Preparation of crystalline THCA

[Gray Wolf]

I think Joe can doe better than he did with those solvent washes.... calling you out, Joe!!

And well you should, but as his partner getting freebies, I don't have room for complaints. It was actually more aromatic without further washing.

He did promise me the next batch would include an additional wash to lighten them, so I'll share those peeectures when ah have mah sample in hand.

I will tell him that you said he should take better care of his parnter......., Hee, hee, hee

 

[Old Gold]

I will tell him that you said he should take better care of his parnter......., Hee, hee, hee

At 5% yield there's barely enough for the two of you to taste. That's all I was referring to! haha

 

[Smoke342]

I use to always be making nice nug run and I noticed if I used 30% propane butane and let the solution sit for an hour or longer it would form a nice layer of white crystals at the bottom. Sometimes with trim run it would hardly form anything or a dark layer sometimes pretty nasty goop, and seemed like Sativas like C99 made "the white" easiest, but you wanted to let it sit for 2-3 hours at least so the crystals could form a solid layer that would mix up too bad when you went to filter it.

My friend told me about a buchner funnel which I tried experimenting with but often times it would get too caked up or slow flowing almost the entire upper part of the funnel would turn into that white powder, sometimes 50% or more of the total volume of oil...at the time we believed this to be dewaxing but it never made sense why it would have so much wax, seeming like there should be more thc in the oil that what was turned into white powder.

Anyway came across a patent for making thcA crystals that has a very similar process to what I use to do to make the white powder and it turns out what I was doing was making ThcA crystals all along and it's fairly simple really doesn't require any equipment but a peice of dry ice doesn't hurt...most of the time but can tend to pull more of the cannabinoids and terpenes into the mix and contaminate it.

Here is the patent:

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

So my process basically was blast into a glass container let the container sit long enough on concrete to form a good amount of white crystals and a solid cake layer at the bottom of the dish then dump the oil threw a screen and be left with a nice layer of white powder we would call "the white" that was big with the coke heads, they loved it.

Some things I noticed

1. The crystals best formed when the solution was evaporated, so if you have a large amount of butane vs hash oil...I would say maybe 4-8 ozs bho dissolved in 32 ozs butane hardly any precipitates formed maybe more of just a few grams of a dewax but once the solvent evaporated more and more crystals would form and there was a sweet spot when 50% or more of the final weight would become crystals however, at this point the solution has gotten fairly thick and the white Crystals would be stained with the yellow oil so I would try to keep the white crystals as pure possible by pulling it a little early. (This was part of the nightmare of using the buchner funnel as the solvent would quickly evaporate before getting sucked down and it would be a big mess of not totally pure crystals)

Almost seemed it would be best for trying to get the most crystals to let the levels falls very far then rewash the crystals to get the yellow terpenes juice off of them.

2. For the longest time I could not figure out how to make shatter because the final oil would always be so unstable but people loved it saying it was the best tasting, but as it turned the white powder is what gives the oil it's stability so removing it your left with such a higher amount of terpenes and less stable substances it makes it nearly impossible to make it into shatter without adding the powder back in.

3. Heating the powder on the stove sandwiched in parchment would turn the white powder into an almost clear shatter we were selling as "colorado clear" but it was totally void of terpenes and a very clean headed high we were under the impression it was like selling dewax void of cannabinoids so started just leaving it all in the oil and making very stable shatter.

So for those that don't want to read through the full patent basically they are single solvent dewaxing first for an hour (probably with a good amount of solvent to avoid too much thcA from crystallizing they claim pulling out 1.5 gs of 66% thcA dewax from 12 gs of oil).

Then they keep refreezing the solution to around -70C for hours to days and keep pulling off precipitate until nothing more will come, and being left with 6 gs of 50% THC oil when done which is essentially HTFSPE.

 

[GNYC]

I just want to say thank you to Pangea, Old Gold, SkyHigh, Live Resin, and a lot of you on this post. so much knowledge dropped here over such a large period of time. Its hard to find open source knowledge on the topic, lots of people trying to profit off just teaching it. This is much appreciated.

 

[Emperortaima]

Best thread when it comes to educating about tetrahydrocannabinolic-acid crystalline thanks everyone for your contributions

 

[Gray Wolf]

68 gms of CBD crystals going into a gallon of topical for about a 1/2 gm per oz concentration. The centrifuge was down, so Joe solvent washed these.

 

[SkyHighLer]

^

https://www.youtube.com/watch?v=eB3RJ1U_MJA

A thanksgiving that canna b'beat.



RECRYSTALLISATION Techniques
The most commonly used procedure for the purification of a solid material by recrystallisation from a solution involves the following steps:
(a) The impure material is dissolved in a suitable solvent, by shaking or vigorous stirring, at or near the boiling point, to form a near-saturated solution.
(b) The hot solution is filtered to remove any insoluble particles. To prevent crystallisation during this filtration, a heated filter funnel can be used or the solution can be diluted with more of the solvent.
(c) The solution is then allowed to cool so that the dissolved substance crystallises out.
(d) The crystals are separated from the mother liquor, either by centrifuging or by filtering, under suction, throughasinteredglass,aHirschoraBiichner,funnel. Usually,centrifugationispreferredbecauseof the greater ease and efficiency of separating crystals and mother liquor, and also because of the saving of time and effort, particularly when very small crystals are formed or when there is entrainment of
solvent.
(e) The crystals are washed free from mother liquor with a little fresh cold solvent, then dried.
If the solution contains extraneous coloured material likely to contaminate the crystals, this can often be removed by adding some activated charcoal (decolorising carbon) to the hot,but not boiling, solution which is then shaken frequently for several minutes before being filtered. (The large active surface of the carbon makes it a good adsorbent for this purpose.) In general, the cooling and crystallisation steps should be rapid so as to give small crystals which occlude less of the mother liquor. This is usually satisfactory with inorganic material, so that commonly the filtrate is cooled in an ice-water bath while being vigorously stirred. In many cases, however, organic molecules crystallise much more slowly, so that the filtrate must be set aside to cool to room temperature or left in the refrigerator. It is often desirable to subject material that is very impure to preliminary purification, such as steam distillation, Soxhlet extraction, or sublimation, before recrystallising it. A greater degree of purity is also to be expected if the crystallisation process is repeated several times, especially if different solvents are used. The advantage of several crystallisations from different solvents lies in the fact that the material sought, and its impurities, are unlikely to have similar solubilities as solvents and temperatures are varied.
For the final separation of solid material, sintered-glass discs are preferable to filter paper. Sintered glass is unaffected by strongly acid solutions or by oxidising agents. Also, with filter paper, cellulose fibres are likely to become included in the sample. The sintered-glass discs or funnels can be readily cleaned by washing in freshly prepared chromic acid cleaning mixture. This mixture is made by adding 10OmL of concentrated sulfuric acid slowly with stirring to a solution of 5g of sodium dichromate (CARE: cancer suspect) in 5mL of water. (The mixture warms to about 70°, see p 3).
For materials with very low melting points it is sometimes convenient to use dilute solutions in acetone, methanol, pentane, diethyl ether or CHC13-CC14. The solutions are cooled to -78° in a dry-ice/acetone bath, to give a slurry which is filtered off through a precooled Biichner funnel. Experimental details, as applied to the purification of nitromethane, are given by Parrett and Sun [/ Chem Educ 54 448 1977].
Where substances vary little in solubility with temperature, isothermal crystallisation may sometimes be employed. This usually takes the form of a partial evaporation of a saturated solution at room temperature by leaving it under reduced pressure in a desiccator.
However, in rare cases, crystallisation is not a satisfactory method of purification, especially if the impurity forms crystals that are isomorphous with the material being purified. In fact, the impurity content may even be greater in such recrystallised material. For this reason, it still remains necessary to test for impurities and to remove or adequately lower their concentrations by suitable chemical manipulation prior to recrystallisation.
Filtration. Filtration removes paniculate impurities rapidly from liquids and is also used to collect insoluble or crystalline solids which separate or crystallise from solution. The usual technique is to pass the solution, cold or hot, through a fluted filter paper in a conical glass funnel.
If a solution is hot and needs to be filtered rapidly a Biichner funnel and flask are used and filtration is performed under a slight vacuum (water pump), the filter medium being a circular cellulose filter paper wet with solvent. If filtration is slow, even under high vacuum, a pile of about twenty filter papers, wet as before, are placed in the Biichner funnel and, as the flow of solution slows down, the upper layers of the filter paper are progressively removed. Alternatively, a filter aid, e.g. Celite, Florisil or Hyflo-supercel, is placed on top of a filter paper in the funnel. When the flow of the solution (under suction) slows down, the upper surface of the filter aid is scratched gently. Filter papers with various pore sizes are available covering a range of filtration rates. Hardened filter papers are slow filtering but they can withstand acidic and alkaline solutions without appreciable hydrolysis of the cellulose (see Table 5). When using strong acids it is preferable to use glass micro fibre filters which are commercially available (see Table 5 and 6).
Freeing a solution from extremely small particles [e.g. for optical rotatory dispersion (ORD) or circular dichroism (CD) measurements] requires filters with very small pore size. Commercially available (Millipore, Gelman, Nucleopore) filters other than cellulose or glass include nylon, Teflon, and polyvinyl chloride, and the pore diameter may be as small as O.Olmicron (see Table 6). Special containers are used to hold the filters, through which the solution is pressed by applying pressure, e.g. from a syringe. Some of these filters can be used to clear strong sulfuric acid solutions.
As an alternative to the Biichner funnel for collecting crystalline solids, a funnel with a sintered glass-plate under suction may be used. Sintered-glass funnels with various porosities are commercially available and can be easily cleaned with warm chromic or nitric acid (see above).
When the solid particles are too fine to be collected on a filter funnel because filtration is extremely slow, separation by centrifugation should be used. Bench type centrifuges are most convenient for this purpose. The solid is placed in the centrifuge tube, the tubes containing the solutions on opposite sides of the rotor should be balanced accurately (at least within 0.05 to O.Ig), and the solutions are spun at maximum speed for as long as it takes to settle the solid (usually ca 3-5 minutes). The solid is washed with cold solvent by centrifugation, and finally twice with a pure volatile solvent in which the solid is insoluble, also by centrifugation. After decanting the supernatant,the residue is dried in a vacuum, at elevated temperatures if necessary. In order to avoid "spitting" and contamination with dust while the solid in the centrifuge tube is dried, the mouth of the tube is covered with aluminium foil and held fast with a tight rubber band near the lip. The flat surface of the aluminium foil is then perforated in several places with a pin and the tube and contents are dried in a vacuum desiccator over a desiccant.
Choice of solvents. The best solvents for recrystallisation have the following properties:
(a) The material is much more soluble at higher temperatures than it is at room temperature or below.
(b) Well-formed (but not large) crystals are produced.
(c) Impurities are either very soluble or only sparingly soluble.
(d) The solvent must be readily removed from the purified material.
(e) There must be no reaction between the solvent and the substance being purified.
(f) The solvent must not be inconveniently volatile or too highly flammable. (These are reasons why diethyl ether and carbon disulfide are not commonly used in this way.)
The following generalisations provide a rough guide to the selection of a suitable solvent:
(a) Substances usually dissolve best in solvents to which they are most closely related in chemical and physical characteristics. Thus, hydroxylic compounds are likely to be most soluble in water, methanol, ethanol, acetic acid or acetone. Similarly, petroleum ether might be used with water-insoluble substances. However, if the resemblance is too close, solubilities may become excessive.
(b) Higher members of homologous series approximate more and more closely to their parent hydrocarbon.
(c) Polar substances are more soluble in polar, than in non-polar, solvents.
Although Chapters 4, 5 and 6 provide details of the solvents used for recrystallising a large portion of commercially available laboratory chemicals, they cannot hope to be exhaustive, nor need they necessarily be the best choice. In other cases where it is desirable to use this process, it is necessary to establish whether a given solvent is suitable. This is usually done by taking only a small amount of material in a small test-tube and adding enough solvent to cover it. If it dissolves readily in the cold or on gentle warming, the solvent is unsuitable. Conversely, if it remains insoluble when the solvent is heated to boiling (adding more solvent if necessary), the solvent is again unsuitable. If the material dissolves in the hot solvent but does not crystallise readily within several minutes of cooling in an ice-salt mixture, another solvent should be tried.
Petroleum ethers are commercially available fractions of refined petroleum and are sold in fractions with about 20° boiling ranges. This ensures that little of the hydrocarbon ingredients boiling below the range is lost during standing or boiling when recrystallising a substance. Petroleum ethers with boiling ranges (at 760mm pressure) of 35—60°, 40—60°, 60—80°, 80—100°, and 100—120° are generally free from unsaturated and aromatic hydrocarbons. The lowest boiling petroleum ether commercially available has b 30-40°/760mm and is mostly n-pentane. The purer spectroscopic grades are almost completely free from olefinic and aromatic hydrocarbons. Petroleum spirit (which is sometimes used synonymously with petroleum ether or light petroleum) is usually less refined petroleum, and ligroin is used for fractions boiling above 100°. The lower boiling fractions consist of mixtures of n-pentane (b 36°), n-hexane (b 68.5°) and n-heptane (b 98°), and some of their isomers in varying proportions. For purification of petroleum ether b 35-60° see p. 324.
Solvents commonly used for recrystallisation, and their boiling points, are given in Table 7. For comments on the toxicity and use of benzene see the first pages of Chapters 4, 5 and 6.


From pages 14-16 of PURIFICATION OF LABORATORY CHEMICALS Fifth Edition
Wilfred L. E Armarego/Christina Li Lin Chai

I just downloaded the seventh edition for free from b-ok.org

https://b-ok.org/s/?q=purification+...ls&yearFrom=&yearTo=&language=&extension=&t=0

https://b-ok.org/book/2613303/43b9d0

 

[SkyHighLer]

https://summit-research.tech/thc-extraction-principle-techniques/


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.
3. filtration.
a. hochstrom filter as needed with stage 1,2,3.
4. ph.
a. ph 12 range test strips
5. chemicals and safety.
a. dichloramethane.
b. heptane.
c. pentane.
d. hexane.
e. ethyl alcohol.
f. lye.
g. hcl acid.
h. distilled water, or ro/di water.
i. chemical resistant gloves.
j. disposal location for mixed chemicals.
k. applicable chemical neutralizers.
l.
m.

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.

still working……

By summitresearch| March 7th, 2018|Uncategorized|0 Comments



If you're not familiar with the jargon/techniques I highly recommend getting a copy of The Organic Chem Lab Survival Manual: A Student’s Guide to Techniques by James W Zubrick. It can be downloaded from Library Genesis for free, no hassles.

Library Genesis home page,

https://gen.lib.rus.ec

A ninth edition download page, close all other windows/tabs, click on GET at the top of the page,

https://libgen.io/_ads/EA63250BE43386C06B4BAE9A9A5C328A

 

[Emperortaima]

Thanks for continuing this thread.

 

[Skunkpassion]

Fantastic thread & a brilliant read.. I'll be attempting making Diamonds...