Safrole from Freeze Crystallization - Tweak/Observations

iodide · Tue Jul 19, 2005 2:09 am

I met an old buddy from Uni, recently, and this is what he told me:

1. The concentration of Safrole does NOT have to be high in order for this method to work. Safrole WILL start to crystallize even when it is present in mediocre quantities.

2. For some unknown reason, a quantity of Sassafras oil will be much more inclined to crystallize if it has crystallized before. He doesn't know why, but swears this is the case. Therefore, before engaging in any purification, simply deep freeze the oil by any means you can. If your freezer does, then great, if not, then get an acetone/ice bath or something. Just get the body of oil to freeze SOLID, impurities and all.

3. Once you've had this frozen solid, thaw out *nearly* all the way, that is, until only a tiny chunk (perhaps the size of a matchbook) remains, then quickly put into the fridge (set on max). This way, the nugget of crystal will act as the seed and allow it to recrystallize slowly! Presto, no need for a seed crystal. This can be done over and over again too! Meaning, once it has crystallized slowly and nicely, and you've decanted the impurities, the rethawing of the safrol should be done until a matchbook size remains, then toss back in fridge for a second-pass rescrystallization!

methyl_ethyl · Riedel De Haen

The concentration of Safrole does NOT have to be high in order for this method to work. Safrole WILL start to crystallize even when it is present in mediocre quantities.

For some unknown reason, a quantity of Sassafras oil will be much more inclined to crystallize if it has crystallized before. He doesn't know why, but swears this is the case.

This unknown reason is a result of the fact that there is a direct correlation between crystalization yield and safrole concentration. You spelled it out yourself.... Re-read your above post....

This topic has been discussed ad-nauseam, in recent and historic threads....

m_e