That’s some pretty heavy isolate in terms of density.
Here’s a picture of the same kilo I’ve melted down. It’s been over 24hrs and I’m very surprised it’s still liquid form. No crystallization like it should be at this time. Our location is around 70degrees with AC blasting all day/night.
Not impressed with my distillate coming in plastic #5 PP. At least use HDPE2 right? Anyone with plastic knowledge chime in PLEASE!
This depends on what you do with it.
If you let it still in a clean container, and it was well filtered, It can stay in such viscous form for extended time (possibly indefinitely I guess).
I’ve found it to vary a lot from supplier to supplier. Some CBD distillate sugars right up overnight, others will take days/weeks. Haven’t really found any rhyme or reason myself. No real correlation to the CBD content either which leads me to believe the lipids play a role in crystallization more than we would think. Not my forte though.
I’m not convinced it’s lipids either, it’s seems more like wax but I’m not certain.
I do know I have done 3 more batches from various starting material and haven’t dropped below 0c and it’s has all come out clear when diluted in ethanol. Now almost every batch made by freezing the solution into a large slab has come out cloudy in ethanol.
My theory continues to remain that when you drop down to sub zero temps during precipitation you freeze some of those impurities and then when you break apart the crystals you don’t free all the impurities, Or your process for grinding is not breaking up the particles enough. Then when you wash they still stay trapped inside the small crystals, which also give you that slightly less than white or slight yellow color. You can either avoid this by never going to sub zero temps and keeping your isolate in a slurry or finding a way to grind the larger slabs into a fine enough powder to free the impurities. Or make isolate from a cleaner starting material that’s is already free of those impurities.
@Mosaic_Co-Labs FYI this isn’t directed at you, just an observation from my personal experience.
Yes. It can take days or weeks for recrystalization to occur. With distillate, finding fats and lipids is super easy. When it cools you will be able to see some wispy stuff suspended.
@thesk8nmidget no offense taken! If you look back at my post you will notice the beaker on the left in my pics is the isolate I made and is completely clear and free of any cloudiness or contaminants.
My SOP for isolation calls for subzero Temps and I do not have the issue of trapped impurities.
I also use a grinder to pulverize crystals into powder before rinsing at -40C with -40C solvent. So again no offense taken because the only product pictured above on the right is from the Slanger this thread is about.
I was under the impression that under supersaturated conditions the cbd will nucleate first and if the solution is cooled too quickly and too drastically the waxes and fats will come next and inhibit the crystallization reaction by literally coating the nucleation points/seed crystals in impurities
Does anyone have data showing the solubility limits of various fats waxes and lipids in a complex supersaturated solution?
I have a thermal conductivity meter that I’m gonna be getting set up to do some data gathering on a bunch of crystallization techniques and equipment I’ve been working on- seems to be a good starting point but I would love advice on any other detectors or equipment I should have to better stock the data-dump
Fuck sake tho… somebody fund me so I can focus on this and not the menial shit
@Dr_Jebril under what conditions are you seeing fats and waxes come out of mother solution BEFORE cbd nucleates? Genuinely curious as that would be a really really nifty trick - I’ve seen some folks speak of ACN as an anti-solvent in supersaturated alkane solutions that would push fats and lipids out first but I haven’t made time to really dink with it.
I would think ACN or MeOH might work almost like louching cannabinoids from alcohol with water due to the solubility of “the goods” in them but the insolubility of the fats. ACN has the benefit of being more than ever so slightly soluble in alkanes although I wonder if EtOAc would also do the trick
Ethyl acetate? That will increase solubility of cannabinoids in an Alkane solution- we use it in foreword phase to elute cannabinoids from a silica puck
Perhaps I missed your objective: I thought you were looking to crash the lipids from a solution supersaturated with cannabinoids *without" precipitating the cannabinoids. MeOH would be my first choice for such a task except it’s not miscible I’m alkanes (kinda). ACN and EtOAc are the next best things I can think of but if that’s not your goal then obviously I’m not solving any problems lol. Were you just talking about an antisolvent for cannabinoids in NP solvent?
Meoh will extract the cannabinoids but leave fats and waxes and lipids in the alkane, reversing and using an alkane to wash a saturated methanolic solution will pull fats and waxes along with cannabinoids but leave polar compounds and sugars in the methanol
Anyone ever used a differential scanning calorimeter for crystallization studies? Measuring enthalpies of phase change you should get consistent runs for isolate which presence of waxes would alter. I’ve also thought DSC could be handy to quantify fat/wax content in extract solutions
I would think if you add EtOAc it would make the cannabinoids more soluble in the solution but the fats less so. ACN more extremely so. TCM might also be an option
They’re supposed to be immiscible but they’re really sparingly miscible and even a little bit of methanol might make those lipids seriously uncomfortable in alkane