Bright star's step 1 help !!!

[andrew.z]

OK i have done step1 i started with 300ml of sassy and i ended 5 hours later with 230ml of i think safrole and a few ml left on the flask of sassy... too tired to carry up to the end any way it is enough.

Please review what i have done and please tell me why i had some troubles.
I started with 500 ml rb flask my fisher 7" aluminium plate, a bowl with peanuts oil and a water aspirator ( plastic one ).

OK OK i started the aspirator and i turned the heat and of course i had boiling stones.
After almost 1 hour the temp didn't want to go upper than 42 degrees C.
I paniced then i got rational again, i turn the water more on... but nothing... so i placed my stir bar in and got it spin at warp 5 but still no more than 42 C.

Then i wrapped the flask and bowl with aluminium foil and waited... a little ... but still nothing... so i put the heat at maximum (10) and after a while the temp climbed and at 110 C some white like water stuff come into the reciving flask... but the temp climbed a lot.... so i turned down the know to 8 but nothing... it was approching 170 C so i took the aluminium foil off and it went down.

To make it short i have tried every way to stabilize the temp but it just didn't.
I have noticed that at 10 the temp after 10 minutes got up... i have noticed that by turning off the stir bar the temp goes down... i have tried to set the temp of my fisher at 8 or 7 but the temp goes down.

So i was unable to stabilize the temp it either goes up or down...

the flask was immerged almost half into the oil and 1 cm of sassy was above the oil level at beginning.

The safrole i have gotten is clear like water it smells more softly but somehow different than sassy and it reflects light with some mild yellow/green shadow ( but to see this shadow i had to put the bottle against the light ...).

My concern now is step 2... how am i supposed to stabilize the temp at 104 ??

Please tell me whatever i did wrong so that i can correctly tomorrow when i start step 2 and 3 .

Thanks guyz.
Andrew

[Bromine]

For the next step, always keeep your stirbar on. You should put another thermometer in the peanut oil as well. It might be a good idea to measure the temp difference between the peanut oil and inside the flask with an experiment. Anyways, it will be a 10-20 degree difference. If you don't change the temp of the hotplate after you find the right place, you'll be fine. Just make sure the peanut oil is stirred as well to make sure of even heating.
I hope this helps some.

[andrew.z]

i am not sured i have understood at all... you are saying to put a stir bar in the peanut oil as well ? anche check its temp ?... but why did i have all those troubles in the first place ?

[Ollie-RSM]

For future use, when you're distilling you usually don't have to worry about manually controlling the temperature. The idea is the temp will rise to the boiling point of the liquid and pretty much stay there until all of that liquid has come over. You just set the heat control so that you get a decent rate of distillation and let it go.

As for temp control in the methylamine synth, you don't need a second stir bar in the oil. Just stir it by hand every now and then. And it is a good idea to put a second thermometer in the oil. You raise the oil temp to ~104C, wait ten minutes or so then check the temp in the reaction flask. If it stops rising and is below 104C, then raise the temperature of the oil by a few degrees. Check the reaction vessel temp again...repeat until it hits 104C.

....or you could by a mantle on ebay for $20  https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000104837-file_n5ac.gif" title="View this image">

[andrew.z]

ok thanks for the help as a matter of fact today without any bowl of oil my temp was constant on 104C.
But if i wanted a temp higher than that.. no way i was already at maximum speed.
Now i understand why a bowl with oil is better than not.
I have done step2 with no oil but i got messed up something is wrong... please read it and tell me ehat is wrong...

[majic22]

sorry guys swim knows this is an old topic but he was doing some last minute studying before he tries this on his own and found something he has a question about.  in one of the above posts referring to sassy distillation...."Ollie-RSM" said.....

"For future use, when you're distilling you usually don't have to worry about manually controlling the temperature. The idea is the temp will rise to the boiling point of the liquid and pretty much stay there until all of that liquid has come over. You just set the heat control so that you get a decent rate of distillation and let it go."

This confuses me.....does this mean that you could just turn the heat up to the highest setting and it wouldnt go above the safrole BP until it has all distilled over?  If not...how do you know what the "decent" setting is that it needs to be set at?
Theres nothing to be afraid of, just concentrate, and trust the music.

[Chromic]

Ok, those words might not help you, but usually a reasonable pace is 1-2 drops per second...

However, I'll say my final piece of advice: "When in doubt, distill slowly."

People like to rush the chemistry all too often (I've been guilty of this many times), patience is key.