Ok, i now undersrand this.

Yep, only things i can think of are that solvent was so over diluted that the water was “bound” in the EA or not in freezer long enough. “Free” water in solvent should freeze into bottom ice layer and perhaps top ice shards.

Finally ready to start the Solvent Repeated Reuse trial.

2/3: I have 5 jars of previously sodium carbonate-water washed solvents in the freezer (washing treatment B): Solvent S (S-S) - used standard solvent; S-B - used solvent from boiled-water paste; S-M - used solvent from microwaved paste; S-C - used solvent from chilled paste; and S-MC - used solvent from microwaved & chilled paste.

Once the ice puck and shards are removed from each jar, the first of three additional serial washing-freezing-extraction cycles will be run with these solvents versus a fresh EA run. The first extractions will be run using the standard tek scaled for 45g cactus powder runs using passive crystallization. The two subsequent sets of runs will be run the same way, but each will use 15g less cactus powder than the preceding sets of runs, to ensure that sufficient amounts of each solvent are available to complete the series.


2/6: Got delayed a couple days, didn’t have any observable effect vs 24-hr freeze. Decanted solutions through wire strainer-paper coffee filter-funnel into collection jars, separating ice shards from solution; frozen sodium carbonate pucks remained in original jars. All jars have a haze, so will let them settle a day or two, and decide whether I take the time & effort to do a dry sodium carbonate addition, before proceeding to the extraction runs. Once ready, I’ll post pH’s and a pic of solvnts.


2/10: Several layers of haze have settled, but jars still remain slightly hazy, I said screw it (with an F), and took the day off to run six 45g standard, scaled cactus powder runs, with the five once-used, washed solvents listed above and a fresh jar of EA. They all started at the same pH=5, nothing unusual to report through salting. Pics of the solvents and combined pulls are attached. Yields and any significant observations will be reported after 72hrs of passive crystallization.


2/13: All runs filtered after 72hrs passive crystallization, jars rinsed 2x w 5ml fresh EA and dumped through filter, filter rinsed 1x w 10 mL fresh EA, filtrated rinsed 1x w 10mL fresh EA. Pic, after filters appeared dry, attached. Jars washed 2x w 5mL hot distilled water, evaporated, scraped. All runs produced same appearance, fluffy white needles; which at these quantities is quite a beautiful sight. Total yield for each run rounded to 1.7%: fresh EA 0.754g, reused standard solvent 0.779g, reused solvent from paste made with boiled water 0.765g, reused solvent from microwaved paste 0.775g, reused solvent from paste made with chilled solvent 0.760g, reused solvent from microwaved paste made with chilled solvent 0.762g. Imo, quantities larger than fresh EA run are the result of slight calcium citrate precipitate from washed solvent.

Solvents will be washed with sodium carbonate-water method (steps 2 - 5 described here: https://www.dmt-nexus.me...mp;m=1133316#post1133316 ), and after settling clear will be frozen for 24-hrs, decanted off of ice, then run in 2nd reuse.

2/20: After cloudiness settled, but all jars still had a haze, jars were put in fridge for 3 hours, appearing clear they were removed and allowed to come to ambient temp, a slight haze remained, but were placed in freezer.

2/21: after 24 hrs in freezer, jars were each decanted through a previously chilled seive-coffee filter-funnel to remove ice shards. Filtered solvents all had a heavy haze (not cloudy), and placed in fridge for 3 hours to settle haze, then stored at room temp.
Approximately 320 mL recovered of each de-iced washed solvent. Ice, defrosted puck water, and some amount of solvent trapped with ice shards were collected in a waste jar for further settling/separation.


2/23: Started 2nd Re-Use Trial, using six 30g cactus powder samples with scaled ingredients in: fresh Ethyl Acetate, and the five used solvents tested earlier. Each paste wss prepared in the standard way, then pulled 6 times (1 min stir, 2 min rest prr pull). This is the 3rd use (2nd re-use) of the five used solvents, Prior to salting each jar with 1.5g of citric acid, each jar was settled for at least one hour. No water was observed in the solvents, however all jars except the fresh EA jar had significant haziness. The hars will be passively crystallized for 72 hours.


2/26: Jars filtered after 72 hrs, jar washes evaporated; pic of drying filtrate below. The fresh solvent yielded 0.4683g, 1.6%, the yields of solvents’ 3rd use were: solvent that originally pulled standard paste 0,5745g, 1.9%; solvent that originally pulled boiled water paste 0.6072g, 2.0%; solvent that originally pulled microwaved paste 0.5863g, 2.0%; solvent that originally was chilled and pulled chilled paste 0.5873g, 2.0%; solvent that was originally chilled and pulled microwaved & chilled paste 0.6845g, 2.3%. Product from each run appeared and tasted similar, and had consistent appearance and taste as earlier runs.

I doubt the higher yields from the reused solvent runs vs the fresh solvent had anything to do with higher M levels, the cactus powder was the same for all runs and I doubt that any M from earlier runs remained in the reused solvents after the sodium carbonate-water washes and freezing. Rather, the higher yields are likely due to precipitation of calcium citrate.

In the next few days I’ll wash the solvents again, settle, and then freeze them. After removing the ice and letting them clear, I’ll do the 3rd reuse (4th run). I will be focusing on doing this next set of runs with crystal clear solvents (unlike the run that just finished), to see if this approach can reduce the suspected calcium citrate precipitation. It may take some extra time to get the solvents to settle clearly.

3/4: Light stirred 42mL of washing solution into each jar containing approx 280mL of solvent; after layers appeared, stirred 5 full revolutions (5 seconds; enough to fully mix layers); washing solution made according to previously mentioned post. Initial pH ~3.0, post mix pH 4.0; got to get back to pH of 5-ish, after an hour stirred 5 more revolutions (5 secs), in hopes of neutralizing with minimum haze after settling.


3/5: Light stirring has helped improve settling speed, solvent layer about 1/4 clear in 24 hrs; However, initial stir-in plus 2 light stirs only partially neutralized pH. Did one additional 5 revolution stir today, pH rose to comparable (5-ish) level of fresh EA. Will let solvents settle, then freeze & decant.

Due to large excess yields in previous run (more than this cactus powder yields), I want to try to rule out the possibility that dissolved M is remaining in the solvents after the washing process. So, after this washing cycle, I’ll re-salt the solvents with citric acid to see if any crystallization occurs; if M crystals do not form, I think it will be safe to assume that the excess yield is due to calcium citrate precipitation. After re-salting, I’l re-nuetralize, wait until solvents become crystal clear w no haze at all, then do another decant to minimize calcium citrate (could be a long time waiting for gravity to do this), and then begin 4th-use run.


3/9: Decided yesterday, in an attempt to reduce haziness after freezing, to syringe decant the cleared solvent (~80%) to clean jars, and then further decanted 90% of the hazy remainder to testtubes. I’ll decant the clear portion in the tubes & recombine the cleared portions after a few more days of settling. The cloudy/hazy residuals were decanted off the sodium carbonate and water, combined to settle, for future reuse.

Hoping to freeze, filter off ice, proceed to salting w citrate (to determine whether any M remains in solution after washing) this weekend. Then do final neutralization, and re-use.


3/12: Syringe decanted (using 100ml glass, gasketless syringe) the haze-free portion of solvents out of testtubes into the previously cleared solvents, put them all in for 24 hr freeze. Will cold filter-decant off of ice tomorrow, and then proceed to re-salting with citrate.


3/13: Cold filtered the solvents, all had significant and roughly equal amounts of ice shards. Dropped one of the jars, no further “boiled” solvent, insert expletives here! After warming to ambient, all jars remained clear; added 0.9g citric acid to each jar and stirred a couple revs. They all clouded, but seem to be precipitating what looks like a slight amount of calcium citrate powder. Will settle until clear, decant, then neutralize.

Sediment and added water runs final, see here: https://www.dmt-nexus.me...mp;m=1136784#post1136784

Thanks Cheelin. So the goo issue remains a mistery.

One interesting thing I can update on is activated carbon (aka charcoal). The low dust product for aquariums worked great. It clears the EA from green color without the annoying difficult to filter black powder. However, it also made new water separate out (!). I think plant stuff helps mix the EA and water together, so there is more than the usual 3% water miscibility. Once that plant stuff was removed by the activated carbon the water in excess of 3% separated out. I think this is an interesting observation/effect I was not aware of.

For the record, I see no practical upside to removing the color at this time, reused solvent has worked fine after a simple sodium carb saturated water wash.

I don't know if this variable amount of added water could be the source of goo for some. Don't think so, but I thought it was an interesting observation. Maybe some cacti have more of this water/EA mixing compounds (?).

Chemichally drying before salting with Na2CO3 would control the water variability. I can't reccomend it because I saw no upside or downside to doing it. We need someone that gets goo to split the extract and chemichally dry a subset of it as a test.

Lol, this search for the elusive goo monster is almost a total waste of time!!! And, doesn’t fit in well with the laziness theme.

If it wasn’t for my hardheadedness and natural curiosity, i wouldn’t have lifted a finger to work on this.

The main benefit of this work, though, is to once again demonstrate how difficult it is to fuck up this exceptionally robust and simple tek…when purposefully following the instructions!

Hopefully future goo experts will provide a good clue about their method of production. BUT, first question for them is: did you follow the instructions, exactly as written on the wiki or by me?

I’m hoping I can resist getting drawn back into this again.

CHEELIN’S GREAT SUCCESS CIELO METHOD
Follow this exactly until you make your first batch of white needles; with a “flavor” that is moderately bitter, but not sour. At that point, you will be an expert.

Then, thank 69ron for the paste recipe, Loveall for the tek, and Shroombee and others who helped refine it. After that, modify the processing method to suit yourself.



Pre-Steps:
1. Start with Humility in Your Heart - Forget anything you think you know about extracting alkaloids from plant material, or from any chemistry experience you have ever had. You know nothing about this tek until you produce the proper product.

2. Focus Exclusively and Purposefully on the Task at Hand - the actual working time for a single run of this tek is approximately 1 hour, set aside a 3-hour block of uninterrupted time, because of pre-step 1.

3. Do Not Begin the Tek Until You Have:
A. Read the wiki and this post completely,
B. Printed out this post,
C. Asked for clarification regarding anything in this post that does not make sense to you.
D. Acquired all the materials and equipment specified in this post,
E. Calculated, re-calculated, and pre-measured the quantities of materials necessary for the complete run,
F. Organized and laid out all equipment required for the complete run and the printed copy of this post.


Equipment Needed: No Plastics if possible, certainly none that degrade upon contact with Ethyl Acetate
A. One timing device that can be easily observed, hands-free, while running the tek
B. One or two pens that can be used to mark off steps, make your scaled materials list & process steps, and to record significant observations
C. A piece of paper to write on
D. A roll of paper towels to protect working surfaces and clean/wipe
E. A scale with at least 100g capacity, that tares
F. One stainless steel spoon to help measure powders and mix materials
G. One long-handle, small scoop, stainless steel spoon for mixing the pulls
H. At least 1 250ml capacity glass or inert plastic graduated cylinder
G. One stainless steel, glass, or ceramic soup bowl for making paste
H. Two 1-qt mason jars, at least one set of lids
I. One smaller mason jar, about 2x the amount of solvent you will be pulling, plus set of lids
J. A stainless steel funnel, to hold your filter when combining/filtering solutions
K. A glass baking dish for evaporating jar wash
L. A pipette/burette or syringe w blunt tip needles (aka industrial syringe needles) for “small”volume solution use
[note: i like using 60mL luer lock syringes for solvent additions and 10mL luer lock syringes for solvent rinsing and water washes. I use plastic ones, cuz I’m clumsy; but the rubber plunger tip deforms after several exposures to the solvent, so if you choose to use syringes, have a couple extras in reserve.]
M. Paper coffee filters
N. Single-edge razor blade for scraping evaporated jar wash
O, Parchment paper & scissors for making envelopes to hold finished product
P. A 4-cup stainless steel french press


Ingredients Needed:
A. Cactus Powder that has been ground to a particle size and consistency of baking flour, with a moisture content no greater than 10%.
B. Food-Grade Hydrated Calcium Hydroxide, also called Pickling Lime (I use Mrs. Wages brand)
C. Distilled Water
D. Food-Grade Citric Acid (I use Milliard brand)
F. Ethyl Acetate, pick the grade that is accessible and comfortable for you (I use KleenStrip or Jasco brands)


Create a Process Tracking Sheet: (OR, just use the below on the post you printed out)
On a sheet of paper, list the following items vertically:

Date:

Pickling Lime
Distilled Water
Cactus Powder

Mix Paste - 8 minutes
Rest Paste - 10 minutes

Each pull: 1 minute stirring 70-90 revolutions, then 2-minute rest, then filter into collection jar.

Ethyl Acetate Pull Volumes:
1st pull
2nd pull
3rd pull
4th pull
5th pull
6th pull

Rest pulls at least 1-hour, do what’s necessary to settle cloudiness and remove visible sediment and water

Citric Acid


Ingredient Amounts:
Here are the standard amounts for a 100g cactus powder run:
Cactus Powder - 100g
Pickling Lime - 25g
Distilled Water - 300mL
Ethyl Acetate - 946mL
Citric Acid - 5g (I realize this is different from the wiki)

To minimize losses and regret, and to improve your chances of early success, use 15 or 20g of cactus powder until you successfully produce the proper product.

To calculate the scaled amounts needed:
1.Choose the amount of cactus powder you will use
2. Divide this amount by 100 to get your scaling factor
3. Multiply each of the material amounts listed above by the scaling factor, to get the amounts you need for your chosen size cactus powder run. Write each amount down on your process sheet.
4. The scaled volume of ethyl acetate needs to be subdivided into pull volumes.
a. Multiply the scaled amount by 25%, this is the volume of the first pull, write it on the process sheet.
b. Subtract the 1st pull volume from the total scaled volume, divide the result by 5. This is the volume of each pull, 2 through 6, write it on the process sheet.


Pastemaking:
1. Put distilled water and pickling lime in mixing bowl and stir until a consistently milky solution is made.
2. Dump in cactus powder, stir until all the milky solution is absorbed by the powder.
3. Start 8-minute timer
4. Stir paste, fold in half, mash all areas, fold in half, mash all areas, repeat non-stop for the full 8 minutes.
Paste should be a consistent color & texture, texture ranging from mashed potatoes-like to cookie-/play-dough-like.
5. Transfer paste into french press, cover, reset timer, rest for 10 minutes


Solvent Pulls:
1. Remove french press lid and plunger-strainer.
2. Chop up paste into roughly 1/2 - 3/4” chunks.
3. Dump in solvent dose for 1st pull
4. Cross off 1st pull on process sheet
5. Start 3-minute timer
6. Stir 70-90 revolutions for 1-minutes
7. Let paste rest for 2 minutes
8. Put plunger-strainer into press, pour solution (won’t be much for 1st pull) through strainer through coffee filter-funnel setup into pull collection jar. Don’t squeeze paste; just let pulled solvent drip out til driprate is less than 1 drip per second, tilt press to upright, let drip again til less than 1 drip/ second.
9. Repeat steps 3 through 8, until 6th pull is completed.
The paste during the last stir should look like applesauce, if earlier that’s even better. The pulled volume should be emerald green, and about 90% of the amount added.
10. Remove filter funnel and put lid on collection jar, let rest 1 hour. The solution should be clear.
11. At the end of settling period, the solution should be crystal clear, with no apparent sediment or water droplets/layer. Settle longer if necessary, filter/decant to separate crystal clear solution from sll else.
12. Do not proceed to salting until the solution is crystal clear, free of sediment and water; else you end up contaminating or reducing the yield of your product.


Salting & Crystallization:
1. Pour your crystal clear solution through a filter-funnel setup into a smaller jar, roughly 2x the pulled solvent volume.
2. Dose with citric acid.
3. Stir a couple times, solution should become cloudy.
4. Cover jar, put in undisturbed location, let crystallize for 48 to 72 hrs.


Filtering & Rinsing:
1. Gently swirl crystallization jar, remove lid, pour 3/4s of solution through filter-funnel setup into used solvent jar.
2. Gently swirl remaining solution, dump all of solution into filter-funnel.
3. Take 5-10mL of Fresh EA, tilt empty crystallization jar, rinse interior walls & bottom of jar, swirl, dump into filter, repeat once. Set jar aside to dry.
4. With more Fresh EA, rinse filtrate with as little as needed until filtrate stops changing color.
5. Let filtrate drain, then remove filter from funnel, place filter on paper towel to dry.
6. When filter no longer appears wet, gently fold up product in filter, set aside to completely dry for several hours.
7. Remove dried product from filter, weigh for yield calculation, store.


Jar Washing & Residue Recovery:
1. When crystallization jar is completely dry, rinse & swirl twice with 5-10mL hot distilled water (contacting all interior surfaces), and dump into a clean baking dish.
2. Let water evaporate w/wo fan, scrape residue with razorblade, weigh for yield calculation, combine with filtered product.


Attached are pics from a 15g cactus powder run, 72hr filter yield 0.222g, evaporate yield 0,006g,Total Yield 0.228g, 1.5%.

2nd goo creation experiment (*/- Lime and +/- Citrate) updated here: https://www.dmt-nexus.me...mp;m=1136901#post1136901


Cielo process pics added to the post above this one.

Ooof, so, I think I've figured out my mistake... I feel really, really dumb for this. Forgot to put the solvent through a coffee filter...twice. My brain isn't as sharp as it used to be.

The solution from my failed attempts appeared clear to my eye (when backlit, more on that later) at the time I started the salting process both times. No water separated after leaving it out overnight, so I thought it was good to go. Droplets appeared fairly quickly after adding citric acid and leaving it to sit (without any stirring, per the instructions in the wiki)

Poor filtration was almost certainly the cause of my goo problem, I think. I did a third run with the proper method yesterday, salted this morning (still using the addition w/o stirring) and it looks like I might be on the way to a success. There's a film of tiny iridescent material forming on the bottom of the jar.

I have a container with a run I did today that I am planning to salt with the addition method cheelin described. I defintely haven't noticed the crystals forming to such a degree as quickly with the no-stir method, but perhaps the material I'm working with is low-yielding to begin with.

But I do want to go back to the cloudiness part. Both the filtered and unfiltered solutions appeared clear when backlit. When shining a light through the solution, the column of light was visible. Unfortunately I wrongly attributed the visibility of the column of light to the fact the the LED flashlight I've been using makes the chlorophyll fluoresce. Lessons learned, for sure. I don't know if anyone would be likely to make the same mistake as me, but it might be worth recommending a flashlight that doesn't make the chlorophyll fluoresce strongly...

Glad you figured it out.

I always give my jar a quick stir after adding the citric acid, clouds up immediately. The run above, it had lots of crystals within a couple of hours but was cloudy for a few more. By six hours it had cleared and will slowly make more & bigger crystals for a couple more days.

I think Loveall likes to just drop the acid in without stirring, starts out a little slower, but eventually gets the job done. So, you’ll probably see your second run crystallize well.

orchidist, Did the filter catch any visible crud?

I think Cheelin's quick stir is better. I tested it and Xtals are the same size and the longer fully passive method. Gonna update the TEK.

If stirring is continued after clouds form the Xtals do get smaller but form faster as we have mentioned before. It's a cosmetic thing I believe. I prefer the larger ones cause they are so pretty. However, the smaller Xatals are easier to out in capsules as the smaller xtal powder flows better and is more dense.

Cheelin, you definitely win the award for most likely to achieve Great Success with anything you put your mind to.

Thank you so much for your enthusiasm, willingness to experiment, and report on your results to the Nexus community. This TEK is 10x better because of your work.

I think this is true for cactus with ~1.3% yield. For higher yielding cactus, more citric would be necessary to convert free base mescaline to a salt

Record that I'm aware of is Ogun at 5% mescaline HCl. That's 8% mescaline citrate. In terms of citric acid that is ~3.8%. The currently reccomend 2.5% in the TEK would not be enough for such a monster cactus. EA would remain alkaline after salting.

Agreed. Thank you Cheelin 🌵

Thanks!

I’ll gladly accept the eager beaver award. But, my work here would not be possible without 69ron, Loveall, you, and the other guys who proofed the tek last year. My strength is taking something great and making it simpler, easier, more accessible; and this is the greatest fucking M tek ever created!!! So, it has been my pleasure & honor being part of it.

I hope i can get a reliable 1g version to work. But what would be the absolute cherry on top of this great tek would be for someone to take the baton and create a titrimetric yield assay method using this technology. I have more chemistry background than a lot of chem majors, but in the end, I’m just a tech not a creator/designer, with degrees in other fields. Lol

Too bad Shulgin isn’t around to see this.

This process has been declared required reading in the TEK's introduction section.

The filter didn't catch anything visible besides a few specks that I would've decanted without filtration, but it definitely seems to have done something important. It seems the water (and whatever else) in suspension was extremely fine. It's unfortunate that I initially mistook it for fluorescence, but it is pretty clear (no pun intended) now that the coffee filter removed it. I'm thinking electrostatic effects hold back the water even if the particle size is smaller than the filter pores (same way masks are able to filter particles much smaller than their mesh size).

The instant gratification of the fast method is tempting...but pretty crystals win for sure! Have no idea when I'm going to have the time to test them anyway, so might as well take the long route

Thanks Cheelin, for the all of this amazing work, it's truly impressive!

👍🏻

My goal: No Excuses!

Lol

Coffee aficionados claim that paper filters are better than metal filters because the paper traps cafestol (https://en.m.wikipedia.org/wiki/Cafestol ), wheras wire filters don’t. So, you are probably onto something there.

I prefer the passive method for the crystal beauty, and also as a visible measure of purity. Lots of things precipitate as white powder that aren’t M (just evap some tap water). This becomes important in trying to estimate purity/potency/dosage when we work with reused solvent.

That is very interesting. We recently switched my coffee filter, might rethink that now.

Once I get this tek down I'll be happy to participate in the reused solvent tests. I recently picked up a TLC kit to test some other stuff. Would certainly be useful here too.

Ok, now I wanna salt a fraction of my next extract without filtering it (decanting only), see what happens...

If I were a cat, curiosity would have killed all my lives 🙃