Ok... just to clarify things out of consideration for all those helpful bees nice enough to answer my post, and in an effort to make better use of their time & effort...
1. My glassware setup consisted of the usual (all 24/40) borosilicate flasks (500ml & 250ml), 200mm Vigreaux (insulated top to bottom w/foam copper-pipe insulation, tie-wrapped), adapters (3-way, 105deg Vac, thermometer) 400mm liebig, metal pot, hotplate/stirrer (Corning), clamps, stands, etc. and 2 thermometers (1 in the adapter, 1 in the oil bath).
2. I measured out 100ml of Sassafras oil, weighing in @ 104.14g, heated in a peanut oil bath with high-speed stirring using an egg-shaped, 1 5/8 x 3/4" Teflon stirrbar, over about an hour, until i hit around 250C. (which is when I gave up). I used tap water to cool my condenser.
3. My observations were as follows:
11:37pm - Started full heat on oil bath, stirr on #8. As the Sassafras oil started to heat up the smell became less sharp, more "warm & diffuse", if i can call it that.
11:42pm - Bath temp @ 100 C, dropplets can be seen forming on the top (empty) half of the 500ml flask containing the Sassafras oil (I'm assuming this is water)
11:48pm - Bath temp @ 136 C, lots of dropplets can be seen forming on the top (empty) half of the 500ml flask containing the Sassafras oil
11:50pm - Temp in top thermometer (in the adapter) starts to rise, now @ 32 C
12:02am - Bath temp @ ~ 200 C, top thermometer @ around ~38 C, insulation on Vigreaux column is getting warm to the touch
12:06am - Bath temp @ 214 C, top temp @ 38 C, no more water dropplets forming, now a there are many steady streams of liquid running down all sides of the top of the 500ml flask containing the Sassafras oil
12:14am - Bath temp @ 232 C, top thermometer temp @ 40 C, heat reduced to #5 (since we've supposedly reached Safrole bp) no other changes.
12:24am - Bath temp @ 246 C, top temp seems steady @ 42 C, there's obvious condensation going on in the lower third of the Vigreaux column and streaming back down into the 500ml (Sassafras containing) rbf. I'm starting to wonder if using the Vigreaux column was such a good idea?
12:29am - Temps still climbing slowly, I'm gonna let the bath cool below 232C & get rid of the Vigreaux column. Heat set @ zero.
12:40am - Streaming in the flask is down to a barely-noticable minimum, I'm guessing that @ 232 the Safrole started to evaporate but for some reason couldn't make it through the Vigreaux column before condensing again. Vigreaux column is now removed so all i have is the 105deg adapter going directly into the Liebig, heating is cranked up to full blast on the oil bath.
12:50am - Bath temp climbing back to 196 C, top thermometer @ 50 C
1:01am - Bath @ 222 C, top unchanged at around 50 C, no streams observed in the top of the 500ml Rbf (containing the Sassafras oil)
1:03am - Bath temp climbs to 228 C, streams of liquid can be observed flowing down the sides of the top half of the 500ml flask containing the sassafras oil.
1:06am - Bath temp @ 233 C, more streaming, top temp unchanged,
1:10 - Bath temp @ 241, same deal.. no changes, I give up! where's my fuckup?
![Huh ???](https://thevespiary.org/talk/Smileys/default/huh.gif)
NOTE: Right before I gave up I shut the stirring down, temp was at around 240C, for the first time i DID observe a bit of bubbling, albeit not much. Thought I'd mention this for whatever it's worth.
There's a transcript of my lab notebook for this procedure. I read Rhodium's write up on distillation of Safrole as well as a few more, though most discuss vacuum distillation - and well, since I don't have a vacuum for the time being.. you can understand.
So far 2 bees have said that I should've pushed the bath temp to 254 C or thereabouts, I'm gonna try that. I will clean out all my glass, grease my joints & give it another shot. I'm gonna be using the same Sassafras that remained in the flask from last night - Hope that's okay. Circumstances surrounding the purchase of the Sassafras oil makes me pretty confident this is the real stuff.. I mean yea, it could be crap.. But then again I *could* be fucking up somewhere.. I'd hate to toast a really really really good source!
Some questions that come into my mind:
- Is a 500ml flask too big for only 100ml of Sassafras?
- I didn't grease my joints, could that have something to do with it?
- Should I heat the oil bath more slowly?
- I was stirring constantly at a setting of #8 all throughout. As I mentioned above, when I gave up I shut the stirring first & observed some (minor) bubbling @ around 240C. Should I perhaps be stirring differently?
- I know the Vigreax column was insulated, some bees have said I should be more patient, how long should this distillation take? what should I expect time-wise with, w/o a Vigreux column?
I'm gonna give this another shot tonight, advice, help, hints, suggestions and even prayers are GREATLY APPRECIATED! Will post results! Thanks to all you bees nice enough to help out!
Peace