I have a friend in an interesting pickle that I’m trying to help him with.
A while ago, I helped a buddy with his small-scale extraction (think poor scientist’s garage); I got him up and running doing room temp extraction, water washing, dewaxing, a quick color removal, to distillation to yield some nice distillate.
He’s been doing his thing lately, and he recently reached out and tells me how he’s doing and that he added a citric acid degumming step and is getting ready to distill it. I asked him a few random questions about it, and then I ask "how did you neutralize the citric acid? He said, what do you mean? I said, if you don’t neutralize it, you’re going to get isomerization. I hear nothing from him for 2 minutes. Turns out he ran across his facility screaming to shut down the distillation and did make it just in time (laughter ensues).
I tell him get it tested before he does anything further because I had a feeling since he rotovaped it, it likely isomerized anyway. I was correct and it’s about 3:1 CBD:d9. So now I’m helping him try to fix this. We fixed the pH, and ran it through the still so we could attempt to recrystallize it.
Right now, I’m trying to recrystallize using heptane. I started with a small batch in beakers using my own distillate as a control, and his. Currently testing 1:1, 2:1, 3:1, and 4:1 heptane to distillate by heating distillate, then adding it to 50C heptane, allowing to cool to room temp, then putting in the freezer (gets to about -15C). My sample currently turns a bit cloudy once it begins to cool, meaning some seeds are forming/growing, but then nothing else happens, even after several hours. My friend’s stays translucent, which worries me that this is unsalvageable, but the fact that I cannot crash my own makes me think something is up.
Does anyone have any tips or tricks that could help my poor friend out? Ultrasound? Ratios? pH? Any help would be greatly appreciated.