So I recently performed my first extraction. I followed Marsofold's tek.

Used vinegar as the acid. Mixed 500g pre-powdered mhrb in a crock pot and 1/2 gallon (~2 liters) of distilled water, heated up for about an hour, decanted the very dark red/brown liquid. I repeated with the remaining 1/2 gallon of water by adding 1/4 gallon twice and filtered all the water from the mhrb with a t-shirt. pH was measured at about 3, more towards 2.8 towards the end.

I reduced the ~4 L of liquid to about 700 mL without boiling (~70-80C). Defatted in a 1L sep funnel by adding warm naptha twice (near 100C- is this too hot?).

Added ~200 mL of NaOH saturated water. My pH meter was calibrated around 7 pH and was having issues reading above 13 (I think I would have needed the ~10 pH calibration solution to be very accurate higher- its actually a nice meter). So I added excess lye after reading it wouldn't be harmful.

Put alkaline solution (which was very black, sorta tar-like but watery) in the sep funnel, and performed 5 pulls with 100 mL of naptha each. Naptha was again warmed to about 100 C for each pull. Each pull was around 5 minutes. That might have been too short? I spun it around slowly, end over end etc.

Performed a calcium carbonate wash with very near saturated calcium carbonate/water solution followed by cold distilled water. Let it all separate very quickly and removed each time.

Lastly, evaporated some of the naptha, freeze precipitated. Left me with a bit of white/yellow crystals after I scraped out the jar. I didn't have a scale, but it was probably closer to 1 g or so (still not impressive!).

Recrystallized with heptane/bestine, I added warm (~55 C) bestine with an eye dropper. I only had to add a very tiny amount to dissolve all the white crystals leaving a layer of dark yellow oil and clear bestine on top. I sucked off the oil and put most of it back in the naptha. The heptane was free precipitated and poured off leaving 120 mg of white crystals.

Where did I go wrong?
Point's I think it may have been- naptha pulls- not long enough? Too hot?
recrystallization- too little heptane? Some tek stated ~15 mL of bestine per gram of crystal, I'm sure I added far less but it all dissolved still.
Quality of mhrb? I bought it from a vendor on bonanza. I recently ordered more from KTBotanicals having heard its good.

Didn't mention that I evaporated the remaining naptha again until it was cloudy, repeated the freeze precip, and repeated the recrystallization with the new crystals and the old crystals combined yielding the final 120 mg

Have you kept the naphta you defatted with ? Maybe it contains other solvents and pulled the dmt acetate, you could try to evap it, dissolve the goo in basic water and pull again.
Also you could try to add lye to your washes and pull again

By the way you don't need to defat mhrb, and washing your pulls isn't needed when you perform an A/B (a simple re-x is more than enough).

Was there any goo left behind during recrystallization?

Do you have access to any other solvent such as limonene or xylene/toluene?

Did you do a few cycles of agitation/letting stand before separating each pull? Was it thoroughly mixed?

Did you ever read of anybody using that supplier before?

(Naphtha will not dissolve dmt acetate, btw.. but yeah no need to defat )

Well since naphta is sometimes mixed with other solvents I thought it might explain this low yield, but I guess the mhrb was very bad quality since it's quite hard
to mess an A/B.

Hmmm interesting.. now im thinking that, if his naphtha had some mixed in polar solvent (acetone, ethanol, whatever), even if in small quantities, this would fuck up his extraction. How sure are you that your naphtha is good, newwaveparticle?

Or if the naphtha had some xylene/aromatics mixed in, it wouldnt freeze precipitate well, and some dmt would remain in solution. What did you do with that naphtha after freezing? Did you reuse it, or maybe evap it all the way? Hopefully didnt throw it away

Unfortunately I didn't keep any of the defatting naptha, all I have left is a tiny bit I evaporated down that was left from the first pulls I did (I've already freeze precipitated it twice). Theres less than 100 mL of it left.

During the recrystallization I separated the yellow goo from the clear heptane so after recrystallization it was pure white crystal left behind.

I probably should have mixed more/longer during the naptha pulls honestly.

I just ordered from ktbotanicals which has good reviews. I plan on doing a lazyman's tek of sorts. I've read its not that great, but I really don't want to go through the acid extraction step as it took quite a long time along with the straining. As far as I can tell I just got to make sure I've added enough water and lye to prevent emulsions...

Go for Noman instead of lazyman. Good luck

That's what I hear, but they're very similar. As far as I can tell the only difference in lazyman's tek from noman's is that noman's tek uses a jar to agitate the alkaline mhrb/naptha mixture rather than putting it all in a bucket and stirring with a spoon. Is that really that big of a difference? I was planning on stirring and allowing the naptha to sit for much longer (maybe overnight on the last 2 pulls or so).

Furthermore, I wanted to do another 500g extraction and I don't have a ~10 L container I could close up and use to agitate with.

Well if you do an STB with that amount of powder and not big enough container, you very possibly will have trouble separating the layers, + more likely to have the brown naphtha problem.

Either do an A/B, then, or reduce amount of mimosa. At least thats my suggestion

Lazyman uses too little water, and also the lye amount is enough but if you add more it helps preventing emulsions. Noman's tek also has sodium carb wash and freeze precipitation, both of which are recommended.

You're right, but I'm going to follow this protocol- https://www.dmt-nexus.me....aspx?g=posts&t=7536
It uses more water, but I figured I'd still do like 10 L for just 500g of powder plus 500g of lye

And I was planning on still doing a sodium carbonate wash and free precip and probably a recrystallization

I also figured I could be a little messier using a glass turkey baster and get extra non-naptha liquid and put it all in the sep funnel to be sure I get all of the naptha after the later pulls with naptha...

I'd use the lazyman tek myself if I could just find a potato masher that I liked.

is'nt 500 ml naptha for 500g bark just too less , maybe you should use 2 liters total , 5 pulls of 400 ml each !!! this can also be very wrong pls cofirm this with more experienced members , swim is just a noob

just checked out the marsfold tek (had not read it earlier) , it use 300 ml as is says ,
but lazymans tek and even vovin's tek uses a lot more than that for a lot less bark ,

swim has not used the marsfold tek before and probably never will
probably this is not the best tek

5x100ml pulls might not get all the goodies but it should def yield a few grams, not 120mg.

Yea I agree

I plan on powdering the root bark myself as well as letting it sit in the super alkaline water for a long time (probably a day or so)