cant get safrole? FREEZE IT!

[RoundBottom]

way to go.  looks awesome, doesn't it?  the trick is the slow freezing.  fast freezing results in more of a crysteline mush.  hard to desribe, like a chunky slushie, i guess. 
i learned a thing or two from charlie dontcha know.

[humidbeing]

Yeah, but it's fun to drop a crystal in supercooled oil
and watch the stuff "bloom" like a mandelbrot painting.
CG I miss you sweety, I really do.

[chem_123]

please go to this post and help with SWIM's problems

Post 294100 (missing)

(chem_123: "steam distillation!?", Newbee Forum)My schwartz is bigger than yours!  

[terbium]

Yeah, but it's fun to drop a crystal in supercooled oil
I actually once had a beaker of supercooled water crystallize on me like that. I was extracting mescaline from peyote buttons and wanted ice cold water to wash the mescaline sulfate.

There was no freezer in the apartment over a garage where I was working so I had someone stick a liter beaker of water in the freezer in the main house. Later they retrieved the beaker and carried it all the way from the main house and up the stairs to the apartment still in a liquid state. When I put a thermometer in it and gave it a quick stir it suddenly all crystallized in a matter of seconds.

[RoundBottom]

ok, does someone want to try this?  take an amount of sassy oil, shake it up for a bit, and split it into two equal portions. 

take one portion and vac distill it.  measure the amount of safrole.

take the second portion, and freeze crystalize it.  measure the amount of safrole.

write a post with the two numbers.

this should answer the question.
i learned a thing or two from charlie dontcha know.

[chem_123]

very scientific of roundbottom to suggest that...SWIM'll be eagerly awaiting the results as well!
My schwartz is bigger than yours!  

[RoundBottom]

bastardo

obviously someone didn't take to heart my statement that SWIM is a lazy bastard.  SWIM would love to do it, but, as above, SWIM is a lazy bastard and doesn't want to run that noisy pump in SWIMs apartment when SWIM doesn't have to.

unless a karma reduction is heading my way, that's where SWIM stands.  :p ptttffftttt!!!!
i learned a thing or two from charlie dontcha know.

[LaBTop]

It was already stated that the sassafras was FIRST professionally fractionally distilled, and gave a product with a FAR off density of 1.088.
Then 3x freezing gave safrole with nearly the right density of 1.0994.
So yeah, it would be nice if someone who knows what he's doing, and not the occasional garage chemist, would repeat that, and checks the densities folowing my posted procedure about calibrating a 1 liter erlenmeyer, or has a calibrated professional 1 liter density testing bottle. LT/
WISDOMwillWIN

[RoundBottom]

guess that means you have to do it hydro!

oh, he means me.  ok, but i won't be able to until next week.  can anyone do it this weekend?  *sigh* i thought my sassy distillin' days were over.
i learned a thing or two from charlie dontcha know.

[humidbeing]

Here are a couple pics of slow grown safrole crystals,
that were obtained from an adulterated soultion of
non safrole components, from natural oil.

http://WWW.rhodium.ws/archive/picture108.jpg

http://WWW.rhodium.ws/archive/picture110.jpg

Those are rods are half inch thick and 3/4 inch long.
CG I miss you sweety, I really do.

[dr_ruthenium]

Did the safrole from those crystals oxidize and aminate, like safrole from non-adulterated oil?

[PrimoPyro]

Of course they did.
Vivent Longtemps La Ruche!

[dr_ruthenium]

Uh, that was directed to humidbeing.  I guess your point is that safrole can be purified from (if it even exists) adulterated/denatured sassy.  This safrole will oxidize and aminate.  VL posted how hsi wouldn't.  Not only that, but the only physical properties that difffered between iso that resulted in honey and iso that didn't were forming pseudonitrite cake without any tan polymer and (one other property which I forgot).  My impetus for posting to this thread is to try to determine where my error lies.  And, I am considering the denatured sassy theory.  I sure hope that I am barking up the wrong tree!

[PrimoPyro]

I had mistakenly written my answer with the assumption of your question being if safrole purified by freezing would react the same as safrole purified by distilling: they would.

If that was not your question, then I apologize for the intrusion.

                                                  PrimoPyro
Vivent Longtemps La Ruche!

[dr_ruthenium]

Yeah, just wanted to know if that safrole isolated from the adultered sassy worked.  No foul dude.  Any help you can give me would be much appreciated.  See my thread "Amination Failure".  Thanks.

[humidbeing]

Swim doesn't know, but has heard yes.
The term adulterated means only that more non-safrole
constiutuents of natural oil were added before freezing took
place.
The actual brand of oil has been known to be authentic.
CG I miss you sweety, I really do.

[Rhodium]

Safrole is safrole as long as it has been purified. It doesn't matter how it has been purified or what it has been purified from - it is still the same molecule.

[LaBTop]

The question here seems to be if an addition is invented that can't be circumvented by our normal lab techniques. It is mentioned already since 1998 in these forums, and it seems to me that it's not a hoax, i've once seen it myself, all goes perfectly well untill the end, then your crystals melt in 5 minutes exposed to the air, or you don't get them at all.
Simplest solution: buy from non US sources, it is definitely contained to the US suppliers only, ...yet. LT/
WISDOMwillWIN

[scram]

How come I never got credit for this shit!

Post 107751 (missing)

(smokemouth: "DP Harma's Sassafras Freezing technique Modified - scwam", Methods Discourse)

Post 107782 (missing)

(smokemouth: "Determining Safrole content thru congealing point - scwam", Methods Discourse)

[LaBTop]

Dammit, already so early posted all that good info, from scwam, DPharma and Osmium and some more, why tend so much info to sip away over the years and get forgotten?
I'm glad dormouse did all that recovery work that time, thus saving all this hours of typing in invaluable info by so many former and recent members. LT/
WISDOMwillWIN