Slow growth of mono crystals is observable without water but they’ll generally grow into the side of a dish as they’re growing and end up imperfect. Some people have really solid ways to avoid that
I hadn’t thought about the THCa being seeded by or growing with deprotonated THCa. I don’t think that’s happening because so little would be in the water when compared to the heptane
I was thinking more of an interface structure with COO-- sticking into
water,a specialized monolayer induced by water, setting up a crystallization platform in hexane side…? or in similar configuration, pair bonding with the submicromolar Ca++
leaching from glass…wild stuff! Does the water interface act as a “crystallization catalyst”?
Yes, the sidewall phenomenon, is simply another interfacial surface. …
Can you substitue a teflon flask for glass?
Thanks in advance, and a very nice piece of work.
Heptane is easier to deal with in a laboratory environment at around 70-90f.
What we would normally do is suspend the oil in an ideal amount of heptane. Some amount where very little THCa will want to hang around in it but there will still be a nice mother liquor of heptane for the pigments to trap into
On top of that heptane solution you can add pentane and then allow it to evaporate slowly
You can also add other solvents to the mixture to effect the crystal shape. I would probably seed using crystals grown in a pentane mixture with ethanol
Step 1:
Use a mixture of heptane pentane with a cosolvent that encourages THCa to grow as needles and with longer terminations
Step 2:
Seed a mixture of heptane and pentane with the seeds from step 1. Grow big clear diamond shapes that aren’t just the normal heptane blocks
I’ve been enjoying the growth of the thread! I thought I’d share a quick video of some work using this tech and big thanks to Alex Siegel for sharing all the information here for us all👍
I have a pentane / ethanol jar going. I’m thinking of adding it to a flask with stir bar and a dry ice cold trap and regulating vacuum to slowly saturate the mixture while keeping the solution cold
Clearly the pentane or heptane saturates with water over a weeks time course.
You mention adding EtOH to pentane 10% to enhance needle like crystals…
some sort of antisolvent?
Have you tried saturating the alkane with water first…then layer that on water?
Or are we talking layering MgSO4/Na2SO4 “dried” solvent-solution layered on water.
When THCA drops out of terp laden sauce…that is an incredibly impure solution…
so ther must be something catalyzing the crystallization step…
Here you stress “it works best for pre-purified THCA” …any thoughts about this?
but I see photos of crystalline material that looks like the Na+COO-R salt form as well.
any comments? No one seems to point out these obvious two types of preparations.
Have you ever done a LLE of the pentane solution with distilled water, let it settle
and measure the pH of the water phase?
So when people say they extract with butane…I am not sure what it is they are extracting
becasue no one knows the state of the of the THCA in the Trichome vacuole.
We’ve done a trial where after setup (THCa, heptane, pentane layer on top of a water layer) then shake. Shaking mixes the two together and seemed to leave some water in the top layer. It was cloudier than normal but mono crystals formed in that solution better than any other, now that I think about it.
So those of you doing this in mason jars and also have a way to remove the water from mother liquor later, maybe try shaking the mixture before letting it sit. I would not try this with ethanol in the mixture because you’ll probably lose some of your alcohol to the water layer
Crystallizing with terpenes and other impurities is more difficult. Slower and lower yields so I would recommend doing this as a recrystallization of already crystallized THCa or use very pure crude that was going to crystallize on its own
I think the crystal shape here is more about the geometry of the surface it’s growing on, nothing more. Are you suggesting that the THCa could be entering the water layer then recrystallizing at the interface? I think it’s far more likely we’re just seeing a physical effect nothing chemically changes
The THCA synthase is excreted into the extracelluar lumen…that means CBGA is also
excreted. The synthase likes to work in aqueous environment at pH 5.0.
At this pH the cannabinoic acids are 99:1 ionized. So I would "assume ’ the speicies loaded into the catalytic cleft is ionized. Since the surrounding milieu is probably a monoterpene
solution of hydroxlyated terpenes acting somewhat as a detergent in some-sort of “aqueous
environment” I would expect Na+and Ca++ ions everywhere. In fact, Ca++ is known to be pumped into plant vacuoles. I do not know how butane solubilizes
THCA or what form THCA is in , in the trichrome. (read the above papers for reference)
Your post is most interesting because it brings the Cannabinoid Alkane Solution/Extract into direct contact with water!
Example:
In their patent on CBDA methyl ester, Mechoulam et al. synthesize CBDA as a precursor to the methyl ester step. CBDA synthesis below:
Synthesis of Cannabidiolic Acid (CBDA):
A mixture of Cannabidiol (CBD, 314 mg, 1 mmol) and 2 molar solution of Magnesium Methyl Carbonate (MMC/2M, 1.5 ml, 3 mmol) in dimethylformamide (DMF) is heated at 130° C. for 3 hours. Then the reaction is cooled to 0° C., acidified with 10% hydrochloric acid and extracted with ether. The organic layer is washed with saline, dried over the drying agent magnesium sulfate (MgSO4) and then evaporated. The crude compound is then cleaned by column chromatography (20% ether-petroleum ether)."
In regards to this posting, look closely at the 1.) acidification step prior to extraction in to ether. They are using 10% HCl which is pH= -0.5. (minus emphasis)
If you want the carboxylic acid in H+ form…this is how you do it.
2.)Then in a second step they back wash the ether with sat’d NaCl before evaporation.
second step confuses me a bit, but it is possible that it is an ion exchage step.
I’m trying to look as this ??? on going.
Comments?
Love it! Always want to play whit water. I want to try this water layer tek with my diethyl refined crude mixture, the dieth carryer a lot of water…and they act as a antisolvent. Before i dry the solution sometimes is very cloudy.
When the solution is very wet, aprox 70%crude 30% solvent, if i seed in this moment start crystalization in the moment.
Sooo lets do some test.
Are you thinking we should acidify the mixture? Sorry I’m trying to keep up with where you’re taking this!
I’m not sure what the acid’s function is in the methyl ester synthesis beyond neutralizing the leftover magnesium methyl carbonate and making sure the CBDa methyl ester is protonated. The ether solvent will then be able to extract it more effectively from the mix if it is in neutral form.