Recrystallization Loss WTF?!

[hexagonomicon]

So a STB tek was done using nomans tek. Only thing difference was that the naptha was washed with sodium carbonate solution before freeze precipitation. Yield was an amazing 500mg+ from 50g of MHRB! We were very excited! The crystals were only slightly yellow, but mostly very white.

Then we attempted to recrystallize this to try and get as pure of a product as possible. The following thread was used as a general outline for recrystallization tek:

Glass Shard Re-Crystallization Pictorial - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

Well it all didn't work out very well. Most of the recrys was spent transferring warm naptha with dissolved DMT in it from one container to another, trying to find a good vessel. No oily layer separated out, so it was decided to just say fuck it and re-freeze it so we could just have the crystals and no more worries.

So upon re-freezing over night and drying the crystals, the yield went from ~500mg to ~130mg! WTF!!!! First of all, there was no layer of "impurities" separated, so the DMT couldn't have gone there, there were only two containers used that had crystals formed on them... and they certainly didn't have a quarter gram crusted on the inside of them.

The naptha that was drained off is being evaporated. It's not completely done yet, but there certainly isn't much coming from there.

So I'm completely fucking baffled as to where my crystals went... I dissolved them and then freeze-precipitated as well as evaporated the naptha... It doesn't make sense. This is really going to discourage me from trying a recrystallization in the future.

 

[acolon_5]

Get 1/2 pint mason jars. The tall ones or the wide mouth will work very well. I use these for all my freeze precipitations as well as recrystalizations. They seal so you won't have an issue of spilling naphtha in the freezer (or having everything in your freezer smell like naphtha. They work well for seperating the oil slag from the clear naphtha (just decant), and they can even be put into a hot water bath to warm up the naphtha during a recrystalization.

Sounds like you might have lost some in the transfer. As long as you have all of your naphtha you should be able to recover it all. Spilling even a portion of it can result in quite a loss.