need help- bad Al/Hg dreams

[sassypants]

Well, I just can't get it right, and all this trial/error is costing me too much $/ketone/whatever.
I just don't know where I'm going wrong. I'm using the method as described in TSII. Now, after I add the 35% NaOH sol'n, after about an hour, things are supposed to settle to the bottom, leaving an alcoholic reddish sol'n. Well, this does not happen. What I get is a little sludge at the bottom, some floating on top, and a greyish cloudy crap liquid. I tried extracting the liquid w/ DCM and got a reddish (pinkish) extract, but furthur work w/ that yielded only crap and headache.

[Rhodium]

Filter the sludge with suction using a filtration aid (like Celite), distill off most of the alcohol, dilute with water and acidify, wash with a non-polar, basify and extract with a non-polar. Dry extracts over MgSO4, filter, and evaporate the solvent to get the freebase. Vacuum distill and crystallize.

For a more verbose description, read

http://www.erowid.org/library/books_online/pihkal/pihkal109.shtml

[sassypants]

yes, I vacuum distilled it.
Also, a note: after leaving it in a cupboard for about a week, the grey mess beaker eventually took on the reddish hue described in TSII (I had left half of it alone, to see if anything would evenyually happen) A *product* of some sort eventually crystallized out of solution, but was not in any way an active compound. Oh well. Try again.