Refining THCA Isolate?

Hash and Stuff Crystallization
1

Hello all!

I’ve tested a method and was able to separate THCA from the terpenes. But now I have these wierd looking crystals. So I attempted to further refine and recrystallize using heptane but wasn’t successful. I essentially dissolved 5 grams of the thca into a small amount of heptane, then put it in the freezer over night. I had hoped it would have recrystallized overnight but there wasn’t any solid formations, just a gel like substance. So I filtered it through a coffee filter but now I’m not sure what to do other than evaporate the heptane.

Does anyone have any experience in further refining THCA for clarity and size of diamonds?

1231190954
12311909543492×4656 4.17 MB

2

You’ll want to use cold pentane to wash them clean.

2 Likes
3

Dissolve in cold pentane then let sit at room temp for a while, then put in fridge, then freezer

2 Likes
4

What’s a good ratio of pentane to thca?

5

Patience grasshopper…

If you want to grow large crystals rather than have powdered isolate, expecting it to happen overnight is your problem.

Large crystals need to be grown. Quick precipitation will always give you powder.

What is your goal?

How much have you read on “diamonds”?!?

3 Likes
6

Yeah I suppose I am rushing it. I’ve been trying to get clear diamonds that are between the size of bb’s and peas.

I’ve read a bit but everything is so inconsistent. Everyone’s teks are different. Results are varying. I’ve tried so many different methods. I still don’t fully grasp supersaturation.

7

That’ll probably be the place to start then!

1 Like
8

Off topic but hypothetically you could use thca isolate to stabilize slabs. Anyone tired ?

3 Likes
9

Would take a lot. You’d be wasting bunch thca isolate imo. But if u had tons probably the most fiesable idea yet

10

I feel like that would do the opposite thing, make it forcably sugar

2 Likes
11

if you managed to get it all dissolved, it would absolutely work.

in practice, I suspect @Krative is on point.

see seeding.

2 Likes
12

Aahhh, so if by some wild chance you were able to get it to fully dissolve you’d get the stability… Heat gun? Try not to decarb shit?

13

have you considered playing with sugar water till you do?

it’s cheap, so you can set up a hundred jars at once.
you also can’t accidentally decarb sucrose…

dissolve as much sugar as you can into a given amount of water
let it cool…at this point it has become super saturated.
drop in a single sugar crystal.

make ten jars the same way. don’t add the seed crystal
wait. notice there is variation in how long it takes to see crystallization.

7 Likes
14

I’ve never had joy using a heat gun to “desugar” more than a couple of grams. you want way better temperature control than that…

and even then it’s not a given. see What's the melting point of THC-A?

1 Like
15

I saw a really cool heat gun at my buddies place the other day that had digital temperature control and you can set exact degrees for it to come out. Still, you’d have to get the wax to melt and act as a solvent for the THCa if you’d want to melt the THCa without decarbing it. The melting point of THCa on its own is waaaay too close to it’s decarb temp.

1 Like
16

Rapid Isolation of D9-THCA-A - Wohlfarth 2011.pdf (629.5 KB)

3 Likes
17

What does the addition of 0.1% pyridine to the mobile phase do? @TheGratefulPhil

1 Like
18

https://digitalcommons.lsu.edu/cgi/viewcontent.cgi?article=4792&context=gradschool_disstheses

Long ass dissertation on the increased solubility of hydrocarbons in mixed solvents. Pyridine and Cyclohexane are both solvents being studied in this paper.

To be honest I have no clue, but my best guess would be that it has something to do with making adsorption and elution more energetically favorable.

Whatever it is…if it gives a 99.8% pure product, it’s worth it

2 Likes