If everything is closer together in the Van, der everything gets friendlier. Some molecules need more assistance in getting closer to the Waal than other molecules.
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If you elaborate a bit more on the cryosift/Kief trichome extractions, it may be a bit closer to the true chemistry of the process? Trichome extractions give you clean answers if you know what I mean. Like comparing a -60 butane extraction of trichomes against a -60 butane extraction of powdered THCA crystalline material. Might just tell us a lot about terp contribution to the standard BHO process and reveal some proposal for what state the cannabinoates might be in if present in situ.
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Are you implying something interesting in the transition of an alkane dilute solution of cannabinoic acids to a âmother liquidâ state? Or are you implying some technical detail of the extraction, i.e., transition from the innate , in situ state to dilute solution in alkane?
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Thatâs a really solid direction for getting to the chemistry beneath the noise. I havenât run the exact experiment youâre describing (crystalline isolate vs trichomes at -60°C side by side), but Iâve done some comparable extractions on cryosift/kief that revealed a lot.
In a few staged runs, I started with a terpene strip at -50°C using propane, and then followed up with a cannabinoid-focused pull around -20°C with a high solvent ratioâsomewhere between 10:1 to 20:1. I found that the cannabinoid fraction still extracts efficiently even when the terpenes are mostly gone.
I have a second method of terpene extraction prior to cannabinoids that has validated the concept. Pulled a sock after terpene extraction and it smelled like hay. Then put back in and ran for acidics and was able to isolate the three fractions (terpenes, acidics, and neutrals) directly from bio with a single solvent system (70/30 propane heavy) and single process (bio to isolates).
Thatâs where my observations diverged a bit from the terpene-assisted solubility theory. It seems that the hydrocarbon solvent system alone can still solvate the acidic cannabinoids, even in terpene-depleted materialâassuming the system conditions are right.
That doesnât rule out the idea that terpenes influence phase behavior or play a structuring role inside the trichome, but Iâm leaning toward solvent density and system state being the key factors in making those compounds mobile.
A denser solvent increases solubility at low temperatures by boosting molecular contact, restoring solvation interactions, and making the system behave more like itâs in an ideal state for dissolutionâeven when thermal energy is low.
This is a thermodynamically backed strategy. Youâre overcoming the entropy loss at low temps with increased enthalpic interaction via solvent compression, which maintains or even enhances solubility.
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there is high tech Raman spectroscopy methodology paper that suggests the THCa in situ is crystalline. Or at least some of it is. I can not imagine a crystalline state that is not in equilibrium with the bulk solution volume element of terpenes present. The authors suggest a ânano dispersionâ. Iâll find that paper and send it.
I have done a bit of acidifying the trichomes with acetic acid or HCl. The trichome storage areas turn an opaque white, or. Opalescent white, when observed under the binocular scope. So we know there is enough aqueous there to effect an optical phase change and assume we are fully protonating the cannabinoates to cannabinoics. You can also add a small amount of concentrated acetic acid (dimer) to alkane . Just an observationâŚnothing really helpful.
With respect to temperature: when you do a pour out of butane and open evaporation, have you ever measured the temperatures obtained at the exact time of fast crash? Do you see fast crash with (prior) terpene stripped material and subsequent extracts evaporating.
Just. Curious.
Regards,
Note added: If you did the terpene strip at -50C âŚOK we have eliminated the terpene âsolution theoryâ at that temp. What binding might be going on that prevents the cannabinoic acid from dissolving? If we were to do the comparison of THCA crystal at same temp, and found it does not dissolve we may be closer to an answer. From a polar protic view, it would seem that -60C concentrated ammonia follow up , might do the trick.
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Hmm i played with ammonia quilt a bit
Not so sure it will help
Wonder of it dissolves in alkanes?
Solubility, is a matter of pH.
Did you ever see the little blurb, I published here about making a THCA extract with an expesso maker and ammonia soaked biomass?
In the case we were talking about, biomass stripped of terpenes at -50C. Well concentrated Ammonia doesnât freeze until about -70C. So I was thinking one could go in and see what might take the THCA out at low temp and step the temp up âŚuntil you hit a sweet spot.
To get rid of it, just acid crash to pH 2.0 and LLE to pentane. The ammonia will be 100 % NH4+ and stays in aqueous phase. You can just do quick ammonia extract if you have some at RT. Check it out.
You know its chemistry is related to the Amberlyst A21 resin chemistry:
The author is Aizikovitch: Patent: US WO 2020/016875. It is the rather notable. Amberlyst A21 (mystery binding COOH)..that works.
Here he is using ammonia in conjunction with Ethanol/water (protic polar ) extraction of CBDA.
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Thats because increased pressure increases solubility.
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Iâve always found that flowing butane will pick up more of the thca than soaking does, constantly being jostled and mixed around by an injection stream always pick up more than a soak style rinse. At most temp of solvent. Warmer grabs more but maybe 10-15% more. While -40still grabs 5+%. Loose values based on cold crash efficiencies and different rinse parameters.
Can you put logic to why sift made from Ln2 is a dream to use as starting material for extraction. Smooth trouble free runs with out of this world throughput.
Vs
Anytime Iâve run freeze dried or dry sift it requires additional measures for a complete dissolve and tends to get muddy if not compensated for immediately. Often leading to extended stays and extra clean up time.
Sublimation of moisture would be my guess
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Can you give us details on LN2 sift process,exactly what you mean. Do you mean the large scale commercial machine, or is this a one-off process you do.? Once done, can you just outline your extraction set up?
I think the LN2 not only knocks the trichome heads off, but freeze fractures the the biomass to a limited extent. (Examine under a stereo microscope) producing a subset fragments that pass through the sift and mix with trichome heads. This particulate particle buffer may enhance flow based extraction , improving efficiency.???
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Canât speak for @Costello and his process but if you check out a company called âThe Original Resinatorâ they have a sift tumbler that includes ln2 ports. Lots of good info on their site.
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Itâs been a few years and maybe theyâve changed since, but in the past they never used ln2. They had recommended and had ports for CO2 gas.
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Well actually I was wondering whether Costello has his hands on a CryoMass , CryoSift Separator for at scale continuous separations, or whether it was an sop he developed him self with LN2? And whether he is referring to Butane, propane or a mixture for his referenced extractionsâŚ
Ln2 sift from a giant ln2 separator.
Vs
Freeze dried water hash
Vs
Co2 extracted kief
Vs
Dry tumble
Kief is loaded into a sock filter (100 micron) along with stainless steel ball bearings.
Sock is loaded into column and flooded with room temp solvent.
At this point the Ln2 sift will be closest to dissolved and ready to run thru system to recovery.
All other sift will require much more manipulation to dissolve and on a few not so lucky occasions (usually freeze dried or dry tumble) will not fully dissolve and worst case just transfer sand to collection.
It was a cryo mass style machine.
Room temp n butane