I love the "Spock's Brain" user name!!!! That's a really cool name.
Spock's Brain wrote:Folks, a friend is considering doing another A/B extraction on some MHRB and would like some advice on some info he read in an extraction TEK that He recently read. This time He's going bigger, and for as close to transluscent crystals as possible, as opposed to an oily residue of insufficient quantity to re-crystalize.
1. An acid phase PH of 6 is purported to be sufficient to dissolve DMT, but leave other substance un-dissolved. Is a PH of 6 sufficient, or optimal? He had previously extracted at a PH of 2.
Bringing the pH down will extract more of some alkaloids and less of others. It all depends on the alkaloid in question.
Almost everyone is going to tell you to use pH 3-4. Extracting at pH 3-4 is the norm because some alkaloids have a low pKa and require that range. Also, some alkaloids are more soluble in dilute acids, but some are less so. For example harmine HCl is more soluble in pure ware than in dilute HCl. If using a Soxhlet, that concept is almost completely irrelevant.
You should know that when shamans make water extractions of DMT plants, they don’t add any acids to adjust the pH. They simply boil the plant material in pure water and that is very effective.
DMT has a pKa of 8.68, meaning that at pH 6.68 99% is in water soluble salt form, and at pH 8.68 50% is, and at pH 10.68 99% is in freebase form. So at pH 6 more than 99% is in water soluble salt form so that’s the perfect pH to extract at using water, if the salt form is highly water soluble, but some are not. Diplopterys and Psychotria contain highly water soluble forms of DMT and so no pH adjustment is ever needed to extract the DMT.
With most plants you can extract nearly 90% of the DMT at pH 6 by simply boiling it 3 times in water for 30 minutes each time. SWIM extracts in a Soxhlet using 91% IPA for 12 hours without adding any acids and gets about 99% of all the DMT out of the plant material (this applies to Mimosa, Diplopterys and Psychotria). The leafy plant material usually has a pH of 5-6 naturally because of the acids present in the plant. This of course depends on the plant material in question. A lower pH is not needed unless the water solubility of the alkaloid salt present in the plant is very poor, and that all depends on what salt of DMT is present in the plant. Different salts have different solubility profiles. For example, DMT HCl is far more water soluble than DMT picrate.
Spock's Brain wrote:"pH of 6 is used because this is the highest pH that will ionise the DMT, and because it is not so low as conventional techniques use, it will not dissolve anything with a pKa lower than DMT."
Yes. That is absolutely correct.
Spock's Brain wrote:2. He's planning on using ACETIC acid, instead of HYDROCHLORIC. Learning that Acetic being volatile, as opposed to more stable Hydrochloric, He's planning on reducing the acid phase to a more managable size, using a double boiler method, as the acetic is purported to "boil off," and not concentrate lowering the PH even more. Also, possibly needing less basification efforts. What's the best available form of ACETIC to use? Also, He wants to remove the concentrated acid from His domain. Overall, more managable volume, advice?
HCl (hydrochloric acid) also boils away just like acetic acid, so there’s no advantage there. But HCl is more dangerous to use so it’s better to use acetic acid.
Spock's Brain wrote:3. "aromatic" (turpentine, xylene) solvents are suggested to be used to wash, ie. defat the acid phase. the "aromatic" solvents are purported to be more powerful to remove unwanted substances, followed by a naptha defat wash to also remove any residue of the prior solvents. Experiences?
"Aromatic solvents are suggested in this step because they dissolve more than any other nonpolar solvent, and thus clean the product more than ether, chlorinated solvents or naptha/shellite. Do a final wash using the solvent that will be used for extraction to remove any excess aromatics suspended in the solution. This is done to eliminate the majority of the high boiling aromatic solvent from the solution so when it is extracted the high boiling component of the solvent is reduced. If there is materials that boil at a significantly higher temperature than that of the DMT (ie much more than 65°C) the dmt will not crystallise or dry properly, as it will boil before the solvent it is mixed with. This is known as 'oiling out' and is best avoided if possible."
SWIM says no. The best to defat with is DCM. DCM pulls out far more junk than solvents like xylene and it evaporates really fast, leaving no hidden residue like xylene. SWIM tested this and after all the xylene defats pulled out no more fats, DCM could still pull out a ton of more fats and oils. And of course if you plan to extract with naphtha, do a final defat with that solvent. But SWIM gets better results extracting with DCM and then doing a freeze precipitation with heptane. SWIM find naphtha to be a very poor extraction solvent.
Spock's Brain wrote:
The advice my friend read is from Soma's Complete Acacia TEK, maybe using MHRB so much defatting is not needed. He previously defatted with naptha His MHRB acid, and removed oily residue each time.
Advice, experiences? I'll post his results when he completes it. Also, he will attempt re-crystalization for first time, this time also.
Don’t skip the defat step if you want really clean results. MHRB has oils and fats in it. Its not as much as the leafy material, but it is there. However, most of the oils and fats in MHRB aren’t very soluble in heptane or naphtha. If the final dried extract is dissolved in a small amount of heptane or naphtha, most of the oils and fats won’t dissolve. The heptane/naphtha can then be poured off leaving behind the junk. Then the DMT can be freeze precipitated for a really clean end product. When freeze precipitating DMT, the defat step is not that important.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.
If you see me at the waterpark, please say hello. I'll be the delusional 50 something in the American flag Speedo, oiling up his monster guns while responding to imaginary requests for selfies from invisible teenage girls.