Degumming of extracts

steam is pretty magical too. pulls out nasty smelling sterols and fragments of decomposed vitamins.

mobin said:

you're the one who makes a living doing this shit right?

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If by living you mean being a few thousand in debt, and not having food around the house, then yeah I guess you could say that....my teenage daughter is making more money working part time than I am.

Thomas@LRL said:

Fascinating, do you do this before standard winterization then? I have been wondering if it's really necessary to go all the way through the process first to avoid slowing down first stage filtering.

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It does slow the filtering process but overall it ends up being much less work. Once I have my continuous feed centrifuge, filtration will will be the least of my worries. However, a 6"x48" column makes for a good push-pull filter with the right filtration media for the time being.

What are people doing with the water and citric acid? Has anyone analyzed for % recovery of THC/THCA? Or compared citric to just water?

G.O. Joe said:

What are people doing with the water and citric acid? Has anyone analyzed for % recovery of THC/THCA? Or compared citric to just water?

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just rolling through oil refining steps.

i wouldn't put a more polar acidic compound in there and not expect loss.

not like i dumped a ton in there for fun or something.

i don't think the amounts i've ended up with afterwards led me to believe i was murdering cannabanoids, in terms of crude/distillate, i'd say less than with standard multistage winterization.

I saw a dude on IG say "you'll still see waxes everytime you do the process so good luck getting them all"

i chuckled a little.

water washes do great. thats kinda what i was getting at with my last pic. i know my losses are less with just steam, but it's time consuming to boil off water until i don't see anything in the condensate. i hit it with water to chase off terps anyways so there's always a steamer at some point.

mobin said:

if i hold your hand now what are you gonna reach for when it's time to swim?

pay to play, google or crack a book.

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And by crack a book, I assume you are referring to Bleaching and Purifying Fats and Oils by Gary List, but please correct me if I am incorrect.

I appreciate your posting and having been using a similar method. This seems to be a reasonably simple purification step when used prior to or in combination with winterization. The downside is that the water reduces the proof of your alcohol making solvent recycle less effective.

Before discovering the acid-degumming process I have found strange gunk or gum in my rotovap and short path after performing a scrub with acid-activated carbon. The gunk was thick and black but could be washed to what I assume to be an insoluble grey gum. Interesting stuff! With the possibility of using washed waxes from winterization for lotions, soaps, and candles, what kind of uses could be found for separated cannabis gums?

Alister.Frazzle said:

what kind of uses could be found for separated cannabis gums?

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it's used in nonstick sprays and as "anti-sludge" in fuel/oil treatments.

G.O. Joe said:

What are people doing with the water and citric acid? Has anyone analyzed for % recovery of THC/THCA? Or compared citric to just water?

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Yes, @ColumboLabs and @Future4200 on Instagram are documenting their trials with oil processing with a caveat that people remember we are processing resin, and not vegetable oil and that accommodations have to be made for that difference.

Thomas@LRL said:

Yes, @ColumboLabs and @Future4200 on Instagram are documenting their trials with oil processing with a caveat that people remember we are processing resin, and not vegetable oil and that accommodations have to be made for that difference.

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yes. res.....oleoresin and even more correctly still.... gummoleoresins.

far few nhp than some food oils, but more than some.

all of the "food oil" qualities desired are the same,

shelf stable (wont oxidize and change color/polymerize on ya),
no stank (deodorized with steam),
transparency(improved with shit removed)

and all of the contaminants are the same or similar and are removed with the same or similar processes.

if everyone abided the food oil refining steps.....well we'd all have good medicine! distillate wouldn't change colors. oh the smoothness.

mobin said:

yes. res.....oleoresin and even more correctly still.... gummoleoresins.

far few nhp than some food oils, but more than some.

all of the "food oil" qualities desired are the same,

shelf stable (wont oxidize and change color/polymerize on ya),
no stank (deodorized with steam),
transparency(improved with shit removed)

and all of the contaminants are the same or similar and are removed with the same or similar processes.

if everyone abided the food oil refining steps.....well we'd all have good medicine! distillate wouldn't change colors. oh the smoothness.

View Image

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Agreed, but then people couldn't pass off less refined products as "less potent" and convince people that "numbers don't matter because it's a shell game". Personally, I'm trying to promote clean, widely available and consumer friendly, which implies cheap so processing has to be efficient. I'm applying these methods to Supercritical CO2 oil that has been diverted from the process stream as "waste" so I can better understand the impact it's having. My products currently enter product formulation as a 98-99% cannabinoid by volume distilled oil typically high 80% delta-9 with some small percentage of CBD, CBG and CBC. I like being able to give the consumer a clear idea of what they're consuming and some sort of informed expectation. I don't want them to have to wonder what the other 30% of the mass they're consuming is. -_-

I would be interested in learning more about your processing techniques. I have a pretty advanced setup and would consider compensating you for your time. Please let me know if you are interested.

Please forgive me for butting in but I've been researching extraction methods for best health benefits. All plants have waxes and many are beneficial for human consumption, such as the skins of fruits, etc. Might it be better, not for potency nor for smoking, but for overall health benefits when consumed orally?

Thank you for the cool thread and for your dedication to healthier medicine. I understand you only covered portions of one method. Okay, you got my attention. Forgive me everyone if I have overlooked any previous post answering these questions, just trying to wrap my head around this process and thought I would get this post up while I finish catching up.

A quick summary to make sure I understand the process: Add citric acid by means of (probably saturated) aqueous solution to the warmed alcohol-cannabis extract. Let gunk precipitate and settle to the bottom, freeze if you want, then separate. The solids are the trash and the liquid is the stash. Correct?

Questions:

1.) In your degumming example, what is the volume of the 4:1 that you add "a couple hundred ml's of water/citric acid" to? And what concentration of citric acid is used? Should it be a saturated acid solution?

2.) 4 parts alcohol:1 part extract in terms of ml:g or ml:ml? The former would be too viscous I think, but maybe not. And how would you calculate this without first starting with extracted oil that can be weighed out? Just estimate based on starting plant material weight? Or do you mean reduce the filtered crude alcohol extract to 20% of starting volume?

3.) How do you avoid ending up with citric acid in the final product? This is the most confusing part. In your example it seems like the final filtered liquid would contain at least some citric acid.

4.) How do you evaporate the degummed alcohol extract now that it is watered down? Having specific measurements of everything would probably eliminate this question if the amount of citric acid solution added is somewhat low, say <5% of total volume. And I guess the silica absorbs some moisture? Could anhydrous magnesium sulfate work?

5.) Can acetone be used instead of alcohol? Are there any other acids that could work? and/or is citric acid the best? I am reminded of FASI/FASA when reading this method, although that is applied to alkaloid extracts of certain plants and not cannabis as far as I know.

Like someone else mentioned, I can't afford to waste a bunch of extract on experimenting. I am now going to research this topic that you brought to my attention, so thanks for that!

Any points you might elucidate are greatly appreciated.

Trying to find anything else I can about this process online, but no luck. I have found references to a patented method of producing thc hemisuccinate for water soluble applications, which actually sounds very promising, but not the point of this thread, as far as I can tell.

I think it is irresponsible of the op to not give the full details of the process. Why post it at all? THC is not water soluble and as soon as you start adding water to the alcohol solution you risk having the extract fall out of solution, especially after most of the starting volume of alcohol has evaporated/been collected for reuse.

If the idea is to remove what falls out of solution, wouldn't you inevitably end up with some thc extract in the filter? After filtration, wouldn't you be collecting citric acid solution mixed with a now reduced concentration of thc alcohol solution?

Basically it seems like the process you are describing would ruin a batch of extract. But you also preface the post stating you don't explain the whole thing, so again, why post it at all? Why be so opposed to answering questions when your post leaves so many questions to be answered?

OP? Anybody? Not trying to ruffle any feathers, but we gotta keep these boards filled with useful information and be responsible about sharing it. Half-information is the same as no information.

mobin said:

steam is pretty magical too. pulls out nasty smelling sterols and fragments of decomposed vitamins.

View Image

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I'd like to understand the setup to do this process. I have a short-path, but don't understand the steam distillation process. If you don't mind sharing, I would appreciate it. Even if it's just the setup you use.

https://www.instagram.com/p/BZtga1Kg2tb/?taken-by=future4200

acid degumming is explained in multiple posts on IG. It may not be a specific step-by-step but one can easily compile enough a procedure that fits their needs with enough browsing. There is also a lot of information online if you google "acid degumming of edible oils" you will get a lot of good info that may not be be specific to our industry but still applies.

Caribbean Smoke said:

I'd like to understand the setup to do this process. I have a short-path, but don't understand the steam distillation process. If you don't mind sharing, I would appreciate it. Even if it's just the setup you use.

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Add water to your boiling flask, heat, stir, low vacuum 20-50 torr for average condenser with a trap, much lower if you can condense it fast enough like with a concentrator head.

Pack rings, beads, scrubbies can help the bumping from getting too far with a short path. Add a small vig column, 2-6" and maybe an additional condensor to run faster on the cheap.

Slow works, but residence times promote degradation especially in a noninert atmosphere. Act accordingly.

You will see oil bubbles seperating in the watery distillate until you are done.

Water in the flask works, a steam genny is better. Or run a second mantle with a vessel that can handle a lil pressure.

mobin said:

Add water to your boiling flask, heat, stir, low vacuum 20-50 torr for average condenser with a trap, much lower if you can condense it fast enough like with a concentrator head.

Pack rings, beads, scrubbies can help the bumping from getting too far with a short path. Add a small vig column, 2-6" and maybe an additional condensor to run faster on the cheap.

Slow works, but residence times promote degradation especially in a noninert atmosphere. Act accordingly.

You will see oil bubbles seperating in the watery distillate until you are done.

Water in the flask works, a steam genny is better. Or run a second mantle with a vessel that can handle a lil pressure.

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Thank you. I will be trying this soon.

Made a process mistake and need to get rid of the "strange gunk or gum"

Made a process mistake and need to get rid of the "strange gunk or gum"

Alister.Frazzle said:

And by crack a book, I assume you are referring to Bleaching and Purifying Fats and Oils by Gary List, but please correct me if I am incorrect.

I appreciate your posting and having been using a similar method. This seems to be a reasonably simple purification step when used prior to or in combination with winterization. The downside is that the water reduces the proof of your alcohol making solvent recycle less effective.

Before discovering the acid-degumming process I have found strange gunk or gum in my rotovap and short path after performing a scrub with acid-activated carbon. The gunk was thick and black but could be washed to what I assume to be an insoluble grey gum. Interesting stuff! With the possibility of using washed waxes from winterization for lotions, soaps, and candles, what kind of uses could be found for separated cannabis gums?

Click to expand...

I just tried acid-degumming and seem to have blown it. I added what was supposed to about 0.04% citric acid by crude oil weight at the outset of winterization. I immediately saw coagulation (might be wrong word) while crude dissolved in warm ethanol. After first freeze this coagulated material came out along with the normal fat. It was whitish in color. A subsequent freeze was filtered, then warmed and it went through a charcoal wash and was filtered through activated earth and 8 um filter paper. The material was lighter as expected. However during the rotovap as it neared full removal of ethanol the oil became hazy. When it was poured I found small particles in the oil and stuck to the walls. After a lot of work I cleaned them out and via scraping and rinsing. I filtered the rinse (was in IPA at this point) and found the material to be hard granules that did not look particularly crystalline. They were gray and varied in size and shape. I found they dissolved in water with a little action and foamed when exposed to hydrated baking soda. I found the bulk of material I left in the lab had absorbed water and become a sticky goo. Which sounds like what you describe.

Now I have a tray of material that is hazy and has these particles making it a failed batch. Looking for advice on what i did wrong and how to clean it up. I am thinking of using a hexane/water wash to pull out the water soluble material. Instead of using salt I was thinking of making the solution slightly basic and warm to aid in dissolving the contaminant.

I also have remaining material that needs to rotovap. I was thinking I should neutralize this and hope it stops the precipitate process that created the junk to begin with. I think I need to use an alcohol soluble base and believe lye, which I have around, would work. But totally unsure if this is going to get me in deeper trouble. Any help from this forum would be greatly appreciated.

sapes said:

I just tried acid-degumming and seem to have blown it. I added what was supposed to about 0.04% citric acid by crude oil weight at the outset of winterization. I immediately saw coagulation (might be wrong word) while crude dissolved in warm ethanol. After first freeze this coagulated material came out along with the normal fat. It was whitish in color. A subsequent freeze was filtered, then warmed and it went through a charcoal wash and was filtered through activated earth and 8 um filter paper. The material was lighter as expected. However during the rotovap as it neared full removal of ethanol the oil became hazy. When it was poured I found small particles in the oil and stuck to the walls. After a lot of work I cleaned them out and via scraping and rinsing. I filtered the rinse (was in IPA at this point) and found the material to be hard granules that did not look particularly crystalline. They were gray and varied in size and shape. I found they dissolved in water with a little action and foamed when exposed to hydrated baking soda. I found the bulk of material I left in the lab had absorbed water and become a sticky goo. Which sounds like what you describe.

Now I have a tray of material that is hazy and has these particles making it a failed batch. Looking for advice on what i did wrong and how to clean it up. I am thinking of using a hexane/water wash to pull out the water soluble material. Instead of using salt I was thinking of making the solution slightly basic and warm to aid in dissolving the contaminant.

I also have remaining material that needs to rotovap. I was thinking I should neutralize this and hope it stops the precipitate process that created the junk to begin with. I think I need to use an alcohol soluble base and believe lye, which I have around, would work. But totally unsure if this is going to get me in deeper trouble. Any help from this forum would be greatly appreciated.

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I had something of the same issue, with what sounds like the same mysterious white substance. I resolved it by putting the hazy or "Dirty Oil" into a beaker and began heating it up to 130c. once it reached temp I began to stir at about 700-1000 rpm. The weird substance started to trail up the sides of the beaker and rise to the surface. there they somewhat clumped together into a weird goo. I scraped off this goo (think skim milk), and carefully poured the "dirty oil" into another beaker. This beaker was then placed in the same position as the previous (on a hotplate with a stirrer at 130c, 500rpm). Next you wait to see if anything else seems to rise to the surface, if not then you should be good to go. Warning- it is a bitch to clean the substance from the first beaker, you may want to use a steel pad.