation? No "goo"? Could it be that the spice is that pure already? (Without going into details, let's just say it came from a VERY reputable source) Or was there a mistake on my end? Don't think the naphtha was too hot, as I measured it at exactly 50 degrees before mixing.. Any thoughts?

 

[Firemetal420]

I've had the same thing happen. I think the reason is that I Stirred the yellow stuff too much. My most successful recrystallizations were when I heated my nps in a hot water bath and then dropped the yellow crystals in. I waited a minute for it to melt and then I gently stirred only the nps on top of the melted crystals without actually touching them until it wouldn't dissolve fast anymore. Decant the clearer nps off of that and place it in a different container for freeze precip. Hope this helps :thumb_up:

 

[Orion]

Don't swirl, just let it dissolve on it's own. Eventually there will be some dark liquid/crud on the bottom which you siphon your saturated solvent away from. You can save the crud from one or many extractions and do a mini a/b on it. Believe it or not ,as long as you didn't suck up any basic liquid before precipitation, it's still mostly DMT.

 

[JustCurious.]

Well, by the looks of things you didn't extract it yourself, I get this from 'source'.
So there is a good chance it has already had a re-x, in which case it would just dissolve in your solvent completely.
Extract your own spice, it's easy.

 

[JustCurious.]

Also, naptha can't really be too hot for a re-x, really you would want a boiling solvent which would allow you to re-x using the smallest volume possible which is what you want.

 

[FLeP]

Klean Strip is made up of part xylene and part aromatic hydrocarbons. Both of those are going to dissolve stuff you don't want. Use heptane or a better naphtha.

 

[SoulPioneer]

Thanks for the replies! Yeah I'll have to order some "Bestine" for next time. Nobody sells it around here lol. But I have collected and am drying the crystals. They look awesome! Yellow, but awesome! LOL. Now for the remaining (now clear) naphtha, I should just evap to make sure to retrieve everything? Or maybe evap until it clouds when blown on again and stick back in freezer?