Sciencemadness Discussion Board - Sassafras albidum bark

Sassafras albidum bark

microswitch - 18-2-2007 at 20:28

Scenario: Two very mature Sassafras albidum specimens are known to me. I've taken a bit of bark off the tree and it smells of the aromatic compound.

I put the bark in a blender w/ some H2O, and a little bit of OTC alcohol (+methanol) and pureed.

The resulting solution smells very powerfully of Safrole. I took most of the solution and put it in some small plastic containers in the fridge to preserve freshness.

I took the remainder (about two or three grams) in 200ml of water and 40ml of alcohol and put it in a FB flask (500ml capacity) and boiled (@105-120 C) with stir bar. After a few hours small oily pools have appeared on the top of the surface of the solution.

Now, I know that the alcohol is fully miscible in the H2O, and the Safrole should be miscible in the alcohol.

My question is this: what am I looking at after this process? Is there a better way of getting the essential oil from the tree bark? I can't steam distill it, but I can fractionally distill a solution.

A related question is this: what kind of pumps for condenser? A search of the board has no OTC advice on the matter, but I know a lot of people have solved this problem and many will come across it.

I would post pictures of the setup (how do you post pics btw?).

Thanks so much to the community who has given me such supportive advice.

roamingnome - 18-2-2007 at 21:14

one of my biggest regrets is taking the time to root up two sass trees that where in my yard back in the Appalachian Mountains
and not having the resolve to grind them all and steam distill them( it had somthing to do with a 32 oz. gift from brasil but anyway)
..... but i ground one pot full into a pressure cooker type aparatus, a pipe coming off went into a copper tube cooled by the sink water....

and all you need is time because alot of water will form that needs to be drained off the bottom of the collector eventually leaving a useful amount of oil.... after playing around i realized how valuable essential oil of any kind really is...

my point is, if your going to kill the tree by bark taking.. you should get the roots as well... but dont let them dry out before you grind them and still them.... ( but your use of solvents like alcohol might be a good adaptation as well)

totally off topic but microwaves dude!!!
researchers have extracted capsicums with acetone and microwaves in like high yield

[Edited on 19-2-2007 by roamingnome]

[Edited on 19-2-2007 by roamingnome]

microswitch - 18-2-2007 at 21:29

Thanks for this useful reply. I do not want to take down any trees, however my friend will take down some sapplings as they are growing too close to a garage. If I get desperate for oil, then the trees are an option. I'd like to have a route to extraction and purification before that happens however.

The bark removed was superficial. It seems as though I may need to set up a still if Im going to continue working in the medium.

roamingnome - 18-2-2007 at 21:45

http://asae.frymulti.com/abstract.asp?aid=9709&t=2

Microwave – Assisted Extraction of Capsaicinoids from Capsicum Species

Published by the American Society of Agricultural and Biological Engineers, St. Joseph, Michigan www.asabe.org
Citation: Paper number 026003, 2002 ASAE Annual Meeting . @2002
Authors: Opal J. Williams, G.S.Vijaya Raghavan, Valérie Orsat, Jianming Dai
Keywords: Capsaicin, red hot peppers, extraction, microwave, solvent

The applicability of microwave irradiation to assist the extraction of capsaicinoids from capsicum fruit was investigated. The procedure involved irradiation of 2g samples in a closed – vessel followed by gas chromatography of capsaicinoid derivatives. The optimum conditions for extraction were determined to be acetone at 30% power for 7 minutes irrespective of ground or whole tissue.

The yield of the compounds extracted was significantly greater (P<0.05) using microwave – assisted extraction (MAE) compared to traditional reflux and shaken flask methods. A single extraction step was efficient in recovering approximately 95% of the total capsaicinoid fraction in 15 minutes compared with 2 hours for the reflux and 24 hours for the shaken flask methods. Due to the considerable savings in time and energy as well as reliability, this technique is suitable for fast extraction of capsaicinoids from large samples.

maybye useful... for somthing at least....

jon - 20-2-2007 at 16:57

read a book by earnest guenther called "the essential oils" He mentions sassfrass albidum and says alcohol isn't very effective I've heard acetone works much better.

PlatinumCal99 - 22-2-2007 at 17:50

I myself am interested in using a steam distillation process to extract essential oils from my favorite root bark.
However, a lot of root bark is necessary for a small amount of oil, so the standard glassware distillation setup will probably not be as efficient as I would like. I was thinking about doing something along the lines of what roamingnome said, using a pressure cooker to hold the water, with a strainer attached inside to hold the bark above the water. But how would you 'attach' a pipe to the lid of the pot? Assuming a copper pipe could you just sweat it onto the lid? Finally, you would also need a condensor type piece coming off of this pipe, which could be easily made.

nightflight - 23-2-2007 at 06:30

Iwouldn´t recommend it, the density/spec. weight of *yourfavouriterootbark* is too close to that ofwater, so you might end up with an emulsion that has to be solved by solvent extraction, or the amount of the oil has to be great enough, that significant tension will keep the non-polars together, even then several layers may form.

But my experience was only very small scale, so maybe adapted to bigger quantaties and apparati it works differently?

conducter - 23-2-2007 at 13:16

what about the dried sassafras root bark sold by some vendors online? ive been told that since safrole is volitale that the root bark from online places wont have any safrole

Sassafras bark from vendors

microswitch - 23-2-2007 at 13:46

Quote:

Originally posted by conducter
what about the dried sassafras root bark sold by some vendors online? ive been told that since safrole is volitale that the root bark from online places wont have any safrole

Yes, I believe there is much truth to that claim. For instance, the bark freshly peeled from the tree smelled very strongly of the aromatic compound in question. However, after a few days the odor was noticably reduced, so much so that one had a difficult time evening getting a hint of the component.

That said, I think that bark which was properly prepared should still yield some aromatic compound, but the fresher the better is probably a good rule of thumb.

chemrox - 23-2-2007 at 14:55

what has evreyone got against soxhlet extraction?

roamingnome - 23-2-2007 at 15:39

$100+ dollars....

for starters...

the facts are it takes alot of plant material....
i wonder who has used any amount of self extracted essential oil ... in any reaction... even microscale?

all i made was a good root beer for peets sake..... but the sassparilla supossly causes cancer now.. boo who who...

not_important - 23-2-2007 at 20:30

Quote:

Originally posted by PlatinumCal99
... I was thinking about doing something along the lines of what roamingnome said, using a pressure cooker to hold the water, with a strainer attached inside to hold the bark above the water. But how would you 'attach' a pipe to the lid of the pot? Assuming a copper pipe could you just sweat it onto the lid? Finally, you would also need a condensor type piece coming off of this pipe, which could be easily made.

Depends on what the lid is made of. But I suspect you could do OK by drilling a hole and putting a fitting through it, using a gasket to prevent leakage.

For common hardware store parts - a brushing

http://www.buyfittingsonline.com/Fittings/cat364_1.htm

with the hex head on the inside of the lid, between it and the lid a washer and gasket, and a nut on the top of the lid to fasten the whole thing together. You can screw the condenser pipe into the brushing, teflon tape between the threads.

There are better ways to go than that, but these parts are easy to find and cheap.

roamingnome - 24-2-2007 at 09:48

this is exactly what i did
actaully it was a brass compression fitting to a smaller size coppper tube...

the pressure cooker had a few leaks that you will discover quickly...
smells good at least...

and if you dont get alot of oil just add alot of sugar, chill it down and drink it as tea...

[Edited on 24-2-2007 by roamingnome]

PlatinumCal99 - 24-2-2007 at 20:25

I don't know how much oil you were able to collect gnome, but it sounds like it wasn't a lot

. I remember reading somewhere that the dried root bark is about 10 percent oil by weight. Some places sell it for around $13 - $27 per pound, from what I've seen. Of course you're never going to come near hitting that 10 percent mark, but with a lot of distilling....

Anyways, how much oil were you able to collect, relative to the weight of the bark?

chemrox - 24-2-2007 at 22:49

soxhlets can be scaled up to handle a kilo and extract at the vapor temperature .. however...

a steam still can be made from pressure cookers. I use one to generate steam and a big one to use as the extractor:

steam in the bottom ... out the top to a copper coil

planned improvements include jacketing the copper coil with a stock pot. fortunately I have a fluid connector specialist down the street... they've been very helpful.. basically I just need a way through the bottom of the stock pot .. there are fittings made for this.

It seems like a system such as this would be better than a retort with water in it.

If I had the money I'd go supercritical using butane or LPG as the fluid. I think it would be ideal for your bark ..

Nicodem - 25-2-2007 at 03:40

Why does anyone want to reinvent the wheel?
Just about any farmer can buy his brandy distillation still. There are models for distillation from a couple of liters to a couple of tens of litters available and they are all suited for steam distillation as well.

PS: What has this to do with organic chemistry? Are there no essential oil and perfume distillery forums on the net?

roamingnome - 25-2-2007 at 16:58

Quote:

but it sounds like it wasn't a lot

no i got extract, but i set up the the process under the guise of root beer making while at home.... but the regret was never processing the 20lbs i originally dug up....
im a tree killer so sue me...

Yes! there are some really nice perfume making forums on the net. and in another thread we talk about our favorite knitting stitches

microswitch - 26-2-2007 at 21:05

Quote:

Originally posted by roamingnome

totally off topic but microwaves dude!!!
researchers have extracted capsicums with acetone and microwaves in like high yield

[Edited on 19-2-2007 by roamingnome]

[Edited on 19-2-2007 by roamingnome]

Acetone is a flammable substance. Is it such a good idea to put a flammable liquid in a microwave? How exactly is the acetone plus microwave going to snatch that safrole and leave the rest?

Capsaicin ((E)-N- (4-hydroxy-
3-methoxybenzyl) -
8-methylnon-6-enamide) has a long nonpolar tail.

Just some observations.

jon - 1-3-2007 at 17:09

I think the answer to your question is a makeshift condensor there was one proposed in green chemistry that used an inverted funnel with a round bottom on top of it filled with dry ice, solid CO2 does'nt absorb microwave radiation very well, so it's useful for this pupose.

an interesting tidbit can also be found here

http://www.erowid.org/archive/rhodium/pdf/microwave.chemistr...

they state that polar or slightly polar solvents become less so as temperature increases on page 9230 that may explan the selectivity of acetone in this process.

[Edited on 2-3-2007 by jon]

PlatinumCal99 - 28-3-2007 at 15:08

Well I finally found the time to experiment with my makeshift steam distillation setup. Very little oil was collected, and I'm thinking this may be because the temperature of the apparatus got so high.
So I decided to buy a bigger 3L flask and tried doing it with a glass setup, and I collected a lot more oil this time around. A much gentler distillation, to say the least.
Just letting everyone know for their own benefit..

majic22 - 8-4-2008 at 21:45

Use a 55 gallon drum. Its perfect for large scale steam distillation and you can get one for free from a business in town that just throws them away. Use a screen on the inside to hold the organic material suspended. Weld a fawcet on the bottom end to hook up a water hose and keep the water level constant. Weld a fitting to the top and connect a copper tube to it for the condensor. Sit it up on bricks and use a grill burner and propane tank for heat. Simple cheap setup.

Do you live in the Southeast??? Juniper Virginiana AND Cinnamomum Camphora

majic22 - 8-4-2008 at 21:51

Does anyone here have any extraction or distillation experience with either of these two trees? If so, please divulge your results. What happened? Good or bad, suggestions, opinions, and all that kinda stuff. Thanks!!

v16 - 9-4-2008 at 11:42

Setting up a still and trying to process that much raw material is a very big job. In other countries these oils tend to be produced seasonly, and in most cases the material is now transported to a large processing facility. You are going through a lot of work for you your quest. Now if you are doing it for the experience, and learning how to steam distill, have at it. For sure something that would be good to know. But...if your motivations are more base, there are much easier ways.

Investigate White Camphor Oil. While most sources claim it is S. free, most isn't.

An interesting UN report.

Published Dec 2007

"Systematic Study of Color Test for Safrole and Safrole-Rich Oils"

http://www.unodc.org/documents/scientific/SCITEC21_07fin.pdf

Looks like they are actively trying to determine which common E. oils are hot. Names of products are not given, but some, UNX 1902a for example, are not hard to guess. I think 1902a is White Camphor. Scientifically, it is not a bad study, and regardless of your motivation, it could be valuable. Even if you use it to help determine the content of any oils you happen to produce.

V16

homeslice - 2-6-2012 at 05:19

Sorry to dig up such an old thread.

Can someone confirm or deny that the actual bark of the albidum tree contains safrole? All ive been seeing is that its the rootbark or the actual root itself in small amount but not necessarily the bark itself.