The Vespiary

The Hive => Newbee Forum => Topic started by: GenericVersion on June 17, 2003, 06:44:00 PM

Title: ketone distallation gone way bad
Post by: GenericVersion on June 17, 2003, 06:44:00 PM: hmm, SWIM started distilling of DCM a lot of vapour was coming out of the system so in order not to stink up the lab SWIM put a hose on the end of the vacuum adaptor and put the other end into water and went for a cig, came back to the entire system backlogged with salted h2O, hmmm formed an interesting percepitate that SWIM filtered off, and procedded to distill, after this and another fuckup where the vacuum pump lost vacuum and oil; got sucked back into the recieving flask SWIM was able to recover 88g already had 26g from previous distillation, so overall decent yields considering the fuckup

Now for the interesting part, when SWIM started to clean up he noticed that the heating flask had a metallic finish to the inside bottom ( uh oh) so SWIM is assuming it's a sodium base, now how in hell does SWIM get this off!(dcm,Acetone, xylene, kerosene all didnt work0 maybe sulfuric acid of hydrochloric acid?
Title: sulfuric and Hydrochloric dont seem to work,...
Post by: GenericVersion on June 17, 2003, 07:29:00 PM: sulfuric and Hydrochloric dont seem to work, no other acids on hand, any ideas?
Title: any idea how to get this out of a flask, it...
Post by: GenericVersion on June 17, 2003, 08:54:00 PM: any idea how to get this out of a flask, it seems nothing works just a thin metallic film around the bottom, 98% sulfuric didnt even touch it
Title: HNO3 would probably do the trick.
Post by: nutlin on June 17, 2003, 09:43:00 PM: HNO3 would probably do the trick. Mabe you should try pirhana fluid. its conc H2SO4 and H202.
Title: Mabe you should try pirhana fluid. Maybe not
Post by: raffike on June 17, 2003, 09:44:00 PM: Mabe you should try pirhana fluid.
Maybe not
Title: If it is indeed a metalllic film, then aqua...
Post by: El_Zorro on June 17, 2003, 10:06:00 PM: If it is indeed a metalllic film, then aqua regia will get it. But it might be that you etched a thin film off of your flask, which means that it won't come off with anything.
Title: a 10% solution of NaOH in H2O worked well got...
Post by: GenericVersion on June 17, 2003, 10:39:00 PM: a 10% solution of NaOH in H2O worked well got 99% of it off, as far as pirana solution SWIM doesnt have H2O2 around nor the other acid needed for aqua regia
Title: you didn't try NAOH first???
Post by: Precursor2112 on July 20, 2003, 03:48:00 PM
Title: Raf has never had any problems getting ketone...
Post by: raffike on July 21, 2003, 01:22:00 AM: Raf has never had any problems getting ketone flask clean.-He really sees no good in letting the post ketone polymer goop cool down so you most throw that flask away.When all ketone is out,let flask cool to 130C or so and add some xylene and you polymer goop comes out with xylene and your flask is as clean as it was before distilling.Then a little rinse with sulfuric acid and your flask is like new.Don't get excited and throw that flask with goop somewhere and then find someday that goop has become solid.