The freezer ICE/xtal is interesting. I did a feezer test too and the mescaline xtals stay at the bottom, the water ICE floats. If you are seeing stuff at the bottom separate from the stuff at the top, the bottom stuff could be the product we want - see if you can separate it out (I ended up dumping the ICE, leaving the bottom part in the jar.

So one thing you haven't tried yet is the simple tek with excess citric acid during salting, right? I highly recommend testing that, it keeps on working for me. Not sure how "anhydrous" my citric acid is because I was sloppy keeping it closed for the past year or so. I will dry it in the oven to be sure. When it works, you will quickly see xtals sticking to the jar. More stuff crasshes over the next few hours, one day seems like enough time to get back the clear solution.

I'm updating the TEK with one observation. Giving the lime paste a little longer to react before adding ethyl acetate gave better yields from the same cactus material, so I'm increasing that time.