# How to isolate and purify THC, CBD, CBN



## greenfriend

There are other ways to isolate these compounds (phase transfer catalysts), but an even better option is column chromatography.

But first, a word about decarboxylation. Whether to decarb can be debated forever, but if you do, it should be heated under nitrogen at 105C for 1 hour.

I like to use a non-polar solvent to extract and a polar solvent to wash. Besides butane, try propane, hexane, and chloroform (especially efficient). Absolute ethanol (200 proof) is my polar solvent of choice.

When you intend to isolate the individual cannabinoids you should stabilize the crude product. With the product dissolved in 100% EtOH before winterization, filter the solution through charcoal, extract with 2% sodium sulfate, then filter through charcoal again. This prevents oxidation of your crude product.

The odoriferous terpenes can be removed by steam or vacuum distillation. Cautious distillation in vacuo yields a fraction of crude red oil (bp 100-220° C/3 mm). This can be purified by redistillation or column chromatography. Use ethanol to remove the residue from the flask while it is still hot. Filter the solution through charcoal, and strip the solvent. Distill the residue to yield pure red oil (bp 175-195° C /2 mm). Distillation must be stopped if smoke appears, indicating decomposition.

Because THC is heat-sensitive, it is preferable to isolate the cannabinoids by column chromatography. The simplest method of column chromatography is performed with ethanol and ether extracts of hemp on alumina, yielding two major fractions: (1) chlorophyll, CBD, and CBN, and (2) THC. A second, more difficult method is performed on Florisil (use 10 times the weight of the oil) with the solvent system hexane:2% methanol. This yields a doubly-concentrated, viscous oil which can be repeatedly chromatographed on alumina to separate the THC and CBD. The CBD fraction of column chromatography can be distilled (bp 187-190° C/2 mm; pale yellow resin) to purify it.


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## JustAnotherAntMarching

Huuuuuuh??????


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## AluminumMonster

JustAnotherAntMarching said:


> Huuuuuuh??????



So glad i'm not the only one! LMAO!!!!!


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## greenfriend

JustAnotherAntMarching said:


> Huuuuuuh??????



Yea it's heavy on the chemistry, but if you've got the lab gear and the inclination, you can make pure CBD at home


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## UpstairsRichie

Just wondering? What kind of lab gear do you need?

What's the reason for a non-polar solvent to extract and a polar solvent to wash?
Why not just extract with high proof alcohol, like Ever Clear?


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## greenfriend

UpstairsRichie said:


> Just wondering? What kind of lab gear do you need?
> 
> What's the reason for a non-polar solvent to extract and a polar solvent to wash?
> Why not just extract with high proof alcohol, like Ever Clear?



Lab gear: fractional distillation setup, basically all your standard chem glassware, vacuum pump, magnetic stirring hot plate, chromatography tubes and filters

High proof alcohol is a very effective polar solvent, so effective that it also extracts chlorophyll and other undesirables. Non-polar solvents will not extract chlorophyll. The ethanol wash removes any residual non-polar solvent (butane), and allows for the winterization step.

You don't want any moisture (h2o) contaminating your product. Everclear, depending on where you live is either 10% or 25% water.  It is best to use anhydrous (200 proof) ethanol. Buy everclear and dehydrate it with Zeolite or calcium oxide. Alternatively, with a strong vacuum pump you can distill 200 proof ethanol because there is no azeotrope at 70 torr.


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## UpstairsRichie

greenfriend said:


> Lab gear: fractional distillation setup, basically all your standard chem glassware, vacuum pump, magnetic stirring hot plate, chromatography tubes and filters
> 
> High proof alcohol is a very effective polar solvent, so effective that it also extracts chlorophyll and other undesirables. Non-polar solvents will not extract chlorophyll. The ethanol wash removes any residual non-polar solvent (butane), and allows for the winterization step.
> 
> You don't want any moisture (h2o) contaminating your product. Everclear, depending on where you live is either 10% or 25% water.  It is best to use anhydrous (200 proof) ethanol. Buy everclear and dehydrate it with Zeolite or calcium oxide. Alternatively, with a strong vacuum pump you can distill 200 proof ethanol because there is no azeotrope at 70 torr.


So I did a search, and realize I know less than I thought I did about chemistry. 

http://www.masterorganicchemistry.c...ic-polar-aprotic-nonpolar-all-about-solvents/


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## Soloma

I do not like the idea of isolating chemical compounds. The synergy of the whole plant is much more attractive to me then processing the plant any more than I have to.

This separation is what has gotten us into this mess that we call healthcare system in the first place.


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## greenfriend

Soloma said:


> I do not like the idea of isolating chemical compounds. The synergy of the whole plant is much more attractive to me then processing the plant any more than I have to.
> 
> This separation is what has gotten us into this mess that we call healthcare system in the first place.



I completely agree with you, however for those who want the medical benefits of CBD (for example in the treatment of seizures) without getting high, separation is necessary.


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## Rosebud

That is way too complicated for me.. I just made a cbd tincture that tasted like heck, but is working for the patient.


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## greenfriend

Rosebud said:


> That is way too complicated for me.. I just made a cbd tincture that tasted like heck, but is working for the patient.



I'm sure it over the top for most, that why a lot of dispensaries in Colorado that are required to produce the concentrates they sell have a chemist on staff. A lot of patients want a precisely pure and consistent product, so I see high tech lab extraction and quality testing as the future of marijuana. 

I wish for the day that these extraction procedures are so ubiquitous that CA dispensaries can no longer rob patients blind selling shatter and cbd for $50-80/g


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## Soloma

greenfriend said:


> I completely agree with you, however for those who want the medical benefits of CBD (for example in the treatment of seizures) without getting high, separation is necessary.



Why not just use a plant that is testing out 19% cbd and >.00whatever% thc?

Once we get into this separation and keep saying that people want this or want that, it implants a suggestion into people that can not think for themselves. They figure since they are being told that other people want cbd strictly or single cannabinoids, they should too.

This opens the door to our disaster of a health care industry completely ******* up what has been working for so many other people. Just another way to give up our freedom, the future of marijuana, brought to you by those in charge.

No, thank you.

These are reasons why I think rso from a spagyric is so important. Alchemists say this tincture with the "body" or "salt" of the plant added back in is a more complete medicine that just a tincture. This medicine is synergistic with itself and us in so many ways, you will never get that by separating out single cannabinoids. You lose out on the potentials of intention and the placebo effect to boot.

All in all, I do not see any good coming from separation of single cannabinoids.


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## greenfriend

Soloma said:


> Why not just use a plant that is testing out 19% cbd and >.00whatever% thc?
> 
> Once we get into this separation and keep saying that people want this or want that, it implants a suggestion into people that can not think for themselves. They figure since they are being told that other people want cbd strictly or single cannabinoids, they should too.
> 
> This opens the door to our disaster of a health care industry completely ******* up what has been working for so many other people. Just another way to give up our freedom, the future of marijuana, brought to you by those in charge.
> 
> No, thank you.
> 
> These are reasons why I think rso from a spagyric is so important. Alchemists say this tincture with the "body" or "salt" of the plant added back in is a more complete medicine that just a tincture. This medicine is synergistic with itself and us in so many ways, you will never get that by separating out single cannabinoids. You lose out on the potentials of intention and the placebo effect to boot.
> 
> All in all, I do not see any good coming from separation of single cannabinoids.



First, no one has a plant with 19% CBD and 0% THC

Second, people do think for themselves and do ask for these products. I have owned 2 cannabis dispensaries, and I assure you my customers knew what they wanted without me telling them.

RSO is just another decarboxylated solvent extraction like BHO, nothing special.

I'm not sure what "alchemists" have to say about all this, but real chemists, you know the ones with a degree from a university, would tell you that your claims of lost "synergy", "potentials of intention", and placebo effect have no basis in actual science.

If someones seizures are remedied by pure CBD, why would you give them an extraction that is a mixture that included unneccessary components?


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## Soloma

> First, no one has a plant with 19% CBD and 0% THC



https://www.cannabis-seeds-bank.co....od-medicine-cbd-rich-blessing-/prod_4615.html

This just happens to note that the seeds in question are crossed from a 21%CBD, 1% THC plant. I had seen adds for other cbd that were in the 19% to 0% range on a seed bank I am sadly finding out might have been a scam. Below is a 19%cbd to 1%thc claim for the ac/dc strain. This being said, you are right, these plants if they are out there are going to be rare and hard to come by. The massive push towards cbd however will change this I am sure.

http://www.leafly.com/hybrid/acdc



> One remarkable characteristic of ACDC is its THC:CBD ratio of 1:20, meaning this strain induces no psychoactive effects. Tests have put ACDC&#8217;s CBD content as high as 19%, which helps many patients treat pain, anxiety, epilepsy, multiple sclerosis, and the negative effects of chemotherapy, all without intoxication.






> Second, people do think for themselves and do ask for these products. I  have owned 2 cannabis dispensaries, and I assure you my customers knew  what they wanted without me telling them.



My point was that people do what they are told by "authority" figures. As soon as the "future of medicinal cannabis" becomes this separation of single cannabinoids, people will go along with it as opposed to seeking the full spectrum of treatment the whole plant offers. It also stays controlled where I can not legally make my own medicine, because you know there is a buck to be made on these single cannabinoids.

By people blindly accepting this via our healthcare system, the chances are very high that my freedom to choose to self medicate will once again be impinged. So while your customers may very well know what they want w/o you telling them, there will be a very good chance that they are listening to someone or something else, like a govt entity.

So skip the decarbox and render the thc non psychoactive? THCA? My understanding of the rso process, the decarbox comes at the very end when the oil bubbles very tiny little bubbles. If this is the case and you dont want to be high, skip this step?



> I'm not sure what "alchemists" have to say about all this, but real  chemists, you know the ones with a degree from a university, would tell  you that your claims of lost "synergy", "potentials of intention", and  placebo effect have no basis in actual science.



Except there is quite a bit of science to support the placebo effect, not to mention some science on intention. Synergistic effects like thc having a different anti cancer effect then cbd. I recall reading that cbd has four or five while thc has one, and they are different. If I had cancer, I know I would choose the synergistic effects of the two cannabinoid compounds combined.

http://theintentionexperiment.com/wp-content/uploads/2011/01/germination-experiment.pdf


> A number of fascinating results emerged. Firstly, the experiment
> showed that the intention had a robust effect.
> As an overall average, the seeds sent intention grew 56 mm,
> compared with 48 mm for the non-targeted seeds. This means that
> seeds sent intention, on average, were 8 mm (about a third of an
> inch) higher than the controls. In contrast, the seeds run in the
> control Intention Experiments only varied by 2 mm.
> This effect was statistically significant (p<0.007). This means that
> there is a 0.7 per cent possibility that we arrived at this result by
> simple chance. Anything less than a p value of 0.05 is generally
> considered statistically significant.





> If someones seizures are remedied by pure CBD, why would you give them  an extraction that is a mixture that included unneccessary components?



I always hear opposition (to self medicating cannabis) saying you cant do this and consider it medicinal, you cant do that. It has to be isolated, quantified blah blah blah. Except there is no lethal dose and everyone can work up to their own appropriate dosages. I also think about what they have already done by singling out thc with marinol and such. Every time I read about it, I seem to find people prefer the whole plant. 

Is there any research on what cbd alone does to people, long term? Do we know for sure the other components are not necessary? Give me the full plant spectrum healing every single time because I know that it has history behind it not dollars, safe as can be. To those who do not want thc, use high cbd, low thc strains that are not decarbox`d? 

Seems simple enough to me without giving up my freedoms. My apologies though, I did not intend on hijacking the thread.


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## growhemp

Hello, wondering if you and I can talk directly. Please email me at [email protected] and i will email you my cell. Thank you for this post and your time. v


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## ShOrTbUs

have you tried super critical co2 extraction? i'm not sure how well it does with separating each individual compound. though, it has been touted as providing the most pure products.


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## Rosebud

Why would you want pure cbd?


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## Bongofury

My head is spinning..................


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## AluminumMonster

I have to agree with Rose. I've  been in the "industry" for a year now and have spoken with many cancer and epilepsy patients. Most of them tell me pure cbd or thc products aren't as effective as say a whole plant extraction that has all of the cannabanoids. There is a synergistic effect between all of the cannabanoids. 

Sent from my SM-N920V using Tapatalk


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## Rosebud

Exactly, I use Harlequin for RSO and it is 6% thc and 12% cbd.. It is the perfect 2/1 ratio and it really really helps patients. They  like it as it works and doesn't bother the marijuana naive.


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## lyfespan

greenfriend said:


> There are other ways to isolate these compounds (phase transfer catalysts), but an even better option is column chromatography.
> 
> But first, a word about decarboxylation. Whether to decarb can be debated forever, but if you do, it should be heated under nitrogen at 105C for 1 hour.
> 
> I like to use a non-polar solvent to extract and a polar solvent to wash. Besides butane, try propane, hexane, and chloroform (especially efficient). Absolute ethanol (200 proof) is my polar solvent of choice.
> 
> When you intend to isolate the individual cannabinoids you should stabilize the crude product. With the product dissolved in 100% EtOH before winterization, filter the solution through charcoal, extract with 2% sodium sulfate, then filter through charcoal again. This prevents oxidation of your crude product.
> 
> The odoriferous terpenes can be removed by steam or vacuum distillation. Cautious distillation in vacuo yields a fraction of crude red oil (bp 100-220° C/3 mm). This can be purified by redistillation or column chromatography. Use ethanol to remove the residue from the flask while it is still hot. Filter the solution through charcoal, and strip the solvent. Distill the residue to yield pure red oil (bp 175-195° C /2 mm). Distillation must be stopped if smoke appears, indicating decomposition.
> 
> Because THC is heat-sensitive, it is preferable to isolate the cannabinoids by column chromatography. The simplest method of column chromatography is performed with ethanol and ether extracts of hemp on alumina, yielding two major fractions: (1) chlorophyll, CBD, and CBN, and (2) THC. A second, more difficult method is performed on Florisil (use 10 times the weight of the oil) with the solvent system hexane:2% methanol. This yields a doubly-concentrated, viscous oil which can be repeatedly chromatographed on alumina to separate the THC and CBD. The CBD fraction of column chromatography can be distilled (bp 187-190° C/2 mm; pale yellow resin) to purify it.


i was just reading on sigma aldrich about the use of chloroform for extraction, and fractional distillations.i think ill stick to the distilling our own n butanes  and using  rosseville ethyl 200.

you following the limonene extractions?


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## EugeneOregon

Here is a demonstration of producing nearly pure thc from an extract.

This ia a chromatography run that demonstrates a much less than perfect setup that produced the fraction shown in the youtube thumbnail for the video. Vaping this pale yellow and sticky substance confirms it is nearly pure thc. Until you do your own chromatography you will not realize how much chlorophyll there is! The green fraction in the video when purged of solvent is a black tar that smells nasty.

This run demonstrated that I need to pack the column tighter, however it is a Dry Column Vacuum Chromatography (DCVC) mode and banding does not present a real problem because the solvent gradient is continuous and thr columns are sucked dry.

This is precisely how to purify an extraction into nearly pure thc if you are on a budget. The second video is the "go to" video if you want yo learn how to do this. It was the second  video that showed me how to start doing this and full credit to those guys!



https://www.youtube.com/watch?v=6A6CXRbKJeA
http://curlyarrow.blogspot.com/2017/02/dry-column-vacuum-chromatography-dcvc.html 

View attachment IMG_0121.jpg


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## EugeneOregon

greenfriend said:


> There are other ways to isolate these compounds (phase transfer catalysts), but an even better option is column chromatography.
> 
> But first, a word about decarboxylation. Whether to decarb can be debated forever, but if you do, it should be heated under nitrogen at 105C for 1 hour.
> 
> I like to use a non-polar solvent to extract and a polar solvent to wash. Besides butane, try propane, hexane, and chloroform (especially efficient). Absolute ethanol (200 proof) is my polar solvent of choice.
> 
> When you intend to isolate the individual cannabinoids you should stabilize the crude product. With the product dissolved in 100% EtOH before winterization, filter the solution through charcoal, extract with 2% sodium sulfate, then filter through charcoal again. This prevents oxidation of your crude product.
> 
> The odoriferous terpenes can be removed by steam or vacuum distillation. Cautious distillation in vacuo yields a fraction of crude red oil (bp 100-220° C/3 mm). This can be purified by redistillation or column chromatography. Use ethanol to remove the residue from the flask while it is still hot. Filter the solution through charcoal, and strip the solvent. Distill the residue to yield pure red oil (bp 175-195° C /2 mm). Distillation must be stopped if smoke appears, indicating decomposition.
> 
> Because THC is heat-sensitive, it is preferable to isolate the cannabinoids by column chromatography. The simplest method of column chromatography is performed with ethanol and ether extracts of hemp on alumina, yielding two major fractions: (1) chlorophyll, CBD, and CBN, and (2) THC. A second, more difficult method is performed on Florisil (use 10 times the weight of the oil) with the solvent system hexane:2% methanol. This yields a doubly-concentrated, viscous oil which can be repeatedly chromatographed on alumina to separate the THC and CBD. The CBD fraction of column chromatography can be distilled (bp 187-190° C/2 mm; pale yellow resin) to purify it.



Here is one of my chromatography runs done in preparation for molecular distillation using a modified kugelrohr concept. Then I post the tech video to set up for  molecular distillation. Finally time lapse of the distillation proceeding. If you look close at the time lapse you will see that the boiling flask bumped some contaminate into the collection bulb. This happens often on the first pass. I place the collected bulb into a new boiling flask and use a hand torch to heat the extract and thusly transfer it into the new boiling flask. This avoids passing any extract across a vacuum grease joint. .then I run it through again then sometimes again. Each run through the rig progressively refines the extract closer to absolute. These are gram sized quantities.

Semper Fi

https://www.youtube.com/watch?v=BIsiCfcLBL4
https://www.youtube.com/watch?v=D-A-ZsU8ZxQ
https://www.youtube.com/watch?v=uBpuKVaXynE


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