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Author: Subject: Cannabis Distillate for personal medical use
lwaali
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[*] posted on 16-10-2018 at 16:36
Cannabis Distillate for personal medical use


Hi Folks, I'm new to the forum and new to chemistry. I am looking to learn about cannabinoid fractional distillation and how to apply this knowledge to other plants found in the Americas.

Background: I am a retired/disabled Electronics Engineer that has been diagnosed with several conditions that have no treatments or cures according to western medicine. Cannabis is legal in my state and I have found some relief from it (suggested by my Doctor). I have been concerned about leftover solvents and pesticides in product I have purchased from retail stores (abnormal popping, crackling, undue residue, chemical taste not obtained naturally from different strains). Additionally, I have read about anecdotal Native American Traditional treatments that might help if I gain enough knowledge to safely apply this knowledge to make my own.

I have been reading Uni textbooks for a few months about the theory of FD and have collected the equipment I believe I will need. BUT! reading textbooks doesn't answer questions that pop up and I definitely do not have the background to understand everything I have read here or in books. I want to be safe above all which is why I am not just throwing things together and running with it.

Is anyone willing to hold my hand and teach me? I have looked into courses but, frankly, I don't have the money and live way out of any town with a college.
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[*] posted on 16-10-2018 at 16:49


It looks like what you want to do is make THC and CBD extracts. For that I would recommend maybe looking into either steam distillation or a sexhlet extractor. I dont know a lot about those topics but that is where I would start.

A soxhlet extractor continuously washes the material you are extracting with warm solvent, for example diethyl ether, ethanol, or even butane.

You can get one on ebay.

https://www.ebay.com/itm/2Pcs-500ml-50-42-24-29-Glass-Soxhle...





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[*] posted on 16-10-2018 at 17:11


Yes, THC, CBD, terpenes and other components. I am very interested in saving the terpinoids which are showing very promising medical uses (https://www.ncbi.nlm.nih.gov/pubmed/19729208).

I also thought soxhlet and/or vacuum extractions would be the way to go (I am expecting the soxhlet piece any day now and making a vacuum trap out of a mason jar as we speak). I would prefer to stick with lab alcohol for the solvent purely because of the nontoxic nature vs the more volatile and toxic options. I don't know if that is a valid reason or not.. please educate me if I am thinking hogwash!

I could list the equipment I am thinking of using if that would help but didn't want to overwhelm with my ignorance or unneeded information.

[Edited on 17-10-2018 by lwaali]
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Jackson
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[*] posted on 16-10-2018 at 19:20


I would reccomend using food grade ethanol as a solvent just because it is food grade and probably safer tha nusing a non food grade solvent.
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[*] posted on 16-10-2018 at 19:43


The usual extracting fluid is butane.
However carbon dioxide is also used commercially.
Butane is better for the home user.
As stated above, you can use ethanol as well but you are going to get chlorophyll and other products you don't want.

The sublimation is used to separate the various compounds in the wax.
The sublimation is usually done using a hot plate/cold plate method with a thin layer of wax.
The hot plate temp has to be carefully controlled.

There is a reason the med shops charge so much.
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lwaali
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[*] posted on 16-10-2018 at 19:43


Quote: Originally posted by Jackson  
I would reccomend using food grade ethanol as a solvent just because it is food grade and probably safer tha nusing a non food grade solvent.


Exactly my thinking. Apologies if "lab alcohol" is something different.
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lwaali
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[*] posted on 16-10-2018 at 19:58


Quote: Originally posted by macckone  
The usual extracting fluid is butane.
However carbon dioxide is also used commercially.
Butane is better for the home user.
As stated above, you can use ethanol as well but you are going to get chlorophyll and other products you don't want.


The first step is to soak the plant material in 200 proof alcohol for several days, filter the plant material out, then winterize the remaining liquid. This winterization process removes all chlorophyll and the waxes from the distillate. The use of alcohol distilling in a vacuum allows you to use a much lower bp and so not destroying the fragile terpines. The freezing temperatures from using the butanes/hexanes/methanes destroys some of the components I am trying to keep. The equipment needed for safe and environmentally sound methods that use the more volatile solvents is very expensive. I am only wanting to do this on a small scale for only my own use.
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[*] posted on 17-10-2018 at 01:19


I've used cannabis since the mid 70s for insomnia and more recently for recurring pleurisy but I would never isolate different fractions because the (all important) "entourage effect" would be lost.

I smoke Ace's Old Timer's Haze because the equatorial genetics produce trippy and euphoric effects.

If you are in a position to grow your own, you would have the satisfaction of knowing it's cleaner than any mersh out there.

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[*] posted on 17-10-2018 at 07:30


Everything you ever wanted to know and more about Butane extractions, super critical CO2 extractions, Ethanol extractions, winterizing, etc. can be found in great detail at:
https://skunkpharmresearch.com/
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[*] posted on 17-10-2018 at 08:00




This thread from a month ago might help.

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[*] posted on 17-10-2018 at 09:41


*sigh* OK, let me put it a different way.. I am old, sick, and poor. Western Medicine says they cannot do anything. I am choosing to try traditional medicines as opposed to laying down and dying. I CHOOSE not to use any other method besides food grade alcohol because I cannot risk ingesting any toxins. I know about the entourage effect which is why I want to SAVE the terpines etc and put them back in after I remove the alcohol. I get the feeling that no one actually read the first post. I CANNOT smoke. I am already on oxygen 24/7. I have read the skunk pharm pages and non of them are methods of making CLEAN and PURE lab grade distillates. I am not interested in learning how to make sludge using croc pots, bailing twine and duct tape. I do grow as a matter of fact but I CANNOT SMOKE and want to use the benefits of the plant. I do not want to just get stoned. I am not interested in other methods. I have already looked into every method out there and this is the one that suits my needs and uses the equipment I have. Thanks for thinking you all know better then me and my doctors.:mad:
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[*] posted on 17-10-2018 at 11:39


Quote:
Thanks for thinking you all know better then me and my doctors.

Sorry Iwaali, I didn't mean to sound patronising and I do apologise.

I hope you have only success in your quest...

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[*] posted on 17-10-2018 at 12:14


OK, lets try this again. You want a "whole plant extract" to maximize potency. Without knowing your target active ingredient(s) it's a sensible approach. If we exclude the usual cellular material we're focusing on cannabinoids, terpenes and so on. What's your preferred delivery system? Oral, vaping? For oral intake you can usually accept more non-active components.
Any of a number of polar solvents fits the bill, but you want to eliminate any harmful solvent residues. Right? Ethanol is shown to work, but IIRC it wasn't considered ideal in the research I found. There are (or were) several papers on extraction methods available online.
I believe butane is fairly benign in the concentrations we're dealing with here, and it's volatility makes it easy to remove. Supercritical CO2 sounds sweet but pretty expensive. Vacuum distillation is probably overkill and requires more specialized equipment. Steam extraction is perhaps the cleanest method.

Then there is this unit: https://www.drizzle.life/ There is even a thread about it here: http://www.sciencemadness.org/talk/viewthread.php?tid=74922




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[*] posted on 17-10-2018 at 12:18


If you're talking about terpenes, by and large they have higher boiling points than alcohol, and should remain in the extract when you boil off the alcohol.

A lot of distillation of cannabis involves just doing a short path distillation to get a stronger product, but not actually separating all the components.

Dividing up those components by distillation may take a fairly powerful column, and very low pressures.
This is problematic for small scale work because good columns tend to have greater holdup, which means trouble when working with small samples.

Terpenes can probably be removed from the oil most effectively without heat damage by a falling film distillation head, but they aren't cheap.

Likewise, a concentric tube semi-microscale column like the 400 mm job Ace Glass makes would seem to be a good choice for the fractionation because of the very low theoretical plate height (10 mm) and low holdup (less than 2 ml), but again, you're talking about a real expense.

And you'll need a good PTO distillation head too.

If you're on a budget; I think there's a lot to be said for easily produced crude extracts and distillates.
CLEAN and PURE lab grade distillates aren't cheap, and with good reason.

The components I mentioned above cost around $5000 new.

Even I had to pay nearly $300 for them with my fabled Midas touch.
And no, I don't distill cannabis with them.
I bought them for shits and giggles, but I reckon they'd just about do the job.

BTW: Internal consistency in your posts is always nice:
You went from a guy complaining about "popping, cracking, and undue residue"
To a highly self-righteous non-smoker who CANNOT SMOKE due to medical reasons.

Does the stuff "pop and crack" while you're eating it?
If so I suggest you stop mixing it with Pop Rocks:.

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[*] posted on 17-10-2018 at 14:11


> Thanks for thinking you all know better then me and my doctors

It's so fucked up to see pentane is obviously more inert than alcohol and all the crap that will be in the black-green tar of an ethanolic Soxhlet extract of leaves, but that wouldn't matter because your winterizing step would remove it (the pentane, not the crap except for colorless ~inert waxes) anyways? If you're not smoking what is this popping and crackling and why winterize?

Bad on us for thinking olive oil would be the best fit to such a story real or imagined...shaking/stirring/blending fresh green whatever and cold everclear for minutes would be brilliance compared with soaking for days or hot repeated extractions for hours.




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[*] posted on 17-10-2018 at 17:23


I would recommend food grade alcohol, for example vodka if you wanted. If you wanted, you could even distill and dry the vodka to increase its alcohol content.

Butane is a great solvent for the alkaloids you want to extract but it is more dangerous. It is very volatile, meaning it boils near rt and can evaporate quickly, and requires lots of cooling. To use butane you would need to do this in a very well ventilated area or outside, have lots of cooling, and have a fire extinguisher handy.

Butane and ethanol are both very easy to get.




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[*] posted on 18-10-2018 at 06:41


Quote:
The freezing temperatures from using the butanes/hexanes/methanes destroys some of the components

Don't worry about this, freezing temperatures wont hurt.

I would recommend ACS grade butane or pentane. Or get technical pentane and distill, as long as you get rid of high boiling residues. Why I recommend this? I think it is easier to get a clean product (if you mind the chlorophyll and waxes that is).

ACS butane will probably hard to get, but pentane at least can be stored in a bottle (bp 36 degrees). I would leave the pentane solution to evaporate mostly and then apply vacuum for some time to get rid of the last pentane.

The product from the pentane extraction (just soak, filter, evaporate, putt a bit of vacuum) can be dissolved in olive oil for consumption. No extracted chlorophyll or waxes extracted, so less work for an equally clean product (but do distill the pentane if it is not ACS)


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[*] posted on 18-10-2018 at 14:45


Not impossibly our new friend hopes this thread to be a SOP for a legal commercial processor, at a location where it's much easier to have permission to extract with alcohols than it is for other typical organic solvents, butane, or CO2.

PS If I was vaping or smoking one of these legal extracts (have yet to do so) and there was popping and crackling, the first thing I'd suspect as the cause is water.

[Edited on 18-10-2018 by S.C. Wack]




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[*] posted on 18-10-2018 at 20:32


This is strictly for personal use. The popping and crackling was from left over solvents. Even the dispensary said so and no longer carries that brand because they had it checked. Once I learn the process I plan on using the same set up to make extractions of plants like Kinnikinnick, Mountain Laural, and other plants I can harvest myself. FD offers me more options and control of what I extract. I collect vapors (anyone remember balloons?) when immediate relief is needed but usually I make my own capsules and pills. There are a lot more in cannabis then just the terps, things that are more fragile like the flavinoids that start boiling at 273f. Self righteous? No, just frustrated that instead of helping me with the request, the majority of the replies have had nothing to do with the instruction on fractional distillation. I did not ask which method should I use or offer to explain my choices. I wanted to come to a place where I hoped to get better information then stoned kids blasting on youtube. Every video I tried to watch started with someone blowing smoke. That is what I should turn to when doing a process incorrectly could blow up my home? Any more questions? Should I find another place for information or is there anyone here that would like to help me LEARN?
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[*] posted on 18-10-2018 at 21:37


Find yourself a cookbook with your spoon feeding requests, rotten attitude and language. Learn?, my ass you just want a recipe which you will immediately shoot down by saying that it will destroy the pixie dust you believe is in there because it was heated, frozen or extracted.
Also without knowing what, as in what group of compounds, in the plants you are after there is no way to rationally develop an extraction method because the physicochemical properties and stability of said group of compounds are unknown.
Hint, fractional distillation (or FD as you seem to call it, why?) involves heating and this will almost certainly change some compounds (by decarboxylation for example). The only work around is a solid-liquid extraction suggested by others, over and over. You don't want to learn, you just want confirmation that you are on the right track,which I doubt you are on.
You'll want to pick up a book on etnopharmacology and read the chapter on extractions carefully.
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[*] posted on 19-10-2018 at 00:01


Quote: Originally posted by lwaali  
FD offers me more options and control of what I extract.


You want to preserve all fragile molecules but distill at the same time? This is not going to work. Even under high vacuum (what is your vacuum source?). Also this requires some nifty skills I don't think you have.

Quote: Originally posted by lwaali  

There are a lot more in cannabis then just the terps, things that are more fragile like the flavinoids that start boiling at 273f.


You could do a steam distillation, but this will destroy other compounds. And I'm not to sure everything will come over with steam.

Just do a cold solvent/solid extraction, get some filter paper and some place to vent.

Quote: Originally posted by lwaali  

I did not ask which method should I use or offer to explain my choices.


Well no, you didn't. But at least we proposed some other methods that actually work and require a lot less skill/equipment.

Quote: Originally posted by lwaali  

I wanted to come to a place where I hoped to get better information then stoned kids blasting on youtube. Every video I tried to watch started with someone blowing smoke.


And you did, the fact you don't like the information doesn't change that.

Quote: Originally posted by lwaali  

Should I find another place for information or is there anyone here that would like to help me LEARN?


If you don't like what you get, please do. But be warned, scientifically you probably won't find anything like what you get here, success with you efforts!

[Edited on 19-10-2018 by Tsjerk]
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[*] posted on 19-10-2018 at 11:00


You did not ask which method you should use or explain your choices.

That's right, so what are you even doing here?

You're asking for advice on how to use some un-named assortment of glassware to do a difficult distillation which it may, or may not, be capable of. Probably not if you're contemplating doing it with your shiny new 300 mm Vigreux.

A distillation which, according to well-informed posters on here, would be best avoided in preference to extraction, chromatography, etc.

And you're apparently using some double-super-secret method because you aren't describing what you intend to do in any meaningful way.

So just what advice were you expecting?

Make sure your diffusion pump is full of mercury?
Adjust the takeoff valve for an appropriate reflux ratio?
Always take notes?
Fill out your lab reports the way your lab instructor wants them, not the way your former lab instructor wanted them?
Don't use the heating mantle to warm your leftover pasta unless it's a model with a solid inner surface?

All we know about your equipment is that you have a mason jar with a couple of holes punched in the lid. Probably with some tubes epoxied into them.

And apparently you plan on moving on eventually from cannabis to making chemically pure extracts with high vacuum fractional distillation from American plants the way the American Indians did.

If you do get this far I've got a pal with an authentic Anasazi spinning band distillation column that you might be interested in.
It's made entirely of clay, and the Chihuahua head motif on the reflux head is quite stunning.

However maintaining an even 1500 RPM on the spinning band is difficult because of the stick and twisted bow drive system which requires a sure hand and very good rhythm.







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[*] posted on 19-10-2018 at 12:02


Quote: Originally posted by lwaali  
Self righteous? No, just frustrated that instead of helping me with the request, the majority of the replies have had nothing to do with the instruction on fractional distillation. I did not ask which method should I use or offer to explain my choices. I wanted to come to a place where I hoped to get better information then stoned kids blasting on youtube.


I was the same way when I started visiting this forum. Most people here are like me; we are happy to help new people but few of us tolerate spoon feeding.

If you want to know about fractional distillation, steam distillation, or sexhelts, then visit those threads.In the library section look up Vogels Practical Organic Chemistry. That book explain the basics of distillation.

Forum members dont like having to repeat things that are easy looked up in the library section. Sometimes I myself get scolded for this. It does not help the forum search function is not great.

Quote: Originally posted by lwaali  
That is what I should turn to when doing a process incorrectly could blow up my home? Any more questions? Should I find another place for information or is there anyone here that would like to help me LEARN?


Blow up your house, no. Loose a finger yes. If you are using butane or diethyl ether then you could make a big fire ball. If you are just learning stick to things like alcohol (isopropyl or ethyl) and water.

No one here is going to help you learn unless you make a big effort. For example, if you show us some sources of what you want to do (be very specific such as a video or book). Then show us your procedure. Then after that tell us what equipment you want or have.

Here is some stuff to help you learn

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

https://www.youtube.com/watch?v=o4CBXkfVHDc

That video is about steam distillation to get a specific chemical out of a plant.

https://www.youtube.com/watch?v=lQoaS0O4zF0&t=187s

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

https://www.youtube.com/watch?v=Iryh0Dp130s

http://library.sciencemadness.org/library/books/vogel_practi...

Here is the equipment you need

https://www.ebay.com/itm/1000ml-24-40-Distillation-Apparatus...

https://www.ebay.com/itm/250ml-Glass-Soxhlet-Extractor-Spher...

https://www.ebay.com/itm/50cm-Chemistry-Laboratory-Retort-St...

[Edited on 19-10-2018 by VSEPR_VOID]




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[*] posted on 20-10-2018 at 17:11


Why is having chlorophyll, etc. in the extracts detrimental to your intended use?
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[*] posted on 21-10-2018 at 06:43


Why bother with extraction at all when you are making doses to take orally anyway? Just for the heck of extraction I can understand, if it's fun to do, but the effect won't be any different
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