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Old 09-07-2017, 09:39 PM #1
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Isolates, HTFSE, HCFSE, Solventless THCA from Rosin, Etc

Hey folks, long time since I've been around,hope all are well! I was wondering, how are these different products being made?

THCA/CBD Isolates (from distillate)
& THCa from rosin this one intrigues me the most!!
HTFSE (high terpene full spectrum extract)
HCFSE (high cannabinoid full spectrum extract)

How are these done? Any of them, I would love to learn how as these are becoming staples in the current industry.

The part that trips me is the full spectrum part, supposedly runny/ saucy live resin is not full spectrum even though it appears to sometimes separate as well.

the supposed expert in this is @Extractioneering on instagram, he claims that this is totally different from a runny live resin extract in that is doesnt use fresh frozen plants (which I definitely thought it did...) also that its extracted from cured dry material and that it separates a certain way in the vials over long periods of time crystalizing the THC (it collects on the walls of vial its in, not top/bottom separation like you'd normally see in a jar). This process occurs over a 1-2 week period separating out the high terpene and the high cannabinoid portions.

I have tried this along with live resins and although the live resins were still up there in terms of flavor and smell (hard to tell a difference after a certain point lol) the potency and loudness of the HT/HCFSE was def on another level...The incredible depth in the smell, the sours, the creamy, the gassy, diesel tones, a sweetness ill never forget, the smell and way it looks is even incredible.

Isolates are cool better than distillate IMO but still I dont like them personally THCa and CBD are the ones Ive had. Would love to know how any of these are made. I know this isnt just a simple answer but its been blowing up lately and I had to ask. The THCa solventless method is crazy to me as Im a rosin freak so would love to hear more on this is anyone has some tech/jewels to drop.

All the best Amigos!
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Old 09-07-2017, 10:19 PM #2
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CBD will crystallize when decarboxylated (CBDa still seems to be in question). THC will not crystallize when decarboxylated, but it's carboxylic acid form, THCa, will crystallize. So THCa from distillate is not possible, as too much heat is involved. It has to do with the location of hydrogen bonds on the molecule I'm pretty sure.

High enough purity of CBD distillate, and the crystals will naturally form. You can assist this by washing the impurities with a solvent, probably cold, or by letting the distillate sit in the right amount of solvent (see my explanation for HTFSE below for more on that technique)

THCa from rosin is most likely re-pressed at a low temperature, through a very fine micron filter (hard to say what exactly - as I don't ever really play with rosin). The best material probably comes from super nice dry sift. I'm sure someone with more experience can chime in on that.

HTFSE and HCFSE are ideally fully dewaxed hydrocarbon runs left for crystallization. Crystallization can be achieved in multiple ways, including centrifuging, pressurizing, agitation, freezing, or just letting it sit at the right temperature and slowly evaporating. The liquid terpene layer acts as a solvent (along with the actual hydrocarbon solvent of choice) to slowly evaporate, growing crystals in turn. They also help to "wash" the crystals clean of impurities and pigments - washing a product with solvent is common practice in recrystallization chemistry.
You can pull it off without dewaxing, but it is more difficult because terpenes, cannabinoids, cartoenoids, phospholipids, etc are all very soluble in fatty acids and lipid structures, so separation is nowhere near as clean.

Hope that helps. I'm sure there are other methods to even go about what I've described.

Last edited by Old Gold; 10-31-2017 at 08:35 AM..
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Old 09-08-2017, 01:07 AM #3
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When extracting with CO2 many people do a "terpene run" first, which is a short 15-20 min extraction at subcritical pressures and low temp. You collect the terpene fraction from the bottom of the vessel, but often a coating of THCa is left on the vessel walls and scraped out.

Various chromatography methods can yield THCa and pure CBD. People with $$$ likely using preparative RP HPLC, preparative super critical fluid chromatography, or RCPC.

Lower cost (and lower throughput) method: run dewaxed extract through a normal phase DCVC column with high loading volume, using step gradient elution with heptane/ethyl acetate, collect cannabinoid fractions. Then run a C18 column with acidified MeOH/H2O to resolve the individual cannabinoids. If you need absolute purity run a size exclusion column after.

As Old Gold said, THCa from distillate is impossible. Haven't seen THCa from rosin yet...

Some of the most terpy and potent extracts I've made are just live resin runs with ultra cold 100% propane, purged below room temp.

Some people define "full spectrum" as a extraction with an aggressive polar solvent that extracts every compound out of the plant, intended for edible consumption. What is your definition of "full spectrum"?
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Old 09-08-2017, 07:14 PM #4
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https://youtu.be/NudRsTb4sb0

By the time you get to the end of the video you'll know in relative detail the most efficient process for producing THC-A and CBD-A crystals.

My take is you spin up gushy, flower top BHO in a centrifuge, and the crystalline THC-A and/or CBD separates out. Temperature probably comes into play along with the spin up.

The Guild swears in a festival video interview, "no solvents, acids" were used, it has to be something as simple as a centrifuge.
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Old 09-09-2017, 02:58 AM #5
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very helpful thanks so much for the great info! Really helpful actually...
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Old 09-09-2017, 03:00 AM #6
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Quote:
Originally Posted by Old Gold View Post
CBD will crystallize when decarboxylated (CBDa still seems to be in question). THC will not crystallize when decarboxylated, but it's carboxylic acid form, THCa, will crystallize. So THCa from distillate is not possible, as too much heat is involved. It has to do with the location of hydrogen bonds on the molecule I'm pretty sure.

High enough purity of CBD distillate, and the crystals will naturally form. You can assist this by washing the impurities with a solvent, probably cold, or by letting the distillate sit in the right amount of solvent (see my explanation for HTFSE below for more on that technique)

THCa from rosin is most likely re-pressed at a low temperature, through a very fine micron filter (hard to say what exactly - as I don't ever really play with rosin). The best material probably comes from super nice dry sift. I'm sure someone with more experience can chime in on that.

HTFSE and HCFSE are ideally fully dewaxed hydrocarbon runs left for crystallization. Crystallization can be achieved in multiple ways, including centrifuging, pressurizing, agitation, or just letting it sit at the right temperature and slowly evaporating. The liquid terpene layer acts as a solvent (along with the actual hydrocarbon solvent of choice) to slowly evaporate, growing crystals in turn. They also help to "wash" the crystals clean of impurities and pigments - washing a product with solvent is common practice in recrystallization chemistry.
You can pull it off without dewaxing, but it is more difficult because terpenes, cannabinoids, cartoenoids, phospholipids, etc are all very soluble in fatty acids and lipid structures, so separation is nowhere near as clean.

Hope that helps. I'm sure there are other methods to even go about what I've described.
Wow a huge help, really seems like you have a great understanding of this . Thank you for helping me understand it a bit more than I did yesterday. Really interesting stuff.
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Old 09-14-2017, 07:55 PM #7
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Quote:
Originally Posted by Old Gold View Post
CBD will crystallize when decarboxylated (CBDa still seems to be in question). THC will not crystallize when decarboxylated, but it's carboxylic acid form, THCa, will crystallize. So THCa from distillate is not possible, as too much heat is involved. It has to do with the location of hydrogen bonds on the molecule I'm pretty sure.

High enough purity of CBD distillate, and the crystals will naturally form. You can assist this by washing the impurities with a solvent, probably cold, or by letting the distillate sit in the right amount of solvent (see my explanation for HTFSE below for more on that technique)

THCa from rosin is most likely re-pressed at a low temperature, through a very fine micron filter (hard to say what exactly - as I don't ever really play with rosin). The best material probably comes from super nice dry sift. I'm sure someone with more experience can chime in on that.

HTFSE and HCFSE are ideally fully dewaxed hydrocarbon runs left for crystallization. Crystallization can be achieved in multiple ways, including centrifuging, pressurizing, agitation, or just letting it sit at the right temperature and slowly evaporating. The liquid terpene layer acts as a solvent (along with the actual hydrocarbon solvent of choice) to slowly evaporate, growing crystals in turn. They also help to "wash" the crystals clean of impurities and pigments - washing a product with solvent is common practice in recrystallization chemistry.
You can pull it off without dewaxing, but it is more difficult because terpenes, cannabinoids, cartoenoids, phospholipids, etc are all very soluble in fatty acids and lipid structures, so separation is nowhere near as clean.

Hope that helps. I'm sure there are other methods to even go about what I've described.

Mobin gave me this short path distilled oil a few months ago. I went to finish off the little bit in the silicone container, and it had somehow turned to shatter. At room temp (75F) I can pick it up, smooth hard surface, it tings when touched with a dabber, and you can see the cracks in the microscope pics.

Was this a second pass Ben?
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Old 09-14-2017, 08:53 PM #8
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Quote:
Originally Posted by SkyHighLer View Post
Mobin gave me this short path distilled oil a few months ago. I went to finish off the little bit in the silicone container, and it had somehow turned to shatter. At room temp (75F) I can pick it up, smooth hard surface, it tings when touched with a dabber, and you can see the cracks in the microscope pics.

Was this a second pass Ben?
i see it's good and oxidized now

iirc that was the last parts of a d9 fraction chased out of receiver with some hot air, 2nd pass but no treatment other than distillation.

i told you i make distillate that shatters at room temp hahahah

polymerization aided by the phosphitides and other shit normally removed in degumming processes or by sorbants, steam, etc.
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Old 09-28-2017, 08:24 AM #9
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ive attempted making full spectrum and gotten some decent crystals at the bottom, but you could still taste sooo much residual solvent in it i wont even smoke it. this is the tech ive pieced together from what ive heard/read:
-take your live resin (whatever material) and pour into a mason jar instead of onto parchment
-agitate that oil inside the mason jar and seal it off
-wait a few days for it to separate and vac for 24 hours at room temp.
-then recap the jars and wait for re separation

should i just vac longer?

am i completely doing some bootleg tech? im curious to see what others ppms are in their full spectrum "sauces"
thanks
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Old 10-03-2017, 05:18 AM #10
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Why not just think film purge everything after the separation?
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