(Newbee)
07-24-02 03:19
No 336310
(Rated as: excellent)
Finally can report success in producing Sassafras Oil from sassafras root bark via Steam Distillation. Now I can hear folks saying "Why bother - just order it!". Well, it was done for four reasons:
1) I have yet to find a good source to purchase.
2) I hate to see all that rootbark going to waste on the trees that are being cut down round here.
3) I will always have a source no matter the restrictions on sassy oil.
4) I need to get my Karma rating up.
Root bark was stripped from sassy roots and dried to approx. 5-10% moisture. Reason for drying was two-fold: so mold doesn't grow as bark quantity being accumulated and can pack more weight of dried bark into steam distillation unit.
Dried and crumbled bark was loaded into pyrex distillation chamber, approx. 200 grams at a time. This chamber has bottom steam feed. Distilling head/thermometer adapter on top of that, and condenser and receiving flask off to side.
Now I was wondering whether steam, at 100 degrees C. would extract the sassy oil/safrole since it's boiling point is like 232 C. A quick check of the literature proved comforting: "The partial pressure of each component of a mixture of immiscible, volatile substances at a given temperature is equal to the vapor pressure of the pure compound at the same temperature and does not depend on the mole fraction of the compound in the mixture; This indicates that the total vapor pressure of the mixture at any temperature is always greater than the vapor pressure of even the most volatile compound at that temperature (in this case the H2O); Thus the boiling temperature of a mixture of immiscible compounds must then be LOWER than that of lowest-boiling component (H2O)". Ah-ha! I've left out the math, but my calculations showed that the mixture of sassy oil and steam should be boiling at about 95 degrees or so.
Sure enough, once the setup reached equilibrium, temp showed a constant 96 C. and oil and water dripped from the condenser nicely. The sassy oil was a nice water white and formed a layer at the Bottom of the H2O, with very little if any other oils on top of the water. Total yield seems to be about 8-9% by weight, which matches nicely with tests done on the rootbark to determine oil %. So there you have it!
From roots to oil. The one thing that strikes me is that the oil produced this way is pure water white, rather than the reddish-gold as commonly seen in the commercial stuff. I suspect this has something to do both with the source of imported oil (tree wood rather than root bark) and the extraction techniques used overseas.
Next need to establish % of safrole in the oil. Any thoughts on this?
If they drive God from the earth, we shall shelter Him underground - Dostoevsky
(Hive Addict)
07-24-02 04:51
No 336341
Can I get a "hell yeah!"???
Good job beavis!!!
Fuck yeah!!
good for you!!!!
weigh said oil
distil
weigh what comes over at appropriate temp (should bee around 70C for your kick assed pump...
divide distilled fraction/origional weight
theres your percentage
better yet, after ya distil, get a miniture vial and start a seed crystal- put said crystal into your refrigerated (not in the freezer) distillate and then throw it in the freezer. After everything crystalizes, decant the crap off the top of your distilate. Do it again if ya want to bee anal. Weigh that.
i FEEL funny.
(Hive Bee)
07-24-02 06:18
No 336366
VERY nice bubble!! Interesting work regarding steam distillation of rootbark. The reason i believe you got a clear dense oil is because you did a slow distillation of rootbark oil and thus produced a much purer oil.
The big companies that make sassy oil probably do rapid steam distillation which gets more tars/terpines and junk so its less impure.
It wouldnt suprise me if your oil is +95% Safrole. Distill that oil and give us the yields.
AWESOME!
hcildoduedn
(Hive Addict)
07-24-02 07:16
No 336378
quick question...
how time consuming was this? -not procuring the bark, but the actual distillation.
i FEEL funny.
(Hive Addict)
07-24-02 08:13
No 336408
The thing that takes so much time is shutting off boiler letting the system cool a bit then replacing spent bark. Then reheating. And waiting another 2.5hrs for around 100ml or more. From 2.5kg you can expect 150g oil being 90g safrolesomething from the ones in my friends neck of the woods. Need I remind 2.5kg of dried bark is a fuck load of digging!?
Very simple and cheap setup but takes forever... Imagine taking a pressure cooker and attaching a pressure relief valve on the steam port of say 30-50-psi or better if your pressure cooker can safely ahndle more. And attach copper tubing from there to an inverted lid of another one. Supported from below with a couple bars running form two lab stands across form each other. Now take 2.5kg of bark (don't pack it too full it wil need a lil expansion room) and tie it up in chese cloth or steel screen or some other avail cloth (or a close fit collander with a silicone bead around the lip to make a tight fit). Then palce net in lid and atach top (act.bottom of pot) The top naturally bottom of pot needs to ahve a hole drilled in it with a flanged copper fitting through the inside and soldered to a piece of copper tubing on the outside then coiled under a sink faucet of into an ice bucket then into a small carboy with an overflow and a bottom drain.
Here are some pics of a small 2L lab scale steam still.
http://www.heartmagic.com/EssentialStill
http://www.heartmagic.com/NewReceiverHOW
(Newbee)
07-24-02 14:54
No 336533
Time isn't too bad - usually let it run for 3 hours or so. Plus, once still is set up and fired up, there's no need to sit and watch it. Just collect oil at end of 3 hours.
I try to keep it so that there's only a drop or so coming over every 2 -10 seconds. Nice and SLOW. BTW, it's fun to see the Oil form a big "glob" on the bottom of the water. Sorta looks like a Jelly Fish sitting there!
FYI, my Distillation setup is all Glass. It's also different from usual Steam Distill setup in that I feed the steam from a glass flask directly into the bottom of the distillation chamber. This way steam has to flow up and through the root bark before going out the condenser. Only water soluable crap drips back down, and only Oil goes up and out.
I don't dig roots - I let the people with the bulldozers do that. After a piece of land is cleared for development, one can go in and see the the up-rooted Sassy trees laying in a pile. Hack the bark off. Also, some of the most potent roots are left just below the surface of the ground. These are about 1-2" in diameter. Grab one end, carefully pull, and you may get 3 or 4 feet of root.
I'd like to eventually make a bigger still, but for now I'm getting 10 - 20 gms. at a time, so thats OK.
If they drive God from the earth, we shall shelter Him underground - Dostoevsky
(Hive Addict)
07-24-02 19:53
No 336598
Well in that case good for you! Lucky bastard. But I still consider waiting 2.5 hours whether you're there watching it or of doing somthing else to be a bit too long and a lot of electricity for so little oil. But that's just me.
(Title on BackOrder)
07-25-02 00:27
No 336702
That's pretty small scale right there. It's a lot easier to do in bulk.
One thing about distilling from root bark is that it needs to be done when the rootbark is still fresh out of the ground. Sassafras oil can evaporate into the atmosphere from the bark over time; this is what makes an essential oil different from, say, a cooking oil. The oil content of a dead tree is significantly lower than that of a healthy living one.
All paths are the same: they lead nowhere