Author Topic: cant get safrole? FREEZE IT!  (Read 13166 times)

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goiterjoe

  • Guest
you are not among the informed
« Reply #120 on: January 22, 2003, 11:37:00 PM »
The stranger title fits you very well, as you definitely know nothing about what you're talking about.  You make fractional distillation sound like an impossibility and a density check appear to be labor intensive.  You're going to have your work cut out for you then.

So how many bees do you think here are working with 20L of safrole at a time?  A couple of dutch cooks maybe that weren't lucky enough to come across MDP2P?  Most of the bees here wouldn't even dream of ordering that much at one time, let alone trying to work it all up at the same time.

If you're too cheap to buy equipment, then shut the fuck up about it already.  When you're bitching about low yeilds on your aminations because you're not properly distilling your isosafrole or MDP2P, you'll hear this all over again from everyone else here.


placebo

  • Guest
I would just like to state that both my new...
« Reply #121 on: January 23, 2003, 02:06:00 AM »
I would just like to state that both my new 2003 13th ed. Merck hardcover and CD both list safrole as "Density: d 20 1.096".
 


LaBTop

  • Guest
Yes,
« Reply #122 on: January 23, 2003, 05:30:00 AM »
Placebo, and which is only 0.004 off from 1.100 found by Argox last year. He mentioned to use a self prepared density equipment which indicates to me that with that (still rough, compared to what Merck can come up with) homemade thingy, he managed to come very close to the Merck value.

Hey, old grumpy friend, they still glue the beerbottlelabels upsidedown downunder?  :)  LT\


hCiLdOdUeDn

  • Guest
Arsenic stop bitching.
« Reply #123 on: January 23, 2003, 07:00:00 AM »
Arsenic stop bitching. The purity of disilled sassafras, i.e. safrole does not need to be 99.999999999999% It will work for isomerization and after simple vacuum distillation of the isosafrole you are left with isosafrole of atleast 95% purity. Most bees do not care if its 95% or 99.9999999999999% because frankly the yields will still be the same!


placebo

  • Guest
I am good, but I don't know what you mean...
« Reply #124 on: January 23, 2003, 07:45:00 AM »

hCiLdOdUeDn

  • Guest
What does the world upside down have anything...
« Reply #125 on: January 23, 2003, 09:14:00 AM »

baalchemist

  • Guest
Baal uses a Mettler/Paar Digital ...
« Reply #126 on: January 24, 2003, 12:55:00 AM »
Baal uses a Mettler/Paar Digital Densitymeter-DMA35 for density measurements on liquids. It certainly takes alot of the guesswork out of determining purity of most liquids Baal deals with. On my meter I get these readings;

Safrole 1.1
Iso-safrole 1.122
Ketone 1.188-1.191  This reflects a ketone that is not 100%, never seen it @ 1.195 as 100% purity is supposed to be, but close enough to run.
 


dr_ruthenium

  • Guest
RB: Only problem when you distill the pooled...
« Reply #127 on: January 26, 2003, 08:08:00 AM »
RB: Only problem when you distill the pooled contaminants is that you may get foaming (up through column, three-way and condensor down into receiving flask.  SWIDR guesses that contaminants act as surfactants, so if you have 20 liters and freeze down to 15-16 liters, then just toss the riemaining 4-5 lters instead of attempting to distill that last liter out.


yellium

  • Guest
??? I've never seen foaming sassafras oil or...
« Reply #128 on: January 26, 2003, 09:33:00 AM »
???

I've never seen foaming sassafras oil or ditto distillations. I do have seen distillations where the temperature was too high, and where an occasional bump to the table resulted in the distillation flask puking all its contents into the receiving flask. But that's bad technique, not bad chemicals.

Of course, if you have bad technique, you might as well throw away the remaining 'difficult' oil, even if it is 5 l....

NeoSynthesis

  • Guest
Sassafras Safrole Distillation @ 1 ATM
« Reply #129 on: September 05, 2003, 08:08:00 AM »
I've read some conflicting posts about distilling sassy @ 1 ATM. Some read that shit might "polymerize" @ heat that high and that is why the vacuum distillation is recommended. Seeing as so many bees are saying that it's safe to distill sassy @ 1 atm i'm going to try it. I'm wondering if the 232 C is constant regardless of where you live? I'm a Canadian bee... XXXX to be specific. I'm wondering if there's anything I should know (or could check) about 1 ATM in XXXX, Canada that would affect the temp @ which the sassy would come over, at 1 ATM?

Thanks....  8)  NOT cool, it's plain stupid to tell where you live in such an incriminating post! LT/

nitrous351

  • Guest
sea level
« Reply #130 on: September 05, 2003, 08:14:00 AM »
the only thing that would affect your distillation would bee how far above sea level you are. If your town is less than 500meters or so above sea level, I would just proceed as normal. good luck peace


gruns

  • Guest
I think I...
« Reply #131 on: November 21, 2003, 02:15:00 AM »
I think I may have been successful in freezing asarone out of calamus oil.  

First I poured about 10ml of nepalese calamus oil into a shotglass and put it in the freezer on its coldest setting.  A day later, it was still unfrozen, at which point I abandoned the experiment and completely forgot about it.   

A few weeks later I noticed it while getting some biscuits (mmmm, tasty frozen biscuits!) and checked on it.  Interestingly, I saw whitish wartlike crystals awash in a darker yellow mass of crystallized oil.  Cool, I thought, so I put it in my fridge.  Two days later, it was still frozen solid, so I set it on my fridge to melt a bit, hoping to get a seed crystal.  Later that day I came back and there were lots of chunky clear crystals soaking in the now liquid yellow oil (considerably more crystals than oil).  I carve a few chunks out and throw them into a chilled shotglass and put it in the freezer, putting the larger crystal mass on the fridge to melt.  I noticed when I came back later that as they melted they had separated into layers, the bottom clearish one having that peculiar irridescent sheen we all know and love.  Anyhow, I poured this into an emptied soy sauce bottle and added the rest of the amount I had purchased (225ml), then put it into the fridge.  After it was good and cold (8hrs) I threw in a seed crystal and went to work.  When I got home, the bottle was full of white crystals but it had obviously trapped much yellow oil in the many crevices, not to mention the thick skin at the interface of oil.

So, onto the fridge it goes to melt.  When it had melted down to the last few xtals (shaking helps) I put my fridge on "2" (it was on "5" previously) and put it back in there.  It kept forming skins on top and trapping the yellow in crevices, so I crystallized and melted until I had huge crystals (~4 times) then turned the thing upside down over another container and collected about 75ml of nasty, stinky, pee-yellow oil.
Thirty percent (most asarone bearing oils being 60-70% asarone) of 225ml is 67.5ml. 

After washing the crystals with ice-cold etoh, I let them melt into a very mildly yellow irridescent liquid.

Maybe I should have recorded the temperatures...

This begs the question... What in "Bob"'s name am I gonna do with this nasty stinky not-asarone stuff?


Rhodium

  • Guest
isolating asarone
« Reply #132 on: November 21, 2003, 02:51:00 AM »
What you have left is probably an 1:1 mixture of asarone and [unusable crap] so just vacuum distill it with a column to retrieve the other half of the asarone. You will probably not be able to crystallize out all of it in pure form from the impure matrix.

Glasya

  • Guest
Creating a seed crystal
« Reply #133 on: December 01, 2003, 12:15:00 PM »
After SWIM tried for 3 days to create a seed crystal with no luck, tried small test tube, small perfume vial, freezer was at -18 and still no luck, so today SWIM decided to take a small amount <100ml> of oil that was in the freezer and dropped in a small cube of dry ice <1cm cube> and instantly it bubbled and a film of white fine crystals grew around the dry ice. SWIM removed the dry ice cube and the film simply fell off the cube. SWIM took the 1L bottle of oil from the freezer and dropped in the film of crystals and put the bottle back in the freezer. 15 min later the bottle was full of large white crystals. This made creating a seed crystal super easy. Followed all the other suggestion for freezing the contents 3 times Ended up with ~750ml of really white crystals that melted to really clear colour liquid that refracted light nicely.

scram

  • Guest
you got a good yield with 75% v/v if its ...
« Reply #134 on: December 01, 2003, 07:27:00 PM »
you got a good yield  with 75% v/v if its completely clear.

MDMA_AcTIvEsTS

  • Guest
MIGHT i SUGGEST
« Reply #135 on: December 01, 2003, 07:41:00 PM »
MIGHT I SUGGEST:

IMHO i would freeze or, slow freeze in the fridge, it may take time but FUCk around with the fridge as to find the a low enough temp to freeze slowly as the freezer does it to fast and you get other crap in with the safrole.

IMHO get the crystal from freezing in the freezer then, crystalize in the fridge as the lower temp freezes slower and you get BIGGER purer crystals.. then repeat this process and just drain of the yellow piss color and distil. Do this process 2 to 3 times then distil, though some may argue this, purtiy is the main convern not time'. :P

scram

  • Guest
Biger crystals that for 6 to 8 sides are more...
« Reply #136 on: December 02, 2003, 09:44:00 PM »
Biger crystals that for 6 to 8 sides are more pure. Also, make sure your d20 is 1.098 to 1.1 and you'll know if it's really pure.