Isolation of THCA

[montroller]

Did you let the polar solution slowly evaporate? If so that would tell me that the real driver behind the process is simply precipitation of a super saturated solution.

This could be tested pretty easily with some boiling ethanol right? I would do the test myself but I don't have any ethanol or a hot plate right now. Looks like I'll be hittin the lab supply store on monday

 

[Daub Marley]

Probably not. If you boil you decarb so you might be able to under vacuum, but I would think the disruption from boiling would not allow crystaillzation. It would need to slowly evaporate. Ethanol also has the tendency to increase its percentage of water as it evaporates and I think this might cause problems with emulsions forming. Im not sure if its this thread but I remember someone posting that a THC-A isolate came from the scrapings on the inside of their chamber. This would make sense because single solvent dewaxing is using cold temps to cause the saturated solution to precipitate waxes which are the first to fall out. If you get too much THC-A in there, too cold, or both it will precipitate THC-A too which is likely what happened, or at least that's what makes sense to me.

 

[Pangea]

Did you let the polar solution slowly evaporate? If so that would tell me that the real driver behind the process is simply precipitation of a super saturated solution.

Basically a definition issue, google precipitation vs crystallization. You can use temp swing to induce it as well or by adding other solvents, but having a properly saturated solution and not super saturated is key to forming nice crystals, instead of a precipitate.

That's a good question. I believe it would. The pesticides would have to be even more similar to THC in crystallization, but I would ask an organic chemist before jumping to conclusions.

Agreed, and if there was some even traces I think because of the purity we could use some common filtration and chemistry methods to clean it up.
It should go without saying they shouldnt be used improperly in the first place, but seems like people are running to distilled to hopefully clean up there crap and if its not working it hopefully this will.

Your posts in this thread have not been follow the leader. You made some interesting discoveries and posted it and we have all been wondering, asking questions, and thinking about it. I love that. I don't like it when people just want something handed to them so they can make money off of it without having done anything. Im sorry if I came off like a dick but I think the bar should be set very high if we ever have any chance of surviving legalization, and sometimes I get discouraged. I just want everyone to be independent thinkers and doers.

For the most part I understand, Ive had similar concerns about the surviving legalization issue, I mean that writings been on the wall for a long time, plenty of time to prepare for that. I guess I have a hard time understanding the basis of your follow the leader vs something else when it comes to extraction techniques or cannabis industry, there can only be so many "leaders" or lead methods.

The question is would you have been better off? If not then don't share it. The thing is by sharing you get questions asked and points made that you might not have ever stumbled upon. Hate to say it but nothing is really earth shattering here. Everything from carboxylic acid extraction to re-crystallization is standard practice in chem labs. I can probably go to any college and ask some organic chem students to do this.

So I guess that sums up your point, if you are better off personally for keeping a secret then dont share it. I know 100% without a doubt I would have been "better off" not sharing this.

There is a reason I posted in this thread to begin with, like I said I was pretty certain of my hunches and did basic research before posting, the only gains I made by sharing were roji sharing the lab that works with mmar patients(cant thank him enough), and by everyone else, including those with a very close beat to the top of the cannabis science community confirming no one else has stumbled across this or even speculated possible.

It may not be earth shattering but it is a significant discovery, did you not know that there are many, many well educated biochemists who have been working primarily or exclusively with cannabinoids for many years. The 20 legal companies in Canada alone are worth several hundred million, with the top few being in the hundred plus on their own, they all employ top scientists.

If I kept this a secret I wonder how long it would take anyone else to figure out how I did it, especially if I only showed or sold recrystallized tetragons or the super pure crystalline powder.
Hindsight is 20/20 seems like a no brainer now but just go back and read this thread for how close people were to isolating thca or even now you are still asking questions and pondering when its all layed out plain as day from my posts, 2 wikipedia pages, 2 youtube videos and 2 science like articles that pop up on the top page of the basic googling terms. Im more surprised no one else had posted pics of crystal since I first posted, im sure more people are on top of it in private now.

Sounds weird but basically I shared because I felt I discovered it specifically because I would not keep it a secret, if I benefit from it monetarily great, if not no biggie its not my primary motivator.

 

[montroller]

Probably not. If you boil you decarb so you might be able to under vacuum, but I would think the disruption from boiling would not allow crystaillzation. It would need to slowly evaporate. Ethanol also has the tendency to increase its percentage of water as it evaporates and I think this might cause problems with emulsions forming. Im not sure if its this thread but I remember someone posting that a THC-A isolate came from the scrapings on the inside of their chamber. This would make sense because single solvent dewaxing is using cold temps to cause the saturated solution to precipitate waxes which are the first to fall out. If you get too much THC-A in there, too cold, or both it will precipitate THC-A too which is likely what happened, or at least that's what makes sense to me.

I was thinking of trying something like this but with ethanol

http://orgchem.colorado.edu/Technique/Procedures/Crystallization/Crystallization.html

I don't think boiling ethanol will decarb that quickly, it's just under 80c and the chart on skunkpharm shows no spikes at that temp. I definitely want to try the technique from that link but maybe ethanol isn't the most ideal solvent. Any better ideas?

 

[Daub Marley]

It may not be earth shattering but it is a significant discovery, did you not know that there are many, many well educated biochemists who have been working primarily or exclusively with cannabinoids for many years. The 20 legal companies in Canada alone are worth several hundred million, with the top few being in the hundred plus on their own, they all employ top scientists.

And probably every single person in those labs can do this. They study things that are far more scientifically complex and remarkable. Most of the time they have to isolate nearly pure cannabinoids to study them.

If I kept this a secret I wonder how long it would take anyone else to figure out how I did it, especially if I only showed or sold recrystallized tetragons or the super pure crystalline powder.

I see THC-A isolates on IG all the time. Its usually not big crystals but if you started showing them off I'm sure it wouldn't take long for the right people to figure out how to do it.
What I meant by follow the leader (and I didn't intend to direct that at you originally) was that we are behind the chemists and we have to constantly keep trying different methods to keep people from jumping in and forcing everyone else out through scale. By following it feed into that because it creates a standardized product in the market and then people start to scale up. By creating you destroy the ability of those with deep pockets to corner the industry.

I was thinking of trying something like this but with ethanol

Ok I misunderstood what you meant. It just has to be hot not necessarily boiling. I work with ethanol in extractions all the time and I have never seen any, but the science seems to say that it should work. If your extract is pure enough and you don't use too much ethanol it should work. Use a dropper to add the ethanol. To find out if all the solute is in solution use a laser to shine through it. If you see the beam then its not completely in solution. Keep adding ethanol until no beam is seen.

 

[Pangea]

All right, I think I got what your getting at with following the leader, I can agree with that.

Admittedly Im not on IG yet, been meaning to but dont really use a cell much. Anyway, I'm sure there are some thca isolates on IG but how many are from column chromatography and or that one sample scraped from inside a closed loop? You say its not usually big crystals? Are there any non micro crystals? The key with the discovery is the ease and scale, scientist can pretty much literally do anything at a small scale in a lab, thats why a gram of pure THCA is worth $100,000CAD from restek. Im sure it would have been figured out and replicated if I didnt share, eventually, but thats all speculative now. And a side note, if your worried about legal future market, just remember that the average acre will produce 300 pounds of THCA, my neighbor knows nothing about cannabis other than the extreme basics, what he does know is how to drive a seeder and combine, he crops around 800 acres of cannabis a year. Once the gates open and the fields filled the price of THCA, concentrates or any cannabis product is going to drop like a rock, worry not about scientist harming your bottom line, the price of a gram of nug run oil will be under a dollar in no time. When the fields are filled.

 

[Daub Marley]

I'm sure there are some thca isolates on IG but how many are from column chromatography and or that one sample scraped from inside a closed loop? You say its not usually big crystals? Are there any non micro crystals?

not of THC-A just clumps of little crystals. I see big shards of CBD crystals though.

thats why a gram of pure THCA is worth $100,000CAD from restek

I think that's based of of purity but I'm just guessing. It gets exponentially harder to get higher purity.

And a side note, if your worried about legal future market, just remember that the average acre will produce 300 pounds of THCA, my neighbor knows nothing about cannabis other than the extreme basics, what he does know is how to drive a seeder and combine, he crops around 800 acres of cannabis a year. Once the gates open and the fields filled the price of THCA, concentrates or any cannabis product is going to drop like a rock, worry not about scientist harming your bottom line, the price of a gram of nug run oil will be under a dollar in no time. When the fields are filled.

I certainly agree with you. I think we have discussed this before in a different thread. I believe there are certain ways to slow or stop the commoditization of cannabis. One key is terpenes because they really differentiate the plants from each other and make each extract unique. You cannot recreate the natural terpene profile from the plant. You can get close, but it will never be right.

 

[montroller]

Looks like I won't be able to do the experiment I posted for a little while. Someone else should try it out and post results. It would only take some ethanol a hot plate and like a gram of BHO.

 

[Gray Wolf]

It seems like the quality of the oil has to do with the purity of the crystals at least a little but I wonder if you could use one of those to seed identical crystals in different BHO, preferably lower grade.

If you could get it down to a process and crystallize enough of the batch for minimal loss it could be a cool final step.

plus the customers would go crazy if you could stock shelves with this
View Image

Do you know the process this was made by? I ran across a sample similar to this, in a batch of non solvent extract judging samples?

 

[Pangea]

Those were made via evaporative crystallization in a non polar solvent, polar solvents so far form a more geometric shape, but this could be due to purity levels increasing with my polar solvent experiments. I'll get some pics of the tetragonal shape soon, they look amazing.

 

[Calilabs]

Great thread! This is what we have been making.

 

[Intoxicus5]

https://www.icmag.com/ic/showthread.php?t=314467

 

[Pangea]

Great thread! This is what we have been making.

Nice! Thanks for sharing! Any thoughts? Im pretty isolated up here so im sure there is much more talk about them around you.

 

[G.O. Joe]

You can use temp swing to induce it as well or by adding other solvents, but having a properly saturated solution and not super saturated is key to forming nice crystals, instead of a precipitate.

Does something happen when winterized BHO is evaporated to before it starts to solidify, then is slowly cooled, maybe to dry ice temperature, and allowed to stay there undisturbed for a few days or weeks?

 

[Pangea]

I bet it would, just the cooling itself would promote nucleation and could be furthered with controlled evaporation over time or more cooling. I havent been able to do much tinkering with this for the past month or so other than just growing more seeds, but plan to take the next step shortly.

 

[weedaholic721]

This thread has come a long way lol..my question now goes back to my original posted method. Pangea do you think that using the a/b extraction to gain a more pure starting material to then use your slow evaporative recrystallization would allow for more consistant growth of crystals or do you think impurities are allowing the crystals to form?

 

[Pangea]

Tricky question, hard to speculate, but if I did I would say it wouldnt really matter, and theres more of a chance it would negatively effect the process, maybe not in the end result but in terms of process complexity / steps involved. There are a few key factors to balance for consistent seed growth, purity of THCA is one of them, but to further concentrate it will effect the other key factors which will make rebalancing more difficult or redundant than if not.

*remember this is not yet recrystallizing, but seeding.

 

[Daub Marley]

Pangea do you think that using the a/b extraction to gain a more pure starting material to then use your slow evaporative recrystallization would allow for more consistant growth of crystals or do you think impurities are allowing the crystals to form?

Higher purity=higher yield
You can always recrystallize to purify, but each time you take a hit in yield. The question really is does a/b extraction yield more? Or if the yields are comparable then how much work does each method take?

 

[Roji]

this is so interesting to me. Love this thread.

 

[Old Gold]

It really is! I'd been meaning to work an A/B extraction and post hopefully succesful pics for this reason for some time now. I got held up by a leaky sep funnel and countless other projects.

From what I understand, carboxylic acids form stable salts in basic solutions. Weak or strong base. Phenols however, will only form these salts when reacted with a strong base, not a weak base, such as sodium carbonate or bicarbonate.

In my original attempt, I used sodium bicarbonate to wash an organic layer of dissolved bho from live resin.
I originally did not realize that the carboxyl group sits right on a phenol ring in THCa. Given that I was unable to recover anything beyond a slight yellow oily residue, and nothing precipitated out of the water with added HCL (and then excess), I believe I separated my intended molecule, removing the carboxyl group from the phenol. Expertise opinions?

I have a jar full of NaOH wash and nonpolar that I need to separate.. I believe it'll work.
Then I'll get to work on recrystallization.

Great thread you guise. Stay innovative.