BieneMaya (Stranger)
12-08-02 10:53
No 387501
      Safrol Boiling point 86 C  Bookmark   

Is it possiple that safrol comes over at 86 C ?
Of course swim has got a profesional vacuum pump
with 0.01 mbar.
Could swim also get a yield of about 95% from sassy oil?

 
 
 
 
    Xicori
(Newbee)
12-08-02 11:29
No 387511
      yeah, 86°C seem to be possible with a oil-pump!  Bookmark   

yeah, 86°C seem to be possible with a oil-pump!

see ../rhodium /equipment/nomograph.html !

have you used a column for distillation?
 
 
 
 
    pickler
(Greenhorn)
12-08-02 13:44
No 387556
      It is very possible to get safrole at 86c.  Bookmark   

It is very possible to get safrole at 86c. Swim's old pump, a ritchie yellow jacket, pulled safrole at 70-72c. 95% safrole from sassy is possible, but more likely you'll get around 90% or so. Usually good sassy oil has about 80-90% safrole. 

I went into the business for the money, and the art grew out of it.-Charlie Chaplin

 
 
 
 
    BieneMaya
(Stranger)
12-09-02 04:24
No 387778
      Yes I used a 200 mm silvered and vacuum jacketed ...  Bookmark   

Yes I used a 200 mm silvered and vacuum jacketed column.
But I ran the system without any seal like silicon grease.

I got a yield of 100ml with 105ml starting sassy.
The destillation ran very quickly (about 5 drops per second) and reached 1 drop per 5 seconds at the end.

I even had could collected more safrol, but it wasn`t worth to wait 5 seconds and more for a drop.
 
 
 
 
    goiterjoe
(Title on BackOrder)
12-09-02 07:20
No 387801
      what you have isn't pure  Bookmark   

If you were distilling over 5 drops a second, you were running your distillation to hot and fast.  Just react the impure safrole collection you have, as it should be good enough for the time being, and try to get cleaner fractions in you subsequent distillations of Isosafrole/ketone.

If at first you don't succeed, try, try again. Then give up. There's no use being a fool about it.
 
 
 
 
    BieneMaya
(Stranger)
12-10-02 04:08
No 388077
      Oh yeah that could be the problem.  Bookmark   

Oh yeah that could be the problem. I`ve got only one thermometer so i couldn`t controll the temperature of
the oil bath.
If I understand it exactly, a destillation runs too hot
and too fast when the oil bath is a lot hotter than
the expected boiling point, right?
But the collected safrol is absolutly water white and
reflects light as it was described.
I think I`ll destill it again and then I`ll see how much
product will be collected.