Sciencemadness Discussion Board - CBD THC extraction

hello,
I have bio mass which have 19% CBD and 0.78% THC which is legal.
If i do ethanol extraction, and concentrate the ethanol until no more ethanol, which % of THC and % of CBD i would obtain? Let's say i will only have CBD and THC and nothing else...

You could theoretically get 100% yield, what ethanol percentage are you using? We always use Isopropanol because of the 0 sugar content. The issue with using polar solvents to extract THC/CBD is you also end up with all the polar crap from the plant. Stuff like chlorophyll, colour, smell, taste, this actually lowers your concentration.

The use of non-polar solvents extracts only the fats and non-polar compounds from the plant. Common in industry for making some extracts is butane, I have purchased shatter here that has been as high as 87% THC in a 1 gram portion, they cure it for 100hrs in a vacuum to ensure all the butane is gone, though that is industry to ensure its legal for sale. Butane is so volatile, most people who make it at home don't cure it at all the they just heat and mix it well. Another common solvent used for making honey oil is hexanes. One method I am not familiar with but I hear works very well is CO2 extraction.

I really suggest finding some isopropanol 99% works best, but ethanol will work too. I just chop the buds up and don't let it soak too long, cannabinoids are very soluble in alcohol and dissolve quickly whereas the polar stuff takes longer so to minimize extraction of that crap do a a couple quick washes with smaller amounts of alcohol, this will maximize cannabinoid extraction and minimize polar extraction.

Edit: If you choose the non-polar solvent method, after extraction put the solvent in a freezer, this will precipitate out the extra non-bioactive lipids then decant solution, it will increase concentration of the cannabinoids.

[Edited on 22-3-2020 by Syn the Sizer]

[Edited on 22-3-2020 by Syn the Sizer]

njl - 22-3-2020 at 11:53

@chemistry007 @syn very good recommendations syn! If you're not worried about other organic contaminants, 99% isopropanol is definitely the way to go. Not sure about availability for you due to virus/location, but I can get it at CVS.

Syn the Sizer - 22-3-2020 at 12:49

Quote: Originally posted by njl

@chemistry007 @syn very good recommendations syn! If you're not worried about other organic contaminants, 99% isopropanol is definitely the way to go. Not sure about availability for you due to virus/location, but I can get it at CVS.

Thanks I have my CannasellSk licence to work in the legal weed industry so I had to take a course on all of that, well some of that, some of it is self taught.

Here Isopropanol is scare in the pharmacies due to virus, but the farm and garden centre here has boxes of 4L jugs 99%, and 4L jugs 29% H2O2 for $30.

chemistry007 - 22-3-2020 at 15:41

The use of non-polar solvents extracts only the fats and non-polar compounds from the plant. Common in industry for making some extracts is butane, I have purchased shatter here that has been as high as 87% THC in a 1 gram portion, they cure it for 100hrs in a vacuum to ensure all the butane is gone, though that is industry to ensure its legal for sale. Butane is so volatile, most people who make it at home don't cure it at all the they just heat and mix it well. Another common solvent used for making honey oil is hexanes. One method I am not familiar with but I hear works very well is CO2 extraction.

I really suggest finding some isopropanol 99% works best, but ethanol will work too. I just chop the buds up and don't let it soak too long, cannabinoids are very soluble in alcohol and dissolve quickly whereas the polar stuff takes longer so to minimize extraction of that crap do a a couple quick washes with smaller amounts of alcohol, this will maximize cannabinoid extraction and minimize polar extraction.

Edit: If you choose the non-polar solvent method, after extraction put the solvent in a freezer, this will precipitate out the extra non-bioactive lipids then decant solution, it will increase concentration of the cannabinoids.

[Edited on 22-3-2020 by Syn the Sizer]

[Edited on 22-3-2020 by Syn the Sizer]

Syn the Sizer - 22-3-2020 at 17:33

But i heard that IPA is not safe as EtOH is it.

Safe as in what? health? volatility?

Butane extraction for large volume need special extraction...you cant let it evaporate...

How much are you extracting? I have know people to do a few ounces at once and just let it evaporate in a well ventilated area like outside.

How long you think i can let the trim in ethanol or IPA? 1 day? Do you do twice the extraction or you think once is enough?

I would chop up the bud and let it soak in alcohol for a few minutes, then pour it off, do that 3 times. Do not let it sit for 1 day or you will end up with lots of unwanted polar crap, you will get some either way but the shorter you let the bud sit the less polar compounds. It really doesn't take long to for the cannabinoids to dissolve into the alcohol.

I dont think i can get 100%... let say how i calculate...lets say i have 100gr of trim, if 19% is CBD and 0.8% is THC i get 19 g of CBD and 0.8 g of THC. So if i concentrate the things to have double concentrated, i may have 38% of CBD and 1.6% of THC....you know what i mean?

Sort of, lets use 10g of your flower as an example. for every gram of flower you would have 0.190g or 190mg of CBD and 0.078g or 78mg of THC. so in 10g of bud you would have 1.9g of CBD and 780mg of THC. Now lets say you got your theoretical 100% yield and the final mass of extract weighed 3.8g. Your extract would then be 50% CBD, 20.5% THC and 29.5% other stuff.

[Edited on 23-3-2020 by Syn the Sizer]

chemistry007 - 23-3-2020 at 00:47

Safe as in what? health? volatility?

Health...i read it some where and as drinking EtOH is not that toxic, drinking IPA should be, but it's true that IPA is not toxic...so dont know why they say that.

How much are you extracting? I have know people to do a few ounces at once and just let it evaporate in a well ventilated area like outside.

10 kilo of bud and things like this...I did it for few grams, like 100...200, it s good, but if you want larger you need lets say pro tools...you can find them in ebay, but they are around 1000 USD and i may fear working with butane in appartement.

I got your point of view now...except that in my case i think you make a mistake: your calcul is like i have 7.8% and not 0.78%
But i get the idea that the end mass is not anymore 100g, but much lower.

[Edited on 23-3-2020 by Syn the Sizer]

Syn the Sizer - 23-3-2020 at 08:04

Yes IPA is toxic to drink but you are not drinking it, its 99% IPA and 1% H2O. The IPA fully evaporates so there is none left and you will not be consuming any of it.

Ok, 10kg is a fair bit, what are you extracting from that much for? And where do you live that you posses 10kg of biomass (you don't need to answer that). Even in Canada we have restrictions on the amount a person can posses.

Yes you are correct I looked at my math and I did calculate for 7.8% not 0.78% so your mass of THC per gram would be 0.0078g or 7.8mg, but you still got the idea.

chemistry007 - 23-3-2020 at 08:27

I have more than 10k, i am company, i can buy large, the matter is the % of THC, it should be low.
First time i tryed to separate the CBD and THC with distillation...big bad smell, like cat pee...then i solved the smell and go further, but got red-violet stuff which looks strange. I did TLC on it and saw different spot...so not pure...So finally i drop the idea of distillating it and tought to maybe chromatography them to separate....but didnt done it yet.
So now i try to concentrate the ethanol extraction to have normal oil concentrate...
As last workiup i pass the ethanol oil trought active charcoal to remove the green color which works not bad, but i sppose i lost some product...

Syn the Sizer - 23-3-2020 at 09:12

I have more than 10k, i am company, i can buy large, the matter is the % of THC, it should be low.
First time i tryed to separate the CBD and THC with distillation...big bad smell, like cat pee...then i solved the smell and go further, but got red-violet stuff which looks strange. I did TLC on it and saw different spot...so not pure...So finally i drop the idea of distillating it and tought to maybe chromatography them to separate....but didnt done it yet.
So now i try to concentrate the ethanol extraction to have normal oil concentrate...
As last workiup i pass the ethanol oil trought active charcoal to remove the green color which works not bad, but i sppose i lost some product...

If you are a business, I would invest in the professional equipment. I don't know about the laws in your local but here you need to use the professional equipment in a sterile environment if you want to sell it for human consumption. Aside from that I only produce for my own personal use.

The only way you are really going to get away from the green colour and smell and taste is non-polar solvents.

[Edited on 23-3-2020 by Syn the Sizer]

chemistry007 - 23-3-2020 at 12:09

Yes, but befor going comercial way, i need to test it to see if it works.
So you suggest Hexane, in same way as ethanol, except hexane? Why there is not that much peole are using it? except that it's more toxic than ethanol...
I find in my archive a picture which is interessting, but dont know where i take it...i must google it to find the source, but you can see that hexane is clear but acetonitrile which is polar is same...So maybe it's about a protic and protic solvent...

chemistry007 - 23-3-2020 at 12:23

I foudn the source: https://blog.restek.com/medical-marijuana-solvent-extraction...

It shouwn that hexane is not that bad, but MeOH is the best. Strange thing is that in the study, the % of CBD is less than 0.1%...maybe because of the strain...

Syn the Sizer - 23-3-2020 at 16:12

Yes, but befor going comercial way, i need to test it to see if it works.

Valid point.

So you suggest Hexane, in same way as ethanol, except hexane? Why there is not that much peole are using it? except that it's more toxic than ethanol...

Because most people use butane or even propane for non-polar solvents, its called BHO or PHO butane honey oil or propane honey oil. Both butane and propane are easier to source for many people than hexane.

The other reason is because if they are not using non-polar solvents they are using methods like cold/hot press methods or steam distillation for pure distillate. Using alcohol to extract cannabinoids from cannabis is kinda gone they way of the dinosaurs.

Dr.Bob - 2-4-2020 at 16:55

First time i tryed to separate the CBD and THC with distillation...big bad smell, like cat pee...then i solved the smell and go further, but got red-violet stuff which looks strange. I did TLC on it and saw different spot...so not pure..

Cannabinoids are highly air sensitive, and oxidize to aromatics if allows to sit in air, or worse yet, are heated in air. You need to keep them under nitrogen and handle them carefully, just like most reactive organics.

If you plan to do commercial work, you should learn the basics before spending a lot of money to make a mess. Maybe work somewhere that knows how to do this first, or take some classes on how to do it. Just like any other pharmaceutical extraction, you must do it correctly to make a safe product, if intended for human consumption.

Good companies use CO2 or USP grade ethanol to do the extractions, as they are completely safe for human use. Using butane or propane might be acceptable if the material is reprocessed later correctly, but the equipment to do that safely is key, people have blown up their house or garage doing it wrong. That is why CO2 is ideal, much safer, and very easy to scale with commercial equipment.

Syn the Sizer - 2-4-2020 at 18:58

Using butane or propane might be acceptable if the material is reprocessed later correctly, but the equipment to do that safely is key, people have blown up their house or garage doing it wrong. That is why CO2 is ideal, much safer, and very easy to scale with commercial equipment.

That's exactly it, you need to cure it properly. In Canada all the major medicinal shatter producers make it using butane or propane with a cure time of 100hrs in a vacuum chamber with moderate heat to drive off all residual vapours. For recreational use, only CO2 has been made legal. From what I have read over the years is CO2 also extracts some polar compounds and and is the solvent of choice for FSE (full spectrum extracts) because it pulls the tenpins out as well. BHO/PHO pulls just the THC/CBD and a few other compounds so you get high cannabinoid concentration and low flavour. Like I had mentioned I have had 1g of shatter with over 80%THC, that's 800mg of THC.

Its handy for cooking too, decarboxylate it in the oven for 45min on moderate temp. Dissolve it into your baking butter, and bake. I always figured a 75% yield of THC mainly because you hit a point where the THC starts decomposing before its all decarboxylated so there will be a point of equilibrium before you start decomposing a loss.

draculic acid69 - 3-4-2020 at 01:50

Few questions: does the bho method also extract CBD or just THC?
Is your goal getting pure CBD for sale?
Or are u going to convert the CBD to THC yourself for personal use?

Syn the Sizer - 3-4-2020 at 09:08

I believe it extracts both CBD and THC. you would need to separate it yourself. Though I have a feeling Dr. Bob may have a better answer to this.

Dr.Bob - 5-4-2020 at 16:33

Most methods extract both cannabinoids, along with many others. Hard to separate them easily, without some form of chromatography. But some companies that are trying to stay below .3% THC have found ways to remove the traces of THF from their CBD with various chrom. methods. Removing CBD from THC might be slightly easier, as CBD is a diphenol, so slightly more polar than THC, so comes later off a column in normal phase. With SFC, I believe it is pretty easy to purify either, but not a trivial piece of equipment.

Syn the Sizer - 10-5-2020 at 10:40

There is a method of crystallizing THCA out of a solvent in a method known as diamond mining. It is achieved by a slow evaporation of a solvent usually in a pressure chamber to help slow evaporation.

This could be a much easier, though longer way of purifying your products. The "diamonds" would be pure THCA which could than decarboxylate for edible or just smoke as THCA. The remaining "sauce" as its called is rich in CBD, cannabinoids and terpenes.

https://weedmaps.com/learn/dictionary/diamonds/

karlos³ - 10-5-2020 at 11:48

Not only blown up their houses!
In Germany, there was some "gangster rapper" who run such a lab illegally three years ago, that was blown up and ran under shock and on fire with heavily damaged hands for a few blocks until he collapsed.
I was intrigued what happened there when it was in the news, and now because of that post of yours I was reminded on that story and looked if there was anything known today.
And it was horrible.
What a consequence, all this from working with dangerous chemicals lacking the appropriate knowledge on what to do!

6 bottles of propane they say where the cause.
I found these shocking pictures:

So CO2 is the solvent of choice ideally.
Not propane or butane.

Syn the Sizer - 10-5-2020 at 12:32

Of course, you need to take precautions. I am sure all the companies that label there stuff BHO or PHO follow safety protocols because they are still manufacturing using both solvents. Its not for stupid people to do in their basement, you obviously do this stuff outside or in a proper fume hood designed for flammable/explosive solvents.

The thing with CO2 is it produces a different product than propane or butane, that is why shatter producers in Canada still use propane and butane to this day.

Why people would try an extraction using explosive solvents in an enclosed area close to a source of ignition is beyond me. As the saying goes you can't fix stupid.

S.C. Wack - 10-5-2020 at 12:58

Static may be underappreciated.
Have you seen pictures of CO2 extract compared to butane? Have you priced big CO2 machines?

Why people would try an extraction using explosive solvents in an enclosed area close to a source of ignition is beyond me. As the saying goes you can't fix stupid.

It was just recently that people here recommended storing ether containers in the fridge. So the cap leaks with the temperature change and on opening the door the light comes on and

[Edited on 10-5-2020 by S.C. Wack]

Syn the Sizer - 10-5-2020 at 15:41

No I haven't priced one out because I use butane or isopropanol for my extractions, I also have no plans on producing for sale so I don't plan on doing CO2 extractions. If I were to invest in something else I think it would be a cold press.

I understand what you are saying about ether, it very volatile so I wouldn't doubt it would leak, that is also why volatile explosive substances should be store in an explosion proof fridge, or very least a bar style fridge with a gravity evaporator and no light. But I also would never do a cannabinoid extraction with ether and butane/propane are in leak proof containers.

I am not saying CO2 is wrong, I am saying that butane/propane also work, make a different product and are still used to produce shatter in industry by professionals in Canada, and if done safely like I have for over a decade, a great route. Though shatter can only be sold as a medicinal product, CO2 is the only concentrate legal to sell for recreational use here, well in my province anyway. You can manufacture however you want for personal use.

nzlostpass - 10-5-2020 at 22:17

Quote: Originally posted by karlos³

6 bottles of propane they say where the cause.
I found these shocking pictures:

So CO2 is the solvent of choice ideally.
Not propane or butane.

Is that the same guy in both pics? Wow! A guy I know got a tooth infection that went to his brain and ended up with a head like that....really sad.
Do you have any english links to the story behind that guy?

G-Coupled - 11-5-2020 at 14:30

Quote: Originally posted by nzlostpass

Do you have any english links to the story behind that guy?

It's the Daily Heil, bear in mind, but here's one.

The comments are a hoot, as per. :cool:

Syn the Sizer - 11-5-2020 at 15:52

Quote: Originally posted by G-Coupled

Quote: Originally posted by nzlostpass

Do you have any english links to the story behind that guy?

It's the Daily Heil, bear in mind, but here's one.

The comments are a hoot, as per. :cool:

Don't get me wrong, it is sad when stuff like this happens, nobody ever wants to see anybody get hurt. However its not a new fact that things like butane and propane are flammable and explosive. But i guess I live in Canada, even before legalization neighbours didn't report you for extractions outside so we didn't need to hide inside. I should look at the bigger picture before making statements such as "you can't fix stupid"

Edit:

This is also why us as a world society need to advocate for the world legalization of Marijuana. So many people are made criminals and injure themselves just for a plant that grows. Ethanol as we all know is produced by a micro-organism while destroying sugar, the ethanol is essentially the urine and feces and the CO₂ is the flatulence, who wants some jenkem.

[Edited on 11-5-2020 by Syn the Sizer]

earpain - 16-6-2020 at 08:17

In response to this and some other statements in this thread:
I believe there is a new meta-industry piggy-backing off of the THC extraction industry. They are usually engineers selling industrial equipment to successful producers who do not have a fundamental grasp of chemistry. Search around with the right keywords, and you will find demo's of giant machines that anyone here knows how to put together for a few $1000 at most. Yet these companies charge up to .5M. Dead serious.

I think the shorter chained alkanes are great solvents for extracting flower. But if it boils BELLOW room temperature, how do you suppose to recycle it?

Yes, butane boils off on it's own. But so does hexane and heptane in a FLASK under REDUCED pressure. There's your best of both worlds

Alcohol:
Why? I read on some super obscure weed-science site one argument for:
THCA and CBDA, with their carboxylic acid groups, are actually bit more polar.

arguments against:
So cured flower is 15% water on average. Sure you can dry your ethanol or isopropanol to the bone, but alcohols are MISCIBLE with water. So you will pull not only alcohol soluble polars, you will pull WATER SOLUBLE POLARS.
Hence the -40C, 2 minute shake recipes.

Here is why trace amounts of hydrocarbons and the like are not an issue:
Extracts are dead. Distillate is what sells. Retail at dispenseries in my state: $100 - $115 per ml
By law GC/MS must be included.

The BP difference between these hydrocarbons and the theoretical BP of the cannabinoid active oils is IMMENSE.

I DO advocate for a two solvent winterization however:
Pull the flower with Hexane or Diethyl Ether or which ever.
Filter for REAL. I mean fine sintered glass under vacuum.

Distill and recover the original Non-Polar, you're left with crude #1.

Now since there is NO WATER, sure why not? Pick an alcohol, I agree iso > ethanol > methanol. Honestly I kind of like acetone for this part too.
Make sure it's VERY dry. Dissolve crude. Filter through sintered glass. Cool down to sub-zero, and quickly run it through the sintered glass again.

Double winterized crude. Can actually be vaped.
OR
Perfect starting point for MOLECULAR DISTILLATION

[Edited on 16-6-2020 by earpain]

Syn the Sizer - 16-6-2020 at 11:29

Great explanation.

I do agree that something like butane is very hard to recycle with a boiling point of -1^oC but the way I see it for home extraction for personal use it is cheap and OTC. As for industry, I don't know how the manufacturers of BHO and PHO recycle it or if they recycle it. I do agree though that using a slightly longer chain alkane would allow for recycling.

Yes, distillate is the big product now, partly because of purity and it is fairly easy to produce. But personally if I can get a g of shatter for 25$ or a g of distillate for 120$ i'll be buying 4g of shatter and 20$ in munchies.

Yes 2 step winterization, I just mentioned winterization of the non-polar solvent, I was typeing faster than I was thinking of course you want to get rid of the non-polar and dissolve it in a polar solvent so you don't blow you place up. I have heard of people using acetone but have never seen it done or used it myself.

earpain - 23-8-2020 at 05:53

Great explanation.

I do agree that something like butane is very hard to recycle with a boiling point of -1^oC but the way I see it for home extraction for personal use it is cheap and OTC. As for industry, I don't know how the manufacturers of BHO and PHO recycle it or if they recycle it. I do agree though that using a slightly longer chain alkane would allow for recycling.

Yes, distillate is the big product now, partly because of purity and it is fairly easy to produce. But personally if I can get a g of shatter for 25$ or a g of distillate for 120$ i'll be buying 4g of shatter and 20$ in munchies.

Yes 2 step winterization, I just mentioned winterization of the non-polar solvent, I was typeing faster than I was thinking of course you want to get rid of the non-polar and dissolve it in a polar solvent so you don't blow you place up. I have heard of people using acetone but have never seen it done or used it myself.

Mmm hmm. Indeed. I found one, non-academic experimental report of a comparison of 10 or so solvents. The website had pictures of the color of the solvent after extracting, and a picture of the crude after stripping. Definitely no Chroma/Spectra/NMR, etc.

Clearly the big dogs are rigorously researching these matters precisely in this way, and THAT data is proprietary, and anyone with access to it is tied up by piles of Non Disclosure Agreements and Non-Competes.

This is why I did my own comparison of a few solvents. Also, with no spectra, or chroma, or the like.

Acetone came up because it is the lowest BP solvent available as mostly pure in any hardware store. Also it has similar solvent properties to alcohol, but a bit more selective.

Incidentally, acetone is unavoidable for cleaning up all of the GUNK afterwards from glassware and filters and all that. So it's probably not a good choice for the first extraction.

draculic acid69 - 24-8-2020 at 00:09

Apparently shellite is the best solvent for initial extraction followed by a water wash to remove sugars and other water soluble stuff.if what I was told is true doing this gives a clean burning product

draculic acid69 - 24-8-2020 at 01:48

The equipment for doing this properly is pretty simple and clever but expensive and whoever said earlier that there's big business around simple equipment being sold for massive amounts to ppl with no chem/engineering understanding is correct.a simple 3pot butane extraction/recycling setup that would cost a hundred bucks to make is being sold for like$10000 to pot growers who want to do the bho supercritical rxn but don't understand it.this setup I'm talking about recycles the butane over and over and is quite a smart idea.its just expensive

Syn the Sizer - 24-8-2020 at 11:28

Anything for a buck, and like you said many people just don't know what they are doing. It is easy to find a business to setup an apparatus for you even if they charge exponentially more.

Edit:

Shellite, no thanks, I will stick to my butane and isopropanol extractions. Though very interesting, do you have and literature on it?

[Edited on 24-8-2020 by Syn the Sizer]

S.C. Wack - 24-8-2020 at 12:42

Where extraction is allowed, it's still regulated. I don't know anywhere that pentane extraction is permitted. The guy whose fingerprints are most over closed loop extraction with butane in a SS sanitary spool, hose, valves, and vacuum system, before the first legalization of it, also took it upon himself to inform senators and fire marshals involved in the first extraction codes that the world's foremost authority says only closed loop systems using CO2, propane, or butane qualify as good manufacturing practice. Butane good, pentane bad. Water or glycerol might be allowed as well. Or heavily taxed and regulated (in theory) alcohol.

morganbw - 24-8-2020 at 12:49

Unless you are doing this out of sight and for your self, this shit is looked at pretty close.
That may be the high price of some of the stuff. They may be selling you a method that is accepted.

I do have a nephew who makes his own stuff from wax he buys but for over all use by everybody, there needs to be a few guidelines.

draculic acid69 - 24-8-2020 at 15:44