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TEK Ethyl acetate approach [CIELO]
- Thread starter Loveall
- Start date
This topic contain a TEK
Cheelin said:
Great, was looking forward to this. Looks like the simple Tek with no options added consistently yielded better in your case. Looking forward to an update to the discussion section. Also, looks like propagating plant C would be good to do.
Did the xtals from the water become more needle like (vs. those straight from the filter)?
You mention better technique could help give more consistent results. Do you see any way to improve the TEK text to help workers with their technique?
Cheelin
Rising Star
Thanks Loveall.
On std yielding more, I’ll say it again: The std tek is just plain great; BUT, you have to do the major processes right. This means: the powder must be dry & fine like flour; the paste must have maximum contact and sufficient time between lime particles and powder particles; the pulls must be stirred sufficiently, rested long enough, and filtered crystal clear; the salting should be done based on the reason for doing it, for the proper change in pH, not for a, seemingly, arbitrary quantity addition. The other variations, do nothing to improve yield or quality; for what purpose? To have lighter colored solvent?
My conclusions on the sourcing of materials: buy a small quantity of the various powders available to you, test them, pick a winner and order a larger amount, especially if vendor is selling it fir 25% cheaper than their other options (the case here, lol).
As for crystals in the wash water: Shoot for getting all the crystals in your filter, minimizing the wash water wash. Again, you were right the 1st time, grow your crystals passively. It is a fundamental fact that time builds crystals , if all other requirements are met; if you want all your crystals in the filter, this is the best way to assure it. (Yes, I have not yet done a systematic comparison with the dump & stir method, but in the runs I have done, significantly more small particles don’t make it out of the jar (could be another technique issue). In the 12 runs of my experiment, i used 2x20mL aliquots of warm water to remove the dry crystals out of the jar. If you look at the yield of residue, all except the final jar filtered (which was the only one that had a faint hint of cloudiness after 56 hours of crystallization/settling) had an avg of~0.05g residue, not enough to grow more than slightly larger than microscopic crystal clumps. So, no, discernable crystal needles.
And, furthermore, if you have significantly more crystals/precipitate that is difficult to get out of the jar, solvent washing is not going to get rid of residual non-mescaline molecules, they just stay in the jar, get water washed into your dish, and gum up that product.
As for better technique hints: follow the method I have specified. It is the most explicitly specified approach so far, w checks along the way. Finally, practice makes perfect; do multiple runs, in sets of 2-3 runs, with a day or two between other sets of runs (let your sub-conscious think about what happened). Keep working it, with the knowledge that the std process is a winner, and you will eventually get up the learning curve.
Sorry to preach, but I made a bunch of shit earlier, and now I can consistently produce the desired product. This is how I did it. If it doesn’t work for you, try something else, I can’t help you.
On std yielding more, I’ll say it again: The std tek is just plain great; BUT, you have to do the major processes right. This means: the powder must be dry & fine like flour; the paste must have maximum contact and sufficient time between lime particles and powder particles; the pulls must be stirred sufficiently, rested long enough, and filtered crystal clear; the salting should be done based on the reason for doing it, for the proper change in pH, not for a, seemingly, arbitrary quantity addition. The other variations, do nothing to improve yield or quality; for what purpose? To have lighter colored solvent?
My conclusions on the sourcing of materials: buy a small quantity of the various powders available to you, test them, pick a winner and order a larger amount, especially if vendor is selling it fir 25% cheaper than their other options (the case here, lol).
As for crystals in the wash water: Shoot for getting all the crystals in your filter, minimizing the wash water wash. Again, you were right the 1st time, grow your crystals passively. It is a fundamental fact that time builds crystals , if all other requirements are met; if you want all your crystals in the filter, this is the best way to assure it. (Yes, I have not yet done a systematic comparison with the dump & stir method, but in the runs I have done, significantly more small particles don’t make it out of the jar (could be another technique issue). In the 12 runs of my experiment, i used 2x20mL aliquots of warm water to remove the dry crystals out of the jar. If you look at the yield of residue, all except the final jar filtered (which was the only one that had a faint hint of cloudiness after 56 hours of crystallization/settling) had an avg of~0.05g residue, not enough to grow more than slightly larger than microscopic crystal clumps. So, no, discernable crystal needles.
And, furthermore, if you have significantly more crystals/precipitate that is difficult to get out of the jar, solvent washing is not going to get rid of residual non-mescaline molecules, they just stay in the jar, get water washed into your dish, and gum up that product.
As for better technique hints: follow the method I have specified. It is the most explicitly specified approach so far, w checks along the way. Finally, practice makes perfect; do multiple runs, in sets of 2-3 runs, with a day or two between other sets of runs (let your sub-conscious think about what happened). Keep working it, with the knowledge that the std process is a winner, and you will eventually get up the learning curve.
Sorry to preach, but I made a bunch of shit earlier, and now I can consistently produce the desired product. This is how I did it. If it doesn’t work for you, try something else, I can’t help you.
The other variations were added in case the folks where having difficulty with the plain Tek needed less plant material in the extract. They are there to improve robustness to hypothetical plant variations (which may not be an issue, IDK), and user error.
I think excess salting is fine. I added more citric to spent EA (which had essentially just been neutralized) and nothing happened. Nothing new crashed. The excess is there because it seemed more robust for some. If there is a problem, it could be overcome with excess citric forcing precipitation. You are right that rinsing is needed if citric concentration is high, but I feel like that happens when removing the green color already with rinses.
On the other hand, I see your point. It may be better to spend time to get the basic TEK correct instead of adding stuff that my or may not make it more robust. I for one, never had an issue with the basic TEK and get xtals with different cactus sources. However, I feel bad for someone getting goo and wanted to see if we could make the process more robust. Also, the simple TEK seemed to good to be true in general, but maybe it is if done correctly.
It is believed that the clearer solvent will have more reuses, but that is speculation. Perhaps washes after a standard extraction are a simpler way to maintain good reuse rate. Or maybe allowing an increasingly deep green color does not interfere at all.
Thanks for your experimental effort, report, and experienced point of view on this process.
I think excess salting is fine. I added more citric to spent EA (which had essentially just been neutralized) and nothing happened. Nothing new crashed. The excess is there because it seemed more robust for some. If there is a problem, it could be overcome with excess citric forcing precipitation. You are right that rinsing is needed if citric concentration is high, but I feel like that happens when removing the green color already with rinses.
On the other hand, I see your point. It may be better to spend time to get the basic TEK correct instead of adding stuff that my or may not make it more robust. I for one, never had an issue with the basic TEK and get xtals with different cactus sources. However, I feel bad for someone getting goo and wanted to see if we could make the process more robust. Also, the simple TEK seemed to good to be true in general, but maybe it is if done correctly.
It is believed that the clearer solvent will have more reuses, but that is speculation. Perhaps washes after a standard extraction are a simpler way to maintain good reuse rate. Or maybe allowing an increasingly deep green color does not interfere at all.
Thanks for your experimental effort, report, and experienced point of view on this process.
Cheelin
Rising Star
Loveall, Shroombee, and all who have contributed:
Believe me, I mean no disrespect to you or your efforts. And, I have read and believe I understand the wiki and this thread well enough to reasonably understand the intent behind the variations and your attempts to make the tek as robust as possible.
On the other hand, chemical manipulation is almost by definition dependent on proper technique, and humans, almost by definition are resistant to following instructions, especially if they have a lot of options. The people who are having problems with this tek, need to stick to the basics and work it till they get it right. The people who already have it nailed already have mastered the required skills, and seem to think that an additional step here and there will overcome the root cause of disappointing results.
I’ll leave it there.
Believe me, I mean no disrespect to you or your efforts. And, I have read and believe I understand the wiki and this thread well enough to reasonably understand the intent behind the variations and your attempts to make the tek as robust as possible.
On the other hand, chemical manipulation is almost by definition dependent on proper technique, and humans, almost by definition are resistant to following instructions, especially if they have a lot of options. The people who are having problems with this tek, need to stick to the basics and work it till they get it right. The people who already have it nailed already have mastered the required skills, and seem to think that an additional step here and there will overcome the root cause of disappointing results.
I’ll leave it there.
highlightprotein
Rising Star
Cheelin said:
I measured out 50g of EA, placed it in the corner of a zip lock and placed it in a mason jar for half an hour. I poured off 50g of EA, so it seems like the EA is not dissolving the zip lock bag, as it weighs the same. In addition the zip lock appears to look and feel the same as it did before. [Edit] I'm actually not sure about the feel. The part of the ziplock back that stored the EA feels ever so less smooth than the other part of the zip lock back. I'm not sure if I am making this up or not.[/Edit].
Is this sufficient for me to conclude it is safe to use a zip lock bag as a separatory funnel with EA?
I also like your idea to just freeze the jar and pour off the EA from the frozen water. But the zip lock would be nice if you wanted to first neutralize with sodium carbonate and follow it up with a brine wash all in the same day.
Cheelin
Rising Star
Please see attached. If i read it correctly EA is rated “S” with polyethylene. So, EA may be ok in a ziploc, in a pinch.
If not doing so already you can check if the 50g of EA evaporate cleanly without leaving plastic residue behind.
highlightprotein
Rising Star
Cheelin said:
Thanks for the find. One concern I have is that at least with the zip lock bag, it definitely feels "less smooth", even after a very short period of contact. Whether it is 5 seconds or 30 minutes, the part of the ziplock that was touched by the EA feels less smooth than the other parts. I have tenatively washed a gallon ziplock back with EA such that all the smoothness was removed, and I am now using the gallon ziplock as my separatory funnel.
Loveall said:
I'm evaporating it now and will check for residue.
BTW Loveall, I did a brine wash just now, and found that the weight of the brine did not increase. I.e., my H2O + NaCl mix originally weighed about 200g, and after mixing with my used EA for 5+ minutes on a stir plate, I separated the brine water from the EA via my ziplock bag, and it still weighed 200g. I would have thought that the brine would pull something out of the EA. Or at least pull out some water that was in the EA.
Does this mean my brine wash was ineffective?
I then dried with anhydrous magnesium sulphate, and was suprised to see that my magnesium sulphate turned green/yellow. After filtering the EA off, the magnesium sulphate had a strong EA smell. I then weighed my EA and found that I lost 50g of EA out of 460g EA.
It seems like drying with anhydrous magnesium sulphate resulted in a significant loss of EA.
Was the NaCl wash after a sodium carbonate wash? You may have found that a brine wash is not needed. Did the brine not pickup any green color? I was hoping it would, chlorophyll has been reported to move into brine.
I have found that a sodium carbonate EA wash is enough to reuse the solvent. It is necessary to remove left over citric.
I have found that a sodium carbonate EA wash is enough to reuse the solvent. It is necessary to remove left over citric.
highlightprotein
Rising Star
I first washed with sodium carbonate. I measured pH before (acidic) and after (neutral), however I was using some low quality pH strips that only show "very acidic", "acidic", "neutral", "basic", "very basic".
I then washed with brine. The brine had no color change that I could see.
I then dried with anhydrous magnesium sulphate, which turned green and seem to steal a lot of EA from me. Is that supposed to happen?
This is the first wash I've ever done with sodium carbonate, brine, and my first time drying anything with ahydrous magnesium sulphate... so it is possible I made some error along the way.
---
Cheelin, I just tried my first 5mg citric acid instead of 15mg based on your theory. I got very nice white needle crystals in my filter. It is much prettier to look at. I'm now evaporating the crystals that were stuck to the wall.
One thing I think I've noticed is that with 15mg citric acid I get this yellow coloring in the crystals that stick to the wall, which fresh EA rinses do not seem to remove. This time with the 5mg, I saw the yellow coloring but after a fresh EA rinse it seems to have all gone away. I'll confirm after this evaporation but it seems like it will not have any yellow.
Does anyone else notice this? More citric acid yields more yellow?
I then washed with brine. The brine had no color change that I could see.
I then dried with anhydrous magnesium sulphate, which turned green and seem to steal a lot of EA from me. Is that supposed to happen?
This is the first wash I've ever done with sodium carbonate, brine, and my first time drying anything with ahydrous magnesium sulphate... so it is possible I made some error along the way.
---
Cheelin, I just tried my first 5mg citric acid instead of 15mg based on your theory. I got very nice white needle crystals in my filter. It is much prettier to look at. I'm now evaporating the crystals that were stuck to the wall.
One thing I think I've noticed is that with 15mg citric acid I get this yellow coloring in the crystals that stick to the wall, which fresh EA rinses do not seem to remove. This time with the 5mg, I saw the yellow coloring but after a fresh EA rinse it seems to have all gone away. I'll confirm after this evaporation but it seems like it will not have any yellow.
Does anyone else notice this? More citric acid yields more yellow?
Cheelin
Rising Star
Very nice HLP!
If you can get the crystals/needles into the filter, fresh EA is very effective at washing the color out. If you can’t get the crystals into the filter, fresh EA in the jar will still separate the crystals from the colored molecules, but you won’t be able to get all of the colored crap out of the jar, so what dries in there with the crystals will end up in the wash water, and will dry sticky and colored.
You can try to wash the dried stuff again through filter within fresh EA, but unless you can powder it, it is very difficult to get the offending molecules to separate from the desired product. So, you either have to have very clean pulled solvent, or big enough crystals, so that there is very little material that needs to be water washed.
[For now i’m sticking with my theory that excess citric is causing other molecules to drop out of the pulled solvent (at least when the pulled solvent is not as clean as skilled operators can get it), causing the yellow-brown molecules to drop out with excess EA, which causes the colored, sticky-/goey-ness. If the paste has been mixed well, and the solvent has been pulled and filtered well before salting, these other molecules may not be in there in sufficient quantities to get dropped or noticed when excess citric is used.]
If you can get the crystals/needles into the filter, fresh EA is very effective at washing the color out. If you can’t get the crystals into the filter, fresh EA in the jar will still separate the crystals from the colored molecules, but you won’t be able to get all of the colored crap out of the jar, so what dries in there with the crystals will end up in the wash water, and will dry sticky and colored.
You can try to wash the dried stuff again through filter within fresh EA, but unless you can powder it, it is very difficult to get the offending molecules to separate from the desired product. So, you either have to have very clean pulled solvent, or big enough crystals, so that there is very little material that needs to be water washed.
[For now i’m sticking with my theory that excess citric is causing other molecules to drop out of the pulled solvent (at least when the pulled solvent is not as clean as skilled operators can get it), causing the yellow-brown molecules to drop out with excess EA, which causes the colored, sticky-/goey-ness. If the paste has been mixed well, and the solvent has been pulled and filtered well before salting, these other molecules may not be in there in sufficient quantities to get dropped or noticed when excess citric is used.]
highlightprotein
Rising Star
Cheelin said:
I just evaporated the crystals that were stuck in my mason jar, and unfortunately they evaporated to a color I can't quite put a name too, some kind of very light brown/yellow mix I suppose. These crystals were sticky and kind of a pain to scrape up.
They are also very dense. The white needle crystals look like a larger quantity by eyeball, but on my scale the light brown/yellow crystals weigh twice as much.
At this point I'm just happy to be getting some crystals. But as I get better I would hope to consistently get dank white crystals that are not so sticky. Or perhaps I could put some effort in to further purify the brown/yellow crystals if I do get them.
HLP, that's interesting, congrats on the xtals. I was thinking of your microwave clumps. They could be a sign that your starting paste was not mixed enough or that it was too wet (or just different). Maybe you can double your paste mixing, really get into it. Make sure the texture stops changing and you end up with an airy souffle. I know I said guacamole texture was fine, but now I worry that may be a little too wet. Perhaps your powder needs less starting water.
Solvent absorption by the drying agent is normal. The less excess drying agent you use the less of an issue. However, I have found that I don't need to dry the EA for reuse. But again, I have the feeling that my paste is dryer than yours.
Cheelin, I've washed several different used EA batches with starting pH paper color anywhere from orange to red (6 to 2 pH I would guess). After a sodium carbonate wash they all become neutral and bubbles stop forming.
Perhaps asking for less starting water and deviating from 69ron's ratios could make the TEK more robust. Maybe we should insist on the paste texture and not on the specific water amount.
I've learned something like this by making churros. The water/flour mix needs to have a very specific consistency. The secret is to poke the dough with a knife. It needs to leave a "peak" behind. Too wet, and it falls over, too dry and it never forms. Here is the kikker: you cannot use a universal water measurement. Different flour brands (and even different bags of the same brand) need a different amount of water. With practice getting the right consistency becomes easy. If this happens with flour, with modern wheat having very uniform genetics, growing conditions, and milling process, it could also be the case for cacti and their varied genetics, growing conditions, powder prep, etc.
I'll poke my next ideal cactus paste and see what happens. I think I'm going to try less water and less citric acid, see if I get larger xtals that are less sticky.
Solvent absorption by the drying agent is normal. The less excess drying agent you use the less of an issue. However, I have found that I don't need to dry the EA for reuse. But again, I have the feeling that my paste is dryer than yours.
Cheelin, I've washed several different used EA batches with starting pH paper color anywhere from orange to red (6 to 2 pH I would guess). After a sodium carbonate wash they all become neutral and bubbles stop forming.
Perhaps asking for less starting water and deviating from 69ron's ratios could make the TEK more robust. Maybe we should insist on the paste texture and not on the specific water amount.
I've learned something like this by making churros. The water/flour mix needs to have a very specific consistency. The secret is to poke the dough with a knife. It needs to leave a "peak" behind. Too wet, and it falls over, too dry and it never forms. Here is the kikker: you cannot use a universal water measurement. Different flour brands (and even different bags of the same brand) need a different amount of water. With practice getting the right consistency becomes easy. If this happens with flour, with modern wheat having very uniform genetics, growing conditions, and milling process, it could also be the case for cacti and their varied genetics, growing conditions, powder prep, etc.
I'll poke my next ideal cactus paste and see what happens. I think I'm going to try less water and less citric acid, see if I get larger xtals that are less sticky.
Cheelin
Rising Star
HLP,
Put that brown sticky crap in a small jar/beaker, the smaller the better. Add some fresh EA, and mix it as well as you can. See if you can liquify the colored stuff, then pour it into the filter and see if you can wash it some more, then let the filter and its contents dry, then warm water wash through the original filter & evap again. If you are successful in washing the color out, your residue will be lighter colored, drier/less sticky, and significantly lighter weight.
If you see this brown, sticky forming in the future, as soon as the water is evaporated, scrape it up and do the process above, I think it’s easier to separate the goo from the end product before they start hardening.
To tag along on Loveall’s paste making suggestions, consider: after powdering your cactus as fine as possible, stick it in your dehydrator at 160-165F to dry until its weight doesn’t change (securely cover it with paper/paper towel so it doesn’t blow around). Then do what Shroombee mentioned, mix well the pickling lime and the powder before adding the water.
When you get those balls/chunks in your paste, mash them until the entire paste is the same consistency and color, uniformity of color and consistency is your friend.
Put that brown sticky crap in a small jar/beaker, the smaller the better. Add some fresh EA, and mix it as well as you can. See if you can liquify the colored stuff, then pour it into the filter and see if you can wash it some more, then let the filter and its contents dry, then warm water wash through the original filter & evap again. If you are successful in washing the color out, your residue will be lighter colored, drier/less sticky, and significantly lighter weight.
If you see this brown, sticky forming in the future, as soon as the water is evaporated, scrape it up and do the process above, I think it’s easier to separate the goo from the end product before they start hardening.
To tag along on Loveall’s paste making suggestions, consider: after powdering your cactus as fine as possible, stick it in your dehydrator at 160-165F to dry until its weight doesn’t change (securely cover it with paper/paper towel so it doesn’t blow around). Then do what Shroombee mentioned, mix well the pickling lime and the powder before adding the water.
When you get those balls/chunks in your paste, mash them until the entire paste is the same consistency and color, uniformity of color and consistency is your friend.
highlightprotein
Rising Star
Thanks Loveall and Cheelin, I'll try them out.
Regarding the ziplock bag test, I evaporated the EA as suggested by Loveall, and this left a definite residue, which is unfortunate.
However, my theory is that the inside of the ziplock contains some kind of coating which is immediately dissolved by the EA. I believe that if you thoroughly was the inside of the zip lock bag with EA and throw it out, that subsequently you can add EA to the zip lock bag without any issue.
I'll test it out today by adding some more EA and evaporating.
Regarding the ziplock bag test, I evaporated the EA as suggested by Loveall, and this left a definite residue, which is unfortunate.
However, my theory is that the inside of the ziplock contains some kind of coating which is immediately dissolved by the EA. I believe that if you thoroughly was the inside of the zip lock bag with EA and throw it out, that subsequently you can add EA to the zip lock bag without any issue.
I'll test it out today by adding some more EA and evaporating.
Cheelin said:
Yeah, I would invest in a separatory funnel HLP. You can get a good borosilicate glass one for less than $50 and it will last.
downwardsfromzero
Boundary condition
The hydrocarbons in the plastic are (in this instance) practically inert. The problem here is the plasticizers that are used to keep the plastic film flexible. Those are what are dissolving in the EA, and many of them have hormone-disrupting properties. A further undesirable complication is that once the surface of the plastic has been leached of plasticiser it becomes brittle and starts shedding microplastic fragments, so the rinsing method will just lead to a different type of problem.Cheelin said: