Skunk pharm's Glycerin Extraction processes

Graywolf

Well-known member
Kosher vegetable glycerin is an effective method for extracting cannabis concentrates directly from the plant material and produces a tasty medication that is easily ingested directly orally, or mixed with drinks and food.

Glycerin is a heavy, syrupy clear liquid sugar alcohol that has approximately 60% of the sweetness of sucrose, and about the same food value.

It is however not actually a true sugar and is often used as a sugar substitute, as diabetics are often able to use it without experienced the blood sugar rollercoaster they suffer with sucrose or other sugars.

Glycerin makes an extremely tasty and provocative cannabis tincture, that when made using cold extraction methods, is reminiscent of wild honey, as it preserves all the individual flavors, so that they dart off in all directions simultaneously.

Hot glycerin extraction also makes a tasty tincture, with the flavor more resembling a fine soup, where the individual flavors are married into one overall flavor. While not as whimsical and provocative as a cold extraction, it can be prepared start to finish in a couple days, where cold extractions take a minimum of 60 days and are commonly soaked for 120 days or longer.

Many of the provocative flavors and odors from cannabis are aromatic terpenoids, and the reason that they are aromatic in the first place, is that they give off molecules at room temperature.

Heating speeds up the rate that the accompanying terpenoids and other aromatics are vaporized off, so many are collateral damage in a hot extraction and are lost.

The glycerin molecule is actually only a three carbon molecule chain, with three hydroxyl groups (OH) attached, and as hydroxyl groups are hydrophilic, glycerin is hygroscopic (absorbs water) and dissolves readily (miscible) in water.

It has a flash point of approximately 177C (351F), and a boiling point of 290 °C (554°F).

It is relatively non toxic. The MSDS tells us that the LD50 Oral rat dosage is 12,600 milligrams per kilogram of body weight, which is approximately 5.7 grams per pound of body weight, or 36 ounces for a 180 pound male.

By comparison, acute oral toxicity (LD50) Oral Rat for sucrose sugar is 29700 mg/kg and about 7060 mg/kg for ethyl (grain) alcohol.

At saturation, Glycerin only hold as 33% as much cannabis oil as the same volume of ethyl (grain) alcohol, so about three times more is required per dose.

To reach maximum saturation however, requires processing more than one batch of fresh material through the glycerin, because as the saturation level increases, the glycerin becomes less aggressive as a solvent and the partially dissolved cannabis boundary layer interface with the solvent is also no longer at full strength and as reactive.

To keep the reaction from slowing to a snails pace, or even stopping, some method must be used to keep removing this stagnant layer and refreshing the boundary between the solvent and resin.

In addition heat dramatically affects resin dissolution rates. The hotter it is, the faster it works, up to the point of overheating.

As glycerin is usually used as an oral med, we also need to consider decarboxylating the cannabinoids so that they are orally active.

If not in excess, some water solubles add to the flavor of a glycerin tincture, and taking all of the water out of the material before processing it, makes it frangible and prone to breaking into small fragments that may be hard to remove.

Let's look at how these four variables can be manipulated to produce delicious and effective glycerin tinctures.

Drying and decarboxylation:

Plant material is typically dried to around 10/15% water content by weight for smoking and vaporizing purposes, which is low enough to make some delicious glycerin, but for those who prefer less water solubles in their glycerin tincture or wish to decarboxylate the material before extracting, you may add a drying and/or decarboxylation step.

To simply remove most of the remaining moisture, I place the plant material on a cookie sheet in a 200F oven and turn it, until it is frangible when I roll it between my finger and thumb.

At that point it is ready for extraction, but if you also wish to decarboxylate the plant material before making your tincture, you can then crank up the oven to 250F and after it stabilizes at the higher temperature, replace the plant material in the oven and hold it at temperature for approximately 30 minutes

That will add a roasted flavor to the tincture and many of the turpenoids will be lost, but it will decarboxylate approximately 70% of the existing carboxylic acids into their non acid orally active form.

An alternative to decarboxylating the material ahead of time, is to do it after the extraction is complete and the plant material has been filtered out. That eliminates the roasted flavor and preserves more of the turpennoids.

Using Temperature:

Elevating the temperature of the glycerin increases the rate of dissolution of the resins, especially if you raise the temperature high enough for the resins to be molten. THC, CBD and CBN are all molten at just under 180F, so we operate at that temperature.

The advantage of using as low a temperature as possible, is that fewer aromatic terpenoids are boiled off at that low a temperature, and it decarboxylates more slowly, so that the process doesn't pass the peak of the decarboxylation curve and start down the other side toward low THC and high CBN. As previously noted, we can finish the decarboxylation later.

Keeping the boundary layer removed:

The boundary layer is the layer of partially reacted resin and dilute solvent that forms on the surface of the resin after the initial aggressive dissolution by the solvent. The solvent at that point is dilute, as is the resin concentration, so that the reaction slows or grinds to a halt.

To keep the reaction operating at a reasonable rate, we need to periodically or continuously remove that boundary layer, and there are four methods that I will present here.

The first is to stir. Simply stir gently and thoroughly with a wooden spoon

The second is to shake. Simply shake a jar of glycerin and plant material by hand regularly. A paint shaker would also work for this application.

The third is to tumble. Placing the jar of glycerin and plant material in a rock or photo film tumbler will keep the boundaries fresh. It is an effective and gentle way to speed up the process.

The forth is vibration. Placing jar of glycerin and plant material in a vibratory cartridge case cleaner, or other form of vibration, creates more shear energy that tumbling and will dissolve the material the fastest of any method we have tried thus far.

Material selection and preparation for hot or cold processing:

While glycerin tincture can be made from anything from prime bud to stems, it is tastiest done from prime bud and least tasty with the stems. I usually make glycerin tincture out of the sweet trim removed from the buds during manicuring and popcorn buds.

It is not necessary to grind up the material, only to break it up any buds so that the material is loose enough for the glycerin to reach all the surfaces. Excessive pulverization of the material will result in color and particulate pickup that is difficult to remove. If you leave some surfaces blinded however, the resins on those surfaces won't be removed either.

Extracting using the cold process:

The cold process is the easiest and tastiest way to make glycerin tincture. We extract using the cold process, simply by soaking the plant material in glycerin at ambient temperatures and agitating it for sixty days or more. Sixty days is about the least amount of time for a cold extraction, and typically they are run 90 to over 120 days. I have one experiment with more than 365 days of soak time.

After the extended soak and agitation, the glycerin is poured off and pressed out of the plant material to yield quality and tasty tinctures. It can also be used with fresh material for another cycle, so as to build up more potency.

There are a number of ways to press out the glycerin from the plant material, and it applies to both cold and hot extraction, so I will cover that in a separate discussion at the end of extraction methods.

The way that I make cold process glycerin tincture, is to load a canning jar 2/3'ds full of plant material, lightly compacted and then cover with glycerin while stirring with a wooden spoon, until every surface is well coated and mixture is homogenous, and then add another inch of glycerin on top.

I place the jars in a cool dark place or cover to exclude light. I sometimes wrap jars with aluminum foil to exclude light.

Every day for the soak period days, I periodically agitate the jars, using one of the above methods and at the end I filter out the plant material for a a light golden to dark amber glycerin tincture, that is tasty and of high quality.

Because the aromatic terpenoids are preserved, it will have many flavors present, interacting and darting off in all directions simultaneously.

You can more easily filter the mixture if you warm it up to 150F or so before filtering.

Potency and gleaning:

As previously noted, to reach maximum saturation, requires processing more than one batch of fresh material through the glycerin, because as the saturation level increases, the glycerin becomes less aggressive as a solvent and the remaining partially dissolved cannabis is also no longer at full strength and as reactive.

In point of fact, the fresh pressed material from the above first cycle will still contain significant cannabinoids, which takes two to three cycles to get it all.

What I do is put the fresh pressed plant material back in the jar and refill with fresh glycerin and add fresh material to the freshly pressed glycerin for another cycle, if I desire more strength.

The fresh glycerin will do the best job of scavenging the remaining cannabinoids, and then can be used again with fresh material to further build up its potency. It is by this cascading technique, that we can leave little behind and yet still maintain quality and potency.

I should note that the most potent glycerin tincture is not necessarily the most tasty, and one cycle produces effective meds, so most of the time we do not bother to bump up the potency with cold tincture.

Hot glycerin extraction:

We prepare plant material and extract cannabis by the hot glycerin extraction process in much the same way as we do by the cold process, though we stir it instead of shaking, tumbling, or vibrating it.

We also use a thermal cycling process and stir regularly, rather than an extended cook as many processes call for. The expansion and contraction of the thermal cycling help break up the resins so that they dissolve more readily.

As with cold tincture, I load a canning jar 2/3'ds full of plant material, lightly compacted and then cover with glycerin while stirring with a wooden spoon, until every surface is well coated and mixture is homogenous, and then add another inch of glycerin on top.

I then set that jar in an electric fondue pot full of hot Canola oil at 200F, and stir it regularly with a wooden spoon until the mixture reaches 180F, and then I adjust the pot temperature controls to maintain 180F.

I stir the mixture regularly with a wooden spoon, for another thirty minutes, and then I take it out of the hot oil and allow it to cool to ambient temperature.

For what it's worth, I use a wooden spoon, because a light tink with a metal spoon against a hot glass jar while stirring, can break it and dump the whole mixture into the hot oil.

After the mixture has cooled to room temperature, I again place into 200F oil and bring it back up to 180F while stirring regularly. When it reaches 180F, after a through stir, I take it out of the hot oil and let it cool to ambient temperature again.

I repeat the last step about five more times and after the last cook and stir, I filter out the plant material while the mixture is still hot.

Filtering glycerin tincture:

Vegetable glycerin is thick and syrupy, so it doesn't filter quickly or easily without mechanical help. The simplest way to filter it is to heat it up so that it isn't so viscous, and pour it into a jelly bag, which you wring out by hand. That works, but leaves a lot of glycerin behind and you are limited to temperatures that you can handle with your hands.

A French coffee press, a potato ricer, or a jelly press can also work, and you can buy tincture presses used by the botanical extraction industry.

I made my own press, using a hydraulic bottle jack inside a scrap metal frame, which presses a filter bag between two stainless dog dishes, at a force of 12,000 psi, and catches the glycerin in a third stainless dog dish.

It presses the plant material into a hard little puck, that I have to break up to reprocess.

Flavoring glycerin tincture:

A well made glycerin tincture is a taste delight in its own right, but for those of ya'll who just like to play, here is how I've flavored glycerin that I had already infused with cannabis oil.

I started by adding equal parts of Bing Cherry and Blueberry raisins in a blender with enough 190 proof grain alcohol to make a soupy paste when macerated by the blender.

I tossed in half as much Japanese Gari and a dash of Almond extract, added another half a cup of 190 proof, and let it blend well.

When pureed, I poured it into a stainless mixing cup and placed it in a 180F hot oil bath. I cooked and stirred it until all the alcohol was gone, and then removed it to cool.

I then put a bout two tablespoons of that concentrate into each 1/2 pint of infused glycerin to be flavored and place it in the 180F oil to cook for thirty minutes while stirring regularly.

At that point I remove it from the oil, filter out the concentrate using a filter bag and the glycerin press. The glycerin is delightfully flavored, and the chef gets to eat the concentrate from the filter bag! Ahwooooooooooooooooooooooooooooooo!!!!!!!!!! Hee, hee, hee....................

If you hold your cursor over the pictures below, you should get the label telling you their significance:

Cold vibrated one week-1-1.jpgSamples A, 1, 2, 3. & 4.jpg
 

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please put a sticky on this one, its so easy to follow and understand that i may give it a try......
thanks for taking the time and effort to put this tutorial together GW!........

:woot:

You're welcome! Sorry about the picture scattering. I will take some more and add to these.
 

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... imho glycerin is NOT very useful in making extractions. it is a very poor solvent, making it very inefficient for trying to pull stuff outta plant material.

for this reason, the glycerite compounds i make at my job start off as alcohol extractions, then we remove the alcohol and add glycerin to the remaining liquid

also, glycering is indigestable... and -sickly- sweet imo
 
... imho glycerin is NOT very useful in making extractions. it is a very poor solvent, making it very inefficient for trying to pull stuff outta plant material.

for this reason, the glycerite compounds i make at my job start off as alcohol extractions, then we remove the alcohol and add glycerin to the remaining liquid

also, glycering is indigestable... and -sickly- sweet imo

i do not tolerate glycerin at all, but have played with making it. for some, it is the only option. what works for some is poison to others.

i don't tolerate alcohol either, but i make tinctures as well. i formulate for others so formulate according to patient need.

i prefer holy anointing oil or holy shit formulations. the point is choice.
 
the point is choice.

certainly!
and i'm not even saying glycerin shouldn't be used, but for the actual extraction process (graywolf even points out how it's lacking in solvent qualities) i'd suggest using high proof ethanol (95% if you can get it), then evaporate the alcohol off, then replace with the gly to stabalize it... in fact if you can recover the alcohol then you can keep reusing it for future runs...

anyone else over here ever heard of a lloyd extractor? it'd work great for this purpose, fwiw :puffpuffpass:
 
certainly!
and i'm not even saying glycerin shouldn't be used, but for the actual extraction process (graywolf even points out how it's lacking in solvent qualities) i'd suggest using high proof ethanol (95% if you can get it), then evaporate the alcohol off, then replace with the gly to stabalize it... in fact if you can recover the alcohol then you can keep reusing it for future runs...

anyone else over here ever heard of a lloyd extractor? it'd work great for this purpose, fwiw :puffpuffpass:

How are you reinfusing the alcohol extracted cannabis oil into the glycerin? I haven't been able to get QWET or BHO to redissolve in glycerin. When I mixed ethanol tincture and glycerin, as soon as the alcohol was gone, the oil mostly separated again.
 
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How are you reinfusing the alcohol extracted cannabis oil into the glycerin? I haven't been able to get QWET or BHO to redissolve in glycerin. When I mixed ethanol tincture and glycerin, as soon as the alcohol was gone, the oil mostly separated again.

I don't have an answer for that, yet... just talked to my source of smoke and we'll be making some on his next pull... I'll let you know how it goes and methods used.
 
I don't have an answer for that, yet... just talked to my source of smoke and we'll be making some on his next pull... I'll let you know how it goes and methods used.

i will surely be interested in the process he uses. i have also tried many ways including what you describe plus added details to that end, with no success. please do school us. no teasing with processes you have not tried yourself or at least witnessed!

also, we want pix! yes?
 
i will surely be interested in the process he uses. i have also tried many ways including what you describe plus added details to that end, with no success. please do school us. no teasing with processes you have not tried yourself or at least witnessed!

also, we want pix! yes?

i truly did not mean to tease! but no, i have not made an mj glycerite before (though i do make gly extracts of well over 30 different herbs/herb compounds). i will definitely take pics as well when we get to it... shoot i'll probably be able to send ya both samples of finished product once we have it

just wanted to throw this by you two (since it looks like no one else is joining in)... my buddy and i were also discussin the pros and cons of a fresh herb extract vs. a dry herb extract... obviously dry herb would be a stronger concentrate, but that doesn't necessarily translate into better medicine, especially w/ how cannabinoids are oxidized... :nbf:

tbh, i've never tried any pot gly (1 oz goes for like 40 bucks at the canna cafe in portland i guess... too rich for my blood) so i don't really have a base of comparison...

so yeah i guess i'll NEED to get ya'll samples for the experts advice :hmm:

this'll be fun, i hope :prop:
 
How are you reinfusing the alcohol extracted cannabis oil into the glycerin? I haven't been able to get QWET or BHO to redissolve in glycerin. When I mixed ethanol tincture and glycerin, as soon as the alcohol was gone, the oil mostly separated again.

k so i've been giving this some more thought (keep in mind this is all theoretical for me atm)... the canna oil that gets extracted w/ alcohol but won't redesolve into the gly... it would seem that with glycerin as your menstruum you wouldn't be extracting those oils in the first place, and you could either remove the oil that seperates, or whip it into suspension before filling dropper bottles, evenly dispensing it, and then the user would just need to shake the bottle before every use to ensure farely equal doses...

or are we looking for precipitate free glycerites?
that would be a different case

oh, and all gly's i've ever made are 1 part h20/herb mix to 4 parts glycerin, so it's a little soupier than just straight up glycerin... fwiw
 
k so i've been giving this some more thought (keep in mind this is all theoretical for me atm)... the canna oil that gets extracted w/ alcohol but won't redesolve into the gly... it would seem that with glycerin as your menstruum you wouldn't be extracting those oils in the first place, and you could either remove the oil that seperates, or whip it into suspension before filling dropper bottles, evenly dispensing it, and then the user would just need to shake the bottle before every use to ensure farely equal doses...

or are we looking for precipitate free glycerites?
that would be a different case

oh, and all gly's i've ever made are 1 part h20/herb mix to 4 parts glycerin, so it's a little soupier than just straight up glycerin... fwiw

Not exactly sure of what you mean with your first statement, but if you mean do I think you should just extract with the glycerin in the first place, then the answer is yes.

Alas, shaking a bottle of glycerin doesn't do much to mix in the little globules of un-dissolved material and they have an unpleasant taste, where a good glycerin extract should taste more like wild honey.

I'm not saying it can't be done, I just haven't had any success myself at it and do sincerely look forward to having the secret revealed to me, so I can move forward with some of my ideas.

I don't personally think a whipped emulsion would market well. As you can see from my pictures, the glycerin gets darker in color with infusion, but is still bell clear.

Precipitates of close to the same specific gravity don't settle out well in glycerin, and I wouldn't try any myself, that isn't bell clear or that has something floating in it.
 
I'm not saying it can't be done, I just haven't had any success myself at it and do sincerely look forward to having the secret revealed to me, so I can move forward with some of my ideas.

not holding on to any real secrets... again i've never made an mj gly before...
the problem with the canna oils may be able to be resolved the same way we remove the fats from our milk thistle seed glycerin (lots of oil in them seeds)... first we make the alcohol extract (in the lab we use boiling alcohol, i won't be doing that), remove the alcohol w/ our lloyd extractor, then add the gly and mix... finally we toss the whole thing into a freezer for a few days, take it out and then remove the hardened layer of fat that has risen to the top, then filter the gly through a mesh screen and voila, clean product!!!

it'd be nice if this'll work with mj too...
i won't have a chance to do this until later next month, so if' you'd like try it out in the meantime, feel free!

i've only been in the herbal extract making business for about a year and a half now, with half that time being spent out at the farm and not in the lab, so many thanks for letting me bounce the ideas off of ya... if you're ever on your way to mt. hood let me know and maybe i can show ya around the facilities =]
 
nice read as always!

what is the best way to store the glycerin(long term) and what is the shelf life?

thanks,
 
about what % does the glycerin pull out in cold extraction for like 5-6 months? can't find where I read it but for some reason I remember mention of cold extraction only pulling out like 30-50% or so, is that accurate?

the reason I ask is that I have some jars sitting for a few months that i shake the piss outta every day, and wondering if it would be efficient to first separate the cold extracted glycerin, then reuse that same plant material that gets strained out and cover it with fresh glycerin for a quick run with the hot extraction and get two extractions from one jar of herb, killing 2 birds with one stone...or getting 2 birds stoned at once as it were, heh

good idea or waste of time doing the second hot extraction of the same material?
 
whats the best way for a poor guy to do the glycerin tinc, turn over once a day for 60 to 90 and use ambered buds if no access to oil? What is the max time for max potency doing it this ole fashioned way? Thanks for your time and trouble.
 
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