What is everyone doing for these jars of crystals

[Old Gold]

I won't say he's "wrong" but the difference in boiling point due to pressure is very significant. Maybe pressure effects lattice structure, I don't honestly know. A quick search tells me pressure can affect lattice formation with some metals.

We could easily find out by dissolving a small batch with solvent, drop-wise...the least amount necessary to fully dissolve the sample, with no nucleation or dissolution happening at room temperature. Split the solution into two batches and pressurize one of them.

As for the attached image, ignore the numeric values.

 

[SkyHighLer]

4" DIAMOND MINER

The 4" Diamond miner eliminates the need for glass jars and adds safety to your degassing procedure. It also gives you multiple viewing angles to see your diamond growth. Remove the 4" x 2" splatter platter to easily remove diamonds from your sauce mix. A glycerin filled compound gauge gives you easy readout of pressure inside the vessel.

Specifications:

304 grade stainless steel
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4" splatter platter
High pressure clamps
MAWP: 100 psi

https://www.bestvaluevacs.com/4-diamond-miner.html

 

[Chonkski]

jeez they move quick

 

[Itsgotatail]

I'm wondering if I can just do this crystal formation, on a large scale, right in my collection spool. I have a 12"x12" collection spool with a 4" deep shatter platter on the bottom. Hoping I can run multiple material columns (each 4"x48", hold about 3lb dry material) since my recovery vessel will be out of commission for a while. Should I just stop recovering when there's still a fair amount of butane in it, keep my recovery bath at ~75-80°F, and just wait a week for the crystals to crash out? Will that happen?

 

[Smoke342]

This is cool and proves pressure is involved with one method of fast crystallization, however I am more interested in how people are getting 0 ppm crystals fron already purged sap like the ones extract engineering grow in a week, as I think any method using solvent to form crystals will be impossible to purge.

Why the white powder isolate is so nice its like snow and purges itself just sitting out but at full vac would purge in like an hour and it can easily be turned into crystals just by heating it for a bit so...just wastes alot of solvent washing it and all that, but it's a nicer smoke leaving it a bit dirty with a good bit of terps.

https://www.instagram.com/p/BdNx7tyhzwI/

 

[WishDoctor]

so I wonder, I think I figured out a way to crash thca crystals in bho...maybe

I did several batches of runs of trimmed nugs, fresh harvest typical cure about 2 months, I used this years ac, and jaegar, platinum kush, and last years bogs sour strawberry kush, a lb of each all separate batches.
average oil = 30g per 125g nugs, I would do 2 bottom up and 1 shower then recover.
I have a modded 6" bi direction terp with a 18" x 3" column no jacket, and a 12" recovery bucket, a wonderful distillery. ansi of course
I run my tanks ice cold, no sub zero stuff ever, dry ice occasionally, but norm is reg ice with salt to drop the temp a bit. and I do warm column recovery as needed to push the butane, old school style. I have the tsr for recovery nothing fancy. I have a chiller and use several driers inline.
when collecting each batch I scraped them onto their own pieces of parchment, folded them and placed them into a air tight box for a week, now here is where it goes weird, normally I would just start to purge each run within moments of scraping, and the oil made would be clear terpy and potent.
Now after several batches just sitting sealed for several weeks, I went back to purge them and they are looking super duper sugary, and smell terpiliciously intense.
Now after purging, the crystals are getting more and more defined.
I dropped/dissolved some into coconut oil and allot of crystals have settled out overnight sitting in the warmth of the shop.
not sure what they are, but the only test now is to make gel caps before with some crystals, and after decarbing to see if they dissolve and then perform separate bio assay's.

 

[SkyHighLer]

The CBDistillery is known for beautiful CBD crystallization (hence the crystals in our logo). Our customers and followers on social media (@the_cbdistillery) have always been curious about these crystals and how they are grown. So on 7/25/17, over five days, we live streamed the crystallization of 150 grams of CBD.

The event was incredibly successful, reaching 1.5 million people on Facebook and was shared over 800 times. Don’t worry if you missed this event, here is a recap of the five-day crystallization as well as all of the answers to your questions about CBD crystals.

What Is A CBD Crystal and How Is It Different From CBD Isolate?

A CBD crystal is grown using CBD isolate or distillate, during the process known as “isolation”. CBD isolation is the method of forcing the CBD molecule to come out of a solution (in our case pentane) and allowing it to reform into a pure substance generally at 99+%. Once the crystals have formed, there is a “mother liquor” left behind which contains the impurities that were removed during the isolation process. Crystallization can, therefore, be performed in order to remove impurities from the isolate or distillate.

How To Grow A CBD Crystal

DISCLAIMER: THE CBDISTILLERY DOES NOT RECOMMEND ANYONE TRYING TO GROW THEIR OWN CBD CRYSTAL. IF IN THE EVENT THAT YOU ATTEMPT TO GROW A CRYSTAL, WE RECOMMEND USING THE PROPER LAB EQUIPMENT, UNDER THE SUPERVISION OF A PROFESSIONAL, USING PROPER SAFETY PROTOCOLS.

As previously mentioned, a CBD crystal is grown using a CBD isolate or distillate typically with a 60-80% purity. Isolate is a powder form of CBD which is extracted from the mature stalks and stems of hemp plants. Under a ducted fume hood, the first step of growing a CBD crystal is to add the isolate to a graduated cylinder or in our case to a mason jar. Then, you slowly add your solution (pentane) to the CBD isolate to create a super saturation.

Once the pentane has been added, seal the container with a lid and place it in a safe location, away from any fire sources (pentane is a highly flammable solution). The now saturated isolate will slowly crash out of the solution, eventually isolating the CBD molecule.

What Do We Do With A CBD Crystal?

During a crystallization, smaller crystals structures generally have fewer solvents trapped whereas the larger crystals can end up with a lot of residual solvents trapped within them. This is the reason The CBDistillery does not sell the crystal formations on the website. After a crystallization, the formation is broken down, the majority of the residual solvents are removed in a vacuum oven, and the now purified isolate is turned into either slab or powder form which can then be shipped directly to your front door.

Here is a time lapse of the crystal growing over a 5 day period. At one point in the first 48 hours, our camera stopped recording, hence the gap in the video.

https://www.thecbdistillery.com/150-grams-cbd-crystallization/

https://www.youtube.com/watch?v=TCXytPCkQH8


This also works for THC-A?


Pentane, and other highly non-polar solvents are available to the general public, click on my Solvents listed as to polarity link below.

 

[G.O. Joe]

People have been getting CBD and CBN to form particular crystals in pentane since 1940, so that still works and THCA-A still lacks a crystalline form known to science. Can you slowly evaporate a solution of amorphous solid to get a glass? Quickly? Cool a hot solution? Wait out a supersaturated solution? Why not, but crunchy and sparkly glass is not the technical definition of crystalline. Vacuum or at least lowering of pressure would make more sense than pressure.

 

[OregrownGreen]

Solubility of THC-A in liquidous terpenes(and high residual solvent at first) creates nucleation and slowly crystals form on each other under low temperature and high pressure(stainless pressure vessel in a freezer work well). Afterwards, small crystals can be washed with cryo pentane to create starter seeds, these seeds can then be used to facilitate further nucleation of later batches(how people get extra big diamonds). Not sure why they do this though aside from the jar appeal, bigger crystals = lower purity

 

[SkyHighLer]

^ Thanks for the clarity concerning crystal versus amorphous solid.

https://en.wikipedia.org/wiki/Crystal

https://en.wikipedia.org/wiki/Amorphous_solid


Don't seal up Mason jars containing butane. At room temperature you're at the burst strength of the jar, and from my own experience the sealing ring/lid will blow off no matter how careful you are when you go to unscrew it. And never put a jar containing butane in the fridge/freezer.

https://www.icmag.com/ic/showpost.php?p=8161714&postcount=1109

 

[Pangea]

Can you slowly evaporate a solution of amorphous solid to get a glass? Quickly?

Like shatter?

Cool a hot solution?

Like this "patent" describes https://www.google.com/patents/US20170008870

Wait out a supersaturated solution?

Like we see in shatter slabs that "sugar", "butter" "nucleate" or in jars/vessels that we let sit to crystallize, exactly like common elementary sugar and salt growth techniques

Why not, but crunchy and sparkly glass is not the technical definition of crystalline. Vacuum or at least lowering of pressure would make more sense than pressure.

I agree with the pressure logic.

The attached images show clear facets and double ended terminations on this apparent, glass?

You specify THCA-A do you mean that other forms of THCA are known to crystallize but specifically not THCA-A?




Also, I disagree with most of what OregrownGreen said, specifically on purity. The purest and cleanest crystals, however, are usually also the ones that grow to be the largest in size. Thats not my statement.

For now, I'm sticking with my original theory of folks using pressure as to keep in a decent amount of tane which keeps the viscosity in a optimal growth range.

Can anyone explain how/if Henry's Law applies with two or more different gasses, say with nitrogen and butane/butane solution, as the law state "the amount of a given gas dissolved in a given type and volume of liquid is directly proportional to the partial pressure of that gas in equilibrium with that liquid"

 

[dro510]

Got to show off these crystals! So damn cool! Thanks for the info ICMAG!!
Burping once a day this was not even at 7 days. But some jars are just showing crystals today which is 7 days. Dewaxed solution.
Also thought I'd add this was extracted from fresh frozen buds.

I read to purge terps n thca seperately. Is this because they purge at different temps? lower temp for terps and higher for thca?
Would appreciate an answer please ^^^^^

 

[G.O. Joe]

Like shatter?

How differently does it analyze than the shatter it comes from? My guess is what most people have is shatter made a different way which is fine if true if that's all it's represented as. There's lots of gray here some say you need impurities or pressure others say say they recrystallize in pentane - which is pretty much proof that what they have is not the pure THCA-A they think. Some say the crystals are pure and others say they're terpy. None of the known esters of THCA with the terpenoids are known to be solids. When Adams distilled his red oil he thought he was on to something when crystals started forming in the condenser. Those proved to be the non-cannabinoid l-quebrachitol, which could also be washed out of petroleum ether solution of the red oil with water. What anyone's crystals are I only know that extraordinary claims demand extraordinary evidence, and it's most likely there's nothing extraordinary going on.

You specify THCA-A do you mean that other forms of THCA are known to crystallize but specifically not THCA-A?

Sure there were earlier threads where that came up with your high melting crystals what could they be what. Mechoulam and el-Sohly both isolated THCA-B and like CBD and CBN it crystallized readily enough. Mechoulam's product was recrystallized from slow evaporation of chloroform for the x-ray crystallography. The A form has a feature that makes it more difficult to crystallize than other cannabinoids.

Also, I disagree with most of what OregrownGreen said, specifically on purity. The purest and cleanest crystals, however, are usually also the ones that grow to be the largest in size. Thats not my statement.

The rule of thumb in chemistry in general is the odds are on larger crystals being more impure.

 

[HashoftheTitans]

Most processors are making large crystals from fresh frozen extracts and then pressurizing to encourage larger crystal formation. The solution is over-saturated with THCA the moment you recover most of your solvent. The key is to keeping the viscosity low enough to allow crystals to fall out through the solution. Whether or not that is done by terpenes or solvent is dependent on the material. After your solution is done separating, you can pour off the high terp layer and be left with high THCA extract that you can rinse with solvent, then recrystallize. The recrystallization can finish in as little as 36 hours with 98%+ purity. Purity is key to speed of crystallization and the total amount of solution that will crystalize. Once your mother liquor drops below 50% crystallization stops in most cases.

 

[Pangea]

How differently does it analyze than the shatter it comes from?

It doesnt come from shatter, it comes from the initial dissolved solution. The analysis Ive done with uncleaned but separated crystals is 96+% THCA, lab results from Guild Extracts has been 99.9+% and from the looks of it crystallize multiple pounds per month for years now.

My guess is what most people have is shatter made a different way which is fine if true if that's all it's represented as. There's lots of gray here some say you need impurities or pressure others say say they recrystallize in pentane - which is pretty much proof that what they have is not the pure THCA-A they think. Some say the crystals are pure and others say they're terpy. None of the known esters of THCA with the terpenoids are known to be solids. When Adams distilled his red oil he thought he was on to something when crystals started forming in the condenser. Those proved to be the non-cannabinoid l-quebrachitol, which could also be washed out of petroleum ether solution of the red oil with water. What anyone's crystals are I only know that extraordinary claims demand extraordinary evidence, and it's most likely there's nothing extraordinary going on.


Sure there were earlier threads where that came up with your high melting crystals what could they be what. Mechoulam and el-Sohly both isolated THCA-B and like CBD and CBN it crystallized readily enough. Mechoulam's product was recrystallized from slow evaporation of chloroform for the x-ray crystallography. The A form has a feature that makes it more difficult to crystallize than other cannabinoids.



The rule of thumb in chemistry in general is the odds are on larger crystals being more impure.

[/quote]

I can appreciate wanting confirmation from some sort of diffraction or similar techniques, I dont think its that much of a stretch considering the photo's, analysis' and experiences shared. If one is yielding 20-50% crystallized material out of the starting solution what other option could it be, there is no other compounds present in this quantity in the solution other than THCA. How do you explain the facets and double ended termination pictured, I didnt carve them out of shatter.

Side thought, I havent been able to recrystallize with alcohol based solvent, perhaps this is why the literature hasnt shown this process, perhaps when using certain solvents it prevents crystallization.

Most processors are making large crystals from fresh frozen extracts and then pressurizing to encourage larger crystal formation.

Is there any explanation to this thought process? Ive yet to see a single piece of evidence that pressurizing encourages larger crystal formation in of itself.

The solution is over-saturated with THCA the moment you recover most of your solvent. The key is to keeping the viscosity low enough to allow crystals to fall out through the solution. Whether or not that is done by terpenes or solvent is dependent on the material. After your solution is done separating, you can pour off the high terp layer and be left with high THCA extract that you can rinse with solvent, then recrystallize. The recrystallization can finish in as little as 36 hours with 98%+ purity. Purity is key to speed of crystallization and the total amount of solution that will crystalize. Once your mother liquor drops below 50% crystallization stops in most cases.

Agreed, been saying viscosity is key from the get go, large singles need time and stillness, makes me cringe when people pick up and play around with there actively crystallizing vessels.

Purity is not key to speed though it certainly can hasten it. Speed is a function of solubility which for a specific given solvent and compound is mainly determined by temperature and the amount of compound:solvent ratio. I can recrystallize any amount of pure thca in less than a second, it literally explodes into existence as the micro crystalline form pictured from my scope.

The reason large crystals are considered more pure than their smaller counterparts is the surface area to volume ratio is much lower in larger crystals, when /if you re/crystallize in a not pure solution with any amount of mother solution remaining it will be prone to trap between crystals not within them.

Hashofthetitans, how large are the individual crystals after people redissolve to wash and recrystallize? IMO washing doesnt involve dissolving any crystallization, washing would involve dissolving or cleaning the surface area of already formed crystals from the non crystallized mother liquor solution.
If people dont care about size of crystal and want yield they'd use temp swings with proper viscous solutions, people winterize out the fats and lipids, why not use the exact same concept/process/equpment to winterize out the other high melting point compounds, though when winterizing out a compound like THCA we wouldnt call it winterizing, we'd call it... crystallizing.

 

[HashoftheTitans]

It doesnt come from shatter, it comes from the initial dissolved solution. The analysis Ive done with uncleaned but separated crystals is 96+% THCA, lab results from Guild Extracts has been 99.9+% and from the looks of it crystallize multiple pounds per month for years now.

I can appreciate wanting confirmation from some sort of diffraction or similar techniques, I dont think its that much of a stretch considering the photo's, analysis' and experiences shared. If one is yielding 20-50% crystallized material out of the starting solution what other option could it be, there is no other compounds present in this quantity in the solution other than THCA. How do you explain the facets and double ended termination pictured, I didnt carve them out of shatter.

Side thought, I havent been able to recrystallize with alcohol based solvent, perhaps this is why the literature hasnt shown this process, perhaps when using certain solvents it prevents crystallization.



Is there any explanation to this thought process? Ive yet to see a single piece of evidence that pressurizing encourages larger crystal formation in of itself.


Agreed, been saying viscosity is key from the get go, large singles need time and stillness, makes me cringe when people pick up and play around with there actively crystallizing vessels.

Purity is not key to speed though it certainly can hasten it. Speed is a function of solubility which for a specific given solvent and compound is mainly determined by temperature and the amount of compound:solvent ratio. I can recrystallize any amount of pure thca in less than a second, it literally explodes into existence as the micro crystalline form pictured from my scope.

The reason large crystals are considered more pure than their smaller counterparts is the surface area to volume ratio is much lower in larger crystals, when /if you re/crystallize in a not pure solution with any amount of mother solution remaining it will be prone to trap between crystals not within them.

Hashofthetitans, how large are the individual crystals after people redissolve to wash and recrystallize? IMO washing doesnt involve dissolving any crystallization, washing would involve dissolving or cleaning the surface area of already formed crystals from the non crystallized mother liquor solution.
If people dont care about size of crystal and want yield they'd use temp swings with proper viscous solutions, people winterize out the fats and lipids, why not use the exact same concept/process/equpment to winterize out the other high melting point compounds, though when winterizing out a compound like THCA we wouldnt call it winterizing, we'd call it... crystallizing. [/QUOTE]
Purity of the initial solution is key to the primary crystallization. The more garbage in the way, the longer it takes to crystallize.

Larger crystals are seldom more pure. That may be what is said among the cannabis industry, but that's because of people's inability to wash the thick mother liquid from the surface of many small crystals. Larger crystals tend to have more inclusions, hence lower purity.

After washing and dissolving, during recrystallization, the size and shape of crystals are subjective to parameters like solvent system, temperature, and pressure. I wash and recrystallize in pentane at 98f and get dried-pea-sized crystals.

 

[Pangea]

Purity of the initial solution is key to the primary crystallization. The more garbage in the way, the longer it takes to crystallize.

Larger crystals are seldom more pure. That may be what is said among the cannabis industry, but that's because of people's inability to wash the thick mother liquid from the surface of many small crystals. Larger crystals tend to have more inclusions, hence lower purity.

Many ways to go about it, but for clarification Ive never heard anyone in the canna biz say that about larger or smaller crystals. When I wrote, "The purest and cleanest crystals, however, are usually also the ones that grow to be the largest in size." Thats not my statement." If you google the exact statement you will find the many sources and background on the statement. Crystal if they have inclusions or occlusions are not single crystals they are clusters or agglomerates, clusters with mother liquid in cavities and directly between them, just like smaller crystals, the benefit of washing from the mother liquor from larger singles is that you can see any impurity by discoloration, if its got yellow inside its almost always a cluster and you can usually separate them with fineness washing teks. If your growing agglomerates and want large singles, slow it down, to fast of growth, to much nucleation, to many crystals, you want the lattice to form on as few singles as possible, not cause a cascade of nucleation off each other, similar to how sugaring spreads on a shatter slab...

Its primarily a matter of surface area though, 1gram single vs 1000 single mg crystals with the chance for one facets surface to be flush to anothers with a contaminate of say a molecule of pentane inbetween them is higher with the smaller sized crystals. A contaminate inside the crystal is much different than surface area, if your cosolvation

After washing and dissolving, during recrystallization, the size and shape of crystals are subjective to parameters like solvent system, temperature, and pressure. I wash and recrystallize in pentane at 98f and get dried-pea-sized crystals.

[URL=https://www.icmag.com/ic/picture.php?albumid=75740&pictureid=1816119&thumb=1]View Image[/url]

Looks good! Any sort of recrystallization should be bump purity, many routes to the end goal. You say pressure again in your parameters, whats the pressure doing? Any residual pentane after recrystallization?

 

[HashoftheTitans]

Many ways to go about it, but for clarification Ive never heard anyone in the canna biz say that about larger or smaller crystals. When I wrote, "The purest and cleanest crystals, however, are usually also the ones that grow to be the largest in size." Thats not my statement." If you google the exact statement you will find the many sources and background on the statement. Crystal if they have inclusions or occlusions are not single crystals they are clusters or agglomerates, clusters with mother liquid in cavities and directly between them, just like smaller crystals, the benefit of washing from the mother liquor from larger singles is that you can see any impurity by discoloration, if its got yellow inside its almost always a cluster and you can usually separate them with fineness washing teks. If your growing agglomerates and want large singles, slow it down, to fast of growth, to much nucleation, to many crystals, you want the lattice to form on as few singles as possible, not cause a cascade of nucleation off each other, similar to how sugaring spreads on a shatter slab...

Its primarily a matter of surface area though, 1gram single vs 1000 single mg crystals with the chance for one facets surface to be flush to anothers with a contaminate of say a molecule of pentane inbetween them is higher with the smaller sized crystals. A contaminate inside the crystal is much different than surface area, if your cosolvation



Looks good! Any sort of recrystallization should be bump purity, many routes to the end goal. You say pressure again in your parameters, whats the pressure doing? Any residual pentane after recrystallization?

I can't be sure what the pressure does, but as we have said that agitation can create more nucleation sites, I assume that increased pressure slows the movement of molecules in the lattice and allows for a more uniform dispersion of kinetic energy as your solvent slowly evaporates and allows you to somewhat control the rate of crystallization.

The crystals are at 1000ppm pentane before purging and about 300PPM after a short, deep-vac purge at 125f.

 

[G.O. Joe]

I can appreciate wanting confirmation from some sort of diffraction or similar techniques, I dont think its that much of a stretch considering the photo's, analysis' and experiences shared. If one is yielding 20-50% crystallized material out of the starting solution what other option could it be, there is no other compounds present in this quantity in the solution other than THCA. How do you explain the facets and double ended termination pictured, I didnt carve them out of shatter.

Side thought, I havent been able to recrystallize with alcohol based solvent, perhaps this is why the literature hasnt shown this process, perhaps when using certain solvents it prevents crystallization.

No one is using alcohols Adams used low boiling petroleum ether to get CBD and CBN in 1940 none of this is rocket science and that's the thing. A lot of chemists have worked with THCA-A and none of them purify it by recrystallization because it's never ever been recrystallized in the voluminous body of peer-reviewed literature. They're the ones who really want NMR from you guys, they want to know how you can and they can't. The lab down the street or in the basement will not do, unless there is silylation and GC/MS. So let's hear about melting points. Shouldn't that be a competition.

 

[Theicc]

THCA will precipitate out of basically any live resin run, and also most crude extracts.

Wht do you mean by crude extracts. I ask because I have a lb of unstable dark oil that I have been experimenting with. It has never been heated above 95 in a vac oven. So I got all this oil to play with. I would like to know if it's possible to do this post extraction or if extraction is part of the process.