Thanks for your reply! I did 5-6 pulls using 100-150 mL of Xylene. From Nernst's distribution law it is clear that it is better to do many small pulls than to do one big one. The problem was that the amount of fat I got from each pull stayed the same over the pulls. I used NaCl when the solution was basic to help with the separation. Other solvents? DCM is too toxic without a real lab and without a real system to get rid of the solvents and MBTE will break down when adding acid.
I guess you quickly reached saturation for the solubility of the fats, that would just limit how efficiently you can separate the fats. It's discouraging but in the end it does determine if you can get rid of it - even with the extra A/B i proposed you would still run into that saturation just the same, unless you are able to physically separate a fat layer in a separatory funnel, if you do that you can turn the tables on it? Isolate it then try to quickly extract residu product back from it for maximum result? idk for sure but does make sense and should eliminate the problem.
If you don't have a separatory funnel, I think I have an extra if you want.
Interesting idea. I guess I would then just make the tea basic, extract with Xylene, decant of the clear Xylene and do an other round of A/B on the fat that remains. Could be much faster than what I did
My yield was also really bad but I would guess that was because so much went wrong.
As with every product from nature you never know I still prefer this over buying stuff from shady places and I optimize for purity and not for profit.
That's absolutely right, though what i meant was there are apparently differences and it is said that Peruvianus is variable but for example Bridgesii is more stable and reliable. But yeah luxury if you can choose.
As I scraped the solids from a pan I think the surface is so big that a simple acetone/IPA (dry!) wash should do the job. If I would have real crystals I recrystallize from acetone/IPA of cause. Thanks a lot for you answers, again!
Also @ previous question about recrystallization: there are two major ways, one being to choose 2 solvents that you combine to reduce the solubility making it crash out, the other way is taking a nice clean solvent, maybe even preferably not that high solubility, then take only a bit of it and heating it, just enough to dissolve the product. Then when you allow the solution to cool down, it's best to make it as smooth and gradual as possible (so you could isolate the flask a bit like a blanket to slow it down). Cool down to room temperature then even freeze it to make the solubility drop out. Filter it quickly while cold (it quickly redissolves when the solution heats up), of course a glassfilter will work better. Whatever is left you can just evap, but that slowly crystallized stuff is good quality.
That's because when it is allowed to cool from a saturated solution, it gets oversaturated and precipitates by crystallization. The more slowly this is allowed to proceed, the more 'perfect' a crystalline lattice is built. Quickly chrashed out product however makes more sloppy crystals that also incorporate other minor impurities, breaking the crystal structure.
Regarding your theory on the tar ball: I agree. Having fat in the final salting will do this.
I am a bit surprised. Is there something about PEAs you do not know anything about?
I do like chemistry. But actually there's probably a lot I don't know about PEAs. You recently pointed something out about NBOMe metabolism (open foundation conference lecture), which I did not know and was not an intuitive insight from actual research and very enlightening.
