THC-A Extraction Principle and Techniques
In this article we will actually post the original summit thc-a extraction method we released, and retracted due to the inherent safety required to perform this process. We feel with our current customer base and the direction the industry is going more and more users are able to afford the hardware to do this easily. This article will talk about the three most common and usable methods with a expansion on the original method of thc-a isolation.
FIRST METHOD. THE SUMMIT ACIDIC EXTRACTION.
This is notably the most complex and will the most extensive to learn as oleo resin material behaves very differently with ph swings. when Elliot Kremerman released this original method it was coveted when the lab technician was able to dial in the process and the variables. this descriptive method is a learning base; how to perform this process and optimize its efficiency. The immediate known efficiency of this described process is approx 51-76% isolation ability, and with some care and optimization with a batch you are consistently working with a efficiency of 85% can be reached with a end result of 75-99.9% depending how many further steps you want to take.
The reason the article was removed was due to the dangers of performing this process and the type of lab wook on the market over two years ago when this was published wasnt able to comprehend the type of hardware required and dangers of performing this process. The part that must be read is the next part were talking about here; hardware.
To perform this process we will talk about the hardware required to process approx 1 liter of refined extract. The very first thing is having high quality glass and components that can withstand chemical exposure as well as hoses, and pumps. In our education process we recommend any chemical duty rotary evaporator, a chemical duty(not chemical resistant) vacuum pump. As well as the highest grade in chemicals to ensure no other reactions are ocuring.
In our testing and refinement process we used:
1. evaporation hardware.
a. across international rotary evaporator.
b. 4c vario pump.
c. polyscience 1.5hp LOBp summit chiller.
2. glassware supplies.
a. 4×36 summit chromatography column.
b. pyrex or schott beakers and bottles as needed.
c. 4l NO-FUSS sep funnel from summit.
d. 20l summit filter bottle.
e. 100mm flanged vessel. for crystallization.
a. hochstrom filter as needed with stage 1,2,3.
a. ph 12 range test strips
5. chemicals and safety.
e. ethyl alcohol.
g. hcl acid.
h. distilled water, or ro/di water.
i. chemical resistant gloves.
j. disposal location for mixed chemicals.
k. applicable chemical neutralizers.
This process will focus on a simple step by step type of extraction in order of steps. We will not support this process so dont call us asking questions. Safety is the number one concern so we used this hardware FOR THIS EXACT PURPOSE, not to light fires in labs or cause a ruckus. If you cannot handle buying and spending loot on gear to be safe them use this as entertainment purposed only. You’ll just end up hurting yourself. So if you think doing this is okay with harbor freight pumps and shitty gear, prepare to have a lab fire in just a mere minutes.
1. Low to medium low temp closed loop extraction of similar sufficient process.
2. Best is inline simple solvent dewax, but dont focus on this, its just a pre step to real winterization.
3. Melt down either a high grade food grade, or even a cold ran extract into ehtyl alcohol.
4. Winterize, carbon scrubbing isnt needed. We winterized in a Summit Hochstrom filter for precision sub 1 micron filtration through the stages 1, 2, 3.
4. Evaporate ethyl to about 2-5%, no more. the less the better, but not to dry or hard in rotovap. we used a chemical duty pump because this is where it gets tricky. Towards the end of the alcohol recovery you need to reduce temperatures to almost room temp, and near no vacuum, and remove all discharged solutions.
5. Low vacuum application, feed dichloramethane(DCM WE WILL CALL IT HERE ON OUT) into rotovap and allow to spin to dissolve all into solution. 1:1 is fine for these purposes of experimentation. This is where per process optimization comes in handy.
6. A wash of regular ph water is done to draw out as much water solubles as possible, about 2-3 washes.
7. We then Poured our dissolved extract that has been winterized and in a dcm solute into a NO-FUSS sep funnel. Under slight vacuum we then washed against our solution with a prepared solution. the solution was distilled water mixed with lye to create a ph of 9.5-10. we did not see much of a result or need to go higher. Ph strips are used and very important to this process and you dont want to over shoot. chemical gloves, neutralizers and face protection as well as ventilation must be used appropriately as lye dust is dangerous.
8. The wash is left to sit. in the bottom layer you will see all the water heavy ph absorb the thca. this process is to be general repeated 1-4x until the sep funnel dcm solution is not drawing anything into the water layer. Remove each water layer and set aside in chemical safe glass containers. It has been said some people reduce a ph of 1/4 value each wash in the water, after the first not to harden original dcm, solution too much.
9. The dcm solution now spent, and removed; can be reduced and distilled out, application of HCL acid can isomerize a result either in d9, or cbn etc. however this is not waste, but can also be reused because the conversion factor here isnt precise and has some left over waste.
10. Take the hardened water with thc-a extracted in it(this is time sensitive), and now place in a large beaker, where there is head space to avoid accidental splashes. the next step is EXTREMELY DANGEROUS.
11. With ventilation again – now apply slowly HCL acid in drops while the flask is on a spinner and at SLIGHTLY LOWER THAN ROOM TEMP.(maybe 60f theoretically wont allow the low boiling point dcm from gassing off). YOU WILL BEGIN TO SEE THE THCA DROP OUT OF THE WATER SOLUTION. it will become hazy, and foggy and start to turn to a cloud. IF THE CLOUD CRASHED VIOLENTLY, YOU WENT TO FAR AND DAMAGED THE THCA, IF IT CRASHES SLOWLY AS IT CIRCLES WITH THE SPIN BAR THERE WILL BE A MOMENT WHERE A SMALL DROP MAKES IT A NEAR SOLID CLOUD EFFECT. THIS IS WHERE YOU ARE DONE ADDING HCL.
12. Remove beaker and now pour into a NO-FUSS sep funnel.
13. Now wash the thca dropped out solution(this is still in a very dangerous and chemical state) neutralized water with heptane or hexane.
14. Repeat wash until the heptane or hexane layer is clear.
You now have chemically extracted pure thca (some minute contaminants too) into your hexane or heptane layer. You now have done the most difficult extraction within our industry removing a physical set of cannabanoid molecules from one layer to another. now using a (safety first) vario 4c, and a rotovap, complete a reduction until almost all heptane or hexane is gone, however LOW TEMP not to affect the thca molecules. Now re introduce pentane to a narrow saturation. and reotovap back down untill its highly saturated. this is because you need to effectively dissolve everything prior to highly saturating it
15. Place solution in a pressure safe vessel.
16. Begin heat and cool cycle, some estimates say a initial cycle of 22-0c or even 20-10c, repeated twice and with a slight vapor burp will prepare the solution when its warm, on the second cycle or even after the first if saturation is achieved you can drop in a seed, and now allow a lower temp stable environment. We used our glass jacketed vessels with valves as a safe location because the jacket can cycle the pressures and easily removed after wit the 100mm flange.
17. Now begin 0-20c temperature cycles, and reduce the cycle and extend them as time goes on.
This process is the crystal morphology process and is expandable and modifiable, each time a cycle is done a small burp is recommended on the vessel via the valve. this will in turn increase saturation levels as crystallization itself decreases saturation levels… its is highly advised to watch this process and learn the cycles properly, and not to share with anyone. this original process Elliot Kremerman released is a basic process that with optimization can achieve amazing results. His time to figure out each process and have multiple users come to the same process is why we decided to post it with the idea NOW PEOPLE CAN EASILY AFFORD the right hardware to do this safely.
The next steps will involve taking the material pre crystallization and effectively establish a method to spike the potency via liquid purity strip.
**15. Take pentane solution and now pour it over a bed of florasil or silica 60. this will strip everything left, a chromatagraphic expression via gel application on the bed is used to even further strip it to highest potency possible. a flash pour and strip is a simpler way with some more losses, and these methods can be expanded upon ion various ways.
**16. a basic crystallization even without chroma column work can be washed with cold pentane, and even crushed up melted down, and re crashed out to yield a better result on its own.
SECOND METHOD. HYDROCARBON CRASH.
One simpler method but less forgiving is crashing out thca-cbd formations in hydrocarbon solution. Most people will still have a residual hydrocarbon content, however the community seems to be okay with that. There are more refined methods of removal including terpene distillations, and post hydrocarbon extractions that would then be crystalized, washed, and re formed; then again to be reconstituted with the previously removed terpenes. The current method we will talk about here is what would be refereed to a all inclusive profile with little selective isolations. The extractor here must recognize a certain level of perameters to be met and often exceeded to yield a quality product worthy of not being called “doo doo sauce”. The reason is because almost all dark slab style products can be converted with ease and deceiving the end user.
Take freshly dried material, and freeze it out prior to storage, and or prior to extraction/column.
Extract material under low pressures and cold temperatures. Inject extracted solution into dewaxing chamber, or a cooling vessel for single solvent dewax. Perform a dewax and then return solution into a clean vessel for recovery. Perform a lower temperature, but still warm recovery of the hydrocarbon. towards the end you will cut recovery off when you are into a 1:1 solution ration or less. This is more or less ratio as some material will behave slightly different.
During the end of recovery heat is also removed from the vessel to not encourage a boiling point azeatrope taking your terpenes with it. This will also act as a cooling effect and chill out the solution.
Pour this solution out of the recovery vessel into a vessel capable of holding pressures. We encourage the use of a glass vessel that can create a cyclic effect of temperature to further promote and speed up the morphology of molecules attaching to themselves in crystal formations. This can be done in a mason jar – stainless – even one of our 100mm pressure vessels.
During the time the solution is self boiling and becoming cold it will begin to look flat on the top without any movement, even if there are still small bubbles rounding up the glass.
Close off the pressure valve, or cap off the mason jar. There are two general methods to do this:
A: leave mason jar in oven around 70-80f and one or twice a day burp remaining hydrocarbon buildup out. Once crystallization begins you can leave it sitting still, sometimes scratching the side will do the trick or adding another material such a seed to encourage it. Heating a cooling is not ideal as it risks breaking the glass with ball jars. After about 3 weeks the crystallization should be effectively complete and most of the hydrocarbon should be purged, however the next step is to pour off the solution onto a fine mesh material and allow as much residual terpene milk to leave as possible. you can leave the crsytals alone and wash it with fresh hydrocarbon solution, or simply just crush it up and use a vacuum oven at 60f top purge off remainder hydrocarbon solution left in the crystal formation.
At this point you can reintroduce your terpene milk back the crystals and enjoy. Some extractors will also recrystallize the washed and ground up formation after dissolving them back in another solvent like pentane. This will take your crystal morphology skills to the next level and increase massive formations.
B. Leaving the solution in a pressure vessel with residual hydrocarbon mixture in this case you do not want it as dry, you particularly want a slightly higher amount of hydrocarbon residuals with this method. Immediately begin a cooling process. With these types of systems we recommend a Polyscience Advanced Programmable chiller to cycle and control temperatures. Begin by dropping temperature to 0c, and timing it so the chiller raises to 20-27c in 40-60 minutes. Repeat this cycle twice, on the second cycle drop a seed in. This can be done with a previous formation, I typically would suggest tossing in 3-5 1/8th inch rocks. Nothing crazy. Try to keep them on the edges. Repeat untill satisfied with initial formations 0-20c in 40-90 minute cycles from hot to cold. So a example would be set chiller to 0c, and then allot after 35 minutes to warm up with 35 minutes heat cycle to 20c. and vice versa. After some time you will begin to be satisfied with initial formations and when the vessel begines to increase in temperature from time to time burp the vessel to remove more and more hydrocarbon once the terepne milk layer is generally purged from the remainder hydrocarbon residuals. the next step to achieve massive shards is to pour off and remove all the terpene milk. As a sacrifice we like to just wash the remainder formations with cold pentane after its been crushed up. Then melt it back down and re crash out the formations in pentane, while cycling the pressure vessel the same way. Purging and further then reintroducing your terpene milk back over the dried crystals is now prepared for consumption. the remainder terpene milk may still have residual hydrocarbon in it.
THIRD METHOD. CYCLIC CRYSTALLIZATION AND CRYSTAL MORPHOLOGY.