The latest EHO batch, from a nug run. It came out nice and clear, but a little acidic. I made a CRC column using a buchner and cakes of medias(from bottom up: Celite, T-5, T-41, AC, and alumina on top) . About halfway through filtering, the solution was coming out crystal clear, and then the acidity of the T-41 caused a slight orange tint. I had double the activated alumina, but that wasn’t enough to neutralize the acid. Any recommendations on a base to neutralize? Should I use 3x the amount of Alumina?
Edit: I’ve read that AC can pull orange pigments, would filtering through a secondary column of AC on top of DE work?
Thanks in advance. Hope you enjoy looking at the shatter
any sort of LLE washing process Can bring back your ph level if the water in your washes are at the ph you want. It doesnt need to be a brine wash.
Say your extract is a ph of 4, doing a LLE with your aqueous layer having a ph of 7 should bring up your ph. it make take a couple washes to get it back to 7 though. you wanna repeat the wash until the water you are draining out is the same as the water you put in your sep funnel.
I have a feeling though that you dont wanna go to a alkane solvent which is why you are doing your color remediation with ethanol and not heptane or hexane to begin with.
I’ll have to read into LLE as it’s a process I’m unfamiliar with. The concept is simple enough to grasp, but would that work well with Ethanol and water? The 2 like to mix together quite well and separating them can be a chore
Spot on about alkane solvents. Ethanol has a lot less restrictions in my state as a solvent, and I’m more comfortable working with it. CEO really wants to try and keep to just ethanol for the solvent as well
No, LLE involves two immiscible solvents. You’d have to dissolve your oil into a nonpolar solvent like heptane and then mix that with water in a seporatory funnel, reactor, etc. There’s also a way to keep your oil in ethanol and bring it into the non polar layer by adding water. Search “louching” (I think that’s the spelling) if that sounds more appealing.
What scale are you working on? How many grams of oil would you generally be remediating per batch? It doesn’t take much to move beyond the scale where a separatory funnel becomes impracticable for this process.
I extract with ethanol and gave up trying to do color remediation with a secondary solvent because it became tedious and impracticable with the equipment I have. But I have gotten nice color shatter with -80C extraction temp. and very short soak times (<5 minutes) with minimal post processing (just filtering over AC and T5).
For what it’s worth, I think the color of your shatter in the OP is great.
Small scale commercial. I typically remediate 250-400g at a time
Do you have a subzero freezer for -80C? I have a hard time cooling ethanol past -50C with dry ice. I typically do a 5 minute wash myself. Been experimenting with a 3 minute wash and a second rinse though, I may like that method more. I’m going to drop the T-41 next time to try and remove the acid that caused the orange-ish hue
Thank you!! It’s been a long journey to get this far. The color is great, no doubt about that, but I’d love to churn out some product that has that crystal clarity
Not necessarily, no. The longer soaks(even at extreme colds) can still begin to pull undesirable compounds from the plant material, increasing the quantity but reducing the value of said product coming out. The wash time makes a huge difference in the color/shade of the end product
2nd longer soak for distillate is a pretty good idea imo. Sounds like a nightmare trying to track that for the state though, at least for me