Well,built a shaker table for this one.Has a 3 inch stroke,180 strokes a minute or 3 per second.Geared down a motor from 1725 rpm,converted rotary motion to linear with crank/rod.
Used 2g PdCl2,10g CuCl2,500g MeOH and 150 g crystal clear sparkly double distilled safrole.Premixed Pd with half MeOH for 2 hours.Premixed all others idividually for 10 minutes and dumped into standard 2 litre pop bottle vessel.Pressurized with O2 from a tank.Sessions were 12 minutes,purge and re pressurize with O2.Coffee colour.First hour,pressure drop 2 psi per session,after an hour or so the colour went a bit olivey and she started gobbling 3.5 to 4 psi per session.Left for 2 hours, came back and psi drop of 9.Did a fewe more sessions, 3 to 4 psi drop, then time for bed. Overnight 8 hours she dropped 19 psi and started looking a bit burgundy.Over the day got more burgundy and then darker,and started smelling sweet..actually quite a nice smell. .O2 consumption dropped ,exteneded sessions to half hour of Shaking With Extreme Prejudice and psi would drop only 1.5 or 2. Jesus what a hungry bitch.Figured she was done.Total SWEP 12 hours.Sitting 11 hours.Total psi drop 170 psi,assume some leakage per gauge check..so 160 or so psi drop.Interesting psi did not seem to make a difference..do 40 psi and would drop 3 psi,next session 32 psi and would drop 3 psi.At the end it looked just like cherry cola, c-o-l-a cola
Dumped into 1 l d H2O, turned to hot chocolate with little burgundy swirls.146 grams of red,very red,I mean Ferrari red oil dropped out.Dropped G D sep flask so use the funnel trick/finger stopper.Washed alcohol twice with 150 g toluene,mixed with oil, and washed oil/ toluene 2 X 250 g H2O.H2O took up some chocolate.Dumped in 150 g peanut oil,Distiiled under vac toluene and mix went back to cherry cola.Forgot to grab a bit of oil to see if reacted with bisulphite.Put in freezer and head to bed. Will report on Pd recovery and results in couple days.If it doesn't work don't care about saf,just happy to get Pd back.Any comments critiques questions?? Want to try Ritter's? IPA .
Piece of advice don't buy digital LCD pressure gauge..methanol vapour gets in and absolutely melts the shit out of it.Took her apart and looks like was stuck in an oven