homeslice
Harmless
Posts: 23
Registered: 28-1-2012
Member Is Offline
Mood: No Mood
|
|
Separation of Sassafras Oil from hydrosol
Any advice on separating sassafras oil from hydrosol post steam distillation?
I read someone suggested methylene chloride.
Any advice?
|
|
|
homeslice
Harmless
Posts: 23
Registered: 28-1-2012
Member Is Offline
Mood: No Mood
|
|
Separated the hydrosol from the oil by gravity. About 55ml was there.
Then extracted the hydrosol using DCM then distilled off. What was left was kind of thick unlike sassafras oil. It seemed syrupy at room temperature.
Only got around 40ml of the stuff from a 1000ml extraction out of at least 10 gallons hydrosol.
The hydrosol was saved in case he decides to try another extraction. He was kind of under the assumption that after the extraction that it would have
cleared up, it didnt. It still appears milky white. Is this normal post extraction of hydrosol with non polar solvents?
Also, is it worth filtering and extracting the actual water used to boil the roots? A hydrodistillation was performed rather than just steam
distillation so there is plenty of water left over that the root chips boiled in. Will that contain any of the oil? Should it be extracted?
Overall, from bark and roots, it appears that maybe 75lb of semi dry bark and roots, distilled in two batches for more than 5 hours each time, yielded
less than 100ml sassafras oil. Not exactly ideal considering the amount of time and effort put into the ordeal.
The two big questions that he is looking for answers to are, should the boiling solution be extracted? And should the hydrosol clear up from its
milkyness after being extracted? Why is it milky colored?
[Edited on 28-7-2012 by homeslice]
|
|
|
bbartlog
International Hazard
Posts: 1139
Registered: 27-8-2009
Location: Unmoored in time
Member Is Offline
Mood: No Mood
|
|
He? Who?
Anyway, without knowing more about the conditions of your distillation it would be hard to guess whether there is still more essential oil to be
obtained. How big were the pieces that you boiled?
At the scale you are working, I would suggest assaying a portion of the material. Take small sample of the remaining root bark, pulverize it, extract
with 50/50 chloroform and hexane. Evaporate that and see what's left in the bark. Then you'll have an idea of whether there is still more essential
oil to be obtained.
I would also suggest adding salt (like CaCl2) to your hydrosol in order to encourage separation of the oil from the aqueous phase.
The less you bet, the more you lose when you win.
|
|
|
homeslice
Harmless
Posts: 23
Registered: 28-1-2012
Member Is Offline
Mood: No Mood
|
|
The pieces were chipped through a chipper shredder.
I think its impossible to make an educated guess at how much oil there should be. Some parts have a higher concentration than others and then its
tough to weigh it because it might not be dried out right and then in certain parts of the season there is more or less. Just too many variables to
guess at.
How much calcium chloride would you add to say about 10 gallons of hydrosol? Do you know why the hydrosol is milky colored? I figured it contains oil
if its still milky but im not sure if thats the case or not.
|
|
|
blogfast25
International Hazard
Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by homeslice  |
How much calcium chloride would you add to say about 10 gallons of hydrosol? Do you know why the hydrosol is milky colored? I figured it contains oil
if its still milky but im not sure if thats the case or not. |
Quite a lot, I'd say. Make a few liters of saturated CaCl2/water solution and add a couple to your hydosol and mix well. Add more if it doesn't clear
fully. The milkiness is due suspended (emulsified) oil(s).
[Edited on 28-7-2012 by blogfast25]
|
|
|
homeslice
Harmless
Posts: 23
Registered: 28-1-2012
Member Is Offline
Mood: No Mood
|
|
Ok i will try that on a small scale today and see if it causes my oil to crash out.
|
|
|
homeslice
Harmless
Posts: 23
Registered: 28-1-2012
Member Is Offline
Mood: No Mood
|
|
Would the liquid that the roots were boiled in contain any oil?
|
|
|
hyfalcon
International Hazard
Posts: 1003
Registered: 29-3-2012
Member Is Offline
Mood: No Mood
|
|
The time of year you harvest your roots makes a big difference in yield also. February is the best time to harvest Sassafras around here.
|
|
|
homeslice
Harmless
Posts: 23
Registered: 28-1-2012
Member Is Offline
Mood: No Mood
|
|
It would be hard if not impossible to spot sassafras trees in february without the leaves on the trees.
How big of a difference does it actually make?
|
|
|
hyfalcon
International Hazard
Posts: 1003
Registered: 29-3-2012
Member Is Offline
Mood: No Mood
|
|
I know where my Sassafras grows. It makes all the difference in the world the time you harvest. February is just before bud break in the Spring. The
roots are primed with all the stored nutrients ready for the Spring push. This is when the old timers always harvested their sassafras for the
strongest medicinal value when it was used as such.
|
|
|
homeslice
Harmless
Posts: 23
Registered: 28-1-2012
Member Is Offline
Mood: No Mood
|
|
Cant do february here. The ground is rock solid frozen.
Heres a question for ya though. Does it matter if the harvested rootbark dehydrates prior to steam distillation? Does the amount of time the harvested
rootbark spend above ground make a difference in the oil yield?
|
|
|
hyfalcon
International Hazard
Posts: 1003
Registered: 29-3-2012
Member Is Offline
Mood: No Mood
|
|
Fresh is always better, but not necessarily. You pick the month before bud break but after you can dig the ground for the most potent roots.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
