This is my exact same sop, except substitute heatpad for incubator. My pad gets things about 85 or so at room temp.
So I do smaller runs, about 100g at a time for personal use, and I’m finding if I jar everything up at about 50ml of liquid it gives me sea salt sized grains after about 4 days to a week.
My normal return is about 20g total of crystals and hte a run, so that is 20g per 50 total volume of liquid prior to capping generally gives me sea salt.
If you venture outside growing fat rocks of THCa and read about neucleation, you will find that science cannot determine a way to make it happen every time, as an SOP, to yield the same neucleation time. Neucleation is an interesting thing. Controlling the variables makes it happen for us, higher THCa content, temp, solvent content in solution, pressure, seeds or neucleation sites. But due to variations in equipment, solvents, SOPs and material…everyone kinda has to figure out what works for themselves.
I just thought I would add in that this MIT post is really good and gives accurate info…but it is describing how to grow a SINGLE crystal for X-ray crystallography. These methods and techniques are not the best for yield or doing anything really above ~1 g scale. It’s the best way to control single nucleation and growth from the one point so that the chemist can obtain an x-ray crystal structure. I wouldn’t advise for THCa unless you’re doing a crystal growing contest and want to get a single rock.
I wanted to throw this out there. I haven’t done any cannabis processing personally, but I do have a chemistry background.
I’ve had mixtures that were easy to crash out. Often, it would turn to mashed potatoes and you really can’t filter mashed potatoes. The likely reasons were a complicated profile of impurities and isomers.
What did help was fractional crystallization. It didn’t crash out all at once very quickly. Any longer than an hour after the first sign of growth, it was prone to crashing. No matter how hard I tried to control temperature, once it started, I knew I had to start over. It was too difficult to control the physical conditions. After that hour passed I decanted the supernate, reheated to dissolve and repeated until I had 4 separate crops of crystals. These crops could then be recrystallized to refine then even further. It was tedious, but at a large enough scale, I would accumulate enough of each grade to test/use separately. And if I wanted the grades back together, I could just reblend.
This seems feasible to try out with cannabinoids. If your strain is being a pain or conditions are unpredictable, fractional crystallization can refine your mixture in a way so that you can more easily recrystallize to big diamonds.
Thank all of you for the replies! @J12 I have recently gone to smaller jars! And it has worked nicely, although still having sugaring troubles even with the same pour split to jars, 1 lesson learned, do not scrape your tool you use to clean your honeypot, my theory, aeration of the oleoresin causes multiple micro nucleation sites, EVERY JAR I HAVE DONE THIS SUGARS!!
Also thank you for popping in here @J12 all respect to you for your facets you grow, absolutely impressive.
@goodquestion, excellent point! But it does outline the basic principles of the standard methodology used, albeit not for this specific subject, it is applicable.
This gave me the idea to use a bottom heated incubator rather than use oven space, ovens evenly heat the jars, I have noticed crystal growth where the hot air meets the jars, will try to get a picture of this, crazy to see crystals up the side of the jar.
Visualizing the soup that is going on is a fun thought experiment, if the compounds at the bottom of the jar are warmer and can gyrate and be more mobile, then they’re more likely they seem to interact and find each other.
Craziest formation I have seen so far, was the crystalline structures grew across the surface of the terp layer, and it was flat as a pancake across the surface, the crystalline growth grew up the side, the molecules had nowhere to go but out and across the surface, (due to the gyrations mentioned earlier).
Yeah definitely no scrape. I found that out years ago that every jar that i scraped into sugared. to much agitation. I also prefer a honey pot pour out to a spout. for the same reason.
Growth on the edges. Friggan neato, and I have an example where it grew across the surface, im honestly just enjoying toying with it until I have my own little set method.
Has anyone here done side by side experiments on different sized jars (4oz, 8oz, 16oz) for the recrystallization step?
I guess another way to do it would be using 16oz jars and filling to different volumes and see how the headspace affects the crystal growth?
I haven’t gotten into a detailed experiment, but Ive noticed I get a better % recrystallization if I use smaller volumes of my pentane/sugar mix, vs filling a 16oz jar all the way up. Its a pain in the ass because I dont want to have 3000 4oz jars floating around my lab.
Any insights on this would be greatly appreciated.
I have noticed since going to smaller jars, that my growth is a little larger, by spreading it across multiple jars you’re increasing surface area, so as for me it seems that smaller jars are an important move.
The jar size mainly influences the head pressure. Its more in how well your lid sealed. So ive noticed how the solution gets thick when its cold, that makes it harder for the crystals to move and rearrange themselves. Im guessing if we added a terpene as a secondary solvent to the soultion it should facilitate the crystals moving at colder temps which also cold temps speed up crystalization. The solution being more viscous now will allow for the crystals to move at cold temps and will prevent them from sticking to the jar due to the terpene that was added. Check this video out if limonene can weaken the bond of the resin to allow the ballon to pop then it should also weaken it so that it keeps the crystals from forming that sticky layer around them that makes the stick to the jar allowing to freely crash and move around.
I think limonene is too aggressive on thca but honestly haven’t done a side by side with other terps. I was passed down this hint to use beta caryophylene from Columbo labs and have tried a few times.
You can add a few drops to dirty crude and the terps will cut through the garbage and form very clean stones
ive added terps to my collection pot before to improve flavor but it made all my slabs sugar out. Fire sugar for sure but it makes sense now they helped crystalize the oil fast.
even with the same pour split to jars, 1 lesson learned, do not scrape your tool you use to clean your honeypot, my theory, aeration of the oleoresin causes multiple micro nucleation sites, EVERY JAR I HAVE DONE THIS SUGARS!!
