Hey there,
Working on an AB mescaline extraction using lye, vinegar, and varsol (toluene/xylene). Everything's great so far, solvent and aq layer separate fine. I add vinegar to the solvent layer, shake, wait, and nothing happens.
I've added a bit more vinegar, shook longer, put it into a hot water bath, but nothing seems to be working.
I realize this is probably due to something screwy I did, but any help would be appreciated.
|
Well, it looks like I may have spoken too soon. Seeing a bit of separation, let's hope it continues.
|
Hey again,
Evap'd three pulls of vinegar and was left with a yellowy-offwhite film on the dish. Scraped it up to yield a pile of yellow-white fluffy crystals. All good.
Here's the fun part.
The crystals burn my tongue. They also clump together and have a slippery texture. I'm thinking there's definitely still some base in there.
Here's my procedure:
450ml filtered, reduced cactus juice added to mason jar
100g lye added slowly to cactus juice, solution stirred and allowed to cool
125ml Varsol (xylene/toluene)added to mason jar, solution shaken, burped, allowed to separate
organic layer removed with glass turkey baster and transferred to mason jar
25x3ml vinegar added, shaken, separated, removed, combined
vinegar evaporated in rectangular pyrex dish on top of pot of boiling water
I could convert to HCl and wash with cold water, but I'd rather not have to go find HCl.
update:
washed half of my yellowish naoh contammed crystals with boiling anhydrous ethanol
after filtering and drying wash yielded white crystals
crystals still burnt tongue, were soapy (!!)
recombined yellowish crystals and white crystals
placed back into mason jar
dissolved in ~50ml water, pH tested 8+
added ~200ml varsol, shook, separated, repeated
leaving to separate further and will pull off varsol tomorrow
checked some mesc acetate solution that has yet to evap for pH, and no surprise, it's high
is this just due to me not waiting for the base'd solvent to separate long enough?
think I may have this figured out, but I'd like to prevent it in the future.
|