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Some Q's about ethyl acetate approach. Options
 
Gibson
#61 Posted : 9/18/2022 5:56:09 PM

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A few more pics from this run. Making the paste, I think I was adding in more dry powder at this point, a pic after stirring the final pull, and a pic of crystals in the flask.

Gibson attached the following image(s):
IMG_1160.jpg (545kb) downloaded 168 time(s).
IMG_1164.jpg (401kb) downloaded 167 time(s).
IMG_1206.jpg (264kb) downloaded 167 time(s).
 

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Loveall
#62 Posted : 9/18/2022 8:18:36 PM

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Gibson, double filter is more robust to different xtal sizes. Depending on how the process goes, xtals can be smaller than what you got. For example, when using reused solvent the xtals can be smaller. Or if doing the fast xtalization, etc.

Seems like you are succeeding now, right? What do you think was your original issue? Is there something we can add to the current TEK to make it more robust/clear to others? Or is the TEK ok as is? Thanks!



💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Gibson
#63 Posted : 9/18/2022 9:34:15 PM

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Loveall wrote:
Gibson, double filter is more robust to different xtal sizes. Depending on how the process goes, xtals can be smaller than what you got. For example, when using reused solvent the xtals can be smaller. Or if doing the fast xtalization, etc.

Seems like you are succeeding now, right? What do you think was your original issue? Is there something we can add to the current TEK to make it more robust/clear to others? Or is the TEK ok as is? Thanks!



Loveall, Feels like success, the crystals look good and clean, if small. I just did the pulls on 59gms of powder. I want to make large crystals this time.

Original issues? First run, sloppiness, didn't have graduates for volume, my pocket scale only had two digits past the decimal point, was 20 years old and a little sticky. But worst was my idea that excess EA didn't really matter, so I used too much and the extract was too dilute.

Then I needed to learn how to decant on my 2-4 runs. Maybe a mason jar would be easiest. I have a few. A beaker wasn't great because there's no incline to keep the water globule more isolated, I'm using a large flask now, and that's better. I have to really focus while I'm doing it because up close the boundaries are a little distorted through the glass. Can't see it that well far away. I think I'm keeping all the water behind, but losing a few ml of extract.

I never really had a problem with goo.

I'm hoping the powder I'm using is weak is why my yields are pretty low.

One kind of consistent thing I'm seeing is congealing of the paste on the last few pulls if I use the TEK amount of water. The last run you saw in the pictures above was the first that didn't congeal at all. It remained workable and drained well through the last pull.

It had the 100gm equivalent of 202ml vs 270ml starting in the TEK.

I'm draining the last pull through the filter of my current 59gm run. It did start to congeal during the final mixing step of the last pull. It didn't want to drain well, so I left the paste on the filter funnel for 15 minutes and it did drain completely, surface is light and airy and I recovered 455ml of dark green EA from a total of 558ml used.

It was prepared with a 100gm equivalent of 236ml water vs the 270ml in the TEK.

I made a feeble attempt to dry the powder before preparing paste this time. 40 gm of powder, in a 1.5cm layer, placed in a convection oven at 150 F for 30 minutes resulted in a .5 gm loss. I couldn't make much of a conclusion from that and didn't want to dry it all overnight, so I made paste with a little more water than the previous run, but it still was a little too wet with 12.5% less water than the TEK. The consistency after working the paste was getting to be like modeling clay.

I prepared the powder for my first two runs, cut up the cactus and dried it out overnight. Cracker crispy. But those runs also congealed early with the TEK amount. Probably all the powder I used is moister than what you use, so I'll adjust accordingly.

I hope to get large crystals from this run. It's in a flask in the fridge now till tomorrow evening, then I'll decant and filter. I'll grind my citric acid fine. Can I add it without any stirring? Merkin felt it's important to add while the EA is still cold for faster crystals.

Last run I needed 2.25 gm Citric acid, and I checked the pH right after one gram and it was already showing slightly acid. I added the rest anyway.

Is the Citric acid amount needed determined by the amount of lime or mescaline or both? Is it lowering the pH and reacting with the mescaline? Reacting with the lime at all?




Gibson attached the following image(s):
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Loveall
#64 Posted : 9/18/2022 10:17:42 PM

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If you are getting goo early you can try to pull more quickly. Warm EA from a warm arage (80 to 90F) seems to congeal the paste faster vs EA at room temp (70F). You are only using lime (Ca(OH)2) and water to make the paste, correct (no Na ions)? Are you keeping the lime/water ratio about the same as the TEK (~9%)? IDK if having more lime and less water causes the paste to congeal faster.

Some catus powder needs less water. Yours seems to need lot less than others. Not sure why.

The minimum ammount of citric depends on how much mescaline is in the solvent. We over salt by a lot, so the solvent should become acidic even at 500mg of citric. The amount of like doesn't notatter when salting because all the like is left behind in the cactus paste.

Yes, you can not stir the citric. That can give biger xtals.

Edit: I've diluted the extract as a test before. It still xtalized. Also, very late pulls with little mescaline xtalized on their own. I don't think mescaline dilution is an issue: it always xtalizes for me.



💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Gibson
#65 Posted : 9/18/2022 10:31:35 PM

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Loveall wrote:
If you are getting goo early you can try to pull more quickly. Warm EA from a garage seems to make a goo faster vs EA at room temp (70F). You are only using lime (Ca(OH)2) and water to make the paste, correct? Are you keeping the lime/water the ratio about the same as the TEK (~9%)? IDK if having more lime and less water causes the paste to coagulate faster.

Some catus powder needs less water. Yours seems to need lot less than others. Not sure why.

The minimum ammount of citric depends on how much mescaline is in the solvent. We over salt by a lot, so the solvent should become acidic even at 500mg of citric. The amount of like doesn't notatter when salting because all the like is left behind in the cactus paste.

Yes, you can not stir the citric. That can give biger xtals.





I guess there's two kinds of goo, goo instead of crystals, and congealed paste goo. Seems the congealed paste is undesirable, because it doesn't drain, and the solvent gets trapped in it.

No, I've been keeping the lime to cactus powder ratio the same as the tech, 4:1, I've been adjusting the water.

And that's all I'm using in my paste, (no Na ions). Room temp EA for extracts.

Wondering what is the lime doing with the cactus powder and mescaline when mixed with water? There's ammonia coming from somewhere. Is the mescaline present as hydrochloride in the cactus? And the lime frees it up?
 
Loveall
#66 Posted : 9/18/2022 10:44:57 PM

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I edited my post for clarity (not calling the congealed paste goo).

Mescaline is in some kind of natural salt/complex. I think malate salt has been mentioned. TThe important thing is that the mescaline has an H+ attached to it in natural form and is positive, and will bind to negative ions

Lime reacts with the natural mescaline, removing the H+, making it neutral and soluble in EA (simply, MesH+ + OH- -> Mes + H2O with the calcium++ and the natural negative ion making their own salt. The ammonia smell is from other stuff reacting with the lime (proteins and such I guess?), it is normal and thankfully does not interfere with this simple extraction.

Since you are using so little water and having early paste congealing issues, you can try to lower the lime amount and keep it at ~9 to 8% by water amount. Let us know if that helps.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Gibson
#67 Posted : 9/19/2022 11:01:14 PM

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Loveall wrote:
I edited my post for clarity (not calling the congealed paste goo).

Mescaline is in some kind of natural salt/complex. I think malate salt has been mentioned. TThe important thing is that the mescaline has an H+ attached to it in natural form and is positive, and will bind to negative ions

Lime reacts with the natural mescaline, removing the H+, making it neutral and soluble in EA (simply, MesH+ + OH- -> Mes + H2O with the calcium++ and the natural negative ion making their own salt. The ammonia smell is from other stuff reacting with the lime (proteins and such I guess?), it is normal and thankfully does not interfere with this simple extraction.

Since you are using so little water and having early paste congealing issues, you can try to lower the lime amount and keep it at ~9 to 8% by water amount. Let us know if that helps.


Very cool, I'll try that lime ratio next.

Looking back at a flask of spent EA that has been sitting for a week. Hasn't been washed yet, It was from my first run that produced mescaline from the bottle wash, but no crystals in the filter. But it has a lot of crystals in it now.


 
Gibson
#68 Posted : 9/19/2022 11:33:15 PM

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This EA was filtered for crystals 12 days ago. None recovered from the filter, mescaline was recovered from the bottle wash evaporate. It has sat, first in the fridge for a week, then on the shelf. Now it has crystals.

Gibson attached the following image(s):
IMG_1266.jpg (1,344kb) downloaded 91 time(s).
 
Gibson
#69 Posted : 9/30/2022 6:26:09 AM

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Smile
 
Gibson
#70 Posted : 9/30/2022 6:28:26 AM

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I recovered 157 mg of long clean crystals from that vial.

My most recent crystallization from 59 grams powder was 433mg or .73%, I was disappointed that they were small crystals, even though I added the citric acid without stirring. I added .6gm first, let it sit for a week and got most of the crystals already, then added another 2.3 gm and let it set another four days and got a few more crystals. All small.
Gibson attached the following image(s):
IMG_1372.jpg (710kb) downloaded 54 time(s).
IMG_1377.jpg (671kb) downloaded 54 time(s).
IMG_1437.jpg (806kb) downloaded 53 time(s).
IMG_1442.jpg (951kb) downloaded 54 time(s).
 
Loveall
#71 Posted : 9/30/2022 2:18:16 PM

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I don't worry about the xtal size too much, effects are the same. Sometimes they grow differently.

Your yields are on the lower side but not unheard of. Your water amount to make the paste is on the low side, you can try to add more water to be closer to the TEK recomendation, yield may improve a little bit. I don't think you tried normal amount of water and fridge rest, right?

The ideal paste is fluffy/airy with little resistance when stirred.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Gibson
#72 Posted : 9/30/2022 6:13:54 PM

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Loveall wrote:
I don't worry about the xtal size too much, effects are the same. Sometimes they grow differently.

Your yields are on the lower side but not unheard of. Your water amount to make the paste is on the low side, you can try to add more water to be closer to the TEK reccendation, yield may improve a little bit. I don't think you tried normal amount of water and fridge rest, right?

The ideal paste is fluffy/airy with little resistance when stirred.


It's good Loveall, I like the TEK, thanks for putting it out there for us! I think I'm done with this powder for awhile, waiting for my TBMs to grow some more then I'll try the TEK with them.

I have been doing a good fridge rest! When I tried a normal water amount I kept getting the paste to congeal, maybe this powder is wetter than normal. Now I processed all my spent EA so I can use it for my TBMS.

Thanks again! This site is invaluable.
 
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