THCA extraction, more details

BobCajun

Well-Known Member
I found this forum thread which has a description of one person's experience with THCA extraction. An interesting part is that he mentions trying it with potassium carbonate instead of hydroxide and it failed. Now when I tried an extraction, which I described in a thread here quite a while ago, I used the carbonate and it did work that first time, but I tried it again a few other times and it didn't work, nothing precipitated. Why it worked the first time I don't know, but apparently it's unreliable. Unfortunately I had bought a brand of pH up which used carbonate instead of hydroxide. So now I have to get the hydroxide kind.

Some people may say that THCA isn't worth extracting because it's less enjoyable than regular extracts because it doesn't have any secondary compounds like other cannabinoids and terpenes. However, you could use it to boost the THC content of other Cannabis products. Then it would have the secondaries but just be stronger. Nobody said THCA has to be used by itself.

You can also make a salt of it with an amine and smoke it and the THCA will decarb and the amine separate during smoking, delivering both compounds at once. You could, for instance, combine it with cocaine. Not that I would recommend it, but it would work. You can use any amine type medicine which would be safe to smoke. Cocaine is just a convenient one that comes to mind. Could also be amphetamine or an opiate. While some may find pure THCA/THC boring compared to other Cannabis products, they may like it as part of a combination. Of course I recommend against using illegal amines but maybe some legal ones instead. In a salt form THCA is also stable at room temperature for years, much like salts of ascorbic acid as opposed to plain ascorbic acid. It would therefore be a good form for long term storage.
 

BobCajun

Well-Known Member
A good thing about the THCA extraction is that it works with fan leaves. There's not much else you can do with fan leaves, except maybe make edibles, and even those are pretty disgusting. But with this you get as potent a product as from bud, just less of it, 1-2% compared to probably 7% from trim and 15% from bud.

You could probably just soak ground leaf in hydroxide water, filter it off and acidify. Then if you just collect the precipitate by filtering you would never have to use solvent at all. I'm guessing it would clog paper filters, but maybe a mesh filter would work well.
 

BobCajun

Well-Known Member
Picked up a bottle of Advanced Nutrients pH up. Says maximum concentration by law but doesn't state the percentage. You can figure it out from the weight though, it says 1.4 kg and it's 1 liter so the chart I found says it's about 40%. To get the required 13 pH for THCA extraction I calculate that you would need about 15 ml of the pH up solution per liter of water. That's trying for a 0.1 N solution, 1/10th of a mole per liter, which makes a 13 pH solution. A mole of KOH is 60 g. That liter of 0.1 N KOH would be enough to extract about 100 g of bud, 200 g of trim or 1 kg of leaf in my estimation, with a little extra unreacted KOH.

I know that you can also use lye, sodium hydroxide, but it's actually quite inconvenient to mix solid sodium hydroxide into water. It produces a lot of heat and is hard to get it all to dissolve. So to me it's worth the extra cost to buy a ready made solution, like the AN pH up.
 
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BobCajun

Well-Known Member
I tried extracting some bottom trimmings fresh with hydroxide water. Didn't work too great. When I added acid something precipitated but it turned out to be insoluble in water and alcohol, and didn't melt when heated, just eventually put off a stink like burnt sugar and turned black. So apparently you do need a solvent to pull the THCA out and leave whatever that other shit is behind. Probably best to extract the weed material with the solvent too. Just putting hydroxide solution in with the material makes a dark red solution, with apparently very little THCA in it.
 

BobCajun

Well-Known Member
I may as well show the method for isolating THCA by using an amine to form a salt. What makes this particularly useful is that the only solvent required is isopropanol, which has low toxicity and is available in USP purity in many drug stores. It's a little more toxic than ethanol but not a lot. You'd have to have a few hundred ml in your body for it to kill you. Less than that is just metabolized to acetone, which is also not particularly toxic.

In the first section shown in this image, it describes starting with an existing extract (80% THCA), similar to BHO, but the second part describes starting from plant matter directly. That part specifies CBDA instead of THCA but it works the same either way. So this would actually be good for extracting CBD from hemp, by decarbing the CBDA. Though CBDA itself might prove to have medicinal value as is, like THCA. The amine they use is toxic but you could use any plant alkaloid or low toxicity amine, a natural product being preferable. Dicyclohexylamine happens to crystallize very well as carboxylic acid salts, and is used for purifying carboxylic acids in that way. I don't know if other amines would crystallize as easily from iso. Might need to use a nonpolar solvent for other amines to precipitate. Using a low toxicity amine you could medicate orally with the salt, which is stable in air at room temp, or convert it back to acid form shortly before use for smoking by simply adding citric acid to a water solution to precipitate it, which I assume would work. This is from a patent. I forget which number.

 
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dabbindylan

Well-Known Member
Wouldnt denatured ethynl work better iso is gross solvent even in its high puritys which are not readily available pure iso can only be rotar evaporated n recovered from impure iso which can be bought
 

BobCajun

Well-Known Member
Wouldnt denatured ethynl work better iso is gross solvent even in its high puritys which are not readily available pure iso can only be rotar evaporated n recovered from impure iso which can be bought
Probably would work with ethanol. I guess iso just works better for crystallizing because it has lower solubility. Iso is probably cheaper though. I never bought ethanol but I suspect it would be high priced like liquor. Iso is easy to get in 99% purity too. I'm sure you could use either if you wanted to.

As the amine, I'm going to try phenylethylamine. It's cheap and practically inert. You can buy it in HCL form for about $50 a kilo. I tried about 400 mg and felt pretty much nothing, maybe some slight mood elevation if I really tried to notice it. Another possibility would be synephrine, though it might have some effect on blood pressure. You would have to convert them to the free base form before adding to the alcohol. I don't know if you could notice an odd taste if you smoked the amine salts or not, since I haven't actually done the process yet.
 

dabbindylan

Well-Known Member
Idk seems dangerous n overly technical. Try doin short path distillations with separate filters. Run ur co-solvents or emulsifiers. Then collect. Degas at decent vac n heat. Dont smoke poison. Id like to experiment with more b-limonene but pure turps are expesive. Pain staking to make. Im rambling.
 

BobCajun

Well-Known Member
Idk seems dangerous n overly technical. Try doin short path distillations with separate filters. Run ur co-solvents or emulsifiers. Then collect. Degas at decent vac n heat. Dont smoke poison. Id like to experiment with more b-limonene but pure turps are expesive. Pain staking to make. Im rambling.
No more dangerous than "RSO", which seems to have become the common term for isopropanol/ethanol oil. What's so dangerous about adding isopropyl alcohol, or Everclear/ethanol, to weed, pressing and circulating it around for maybe 10-20 seconds and filtering it off, then adding an equimolar amount of an amine and chilling in the freezer overnight and straining to collect the crystals? It's only dangerous if you're an accident prone person. What's the worst that could happen, you somehow get the alcohol in your eye?

Probably not a great idea to smoke it in the form of the amine salt though. It's just a way to make it easier to isolate high purity THCA without having to use a toxic non-polar solvent, just alcohol instead. By crystallizing the amine salt a couple times you can get purity in the high 90 percents. Then you can store it like that for long periods and when you want the high-pure THCA or CBDA you just add the citric acid.
 
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BobCajun

Well-Known Member
I mentioned synephrine before to make a THCA salt. Reading more about it I found that it's fairly soluble in water, 1 part in 20. That would make it hard to isolate as the free alkaloid, assuming you had to buy it as the HCL.
 

dabbindylan

Well-Known Member
I didnt mean process seems dangerous. Even tho it kinda is. I meant ur finshed smoke. Were try to isolate using less solvent or more naturaling occuring 1s. This process is intresinting tho. Do u have picture of finsjed product
 

BobCajun

Well-Known Member
I made a very small amount of the phenylethylamine salt, like a thimble full of iso extract and a couple drops of PEA free base, which is an oil. Didn't see any crystals after an hour in the freezer, just some slight cloudiness. So I just dried it onto a little weed and smoked it that way. The amine taste was very noticeable and it was less than good. Pretty putrid really. Probably need that special amine mentioned in the quote I posted an image of to get good crystallization.
 

qwizoking

Well-Known Member
You remind me of finsgaggy. Or that sybian dude..Or maybe oilmkr or maybe some other delusional poster
 

BobCajun

Well-Known Member
Limonene extracts tho.
Yeah that might be good as a non-polar solvent. Just not particularly easy to find locally. If only there was a non-stinky terpene. Though orange smell is at least better than turpentine smell. I got sick of that very quickly.
 

dabbindylan

Well-Known Member
Internet u can buy synthetic Limonene. Food grade. This might also help in ur endeavor of chemical isolation..a centrifuge may be handy also?
 
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