I have a question to see if I can’t more easily integrate the degumming step into my current workflow. What would happen if I added crude to ethanol, let it dissolve, then added the citric acid to the ethanol + crude. Then winterized the crude + ethanol + citric acid, filtered cold, take the filtered solution and pulled ethanol in a rotovap, then purged the resin and loaded it into a short path and distilled the crude. Would the citric acid get into my short path? Would the citric acid get distilled into my resin distillate if it go into the short path, promote isomerization, and is there anything I could add to the short path to stop isomerization and just clean out the acid when it was time to clean the short path?
Another question, do I need the magnesium enhanced filter, or would using a few extra filters do the job of getting rid of most of the gum and citric acid? Could I pull the ethanol and wash the crude + citric acid with saline to remove the citric acid? Using these other solvents or the magnesium filter isn’t the best option since I can’t get them easily.
Something I noticed, something seems to be removed to an extent by paper filters and not silk filters. It forms a layer that looks like it is made of fish scales.
Well, it sounds like a bit of a mess. It is helpful to Winterize before degumming for a few reasons, like being able to tell when it is done.
The method you describe naturally leaves the citric acid in the crude unless you do a liquid partition extraction from aqueous ethanol with non-polar solvent. Otherwise you must neutralize the citric acid to make a salt that is stable at cannabinoid distillation temperatures.
Cold precipitation and filtration of the fatty acids created during degumming works, but a hydrated silica type media works best to sequester the smallest chains and phospholipids. However, that only works well when filtering from non-polar solvent, not so well from ethanol… just because ethanol gets stuck in said media.
Not sure you understand a “saline wash” also requires non-polar solvent, but it does.
I will winterize the crude before degumming for sure. Thanks for the tip.
I did think the saline wash referred to salt water. I would have to use hot water to liquify the filtered crude and wash out the citric acid without ethanol. I had mixed results washing hot winterized oil with hot distilled water in the past. I noticed the purple rose color that appears in my concentrates and has a burnt rubber smell washes away in the water, and all I need to do is dry our the concentrate. Unfortunately I think the water promotes oxidation partially defeating the purpose and its a lot of work to work with hot resin and water.
Have you ever tried distilling with citric acid in the short path. I’m worried it will promote isomerization of THC. Is a lot left without the magnesium filter even if the filtration is done ice cold in fractions?
My ethanol tests at about 3.5-4 pH right out of the barrel
Could I get some clarification - should I bring my solution back to the starting pH of 3.5 or bring it all the way up to a neutral 7? End goal is distillation
EDIT: forgot to mention the cannabinoid:etoh solution is currently reading 2.5pH
If it started at 3.5, then 3.5 is “neutral”. However, if all you did was dissolve cannabinoids in ethanol, then don’t mess with the pH. You only need to adjust it for very particular operations. Simple extraction is not one of them.
If making an oil not meant for distillate, could a person still degum using this tek and effectively filter out the compounds added for degumming with repeated filtrations over magsil?
Aside from the could… Would you want to degum an oil that wasn’t going to be distilled, but was still intended for disposable cartridges?
I don’t think it matters much. The carts have terpenes (added or naturally occurring) that discolor with light, air, and repeated heat exposure all present in cartridges. Ultimately, if those “gums” are really the antioxidants I believe they are, leaving them in the cart juice is actually beneficial to retaining the cannabinoid potency over time.
Could you clarify for me “Water clear Δ8 is made most often by adding acidic decolorants (such as activated charcoal) to the boiling flask”. So you add activated charcoal straight into distillation?
Afaik, a “small” amount of citrate doesn’t do much, but although it is a weak acid, it still has 3 relatively labile protons, so it can still affect some amount of isomerization. Because citric acid’s 1st proton is just a barely stronger acid (1st pKa 3.13, then 4.76 and 6.40) than THCa (pKa 3.41), and because citric acid does not readily decarboxylate, there is probably a slight possibility for some isomerization. I’m pretty sure that THCa has 4 proton accepting sites and 1 donor site, and I am not certain of the relative strengths of these acceptor sites, but they are strong enough to allow isomerization. I would be more concerned with isomerization of CBD to Δ8-THC in a weak Brönstead acid like citric, as its isomerization rxn happens more readily with less activation energy than that of Δ9-THC to Δ8-THC.
So if I have performed a citric acid degum and am going into scrubs, should I neutralize pH before the charcoal scrub? I was thinking of doing the charcoal scrub at a low pH and then correcting it in the filter cake that removes the charcoal, and then doing a second scrub at neutralized pH with bentonite.
The short answer is I don’t know. I don’t recommend neutralizing the acid with a base, since that creates water and a salt, which stay in the crude. A partition of a non-polar solvent and the alcohol (if it’s in ethanol:water azeotrope, which I assume it is, since you talk about adjusting pH) after adding excess water is the best way to wash out the acid. I also don’t think degumming is entirely necessary if you are scrubbing or adsorbant filtering in the first place.