Would isolating the goo, adding freh (dry) EA to it and waiting move the water and citric citric acid out of the salt?
Quite sure it would not do much, as M-Cit + CA + water would be totally mixed up together, so the
only way would be to one-time dissolve all of them at once and then only precipitate the M-Cit again. So therefore I think this re-x in OTC alcohols is the way to go.
I put some solubility data in the chemical guide thread, but as it is a goo it is not easy to be measured. So simply just use low amounts of IPA or Ethanol (IPA preferred, as it is easier to come by as 99+ %). The issue would be that the goo is very sticky of course. Therefore it cannot easily be transported into another vessel, which can be heated, without leaving behind a bigger load. Therefore if people encounter goo more often, then I would already start crystallizing in a vessel that you can also heat up. With many glassware it might not work. But going low on the alcohol and therefore heat it as much as possible is the key to not loose too much during this re-x.
Formed crystals so I filtered everything but there was a layer of sticky crystals in the bottom of the flask and they were impossible to pickup with fresh EA. I had to pick them all up with water and evaporate that. This left behind almost the same thing. A sticky layer with crystals through it. In the end I used a small amount of water to pick it all up and bombed it with IPA which precipitated everything straight away. Adding water to the mix early on certainly made a mess of things.
Great that it gave you nice crystals, but here I would say 2 things:
1. dont already pre-dissolve it in water. It is just enough to simply use hot IPA and start stirring. It will also dissolve. Pre-dissolving it in water will add more water to the whole system and then make less of your crystals precipitate when adding the IPA. Secondly also as always put it into the freezer to get the max of your crystals back :thumb_up:
2. Now regarding simply dissolving in something (being it water or ethanol) and letting it evaporate again:
This will not help anything sadly. As I said the goo seems to also carry a huge load of plain citric acid. It will also remain like this obviously. Some time ago Twilight Person told to use Ethanol and then simply evaporate it off again. Maybe that can get you something which is solid, because the evaporating ethanol will continuously carry away the excess water. The remaining stuff will be very low or free of water, but still contain a mix of M-Cit + CA. And with water isntead of Ethanol you dont even have the side effect of dragging away the water continuously, so excess water even end again inside of your remaining stuff, making it a goo again.
But in any way this shows that you need to precipitate it from an alcohol if you ever want to separate it from excess citric acid and water. IPA is probably better, it will be easier to get it as waterless as possible. Manual drying not needed (the goo anyways brings water), but definetly use 97+ % IPA instead of 90 %!
So now sadly as I told I have the nice CIELO product and the re-x product sitting and waiting for the instrument, but I cannot do currently
So instead of posting all the data for the goo experiments prematurely, I instead will just give some numbers so you can see what is going on.
The final CIELO product will probably be quite the same all across the world, if you get those nice long needles
So for goo it might be different as I said, which might depend on various factors like actual excess of water or citric acid etc. ... but still I guess the overall composition will be quite the same, like there will be nobody who has a goo and 0 % water inside.
Goo from CIELO, no modification:
19 %
Mescaline Freebase
43 % Citric Acid (so roughly ~ 1:1
Mescaline Citrate : excess Citric Acid)
38 % Water
Goo from CIELO, after full evaporation to dryness (50 °C at 40 mbar):
22 %
Mescaline Freebase
51 % Citric Acid
27 % Water
This shows even if you leave your goo for ages until it fully dries, it will still contain a LOT of water. So you should always go for the IPA re-x.
Attached pictures:
Up-Left = "wet" Goo
Up-Right = "dry" Goo. While drying it formed big bubbles, which then solidified as popped bubbles upon solidification
Down-Left = Product after IPA-re-x. Not analyzed but water-free and probably CA-free.
Down-Right = just some regular CIELO needles
These bottom last 2 still missing and then can make a post about full process ...