Time Temp Heat
+ 0m 24°C 0/26
+ 30m 36°C 26 vac off
+ 210m 112°C 26/30
+ 300m 144°C 30/28
+ 540m 156°C 28/27
+ 600m 164°C 27 sleep
+ 960m 152°C 27
+1290m 151°C 27/0
- liquid was very dark brown and almost opaque
- set up for vac distillation in the same 5L RBF flask
Time Temp Heat
+ 0m 27°C 0/30
+ 100m 28°C 30/32
+ 120m 28°C 32/34
+ 160m 32°C 34/36
+ 180m 36°C 36/38
+ 210m 42°C 38 (added loose tin foil shroud to distillation flask)
+ 212m 138°C 38/36 coming over > 1 drop/sec
+ 395m 141°C 36/0 replaced receiving flask*, and restarted distillation
+ 570m 144°C 38 replaced receiving flask*, and restarted distillation
+ 705m 146°C 38 stopped distillation**
* don't ask, SWIM only has a 1L receiving flask, it SWIMs largest 19/22 flask. owing to breaking SWIMs only 24/40 vac adapter, SWIM must use a 24/40 - 19/22 adapter and a 19/22 vac adapter and, therefore, a 19/22 flask. SWIM is still awaiting a replacement 24/40 adapter.
** you know you are done when the stir bar no longer spins due to being trapped in the solids
total clear, water white fluid recovered: == 2370mL, 98.7% v/v
the distilling flask had a chunk of brown solids on the bottom, and brown solids splashed on the sides. when the flask had cooled down a bit, maybe 20m but hadn't cooled off completely, it was easily cleaned with water. no acetone or other solvent was needed. SWIM was very impressed by the ease of removal, as ketone distillation tar removal is about as fun as chewing glass.