Pardon my ignorance but how are everyone getting their safrole crystals?

Sometimes even at -18C it wouldn't crystallize for me. Get a seed crystal take a test tube with 1ml or so of your oil, put the test tube in a bowl of alcohol in the freezer and drop the temp as low as possible. Wait a night or 2 and add the seed crystal to the supercooled oil and watch it crystallize. Pour out the remaining oil, which was thick and smelled of cloves.

"dilute it with 3 parts water and use that as a wash.
then once it's lightened up a bit take it into dcm and wash out the acetic acid with water.
dry the dcm with a drying agent filter and evaporate the dcm should be pure enough to use."

i found it got very emulsional doing it like that and the water/acetic washes. kept some of the oil and caused losses.

to be honest i took it into dcm first and then washed the dcm several times with the acetic then with water then filtered - then i evaporated the dcm with a hair dryer at a distance (held with a retort stand facing out doors) to get some nice golden oil.. still not clear but i was working with too small of a qty to distill with my 24 40 kit
my acetic was ice cold too, i dont know if that helped.

if your oil is dirty, take it into the dcm first then filter the crap out before you wash, that will help prevent emulsions

i know my oil is mostly safrole though so im ok.

EDIT

now i think about it, my oil is different source to yours, and is alot more pure i think.

when i had indian oil (mixed fractions every where), when i distilled i always washed the eugenol out of my oil with 5% NaOH a few times then water. the washes will be really red. you have dirty china oil maybe you should do that.

heres what i would do. if it is not visibly dirty (like black) and you have a decent vacuum. Vac distill it all accross FIRST

take down the temps and you dont have to take it really slow either

then wash that oil with 5% NaOH till the washes are clear, then wash a couple times with water THEN

Distill that clear oil without vacuum to get a positive id of your oil. you will melt plastic keck clips here on the hot side and an oil bath will smoke you out. i wouldnt worry about a fractionating column, it isnt needed

its a real bastard of a process but it will safe all this guessing about where things ever went wrong

The iodo route is hard Pd, i say forget it for now and get benz or 02 wackers working consistanly. there is so much to learn before you can just pull off the iodo route IMO

Also palladium jons iodo route keeps in the other alkaloids and phenols in the sass oil as it helps prevent side reactions or something in the bromo synth. in the benz wacker this is not the case, they will screw up your distilling tempretures and casue you problems.

you are right, save your dcm. i have a big drum of it though lol

At least take 50 mills of your oil, do a 5% NaOH wash and if the washes are really red you know it was worth it. then wash the NaOH out of the oil with water before you distill, not doing this has turned my oil to plastic once before

I'm into trying the washes only as an alternative to distillation... if the oil has high enough saf % as mine does, this should be a viable option. However if the washes were to render my oil a lot easier to distill, this would be good too. But if washes alone can get most of that 8% or whatever of non-saf constituents out, then that's wonderful.

Thanks for the last several posts on this guys, I only just got back to this thread this morning.

Ya, I have been keeping all my washes already! I know I'm stupid enough to accidently throw away my product! Should the sassafras layer be a creamy cloudy suspension?

i cant believe some of you SOB's still have access to sass 

MM (its really you?), given my experience with distillation of oils that are a mixture of many compounds of varying BP's, my guess is that your problem is excessive vacuum and that your oil contains some lower boiling compounds just as others have mentioned.

As an example, if I hold say 100mm Hg of vacuum and bring the flask to 100°C, then quickly reduce the vacuum to 30mm Hg I get some serious bumping, even with the stirrer going at full speed. For several reasons, I found that my vacuum can increase quite some time after its already stabilised and when your already at  a temp that is boiling some low BP substances, when this happens I get sudden bumping even if the change in vacuum is only 30mm Hg. Dont know if you have a vacuum gauge, but if you dont you will have no idea that such small changes are occurring.

My suggestion, distill without vacuum up to 150°C, once nothing else comes over, bring temps back to 100°C and SLOWLY increase your vacuum to full, using your bleed. Then start slowly increasing your temps.

are you using insulation palladium. alfoil wrapping all over your hotside? that is a must.

I had trouble even getting the oil bath and sass > 200c the last time I tried and then it turned really dark red/black and nothing came over

the hotside flask always goes black, as long as there is no NaOH in there your all good, the fact that you can actually SEE the hotside means you dont have it insulated well enough with alfoil

i told you, if you want to do this right, with your multi fraction china oil, you need to vac distill, do the washes then atmosphere distill, in that order. it is a bastard i know but i have had oil like yours and been through so much with it and wished i did this from the start. you will never know what you are dealing with otherwise

you have already seen multiple fractions distilling under vac, how can you ever tell which is the one..

try using a dry bath, fill your pot up with salt instead of peanut oil, see how you go. Peanut oil will smoke your whole life out lol

start your distill with out vac once all that snap crackel and pop is gone then let the
shit cool and wack the vac on.



oh post edit ....

for the origonal question at hand.

looks great Pd! great work. keep us updated
btw, how are all you guys getting your sassy oil? I thought it was really hard to get now and i havent tried for a long long time in fear of LE. not asking for sources or anything, just general thoughts and guidelines maybe?