Author Topic: cant get safrole? FREEZE IT!  (Read 14032 times)

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wyndowlicker

  • Guest
cant get safrole? FREEZE IT!
« on: April 04, 2002, 05:34:00 PM »

still having problems from the begining it went like this.

Simple distillation of 250ml  sassy
got silocone grease
got ice water running threw the condenser
first start stirring on 5
attach vacuum already running
then turn on heat to 1 out of a possible 10
first thing to come over was 64c 30ml of very clear watery oil that doesnt sink when dropped in water.Bath temp 110c.
then temp raised to 74c held there gave 10ml or so.then raised up to 84 holds there 1dp per 13 sec or so.bath temp 145.
when nothing came over for 2 min took off emptied put back on.
then it skyrockets to 114c  then slowly raises to 120c oil temp 167.stays there for a while then nothing.
So now total swiw has maybee 50ml.
took it up slowly till it hit 130 then it gave off a slightly clear yellow oil with what looks like rainbows its like what a puddle looks like when oils in it.It didnt give alot maybee 10ml and it stopped took it up to 140c and nothing so swiw stopped never got the bath temp past 200c to keep from frying the oil till swiw  figures this out.think possibly the oils bad.
Now keep in mind swiw has raised the temp no more than 1/2 click every hour and still nothing. :P

I will choke untill I swallow!Who are you to judge or strike me down!Miss you Kerra!

wyndowlicker

  • Guest
come on someones gotta help out.
« Reply #1 on: April 04, 2002, 06:53:00 PM »

pickler

  • Guest
sassy
« Reply #2 on: April 04, 2002, 06:59:00 PM »
Sounds like u might have some none safrole containing sassy oil. Is it essential oil of sassafras?

We'll soon find out if I'm a chemist or not!

Elementary

  • Guest
vacuum
« Reply #3 on: April 04, 2002, 07:00:00 PM »
Either your vacuum source is not strong enough or you have bad oil.

Leonard Cohen cheers me up !

skapeGoat

  • Guest
ATM
« Reply #4 on: April 04, 2002, 07:39:00 PM »
Try distilling ATM up to Safrole's BP (234*C) it should withstand that temp. Later

wyndowlicker

  • Guest
yes its essential oil Swiw knows what hes looking ...
« Reply #5 on: April 04, 2002, 07:51:00 PM »
yes its essential oil Swiw knows what hes looking for no internal use external use.sasafrass albidum.And swiws pump is supposed to be prime for this yelowjacket 15 microns.

I will choke untill I swallow!Who are you to judge or strike me down!bye bye red bee.

noj

  • Guest
do this
« Reply #6 on: April 04, 2002, 09:10:00 PM »
LOSE THE VACCUUM

I think it's been suggested 5 times, in several thread on this subject. TRY IT. I seriously believe the vaccuum is way to strong for this. Safrole doesn't scorch at its boiling point. There is no need for you to be afraid of it. There is no need for you to post over and over about how you can't get safrole while refusing to try the suggestions the bees here give you.

So if you want to keep trying to get safrole with your yellowjacket pump, and won't try to do a simple distillation to verify that there is any safrole in the sassafras to start with, maybe you should try a new hobby.

I'm sorry for being rude. Maybe it will wake you up.

MDP2P is when you need to be careful about the high heat.

Mastery is based on the understanding and practice of technique.

VinnyC

  • Guest
oil...
« Reply #7 on: April 04, 2002, 09:11:00 PM »
Was this portion of sass oil one that you tried to distill previously? Or was it a fresh/new sample?

Describe the sass oil, its appearance, color, odor.

"Have we descended to the level of dumb beasts?" Fear & Loathing
Be loved and blessed hp and cg!!

RoundBottom

  • Guest
cold
« Reply #8 on: April 04, 2002, 11:36:00 PM »
freeze it and be done with it. 

i learned a thing or two from charlie dontcha know.

raffike

  • Guest
some advice
« Reply #9 on: April 05, 2002, 05:22:00 AM »
I may be so that your sassy doesn't contain any safrol(like said before) because some distributors sell sassafras oil that contains no safrole.Try 232C without vacuum or just freeze it to -14C(safrole melting point) like Strike wrote in his/her book

noj

  • Guest
safrole mp
« Reply #10 on: April 05, 2002, 06:49:00 AM »
11.2°C is the mp of safrole according to Merck and chemfinder.

Mastery is based on the understanding and practice of technique.

soundwave106

  • Guest
You may not see safrole crystals form without ...
« Reply #11 on: April 05, 2002, 11:50:00 AM »
You may not see safrole crystals form without agitation in the freezing method, though, right? Or at least crystal formation will be slow.

(In a dream, I saw a beautiful maiden place some sassafras in a small glass container, and put in a freezer. Tiny white crystals formed on top. The beautiful maiden then blew on the sassafras. More crystals appeared. Afterwards, she shook the container for further agitation. The maiden put the sassafras back in the freezer. Unfortunately, I woke up before the dream finished. Perhaps the dream can finish in the next few weeks.)

utopium

  • Guest
saff
« Reply #12 on: April 05, 2002, 01:00:00 PM »
Buy an aspirator and see if there's a differnce, then try no vacuum at all, as noj and a bunch of other people have already told you, in this thread and others.  If you get the saffrole, then it's your pump.  If not, it's your oil.  Right?

"No...why would I need a fire extinguisher?"

wolfx

  • Guest
Try again with an aspirator, buy a GOOD one ( for ...
« Reply #13 on: April 05, 2002, 02:17:00 PM »
Try again with an aspirator, buy a GOOD one ( for instance, NALGENE, plastic, very good even with low water flow ) and use it also for filtering, evaporating solvents, etc. Save your vacuum pump for serious work, like ketone.

Also, your oil might be dirty again. I have this problem with my vacuum pump, is a good one, single stage rotary vane, but everytime I use the vacuum degrades, I have to replace the oil. How do I know ? I measure the vacuum with my vacuum gauge. I am planning to add a trap, but I can't do it right now, so I just distill fast, start with aspirator to get out a bit of H2O vapor and other stuff that degrades the vacuum when absorbed in the oil.

Repeat, get an aspirator. Also test your oil, use the FSE.

wyndowlicker

  • Guest
ok!
« Reply #14 on: April 07, 2002, 01:13:00 PM »
Alright here is swiws reason for not taking it to atm tep.
the oil smokes out my space and there is not sufficent ventalation.as far as freezing goes the oil swiw has been in the freezer for some time now without freezing swiw will try turning up the freezer and see if this works.doesnt anyone else have problems with there peanut oil smoking?

I will choke untill I swallow!Who are you to judge or strike me down!Miss you Kerra!

pickler

  • Guest
oil smoke
« Reply #15 on: April 07, 2002, 02:40:00 PM »
your oil will smoke if it's old and used. try fresh oil.

We'll soon find out if I'm a chemist or not!

Flip

  • Guest
Sassy distillation
« Reply #16 on: April 07, 2002, 03:20:00 PM »
Smoke and fumes sometimes cannot be avoided.  the smoke from peanut oil, although being slightly irritating to the eyes, it really not all that bad.  A friend of mine has the same pump that you are using, and it is pretty strong.  If you have never done an ATM distillation you might want to try this first.  Make sure that the container your oil bath is in has good contact surface on the plate, and sometimes insulating the oil bath is neccessary.  You should see the safrole vapors come up almost like smoke if you put a black peice of paper behind you apparatus.  The higher the temp, the higher the vapors rise.  Make sure they are flowing into the condenser consistently, this will be visible.  Use a small flask, as often there is a lot of reflux on the walls of large flasks which slows things down.  A tip that I read here and tried, and can vouch works well, is to completely immerse the flask in the oil bath.  A good drip rate (at ATM) would be a drop about every 3-4 sec.  Sometimes atmospheric distillations take forever, especially if you have a lot to distill, but you should probably try this if you are having difficulty with your vacuum.

Flip

_flip_@hushmail.com

RoundBottom

  • Guest
seed crystals
« Reply #17 on: April 07, 2002, 03:49:00 PM »
take a small amount of your oil, about 4mL, and put it in a small glass vial (like the kind you get GHB in).  stick this in the freezer, and it should crystalize.  scrape a small amount of the crystals and put in pre-chilled flask/jar of oil.  put the oil back in the fridge (not the freezer).  crystals should be noticable in 5 minutes. 

pre-chill the oil, as if you put the crystals in warm oil, they will just melt.  replace the small vial of frozen oil into the freezer to keep it crystalized.

i learned a thing or two from charlie dontcha know.

wolfx

  • Guest
Please be careful, I think if your oil is ...
« Reply #18 on: April 07, 2002, 06:20:00 PM »
Please be careful, I think if your oil is starting to make smoke it is also close to igniting. I have never tried to distill sassy oil at normal pressure, is is very easy with an aspirator. If you would like to try it at normal presure, could you use a heating mantle ? Boiling stones might be OK in this case.

hoyt

  • Guest
AGAIN!
« Reply #19 on: April 07, 2002, 06:31:00 PM »
Do what roundbottom says!
 You've been dealing with this since our mutual friend
talked w/me about it!
  Do exactly what RB says, htis is in fact as good a method of purifying as distilling at least for 1 alkene > 2 alkene
Ketone is gonna bee exstremely problematic if ya can't
get this one ouy of the way, and freezing won't help in
that area!
This is humid by the way.
Also this is the preferred method >safrole for some respected bees here1 (madmax for one) :P