The wacker ala MM has proven to be a lesson in frustration, afoaf does not own a stirer hotplate combe so has his flask's heated in a shallow fryer with mag stiring from underneath, also doesn't own a distilation column, just flask ->distilation head-> condensor.
He after what he assumes was successful wacker, as all behaved as described and all noted observations matched those posted, ie color changes in wash's, scumm emulsion etc.
After seperation Dcm/Ketone was fired into 1l rbf, 1" stirbar. The vac source applied, aspirator, with the aid of autogauge showed to pull 27"merc. Same as used for safrole dist. What happened next is still shitting him, The DCM came off no probs, then some heat was applied (perhaps a little to fast, to much, oil bath about 60deg.
Some water came over, as noted by vapour temp, then the whole contents of flask foamed over massively. Oh the safflower oil was added as buffer (?) The mess was back washed into the flask with some distilled water(? not a great choice)
The Ketone in the flask before the h20 was added looked as brown as earlier just foamed onto side of flask. This was then tried again, same thing happened once water had been removed. Contents stay dark until foaming starts then turn yellow, then back to dark once vac source is pulled.
So to finally get to some point here, if afoaf has degraded ketone, ie fucked, how does it behave?
how quickly does the ketone from the wacker have to be seperated?
Does it have to be constantly cold to stop it decomposing? Then when and if it is ketone, which by observation and workup is assumed so, how sensitive to the distillation process is it?
Has he ruined it by heating?
How fast is to fast to heat to bp, and what happens to ketone when heated rapidly?
Everyone keeps saying heat slowly to temp over two hours, what increments in temp are we talking here?
Well there are many more questions, he will try what was mentioned about smaller amount in flask and see if this helps in this instance. The whole incident performed for educational purposes has carved a runway in the carpet from the mad pacing back and forth,
You dont learn from doing things the right way, coz if you did you would already know it.
Keen for some feedback, tired, frustrated, amused and confused.
Happy ?