Author Topic: Sassafras purification using NaOH and distillation  (Read 806 times)

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abuse

  • Guest
Sassafras purification using NaOH and distillation
« on: October 03, 2003, 03:48:00 PM »
Can someone please confirm this route for isolating safrole from sassafras oil.

1) Treatment with 5% NaOH

Treate sassafras oil with an equal amount of 5% NaOH solution (I'm assuming this solution is calculated by weight, for example 25g NaOH + 475g dH2O). This will create eugenol anion crystals in the water layer, which is decanted from the oil. Wash the remaining oil with 3X dH2O and decant the water layers from each washing.

Transfer oil to a cooking pot and raise temp. to 100C to remove excess water.

2) Distillation of safrole
Set up for simple vacuum distillation. If the vacuum pulls 20mm, then the following should occur under slow and controlled heating conditions...

at ~55C, pinene distills over
at ~70C, phellandrene distills over
at ~100C, d-camphor distills over

Once the remaining d-camphor distills over, the tempurature of the distilling flask will begin to rise to the bp of safrole under vacuum at 20mm, namely, 125C. At this point, the contents of the distilling flask can be considered relatively pure safrole.

Look ok?

Osmium

  • Guest
> Look ok? Nope. 1) It's not necessary to...
« Reply #1 on: October 04, 2003, 06:01:00 AM »
> Look ok?
  
Nope.

1) It's not necessary to do this NaOH wash.
2) heating safrole to boil out water is wasteful and smelly.

> the tempurature of the distilling flask will begin to
> rise to the bp of safrole under vacuum at 20mm, namely,
> 125C. At this point, the contents of the distilling flask
> can be considered relatively pure safrole.

Temperatures are taken in the vapor phase, not inside the distillation flask.
And you need to distill the safrole, you cannot simply heat it up to its boiling point and expect it to be pure.


abuse

  • Guest
The correct temperature of the distilling...
« Reply #2 on: October 04, 2003, 09:01:00 AM »
The correct temperature of the distilling flask is read from the thermometer as long as there is condensation on the thermometer bulb. Is this what you mean by "vapor phase"?

>And you need to distill the safrole, you cannot simply heat it up to its boiling point and expect it to be pure.

Ok, understood.

mindlib

  • Guest
re
« Reply #3 on: October 04, 2003, 12:31:00 PM »
The temperature should be from the thermometer in the 3-way adapter or the whole piece condenser. It´s the temperature from the vapor fraction.

btw,  double or triple freezing, as abolt told...wonderful...

abuse

  • Guest
I should have been more clear...
« Reply #4 on: October 04, 2003, 02:38:00 PM »
Yes, the thermometer in the 3-way adapter; that's the one that displays the vapor temp.