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Re-X - no goo?

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Swarupa

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I recently did a small STB on 50g MHRB, i evaped on glass trays and ended up with waxy crystals, i scraped them up, put em in a beaker, added some warm Naphtha, but it just dissolved it all back into a yellow liquid, there was no goo on the bottom, is there any reason to cause this? Naphtha too hot? Not hot enough?

Im just putting it in the freezer now, hopefully what precips out (if anything) will be whiter & less waxy, i'm still concerned about my re-X process though, i just boil the kettle, pour into a dish, let the beaker of Naphtha sit in the water for a couple minutes then add it bit by bit to the DMT beaker until its all dissolved, maybe i added slightly too much Naphtha and that caused it to not 'goo' at the bottom?

Thanks
 
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After a freeze precip there was loads of yellow crystals in the jar, i wasn't satisfied to try & scrape waxy yellow stuff out the jar so placed it all back in a hot water bath, then left it to sit for a few hours in hot water bath until it cooled, still no separation of goo...

Gonna freeze precip again, pour away Naphtha, then redissolve the yellow crystals using really hot Naphtha (like that link described) then let it cool slowly, hopefully it'll work then... although im not sure what the difference will be as both times i will have used hot Naphthga that has been allowed to cool...

I just have one question, can i reuse the freeze precip Naphtha to re-X with even ifits yellow or should i use fresh Naphtha?

Thanks
 
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To get rid of the yellow goo, I heat up fresh-new naphtha in a warm water bath, just enough to warm it slightly. Then I put the spice in the naphtha, wait a few seconds until the crystals dissolve completely and a layer of goo form at the bottom. In my few attempts to re-X that separation occurred almost immediately. Then I transfer the DMT+naphtha to a new glass, being careful not to bring the goo.
 
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When i heated the DMT/Naphtha straigh out the freezer a tiny bit of oil did drop to the bottom, anymore heat & the oil dissolved, but if you have a glance at that link i posted he actually heats the solvent in boiling water for 15 minutes, adds to DMT, then lets the saturated solvent settle & cool in the water bath, ending with a separated layer of oil at the bottom. When i did this i didn't get that layer of oil at the end, just yellow Naphtha.

Im thinking this didn't work for me as i didn't use fresh Naphtha & maybe added too much Naphtha to the DMT as i was only recrystallizing about 300mg, so the Naphtha held onto the oil rather than only holding the DMT & rejecting the oil to the bottom.

At the mo i'm freeze preciping in a jar again, then will pour off Naphtha (onto dish incase theres anything still in there) and then remelt the DMT still stuck to the jar with fresh Naphtha, with the tek in that link...
 
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I did the above & think i vaporized all the DMT or something

I added hot Naphtha to the jar of precipitated DMT, there was about 1/2g of crystals in there, the DMT melted leaving oily residue, i poured off the saturated Naphtha (nice & milky) & then i placed it in hot water bath (forgot to add ice to cool to 150f!) it then soon turned back to yellow, and when evaped left nothing but some oily residue in a glass tray with a slight hint of DMT

I 100% had a beaker full of DMT after the freeze precip.
 
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