TEK Ethyl acetate approach [CIELO]

[Cheelin]

Started reused solvent test, part I., see above.

 

[Loveall]

Started reused solvent test, part I., see above.

Looking good. Thanks for your efforts.

One question I have is regarding the ice xtals. After they melt, do they separate in layers? Is the EA layer significant? I wonder if there is a lot of EA in them or just a little around them.

 

[Cheelin]

Good question, especially wrt to conserving used solvent. I’ll check that in future runs.

 

[Cheelin]

Nice results coming in on latest recovery run, see above.

 

[Cheelin]

Although not that useful for M production itself, small runs are useful for recovering crappy product, and for assaying M % yield in plants and experimental treatments. The following test is to see how sensitive 5g samples are to changes in the pastemaking variables.

Did 9 individual runs using 5g of cactus powder processed as follows:

1. Standard Paste (Std): 5g cactus powder, 1.25g pickling lime, 15mL distilled water; mixed 8 minutes, rested 10 minutes. Yield: 0.053g, 1.1%.
2. Minus 50% Lime (-L): same as Standard Paste except that pickling lime is 0.63g. Yield: 0.051g, 1.0%.
3. Plus 50% Lime (+L): same as Standard Paste, except that pickling lime is 1.85g. Yield: 0.058g, 1.2%.
4. Minus 33% Water (-W): same as Standard Paste, except that water is 10mL. Yield: 0.055g, 1.1%.
5. Plus 33% Water (+W): same as Standard Paste, except that water is 20mL. Yield: 0.054g, 1.1%.
6. Minus 50% Mixing (-M): same as Standard Paste, except that mixing is 4 minutes. Yield: 0.057g, 1.1%.
7. Plus 50% Mixing (+M): same as Standard Paste, except that mixing is 12 minutes. Yield: 0.055g, 1.1%.
8. Minus 50% Resting (-R): same as Standard Paste, except that resting is 5 minutes. Yield: 0.052g, 1.0%.
9. Plus 50% Resting (+R): same as Standard Paste, except that resting is 15 minutes. Yield: 0.050g, 1.0%.

All runs pulled 6 times (in a 1-cup stainless steel french press), with 1 minute of stirring & 2 minutes of resting per pull; 1st pull 25mL fresh EA, pulls 2-6 15mL fresh EA; 0.3g citric acid salting; passive crystallization.

The only paste that was unusual during solvent pulling was L1: its 1st pull was gummy, all if its subsequent pulls were snotlike.

Amazingly consistent product quality and yield over a huge range of each pastemaking variable.

Looks like there may be further opportunities to minimize pastemaking variables without reducing yield. Improvements in paste quality and yield may be possible by increasing pickling lime.

[pH pic note: “1” = -, “2” = +; eg L1 =—L above]

 

[Loveall]

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, after deducting, 0.055g (1.1% that this powder yields), 0.492g or 54.7% recovery, so far. Will do final filtering at 72hrs, then water wash jar & evap.

Wiki's FAQ section updated with this info

 

[Cheelin]

I’ll update with final numbers, after the wash evaps, in a few days.

I was very happy to see that this method, using only 5g of new powder, recovered almost 3 times more when I used “pure” product. So, we know, for sure, that this method has the potential to recover more than half of the M content of rehab’d material.

I’m hoping we can optimize it to recover more. At at an overall level, it would be nice to demonstrate that Cielo can recover whatever M content the input material contains.

I think, judging on how the paste looks in the press, that there is definitely some more potential. I’m hoping the current 5g paste test, provides a lead.

 

[Loveall]

Cheelin,

A couple questions:

1: Do you know what % of mescaline is in your goo, that is, is there an expected recovery target?
2: When you say 5g equivalent of citric acid, what do you mean? Is it 5/20 = 250mg, or is it 5/20 + r * 192/(211+192), where r is the grams of mescaline citrate you expect to have in the goo? Note that if you only added 250mg of citric, the max product you can get is 250mg * (211+192)/192 ~ 530mg. Any more product than that and more citric is needed to neutralize and precipate the FB.

 

[Cheelin]

The most recent recovery run used “pure” needles that were recovered earlier, so no goo. The previous goo recovery runs used input goo from multiple runs that used “equivalent” levels of 5g and 15g. But, the goo from these runs were mixed before recovery, so trying to quantify the citrate levels is hopelessly confounded.

When I use “equivalent”, i am referring to the proportional reduction in citric acid based on amount of cactus powder as a percentage of the quantity in the tek.

So, for 100g powder, the tek said at one point to use 5g citric acid (yes, I realize the citrate quantity was based on a solvent quantity & solubility calc, but I took laziness approach); so for 5g of cactus powder, I used (5g powder used/100g powder in tek) x 5g citric = 0.25g citric acid, which I actually bumped to 0.3g for convenience.

Working with these small quantities, while trying to keep things accessible to kitchen chemists, has its issues. After I get the paste nailed (the std paste with the addition of crap or needles is too sillyputty-like), I’ll focus on tuning up the solvent volume used in the pulls, and see if various citric levels make a difference.

At these small powder quantities it seems that the addition of as little as 1g of crap or needles has a big effect on the paste texture, affecting how well the solvent can extract the goodness. Additionally, french press size and proportional reduction of the solvent volume, (from what is specified in the tek) is not really practical for 5g runs.

For the paste, I think lime amount needs to be optimized, maybe water. Perhaps powder quantity (as a substrate) limits potential.

I think the 1-cup french press I bought, solves the equipment issue.

I’ve arbitrarily (for now) increased EA volumes in the pulls, so the combined amount will be large enough to work with in half-pint jars. I haven’t yet taken the time to adjust the citrate addition for this, using the logic in the tek.

So, various opportunities to further tune this up.

 

[Loveall]

Ah, gotcha, so the 0.9g added where needles. Interesting.

To re-crash 0.9g you need ~430mg of citric, and you are below that. I think you need to increase the scaled citric acid by the amount needed to take care of the added needles:

250mg (scaled TEK)+ 430mg (added needles) ~ 680mg (total needed)

Since you added 300mg of citric I would check the pH if not done so already. It may not be acidic yet. Then I would add ~380mg more of citric acid and see if it clouds up and more needles form.

 

[Cheelin]

I will do this next time. Can’t remember if i measured pH on the recent recovery run, will also do that on next recovery run.

Thanks for your help!

Btw, I did measure before & after salting pH levels on the 9-run 5g powder runs (no goo/crap). I’ll attach that in the post above. Most runs 5-6ish before salting with 0.3g, 3-4ish after.



Edit: a little rushed this morning, reread your post…will boost citric in the one that is still finishing, after 72hr filter, then let it run some more.check before/after pH too.

Follow-up report: No cloudiness upon adding extra citrate, no additional crystalls formed. Pre-re-salt, pH was at normal post-salting level. Final yield above.

 

[Cheelin]

So, pH strip showed similar acidity as normal. I filtered needles (got another 0.096g), then added 0.4g citrate, no cloudiness, will let it go 48 hrs more, then filter & wash jar. 65% recovery so far, might get to 2/3s.

 

[Cheelin]

Looking like the toughest part of developing this tek is going to be the work on reusing solvent. Take a look at the 36 hr yields for part I. of the reused solvent trial above.

 

[Loveall]

Looking like the toughest part of developing this tek is going to be the work on reusing solvent. Take a look at the 36 hr yields for part I. of the reused solvent trial above.

So yield was higher with reused solvent? That is surprising.

The yield stayed the same for me when reusing, but I didn't freeze to remove water. I'll repeat your experiment and see what I get.

 

[Cheelin]

If no surprises in final filtering, I’ll rerun as soon as the solvents are washed, probanly won’t have enough 15g citrate solvent.

 

[Loveall]

I've started a separate test salitng with different organic acids just for the fun of it after doubledog posted some pretty mescaline tartrate xtals this morning.

I extracted 50g of powder into EA (703g) after about 45 minutes of work . I split this into 6 small jars with 65g of extract each and reserve the rest (703-65*6= 313g).

Expecting ~ 65mg of mescaline citrate equivalent in each of the small jars.

I'm passively salting each jar with 120mg of different organic acids:

- Citric (control): Usual cloudiness
- Malic: Cloudy
- Tartaric: Cloudy
- Vitamin C: Cloudy
- Fumaric: Cloudy
- Benzoic: No clouds (bottom left in second picture), instead, I saw bubbles in EA after adding this acid. So it seemed like it didn't work originally, but now I'm seeing a tiny amount of xtals forming (?). This acid is interesting because it should be soluble in Xylene, so one could use it to salt that solvent directly, lazy stile (CIXLO?).

Will report back on what precipitates in each jar and weight of each salt. The weight ratios could illuminate the salt stoichiometry too. Hopefully we get a bunch of different CIELOs.

 

[Cheelin]

So, I just finished doing the 48hr filtering on the 9-treatment set of runs, using 5g of cactus powder, with powder that has ~1.1% yield with this tek, and fresh EA. These runs appear to be demonstrating, especially at this small run size, the amazingly consistent robustness of the paste recipe and pastemaking process.

Congrats to Loveall, Shroombee, and all the others who contributed to the pastemaking development effort.

Since the quantities of product are small (1.1% of 5g = 0.055g), the final filtering and jar wash/evap yields could swing the apparent results, i’ll hold off on any further comments until those results are in.

 

[Cheelin]

Good work by you, Loveall; Doubledog, too!

Perhaps the salting option will have several acid and crystallization options.

 

[Loveall]

Good work by you, Loveall; Doubledog, too!

Perhaps the salting option will have several acid and crystallization options.

Looks like it.

I may be jumping the gun here, but fumaric is kicking ass with super fast xtalization, very shiny transparent xtals, and no signs of sticking to the wall at all . Meanwhile the other jars have the clouds still hanging around and benzoic hasn't changed much.

Originally I didn't focus on fumaric cause it is not as soluble as citric in EA and I wanted the biggest process window possible to be robust. But if xtalization is better I may switch to it.

Product from a different acid will need lab analysis, it may be selective to different alkaloids (e.g. precipitate something new that citric doesn't).

 

[Loveall]

So, I just finished doing the 48hr filtering on the 9-treatment set of runs, using 5g of cactus powder, with powder that has ~1.1% yield with this tek, and fresh EA. These runs appear to be demonstrating, especially at this small run size, the amazingly consistent robustness of the paste recipe and pastemaking process.

Congrats to Loveall, Shroombee, and all the others who contributed to the pastemaking development effort.

Since the quantities of product are small (1.1% of 5g = 0.055g), the final filtering and jar wash/evap yields could swing the apparent results, i’ll hold off on any further comments until those results are in.

I'm looking forward to the final data on this