Isolation of THCA

Pangea · Sep 18, 2015

I was able to ramp it up and get a melt point, only took some pics at the 115c mark to show they were still stable and solid.

They melted at 135c, almost double the cited 70c, wtf.

Slow bubbling started at 140c, it solidified quickly when cooled, and seems to powder the same as pre melt.

Anyone with a HPLC hookup in Canada?

Daub Marley · Sep 19, 2015

Pangea said:
Anyone know how Horatio's making his isolate?

Column chromatography.

G.O. Joe · Sep 19, 2015

Pangea said:
Yeah im not saying its distilled

There are posts before mine about distilling THCA.

Pangea said:
I was able to ramp it up and get a melt point, only took some pics at the 115c mark to show they were still stable and solid.

They melted at 135c, almost double the cited 70c, wtf.

THCA will not melt that high. It could be one a lot of odd things - anything but THCA.

Pangea · Sep 19, 2015

Any guesses? What are the options it could be in this quantity of concentrate?

Heres an album showing 1.2g of em and the 115c temp shot.

http://imgur.com/a/wylf0

mofeta · Sep 19, 2015

Pangea said:
Any guesses? What are the options it could be in this quantity of concentrate?

Heres an album showing 1.2g of em and the 115c temp shot.

http://imgur.com/a/wylf0

I don't see a pic of the mp?

What method are you using to determine the mp? Unless you are using one of the standard ways, like a cap tube in oil, it is very easy to get a result that is way too high.

This is very interesting. Thanks for posting this.

Pangea · Sep 19, 2015

No pic of the actual melt point, just was able to get one during the heat up at 115c, took another half hour to ramp it to 135 as I was doing other chores.

I probably should have googled actual methods, I just used a pot chamber with some parch and put it on a sand bed hot plate to determine its "melt point" Just have a distant memory from that scene in Blow where they do a melt test to go from

My pleasure :tiphat:

thanks for the tip!

Pangea · Sep 19, 2015

Got a hook up(thanks!) to a pro lab with uhplc, looks like we'll get it figured out soon!

thegreenman91 · Sep 20, 2015

Can't wait! Please deliver!

Sam_Skunkman · Sep 20, 2015

What does it taste like?
100% Pure THC has little to no taste or smell even directly on the tongue, do these have a taste?
So it has zero smells like hash or Cannabis? No terpenes?
I am curious. Looks interesting.
-SamS

Pangea said:
If I had to put a wager down, Id say the terpenes are precipitating the thc or thca. Anyone know how Horatio's making his isolate? He's playing with terpenes a lot, wouldnt be a stretch to imagine he's stumbled across the same thing.

All the talk about nucleation, isnt that the first step to crystallization?

Either way, I dont know what my crystals are, but more tokin science has been done, I dont want to say its got a lot of butane in it anymore, I suck at tasting residual butane, but yesterday smoked quite a bit of it and didnt notice any of the taste I thought I did previously. It hits very hard, weak knees had to sit down hard, from 35mg.
ps: that large crystal ended up 18mg cleaned up.

Pangea · Sep 20, 2015

I was asked about the taste yesterday on a different site as well, it has no discernible taste or attributes, no smells either.

Based on its effects, if its not some form of THC i will be surprised.

I am trying to limit my sampling of it, after a day of heavy consumption of regular cannabis products and building of tolerance, a 50mg toke hits so very strong if you were standing up without a tolerance you would wake up on the ground.

Pulled out some more 20mg honkers, they really are big, these things gotta be more precious than any diamond.

Also, I have started a few very basic experiments to recreate them.
Another uncontrolled storage vessel from a few days back with a different batch is already nucleating in a similar manner. I have also looked at an unpurged thin slab which is around 10months old, it has developed some small crystals of about 4-5mg in size in certain area's of the slab, with no regular "waxing" nucleation present.

weedaholic721 · Sep 21, 2015

Very interesting pangea..seems like your conditions are similiar to crystalizations methods and your pictures show that something indeed crystallized..cant wait for the lab results..thank you for sharing

Pangea · Oct 3, 2015

Came back at 94.606% Cannabinoid Acid, 1.4% Decarbed. Mostly THCA with CBGA, THCVA, CBCA, and CBDA.

Ive managed to recrystallize a small amount in Etoh+H2O, it formed a 6mm long tetragonal with end pyramids, about 2mm wide and .5mm thick, its a near perfect form and shape minus small precipitate surface contam. Ive also managed to come up with a method to easily purify the crystals further but have to send out sample of that for analysis before further comment, the end form of it is a crystalline powder not large single crystals, but if the powder is pure should make it easier to recrystallize.

Pretty interesting going over it all and having it all click together, from all the nucleation talk, father earths microscope pics of crystallization, and the one dude posting about pseudopolymorphism, and how it all relates to the purging process and the various forms of concentrates, to now being able to grow single large pure cannabinoid crystals.

The largest ones are 1/4ct. What is the value of such a product? I'm not so sure the big singles should be consumed more rather admired like jewelry, but now that ive "spilled the beans" I would expect other folks are going to do their best to make it not that much of a rarity. Obviously not as pure as a analytical sample(yet)but those are worth $100,000per gram, and are not pretty to look at, nor easily get you high.

If any producers in Hawaii are interested in hiring a crystallizer consultant for the winter Id be interested in that.

montroller · Oct 3, 2015

Thanks for coming through on those results! I wonder if you could use a little bit to try and seed larger crystals.

I also found another guy who had something similar show up in his "live resin"

Pangea · Oct 3, 2015

Yes ive got a few different micro scale growth from seed experiments, just wide parameter type thing, but so far have managed some good success all things considered.

The pic happens often, any common form of carboxylated oil is primarily a type of crystal form of cannabinoids, from sugar wax to shatter to large crystals its just a different way of cannabinoid crystal forming when dropping out of the solute.

Cool side note: the purified powder has a lot of suface area, 30mg fills 1.5ml vial if shaken, if tapped down it will only fill 1/8 of the vial.

montroller · Oct 3, 2015

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 :biggrin:

Daub Marley · Oct 3, 2015

1.The terpenes play a role by providing decreased viscosity and allow the cannabinoid acid molecules to become mobile and crystallize with each other.
2. Terpenes are also acting as a solvent and as they dry out they are precipitating more cannabinoid acids.

It's likely that these two functions work together to grow the size of the crystals, but I'm not sure how much each one contributes to the effect. Thoughts?

montroller · Oct 3, 2015

Also Pangea mentioned that these formed in unpurged oil which would allow the cannabinoids to travel through the oil more easily. So maybe it can be done with oil that isn't terpy if you just have it in a solution of some kind.

Daub Marley · Oct 3, 2015

Agreed. I would only speculate that in order to reproduce large crystals like this the solvent would need to have similar properties to the terpenes ie very non polar, and evaporates slowly.

Pangea · Oct 3, 2015

For sure the terpenes play a role, but I do not think they are necessary or key to larger crystals, they evap much slower than saturated butane so the effect they have on the formation is paramount if dealing with a reg solution. The polarity issue is one ive been wondering about, but I have formed nice crystals with polar solvents as well. The same parameters and methods of basic crystallization techniques follow true to cannabinoids from what ive seen and read, meaning the keys are; time, evap speed and saturation level.

I have little to no doubt very very large single crystals will be grown, first to a kilo gets a prize.

One of my main question is about pesticide contamination, seeing as how distillate is not removing those contaminations I wonder if crystallization or different recrystallization techniques will do the trick, for consumers sake it would be nice to be able to buy a product that inherently excludes such contams with the peace of mind that it doesnt have poisons in it, unregulated analysis is not up to par. I have a wager that cannabinoid hyperemesis syndrome is a result of pesticide consumption not cannabinoid overdose.

@daub
I cant help but remember this recent post of yours:

I used to really help people, but they just take advantage of me. There is absolutely nothing to gain by giving you the process. Nobody gave it to me I just used my brain and a little experimentation to figure it out. Along the way I figured out lots of things and I hope you do the same and find your own way to do it. Nothing is to be gained by following the next person. That's why everyone uses the same stupid system and there's a thread about how to make this stuff because believe me, people should have found it 10 years ago.
Instead of having an open sourced method of information sharing and (building) the model is now everyone follow the leader. I feel sorry for you guys that have attempted to build a living off this model. I am stupid. I only know very basic chemistry and I am lightyears ahead of most people. When cannabis becomes legal the qualified chemists that currently don't want to risk their career are going to skin us alive

How do you view my sharing of this vs not? Are the question your asking taking advantage? Not gaining anything by following along? Would we have been better off if I kept it more hush hush and let people figure it out on their own? My wallet would be better off short term, but probably not the community.

Daub Marley · Oct 3, 2015

Pangea said:
The polarity issue is one ive been wondering about, but I have formed nice crystals with polar solvents as well.

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.

Pangea said:
One of my main question is about pesticide contamination, seeing as how distillate is not removing those contaminations I wonder if crystallization or different recrystallization techniques will do the trick

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.

Pangea said:
How do you view my sharing of this vs not? Are the question your asking taking advantage? Not gaining anything by following along?

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.

Pangea said:
Would we have been better off if I kept it more hush hush and let people figure it out on their own? My wallet would be better off short term, but probably not the community.

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.

Isolation of THCA

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