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crystals forming in solution after basing

Started by oi281, December 30, 2003, 09:41:00 AM

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oi281

swim ran a 7 gram 20 hour reaction, using generic 60's which were recrystalized twice, lab grade iodine and mbrp. after completion added 100ml dh20 and boiled for 10 mins, washed with xylene 2x, then based solution, a greenish cloudy mix floated up to the top of sep funnel, then 40ml zxylene was added, let it sit for about  a hour, when returned all looked good, when seperating the two layers crystal shards started-forming rapidly, causing swim to get panicky now the solution has a orangeish color with tiny slivers in it.- are those glass needles meth or is it something else, and what can swim to reclaim the goods now------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------







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Osmium

Add hot water.

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geezmeister

After you add the hot water, complete the extraction and let us know what you collected.

Next chance you have, get some NaOH rather than RDL. You will find it more to your liking.


CharlieBigpotato

one time , bizarium claimed to have isolated the mcc from a dream gone south.

he said they were gorgeous , glassy chunks, with the slightest pink hue.
beecause they defied normal logic as to where they would crystalize, biz never bothered to taste the stuff.

why would anyone?

hey geez!

what makes you think he didn't have naoh?
beesides, what is rdl possibly going to add to the equation?

its too cheap to fuck with

oi281

swim added h20 and the solution cleared up, with little clouds floating up towards the top, swim did use NaOH, but swim is colored blind and has given up using test strips, and is using observation skills untill a ph meter is bought, is swim geting the ph to high and this might be the reason for the crystals to crash out of the xylene? now would the best thing bee to just add some more h2o and boil dow down, and start over? thanks for all your help, you guys are all awesome

geezmeister

I've used more than one bottle of RDL that had something which turned the reaction fluid green, or black, or some strange colors. I guessed that the green color was from a strange batch of RDL, and was incorrect.


now would the best thing bee to just add some more h2o and boil dow down, and start over?




No, just add your nonpolar solvent and extract. If you boil the fluid content down, you will just be back where you were.




fierceness

swif has seen the gorgeous glassy chunks before but it was from a sucessful rxn.. it was just NaOH + impurities that he let sit out for too long.. does not mean you have a failed rxn