I am currently doing an A/B from 100g accuminata, i pressure cooked in phosphoric acid, strained/leeched all the salt out, then boiled down to about 500ml, did a toluene defat, and now have basified it, resulting in a lot of tannins i assume, precipitating. the solution is quite thick too, i attempted to vacuum filter the tannins out but to no avail, it clogs the filter paper immediately.
my solvent is toluene.
upon trying to extract the spice i found that it produced horrible emulsions, ok, no problem ill just collect them instead and combine later after heating with gentle mag stirring.
it helped somewhat, 90% of the toluene seperates although as soon as i pour it into the sep funnel it mostly re-emulsifies for a few hours, now i can, if im lucky, drain off the emulsion giving 2/3rds of the clear toluene. the rest is locked in an emulsion, and i now have a question: what exactly is this emulsion made of? at first i thought it was solid tannins forming nucleation sites so i painstakingly vacuum filtered some emulsion and while it was much nicer and less prone to emulsions, it still did if shook, and even with re-filtration would form this perculiar waxy skin, for the emulsion bubbles yet when they burst, the skin remained.
What is this? and how can i avoid this? to ensure that if i get emulsions at very least they will break down? universally the answer ive been given is salt and/or base, this hasnt worked, if anything it makes the issue worse as enough salt causes all the tannins to float in solution pushing it right into any emulsion preventing it from settling readily.
earlier today i painstakingly washed my toluene, drained off the emulsified waxy skin layer hoping to settle it, dilute and decant off, to minimize the losses, but just randomly i thought, i should see what happens if i use distilled water instead of basified water or brine as i had before, my main volume of toluene was at least free of water at this point so it was a good opportunity to reduce any hydroxide content. upon doing so it, immediately settled, no waxy emulsion skin and the bubbles all settled and formed a perfect binary system. this contradicts everything ive ever been told.
I had drained off the emulsion-skin into a second, smaller sep funnel, i tried washing that with distilled water too, but sadly doing that did not fix anything, it prevented the emulsion-scum forming in the first volume, but it doesnt seem able to destroy it in this one, so im still stuck with the inconvenience of producing clean-enough solvent to move onto the second stage. especially since i dont know the composition of this skin/film/scum.
can someone please help me understand whats going on?
my solvent is toluene.
upon trying to extract the spice i found that it produced horrible emulsions, ok, no problem ill just collect them instead and combine later after heating with gentle mag stirring.
it helped somewhat, 90% of the toluene seperates although as soon as i pour it into the sep funnel it mostly re-emulsifies for a few hours, now i can, if im lucky, drain off the emulsion giving 2/3rds of the clear toluene. the rest is locked in an emulsion, and i now have a question: what exactly is this emulsion made of? at first i thought it was solid tannins forming nucleation sites so i painstakingly vacuum filtered some emulsion and while it was much nicer and less prone to emulsions, it still did if shook, and even with re-filtration would form this perculiar waxy skin, for the emulsion bubbles yet when they burst, the skin remained.
What is this? and how can i avoid this? to ensure that if i get emulsions at very least they will break down? universally the answer ive been given is salt and/or base, this hasnt worked, if anything it makes the issue worse as enough salt causes all the tannins to float in solution pushing it right into any emulsion preventing it from settling readily.
earlier today i painstakingly washed my toluene, drained off the emulsified waxy skin layer hoping to settle it, dilute and decant off, to minimize the losses, but just randomly i thought, i should see what happens if i use distilled water instead of basified water or brine as i had before, my main volume of toluene was at least free of water at this point so it was a good opportunity to reduce any hydroxide content. upon doing so it, immediately settled, no waxy emulsion skin and the bubbles all settled and formed a perfect binary system. this contradicts everything ive ever been told.
I had drained off the emulsion-skin into a second, smaller sep funnel, i tried washing that with distilled water too, but sadly doing that did not fix anything, it prevented the emulsion-scum forming in the first volume, but it doesnt seem able to destroy it in this one, so im still stuck with the inconvenience of producing clean-enough solvent to move onto the second stage. especially since i dont know the composition of this skin/film/scum.
can someone please help me understand whats going on?
