Citric Acid Degumming Tek


#61

Is the citric acid fully dissolving still?

Or is there some left floating around when swirling?

Is it cloudy?


#62

I added the citric acid two ways in separate trials. First time, I added solid, and it was difficult to tell if it all dissolved (my solution is very dark). Second time I added the citric already dissolved in a concentrated water solution, and it seemed to mix in well. There was some cloudy precipitate, but i thought it could have been just the water causing it. Either way, the pH strips weren’t really reading anything.


#63

All you have to do is shoot for water white transparency and high cannabinoid purity, since the cannabinoids will naturally turn salmon pink by oxidation to quinoids. That said, I have achieved salmon pink by simply utilizing a typical quantity of C-bleach and the antioxidant Eugenol in minute quantity simultaneously during a spinning band run from 1st pass out of a stainless wiped film (which tests in the mid 90%s). I have also seen a very strange (reversible by temperature fluctuation between room and refrigerator temperature) version of salmon pink develop from yellow Δ8 that was made from CBD using standard Brönstead acids. There is much we have yet to learn.


#64

You are degumming with the citric acid… the vegetable oil being produced in that reaction is the precipitate. The acid is likely being buffered by the presence of phospholipids, which are being torn apart and neutralizing (actually complexing) the acid on the “alkaline” phosphatide ligand left over. You may have quite a lot of “lecithin” in your crude. Just the strongest hunch of a few.


#65

Thank you, that does make sense. Does that mean I should add more citric acid to overwhelm the buffering, or am I good at this level?


#66

Strangest thing happened today…

I’m assuming I’m either close or I messed something up lol.


#67

What are you trying to accomplish? My gut says you should add citric until it no longer dissolves OR until you see a tiny increase in pH. Btw, I forgot you added water. Be careful doing that, as it can begin to precipitate cannabinoids.


#68

That looks purple to me.


#69

Very VERY purple… except it condensate on the top of the glass.

As the gold the stream was thick and steady, the purple condensed all along the top and the two did not meet until falling into the same flask.

Literally a gold thick stream on top and a purple thin film stream on top…


#70


#71

Run your condenser hotter you can get the purple to bypass the flask. I think that the purple that condenses separately comes from anthocyanin. You can also remove it with a saline wash. I’m guessing it smells kind of sour and streaks when it is coming down the condenser.


#72

It sort of looks like smoke particulate. Have you ever smoked a ham or turkey? It is that color that permeates. I have seen that color in steam distillations come out in the aqueous layer. I believe I was smoking the oil inside the flask with a very hot mantle.


#73

The purple may be CBD if you had MgO or other alkaline treatment.


#74

I second @highestzen if you run your primary condenser at a higher temperature you can prevent that purple from condensing with the Cannabinoids


#75

I normally run the consenser dry
First time I’ve ever seen this

I just finished another run and it didn’t happen…

Definitely not any plant material burnjng

Not high cbd or anything

First and only time that’s happened… thanks for all the help guys!!!


#76

So I’m in the middle of doing this right now and some kinda weird things are happening…

I was given some (not so great) BHO crude. Normally, when dewaxing/winterizing BHO I lose about 30%. Now I knew this stuff wasn’t the greatest, came from old oxidized trim that was blasted in a closed loop w/o a filter or dewaxing column, and probably not as cold as it could of been. Anyway, thats the crude I’m working with and I have quite a few kilos of it.

I may of rushed things by not doing a neutral pH winterizing first. I wanted to combine winterizing with this degumming step. So I diluted at 25-30C and slowly added food-grade anhydrous citric acid until it wouldn’t take anymore. I noticed the solution turned more amber/orange in color after adding it, and the fats really started to curd and separate, looking like a colloidal solution. Basically looked like when you pour bad half and half into hot coffee. So I froze it like that.

I separated the dilute solution into 2 separate containers. I added MgO to one of them, and tried pouring the other through a MagSil bed, which clogged with so much shit that I have up and dumped it. So I went the MgO route on all of it, but must of added to much to one of the containers as it went purple and was reading around 11 pH on the strips. So I slowly added more citric acid, and it got less purple and more fat curding. WTF! I had to go through all the filter paper stages again, and winterize again, and more precipitate. It seems never ending! I ended up adding some citric that didn’t stir in right and was still solid and it fell into the filter and got sucked to the paper. When I got to the bottom, all this fat was clumped around the citric acid crystals. The carboy also had this webbing of fats that I couldn’t remove with solvent alone. Solvent + KOH removed it though, luckily.

At this point I have almost a bucket full of fats and waxes and it just keeps precipitating. I keep filtering and just keep getting more and more and more. I haven’t weighed how much fats I’ve pulled off because I haven’t removed the residual solvent from it, but volumetrically it looks like almost the same as the starting material.

I’m down to the 1um filter paper, and I’m still getting more and more. I set some aside to play with, and adding citric makes fat fall out, raising pH with MgO or KOH makes the fats dissolve back into solution, or at least turn into this semi-soluble sludge that doesn’t flocculate well. It seems that no matter how much I filter, repeating this cycle of raising and lowering pH just makes more fats precipitate. How do I know when I’m done? Am I losing cannabinoids? Is this crude really that shitty?


#77

Magnesium citrate salt may be insoluble in the ethanolic solution. Perhaps that is what you are seeing, since you added so much citrate. Normally, one would add citrate until no more “gums” appear to be precipitating, but that is only easiy visible after an initial (at least room temperature) filtration of the ethanol:water:resin solution.


#78

So would you recommend winterizing first at a neutral pH, and then degumming and filtering at room temp?


#79

The last step to add would be some more cold filtration after adding degum acid or enzyme, but yes.


#80

BHO crude ALWAYS does that. I’ve resorted to pouring my winterized material through a 100micron aquarium filter sock to get most of the chunkiest stuff separated before my finer filters to attenuate the clogging. I dump that filter sock’s contents on a Buchner of its own and rinse that crap with fresh solvent. Winterization on BHO can be as lengthy as all it’s subsequent processing combined if you’re really trying to get everything outta those lipids and wax.