TEK Ethyl acetate approach [CIELO]

[Loveall]

Conclusion is very is simple: Multiple data are consistent with the monomescaline citrate forming in the CIELO Tek because of excess citric acid.

Backtracking a bit here but my view on this is that as soon as the molecules of citric acid have ionised and protonated the nearest available mescaline molecule, the electrostatic forces are sufficient that the two ions precipitate from the EA as they have become too polar to remain in solution. The lattice energy of crystallisation exceeds the solvation energy of the EA for the respective ions. The upshot is that there simply isn't time (or energy) for the dibasic or tribasic salts to form. It may be possible to form these higher salts by using mesc freebase dissolved in water.

I find it elegant how a trace of water aids this proton transfer that leads to crystallisation, but too much will spoil the formation of crystals.

Thanks DWZ. I can't say I know what is going on exactly, but when I added citric acid in a 1:3 molar ratio for citric:mescaline (based on expected yield from previous runs), an oily precipitate very slowly formed over a few days. This oil was isolated and converted to the usual needless and gained some mass.

My guess is that the monomescaline citrate does form first as clouds. If there is still excess mescaline eventually it reacts with the monomescaline citrate to form a different salt. The reaction is slow, possibly because the first salt is mostly out of solution.

Or something else could have happened, IDK.

At the end of the day, adding excess citric is the way to go experimentally from what I can see. It reliability forms what seems to monomescaline citrate which readily xtalizes even in gunky dark solvent that has been reused twice (3 times total) and is loaded with chlorophyll and almost opaque.

 

[Cheelin]

Another day or two and I will choose the solvent washing method (for the time being), so I can move on to testing the various reused solvent samples I have.

One of the primary concerns throughout the development of this tek has been what I refer to as “hue”, the color and its intensity, of the reused solvent. I doubt hue matters much (except, to the extent that hue is an indicator of microscopic non-M plant material that will eventually precipitate), but this is one of the primary things i will test.

I think solvent clarity and water content, are much more important,

Sodium carbonate washing, plus gravity, time, and basic filtering can deal with citric acid neutralization and clarity issues.

At a minimum, removing the water layer that develops when using a sodium carbonate wash is required. Storing the used solvent in a freezer for 24 hours is an effective method for easily decanting from the (frozen) water layer and appears to also entrap green material to some extent, using a seperatory funnel or syringing/pipetting the water layer also work well.

Furthermore, freezing shows that there are also significant amounts of water that do not end up in the water layer, but rather, remain in the solvent layer, becoming floating ice crystals when frozen. It is tricky removing all of this ice, since it melts faster (outside of the freezer) than the solvent can drain through a coffee filter. But, using a stainless steel sieve can remove most of the ice fairly rapidly. Besides removing this additional water from the used solvent, the solvent becomes a noticeably lighter hue.

So, if future testing shows that reused solvent hue adversely impacts solvent life or effectiveness, freezing, exposure to light, activated carbon, and perhaps some of the earlier treatment options, will help in this regard.

 

[Loveall]

Another day or two and I will choose the solvent washing method (for the time being), so I can move on to testing the various reused solvent samples I have.

One of the primary concerns throughout the development of this tek has been what I refer to as “hue”, the color and its intensity, of the reused solvent. I doubt hue matters much (except, to the extent that hue is an indicator of microscopic non-M plant material that will eventually precipitate), but this is one of the primary things i will test.

I think solvent clarity and water content, are much more important,

Sodium carbonate washing, plus gravity, time, and basic filtering can deal with citric acid neutralization and clarity issues.

At a minimum, removing the water layer that develops when using a sodium carbonate wash is required. Storing the used solvent in a freezer for 24 hours is an effective method for easily decanting from the (frozen) water layer and appears to also entrap green material to some extent, using a seperatory funnel or syringing/pipetting the water layer also work well.

Furthermore, freezing shows that there are also significant amounts of water that do not end up in the water layer, but rather, remain in the solvent layer, becoming floating ice crystals when frozen. It is tricky removing all of this ice, since it melts faster (outside of the freezer) than the solvent can drain through a coffee filter. But, using a stainless steel sieve can remove most of the ice fairly rapidly. Besides removing this additional water from the used solvent, the solvent becomes a noticeably lighter hue.

So, if future testing shows that reused solvent hue adversely impacts solvent life or effectiveness, freezing, exposure to light, activated carbon, and perhaps some of the earlier treatment options, will help in this regard.

Great summary. I would also say that adding sodium carbonate to the solvent after removing the neutralization water layer chemichally dries the solvent as the sodium carb absorbs water.

I believe most comertial washing soda comes a stable monohydrate form at room temp conditions and the decahydrate forms in the presence of water. Since wet EA is ~3% water, 50g of washing soda should chemichally dry a quart of EA. We could confirm with a freezer test after a chemical dry.

 

[Cheelin]

I’ve been filling a quart jar with about 700ml of used solvent, and 140 ml wash solution (approx 50g sodium carbonate, 90 mL distilled water).

Note that pics have been added to my previous post.


Technical Note: My (corrected) understanding is that EA can hold up to 3% water; and water can hold up io 8-9% EA.

 

[highlightprotein]

Oh no, my Klean Strip MEK Substitute is leaving a residue upon evaporation!

Loveall, I think you are using Klean Strip MEK Substitute. Does it even make sense that I would see a residue, while you do not? I would think that it was standardized.

Is it somehow possible I messed up the evaporation test? I did it twice. The first time I used a very small amount of EA and noticed that left over liquid that didn't evaporate. I put a fan to it for an hour or so and saw the residue.

I then cleaned the dish with water and IPA and dried with a paper towel, thinking that perhaps the residue was due to something else in the dish that was not cleaned. I repeated the test, but poured out a larger amount, enough to fill a small layer in a dish. The majority of the liquid evaporated away quickly with no residue, but left behind was small amount of liquid. A few hours later, this liquid still remained- obviously this is not EA because EA evaporates quickly. I looked closely at the liquid and saw some specs or flakes of some solid floating in the liquid. This morning, after 10+ hours, the liquid has evaporated but there is some kind of oily residue, and those specs/flakes can be seen.

I've eaten about 300mg of mescaline produced with this EA... gross. I guess I have to throw away my 1.8g of beautiful white needle/rock I just made. Originally I was using laboratory EA but switched to Klean Strip due to cost.

 

[Loveall]

I use Klean strip with no issues.

Did the residue have any smell? Sounds like it could be water condensation from the quick EA evap causing cooling. The particles could be concentrated dust from the air.

I would not throw the needles away, they are probably OK. Wash them with acetone if you have any worries.

 

[Loveall]

Technical Note: My understanding is that EA can hold up to 8-9% water; and water can hold up io 3% EA.

I think it is the other way around: The water layer holds 7.1% EA, and the EA layer holds 3.4% water. As ions are added to the system separation is improved: EA moves out of the water layer, and water moves from the EA layer. With NaCl used as a saturated ion source, the EA in the water layer drops down to 0.71% (10x less!) and the water in the EA layer goes down to 1.86% (nearly cut in half). See screenshot below. I can't find the data for Na2CO3 but I imagine that to first order the improved separation would be similar to NaCl.

 

[Cheelin]

I have 3 sources of EA evaporating, atm, all supposedly > than 99% pure: KleenStrip, Jasco, Lab Chemical Supplier. I’ll see if/what residue remains after evaporating in my kitchen.

It is important to realize that EA is a pretty strong organic solvent. It will degrade/decompose paints, plastics, lots of stuff it touches, including grease, detergents, biofilms, alcohol residues, etc. So, before going nuclear with fear, it is important to identify the source of any possible residue considered of significant level or composition. Just because a residue is in a dish does not mean the manufacturer shipped contaminated product. But as in all things, if you believe the material you are using is unacceptably contaminated, don’t use it. Find an alternative source or don’t use the tek. There is absolutely no grade of any organic solvent that is absolutely 100% “pure” before the container is opened, let alone afterwards.

If you are concerned enough to toss your product, consider Loveall’s suggestion to have a micro amount analyzed, he can tell you how he did it.

 

[Cheelin]

Technical Note: My understanding is that EA can hold up to 8-9% water; and water can hold up io 3% EA.

I think it is the other way around: The water layer holds 7.1% EA, and the EA layer holds 3.4% water. As ions are added to the system separation is improved: EA moves out of the water layer, and water moves from the EA layer. With NaCl used as a saturated ion source, the EA in the water layer drops down to 0.71% (10x less!) and the water in the EA layer goes down to 1.86% (nearly cut in half). See screenshot below. I can't find the data for Na2CO3 but I imagine that to first order the improved separation would be similar to NaCl.

Thank you for correcting me. I misread this: Ethyl Acetate Solvent Properties

 

[highlightprotein]

Did the residue have any smell? Sounds like it could be water condensation from the quick EA evap causing cooling. The particles could be concentrated dust from the air.

No, it had no smell.

I have 3 sources of EA evaporating, atm, all supposedly > than 99% pure: KleenStrip, Jasco, Lab Chemical Supplier. I’ll see if/what residue remains after evaporating in my kitchen.

Thank you.

 

[ijahdan]

Well, after filtering and evaporating, I got a low yield of (presumed) mescaline citrate. 100mg of tan coloured, sticky powder from the first salting attempt, to which 5g of citric acid had been added to the solution and left for 72 hours, and 250 mg of dry white powder from the same solution to which an extra 10g citric acid had been added, stirred vigourously and left to stand for another 72 hours. Both types of powder are bitter, not sour.

NB I started with 100g san pedro inner flesh, dried and finely powdered. Ive had better yields from the same batch in the past, (eg 500mg mescaline hcl from 100g powder using 69ron's tek with limonene), as well as very strong experiences from ingesting around 50g of the whole powder. However, the powder is now about 6 years old, so may have degraded.

As to the oily residue from my ethyl acetate, it is colourless, odourless and tasteless. Still rather it wasnt there at all though!

6 pulls were done, using a total of 1 litre ethyl acetate.

Im thinking, maybe my low potency powder gave too dilute a solution, which then made it harder to crash out the salt (?)

 

[Cheelin]

I’ll leave the detective work to others.

But my feeling about getting up the learning curve is “practice makes perfect”, with the corollary, start with 15 to 45g of powder (ingredients reduced proportionately, times kept constant). The process involves focused effort to make good paste and do good quick pulls, these are the places where yield is most likely lost. Quality, imo, is lost during the salting through collection steps.

If possible, a few more runs, with end product that is white, will give you a good feel for what’s available in the cactus, using this tek.

If you haven’t already seen them, and are interested, I have a couple posts in this thread which detail my process.

 

[Loveall]

Well, after filtering and evaporating, I got a low yield of (presumed) mescaline citrate. 100mg of tan coloured, sticky powder from the first salting attempt, to which 5g of citric acid had been added to the solution and left for 72 hours, and 250 mg of dry white powder from the same solution to which an extra 10g citric acid had been added, stirred vigourously and left to stand for another 72 hours. Both types of powder are bitter, not sour.

NB I started with 100g san pedro inner flesh, dried and finely powdered. Ive had better yields from the same batch in the past, (eg 500mg mescaline hcl from 100g powder using 69ron's tek with limonene), as well as very strong experiences from ingesting around 50g of the whole powder. However, the powder is now about 6 years old, so may have degraded.

As to the oily residue from my ethyl acetate, it is colourless, odourless and tasteless. Still rather it wasnt there at all though!

6 pulls were done, using a total of 1 litre ethyl acetate.

Im thinking, maybe my low potency powder gave too dilute a solution, which then made it harder to crash out the salt (?)

Thanks for the data. I don't believe mescaline degrades. Lower yields on this new TEK should be something to watch out for.

On my part I've seen matched to slightly better yield vs the 69ron process with less work to get to the clean product.

I wonder where the rest of the product is. If you still have the spent paste you could try to dry it to remove EA, rehyrate it and do the limonene process.

If you still have the used EA, you can add 10 more grams of citric acid to it to see if anymore product crashes. It shouldn't in my experience, but the high amount of citric you needed is odd also.

 

[Cheelin]

HLP,

All three glass bowls dried with no visible residue or film inside them. I will attach a pic of the bowls, but the gyrations I have to go through to upload pics from my phone, and this app itself, make details hard to see. Left to right: Lab-grade, Jasco, KleenStrip. The background is actually black, no flash was used.

My conclusion based on this test, is that if you have contaminated solvent, it is from that specific container or from contamination subsequent to pouring the solvent out of the container.

You might re-run the evap test of your fresh KS solvent, just to confirm your previous results. If you have 2 or 3 clear glass containers, i’d run 2-3 at same time.

 

[Cheelin]

HLP, thinking about the ‘unusual’ crystals you found in the product.

You used Reused solvent in your pulls, correct?

If so, how did you treat your solvent before using it this run?

If you washed it somehow, how would you describe the clarity when shining a flashlight through the solvent, after it was washed and ready for re-use? Set aside the color: could you make out the details of the flashlight through the glass and solvent, could you see the light relatively clearly but not the details of the flashlight, could you see a haze/cloudiness/sediment?

You might do an evap test on your reused solvent, too.

 

[Cheelin]

Got a new batch of powder, from same vendor, labeled same as previous batch, Equador, T. pachanoi. Ran a 45g test batch, using standard process, fresh EA, Loveall’s suggestion to do 6 pulls in one jar and 3 additional pulls in a 2nd jar, 5g equivalent of citric acid, and passive crystallization.

Did a 1st filter of both jars after 48hrs, then final filter at 72hrs, let jars dry, then water washed jars & evaporated.

So pleasantly surprised on the yield,

Pulls 1-6 gave 0.744g (~1.7%), pulls 7-9 gave 0.054g (~0.1%), 0.798g (~1.8%) total. Moderately bitter, no acid.

Nice when a vendor surprises on the upside!

 

[Loveall]

Got a new batch of powder, from same vendor, labeled same as previous batch, Equador, T. pachanoi. Ran a 45g test batch, using standard process, fresh EA, Loveall’s suggestion to do 6 pulls in one jar and 3 additional pulls in a 2nd jar, 5g equivalent of citric acid, and passive crystallization.

Did a 1st filter of both jars after 48hrs, will do a final filter at 72, let jars dry, then water wash jars & evap

So pleasantly surprised on the yield, I couldn’t wait until Mon/Tues when the complete yield will be tallied.

Pulls 1-6 gave 0.717g (~1.6%), pulls 7-9 gave 0.045g (~0.1%), prob end up 1.8+%. Moderately bitter, no acid.

Nice when a vendor surprises on the upside!

+0.1% on top of 1.6% (~6% yield boost) roughly matches my result for the second set of pulls. This tells me that the first set of pulls is efficient at pulling mescaline. A poor solvent would give more yield on the later pulls.

 

[Cheelin]

Thought you’ld like that part.

 

[Cheelin]

Aways back I started a post about testing reused solvent. I discovered that the washing method, imo, needed a little more specification, so because it took some time to work out the method i’ll use, for now at least, I moved the post up to be a little more convenient.

Here is how I do the Sodium Carbonate washing:
1. Fill a jar 2/3 - 3/4 full with used solvent. The headspace is needed to accommodate the volume of the wash solution, as well as, for potential expansion of frozen water-precipitate puck.

2. Determine the volume of used solvent. I do this by filling the same type jar that the used solvent is in with tap water, to the same level as the surface of the used solvent; then I pour the water into a graduated cylinder/measuring cup to determine the volume. [I don’t directly measure the volume of the used solvent, because it dissolves the inked markings on my cylinders.]

3. Do the the following calculations, based on the instructions in the wiki:
a. Total volume (mL) needed of sodium carbonate solution = volume of used solvent x 0.20
b. Amounts of sodium carbonate solution ingredients:
i. Grams of sodium carbonate needed = Total volune of sodium carbonate solution needed x 0.35
Ii. Put grams of sodium carbonate needed in mixing jar, add distilled water to equal total volume of sodium carbonate-water solution needed.

4. Mix sodium carbonate and distilled water for 1 minute. Solution will become noticeably warm, sodium carbonate will not fully dissolve.

5. Pour sodium carbonate solution into used solvent, stir well for 1 minute; cover jar but do not screw on lid, as there may be off-gassing of evolving carbon dioxide. Three layers will form: bottom, water layer; middle, sodium carbonate-water layer; top, solvent layer. Initially the solvent will be clear and 2 to 4pH. Over a 20-minute period, mix the solution 3-4 times, 1 min each, to breakup & redistribute the sodium carbonate. The resulting solvent layer should become cloudy and pH will move closer to 5 (pH of fresh EA is solid 5ish). Screw on jar lid, and let solution clear as best possible, for approximately 1 week..

6. After most of the cloudiness has dissipated, place jar in freezer for 24 hours.

7. After freezing solvent for 24 hours, decant solvent through a stainless steel sieve into a coffee filter to remove any floating ice crystals and other residues. As soon as all the floating ice has been collected in the sieve, remove it from above the coffee filter so that you minimize the opportunity for melted ice to reintroduce water back into the solvent. After the solvent is filtered, put lid on collection jar, and store at room temperature until the cloudiness settles and solvent becomes clear. A haze is likely to be present even after the solvent is no longer cloudy. When you shine a flashlight through the solvent, if it looks clear but you can’t make out the details of the flashlight, you still have a haze of particles that will eventually settle out. I want my solvent to be as clear as possible, because I don’t want this crap ending up in my product, so I’m willing to wait however long it takes to fully clear, which could be a week or more. Once at a satisfactory level of clarity, decant the clear solvent off of the settled particles, and store for future use. You may collect the remaining cloudy solvent/sludge in a smaller container, letting it settle until the solvent clears and then decant/syphon that off, to increase the amount of solvent recovery.

For those with Buchner funnels, I have some Whatman qualitative filters ordered, #5 and 602H, to see how well they do at reducing the haze. This doesn’t work, cloudiness/haze particles too small.

Did a new sodium carbonate wash (steps 1- 5 above) on 3 jars of used standard run solvent, and 4 used “yellow” solvents (from boiled water std paste, microwaved paste, chilled paste, microwaved & chilled paste runs). See Yellow Solvent pic below. 2 of the 3 used standard solvent jars were then treated as described here: Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus These treatments will then be used in a second attempt/version of part I below. The other 5 jars will be treated with the “best” washing method from this trial, then used in part II below.

See pics below “2nd Approach 72 Hrs After Washing” and “2nd Approach 72Hrs Bottom”; showing the washed solvent at the 72 hr mark, very difficult to get a good pic, but the separation between the top 2 layers of the solvent is evident (about 5” in total; 40% clear upper, 60% cloudy lower). There are two water layers at the bottom of the jars (about 1” combined); the lowest layer is a heavily saturated with suspended sodium carbonate crystals, the layer above it looks like pure water. The boundary between the top water layer and the bottom solvent layer has a very thin layer of colored particulate.




I. Experiment comparing fresh solvent, washed & chilled used solvent (@2 citrate levels from previous use: equivalent of 5 and 15% of material wt), and unwashed used solvent (@2 citrate levels from previous use: 5 and 15% of material wt); using individually prepared 15g runs of standard paste; 6 pulls, 1st one 35mL, 2-6 25mL; 0.75g citric, passive crystallization.

Attached are views of the solvents and their pH strips. All the solvents were crystal clear, the unwashed solvents had visibly darker hue than the washed solvents.

The unwashed pulls are nearly worthless. The 15% citric unwashed pulls were heavily sedimented in each pull, hardly draining through the filter by the end of pulling; the 5% citric unwashed pull was also heavily sedimented, but fully drained through the filter. Additionally, both unwashed solvent pulls became sticky, snot-like, and unstiirable, the 15% citric starting with the 4th pull, the 5% citric with its 6th pull. Both runs. even after multiple filterings and several days of settling, remained so cloudy that light beams from a high intensity flashlight were not visible through the cloudiness. I tried to rehab these with ultrafiltration, with no improvement at 2 mucron pore size. Washes were salted despite cloudiness, 15g equivalent produced a pure white mixture of mescaline citrate needles and what is brlieved to be calcium citrate. Total yield was 2.9%, at least 1/3 if this is suspected to be calcium citrate. The 5g citrate equiv run produced 2.5% yield, about 1/4 of this suspected to be calcium citrate. Use of unwashed solvent is not recommended. Wash & clear your used solvent before running it again.

The fresh solvent and both the washed 5% and 15% solvents ran normally. The final yields were 0.215g (1.4%), 0.296g (2.0%), and 0.379g (2.5%) for fresh, washed 5g, and washed 15g solvent runs, respectively - the exact opposite order of what I expected! The products look the same, 100% needles; and taste the same; and are not mislabeled. Doing jar wash-evap; might be a few more crystals each, but i don’t expect any dramatic changes. Maybe i messed up somehow, but I doubt it. A headscratcher,

Ran another version of this experiment, with the second washing method described in bold above, see Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus



II. Experiment comparing multiple re-uses of solvent from the various treatments that were previously listed as options on the wiki. We know that those treatments reduced yield when using fresh solvent, now I want to see how product quantity & quality, as well as useful solvent life, compare with repeated solvent re-use, using the same treatments: standard paste, boiled water paste, microwaved paste, chilled paste and solvent, microwaved paste with chilled paste and solvent.

The details of this experiment can be found here: Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus

 

[Cheelin]

Had a few minutes, did another crap recovery run using 5g of cactus powder (that has previously shown 1.1% M yield) and 0,9g of previously recovered product from part I. In post 702; standard paste, but with a 5 min stir, 6min rest; 6 pulls with 20ml fresh EA per pull; 5g equivalent citric passive crystallization.

Did less manipulation of the paste in hopes of improving the consistency from silly putty-like to something more normal, and have it be less snot-like when pulling. Also wanted to see if/what amount of relatively pure product would be lost in the recovery process.

0.547g total at 48 hrs, incremental 0.096g at 72 hrs, incremental 0.005g at 168 hrs, for grand total yield of 0.648g. After deducting, 0.055g (1.1% that this powder yields), 0.593g, or 65.9% (.593/.9) recovery.

Added 0.4g citric, on Loveall’s advice at ~48 hrs after initial salting, to ensure sufficient acidity.

Later: measured pH prior to re-salting, no different than normal post-salting pH; re-salted, no additional crystals formed, Final, minimal yield increase was what remained stuck to jar walls from initial salting/crystallization.