I read on this website, forgot the name, of this guy who was performing a standard mm al/hg and it his failure went like this.
First he used different ketone as his last couple successes. This time his tone has a less flourescent yellow green and is more pickle juice colored. Smelled the same he said and tasted the same.
Amalgum -- He used 350mg hgi2 instead of hgcl2 and prestirred it a good 30 minutes it said. When he added the ingredients to the sep funnel he did so very carefully and slowly allowing the layers to seperate. He added nitro, then meoh, then ketone. His ketone sank to the bottom of the layers, he thought it floated on the other 2 layers the last couple times but he could be mistaken. The amalgum went great. Addition in 25 mins, nice and hot, blue, 1/2 up the condenser pourin like a faucet. Everything looked the same as last time except, there was much more tinfoil left. Now he didnt mean there were chunks but alot of tiny little flecks. Much more than previous attempts. His NaOH solution ate all of it though. But he trudged on, assuming it would only hurt his yields a little bit, IF he was even wrong.
Washes -- Extractions went fine with toluoene it said. During the first water wash, there was a white semi solid interface, very cruddy looking. He didnt keep it. During the 2nd there was the same but not as big. 3rd wash - normal. 4th wash he washed with saturated nacl and it went fine he said. And with a final wash he washed with dh2o again and it was fine looking. Dried with 40 grams oven dried epsoms. What are the water washes used to wash out?
Gassing -- Set up was h2so4 over anhydrous nacl saturated with muriatic. Gas traveled through a vigreux column jammed pack with cacl2. Same set up as before. Started gassing slowly and it was going fine, he could see cloudiness in the water. Stopped for a second, resubmerged and noticed a little suckback occurincg slowly. So he turned on the funnel and accidently allowed a stream of h2so4 to fall. Enough that it made the sep funnel make a glug. He reached to take the glass tube outta the solution but it was already bubbling viciously. He noticed the solution turn a little tannish with not precipitants and said mother fucker god dammed fuckin funnel thingy mother fuckin bitch. So he MAY have overgassed. Not sure. He gassed a little more but nothing. Just turned a little more tan. Obviously he saved the contents of his tan solution.
He thinks he should have at least gotten SOMETHING. After the NaOH addition it had that fishy smell that it always has in the past, signifying to him that it was a successful reaction, he said. He said he was going to look up overgassing.
Edit: Ya know even if the ketone wasnt the absolute best, it had enough qualitys to produce at least some honey... bah.. thinking too much about this is hurtin my brain