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Author Topic: safrole separation  (Read 324 times)

fresh1

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Re: safrole separation
« Reply #20 on: May 25, 2012, 07:22:06 AM »
Quote
If I want to freeze this sassy I'm going to need some CaCl2 for a proper ice bath, or some dry ice.

I would imagine just plain ole NaCl on ice will bring the temp down enough for this purpose, I forget how cold it gets but definitely several degrees below zero :-\
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uchiacon

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Re: safrole separation
« Reply #21 on: May 25, 2012, 10:28:14 PM »
Quote from: fresh1 on May 25, 2012, 07:22:06 AM
Quote
If I want to freeze this sassy I'm going to need some CaCl2 for a proper ice bath, or some dry ice.

I would imagine just plain ole NaCl on ice will bring the temp down enough for this purpose, I forget how cold it gets but definitely several degrees below zero :-\

Well unfortunately I tried that too. Left it for quite some time and it didn't solidify at -13C if I recall correctly. Trying to get this CaCl2 bath to work.

salat

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Re: safrole separation
« Reply #22 on: May 26, 2012, 10:16:14 AM »
Try acetone, methanol, or IPA for your liquid.
Salat

Twilight Mom

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Re: safrole separation
« Reply #23 on: May 27, 2012, 01:12:41 AM »
At -13C you just need a seed crystal. Mix up a saturated aqueous solution of MgSO4 and place a few drops of safrole in it. Put it in the freezer for a day or two and it should solidify with the safrole producing small sparkly needles around the edge of the container. Scrape up a bit and drop it into your supercooled safrole which will immediately crystallize.

The first picture shows the MgSO4 solution frozen solid.
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