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Author Topic: Help is this safrole?  (Read 422 times)

doow4681

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Help is this safrole?
« on: May 18, 2011, 06:22:09 PM »
 over the course of a few summers swij  hiked through the forests and on his travels he slowly harvested sassy roots. collecting about six rubermaid totes of that lovely aromatic root. Then after feeling confident that he had enough he invested in an essential oil steam distillation app. and began the slow and tedious  distillation of his wonderful smelling root chips yielding 800ml of a wonderful smelling oil. up to this point his nights were filled with wonderful dreams. he then started to distill in a simple distillation without vacuum because was told it could be done. the distillation was started, the temp rose to about 160 degrees c  when first fraction came over,the temp slowly rose to 180 then next fraction came over. then temp shoots to 224 when next fraction comes over from up to 228. then temp plummets drasticlly. it is in between 224-228 when 80% of flask contents come over. what is it, this is not within the desired temp range what went wrong? now his nights are filled with nightmares fearing all his work was in vain. is there anyone who can help swij sleep sound again?

antibody2

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Re: Help is this safrole?
« Reply #1 on: May 18, 2011, 06:35:31 PM »
What kind of thermometer are you using for you distillation? If you are using an immersion thermometer for distillation and the immersion line is well above the three way split in your distillation adapter, it is possible you are getting a low reading. Try bringing a small sample to a boil in a beaker and immerse your thermometer (up to the immersion line) in it and see if you get a different reading. The BP you are after is 232°C.

Its also possible you have a poorly calibrated thermometer, you might try the above test with a different thermometer too.

You might have what you have been dreaming of 8) don't give up just yet.

Good luck
« Last Edit: May 18, 2011, 06:39:03 PM by antibody2 »

fractal

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Re: Help is this safrole?
« Reply #2 on: May 18, 2011, 07:45:58 PM »
Holy shit man use a vacuum. Your going fry all your hard work. Like AB said sounds like you have sass. If your not going to use a vac source you should just skip the distillation and isolate safrole through washes. You can find the procedure on here. Trust me you need a vac.

antibody2

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Re: Help is this safrole?
« Reply #3 on: May 20, 2011, 01:03:07 AM »
Quote from: doow4681 on May 18, 2011, 06:22:09 PM
collecting about six rubermaid totes of that lovely aromatic root.

Out of curiosity (and not knowing how big these "totes" are) how much root material did you need to steam distill to get 1000ml of sassafras oil? Also did you chip the entire root, or just the root bark?

Sedit

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Re: Help is this safrole?
« Reply #4 on: May 20, 2011, 01:17:27 AM »
A 1 liter jug full of ground wet root bark yeilds between 25-50ml of oil or so i'v heard ;)

Rootbark generally contains betwen 5%- and 9% essential oils per weight of dry bark.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

sassa

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Re: Help is this safrole?
« Reply #5 on: May 20, 2011, 01:30:21 PM »
I think too that 224-228ºC fraction it´s 99% sure your safrole.Like people said,I have seen too position of the thermometer on the 3 way adapter it´s crucial to get an exact distilling temperature,and too the accuracy on plain thermometers it´s not allways perfect.That fraction have to be water like with little drops milk on it,like very very diluted milk on water,and smells like the raw oil,but more anisse acentuation.
    Ner proved to distill at atmospheric pressure,but seems one most important photo-articles about the process,begins distillation safrole this way,with temp as yours,and claims to not be a problem.But you must of course fractional distillation it better.Safrole it isn´t hard to fractional distill like can ketone be.Posibly you will degrade a minimal amount,but you have a lot anyway.I would recommend distill it on 2-3 batches ,to not stress the oil too much time at too high temp.
    Related to that,seems sassafras oil it´s getting harder and harder to find these days.Like supossed,each guy have his source and don´t want to let to anybody.Posibly, if i lost my source,i think will be almost imposible to get it again at this moment.
   Posible our sons will have to get sassafras seeds on the illegal market!  ;)

Shake

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Re: Help is this safrole?
« Reply #6 on: May 20, 2011, 03:39:52 PM »
yes, that is close enough.. if you fractioned then the only close boiler will be eugenhole, and i think thats a little higher..
 besides eugenol washes out with 5% NaOH washes


yeah these totesmust have been 10kgs worth or more then.. lol a liter is quite a bit!
« Last Edit: May 26, 2011, 09:55:06 PM by Shake »

doow4681

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Re: Help is this safrole?
« Reply #7 on: May 26, 2011, 04:13:59 PM »
to give a better idea of the the amount of root steam distilled the totes were 18gallons. I used the entire root. i first peeled the bark from the root and spread the root peelings out on the tote covers and would place them on top of the kitchen cabinets to dry out this is very important because if the root peelings are not sufficiantly dry they will mold lightning quick, i mean like over night. i them cut the rest of the root up into small pieces i used a pair of garden clippers which were very time consuming, Im sure who ever can find a much more efficiant way im just saying what i did.
 know after seeing my finally yield of oil people should look no father than there own back yards, because the amount of work it took wasnt all that much and could be done  much faster if thats what you were set out to do. my sassafras was collected while going on short hikes about ten total. once I got  the hang of harvesting the root and learning how the runners grow i could dig up large roots fifteen feet long that would only be about 8 t0 12 inches deep in the ground . in like twenty minutes. with that being said what a good feeling it was to looking at all that wonderful oil knowing that i was the one who took this from the earth. hard to explain, i guess a feeling of accomplishment. i can only imagine what the future holds.

Shake

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Re: Help is this safrole?
« Reply #8 on: May 26, 2011, 09:54:19 PM »
doow4681 nice work! what tree exactly are we after here? i mean the specific name, there are tons of saf containing trees.. i guess america is the place for them.

I had no idea there was so much oil in the roots, i guess it all just runs to the bottom haha

def a viable way, i would do a super efficient, 1/4 scale set up in glassware with well ground roots. one could probably yeild another 30% that way, i would imagine this would collect more unwanted alkaloids though.

hypnos

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Re: Help is this safrole?
« Reply #9 on: May 27, 2011, 01:29:40 AM »
 "Cinnamomum Camphora"   aka Camphor Laurels bro--there fuckin EVERYWHERE ...its "classified" as a Noxious Weed downunder
 I'll pm you soon shakey matey...been a bit busy last 48 hrs...
"the two things you can give away and never lose, are what you know, and how you feel...."

jon

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Re: Help is this safrole?
« Reply #10 on: May 27, 2011, 02:31:00 AM »
with these kind of trees the rule is in tropical climes the oil is above ground in the tree that's why jungle safrole bearing trees are commercially harvested.
this is due to the fact that in jungles the pests are found above ground.
in temperate climes the oils are in the root and only in sandy soils not in clay soils.
the roots are best harvested during the spring or the fall during full photosynthesis is optimal.
the reason you don't see so much american sassafras oil is because it is so labor intensive to harvest.
where in the jungles of brazil/cambodia etc you just chop down the tree and feed it to the wood chipper.
then distill it.

see the documentary 'forest of ecstacy'
on www.current.com

those camphor bearing safrole trees are easy to refine the safrole the camphor can be simply crystallized out.

the funny thing about it is when the journalist smelled the oil at the government office he remarked 'he was ready to go to a rave!'
it was funny because you can tell that obviously adam yamaguchi takes ecstasy.
« Last Edit: May 27, 2011, 02:32:52 AM by jon »

doow4681

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Re: Help is this safrole?
« Reply #11 on: May 27, 2011, 07:07:31 PM »
the type of tree was  Sassafras albidum. they grow everywere in the northeast and once you have a good idea youll be astonished when you start noticing all the places they grow in the north east that is.

beanhead

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Re: Help is this safrole?
« Reply #12 on: June 04, 2011, 02:14:21 PM »
I'm not sure how well that will get it all out... With steam distillation the water vapor passes through the bark leeching out the oil and distilling it over as an azeotrope.

Anyone have any knowledge about said azeotrope?

whp141

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Re: Help is this safrole?
« Reply #13 on: July 11, 2011, 11:38:15 AM »
Quote from: fractal on May 18, 2011, 07:45:58 PM
Trust me you need a vac.
Trust him :)

Sedit

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Re: Help is this safrole?
« Reply #14 on: July 11, 2011, 05:50:55 PM »
Quote from: beanhead on June 04, 2011, 02:14:21 PM
I'm not sure how well that will get it all out... With steam distillation the water vapor passes through the bark leeching out the oil and distilling it over as an azeotrope.

Anyone have any knowledge about said azeotrope?

I don't believe its an azeotrope beanhead, look into steam distillation more its a function of vapor pressure and a form of codistillation but I don't believe its a true azeotrope. I could be wrong however.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

NeilPatrickHarris

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Re: Help is this safrole?
« Reply #15 on: July 22, 2011, 01:40:51 PM »
Quote from: Sedit on July 11, 2011, 05:50:55 PM
Quote from: beanhead on June 04, 2011, 02:14:21 PM
I'm not sure how well that will get it all out... With steam distillation the water vapor passes through the bark leeching out the oil and distilling it over as an azeotrope.

Anyone have any knowledge about said azeotrope?

I don't believe its an azeotrope beanhead, look into steam distillation more its a function of vapor pressure and a form of codistillation but I don't believe its a true azeotrope. I could be wrong however.

everything i've ever read supports what sedit is saying.

from personal experience i can say that steam distillation is hands down the way to go rather than solvent extraction.  just be sure to get a big enough still and one more thing that is VERY important is to make that still 100% leak-free.  if you have any water or steam that is leaking out of the still rather than being sent as a vapor to the condenser, then you have a big problem.  even small leaks have hurt yields considerably for me.

salat

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Re: Help is this safrole?
« Reply #16 on: July 22, 2011, 02:04:07 PM »
We just returned from a trip up in the appalachian mountains and sassafras is everywhere.  The way the leaves hang is very distinctive and I learned to spot em going 70 mph on the highway.

While we were visiting my mom-in-law I went out and dug some (more to keep from killing her than any great need).  I didn't have a way to freeze it so I got a gallon container and put IPA in it and stuffed the fresh roots and bark into it.  I'm in the process of distilling the IPA to see if I collected any oil that way - it has a strong rootbeer odor and color.

 Meanwhile the bark went into the freezer.  I'm planning on cooking it up in our pressure cooker with a needle valve feeding to a condenser.  Will let you know how much oil I get, I only got about a 2 gallon bag and it's the wrong time of year to collect it.  I mostly collect the young shoots - I read old timers did that.  I found some of the young shoots are connected to the bigger trees so I can dig up a couple of feet of root at a time - t-shaped.  And there was a tree recently cut down that had some exposed root that I cut the bark off of.  After soaking in the IPA it cut like tender meat.

Salat

Salat

hypnos

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Re: Help is this safrole?
« Reply #17 on: September 28, 2011, 02:24:48 PM »
as you say
   "those camphor bearing safrole trees are easy to refine the safrole the camphor can be simply crystallized out."
    Steam distillation works a treat, but jon, virtually NOTHING grows under most Camphors, due to the trees oils leeching into the soil.
 If you go underneath one and just grab a handful of soil, to see what I mean, It Stinks of Camphor oil. SO much, you could probably get some oil from the soil alone!!..

  And its extremely hardy, invasive and destructive, to the native flora, and fauna which eat the seeds/berries, and sometimes die as a result. hence why they are Classified as, a Noxious Weed!
  I lived amongst forests ot them for years, and as salat mentioned, oil content varies with the seasons undoubtedly.

 I too agree with NPH and Sedit, FWIW

 IF you're downunder, its EVERYWHERE (almost, except down in the southern 4 states)

 I personally enjoy essential oil extractions, as I have had a long standing interest in Fragrances--compounding "special mixes" to give as presents to friends....only several years ago, did I become aware of the value of this 'unscientifically learned' knowledge, I had
 which, as I read, is nothing New..all I can say is "steam distillation" is Not difficult. IMO

 The pressure cooker idea can work well, but the temperatures generated in it, can affect your product, so sometimes much lower pressures and temperatures, sometimes yeild better results IMO

 Cheers Hypnos
"the two things you can give away and never lose, are what you know, and how you feel...."

reDEEMed

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Re: Help is this safrole?
« Reply #18 on: September 28, 2011, 02:56:30 PM »
Salat, you never said what you yielded. I really wanna hear that, if you don't mind.
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