Acetone crystallization of THC-A


#41

Also, I have ~1500g of BHO that has been in the freezer for a looong time but was ran with good quality material that I never got around to working on. I want to crystallize this as well.

What is the limit of material I should have in each jar? I’m concerned with overloading it and getting no crystals.


#42

ive seen both cannabinoid and other crystals with high residual solvent levels not saying this would be lik that just curious what acetone might be trapped in the crystals


#43

I can send some in for testing and find out. I may end up recrystallizing them though to achieve a higher purity and larger size.


#44

yea i was gonna say even if it does leave high levels this would still be useful cause u could do another recrystallization


#45

Have any helpful tips for recrystallizing? Going in blind right now.


#46

i dont have much experience so i wouldnt call them tips but i have read that once its that pure its easier to crystallize in general including a paper were they bought isolate and recrystallized out of ethanol in a seamingly standard way. that wasnt what the paper was about and it was just talked about briefly. if u hav a pressure vessel u could experiment with adding dense co2 as a antisolvent. it wouldnt even be supercritical so standard high pressure sanitary unions could work


#47

reference, or it didn’t happen :wink:

…because crystallizing out of Ethanol is way easier to get past the fire marshal, and Oregon doesn’t have a limit on residual ethanol!!!


#48

tests at a small scale from 94% alcohol and 8 g of vegetable


should I close or open the lid and also should I drop it in the freezer or just on the kitchen counter


#49

for the moment I put them in the freezer with the lid close
sorry for the bad translation ^^’


#50

Your going to have to rotovap the solution until it is at its saturation point. It looks like you have an excess of solvent. I don’t think cold precipitation would be possible. Before recrystalazation it might be a good idea to clean the solution.


#51

pretty green.

did you freeze your material & solvent? Color suggests no.
that was step 1.

the freezer is appropriate. because you now need to winterize it.
which is step 3.

then you need to evaporate it to less than a 1/2 teaspoon to achieve something approaching a super saturated solution. at a guess, that’s around 2ml vs the 250ml in your jar at the moment.

do that after you’ve filtered the waxes out.

once you’ve got it down to 2 or 3ml. then transfer it into a small vial. then wait.


#52

How about taking it to supersaturation while hot, then cooling the small amount of supersaturated solution slowly over the course of a week in a gradual slope.


#53


But what is it? fat ??


#54

Alcohol of any type will denature the proteins known as DNA. This happens faster at room temp. In fact you can see it happen before your eyes if you gently heat the alcohol but you have to watch close when doing this. Seemingly out of nowhere you will see strands begin to unwind into a pretty long hyper thin group of strands. They are white and they sort of roll out over a minute or two when the heat hits right. Then in another minute or two they stop expanding and if under enough heat they then begin to shrivel. They pretty quickly shrivel to a tiny black dot then… gone under heat.

The DNA strands are tightly wound up and the alcohol causes them to unwind which is called denaturing. More heat accelerates this and enough heat then destroys the strand from what I have seen. Normally they unwind into fairly long spindly white strands that tend to clump up. When they unwind they come out of solution.

From the photo it looks like you are seeing the denatured DNA clumping up and dropping out of solution. This is normally a component of the catch all term “wax”. I have seen this for a very long time. It filters out easily pouring through alumina.


#55

If you are recrystallizing, you can try to wash the surface off with cold acetone and a pipette (glass). Hold your dish on an angle and drip slowly at top to allow it to roll over the surface. When you are happy with what you removed, set it back flat again, add a ml or 2 of acetone to redissolve the smaller crystals and the outer surface of the bigger ones.

Collect the surface wash into a smaller dish to see if any crystals remain. You can keep an eye on how much dissolved during the wash this way. And or separate again, redissolve the crystals and pour that on top of the first dish again.

Let it do its thing again. This allows it to seed itself, minimizing losses along the way.


#56

1 tests the butane sample in the freezer

2 same thing but more concentrated

3 tests in 94% alcohol on kitchen counter


#57

so this is not good ??


#58

not to get off topic, but I can’t let that one slide.

DNA is certainly coated in protein in it’s normal cellular state, but it is not itself a protein. Proteins are strings of Amino Acids (20 flavours) . DNA is a (generally) much longer string made up of (4 flavours) of Deoxyribonucleotides. DNA encodes the information for assembling proteins.

DNA definitely precipitates in alcohol, I have no doubt that some of that precipitate could be DNA. However, DNA is water soluble, so I don’t believe it is the majority constituent seen here, because it would not have been extracted with Ethanol, nor I suspect with Butane. I would certainly expect some the ppt seen to be denatured proteins. Again limited by their solubility in either of the solvents mentioned.


#59

After the crystallization is done, what should we do to remove the product from the mason jar and where should put them? My terps are too thick to pour easily.


#60

The crystallization process can be repeated after you pour off the mother liquor and then redissolve the crystals for a second round of crystallization in a process known as recrystalization.