sassafras crystalization...

Soap · Mon May 02, 2005 10:30 am

sorry to start a new thread on an old topic, but swim has yet to find any information on what has happend. Swim put 60 or so ml of sassafras oil in the freezer and after several days it has become one solid crystal. swim turned the glass bottle it was frozen in to decant any liquids that may have been present but there was nothing. not a single drop. should he try washing the crystals with some solvent that wont desolve teh safrole???? the crystals are realitvly pure looking not to much off color. i dont think swim has ever heard of anyone getting 100 percent safrole, sassafras oil.... Confused

Pemulwuy · Mon May 02, 2005 2:13 pm

Safrole can extracted from sassafras oil by crystallisation in the refrigerator

Take a small portion of your frozen block and return it to the freezer as a seed crystal. Next, thaw out the rest of your oil and place it in the refrigerator overnight.

In the morning take your seed crystal from the freezer and drop a third of it in the oil that you left overnight in the refrigerator, then return the oil and leave it for a day or two in the refrigerator.

After the allotted time, take the oil out of the refrigerator and decant away the impurities.

Re-thaw out the oil, cool it again, in the refrigerator, and repeat the process twice more for fairly pure Safrole.

Served chilled with Sweet Vermouth. (garnish optional)

Soap · Wed May 04, 2005 12:39 pm

swim would like to recomend this method to any new bees that want to purify thier sassafras oil. swim will be posting pictures of the crystals that were created with this method, hopefully by later today. very beautiful Very Happy

sg43 · Thu May 05, 2005 10:26 am

Soap, glad to hear that swim is having some luck with that sassy Wink

, please do post some pictures, swim finds this method very interesting Laughing

Soap · Fri May 06, 2005 10:37 am

well swim had some problems borrowing the camera so it took some time. but here it is (nothing to amazing) swim couldnt get the camera to focus on the crystals but you get a general idea. this was done with about 60 ml sassafras oil (1st freezing). this was swims first tiem so he used very little... If his results are satisfatory (are they?) he may consider doing an illustrated write up on the whole procedure.

echoes · Tue Jun 07, 2005 11:09 pm

how pure is the safrole obtained from such an endevor? pure enough? I have just recently found out about this method, you should definatly do an illustrated write up, that would be great

ApprenticeCook · DILLIGAF

soap... nice...

The sassy from crystalisation is pretty good purity provided you do the process several times with the resulting solids being re-processed each time. It is however in the best interests of proceedure to then vacuum distill the safrole to gain the purity levels which allow the best yields to be obtained from isomerisation and peracid oxidation.

The best method swim used was to freeze out safrole 4 times followed by distillation, the benefit of freezing out first is that when it comes to distillation you dont need to be constantly stopping and starting for fractions other than safrole (if you dont have a fraction cutter or perkin reciever).
With distillation after crystalisation all you have is the safrole and the components with a higher melting point than safrole which in sassafras oil is not much as most of the other components in the oil have a lower melting point than safrole and are hence excluded in the previous crystalisation steps.

-AC

Soap · Wed Jun 08, 2005 8:53 am

great post a.c let ii be a lesson to all that distilling the sassafras extract (after freezing) can definetley make a difference. Swim believes taht the reason his isomerization was so unsucessful was due to the fact that he did not distill. so dont be lazy! we are talking about potentionaly thousands of dollars at stake here (only in dreams of course)