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?
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Yes, but that is a method that yields a mixture of Δ8 and Δ9.
What is a known. Consuquence of having small amount of citric acid in the boiling flask ?
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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.
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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.
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What happens if i do form a tough emulsion?
Should i simply add brine to break the emulsion?
Could i intentionally make an emulsion for any beneficial purpose? For example salting out cannabinoids
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What happens is the polar and non-polar become hard to separate… that’s kind of a defining feature of an emulsion.
Sometimes using brine helps keep it from forming in the first place, but adding salt to an existing emulsion can backfire sometimes.
Yeah, people make useful emulsions all the time.
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Anyone try this with tartaric acid? I recently read someone mention they much prefer it over citric acid, but I was a bit inhebriated at the time reading it and can’t find reference of it for the life of me in the search bar to ask them why that was? Though I may have seen it on Instagram…
Magnesium hydroxide will react with citric acid to form magnesium citrate and water, and a little heat.
You could react numerous hydroxides with the citric acid to neutralize it- calcium, potassium, etc
I’ll be trying this as soon as I am up n running.
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I’ve got a boatload of fumaric acid, lactic acid, phosphoric as well- would be interesting to see if these change things at all.
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We also supply analytical standards. Always down to talk Kratom.
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Would adding magnesium hydroxide to the solution work to correct the PH?
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yes it should. depending on the strength of acid applied in wash, you can used a variety of solutions to neutralize (sodium bicarbonate, sodium hydroxide etc.)
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As mentioned, the strength of the acid is critical here! You can dilute your concentrated acid to the correct pKa (slightly more acidic than THCa - pKa = 3.4)
And then neutralize with a base of your choice, @Photon_noir seems to prefer MgO…I think? But this will then require a liquid liquid partying to solubilize the Magnesium Citrate into the aqueous phase.
If you read above he talks about how magnesium citrate doesnt start to degrade till over 200c, I don’t think you’d have any problems leaving it in there.
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So fill the sep funnel with the filtered crude ethanol slurry and then add water. The water will move the cannabinoids out of the ethanol.
Why can’t I just collect the two layers separately? What is the purpose of adding an alkane (In my case we’re using hexane)?
Is the salt water what neutralizes the citric acid? why not just wash the resin with salt water?
Just learning the why behind what I’m doing.
We processed a ton of crude with the citric acid and it’s amazing how much gum we are getting out. Thank you so much for the write up
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The louching forces the cannabinoids (resin) out of the aqueous phase (alcohol) and without a carrier solvent to move into the resin will likely deposit and stick to the container you louched in (or form emulsion in water). You want to add an alkane (non polar solvent) to pick up those cannabinoids that got kicked out of the aqueous phase thereby separating your target compound(s) from (polar) undesirables.
To neutralize the citric acid MgO is commonly suggested since the end products are pretty bening when it comes to further refinement processes. Neutralizing acidity is suggested if your resin’s pH (in alcohol) went <5. If I recall (somewhat) correctly, the ideal pH is between 5.5 and 7 (depending on what intended end product is). Mind you ethanol/isopropanol are inherantly slightly acidic.
You might also want to employ MgSO4-Anhydrous which absorbs water into the salt solids thereby drying your alkane - great to use before decanting resin-laden alkane out of sep. funnel. Filtering out the residual salt solids with filter paper and/or filter aid such as celite/T5 would catch any residual salt solids, depending on how well you decanted.
Salt water (brine) is a more polar solution than distilled (or plain) water. Having the aqueous phase to be more polar increases the non-polar solvent’s ability to pull up the cannabinoids while at the same time leaving behind polar components (non-targets). Washing the resin in salt water would be a bit cumbersome in my opinion being that the resin is somewhat hydrophobic, unless it was mixed in while resin was hot…but then you likely have to add an alkane to be able to separate the resin from the saline solution. Can’t just freeze away the saline from a resin afaik.
If you were to wash an alcohol slurry with salt water, well, then you aren’t doing a LLE (since only having one phase - aqueous) which requires the use of two phases to move target compounds from one to the other, often leaving behind undesirables as it transfers.
Hmm… perhaps one might louche to the point of making the aqueous phase mostly water and then freeze the solution to try to perform some separation. Not sure that would be an effective path to take.
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Hello and good day Sir,
I love Future4200 it is the best source of cannabis information on the web in my opinion! Kratom has been a Godsend for me! Many many years in the growroom and other forms of manual labor has ruined my lower back. I don’t like to take prescriptions for anythung and I absolutely refuse to take opiate painkillers. I do understand that kratom can be addictive due to the opiate like alkaloids so I do use caution when taking it. I would like to be able to target Mitragynine and 7-OH-Mitragynine for extraction. Have you done any kratom extractions? I have done some room temp ethanol extractions with good success. Just wondering if you have any tips, tricks or other methods for kratom extraction that you would be willing to share. Also curious if you have any good suppliers? I currently get mine from Gaia Ethnobotanical (now MitraGaia.com). I have never been disappointed with thier products. They had a black friday sale offering $65 kilos not sure if they ended the sale yet.
Thanks in advance for any advice or input!
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