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Super freezing the solvent. [questions] Options
 
fireup6
#1 Posted : 12/9/2010 3:54:35 PM
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If lets say SWIM needs to freeze percip some xylene saturated with spice, would it be possible to put the container in a bucket filled with dry ice and cool it to very low temperatures in a matter of minutes?

Could SWIM drop a chunk of dry ice into the solvent?

Once the solvent is cooled to the needed temperatures, does the DMT crystallize and crash out instantly? Or does it take the reccomended 24-48 hours?

My main idea is to bring the solvent to very low temperatures very quickly, and hopefully get the DMT out within an hour, instead of keeping it in the freezer overnight. Would this be possible?
 

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DiMiTriX
#2 Posted : 12/9/2010 5:37:39 PM

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swim thinks you could drop it into..couse co2 doesn't react with naphta..it's just solid co2 isn't?
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gammagore
#3 Posted : 12/9/2010 5:57:27 PM

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You can't freeze precip xylene, you going to need to evap it or salt it out.
 
Infundibulum
#4 Posted : 12/9/2010 6:00:53 PM

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fireup6 wrote:
If lets say SWIM needs to freeze percip some xylene saturated with spice, would it be possible to put the container in a bucket filled with dry ice and cool it to very low temperatures in a matter of minutes?

Could SWIM drop a chunk of dry ice into the solvent?

Once the solvent is cooled to the needed temperatures, does the DMT crystallize and crash out instantly? Or does it take the reccomended 24-48 hours?

My main idea is to bring the solvent to very low temperatures very quickly, and hopefully get the DMT out within an hour, instead of keeping it in the freezer overnight. Would this be possible?

Don't do it, waste of time.

SWIM has tried that with both xylene and (heavy) naphtha. Xylene freezes in dry ice and it is pretty difficult to understand whether what you see is dmt precipitating out or solvent crystallising while it freezes. All these happen pretty fast too, within minutes

Naphtha is better, because dmt crashes out very quickly, but then these crystals are extremely fine and takes them a long time to precipitate. You'll have to stick the naphtha in the freezer fo rat least overnight, because on the dry ice the naptha will freeze. So unless you have a more sophisticated machine to harvest the tiny crystals pit of naphtha (e.g. a centrifuge) do not bother.


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Elf Machine
#5 Posted : 12/9/2010 7:13:16 PM

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A container of dmt saturated naptha was put in a cooler of dry ice overnight. The naptha got to roughly -35c where waxy impurities began to precipitate.
 
fireup6
#6 Posted : 12/10/2010 1:10:56 AM
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Infundibulum wrote:
fireup6 wrote:
If lets say SWIM needs to freeze percip some xylene saturated with spice, would it be possible to put the container in a bucket filled with dry ice and cool it to very low temperatures in a matter of minutes?

Could SWIM drop a chunk of dry ice into the solvent?

Once the solvent is cooled to the needed temperatures, does the DMT crystallize and crash out instantly? Or does it take the reccomended 24-48 hours?

My main idea is to bring the solvent to very low temperatures very quickly, and hopefully get the DMT out within an hour, instead of keeping it in the freezer overnight. Would this be possible?

Don't do it, waste of time.

SWIM has tried that with both xylene and (heavy) naphtha. Xylene freezes in dry ice and it is pretty difficult to understand whether what you see is dmt precipitating out or solvent crystallising while it freezes. All these happen pretty fast too, within minutes

Naphtha is better, because dmt crashes out very quickly, but then these crystals are extremely fine and takes them a long time to precipitate. You'll have to stick the naphtha in the freezer fo rat least overnight, because on the dry ice the naptha will freeze. So unless you have a more sophisticated machine to harvest the tiny crystals pit of naphtha (e.g. a centrifuge) do not bother.



Ah i see. Is there a temperature which is optimal for precipitating out clean DMT without impurities? SWIM's freezer is at about -17 C.
 
Swarupa
#7 Posted : 12/11/2010 12:16:53 PM
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Patience is key with freeze precip ime.

I usually left the glass dish in the freezer for 24 hourzs, 48 max, but recently i forgot about the dish in freezer (it was the 5th pull) and after around a week of being the freezer i yielded as much as my first pull.
 
FiorSirtheoir
#8 Posted : 2/21/2011 1:28:00 AM

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Did it precip impurities when the naphtha freezes or was it frozen naphtha that dropped out with the crystals? If it was just frozen naphtha seems you could collect and evaporate leaving behind the crystals? Or is the -10F to -20F specific to the alkaloids you want?
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