FractAlien
Esteemed member
I'm happy to see more Brazilians here!
I'm really curious about water extraction. Tell us more about it.
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TEK Ethyl acetate approach [CIELO]
- Thread starter Loveall
- Start date
This topic contain a TEK
I'm really curious about water extraction. Tell us more about it.
Criptomind
Rising Star
Yeah, it's nice. I tried a limonene tek yesterday, and it was an absolute fail—nothing came out of the vinegar.
I thought about doing something more aggressive, but, lo and behold, I couldn't find the right precursors... sigh.
But @modern gave me some hope.
Limonene on cactus powder with lime? That one can be a bit "iffy". Sometimes it responds to drying out the paste, crushing to powder, then mixing with more lime and water again.
Were you sure the cactus was an active specimen?
Criptomind
Rising Star
Yeah, the 69rons tek.
I'm thinking maybe it's the cactus or my limonene wasn't pure enough. Got d-limonene somewhere else and will give 1 more try next week.
Even if the cactus wasn’t the right one, I should still get some alkaloids, right? Even if they're inactive.
I got absolutely nothing.
Even ostensibly active species can sometimes produce practically zero alkaloids in a given specimen. And an inactive cactus will not necessarily contain any alkaloids, not even inactive ones. Also, if those alkaloids are phenolic (as many of the 'inactive' ones are), they'll stay bound to the lime paste and not get picked up by the limonene.
It's kind of helpful if you know that you're working with active material before starting the extraction. But again, the 69ron tek sometimes produces dud runs that end up yielding something when dried out and repeated, even if the first run drew a total blank.
You do need to be sure your limonene is the right stuff - I've seen people attempting to extract with limonene-based cleaning agent before. It was only 5% limonene and mostly consisted of water and detergent. :MAJOR_FACEPALM:
Check the SDS/MSDS.
Criptomind
Rising Star
Thanks for the info,
then it's most likely my cactus, which is worse cause I still have 200g of it.
I do believe I did everything right, so maybe no point on trying again, will find another source for my cacti.
Cheers
OK, but I'll say it one more time, you may still get something out of that paste if you dry it out and reprocess it. It's an intrinsic flaw of the limonene process, we're not sure why. It's also a reason why we've got this ethyl acetate thread here
You don't know for sure that your cactus is inactive. Best of all would be to use a more reliable solvent for the second try, if you still have the paste from before. You may still need to dry the paste out as suggested - and the dry powder might be amenable to pulls with IPA - check @modern's posts.
if you have oxalic acid (sal azedo) you can do an extraction using OASIS. You can skip the alcohol all together as someone messaged me saying you can just add to the tea and it’ll produce the crystals the same manner. I have not tried it but I did believe it could be possible considering the properties of the Crystal. First add small amount until fine precipitate forms and keep only the liquid. Then boil down until you get crystals forming or let it cool… don’t reduce 100%. The first fine powder is calcium and other oxalates not what you want (I tested twice)
You will however probably want to change the salt form to a “safer” salt. I can confirm you can add h2o2 concentrated and get mescaline carbonate/freebase. You can add hcl concentrate(20% may be strong enough) you will free the oxalic acid the. Need to wash with 99% isopropanol to remove the oxalic acid. Or do a mini a/b and convert to any sat form you want. Personally I haven’t tried the oxalate yet since using to experiment but I’ll test in the future orally. Do your own research.
This is a great method if you are limited access to solvents… OASIS. I’m gonna attempt a different method with only water as the solvent but have no idea if it’ll work from tea… will first try with pure extract as POC.
BTW try to understand each step and why you do them it’ll help you a lot. Also I’ve learned the hard way… don’t toss anything until you are done and know you got what you want. Most likely you can recover if you mess up asking for help.
You will however probably want to change the salt form to a “safer” salt. I can confirm you can add h2o2 concentrated and get mescaline carbonate/freebase. You can add hcl concentrate(20% may be strong enough) you will free the oxalic acid the. Need to wash with 99% isopropanol to remove the oxalic acid. Or do a mini a/b and convert to any sat form you want. Personally I haven’t tried the oxalate yet since using to experiment but I’ll test in the future orally. Do your own research.
This is a great method if you are limited access to solvents… OASIS. I’m gonna attempt a different method with only water as the solvent but have no idea if it’ll work from tea… will first try with pure extract as POC.
BTW try to understand each step and why you do them it’ll help you a lot. Also I’ve learned the hard way… don’t toss anything until you are done and know you got what you want. Most likely you can recover if you mess up asking for help.
I don’t recommend the dry tek due to limited penetration of the solvent… OASIS using like 50% alcohol works much better or even skip the alcohol based on someone’s msg to me. I’ve yet to try myselfOK, but I'll say it one more time, you may still get something out of that paste if you dry it out and reprocess it. It's an intrinsic flaw of the limonene process, we're not sure why. It's also a reason why we've got this ethyl acetate thread here
You don't know for sure that your cactus is inactive. Best of all would be to use a more reliable solvent for the second try, if you still have the paste from before. You may still need to dry the paste out as suggested - and the dry powder might be amenable to pulls with IPA - check @modern's posts.
BASI was the dry tek using benzoic acid… OASIS is what I am mostly working on now since not dry tek
Could replace EA with pure d-limonene and citric acid with benzoic. This has not been test but could work if mesc benzoate is Insoluble in limo.
NP solvents like toulene works and limo dissolves benozic acid well, so I'd wager it would likely work.
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ok. just cant seem to not get goo on the next two. even failed the reclaim, maybe? ... maybe its the material?
run A -
100g powdered with cacti that were put into a freezer after getting frozen(included a couple fore arm sized bridgesii, some PC and about 10 seedlings/yearlings all spanish Pachanoi. it's a light tan/beige color. is dehydrated at 165 until pulverized, dehydrated again for an hour or so. in this case was stored in a jar with desiccant packets. saw a thread with opposing data re whether frozen material would cielo. this would cloud in the air a bit when moving from jar to mixing bowl. added 25g ms wiggles lime. powders mixed before reverse osmosis water was added, in 1:1 ratio, ~100g h2o. mixed well, wasn't quite a dough i wouldn't say but there were no dry spots and it would clump/hold shape when you grabbed a fist of it. immediately began adding EA, ea is klean strip mek sub. 200g initially, followed by the 150g pulls + 2-3 minutes with the electric mixer. the humidity was 40%, temp 62.9degrees. pulled a whole jar and it was a nice light color, could see through it. no green somehow. did a fridge rest with 1 tbspn sodium carbonate, for about 6 hours. didn't see a water layer (would it be on top or bottom of mason jar... with the sediment?), wasnt sure if i saw clumping of the soda ash?maybe a little but mostly still powdery. removed soda ash and continued to salting with a teaspon and a half of milliards citric acid. with the clearer soln the clouding was clear, started the mag stir and let it mix. xtal began to drop out shortly after, i think. hasn't tested. maybe a couple hundred mg at most? white small. mixed for a few hours then poured off. although got some little back, there was so much that was stuck to the sides of the jar where it would hit on its rotation and sticky to the bottom. it just seemed sticky. maybe if better % material this would have been a success? but im not satisfied with the amount of goo that still happened.
run B (same conditions as above)-
66g fresh bridgessi suspected/known 2+%, dehydrated, pulverized, dehydrated, mixed with 17g of lime as above, 66g RO h2o added. mixed until no dry spots, remember thinking that it seemed too dry .... began pulls as above. this one was awful. the whole thing, took forever filtering. had to swap filters out and pour off. used maybe 30 filters. collected so much like ... fine dust? refiltered the EA collection jar and separated into two 32oz mason jars. did fridge rest and sodium carbonate with one and not with the other. didnt notice clumping nor water. salted both of them with a teaspoon of milliards . both of them on the stir plate, INSTAGOO. one of them thick green and the other a brown, huge clumps of goo.
attempted re-xtalization with 99ipa... failed, or it was cumbersome. ran on hot plate to boiling in the jars,poured off some catch. slow filtering. freeze rest to drop out anything else? i didnt see anything or just a couple little bits? then evaporate the liquid? im confused at this point... does the alkaloid go into the IPA or does it stay out? because i did evap a little tray and got some sticky white xtals that trying to dry more caused some browning at other points. i later threw a bit more ipa soln in there and it ruined it, made it so sticky.
the goo is discouraging; wonder what it is? taking it as a sign as not now. maybe the molecule chooses? studying my heart and with my mind until it becomes time again. initially going for those nice long crystals in the tek. have had more goo than would get us there and wonder what's about it. maybe the recent mention of the fumaric acid(is this what it is, someone said because its less sticky?)? should an attempt with the same process but this other acid be considered? don't think there are potency issues most of the time, except where pointed out above.
what are the variables that influence goo?
i have some photos/videos from the experiments i can put in a proton drive folder, dm me if you want to see
run A -
100g powdered with cacti that were put into a freezer after getting frozen(included a couple fore arm sized bridgesii, some PC and about 10 seedlings/yearlings all spanish Pachanoi. it's a light tan/beige color. is dehydrated at 165 until pulverized, dehydrated again for an hour or so. in this case was stored in a jar with desiccant packets. saw a thread with opposing data re whether frozen material would cielo. this would cloud in the air a bit when moving from jar to mixing bowl. added 25g ms wiggles lime. powders mixed before reverse osmosis water was added, in 1:1 ratio, ~100g h2o. mixed well, wasn't quite a dough i wouldn't say but there were no dry spots and it would clump/hold shape when you grabbed a fist of it. immediately began adding EA, ea is klean strip mek sub. 200g initially, followed by the 150g pulls + 2-3 minutes with the electric mixer. the humidity was 40%, temp 62.9degrees. pulled a whole jar and it was a nice light color, could see through it. no green somehow. did a fridge rest with 1 tbspn sodium carbonate, for about 6 hours. didn't see a water layer (would it be on top or bottom of mason jar... with the sediment?), wasnt sure if i saw clumping of the soda ash?maybe a little but mostly still powdery. removed soda ash and continued to salting with a teaspon and a half of milliards citric acid. with the clearer soln the clouding was clear, started the mag stir and let it mix. xtal began to drop out shortly after, i think. hasn't tested. maybe a couple hundred mg at most? white small. mixed for a few hours then poured off. although got some little back, there was so much that was stuck to the sides of the jar where it would hit on its rotation and sticky to the bottom. it just seemed sticky. maybe if better % material this would have been a success? but im not satisfied with the amount of goo that still happened.
run B (same conditions as above)-
66g fresh bridgessi suspected/known 2+%, dehydrated, pulverized, dehydrated, mixed with 17g of lime as above, 66g RO h2o added. mixed until no dry spots, remember thinking that it seemed too dry .... began pulls as above. this one was awful. the whole thing, took forever filtering. had to swap filters out and pour off. used maybe 30 filters. collected so much like ... fine dust? refiltered the EA collection jar and separated into two 32oz mason jars. did fridge rest and sodium carbonate with one and not with the other. didnt notice clumping nor water. salted both of them with a teaspoon of milliards . both of them on the stir plate, INSTAGOO. one of them thick green and the other a brown, huge clumps of goo.
attempted re-xtalization with 99ipa... failed, or it was cumbersome. ran on hot plate to boiling in the jars,poured off some catch. slow filtering. freeze rest to drop out anything else? i didnt see anything or just a couple little bits? then evaporate the liquid? im confused at this point... does the alkaloid go into the IPA or does it stay out? because i did evap a little tray and got some sticky white xtals that trying to dry more caused some browning at other points. i later threw a bit more ipa soln in there and it ruined it, made it so sticky.
the goo is discouraging; wonder what it is? taking it as a sign as not now. maybe the molecule chooses? studying my heart and with my mind until it becomes time again. initially going for those nice long crystals in the tek. have had more goo than would get us there and wonder what's about it. maybe the recent mention of the fumaric acid(is this what it is, someone said because its less sticky?)? should an attempt with the same process but this other acid be considered? don't think there are potency issues most of the time, except where pointed out above.
what are the variables that influence goo?
i have some photos/videos from the experiments i can put in a proton drive folder, dm me if you want to see
wow, maybe this is what needed doing with those jars... just has little specs where it was stirred on the sides and the bottom too had some buildup. so you get some water to collect that and then what? pyrex and dehydrator?
I just did two 1:1s, dried the same way and one of the material had so much sediment the other had none at all. both goo'dYep, looks like it needs an update. If the crumbs are completely wet it appears people don't get sediment AND are more robust to goo
That looks like unpromising material, apart from the bridgesii!
Both the filtering (particulates) problem and the goo formation sound like the result of too little water in this instance, but I could be wrong.
There was some discussion here a while back of how the crystalline monomescaline dihydrogen citrate is hydrated, whereas the low water goo was suspected of having a higher proportion of mescaline. [I suspect it may even be a highly viscous ionic liquid.]
I'll have to check up on whether any analyses were done on this goo - it would be more useful to be able to state these ideas withmore confidence, or refute them entirely, of course.
Posted this elsewhere but lots of knowledgeable people here.
So with Ceilo now suggesting stir bar for faster crystallization wouldn’t that increase impurities? The 97% purity is very high and I got that figure from here. The impurities increase due to higher surface area and trapping others from fast formation. If it is always that pure from precipitating once ignore everything I mentioned
Also like I mentioned someone showed me ethyl acetate used after extractions and filtered before neutralizing and they had quite a lot of citrate that formed a few weeks after the fact. When “recycling” with wash soda you basically make any remaining mescaline citrate freebase again and will offset results of future extractions. We would need to do a water wash of the ethyl acetate to pull any unprecipitated citrates to keep results more accurate.
As cool as it is to be finding these high yields they seem disproportionate to literature considering most use whole plant and not just outer flesh. I don’t have enough understanding of the tests to give a response but I think there are more accurate tests like UV-Vis and GC/MS but idk costs and practicality vs NMR
The reason I say this is even with 3 crystatillizations mescaline hcl seems to remain in the 93% range from 70% starting from early lab settings. For hobbyists it doesn’t matter much really but when sharing results the ranges are quite large. Even a 20% impurity of hcl like I mentioned is a large difference. They even use a much tighter ph alkaline range of 9.5 vs 12 used as hobbyists.
In theory I know Ceilo does a great job at selecting mescaline due to the xlogp3 being so similar but I’m sure there are other things that are also pulled. Plus the fact that rapid crystallization and reusing solvent without distilling may be affecting results. Oils and other similar products im sure are also pulled.
Just wondering really since I see many report needing such high doses of citrate many times much higher than the conversion rates of the salts. Also recently have been seeing reports of 5-6% yields from whole plant. 1:1.9 ratio hcl:citrate that is quite high.
Was wondering if anyone has more info on how the citrate used to test purity was obtained… from an extraction or from pure salt used to test the process? Also if any recystalization was preformed.
Looking at old posts I found some very high yield reports but was from questionable members that seem to have had alternative purposes to report high yields. Even attitude on the reports share they don’t include measurement uncertainty and no margin of error +/- so someone would need to send identical samples in for two different tests just to see how close the results are but that would be costly.
So with Ceilo now suggesting stir bar for faster crystallization wouldn’t that increase impurities? The 97% purity is very high and I got that figure from here. The impurities increase due to higher surface area and trapping others from fast formation. If it is always that pure from precipitating once ignore everything I mentioned
Also like I mentioned someone showed me ethyl acetate used after extractions and filtered before neutralizing and they had quite a lot of citrate that formed a few weeks after the fact. When “recycling” with wash soda you basically make any remaining mescaline citrate freebase again and will offset results of future extractions. We would need to do a water wash of the ethyl acetate to pull any unprecipitated citrates to keep results more accurate.
As cool as it is to be finding these high yields they seem disproportionate to literature considering most use whole plant and not just outer flesh. I don’t have enough understanding of the tests to give a response but I think there are more accurate tests like UV-Vis and GC/MS but idk costs and practicality vs NMR
The reason I say this is even with 3 crystatillizations mescaline hcl seems to remain in the 93% range from 70% starting from early lab settings. For hobbyists it doesn’t matter much really but when sharing results the ranges are quite large. Even a 20% impurity of hcl like I mentioned is a large difference. They even use a much tighter ph alkaline range of 9.5 vs 12 used as hobbyists.
In theory I know Ceilo does a great job at selecting mescaline due to the xlogp3 being so similar but I’m sure there are other things that are also pulled. Plus the fact that rapid crystallization and reusing solvent without distilling may be affecting results. Oils and other similar products im sure are also pulled.
Just wondering really since I see many report needing such high doses of citrate many times much higher than the conversion rates of the salts. Also recently have been seeing reports of 5-6% yields from whole plant. 1:1.9 ratio hcl:citrate that is quite high.
Was wondering if anyone has more info on how the citrate used to test purity was obtained… from an extraction or from pure salt used to test the process? Also if any recystalization was preformed.
Looking at old posts I found some very high yield reports but was from questionable members that seem to have had alternative purposes to report high yields. Even attitude on the reports share they don’t include measurement uncertainty and no margin of error +/- so someone would need to send identical samples in for two different tests just to see how close the results are but that would be costly.
So at Loveall answered most of these on Reddit but I’m curious on the correct salt conversion rate. I’ve seen 65% and I’ve seen 1:1.9 hcl:citrate I’ve seen the salt conversion but doesn’t include weight of the water? I think the 1.9x is the correct conversion rate since the 65% doesn’t take into account the monohydrate