We currently winterize down to -10f in Methanol with a ratio of 5-6 to 1. It seems as if 0f is sufficient, I base this off of not seeing fats come over during distillation. How ever, I took a sample of the Methanol/Crude and dropped it down to -79 ish an saw something falling out. Doesnt seem to be Fats, lipids, or waxes as the distillate is beautiful and shows no signs of fats being present.
Any ideas what could be dropping out, CBD maybe?
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After distillation, when winterizing I have come across a clear gelatin like precipitation. However, at a 5 to 1 ratio and -80 I could imagine cannabinoids crashing out
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Might be DNA, If I didn’t loose the files I’ll post DNA isolation protocols.
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It didn’t seem to be fats. by the time I poured it into the Buckner and filtered it trying to catch it, it had redissolved already.
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Right? I was thinking to myself, is the methanol fully saturated at -80 and crashing out cannabinoids? This would make sense I think, since during filtration is warming and redisolving
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I’m not sure how much it changes with temperature but the solubility of cannabinoids in MeOH is pretty high (higher than EtOH I think). That being said, adding water to EtOH to make it more polar can certainly cause cannabinoids to louche especially at low temperatures and MeOH is more polar than EtOH already. 5:1 is a pretty concentrated dilution already. Does the precipitate look like oil in water?
Seemed to be more flaky. Looked just like fats. Kind of a light brown ish.
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What’s the extraction method? Sometimes we get some nasty flakey looking stuff from our warm alcohol extracted material with the emulsion layer during hep/MeOH LLE. The stuff likes to stick to the glassware/sight glasses. I suspect it is either “gums”/phospholipids. Not sure what their solubility would be like in the low temp MeOH but I’ve never run that concentrated or that cold before
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Warm Hexane to raw then hot filter in methanol followed by a cold filter once we reach at least 0f.
What ever it was that fell out didn’t start falling out until I got past -60.
I wonder if you’d get more of it if you went even less dilute or added a bit of water. Probably academic if you’re getting good results without having to go to cryo temps but you know what they say about curiosity killing the cat: satisfaction revived it
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Dude that’s the truth! 6-1 down to 0f always does the trick but we didn’t want to freeze a small sample over night so we just dropped some dry ice into Acetone and made a cold bath to sit a jar in. That’s when we saw this. If it’s a day it doesn’t come over in the short path. Wonder if it’s a terp falling out.
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Not gonna lie, winterizing with MeOH is like an easy button. When we deal with really fatty CO2 crude it’s very apparent how well it works because it’s a real bitch getting the fat to dissolve even heated with agitation. I imagine warm hex makes for a hell of a lot of fat though
Thinking about it, I’m pretty sure you’d crash some cannabinoids before any terps just from experience louching in ethanol but it’d be cool if it was a terp
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Yeah man it’s the best solvent I’ve tried so far. The Hexane isn’t bad we usually see about a 20% loss when winterizing.
20% mass or 20% yield? We see almost no yield loss with 7:1 using 90% MeOH/10% water
Mass loss. If I put in 100 I get back 80 pretty consistently except for that Stormy Daniels strain it was full of fats.
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I haven’t don’t potency testing on the fats from methanol winterization but ethanol used to hold 12% by mass in the fats.
That’s actually not too bad, we’ve seen some 50% fat stuff when we run high pressure CO2 (15 ksi+)
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I saw pretty close to that with Stormy Daniels, if I remember right it was around 47%. I thought I messed up so I went back and winterized 75 kilos of straight fat and only got a kilo out of it.
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Lol yeah I’ve been there. Fucking laughed my ass off once because the alcohol was coming through the filter nearly translucent when we rewinterized a some filtrate we were sure had been botched
Lol that’s how we learn!
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