Isolating Cannabis Terpenes: Full Spectrum Cold Distillation.

Hey pangea.... Are you still in the boat that believes the guild and others are doing slow crystallization.

I'm still skeptical of how it's being done however to support your theory i've seen some instagram comments stating that the pure crystals take a LONG time to make..

Im not aware of another method that would produce single large crystals, takes time, they make competitions out of it in schools.(not thca)

Pangea said:

Im not aware of another method that would produce single large crystals, takes time, they make competitions out of it in schools.(not thca)

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Couldn't they be extracting large amounts of thc-a through column chromatography or acid/base extraction and then recrystallize from that point on?

I just can't imagine a finicky method such as recrystallizing from a varying mixture of BHO extract in large quantities. It just seems like it would be hard to scale up that method.. although it has been proven to work of course.

What do you think? Combination of extraction and recrystallization, or just scaled up and finely tuned crystallization out of extract soup?

They could be, but what method / solvent did they use to obtain their starting solution for the column separation? The higher the starting purity when forming crystals the better, and column separation is a additional step to get a higher purity, but we know that extracting with butane at subzero temps can produce a purity to allow sufficient seeds to form.
It may be finicky, but there is little to no loss, what ever doesnt crystallize is just purged as reg bho, its incredible easy to scale up. Its all similar paths to the same end, which is large crystals.


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Back to terpenes,

Im getting closer to being able to order some parts and pieces, im thinking dry ice milling to open up the trichs would be a good to express terps in a "low volatization" manner. Pretty sure if cold vac distilling without water you'd want a dry ice condenser.

Pangea said:

we know that extracting with butane at subzero temps can produce a purity to allow sufficient seeds to form.
It may be finicky, but there is little to no loss, what ever doesnt crystallize is just purged as reg bho, its incredible easy to scale up. Its all similar paths to the same end, which is large crystals.

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But with the amount they seem to have, surely at MOST they attain a few seeds from tane soup. I'm leaning towards high quality bho or winterized with secondary solvent, and than ran on a chromatography column. Final recrystallization for big, sexy crystals is slow evaporation of some sort...could even be butane recrystallizations after column chromatography.

Pangea said:

They could be, but what method / solvent did they use to obtain their starting solution for the column separation? The higher the starting purity when forming crystals the better, and column separation is a additional step to get a higher purity, but we know that extracting with butane at subzero temps can produce a purity to allow sufficient seeds to form.
It may be finicky, but there is little to no loss, what ever doesnt crystallize is just purged as reg bho, its incredible easy to scale up. Its all similar paths to the same end, which is large crystals.


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Back to terpenes,

Im getting closer to being able to order some parts and pieces, im thinking dry ice milling to open up the trichs would be a good to express terps in a "low volatization" manner. Pretty sure if cold vac distilling without water you'd want a dry ice condenser.

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Yeah a cryogenic grinder / freeze mill / cryomill.
Had a few ideas and can easily swap or replace steps with other methods:
1. Dry sift to isolate resin heads or ice water extraction if going with cold distillation process.
2. Rosin Press the sift to break open trichromes or add alkaline water to emulsify
3. Freeze dry Rosin or cold vacuum distill the emulsification
4. Cryo / nitrogen cold trap terpenes
5. Open cure terpenes to release monoterpenes

But with the amount they seem to have, surely at MOST they attain a few seeds from tane soup. I'm leaning towards high quality bho or winterized with secondary solvent, and than ran on a chromatography column. Final recrystallization for big, sexy crystals is slow evaporation of some sort...could even be butane recrystallizations after column chromatography.

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Could be, wish they'd be more open about it, all we can do is speculate and do/try it ourselves. I havent tried to recrystallize large singles with pure butane, its to hard to control evap over long times properly ime, but it works great for quick recrystallization.
Always be sure to use a fume hood.

Yeah a cryogenic grinder / freeze mill / cryomill.
Had a few ideas and can easily swap or replace steps with other methods:
1. Dry sift to isolate resin heads or ice water extraction if going with cold distillation process.
2. Rosin Press the sift to break open trichromes or add alkaline water to emulsify
3. Freeze dry Rosin or cold vacuum distill the emulsification
4. Cryo / nitrogen cold trap terpenes
5. Open cure terpenes to release monoterpenes

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Yes sir lots of paths to get to the same end. Good ideas!
I prefer the idea of starting with as little handling as possible, having to sift or extract in any manner rather than start from whole flower will result in losses or inefficiencies. Breaking up herb to sift and sifting usually smells way to good!
Using compression like a rosin press to express the trichs is also a good idea, they make pill press molds with vac line attachments for removing and/or capturing gasses when compressing. There are a few methods of compression that could be used to express, but all seem difficult to do efficiently. Roll press's, plunger press, expeller press, plate press, all will do the trick to express terps, but doing so in a low or no oxygen environment while capturing / vac'ing the volatilization is or would be tricky. Which is why I like the idea of flash freezing a decent amount of herb with dry ice and paddle blending to a fine powder in a vac chamber, a proper ball mill or cryomill is probably over kill for such a delicate herb. Its going to be interesting to see either way, but Im figuring water is going to be quite helpful for cold temp distilling, at least with my not so powerful cps vac pump

You must follow church to suggest to open cure to release mono's? The harsh mono's are precious but so harsh, its an interesting situation, we obviously dont want to remove them all, but just enough to make it palatable, the excess could be used in a few manners not needing to be heated and inhaled.



Who's going to have the first seed catalogue with scratch and sniffs?

Both "Tony" and "K" at trichome technologies have told they they have filed seperate patents for some sort of cold trapping terpene collection method. Just because you can't find the patent applications does not mean it has not yet been filed. Maybe patent pending? Both Tony and K are friends of mine they both will enforce their patents if and when granted. I wish they would both be more open but it is their work.
On a side note, I have yet to smell any Cannabis extracted terpenes that are as loud as the terpenes in a fresh living Cannabis plant. I want to see GC-FID terpene analysis of the fresh plant and the extracted terpene suite oil side by side to see what any differences are, but they are different. I knew in 2000 when we, RCC and myself with others helping, discovered the modifying and potentiating effects of terpenes, that terpenes would shake the Cannabis world. We have just scratched the surface, both in which terpene or combo of terpenes in what ratios does what, as well as how to breed Cannabis to have just the desired terpenes in the correct ratios and no others that are unwanted for that goal. I am still looking forward to single terpene plant varieties high in THC and only one terpene so patients and rec users can judge for themselves which terpenes are wanted in what ratios for what, be it for medical or rec. If we had a variety high in THC with only limonene, another variety high in THC with only B-myrcene, another with high THC and only linalool, etc, etc, etc, then the herbal materials could be blended to find combos and ratios of the terpenes that are desired most as well as determining which terpenes are not wanted for specific goals. Then you can breed varieties with exactly what terpenes you want in the ratios you want with no unwanted terpenes for that goal. It is a new world. And DNA research will help to speed this work for sure.
-SamS

they have filed seperate patents for some sort of cold trapping terpene collection method. Just because you can't find the patent applications does not mean it has not yet been filed. Maybe patent pending?

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I'd be very surprised if they have come up with a unique enough concept for cold trapping or similar in order that it would be patentable.
The maximum time for an application from filing to being made public is 18 months, when applications are published in the Gazette.
So much of this tech is well established, (not patentable) but R&D is expensive so nobody wants to share their techniques.

They Cannot use the "Patent pending" title until a patent has been examined, prosecuted and approved by the examiner.

RB

edit: Just to note: Tony responded via a different platform to the initial part two post, I wrote this post before I read his response.

Both "Tony" and "K" at trichome technologies have told they they have filed seperate patents for some sort of cold trapping terpene collection method. Just because you can't find the patent applications does not mean it has not yet been filed. Maybe patent pending? Both Tony and K are friends of mine they both will enforce their patents if and when granted. I wish they would both be more open but it is their work.

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As Ricky said here and I in the other thread, the patent publishing date usually takes 18 months after submission. I dont doubt they have filed patents, anyone can file a patent for anything, its called patent trolling and is a huge issue. I, like Ricky, question the defend ability of their process, if they are indeed as you mention patenting a "cold trapping" method I think it will fall into the previous art, obvious, or public domain area, its why I mention Freeze Pump Thaw, its a fundamental and open degassing process. Its a messy thing patenting process that are fundamental to an community/industry, especially when its a simple and obvious and prevents others from access.

I can appreciate when friends make decisions or act in manners that are unbecoming, business, profit, investor and "duty to the shareholder"(Tony quote) influence start to creep into the mix it becomes ugly and uncomfortable.

Everyone seemed to jump down Matt Rhize(sp) throat and believe and say all sorts of things publicly, all because his concentrates are sold for very high dollar amounts per gram. Matt and Cuban got into it pretty good on HC about it, everyone had their say and shit on Matt for his high prices. I couldnt agree more, but its obvious that certain products will demand and fairly deserve a higher price, such as high purity dry sift. Even with such rare products those with scruples find ways to improve the standard situation, such as Cuban refusing to sell to clubs whos standard 100-500% markup only fucks the end user, he thwarts that by selling direct because he can, that is commendable!

During that heated discussion I remember a few on the panel chiming in to put Matt down over the price and product he was moving, $200+ per gram for water hash is insane. I didnt notice Tony chime in to much. Which I presume was because he didnt want to draw unneeded attention to the fact that his Prana line of edible oil infused cannabis has MSRP prices ranging from $120 per gram to $300 per gram I dont care what they spent on R&D, eat those costs or amortize them over 10 years of profiting, dont charge $300 per gram for edible oil infused product as a medicine. That deplorable and indefensible.

I love the way the Prana line is set up, it does make it somewhat more understandable for a patients, as well as makes it very nice for trying out different solutions for people to find solutions to their ailments.

Everything Ive watched and heard from TV has given me the impression he is a good dude, and is a true cannabis lover, but as I said we must check our selves and I guess also check our friends as we step further into the murky waters of a legalization and regulation we must as a community and voice of a plant ensure that legal cannabis is as much or more of a revelatory and revolutionary force as it has been for society and community as well as our personal minds. The legal world we are moving into is rife with inequality and corruption, many already in the thick of that have no qualms trying to bring cannabis down into that and are making a quick buck no doubt. Cannabis can stem all of that, imo, its the vaccine that can cure our societal and environmental suicide.

Plant fields and greenhouses bring the price down, if you cant do that without charging extreme amounts of money to build the funds, stepping on the neck of the sick, then you shouldnt do it at all, someone else will do it without compromise.

On a side note, I have yet to smell any Cannabis extracted terpenes that are as loud as the terpenes in a fresh living Cannabis plant. I want to see GC-FID terpene analysis of the fresh plant and the extracted terpene suite oil side by side to see what any differences are, but they are different. I knew in 2000 when we, RCC and myself with others helping, discovered the modifying and potentiating effects of terpenes, that terpenes would shake the Cannabis world. We have just scratched the surface, both in which terpene or combo of terpenes in what ratios does what, as well as how to breed Cannabis to have just the desired terpenes in the correct ratios and no others that are unwanted for that goal. I am still looking forward to single terpene plant varieties high in THC and only one terpene so patients and rec users can judge for themselves which terpenes are wanted in what ratios for what, be it for medical or rec. If we had a variety high in THC with only limonene, another variety high in THC with only B-myrcene, another with high THC and only linalool, etc, etc, etc, then the herbal materials could be blended to find combos and ratios of the terpenes that are desired most as well as determining which terpenes are not wanted for specific goals. Then you can breed varieties with exactly what terpenes you want in the ratios you want with no unwanted terpenes for that goal. It is a new world. And DNA research will help to speed this work for sure.
-SamS

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Word to the bird, looking forward to see how fast and where we'll be in a year from now.
As always much love and thanks for your contributions!

edit: Just to note: Tony responded via a different platform to the initial part two post, I wrote this post before I read his response.

I am striving for constructive criticism not just stiring shit at one group, I specify Blue River now specifically because I believe there is probably more to them than the average large cannabis corp, such as what we see in Canada's LP's.

For posterity and non facebookers:

Tony Verzura Interesting read and decent analysis of what info has been shared on what you watch on Hash Church. So since you specifically named Blue River you know I'm going to have to comment... obviously smile emoticon. Firstly, there are many ways to isolate terpenes or full spectrum terpenes using setups like this, steam, cold traps, fractal, solvents, etc. At the end of the day the terpenes present in the plant are what they are and you can't magically extract more. Just like resin. You either did a good job as a farmer or you didn't we know the truth when we extract the resin. On cost: The cost of blur river terpenes is 100% dictated by the cost of the flowers. We pay 1600 to 1900 for a lb of sun grown organic clean product as Grade A. We sell 50% of our terpenes via wholesale, include shipping, taxes, all major credit card processing fees, refunds, replacements, staff, overhead, events, etc. We offer discounts on volume as well. We are currently working on Grade B and a new split program to try and offset costs as much as possible. I support local growers and quality so we prefer buds vs trim run. If your truly doing your homework you would discover that "10 drops" is not the same as the next guys "10 drops". What I mean is we consider 10 drops as .25ml. Terpene density is 50% less then water. 20 drops of water equals 1ml. Terpenes bc they are less dense then water would have about 40 drops per 1ml. Nearly everyone that is selling terpenes aren't selling them at .25ml / 10 drops. They are selling them at .2ml to .15ml. So if I sell $60 .15ml "10 drop" vials your actually paying 60 for 6 drops of Blue River. I sell 85 to 100 / .25ml with 10% of each step up... .5ml... 1ml on volume. Your actually paying more. If your paying for 70 for .2ml / 10 drop thats actually 8 Drops of Blue River again same price. If I were growing my own I'd 100% reduce my cost but unfortunately I'm not. I think when you look at the value of 1lb of good herb you will find an average of 1800lb or more right now in CA or even 3000. If flowers average 1% to 3% terpenes alive and dry .1% - .3% they will hold a certain value directly related to the cost of cannabis. You want to lower the cost start with the cost of herb. I personally lived thru the CO race to the cheapest herb and no offense the quality went with it. When I said I support local growers I mean it. I pay a premium for premium product to help support and reward them for what they do. If you buy blue river your supporting local farmers period. Your supporting the products we stand behind because of the quality throughout the process. Kind of like apple... it's expense but they are built with a service and software to support the hardware. I've had my funds and packages take 2x and told the feds to release my packs and they did. I have banking, shipping, processing, etc and it cost us in the process. So it's not like I'm making it rain our here... well.. maybe making it rain terps lol. Lastly... patents IP etc.... part 1

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Thanks for sharing all that information. My critiques or issues brought up in my post are not really touched on in your part one post. I can appreciate and understand that you are middle manning and the cost involved with operating. I too run a cannabis organization, though small its not easy. I do not expect anyone to do anything at a loss to themselves monetarily. As an aside to the overall conversation, I have done my "homework" on what a drop does or doesnt represent, Its like selling a bag of potato chips and labeling it by how many individual chips are inside, aka basically useless. Label your terps by milligram, gram or kilo, I cant imagine any acceptable reason not too.

The specific issue is about not sharing a safe method of cannabis based terp extraction when acknowledging there is rampant use of unsafe terpenes being sold to cannabis users. Your secrecy for profit while talking about others using contaminated products.

Part 2... I don't have a provisional patent application in for terpene extractions. I believe someone else else has that patent application in. There are many ways to extract terpenes and I don't believe basic science and reconfiguration of such existing apparatus for cannabis terpenes extraction would hold up thru the patent process. I could be wrong but idk I think if you focus on what you know the most and perfect it your probably ok. If you have access to terpenes that aren't yellow,cloudy, use solvents, bubbles or other floating objects in them and your experience on the nose and tongue are of pleasure your probably all right. It's the cats using terpenes they buy not extracted for cannabis only that I have concern about. Do I think steam distillation is actually harmful when don't properly and purified abosulltey not. You would see me blasting folks like gemstone but I don't. I don't grow my own so I guess I'll always be on the higher side but I offer refunds and replacements so from my perspective I don't see huge profits rather the unilateral support to the farmer and the brands we utilize our terpenes into. The public company I own has a provisional patent that was accepted and public domestically and internationally for the Prana. That covers various extraction methods and uses of cannabinoids, specific ratios, cannabis derived terpenes, in a specific caporic fatty acids, lipids, etc. The patent does cover the use of cannabis terpenes in capsule, sublinguals, topicals, and as a diluent in vaporization. So technically if your using terpenes as a diluent in Rosin, co2, hydrocarbons vape pens dabs etc technically it would be in violation of the patent. However, I didn't take this medicine and idea into patent and go public to go after ANYONE in the industry. Rather give everyone who wanted to support our mission of Prana, blue river, and bubbleman they could buy stock and help us fight pharmaceutical companies from coming in and taking out farmers, processors, and centers. The whole idea was create unity in the fight. For every gram, every drop, every capsule we sold we could strengthen our position to protect them from patenting everything and taking it away. I'm not sure anyone gets that but that was the point. You don't see me sending letters out to stop anyone and I certainly can't teach people to do it either bc i could be sued from my shareholders. I'm stuck but I'm not fucked. I also think it's not fair to call me out as if I'm someone who doesn't share info especially on hash church. All I do is share. In fact I shared a near identical setup on hash church for cold trapping and said I didn't use this method to extract terpenes but you could... you just needed to use your imagination. smile emoticon it looks lime your doinh thst which is cool. you can do it other ways too and I think a general concensus was made Sunday. We want 100% cannabis derived terpenes that have been safely purified for vaporization not individual terpene standards or combinations and certainly can't have solvents used in the process. Support your farmers, support your extractors, support what represents what you believe in. If you support blue river awesome if you don't ok there are others but don't just call us out as if we are rapping people bc it's nothing further from the truth. If I didn't go live with Blue River and fight thru card processors, shippers, and the laws all out of my pocket would we even be having this discussion. I could of stayed quite like I had been since 2014 awards in AMS making products and people never knowing. Instead I opened that can of worms. I pushed the envelope and hoped to inspire others. Which is what just happen to you in this project. If I could sell them for less I would I just can't so love it or hate it I'm doing the best I can.

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I was under the impression you had filed a patent relating to terpene extraction based on your reddit post from a few months ago. Your first sentence: "I am Tony Verzura the guy who actually invented the process, and owns the patents on the use of the terpene extraction. " I can see now that you meant the use of terpene extract? Skunkman said: "Both "Tony" and "K" at trichome technologies have told they they have filed seperate patents for some sort of cold trapping terpene collection method."

Either way you dont believe such simple, basic or obvious process will hold up as patents, prior art, obviousness and public disclosure would prevent it from being a solid patent.

But somehow what you have patented doesnt deserve the same attitude?

The patent does cover the use of cannabis terpenes in capsule, sublinguals, topicals, and as a diluent in vaporization. So technically if your using terpenes as a diluent in Rosin, co2, hydrocarbons vape pens dabs etc technically it would be in violation of the patent.

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Road to hell is paved with what? If you want to protect the cannabis community from big pharm or big corps then you would publically disclose what you would normally intend to patent. Duty to the shareholder comes second to the cannabis user/patient in all cases no exception. You are talking about fundamentals to cannabis use. Your repute or anyones should not have to enter the equation on such matters. Patent law more than allows and provides this.

Steam distillate of cannabis terpenes predate you and Blue River, Patents on Hot Gas extraction specifically for static and continuous terpene isolation are held by GW and have been for close to 20 years. We would be having this conversation if blue river didnt exist or your isolates, you just happen to be the first to do it in such public, scaled and open manner. Your can of worms is not yours and your secrecy "inspiring" others to waste the same time, money and efforts that youve already spent is the definition of redundancy and stifling of progress. Progress that would have prevented orange cleaner terps or 95% food grade terps from inundating the market.

You don't see me sending letters out to stop anyone and I certainly can't teach people to do it either bc i could be sued from my shareholders. I'm stuck but I'm not fucked. I also think it's not fair to call me out as if I'm someone who doesn't share info especially on hash church. All I do is share.

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Your patent wont hold weight, and your lawyer fee's would destroy you if you did try to enforce it. Basically its looks good on paper for your investors, one of the two main uses for patents; investor/shareholder appeal.

To say you could not have taught people your method or a method like the one ive share is the perfect example of why you cant trust a public corporation, your duty and fear of the shareholder trumps community standards. Im reminded of Sagans Mr. X and the McKenna Bro's Oss and Oerik and others who've shared information when they werent suppose to, except they faced a lot more than possible shareholder rebuke.

Do we need to bring up Prana's MSRP for 10mg capsules per gram of cannabinoid? I think I covered that in my previous icmag post.




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posting here for posterity and those that dont have facebook

Sam_Skunkman said:

-SamS

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Am I incorrect in thinking that gas chromatography won't accurately quantify things as volatile as monoterpenes?
Also, Sigma terp standards from what I saw were like $60-70 per ml.
I'm sure I could do the molar math, but how much does a ml weigh? Of each: monoterpenes, sesquiterps, etc

Wrong...
We used GC-FID for the last 25 years, that is the very best way for analysis of terpenes that I know of. Get the recent paper below:

http://www.ncbi.nlm.nih.gov/pubmed/26651562

Or how Mark did the work for the paper:

http://www.medicinalgenomics.com/cannmed2016-videos/

See video
Playlist
#15 Mark Lewis

Thanks Sam! Fantastic presentations all around from what I've so far seen.
I really, really, really ---did I say really? --- like Mr. Lewis's cultivar classification method. So much sense in it.

I missed Pangea's post, looks like he answered my question and then some (via Tony's facebook)

Ive just been using steam and having fantastic results. Ill post some of my profiles when they arrive back from the lab.

Pangea said:

Tony Terp on reddit:


Prana about:


Read the bolds a few times.

How cold? Who knows, cold enough not to cause any degradation, im shooting for 20oC to start. You want to at least be able to boil water at the temp you are shooting for, everything that we are aiming to boil is lighter than water.

Nitrogens importance, no idea, all I know is I dont want anything exposed to oxygen so when I am expressing I want to flush out and fill with nitrogen. Maybe Tony's bubbling with it as well, not sure what all the possibilities could be?

The best way I can figure to express any aromatic in a controlled manner, is in a ball mill jar that has a two valve ports, one for a vac line the other for gas flushing.

The cold trap better be 99+% efficient as well.

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You're onto something here. Could never get very far form his hints, thanks for much for sharing.

On the topic of the THC-A crystals again, couldn't it be they are doing a NAOH to HCL reaction and then taking that powder, rewetting with limonene or ETOH and then re-x from there?

And a method for cold distilling terps.. could one take the water from making bubble hash, put into a container in a vacuum oven that is connected to a cold trap and vacuum pump, and collect the terps in the cold trap? The water would boil at room temperature and could even be heated, and would allow the terpenes to boil off as the water starts to..

One could def be re-x from a powder or as mentioned recently in the crystal thread just re wetting a winterized absolute.

Re: Terps from bubblehash, one could do that but probably not the best route imo.

I should have linked this thread to the newer, part 2, thread: https://www.icmag.com/ic/showthread.php?t=326869

Has anyone found a better way? Blasting material putting it in a vacum with cold trap seems to be the only way i have seen results terpine rise.. The material that is left behind still stinks up the naborhood what then is their another way to further extract terpines left in plant material becuase it just a head ack trying to save terpines of difrent flavor with selfs raked up with diffrent strains. What about in the fractions that ruber smell how do seperate them their or in you ethanol i wash the remaining glass with ethenol in bho extraction all the vesells that are used to grab a few grams from the walls not the science glass but the bho vesells as the ethenol is seperated from the material im left with ethenol that smells like dank what about then.. Is ther a way to separate terps from ethenol??If anyone got some insight please help. This is fucken crazzy im out thank amyways jumping on another forum hoping to do rnd