Freezing sassafras--review

[ephemeral]

After carefully reveiewing what seemed to be all posts on this subject, it was found that, as stated in Labtop and Organikum posts among others, that using pure  (in this case double frac distilled) seed crystals added to a 10 C chilled impure batch of sass, that in minutes there was a near perfect crop of almost pure saf.  Melting and repeating 2x's yielded perfect starting material.

 The question is:  Sources show saf  freezing point (MP) at 11.2 C,  while Eugenol comes in slightly higher at 15.22  (MP).  If, as in this case, the temp is 10 C to get as close as poss to pure saf, will it not also contain the full content of Eug? 
  What affects will this have on conversion to isosaf and then use in the Buffered Performic, then Really Wet reduction?

 Am I missing something here?  Comments and constructive criticism greatly appreciated.

[Rhodium]

There is little or no Eugenol in Sassafras oil.

[Bond_DoubleBond]

eugenol does not interfere with crystallization, according to some...

Post 295212

(LaBTop: "Foxy2,", Methods Discourse)

[pooky]

This works,but what the F%$# is the problem with distilling?One can distill a kilo of the stuff in a couple hours but it will take you  days to freeze and thaw and F%$# around etc..stinking up your fridge and house,and making your food taste foul.
Sorry for grouching but it drives P crazy reading of Bees taking "shortcuts" that are really more work,take longer, and give inferior products with lower yields.Look,the post for freezing calls for distilled seed crystals anyways,so why not just leave the MF-ing machinery running for a bit longer,dammit??Just get on with it.

[Bond_DoubleBond]

distilled seed crystals are not necessary.  deep freezing a couple mls of raw sassy in a vial works fine.

freeze purifying if done correctly is far from being a "shortcut."  slow freezing and decanting the crap results in a product with a density of nearly 1.1 g/ml.  swim has never tested the density of his fractionally distilled safrole, but labtop reports it is no where close to that obtained by slow freezing.

Post 294290

(LaBTop: "Additional:", Methods Discourse)

but it will take you  days to freeze and thaw and F%$# around etc...

slowly freezing a liter of sassy does not take days.  it takes about 8 hours.  then it takes 30 seconds to decant, then 5 minutes to thaw.  thats 16 hours and 11 minutes to have purer safrole than you'll get from distilling.  and you don't need your vacuum and hotplate running for hours on end.  and you barely need to lift a finger.

..stinking up your fridge and house,and making your food taste foul.

stopper your fucking flasks if you don't want shit smelling up your refridgerator.  for fucks sake, that should be a no-brainer.

[pooky]

I've done lots and lots of this, and distilling is the fastest and best way...period.
P has frozen it to get the nice,clear and dry inch long crystals of saf, and the only way is to have them form over a couple days,and do it twice or more.As for the smells,I guess you have never ever had half a drop spill...maybe you don't realize that this amount will smell up a house,much less a 6 cubic foot fridge.That should be a no brainer.

[former_chemist]

SWIMs method of treating sassafras is to boil first to drive off the lighter aromatics then freeze.  The higher BP, aromatics (fragrance sense rather than chemical) such as safrole, don't smell stuff up as bad without the high vapor pressure stuff.  Freezing is not as fast as distilling but it is the prefered way of producing a large number of ultra pure chemicals.  Silicon and benzene are two of them.

[Bond_DoubleBond]

out of curiosity pooky, what is the density of your distilled safrole?

i bet mines purer.

and one liter will freeze in 8 hours at 10c if it's sitting in a flask that affords a large oil/glass contact area (>=2L).

several very well respected bees who have processed many times more safrole than you or swim disagree with you.

swim can freeze 5 liters of safrole faster than you can distill it.  and it's purer.  period.

[baalchemist]

Baal gave up distilling safrole many years ago, distillation has its place further on in processing. Fractional crystallization works equally as well on safrole, S.D. measurements have proven this to be fact. As everything in the chem world, one's technique is the key to success or failure. If your worried about stinking up your fridge, here's a simple solution; use a beer cooler filled with ice.

[ephemeral]

Wow-  a  goldmine of replies, thank you all.  Rhodium, thanks for correcting my misbelief  re: eugenol. For anyone interested, I have followed this up and the requirement of distilled seed crystals is unnecessary.   It seems I had an extremely poor starting oil, which, when replaced with a nice high grade  from the far east solved  the problem.
   At 0-10 C,  500 mls in a 1 Litre flask  yeiled perfect crystals overnight with no seeding.  These were extremely large, ideally shaped, and perfectly clear.  Decanting once,  partially thawing , and refreezing gave excellent purity.
  It seems, after 3 different oil sources  ( I didnt mention the first), that oil quality is a major factor.  The brazillian version and most particulaly the North American version  (of course these are sources swim  used and there may be others,  but  it should be noted that they were carefully researched from  numerous suppliers) were very impure and very difficult to freeze without seed crystals  (the NA version would not freeze at all w/o seeds).  The latest source responded as noted and had a very high yield  (95% +).
       There has been no problem with odors, any spillage is easily and quickly cleaned with windex (the ammonia works wonders) to eliminate all traces. A simple celophane wrap over the lasks works perfectly in the fridge.  Chose to obtain a small second  fridge for this purpose now, because the technique is so very effective, though there was never any odor (or other) contamination in the main fridge.
 The idea of preboiling to remove more volatile aromatics is appealing and will be tried.
 Thanks again to all.

[former_chemist]

SWIM tells me that boiling to remove lighter stuff seems to help in freezing.  Some stuff appearently has a good bit of some type of alcohol that prevents freezing (prolly ethanol from the smell).

[Bond_DoubleBond]

in this last batch of sas that swim processed, he couldn't get 5ml to freeze in a sealed dram bottle in his freezer, as he had done several times before.  and swim's freezer can get pretty goddam cold when turned up.  finally swim had to admit defeat and get some dry ice to do the job.  all of it froze beautifully once swim had crystals, and the oil was 70% good stuff. 

what's interesting is that this particular raw oil looked clearer than swim had recieved previously , and the smell was notably different.  this was a new supplier and most past stuff was transluscent, not transparent.  there was nothing about the smell that reminded swim of alcohol, but it was certainly distinguishable from others.

it would definitely explain the bitch of a time swim had freezing the stuff.

boiling off low volotiles prior to freezing is a great idea if you don't have access to dry ice.  but after having to do it last time, swim is gonna continue to.  all you need is a chunk of dry ice half the size of your fist and some acetone in a tiny soup pot and you have crystals in minutes.  sure deep freezing works, but swim is impatient and dry ice is cheap.

[XrLeap]

to vacuum distill 20L of safrole(in a day) is pain in the ass. using freezing can free up your time to do more important stuff like distilling ketone? unless swix wants to watch his crystal grow:)