Disappointing yeilds

[Winemaker]

Okay so SWIM followed an STB that I found online. Looked pretty simple but ended up taking a while.

He and his friends got together to buy a bunch of ACRB. They blended everything up. Not to a powder, but was still somewhat chunky. Didn't do the whole freeze/thaw/blend process, just cut the whole bark into chunks and blended. It still had 1/4" chunks being the biggest pieces, with a decent amount of sawdust consistency.

Anywhoo, they mixed it all into a couple wine jugs with a bunch of filtered water, with a bunch of lye. They made sure to measuse the ph to at least 12, or at least in the general vicinity. They also added a little more a week or two into the process because they heard that the ph will change a bit after it all settles.

Anyway, the majority of the bark sat in solution for a month or two, with some of it being drawn off for extraction. All the bark has now been filtered off and it's just juice. The juice has been napped and extracted 5-6 times in total, between all the different batches.

Now, they've been freeze precipping and filtering everything, xtals and yellow/orange goop. They have about 10 g of goop now, with a mini a/b expected to be completed, along with a vitamin C (ascorbic acid) redox, just to make sure any goop that is oxide is converted back before the final extraction.

So they were expecting quite a bit more extract, but realized one problem came from the fact that the bark wasn't completely pulverized. They also didn't do the vinegar boils.

Any other ideas as to why yield would be on the low side? Considering that the goop is still going to be processed, bringing yield down to an estimated 7-8 g xtal.

Thanks in advance!

 

[Winemaker]

Also, the goop is definitely active.

 

[DansMaTete]

If you think you didn't get all the magic you still can process a new extraction if you kept the bark :

Freeze&thaw
Acid boil
Basification
Pull
Freeze precipitation

 

[ColorfulColorado]

It helps if you post things like starting amount of bark, amount of lye used, how you tested PH, what your solvent is(think I saw naphtha, but not positive).

If you want to talk yield, you have to start first with the amount of product that went into the extraction.

 

[Winemaker]

Oh geez XD

I got so caught up in the process that I forgot to mention something else. The process is pretty simple but not at the same time.

SWIM and his friends got 2.5 kg ACRB, using naptha to extract. The goop and xtals (some were solid coming out of freeze precip, the size of coarse salt grains! There was a heaping teaspoon of xtal pulled out of one freeze precip!) were all combined into a goopey pile knowing further extraction/purification would be necessary due to the inherent oils that come thru in a STB procedure.

Tested the pH with simple test strips, a buck a bottle at a local supply shop!

And yes, there are plans to further process the bark later on. Going to freeze/thaw/acid wash and zinc treat it all when there are supplies and a better location.

Hope this answers everything ^_^'

 

[ColorfulColorado]

Oh geez XD

I got so caught up in the process that I forgot to mention something else. The process is pretty simple but not at the same time.

SWIM and his friends got 2.5 kg ACRB, using naptha to extract. The goop and xtals (some were solid coming out of freeze precip, the size of coarse salt grains! There was a heaping teaspoon of xtal pulled out of one freeze precip!) were all combined into a goopey pile knowing further extraction/purification would be necessary due to the inherent oils that come thru in a STB procedure.

Tested the pH with simple test strips, a buck a bottle at a local supply shop!

And yes, there are plans to further process the bark later on. Going to freeze/thaw/acid wash and zinc treat it all when there are supplies and a better location.

Hope this answers everything ^_^'

That looks much better!:d
2.5kg=2500g, at average yield of 1% you should be pulling roughly 25g of SPICE from the bark, if it is root bark. If it's trunk bark, I think that yield diminishes quite a bit, and it's entirely possible that TB got sold as RB(think it happened to me too). Some of the goopy consistency can be attributed to NMT, and seeing as you did a STB, some of it can be attributed to plant fats as well.

How much solvent are you using per pull? With an expected yield of only 7-8g, you definitely haven't cleaned that bark out at all. If the bark was indeed mush as you say, then a vinegar soak wouldn't even come into play, the DMT would be freebased as the bark is destroyed. I'd say keep running pulls on it until literally nothing crashes out in the freezer, and then do one more and evap, if you get more yield, do another with evap, until there's literally nothing left. I think you're just leaving behind goodies in your soup is all.

 

[Winemaker]

Well yeah, that's what SWIM and his friends figured. Maybe it's coming into question because the solvent isn't coming out even close to saturated. The first couple freeze precips he didn't do right. He just stuck the whole volume in the freezer without even evapping any prior to. He still pulled out some stuff, and then he figured out he should evap by half then freeze precip.

After all these pulls, the solvent keeps taking on yellow colouring, and SWIM is just concerned as to whether it's just plant fats now, as DMT is more soluble than fats. Should it not be really easy to get the DMT out at least compared to the fats?

Solvent volume isn't really being measured. Have about 250 ml in at any one time, but there's a series of processes going on at once. One litre jar will be half full, freezing. When it gets the coffee filter treatment, it goes right back in, after the mixed solvent is pulled. Then it keeps getting exchanged, with a bottle or two of fluid going in every so often, to keep volumes similar in the face of evaporation (prior to giong in the freezer now lol).

SWIM and his friends were kind of stupid, in thinking it would be easy to run the whole thing at once XD

As for the amount of lye.. It was a total of 1 kg of lye in about 5 gallons of water. Would that be basic enough to destroy the cell walls? Like I said, they tested to 12 ph~ and put in a bit more lye afterwards just to make sure.

I guess they'll keep pulling. They've gone thru so much solvent alraedy but yeah makes sense to keep going. Do they keep going until there's simply no more colour transferring?

And pretty sure it's RB, based on descriptions.. Got it from a reputable-looking company in the country, although it's so hard to find good reviews of companies that deal in 'natural incense products' LOL

Thanks a lot for the help though, really appreciate you taking the time to walk me thru this. By the time SWIM gets to the end of the project and does the whole redox and re-x, I'd love to put up a pictorial tutorial to help others dealing with the 'dreaded goo' ^_^

 

[ColorfulColorado]

The solvent will continue to take on a yellow color as there was no defat step thrown in, I made a post about that exact problem here. Your yellowing is simply due to plant fats, I thought it was oxide, but after doing the research, I learned oxide isn't soluble in naphtha. Your best bet is to re-x after you guys pull every bit of goodies out of the bark, which it sounds like you're planning on doing anyway.

I won't hound you on chemistry practices, but it's usually a better bet to be precise with your measurements of EVERYTHING, less room for error. And what I would do is pour your base solution off into smaller jars, and then do pulls on that with a much lower volume of solvent. If memory serves, 50mL Naphtha can hold 1g spice. Did you save your coffee filters at all? I'd run clean naphtha through those, you could lose quite a bit in those filter papers depending. The hardest part is NOT touching the jars, I know, but it needs to be done, every time a jar gets bumped or nudged, the crystals fracture & start growing at a different angle(if that makes sense), leaving you with smaller crystals, that are more likely to get caught in a filter or lost in solution.

Not stupid at all, that's science buddy, figuring this out as you go is half the fun I would however recommend a smaller batch next time, that way you can figure out expected yield & tune your process.

One more tip, try to keep things metric, it simplifies ratios. I think for STB though, the recommended ratio is 1:1 NaOH:ACRB, so you might be (quite a bit) under that amount. That could have something to do with your low yield. PH of 12 would, of course, that's an extremely basic solution, but a PH of 14 should've been 'shot for' so to speak, in STB, the higher the better.

Colour transfer won't be your main indication, amount of spice in freeze precip, or after evap is. Just pull and pull and pull until there's nothing left, even if it's just coming out as goop, even if it's mostly NMT, on re-x you can get the little bit of goodies(every bit counts when you drop that much $$).

EDIT: I noticed you called it the 'dreaded' goo, have you bioassayed any yet? In my experiences ACRB 'goo' is much more active than crystals alone. I prefer it honestly, it's excellent for changa. The full alkaloid content = yummy!

 

[Winemaker]

Well, as for the oxide, because SWIM's been reusing the NPS, it's got a lot of plant oils in it. And from what I read, oxide is soluble in NPS when there's plant oils present. Was this wrong?

And yeah SWIM's been using larger amounts of NPS because of the large amount of soup (also because it's easier to pull when there's a thicker layer.. The vessel is 1.5-1.75 feet in diameter so 50 ml spreads really thin and is nearly impossible to really pull lol.

SWIM and his cohorts did have it separated into smaller jars at first, but after doing a number of pulls they combined into one large vessel for ease of use.

Definitely saved filters. Usually (during the pull/evap/heat/freeze cycle) NPS is pulled, then heated up, then the filters are torn up and stirred in before being pulled out and squeezed out, coming out basically clean.

Yeah the ph may have been lower than it was supposed to be. The cohorts were measuring as they went, so it's surely a basic soup but yeah it may not have broken the bark properly. Thus, why I suggested the cohorts keep the bark for further processing at a later date (after reading that it can sit like that for a long period of time without hurting the entheogens).

Also, I posted a new thread on re-x'ing, and you'll see why when you read it. I'd love your input if you've got some more golden wisdom to share

On STB re-x procedures - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

 

[Earthwalker]

First of all working with acacia stb will not work as well as a ATB TEK and 2-1/2 kilo of bark is a rediculas amount to do in one go !

So I'd expect to lose a lot more dmt then doing it in smaller batches , maybe try smaller amounts say 500gram until you get it dialed in !

Also if you're reusing you're naps that's not a smart thing to do because it's going to be over loaded with fats
" fats and oils isn't always nmt "

Anyway I'd suggest you do a ATB for the next extraction and have you're bark powderised ! And a defat is a must whether you do it before the basifying stage or do a mini ab at the end !!

 

[Winemaker]

Thanks earthwalker. Yeah, SWIM and cohorts definitely underestimated it. They'd performed a smaller batch a bit before attempting, so they thought it would be a quick one-off. HA. HAHA. HA.

Like I mentioned though, they've got all the bark saved and it's sitting mostly drained but still with the lye soup soaked into them. So they're going to leave it sit until they get a good lab setup again, then they'll blend it up, freeze it, and then do a full a/b. There's still lots left in the bark.