Hey, from the reddit info Emulsions are a pain with fresh cacti and it less work to dehydrate the plant and follow the TEK.
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TEK Ethyl acetate approach [CIELO]
- Thread starter Loveall
- Start date
This topic contain a TEK
So I've reattempted cielo and used less water as now suggested. I was still in doubt so added sodium carbonate at .5g per L and it did seem to remove some water. I then proceeded to salting. It clouded as normal I gave it a quick stir and left it allow covered. 12h later I could see a layer of 'white' dust on the bottom of the jar. So I decanted the top portion of the EtOAc and then swirled the bottom to get as much loose as possible. The issue was it became a red goo AFTER I swirled everything. I proceeded to decant leaving the goo. So now I added 99% ISO heated slightly and into the freezer. Before heating I could see clouds form once the ISO came into contact with the goo. After Freezing for a couple of hours I could see lots of precipitate. So I filtered off the ISO and caught most of the fine crystals. I collected the ISO again refrozen as some was still there.
Now the issue is the crystal as it dried on the filter paper it seems to have seeped and dried within the paper. One of the extracts visually had MUCH more crystals by volume but ended up with just a few hard rocks and the other also 'lost' volume and was also a hard mass.
Is there a way to prevent this loss to the paper filters? In the end I still didn't use enough starting material to be able to weigh my final product.
The sodium carbonate did prevent the 'clear goo' that I've had in the past and didn't dry excessively that I got a hard red goo but now had a different red fluid goo which is new to me.
Now the issue is the crystal as it dried on the filter paper it seems to have seeped and dried within the paper. One of the extracts visually had MUCH more crystals by volume but ended up with just a few hard rocks and the other also 'lost' volume and was also a hard mass.
Is there a way to prevent this loss to the paper filters? In the end I still didn't use enough starting material to be able to weigh my final product.
The sodium carbonate did prevent the 'clear goo' that I've had in the past and didn't dry excessively that I got a hard red goo but now had a different red fluid goo which is new to me.
Twilight Person
Esteemed member
I tried the boiling variant now where you heat the paste inside the EA.
I used a super low amount of water as you mentioned, it was mostly a powder still. So i put the EA inside and put it on boil for 5 min. But then it transformed into a terrible goo. It basically became the Same consistency as during the old TEK after like 5+ pulls, where you also just get a slime where you cant extract anymore, just this time it was the very first pull... : (
So any more people tried to boil it and it became a slime? Now trying to dry it since 12 h already but only the surface is dried - inside still slime. Need to wait for All the EA and Water to evaporate because then of course it must be a powder again, but before i cant do any more pulls :/
PS: to modern, why not try put it into freezer instead before? What i could recover from slime pull is also in freezer now, this evening adding the CA after filtering off ice.
I used a super low amount of water as you mentioned, it was mostly a powder still. So i put the EA inside and put it on boil for 5 min. But then it transformed into a terrible goo. It basically became the Same consistency as during the old TEK after like 5+ pulls, where you also just get a slime where you cant extract anymore, just this time it was the very first pull... : (
So any more people tried to boil it and it became a slime? Now trying to dry it since 12 h already but only the surface is dried - inside still slime. Need to wait for All the EA and Water to evaporate because then of course it must be a powder again, but before i cant do any more pulls :/
PS: to modern, why not try put it into freezer instead before? What i could recover from slime pull is also in freezer now, this evening adding the CA after filtering off ice.
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@Twilight Person - it sounds like heating has hastened hydrolysis of the solvent. This produces calcium acetate and ethanol, which form a gel. I guess some cactus components may contribute to the slime as well, and ethanol could be bringing them into partial solution. Did the slime persist on cooling?
Looking forward to seeing tonight's results all the same!
Looking forward to seeing tonight's results all the same!
I kept thinking what might have gone wrong... either humidity from only placing foil over the beaker causes water OR mescaline isn't saturated enough to properly crystalize? When I went thru the trouble of a/b I used less solvent since doing liquid liquid extraction so easier to pull so more saturated.
I was also thinking considering that pka is 9.56 wouldn't a ph just under 7 be enough to salt? is the amount of citric acid not excessive? Increasing the chances of the hydro citrate goo? I have zero idea just something I wanted to test in the future.
I was also thinking considering that pka is 9.56 wouldn't a ph just under 7 be enough to salt? is the amount of citric acid not excessive? Increasing the chances of the hydro citrate goo? I have zero idea just something I wanted to test in the future.
Twilight Person
Esteemed member
Oh no i never thought about hydrolysis. That is indeed what surely happened.
Yes I dried the whole cake again back to 0. Sadly that means I had to heat it, it otherwise only dried on the first 1 mm crust and then just stayed a slime inside. So mescaline freebase heated 12 h at 40° C in the food dehydrator might have anyways destroyed quite some goodies. Or at the absolute maximum it would be just neutral to the whole process.
Still I now fear that I at least partially screwed my extraction. It was from 6x cacti thrown together, oh no it is too sad. Will never heat it now.
From the first EA that I at least had recovered from the day I firstly wrote, I already put the CA yesterday and now I see crystals, but they grow much less beautiful than the original CIELO crystals. Could be because the ethanol is now also in the mix I guess.
Yes I dried the whole cake again back to 0. Sadly that means I had to heat it, it otherwise only dried on the first 1 mm crust and then just stayed a slime inside. So mescaline freebase heated 12 h at 40° C in the food dehydrator might have anyways destroyed quite some goodies. Or at the absolute maximum it would be just neutral to the whole process.
Still I now fear that I at least partially screwed my extraction. It was from 6x cacti thrown together, oh no it is too sad. Will never heat it now.
From the first EA that I at least had recovered from the day I firstly wrote, I already put the CA yesterday and now I see crystals, but they grow much less beautiful than the original CIELO crystals. Could be because the ethanol is now also in the mix I guess.
So I did a water wash of the filters and what I was able to scrape off. I dried the water to get a hard orange/red goo. I added 2mL of ISO and heated. Then rather putting in freezer I put on watch glass and kept swirling it so the outer edges would dry and the center would start concentrating to the goo. At the very end I removed the goo by blowing it off and then scraped off the white precipitate that formed which looked like white paint. I was able to weight it and got around 10mg of citrate salt so a very low .6% yield from still immature seedlings. 20 inches only ended up with ~15g dry with core, skin and white and green flesh.
Attachments
Mitrafiner
Rising Star
Hello. Awesome efforts to all and thanks.
I hope this is the right place for this question, if not tell me where to go
...
In the CIELO tek I see:
'' Consumables
Crystallize
Drop ~5 grams (~1 teaspoon) of citric acid into extract. Do not under salt with citric acid since it is necessary to have excess citric acid to form crystalline momomescaline citrate (gooey trimescaline citrate can form in alkaline conditions). Allow the citric acid to dissolve by diffusion without stirring. Extract will cloud as the dissolved citric acid reacts with mescaline freebase to form insoluble mono-mescaline citrate. Cloudiness may be hard to see in darker extracts (a backlight may help). If the citric acid is anhydrous and/or coarse it may take a while to dissolve, however it WILL dissolve fully. Leave cloudy extract undisturbed and sealed with a lid. Crystals of monomescaline citrate should begin to appear after a few hours, and take a few days to completely crash out (at least 3 days of wait is recommended). ´´...
> : The thing that I am confused about is salt:
1) if it is added at the same time as the citric acid?
2) Do I pre mix salt and citric acid?
3) Did I miss a step somewhere regarding the salt?
4) Is pure NaCl required?
Whooooooo to everyone.
I hope this is the right place for this question, if not tell me where to go
...In the CIELO tek I see:
'' Consumables
- Washing soda (Na2CO3) and salt (NaCl) for solvent reclaim (neutralization and wash)
Crystallize 
Drop ~5 grams (~1 teaspoon) of citric acid into extract. Do not under salt with citric acid since it is necessary to have excess citric acid to form crystalline momomescaline citrate (gooey trimescaline citrate can form in alkaline conditions). Allow the citric acid to dissolve by diffusion without stirring. Extract will cloud as the dissolved citric acid reacts with mescaline freebase to form insoluble mono-mescaline citrate. Cloudiness may be hard to see in darker extracts (a backlight may help). If the citric acid is anhydrous and/or coarse it may take a while to dissolve, however it WILL dissolve fully. Leave cloudy extract undisturbed and sealed with a lid. Crystals of monomescaline citrate should begin to appear after a few hours, and take a few days to completely crash out (at least 3 days of wait is recommended). ´´...> : The thing that I am confused about is salt:
1) if it is added at the same time as the citric acid?
2) Do I pre mix salt and citric acid?
3) Did I miss a step somewhere regarding the salt?
4) Is pure NaCl required?
Whooooooo to everyone.
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"solvent reclaim" will follow "crystallization" - read the method through carefully at least a couple more times.Hello. Awesome efforts to all and thanks.
I hope this is the right place for this question, if not tell me where to go
In the CIELO tek I see:
'' Consumables
...
- Washing soda (Na2CO3) and salt (NaCl) for solvent reclaim (neutralization and wash)
Crystallize
Drop ~5 grams (~1 teaspoon) of citric acid into extract. Do not under salt with citric acid since it is necessary to have excess citric acid to form crystalline momomescaline citrate (gooey trimescaline citrate can form in alkaline conditions). Allow the citric acid to dissolve by diffusion without stirring. Extract will cloud as the dissolved citric acid reacts with mescaline freebase to form insoluble mono-mescaline citrate. Cloudiness may be hard to see in darker extracts (a backlight may help). If the citric acid is anhydrous and/or coarse it may take a while to dissolve, however it WILL dissolve fully. Leave cloudy extract undisturbed and sealed with a lid. Crystals of monomescaline citrate should begin to appear after a few hours, and take a few days to completely crash out (at least 3 days of wait is recommended). ´´...
> : The thing that I am confused about is salt:
1) if it is added at the same time as the citric acid?
2) Do I pre mix salt and citric acid?
3) Did I miss a step somewhere regarding the salt?
4) Is pure NaCl required?
Whooooooo to everyone.
Citric acid is added to form mescaline citrate, which crystallizes. The solvent is poured off the crystals. Sodium carbonate is added to the solvent to remove remnants of unreacted citric acid. The solvent can then be re-used for further pulls from cactus/lime paste.
Mitrafiner
Rising Star
Thanks so much for this answer!
I am still confused, though:
´Citric acid is added to form mescaline citrate, which crystallizes´
´Sodium carbonate is added to the solvent to remove remnants of unreacted citric acid´
But in the ingredients:
´Consumables
- Washing soda (Na2CO3) and salt (NaCl) for solvent reclaim (neutralization and wash)´
The key ideas that I am still misinterpreting are:
1) NaCl: At which step?
2) NaCl: Added at what ratio? Or simpler, how much?
Cheers in advance for any clarifications to my confusion.
Common salt can be used to absorb moisture.
Edit: if you use "find in page" with the search term "salt" on the CIELO wiki page, you'll find the 15th result to be relevant.
Edit: if you use "find in page" with the search term "salt" on the CIELO wiki page, you'll find the 15th result to be relevant.
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navegandouniversos
Esteemed member
Hi man, maybe this can help you
Wash neutralized solvent with a tablespoon of salt and ~50ml of water. The solvent cloudiness will change after shaking for a few minutes. Rest the solvent in the fridge for a few hours until a backlight shines through clearly. Decant into a long term storage container (e.g. original solvent can if empty). As before, you will need to leave some solvent behind wich can be added to the next brine wash). Optionally, use a separatory funnel to recover all of the washed extract.
Good luck! let us know if worked
Mitrafiner
Rising Star
YAY!
So I don´t need to be too anal with mgs of NaCl (Salt)? Is that the case?
Thanks
So I don´t need to be too anal with mgs of NaCl (Salt)? Is that the case?
Thanks
Mitrafiner
Rising Star
Edit: if you use "find in page" with the search term "salt" on the CIELO wiki page, you'll find the 15th result to be relevant.
Yeah, thanks. It is good. Just for beginners, it might make sense to put the predicted amount or if specificity is required for the washing soda and salt in the initial ´consumables´ list. I still wasn´t sure if a tablespoon was a specific amount or eyeballed.
Thanks agan.
Yeah, thanks. It is good. Just for beginners, it might make sense to put the predicted amount or if specificity is required for the washing soda and salt in the initial ´consumables´ list. I still wasn´t sure if a tablespoon was a specific amount or eyeballed.
Thanks agan.
You might not need the salt at all, if the moisture content of your EA is in the right range.
A standard tablespoon can be considered to be equivalent to 15 g or 15 mL. To that end, kitchen scoops are quite handy - they typically come as a set with 5, 10 and 15 mL sizes. These correspond to teaspoon, dessert spoon and and tablespoon measures. But why is "dessert spoon" written as two words?
A standard tablespoon can be considered to be equivalent to 15 g or 15 mL. To that end, kitchen scoops are quite handy - they typically come as a set with 5, 10 and 15 mL sizes. These correspond to teaspoon, dessert spoon and and tablespoon measures. But why is "dessert spoon" written as two words?
Mitrafiner
Rising Star
> Thanks all I think I feel more confident to poceed now.You might not need the salt at all, if the moisture content of your EA is in the right range.
A standard tablespoon can be considered to be equivalent to 15 g or 15 mL. To that end, kitchen scoops are quite handy - they typically come as a set with 5, 10 and 15 mL sizes. These correspond to teaspoon, dessert spoon and and tablespoon measures. But why is "dessert spoon" written as two words?
´ But why is "dessert spoon" written as two words?´
- next fkn level of reasoning...keep up the expansion
Tangent warning: ELT Concourse: compounding
- read this and tell me, so I can do my job better
> Thanks all I think I feel more confident to poceed now.
´ But why is "dessert spoon" written as two words?´
- next fkn level of reasoning...keep up the expansion
Tangent warning: ELT Concourse: compounding
- read this and tell me, so I can do my job better
about settles it
Actually, it's probably because "dessert" has the stress on the second syllable. And anyhow, my dictionary has it as a single compound word so the real answer is "Transform got it wrong"
@Loveall you posted somewhere the ph strip after each ethyl acetate pull and indicated it as proof of the strength at pulling the mescaline from the paste. HOWEVER wouldn't that indicate that we should add more LIME each pull to increase the ph to around 11 each time for maximum freebase mescaline to be pulled.
While working on perfecting my own extraction method I noticed a pull from tea had ZERO precipitate which was very strange to me... I poured half the tea away before I thought to test the ph. I used lime which I won't anymore with tea due to the behavior. The ph was 12 at first but quickly dropped to around 8-9 which only allowed a few crystals to be pulled.
EDIT: I got a reply answering my question on this topic. PH was of the ethyl acetate after each pull so assuming the ph of the paste is still around 11 means less and less alkaloid is being pulled since there is less ph difference in the solvent.
While working on perfecting my own extraction method I noticed a pull from tea had ZERO precipitate which was very strange to me... I poured half the tea away before I thought to test the ph. I used lime which I won't anymore with tea due to the behavior. The ph was 12 at first but quickly dropped to around 8-9 which only allowed a few crystals to be pulled.
EDIT: I got a reply answering my question on this topic. PH was of the ethyl acetate after each pull so assuming the ph of the paste is still around 11 means less and less alkaloid is being pulled since there is less ph difference in the solvent.
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starbob
Esteemed member
I thought it might be interesting to try CIELO with ascorbic acid, so I tried a rough solubility test with EtAc and the result was much worse than citric acid. I used L-ascorbic acid 100% food grade, roughly 10mL dry pure EtAc, and ~55mg ascorbic acid, but it would not dissolve. I was shooting for the CIELO equivalent 5g/L proportion like the tek roughly is currently. Perhaps some dissolved but a lot did not. I tried heat for awhile >55C but didn't help. Added 0.1mL distilled water at a time, shaking, returning to heat awhile, shaking and checking, and ultimately ended at 0.4mL (4% of EtAc volume) before it fully dissolved. It didn't precipitate any out after chilling a bit and left at room temp, so maybe I could have done 0.05mL water increments and ended at 0.35mL with some precipitating out after cooling.
I think I'll try a 2.5g/L proportion with ascorbic acid in a CIELO tiny batch. I assume that will be OK with the typical water content in the CIELO extract and given however much ascorbic acid will be consumed by the mescaline ascorbate crashing.
I think I'll try a 2.5g/L proportion with ascorbic acid in a CIELO tiny batch. I assume that will be OK with the typical water content in the CIELO extract and given however much ascorbic acid will be consumed by the mescaline ascorbate crashing.