Author Topic: The Freeze Method....  (Read 334 times)

Terror

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The Freeze Method....
« on: June 10, 2011, 08:16:28 AM »
SWIM knows of someone who has a small amount of sassafras EO, SWIM suggested it be put in a freezer to see if there were any goods but swim is wondering how long someone should wait to see if any crystallization occurs? Days? Weeks?
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NeilPatrickHarris

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Re: The Freeze Method....
« Reply #1 on: June 10, 2011, 12:17:23 PM »
depends on the purity of the EO itself and what the percentage of safrole content is at the moment.  could be days or weeks.  even if it's "weeks" it would be more like a little over a week at most IMHO.

Sedit

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Re: The Freeze Method....
« Reply #2 on: June 10, 2011, 01:03:09 PM »
I think its a pain, you should place a small vial in there as well as you will find this freezes first and scrape that into the larger one as a seed crystal.

No matter how you look at it I think its a pain when distillation goes in a few hours but I have only work with fresh home grown oils. Maybe some where luckier and using commercial oils the degradation of the oil over time made this a simpler process.
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Terror

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Re: The Freeze Method....
« Reply #3 on: June 13, 2011, 12:18:36 PM »
Okay..swims friend said it took 3days for under 50mls to freeze in a wine glass. The only strange observations swims friend made was that the total volume froze - ie implying the concentration is very high?
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Shake

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Re: The Freeze Method....
« Reply #4 on: June 13, 2011, 09:23:08 PM »
Can we not SWIM? god nothing stands out as much as SWIM in big capital letters.

the total volume will always freeze if it freezes, it is what temp it begins melting at that indicates purity. And as for that oil, i believe you are aware of the plant it was sourced from, one should be able to tell alot about purity from that alone. Then 2x 5% NaOH wash then water wash, then 20%GAA wash 2x then water wash again.. then either distill or use it straight. (assuming it is american 90+ stuff)
« Last Edit: June 13, 2011, 09:25:09 PM by Shake »

lugh

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Re: The Freeze Method....
« Reply #5 on: June 14, 2011, 02:03:29 AM »
Fish have been swimming for a very long time, but newbees don't on this web site  ::)  As far as your query, perhaps this article that was hosted on Rhodium will answer your question  :-X  You could have found this information by using any number of search engines, that's for sure  8)
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Terror

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Re: The Freeze Method....
« Reply #6 on: June 15, 2011, 03:12:22 AM »
Can we not SWIM? god nothing stands out as much as SWIM in big capital letters.

the total volume will always freeze if it freezes, it is what temp it begins melting at that indicates purity. And as for that oil, i believe you are aware of the plant it was sourced from, one should be able to tell alot about purity from that alone. Then 2x 5% NaOH wash then water wash, then 20%GAA wash 2x then water wash again.. then either distill or use it straight. (assuming it is american 90+ stuff)


Thanks Shake, I was looking at the congeling point references on Rhod's that makes sence, as the fluid reaches a lower temperature and freezes it will also freeze the other products produced. I read about the application of naOH for removing Eugenol content in TS2


Fish have been swimming for a very long time, but newbees don't on this web site  ::)  As far as your query, perhaps this article that was hosted on Rhodium will answer your question  :-X  You could have found this information by using any number of search engines, that's for sure  8)

Hi Lugh, im not sure what that is implying but thanks for answering anyway. I did look at the article on Rhods but my interpretation was a little off as there is a lot of reference to "Freezing Sassafras" online and in a number of underground books. Also, I had a look at the attached and my German? or Africaans? is not very good.. but thanks anyway.
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Shake

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Re: The Freeze Method....
« Reply #7 on: June 15, 2011, 03:21:17 AM »
if it freezes your on the right track. As i said above, 5% NaOH wash will remove eugenol, it will wash out red heavy separations and if there is alot (usually chinee oil) then the washes will switch layers and the washes become heaver than the oil.

As for the GAA washes they tend to clean dirty oil up to a nice yellow. dont forget to rinse out the NaOH and OR GAA with  final water washes before you distill or you get plastic. I personally wouldnt bother distilling as your oil will be ok. but if you are fresh then you need all the practice you can get i guess.
« Last Edit: June 15, 2011, 03:23:19 AM by Shake »

oldguy

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Re: The Freeze Method....
« Reply #8 on: June 17, 2011, 12:35:47 AM »
Long ago I heard reports of a sassafras oil containing about 75% safrole in a freezer, it took two weeks to freeze, then froze solid.  Saving a few seed crystals, melting and recrystallizing gave a satisfactory initial separation.  After that, seed crystals weren't needed, repeated melting and freezing resulted in excellent separation.

akcom

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Re: The Freeze Method....
« Reply #9 on: June 17, 2011, 02:20:47 AM »
Just an FYI, if you're going the isosafrole route, don't even bother distilling your safrole.  Just isomerize with KOH and distill iso straight from the reaction mixture

Methyl Man

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Re: The Freeze Method....
« Reply #10 on: June 17, 2011, 02:48:14 AM »
I'm not sure what to think about these freezing comments. The cat next door has some water-white saf distilled out of e/o he already knows is high-90s %, and the saf has been in the freezer for months and has not crystallized in any way. He has no doubt that it's the goods, but it's not freezing solid by any means. Could this be simply because it's not totally pure? Like maybe it's got 2% or 3% of some other fraction that doesn't let the saf crystallize? If so, why would the saf in oldguy's story freeze in two weeks, and this not at all?
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Enkidu

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Re: The Freeze Method....
« Reply #11 on: June 17, 2011, 02:54:24 AM »
^ he might need a seed crystal. Try scratching the sides of the jar.

fractal

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Re: The Freeze Method....
« Reply #12 on: June 17, 2011, 03:04:49 AM »
If you ran it from a column you shouldn't have ANYTHING to worry about. Could also check the BP to make sure which is much easier and more accurate then freezing point usually with whats on hand, same concept.

Methyl Man

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Re: The Freeze Method....
« Reply #13 on: June 17, 2011, 03:20:45 AM »
Well it wasn't done with a fractionating column nor was it any kind of fractional distillation; it was a fast, rather rough vac distillation with the water-white fraction rushing away from the orangy oil rather spasmodically...

He's not worried though, he knows it's the stuff... I was just wondering why it isn't exhibiting the freezing behavior.
« Last Edit: June 17, 2011, 03:23:15 AM by Methyl Man »
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akcom

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Re: The Freeze Method....
« Reply #14 on: June 17, 2011, 03:45:55 AM »
Thats curious.  I never distill with a column and my sass always freezes right away.  I'd be really concerned if it didn't crystallize TBH.  Even if the impurity is a couple percent it shouldn't prevent it from crystallizing in the freezer

Shake

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Re: The Freeze Method....
« Reply #15 on: June 17, 2011, 06:45:00 AM »

Quote
Just isomerize with KOH and distill iso straight from the reaction mixture

lol get ready for some plastic! Without an awesome pump and some nice technique, this will polymerise!

Terror

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Re: The Freeze Method....
« Reply #16 on: June 17, 2011, 07:20:38 AM »
Thanks for the comments guys!! Good thread
Confidence and arrogance are easily confused, but only one breeds contempt.

hypnos

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Re: The Freeze Method....
« Reply #17 on: June 17, 2011, 09:31:29 AM »
"lol get ready for some plastic! Without an awesome pump and some nice technique, this will polymerise!"

  I think shakey might have something here
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Methyl Man

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Re: The Freeze Method....
« Reply #18 on: June 17, 2011, 02:45:21 PM »
Thats curious.  I never distill with a column and my sass always freezes right away.  I'd be really concerned if it didn't crystallize TBH.  Even if the impurity is a couple percent it shouldn't prevent it from crystallizing in the freezer

I wonder if it could have something to do with the fact that it's 10-11 years old...? Could it degrade simply with time, but in a way that isn't visible (or smellable)? Hope not, as that's the only supply the cat has...

I'll suggest he try scratching the glass of the bottle a bit to see if this helps.

You know what though, I just recalled something else... when I was using the exact same material 10 years ago, it did the same thing... that is, it remained just a water-white semi-viscous fluid in the freezer.
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flush_it

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Re: The Freeze Method....
« Reply #19 on: June 19, 2011, 02:17:40 AM »
well oil which was atleast 6years old has been done by freezing dip some metal scissors in oil put them in freezer with oil for some days then dip scissors in oil and scratch side of glass then watch magic happen.Once frozen turn down fridge to min watch non wanted oil defrost..so i been told.... ::)