An appetizer to entice you to read further: from 3 A/B extractions done pretty much the same way each time, I got a final net yield of 2.01% (freebase). Picture below shows final product.

What I'd like to see here are comments from people that have done extractions with soup at lower and higher pH values (i.e. one extraction @ pH 11.6 and another done @ pH 13+), and any notable differences in experience from resulting product. I wouldn't doubt that pH will affect the appearance of the spice in the end, but I'd rather keep that topic at a minimum here.

I'd also like to see comments on any notable difference in experience from product made at 70°C vs 90+°C using naphtha as the NPS.

Reading the outline of my extraction method below is not required to answer the above questions, but it's here if you want to read - however, the most pertinent details for this topic is the ratio of NaOH/soup @ 100g/1850mL which I suspect made pH around 13.5, maybe more; and the near boiling temps maintained throughout the extracts.

Naphtha as NPS pulls *mostly* just the DMT as I understand it, at least at lower temps like 60-70°C, but what I'm hoping for with the higher temps is more full spectrum from the MHRB (jungle spice), but unsure if this is the case or not - please mention whether your input in comments is speculation or actual experience

---

4mL HCl added to 1400mL H2O in 2L Erlenmeyer flask, then 100g mhrb added and stirred near boiling temp for 75-90 minutes. I don't have normal heat plate for this, but I have this device with a stainless pot that has heating coil in it and magnetic stirrer underneath it, and oil is added to the pot and Erlenmeyer flask placed in this pot of heated oil. Then 400mL H20 that has 100g NaOH dissolved in it gets added to soup, still being heated and stirred (bark material is NOT filtered out). Then naphtha gets added to this and stirred strong enough to create full vortex - this does create emulsion but pretty much guarantees maximum contact of naphtha with 100% of the soup.

The stirrer is then turned way down almost to a halt, and emulsion takes awhile to break up and separate, but again this is done with the oil @ 105-110°C and I do this on purpose because it makes continuous bubbles that break up the emulsion. Once a clean separation line is seen, oil temperature reduced to <90°C to stop the bubbles, and the naphtha is pulled from the top with pipette. I leave approximately 1-2mm of naphtha in there so I don't get any basified soup in the pipette.

Approx. 700mL naphtha collected from 4 pulls for each extract, and the collected pulls go into distillation apparatus. The first extract I did, I had about 230mL dmt/naphtha that went in the freezer and 470mL was distilled out. Yield was 1.28g for first extract, but then of course the yellow naphtha was carried over to next two subsequent extracts. I combined the naphtha from the second two extracts (1400mL) and distilled this down to 75mL, emptied this into small fritted buchner to collect the glass beads used for boiling flask. Then the boiling flask was rinsed with 100mL fresh naphtha this was also ran through the buchner still with the glass beads in it, and this now yellowish naphtha was added to the 75mL in crystallization dish, then got wrapped up and placed in styrofoam box, then into fridge, then freezer. 250mL clean naphtha was also put into freezer at this time...

The next day, the crystallization dish was taken out and majority of precipitate was scraped (as quick as possible before it warmed up) while still in the cold naphtha, and everything went through the fritted buchner, then the 250mL clean naphtha from freezer was pulled through the buchner to wash and minimize any oily product, as I desired this to be powdery with no oil.

To my delight, the yield from second two extracts combined was 4.76g - pretty sure that spice carried over in yellow naphtha from first extract that didn't precipitate out. In total, 6.038g from 300g bark.

Dang. Nice job.

I've been told that higher temps break down DMT and create emulsions, but with a 2% yield, I don't know if that statement holds water or not. I'll leave that to the experts.

I can't account for yield in terms of pH being closer to 12 vs 13.5 as I too add 1g of NaOH per 1g of MHRB. Would like to know as well.

Just wanted to chime in and give you a congrats for the nice yield. Product looks great!

I do everything hot. Get more with less solvent that way.

Heating the soup properly doesn't raise the temp enough to destroy DMT in the soup. And using heat is how one would break up emulsions.

And great job!

One love

Thank you, both! I can't deny I'm feeling smug about the yields. I have yet to bioassay.. just want to finish extracting and put the equipment completely away, then try some re-x and convert a bit to fumarate for preserving and oral use. If I had more time and less paranoia, I would try experiment with filtering bark material for a batch with all other things being the same, to see difference in yield, appearance and experience of spice (some complain about the yellow being sub-par, others say they prefer experience of yellow over the pure white).

I want to compare the yellow to re-x white, but not going to lie, I'm slightly terrified of the bioassay work ahead of me....

The higher heat is definitely transferring more product, I guess I wonder if it transfers anything undesirable from MHRB. Someone mentioned that with Acacia, lower temps 60-70°C are preferred to prevent unwanted plant material from transferring,

One thing I did try is another batch with 50g NaOH instead of 100g. The yield was still over 2% and appearance is indiscernible from the extracts with 100g NaOH. The only difference I noticed is that the emulsion in flask with the smaller amount of NaOH broke up much faster.

Last thing I want to mention, and should've said it in original post, is that at these near-boiling temps, it is a hazardous situation, and I'd hate to see anyone get hurt from caustic solution expand/boil and shoot out top of Erlenmeyer flask with highly flammable solvent on top... stay safe everyone.

If it's crystal, it's likely all DMT. I feel that much concern over yellow vs white is 1. a matter of preference, and 2. a byproduct of the power of suggestion.

I did two extractions side by side. The only difference between them was that in one only distilled water was used and filtered was used for the other. The yields were relatively the same, however the extraction that had filtered water came out with denser and yellow crystals than the distilled water soup which produced snow white flakes.

Interested to hear how your bioassay trials go. Stay strong, you got this.

One love

Just to share (more with respect to heating everything before pulling).

This was from 2 pulls of about 75ml each. So, with the heating process I've been experimenting with. A major difference in this method is that the crystals precipitate with more density, and along with that, a yellowing (polymer).

One love

That's useful data. I've posted on the minimum polymer thread about taking my yellow/orange FB and doing a mini A/B, using citric acid and water to back-salt, remove old NPS and add fresh heptane, then slowly basify, then do heptane pulls, all while keeping temps <50°C. The result was a barely noticeable reduction in yellow/orange... I thought the acid during back-salting was supposed to break up any long polymer chains of DMT (orange).

I've kind of given up on the minimum polymer approach, and now getting things lined up to take FB->fumarate->FB, by dissolving FB in anhydrous acetone, filter out solids, add FASA to the filtered acetone till it stops precipitating the fumarate, decant/dry, then convert back to FB (dissolve fumarate in vinegar water, basify, heptane pulls, evap)

Orion shared some crystal pics where he followed this process (to best of my knowledge) and the results were stunning. For one thing, very large crystals; but also beautiful clear/white.

Do not worry about temperatures. For over 4 days I kept DMT at 170C. It didn't decompose at all.

Wow. 4 days @ 170°C!? Thank you for helping me weed out rabbit holes I don't need to go down...

Famine, was it in a solvent? Or was it in an acidic solution? Water? Just sitting out by itself in FB form?

By itself as freebase form

Then I guess everything I've read has been a lie! The cake isn't real!

Yes it is quite beautiful. On cooling it spontaneously crystallises completely! Very beautiful. You check and it's liquid, check again and it's just big crystals everywhere haha

So hot pulls = yellow spice but higher yields due to increased solubility


Room temp pulls = white spice with slightly less yield and anything colder you risk even lower yield.






If I'm understanding correctly based off everything I've read?

In my extremely limited experience and knowledge, evaporating Naptha gave yellow crystals whereas freeze precipitating gave white.

Yeah... but with heptane recristalization you can compensate excess oil and fats in hot pulls