Isolates, HTFSE, HCFSE, Solventless THCA from Rosin, Etc

cyphaman · Sep 7, 2017

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!

Old Gold · Sep 7, 2017

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.

live resin · Sep 8, 2017

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"?

SkyHighLer · Sep 8, 2017

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.

cyphaman · Sep 9, 2017

very helpful thanks so much for the great info! Really helpful actually...

cyphaman · Sep 9, 2017

Old Gold said:
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.

SkyHighLer · Sep 14, 2017

Old Gold said:
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?

mobin · Sep 14, 2017

SkyHighLer said:
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.

gumby420 · Sep 28, 2017

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

Smoke342 · Oct 3, 2017

Why not just think film purge everything after the separation?

Smoke342 · Oct 3, 2017

For HTFSPE/ HTCFSPE All you really want to do is dry ice out the THCA, similar to a single solvent dewax for as long as hours to days.

The people with the patent say they take 12 grams of 75% thc oil, dewax out 1.5 gs of 66% thcA+ lechitins and other lipids, then continue with a similar dewax process over hours to days to precipitate out more thcA in a similar manner until they are left with 4 gs of 50% thc sap (HTFSPE), the 1.5 gs dewax and 6.5 gs of fairly pure thcA crystals in the range of 95% pure I believe.

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https://www.google.com/patents/US20170008870

cyphaman · Oct 3, 2017

gumby420 said:
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

Supposedly HTFSE can be purged for 100 hours and will still be liquid, if it separates before then its not HTFSE, thats just based on Extractioneering on IG's posts. I cant back it with any valid proof myself.

I think purging a liquid at room temp, makes sense beacause it will boil off solvent without any heat, whereas if yours has already separated and it viscous and or has solids in it, I would definitely think that to purge it fully youll need some more heat, just my opinion.

Smoke342 · Oct 3, 2017

For sure the technical definition of HTFSPE is essentially the oil you get using their tech, but anyway you remove the THCA to get a liquid/sap that is around 50% thc with double the terpenes and pure thcA are essentially the same products in the end. Extract engineering is defintiely doing the crystal growing method, probably mostly focused on a certain viscosity that is dialed in for fast Crystal growth.

I feel purging this too long would kind of ruin the product as what good is making 2-3x terp sauce if you purge out half the terps, but heat purging would be fairly effective probably get rid of the solvent in a few minutes of boiling but again killing tons of terps, a short thin film would probably be very effective essentially considering its viscosity, not like shatter where the terps are trapped inside.

I was just asking the person who said his HTFSPE and HCFSPE had solvent why he doesn't just purge them longer lol, really a few minutes on heat would solve that problem but sacrifice alot of terps so thin film is probably best.

I feel adding in some crystallized thcA would speed up the crystal growing process as well.

cyphaman · Oct 5, 2017

SOlventless THCA from ROsin Budder: Thanks to @Rosin.Ryan on Instagram (see his page for better pictures of each step if youre confused, I think he only does this with Hash rosin but I may be wrong, wax content may interfere with the process from Flower rosin, hard to say)

The higher the purity / quality the better the result.

Take a fully nucleated / buddered slab of rosin, (think of it as a hash press)
For whatever reason it doesnt seem to work with sap or shatter consistency so just get to whipping if need be*

Place budder in teabag under 30u (25 is preferred) press very light and slow around 120-130F , The terpene rich oils will begin to flow, (very hard to collect but very terpy and liquid)

increase temp a few degrees, and re press (you will want to remove any visible sign on the terp layer so usually a few more presses are required)

Ramp temp again and again until youre sure that whats left has no terps whatsoever, you may want to empty bag, mix it up evenly and repress it..

The idea is to fully squeeze out every bit of terps until youre left with a dry crystalline powder) this will be white in appearance and likely about 95% in purity

I was amazed at how simple it was, anyone tried this?

cyphaman · Oct 20, 2017

Smoke342 said:
For HTFSPE/ HTCFSPE All you really want to do is dry ice out the THCA, similar to a single solvent dewax for as long as hours to days.

The people with the patent say they take 12 grams of 75% thc oil, dewax out 1.5 gs of 66% thcA+ lechitins and other lipids, then continue with a similar dewax process over hours to days to precipitate out more thcA in a similar manner until they are left with 4 gs of 50% thc sap (HTFSPE), the 1.5 gs dewax and 6.5 gs of fairly pure thcA crystals in the range of 95% pure I believe.

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https://www.google.com/patents/US20170008870

this is incredible thank you so much. Makes perfect sense now....I always said it has to be at a certain level or purty to crystalize, and this just proves it. Super stoked thanks for contributing! :tiphat:

Itsgotatail · Oct 21, 2017

So basically, they're dewaxing in butane at -70°C, and then getting THC-A crystals just by just adding spheres and dropping it to -75°C for a few days?

Patmando22 · Nov 12, 2017

Is the rosin sauce made by jarring rosin and heating slightly??? With good terp rich material of course

hash head · Nov 13, 2017

for terp sauce.. dewax with very low temperatures.. and then likely added terpenes could make it separate more easily..

for THCA isolate don't know how it would be made from distillate or rosin.. I think a lot of people saying its made this way are trying to throw people off.. I think best way would to be to use preparative chromatography with silica gel.. I want to try with limonene as the non polar solvent for safety instead of using heptane..

Griffin_Labs · Nov 25, 2017

Sorry if I missed it but does anyone have any info on the terpenes that look like water, something like https://www.instagram.com/p/BbsEvS2FnU4/?taken-by=ascend.cannabis I believe they use a waters sfe system but don't know if that is what they used to make this.

Starwarrior · Feb 4, 2018

Hi guys. I want to make vacuum oven for making HTFSE. I want use plexiglass for making box, nichrome spiral as heating element and converted aquarium compressor as vacuum pump. Tell me please if I do right? I am not sure what temperature and what pressure I need? Does someone have this info?

Isolates, HTFSE, HCFSE, Solventless THCA from Rosin, Etc

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