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Recovery from NPS (Freeze Precip) Options
 
tolu
#1 Posted : 4/30/2009 9:52:44 PM
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pyx wrote:
SWIM has 4 ~50ml naptha pulls in 4 125ml mason jars in the freezer. The first 3 pulls have some snowy flakes growing. SWIM's question is how exactly would SWIM remove the NPS from the jars. SWIM's main concern is removing the floating crystals. Simply pouring the NPS through coffee filters seems a bit messy and SWIM doesn't really have the tools for this, decanting 5ml at a time with an eyedropper seems ok, but SWIM is worried it would take too long and risk redissolving crystals as the NPS warms.

To SWIY:
If possible, perform the removal of naphtha in the freezer to try and keep it from warming; otherwise you just need to be really quick.
I advise against using a coffee filter, you're going to lose product in it.
Instead you could try using a fine sieve such as this http://upload.wikimedia..../commons/0/00/Sieve.jpg, small enough to stop crystals falling through, large enough for the naphtha to pour easily.

pyx wrote:

Additionally, what exactly would SWIM do with the removed NPS? Would just evaporating it be sufficient in recovering and possible alkaloids caught in the NPS?

You could do that but you've defeated one of the main purposes of doing a freeze precipitation; no evaporation and you recycle your naphtha. You should of done one pull, freeze precipitated that, then used the same naphtha to do the next pull and so on.
No worries though, could save it for your next extraction or, like you say, evap it to recover anything that didn't precipitate out (might as well of just evaporated it all in the first place).

pyx wrote:

The 4th pull was with the lye/bark mix for about 18 hours and has been freeze precipitating for about 12 hours. It is just cloudy and yellowish with no crystal formations. Would evaporating about 50-75% of this pull and then attempting to freeze precipitate again be the recommended solution?

My friend would just straight evaporate it, however marsofold and others recommend evaporating to 10% of the original quantity then freeze precipitating. Either of these should be successful.

Hope it works out Smile
 

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pyx
#2 Posted : 4/30/2009 10:06:37 PM
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pyx
#3 Posted : 5/1/2009 1:54:40 AM
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