TEK Ethyl acetate approach [CIELO]

[Cheelin]

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

Lol, Oh No, I’m not getting sucked back into searching for biggoo/abominable gooman again!



But…maybe that green eluted substance in the pull filter is a biggoo footprint.

 

[Cheelin]

Making molasses-like progress on the Used Solvent Multiple Re-Use trial, see minor update here: Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus

 

[orchidist]

My second unfiltered run developed droplets of water (looking like little pebbles) all over the bottom and slightly up the sides of the jar. The droplets looked like they formed exclusively in the lower, yellow layer of the solvent where the chlorophyll decomposed. I'm wondering if some kind of osmotic effect pulled the suspended particles to that layer with higher citric acid concentration, causing them to coalesce. The clouds have pretty much cleared at this point, so I'm not sure if there's potential for any more crystal formation.

I'm considering placing the open jar into a larger jar, and closing it up with a dessicant in it to see what happens.

I have a pretty strong suspicion that I was incorrect jumping to the conclusion that the droplets are water. I touched some from unfiltered run #2 with a glass rod, it stuck to the rod. It's colorless, viscous, sticky. Taste is bitter, no detectable sourness. Strong orange reaction with Marquis reagent. Seems for some reason my product is oiling out instead of crystallizing. The runs I did this weekend with proper filtration look to be evolving in the same manner. Will let everything sit for a few more days in hopes it'll spontaneously crystallize.

 

[Cheelin]

My second unfiltered run developed droplets of water (looking like little pebbles) all over the bottom and slightly up the sides of the jar. The droplets looked like they formed exclusively in the lower, yellow layer of the solvent where the chlorophyll decomposed. I'm wondering if some kind of osmotic effect pulled the suspended particles to that layer with higher citric acid concentration, causing them to coalesce. The clouds have pretty much cleared at this point, so I'm not sure if there's potential for any more crystal formation.

I'm considering placing the open jar into a larger jar, and closing it up with a dessicant in it to see what happens.

I have a pretty strong suspicion that I was incorrect jumping to the conclusion that the droplets are water. I touched some from unfiltered run #2 with a glass rod, it stuck to the rod. It's colorless, viscous, sticky. Taste is bitter, no detectable sourness. Strong orange reaction with Marquis reagent. Seems for some reason my product is oiling out instead of crystallizing. The runs I did this weekend with proper filtration look to be evolving in the same manner. Will let everything sit for a few more days in hopes it'll spontaneously crystallize.

Bummer! Let’s try to figure out that secret orchid sauce.

Which equipment, material, and process steps vary in any way from the Great Success method? No variation is too small.

 

[orchidist]

I'll preface with this: I do not know much about the identity of the cactus I'm using, it was obtained from a third party. Maybe it's whole bridgesii and I'm having a similar experience as mentioned in the TEK FAQ.

But, here goes! All measurements correspond to 25g starting material

Pastemaking:

Quantities are the same. My first failed run used tap water, all others have used reverse osmosis water with a TDS of 12. Mixed by thoroughly folding and rotating for 8 minutes with a silicone spatula, arm was screaming by the end of it.

Extraction:

I measured my solvent by mass according to extraction section of the the wiki, first pull, 50g, pull 2-8, 31.25g. This corresponds to using approximately ~916ml of solvent instead of the 946 for a full scale run. 3% less.

For the pulls, I measured solvent, recorded the mass, added it to the paste without pre-mashing, started a metronome app set for 60 seconds at 90 bpm and used that to maintain pace. Instead of a spoon, a pair of glass rods held like chopsticks was used for stirring. Care was taken to evenly stir the material by rotating the french press 90 degrees halfway through the stirring process. Once the metronome stopped, I began a two minute timer, and used that time to prepare the next portion of solvent. Pulls 1-6 were combined, and 7,8 were combined in their own beaker. After all pulls were completed, the solvent was filtered through a double layer of coffee filters into a thoroughly cleaned jar (washed with water, then 100% isopropyl alcohol, then rinsed with fresh ethyl acetate)

Paste has become applesauce texture on the first addition every time. My pouring technique differed from yours. I did not upright the press and then pour again as in your method. I avoid squeezing the material.

I do have to note that the temperature of the room was quite cold. It's well below freezing in my part of the world right now. I've been using a window mounted fan to ventilate my workspace. It would be useful to know the exact temperature at the time, but I unfortunately don't have that information.

Crystallization:

The pulls were allowed to sit, and after the solution was observed to be clear, assisted with a flashlight, 0.625g (the quantity recommended on the wiki) citric acid was added to the combination of pulls 1-6. The separate pulls 7-8 were given 0.156g. This was done without stirring for the first three attempts. Attempt four was stirred briefly after the same quantity was added. Each time, 1-6 became very cloudy, 7-8 only slightly cloudy. During crystallization, since the windows are now closed, the room temperature is warmer than it would be during the actual procedure.

So in summary

- RO water vs distilled water
- Probably colder conditions
- Slightly less total solvent
- Pulls slightly longer than 2m due to switching between timers
- Different stirring tool
- Extract was filtered after all pulls were complete instead of between iterations
- Possibly less efficient solvent removal between pulls
- Temperature during crystallization higher than temperature during extraction
- Lower citric acid concentration during crystallization

 

[orchidist]

Hi Loveall,

Forgive my ignorance. Are you saying that if we use a much smaller amount of citric acid than we currently do (5mg/g citric acid/EA) that we will result in a more potent product (di- or tri- mesc citrate)?

Yep

Hi Loveall,

Is there no concern that we might end up with a mixture of different forms of mescaline citrate, which could make dosing difficult?

If some noobie accidentially adds a very small amount of citric acid, would they end up with a more potent product? E.g., they might assume that 500mg of citrate = 310mg of hcl, whereas in can be much stronger than that.

Not concerned with a mixture, one salt should precipitate based on the amount of citric. The trimescaline citrate precipitates as an oil and takes a long time to crash, don't see anyone confusing it with monomescaline, but I guess anything can happen out there. Don't know much about the dimescaline citrate thought. People simply need to add enough citric acid, if they can't do that I don't know what to say.

I wonder if this is what I'm observing. Just calculated the concentration of citric acid I used. I'm at 3.03 mg/g. Don't know if that counts as much less than 5 mg/g, but the precipitate I'm observing does seem consistent with trimescaline citrate

 

[downwardsfromzero]

Have you obtained crystals from any other extraction attempts with this exact same batch of cactus, orchidist? And have you ascertained its mescaline potency, even subjectively?

My thinking is if you happened to have a cactus that produced significant amounts of another similar alkaloid - maybe DMPEA - and if that alkaloid co-extracted into the EA, then you might see goo rather than crystals.

Performing a TLC test on a sample of the goo or getting some more sophisticated analysis done would be instructive as regards my hypothesis here.

Do we know what colour DMPEA might give with Marquis?

Taste is bitter, no detectable sourness

This is almost as though you're getting a different stoichiometry, but bitterness could of course be caused by any of a range of other substances including phenolics and saponins. [I see that Loveall has covered the stoichiometry question while I was composing this post. Best choice when applying Occam's razor.]

 

[orchidist]

Have you obtained crystals from any other extraction attempts with this exact same batch of cactus, orchidist? And have you ascertained its mescaline potency, even subjectively?

My thinking is if you happened to have a cactus that produced significant amounts of another similar alkaloid - maybe DMPEA - and if that alkaloid co-extracted into the EA, then you might see goo rather than crystals.

Performing a TLC test on a sample of the goo or getting some more sophisticated analysis done would be instructive as regards my hypothesis here.

Do we know what colour DMPEA might give with Marquis?

Taste is bitter, no detectable sourness

This is almost as though you're getting a different stoichiometry, but bitterness could of course be caused by any of a range of other substances including phenolics and saponins. [I see that Loveall has covered the stoichiometry question while I was composing this post. Best choice when applying Occam's razor.]

No crystals to report yet, this result has repeated with every run I've attempted with this material (the only material of this type I have, or have ever had)

I have begun looking for marquis color of DMPEA, so far haven't found anything. I just got a TLC kit, I'll do that soon. The unseparated oil turns a very clear orange w/ Marquis, so there's definitely an alkaloid there, and any other candidates are not orange too

 

[Cheelin]

Hi Loveall,

Forgive my ignorance. Are you saying that if we use a much smaller amount of citric acid than we currently do (5mg/g citric acid/EA) that we will result in a more potent product (di- or tri- mesc citrate)?

Yep

Hi Loveall,

Is there no concern that we might end up with a mixture of different forms of mescaline citrate, which could make dosing difficult?

If some noobie accidentially adds a very small amount of citric acid, would they end up with a more potent product? E.g., they might assume that 500mg of citrate = 310mg of hcl, whereas in can be much stronger than that.

Not concerned with a mixture, one salt should precipitate based on the amount of citric. The trimescaline citrate precipitates as an oil and takes a long time to crash, don't see anyone confusing it with monomescaline, but I guess anything can happen out there. Don't know much about the dimescaline citrate thought. People simply need to add enough citric acid, if they can't do that I don't know what to say.

I wonder if this is what I'm observing. Just calculated the concentration of citric acid I used. I'm at 3.03 mg/g. Don't know if that counts as much less than 5 mg/g, but the precipitate I'm observing does seem consistent with trimescaline citrate

Have a few nits about overzealousness, but they are about saving you effort.

I personally would go with double the citric acid to just make sure it is not the cause. I always ratio from 5g, and that is cuz it works for me, especially after the loveall post that your second post refers to.

You did not comment of the specific materials you are using, besides the cactus powder (which i assume met the conditions i mentioned?) and the water (what is its pH?). Did you use the same lime, EA, and citric as I mentioned?

If the materials are not diff, the water pH is w/in tolerance, the cactus powder size-consistency-mc% are w/in tolerance, and doubled citrate level makes no difference…then, seems the cactus itself could be the issue. So, some testing like that which DFZ suggests, or some other chem analysis of the cactus would then be in order.


Btw, i don’t want to get too deep into the verboten subject of sourcing, but… i have used two differently named species of trichocereus incense powder, one of them from 2 different countries, all from the same source - none of them bridgesii. One of the species/country options, purchased a couple times, were apparently different batches, producing different yield %s. They all produced similar looking crystals.

My first 6 batches, from cactus logs, that I processed into powder, did produce goo, but i attribute this to poor rinsing/washing technique, which occurred later in the process than when your goo is becoming evident. I have a couple T. pach logs, from a 3rd party (but a different one than used earlier), that have been hibernating for 3-4 mos, sometime soon I’ll process them. Perhaps my winning streak will change when it’s their turn.

 

[orchidist]

You did not comment of the specific materials you are using, besides the cactus powder (which i assume met the conditions i mentioned?) and the water (what is its pH?). Did you use the same lime, EA, and citric as I mentioned?

If the materials are not diff, the water pH is w/in tolerance, the cactus powder size-consistency-mc% are w/in tolerance, and doubled citrate level makes no difference…then, seems the cactus itself could be the issue. So, some testing like that which DFZ suggests, or some other chem analysis of the cactus would then be in order.

Sorry, I didn't mention those because I did use the same lime (Ms Wages, recently purchased) and citric acid (milliard, have had it for about 6 months), and EA (kleen strip) as you do. The cactus powder is also the correct consistency. Fine as flour, easily ends up in the air when agitated.

I will get a pH reading of my water and take some time to calculate MC% of my cactus. I didn't do that considering the discussion of the tolerance for water amount in the paste being pretty wide. At this point it seems like it's going to be necessary.

I'm currently working on TLC of some oil collected from the bottom of one of my earlier runs. Will have results soon. I had some other stuff that needed testing anyway, so while I'm at it I might as well.

 

[Cheelin]

Thanks for info, just making sure.

If your cactus powder becomes airborne when working with it, the mc is likely fine. My guess is pH of water is w/in tolerance, but jic.

 

[orchidist]

TLC Results in: Pulled some oil off the bottom of the jar w/ a glass rod, washed with fresh EtOAc, ran the TLC. One spot for each column, with expected results for mescaline for all of the test reagents I have on hand.

RO water pH is ~7

Interestingly, the oil solidified when washed with fresh ethyl acetate.

 

[Cheelin]

Would it be possible to put 50-75mL of your fredh EA in the freezer for at least 24 hrs, to check for ice?

 

[orchidist]

EA going in the freezer right now

 

[Cheelin]

What’s the pH of your salted solution?

And, how would you describe the color, form of the solid?

 

[Loveall]

TLC Results in: Pulled some oil off the bottom of the jar w/ a glass rod, washed with fresh EtOAc, ran the TLC. One spot for each column, with expected results for mescaline for all of the test reagents I have on hand.

RO water pH is ~7

Interestingly, the oil solidified when washed with fresh ethyl acetate.

I think water is being absorbed by fresh EA and leaving solids behind which could be mescaline citrate plus any solid junk the water had.

Have you had a chance to try a chemical EA dry on the extract before salting? CaCl2 pellets and Sodium Carbonate (monohydrate from arm and hammer super washing soda) had not negative effects (no positive for me because I get Xtals without a chem dry, but it may help in your case).

 

[orchidist]

What’s the pH of your salted solution?

And, how would you describe the color, form of the solid?

Going by the center of the pH paper, it looks to be between 5 and 6, however, the edges of the paper lean more acidic, I am guessing because of evaporation/capillary action and reading from there may be less accurate. Want to follow up with some CA solutions in fresh EA to make sure my readings are actually accurate.

The solid was off-white, and formed a crust around the glass rod when it was washed with fresh EA.

I think water is being absorbed by fresh EA and leaving solids behind which could be mescaline citrate plus any solid junk the water had.

Have you had a chance to try a chemical EA dry on the extract before salting? CaCl2 pellets and Sodium Carbonate (monohydrate from arm and hammer super washing soda) had not negative effects (no positive for me because I get Xtals without a chem dry, but it may help in your case).

I think that's possible, I haven't tried a chemical dry yet, but I will on my next round.

 

[Cheelin]

What’s the pH of your salted solution?

And, how would you describe the color, form of the solid?

Going by the center of the pH paper, it looks to be between 5 and 6, however, the edges of the paper lean more acidic, I am guessing because of evaporation/capillary action and reading from there may be less accurate. Want to follow up with some CA solutions in fresh EA to make sure my readings are actually accurate.

The solid was off-white, and formed a crust around the glass rod when it was washed with fresh EA.

I think water is being absorbed by fresh EA and leaving solids behind which could be mescaline citrate plus any solid junk the water had.

Have you had a chance to try a chemical EA dry on the extract before salting? CaCl2 pellets and Sodium Carbonate (monohydrate from arm and hammer super washing soda) had not negative effects (no positive for me because I get Xtals without a chem dry, but it may help in your case).

I think that's possible, I haven't tried a chemical dry yet, but I will on my next round.

pH is 1-2 units higher than my normal….sounds a lot like the near neutral pH in the Loveall post you were referring to, earlier. But his product was orange and not solidified, iirc.

If your fresh EA doesn’t have ice, any water must have come from your paste, presumably. What did your paste look like after10 min rest?

 

[orchidist]

Wish I'd taken pics, after the rest it was like dough. Moldable, but left a thin coating of itself behind when touched, which would dry quickly. Not sticky or slimy. Seemed within tolerance of the descriptions I've read here, and behaved as expected when exposed to solvent, but maybe could be dryer. When mixing it more resembled the stiff mashed potato description in the wiki.

 

[Cheelin]

Wish I'd taken pics, after the rest it was like dough. Moldable, but left a thin coating of itself behind when touched, which would dry quickly. Not sticky or slimy. Seemed within tolerance of the descriptions I've read here, and behaved as expected when exposed to solvent, but maybe could be dryer. When mixing it more resembled the stiff mashed potato description in the wiki.

It’s tuff getting grilled, I appreciate your great attitude.

Keep in mind you are improving, your chromatography shows you are extracting M.