Heh... Ethyl would you believe that this dawned upon SWIM only after the distillation of water - When SWIM realized (about an hour later) that there was no change in the temp on the thermometer (which by now was laying in the sink!). Fascinating this chemistry thing really is.. And another thing... All you said makes perfect sense
You're far too humble!
Now for SWIM's much-anticipated "detailed lab report" (for school of course)
Setup:
- (2) 250ml RBF (rxn flask & distillate reciever)
- Vigreux Column (insulated with multiple layers of aluminum foil & covered with foam pipe insulator from the hardware store. The pipe insulator was bought in the correct size to fit the diameter of the vigreux col. & an extra 1/4" to fit the tin foil that it was gonna be wrapped in. On the subject of foam pipe insulator, there are a few types. The best one is the one that has adhesive on both sides of the slit down the middle. Just cut a piece of it down to the length of your column, wrap it around, then peel off the adhesive & boom! you're all set - A nice clean job and absolutely flawless insulation)
- 3-way adapter & thermometer adapter
- (2) thermometers (1 to measure rxn temp & 1 for oil bath temp)
- 400mm Liebig condender (cooled by tap water)
- 105 deg. vacuum adapter.
- stainless steel "salad bowl" (heavy duty - for the oil bath, and YES IT WORKED!)
- Corning hotplate/stirrer combo
- (1) 1 5/8 x 3/4" magnetic teflon stirrbar (egg shaped)
- keck clamps on either side of condenser
- (3) stands, (4) 3-prong clamps in total to hold the glassware
- Robinair 15600 vacuum pump, thick-walled rubber hose with a couple of hose clamps (home depot)
** Glass was cleaned with acetone, and all ground glass joints (24/40) were greased prior to use.
Now here's what happend:
SWIM started by measuring out roughly 100ml of Sassy in a graduated cylinder. SWIM weighed the empty cylinder before pouring the Sassy into it, so that he would know exactly how much Sassy (mass) was in the reaction (so that SWIM would later know roughly how much safrole was in his Sassafras essential oil %).
SWIM then poured the Sassy into the rxn flask, fired up his vacuum pump & set the hotplate/stirrer to low heat (#3), stirr (#8) expecting the Sassy to come over at around 66-68 C.
Oil bath temp started to rise slowly, but temp of the rxn remained at ambient levels (room temperature). SWIM started getting restless so he turned the heat up a notch, just to help get things going.
SWIM noticed that the few droplets of water that were in the distillate flask when he setup the glassware were now gone, which lead him to note that he should get a fucking water trap if he doesn't want to kill his brand new vacuum pump!
Bath temp was climbing nicely @ heat setting #4, roughly 1 degree C every 1-2 minutes. (ambient temp was 29 C). SWIM mistakenly decided that when bath temp would hit around 64 C, he would drop the heat back to #3 & start the water in the condenser - Truth is, doesn't make one fucking difference what the bath temp is cuz the bath temp (IMHO) has to be at least 25% hotter then the rxn temp SWIM was aiming for! SWIM cranks the heat up to full blast for a couple of minutes, just until bath temp hits around 80 C, intending to roll it back to heat setting #3 at that point.
It then occured to SWIM that that's also retarded! Why play things by ear? When the safrole is ready to evap it will fucking tell you by itself!!! Temperature in the reaction flask will begin to rise rapidly. THAT is SWIM's cue to drop the heat back to #3!!! revelations!!!
Few minutes later..... BINGO! bath temp @ 84 C, and rxn temp just started to rise. That's SWIM's cue to drop the heat setting to #2 (just to maintain bath temp at around 90-100 C) Distillate starts coming over at roughly 2-3 drops p/second, rxn temp @ 50 C. SWIM's guessing this stuff is forerun since there are "swirlies" in the flask (difference in refraction indexes of two substances I guess).
SWIM changes the recieving flask & continues to heat. Bath temp is @ around 90 C, rxn temp seems stable @ ~ 56 C. Distillate coming over at roughly 2-3 drops p/second and NO SWIRLIES!!! SWIM drops the heat setting to #2, hoping to simply maintain the bath temperature at the current level.
15 min coffee break.....
SWIM returns from his coffee crisp only to find that distillate has slowed to a trickle.. about 1 drop every 2 seconds or so. Rxn temp dropped down to around 55-54 C, and bath temp dropped to around 70 C. Woops.. I guess the #2 heat setting wasn't high enough to maintain 90-100 C in the oil bath.. Oh well... SWIM cranks up the heat to about #4 but that didn't do much so he went with #5. (didn't want to overshoot). At setting #5, bath temp appears to climb 1 deg. C every 30-45 seconds.
(SWIM thinks in the future he'll simply crank up the heat to full blast until bath temp hits the 70's, then reduce it to #5 to level out in the 90's, and then reduce it to #4 to maintain this optimal bath temp).
Whoopi! bath temp back into the 90's, distillate flow rate starts speeding up again. SWIM reduces heat to #4 to maintain this temp & goes for more food!
That's it... It worked! Ideal rxn temp seems to be 56 C. That's where the safrole comes over steadily @ 56 C!
Hurray for SWIM!!!!
Note: Even though all these settings are exclusive to SWIM¡¦s pump (and it¡¦s vacuum output). I¡¦m hopeful that my experience will help other bees understand what¡¦s going on with their rig ¡V Again, maybe this is all one big fuckup & I¡¦m making things worse? But the intentions are good ƒº
Peace out¡K
