Safrole Isolation thru Freezing?

ApprenticeCook · DILLIGAF

It works well for safrole in sassy due to its high % safrole content and the melting point of safrole being able to be reached in a home freezer.
As for it working for other compounds it would depend on their relative melting points compared to the other constituents in the oil and the % of those components.

-AC

iodide · Mon Jun 20, 2005 9:53 pm

Update:

1. SWIM put 250ml of Sassafras oil into a freezer set to the highest setting. Within a few hours, tiny crystal, looking like the shape of a few millimeters of pencil lead were present throughout the oil like a colloidal-suspension. Swirling did nothing.

2. SWIM took this out of the freezer and put into fridge set to highest setting. SWIM put 3ml in a tiny glass dish and placed in freezer.

3. In an hour, 3ml hadn't fully frozen but a large white slushy/slurry existed with a little oil left unfrozen. The slurry quickly started melting, but SWIM was able to dump it into the 250ml botting that had been sitting in the fridge. Upon dumping into the oil, the slurry sat suspended in the middle of the oil looking like a peice of cotton. SWIM placed bottle in fridge, expecting this "seed" to start the full freezing process.

4. 2 hours later, SWIM looks at bottle and sees the oil as fully clear! White slurry must have melted. Sad

Is SWIM's freezer simply not cold enough? What's going on?

2spun · The Resistor

iodide ,

frez'r or fridge,
freaz'r sound'd cold enuff but not yer fridge.
it's possable i'm misread'n if 2 see i to eye right now,(hint)
wipe'd out Smile

methyl_ethyl · Riedel De Haen

How you will get good product from not distilling is beyond me.

I get the feeling no one is taking the time to read the entire thread that primathon posted.

Click on the blue "here" at the top of primathons post and read the whole damn thread.

I think everyone can learn something from that thread, and not just about freezing sassy.

Thank you for that post Primathon,

regards,

m_e

2spun · The Resistor

methyl_ethyl,
your right bro. what primathon put for every eye to read did deserve a thanks
my f-up i thought it was great!

ApprenticeCook · DILLIGAF

dont use your fridge... its just not cold enough. FREEZER.
Place the small volume of oil in the freezer and let that freeze over, let the rest of the oil chill in the freezer and place the small seed crystals in the rest of the oil in the freezer and this will hopefully initiate the rest to freeze.
Alternativly you can rub the interior glass walls of the container with a thermo or glass rod to start it off, but the oil needs to be freezer cold first.

-AC

Soap · Tue Jun 21, 2005 8:38 am

swim here had great success with the refrigerator, i guess it depends on the purity of your sassafras oil, swims was realitvley pure... the only problem with using the freezer that i see is that the safrole would crystalise to fast possibly traping some impurites in it. do not forget to do the process several times over and over. swim had a failed isomerization after freezing only once... is there any way we can combine this with the otehr thread that i started?

iodide · Tue Jun 21, 2005 8:43 am

methyl_ethyl · Riedel De Haen

i guess it depends on the purity of your sassafras oil

Exactly, that and many other factors far too numerous to mention. There will never be a cut and dry robust procedure that will work for everyone that has procured the oil from Chinese Producers, Brazillian producers, or extracted, steam distilled, or vacuum volatilized sasafrass oil from root bark, or any other means of procuring the oil. Everyone who investigates this method will have to do so emperically.

That was my main point in telling everyone to read the link that primathon posted in it's entirety. You will find that everyone argued that their way was the only way to freeze isolate safrole, and denounced any other ideas or findings. The fact is; what works for your sassy oil may not work for someone elses. This stuff is not in any way consistent from producer to producer, batch to batch, species to species, country to country etc etc., the thought that one method will work better than another is at best nonsensical.

It's not like we are finding variability between manufacturers of molecular biology grade reagents here. It is more akin to finding variability between sequencing grade trypsin, and using an actual porcine pancreas to digest a protein for MS analysis.

Perhaps that is a bad analogy but that's all I gots for now.....

m_e

GOD · Wed Jun 29, 2005 3:39 am

freezing works FANTASTIC!

swiG heard this:

to obtain seed crystal, use one of them small-assed bottles they use for fragrance oils, put a bit of sass in it, and a few drops in the cap.
close, and put in freezer over night. The reason for a drop or two in the cap is to get some oil on the threading.

fridge should be preadjusted so as to be within a few degrees of melting point

next day (or so), without any dillying around- dont want any melting going on- so larger container should be ready to accept seed crystal (open in frigde). Inside the freezer, open small glass jar being careful to keep fingers on BOTTOM of jar

quickly take little glass jar, and invert it into the mother jar in the fridge so that the threading of the little jar dips into the oil. Shake little jar a bit, recap, and put back in freezer in case another go is needed (the walls will be coated). Chances are pretty good that even if there is no crystalization within the little flask, the threading itself will have some crystalization, hence the need for a quick transfer (very thin crystals, melt quick.....).

If it works, it'll look like its snowing in the mother jar- give it a little swirl, and the 'snow' will multiply. Notice how the snow grows as it makes its way to the bottom of the jar. Cap the mother jar, and "set it, and forget it". In swiGs experience, it'd take about three days to fully solidify. Dont remove the impurities too soon, it will get darker, and darker. Wait until its deep, deep piss yellow, like your kidneys and liver are screaming mad at ya after a nice, long alky binge.

Poor the impurities out into a separate container- ther'll still be some good stuff in there.

Allow the oil to melt, and repeat a few more times, each time collecting the dirty fraction for another round once enough is collected.

Growing crystals is good wholesome fun for the whole family!

swiG posted about it in the hive a few years back after reading the above referanced post.
worked very nicely thank you very much!

primathon · modified

I've always thought this would be a really easy way to make seed crystals:

You need a piece of glass, an eyedropper, and your oil. Place the glass in the freezer, and carefully place a few drops on it (get 'em as round as you can). Let it freeze (there's no way that such a small amount can't freeze at such a low temp, given time), then chip off as needed. Quick, easy, convienient, and you can do as many as you want at once. Then you can just take one (or many, if you prefer) of the sass-pellets, and drop it straight into your "mother jar". If it doesn't work, drop another one in. Lather, rinse, repeat.

Also, how about taking a chunk of dry ice and just dropping a single drop on the surface? It would probably be frozen by the time it slid off the side.

Again, just thinking out loud. Your mileage may vary. Use at your own risk. Always consult your physician.

mycoguy · Wed Jul 06, 2005 9:33 am

Here's a link from a discussion at DF
http://www.drugs-forum.com/forum/forum_posts.asp?TID=6413