Swims sassy is brown, and after distillation, there is a very small amount of sediment and brown residue that obviously has a bp higher than safrole. The oil is ~85% safrole, and takes about 3-4 cycles of freezing/thawing (at~8C) in order to remove all of the brown colored impurity, further freezing doesnt seem to clean it any further, and there still remains a little (teeny tiny bit) of cloudyness.
Swim has performed three isomerizations that have for the most part failed (very minimal yeilds of iso). He ASSUMES that this may have been because he couldnt find KOH anywhere in his vicinity including (finally) the chem supply which would only order a big assed drum. The only thing he had was pH raise (solution) from the hydroponics store, he boiled it to dryness (actually scorched it) then baked in the oven. When added to the sass, it turned dark (brown-red-almost blackish). He applied vac for a good hour, his pump must have sucked up any moisture 'cause nothing condensed. He tried one run with vac overnight, one run atm. Two oxone runs yeilded very little product, and the temp for both of em never got much past 30C.
Swim finally (after much planning and scheeming) aquired some KOH PELLETS (which hes going to lightly grind and filter w/bug screen) and is gonna give abacus' method a whirl. The reason swim says this- is now he wonders if eugenol is present (hes got that funny sass dontcha know!)will that fuck up the isomerization as well? -so swim knows whether or not he should just go ahead and distill that sass anyway.
BTW, speaking of freezing out sass-
swim has managed to separate safrole/iso out of dirty ketone post oxone+hydrolysis . It was distilled, but for some reason, even with a vigreaux (granted it was jacketed with foam insulation, swim will switch to fleece material) everythin came over between 86 and 96C! He has also managed to separate a bunch of safrole from his unreacted iso/safrole mix- although he has yet to confirm by atm bp (hes still in the process)- he has been alternating freezer (freezes both iso and safrole, fridge ~10C separate unfrozen supposive iso, thaw frozen safrole, reseed in fridge, separate etc....will post a new thread if successful (will check by doing both atm bp, then distilling to see if 2 fractions come over).
As far as vac distilling goes, swims been using a ritchie yellowjacket, oil changed after every use -plus, swim finally got good silicone greece and used clamps on the vac hoses as well as using ptfe tape on vac nipples and thermo adapter- swims gotta do something about that vac, its too damned strong - even with gas ballast full open). The adapter that fits to swims pump, its a 2-way adapter- will it harm the pump if he slightly unscrews the cap on the unused nipple? Swim is at a loss, and doesnt have the $ to invest in a weaker pump at the moment. Any other ideas- that wont end up doing damage to the pump?
