Practial small-scale sassy-->iso help please

ApprenticeCook · DILLIGAF

get a microdistillation set to vacuum distill such a small volume.
"practical hypothetical experience" is not experience.
Get the micro kit and distill it, use the same kit for all your steps. Done.

-AC

the alchemist · Mon Jul 11, 2005 8:02 pm

Try to aquire more oil before distilling your sassy oil.

For stirring, just use a stirbar and a magnetic stirrer/hotplate combination. It would be preferable to use a heating mantle and a variac instead of a hotplate. If you need to use a hotplate as a heating source, you will need to immerse your rbf into a silicon oil bath to ensure that the rbf is evenly heated.

Skip the isomerization step and Wacker that purified sassy directly to MDP2P. It is much, much easier.

ApprenticeCook · DILLIGAF

distilling the 20mL sassy is no problem, the problem comes from the massive glass surfaces in normal distillation setups, the 20mL distillate can be spread as a film (as all distillates are) over the glass surfaces, however seeing as there is only 20mL the glass may take all of this. With a micro distill kit the glass is smaller and this allows better distillation of the smaller volume.

-AC

Ephoton · Tue Jul 12, 2005 2:51 pm

I would use lithium and alcohol for the isomerisation then
mercury acetate for the purification.

2spun · The Resistor

Ephoton,

No disrespect here but what type of lithium are we talking about?
Just so to clear the air
Li and alcohol can make for nice fire balls.

bio · Working Bee

............Anyhow, is a 30cm 20/40 vigurex column, + 30cm leibig condensor 20/40 + 250ml rbf too small for say 100ml distillation? ..............

Ground joints are 24/40 around here. This size is fine as you should fill the flask 1/3 to 1/2 max when cacuum distilling A 300mm vig will distill any amount of oil that runs through it. The hold-up is about 15-20ml. Put a few big marbles in the vertical of a Claisen adaptor for a little less.

Round flasks need the egg shaped stir bars. One size fits about three sizes. Better the fit the faster the controllable stirring. Cooking/frying oil (the hard stuff) is fine on a hotplate as bath as long as the thermostat on the plate is decent.

Ephoton · Thu Jul 14, 2005 5:04 pm

ive used Li from energizers heaps with alcohol makes butifull and very strong lithium alkoxide never had one fire. just used small bits at a time and kept it cooled
in salt ice water.
cant see why it wouldnt work.
stuffs so basic you can smell the crystals (ouch)

2spun · The Resistor

OK swiy can see the small pice at a time,
swiy has use'd that method on a few things.. very time comsue'min.
cold alcohol and li-aluminium swiy has not.
swiy can't find it in his hart to mix Li/aluminium with anything that has h2o in it.
Thats just swiy.

Ephoton · Thu Jul 14, 2005 6:41 pm

hehe and rhodium said this wasnt possible.
iso saf no glass in small scale got admit its a possibility now.
few thermomiters some batteries some photostop, battery acid
some filters and a few glasses might just be the way for the moving chemist
or the chemist who wishes to have no glass.