After conducting a patchwork extraction procedure incorporating elements of the FASA, STB, and jungle spice methods, I now have a less than expected yield and acetone contaminated toluene. I think there's more to be extracted, but first I need to get the acetone out of my toluene so it doesn't pull up other polar compounds or otherwise complicate things. I remember reading somewhere that they can be separated simply by adding an equal volume of water, being that it's miscible with acetone and insoluble in toluene, but I can't find the reference. Can anyone provide confirmation?

http://orgchem.colorado....upport/ext/extsqans.html

^Looks like you can add water to separate, and information can be found on that link on how to properly perform the procedure.

I'm afraid I don't follow. All I got out of that besides some useful insight into general organic extraction procedures is that toluene and acetone are in fact miscible, which would only seem to complicate things. Am I missing something here, or were you implying that the general procedures outlined there could be applied to separating acetone and toluene?

Then again, I suppose it doesn't have to complicate things. Miscible or not, acetone and water are polar while toluene is not. So it stands to reason that the polar compounds would form a separate layer as they usually do. As per why this didn't happen in the first place, perhaps the organic constituent of acetone contributes a degree of nonpolarity. In that case, the water must have some kind of polarizing effect. This would also explain why some nonpolar solvents like ether have a minute solubility in water.

The point is: wash many times with water (mix well, let separate, discard water), each wash will carry away some of your acetone, leaving your toluene without any acetone after a few washes.

Yes, good. Thank you for reiterating.