Bubbles

[experimentalbois]

SWIM's experiencing something strange and wanted to see if anyone else has experienced the same thing....SWIM's in the middle of the final stage(distilling ketone) of MM's wacker, and is witnessing some weird shit....the distilling flask has really really big bubbles in it and when they come up towards the three way and to the condenser, they're forming black tarry shit.....hydroquinone? SWIM did all of his washes and has never experienced this before.

this is SWIM's 4th ketone distill and never has he seen anything like this...any help would be most appreciated    

[experimentalbois]

and all of your help was so useful and appreciated....


anyways, SWIM stopped the distillation and washed his equipment....and the continued the distillation and ketone came over....so SWIM's assuming it was just hydroquinone but i guess he'll never know

[Noid]

Sounds like water in your wacker thats being distilled.. whenever water comes over huge bubbles are noted here, but they don't make it up to the 3 way however.. close, but not that high, are you using a rotary vane pump or a diaphram?

Also, I have found that every single wash is very critical to have an easy distill afterwards.. when you do the NaOH wash to remove the hydroquine, really mix the two up as much as possible and don't think 1 wash will cut it.. all 3, at 5% a wash will save you lots of time and frustration later..

[pickler]

Swim had that problem many moons ago. How much dcm did you use. By lowering the amount of dcm used in the extraction of the tone, the tone is harder to clean. You need to make sure your washes are done very well. Swim sometimes had to do 3 or more naoh washes to get it clean enough to distill.
If you dont do your washes good enough your tone will get all kinds of unwanted problems.

[experimentalbois]

Thanx a bunch for all the input....

Just to let you all know, due to the small size of SWIM's equipment(lab equipment that is.... ), SWIM cuts MM's benzo in half and has been doing this successfully for some time now....so when SWIM does the NaOH washes(3 of them), he makes a 5% solution, but cuts it in half(15g NaOH in 250ml of water)...should SWIM do regular washes(30g NaOH in 500ml of water) or just do 3 of the half washes??