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help! first extraction result: brown powder Options
 
daoist
#1 Posted : 4/25/2010 7:21:03 PM
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oh yeah, I messed up the extraction...
cause I used the sep funnel but didn't have the pipette, so quite much of brown mimosa liquid ended up in the jars with the solvent pulled. Now, after refrigeration, I have mostly brown granuleted material...
What I need to do?
As far as I'v learned by reading posts here, I need to recrystalize... or maybe to make a sc washing.. that's is my doubt.
I still have in the freezer the jar with the last pull - the one you supposed to wait 1 day to pull..
My idea was to take this last pull off the freezer and join in his solvent my brown granulated material.
Then make a sodium carbonate wash of this mix.
Then put in the freezer and after that recrystalize if needed.

Do you think this could be the right solution?

Or maybe a simply recrystalization of my brown powder would be enough?

Thank you, forgive my english I'm from Italy.. and anyway, very nice forum you have!
 

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endlessness
#2 Posted : 4/25/2010 7:41:36 PM

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yeah I think you pretty much got it.. redissolve what you have in solvent in a thin tall container (and decant away from as much of the brown bottom goo that doesnt dissolve), do a sodium carb wash and freeze and retrieve crystals, and if necessary later recrystalize Smile

welcome!
 
daoist
#3 Posted : 4/25/2010 7:48:53 PM
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endlessness wrote:
yeah I think you pretty much got it.. redissolve what you have in solvent in a thin tall container (and decant away from as much of the brown bottom goo that doesnt dissolve), do a sodium carb wash and freeze and retrieve crystals, and if necessary later recrystalize Smile

welcome!


thanks man!! I'm gonna do that now..
 
endlessness
#4 Posted : 4/25/2010 8:02:22 PM

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good luck! tell us how it went
 
daoist
#5 Posted : 4/27/2010 8:56:34 AM
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endlessness wrote:
good luck! tell us how it went


I guess pretty fine! Now, after 24 h of freezing I puored out the solvent and was left with a large group of granulated white - some lightly yellow material..
I don't know if I can call that crystal, beacause I don't see any big crystal in cave fashion way... but maybe need need a microscope....?
anyway I left the thing dry for one night and now I have 1,2 g (from 100 of mhbr). I don't know how much it takes to evaporate all, still smells like nafta..
maybe do you know how much it takes, and if the smell will go away eventually?
thanks
 
endlessness
#6 Posted : 4/27/2010 9:46:06 AM

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yeah they are crystals but maybe too small for you to notice the crystally formations. Anyways, the naphtha smell should definitely go away eventually.. just break it all up, spreading it in a plate or something and leave it open for a couple of days.

alternatively, you can redissolve it all in ethanol/IPA/acetone and let it evap again to help getting rid of naphtha traces.
 
daoist
#7 Posted : 4/27/2010 11:18:51 AM
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endlessness wrote:
yeah they are crystals but maybe too small for you to notice the crystally formations. Anyways, the naphtha smell should definitely go away eventually.. just break it all up, spreading it in a plate or something and leave it open for a couple of days.

alternatively, you can redissolve it all in ethanol/IPA/acetone and let it evap again to help getting rid of naphtha traces.


Thank you, man!
I can't wait to find out what this spiritual molecule is about.. no problems if I do that alone, right? with no sitter.. I read I just have to pay attention to the pipe not to drop starting a fire..
 
 
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