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TEK Ethyl acetate approach [CIELO]
- Thread starter Loveall
- Start date
This topic contain a TEK
Cheelin
Rising Star
Doubledog, I was wondering about activated charcoal. Some questions, please:
What is it doing for you, color removal? Anything else?
Assuming it doesn’t neutralize pH, would you neutralize pH then remove color, or vice versa?
If a two-step process, is filtering between steps better or not?
What size AC particles are you using?
Thanks
Chemists, for future reference, this might be something to experiment with adding into tek, to remove unwanted molecules from green solvent, prior to salting.
What is it doing for you, color removal? Anything else?
Assuming it doesn’t neutralize pH, would you neutralize pH then remove color, or vice versa?
If a two-step process, is filtering between steps better or not?
What size AC particles are you using?
Thanks
Chemists, for future reference, this might be something to experiment with adding into tek, to remove unwanted molecules from green solvent, prior to salting.
doubledog
Established member
I have never used it for EA, only for xylene, so it is just speculation from my side.
It removes mainly color from the solvent, it seems much cleaner after such treatment.
I would neutralize solvent before adding charcoal, but probably it doesn't really matter.
Filtering is always last step of the cleaning procedure for me, so my proposal for EA would be:
1. wash with slightly basic water (washing and neutralizing), separate water.
2. Drying (probably with calcium chloride) and cleaning with charcoal.
3. Filter to remove CaCl and charcoal (through cotton)
It removes mainly color from the solvent, it seems much cleaner after such treatment.
I would neutralize solvent before adding charcoal, but probably it doesn't really matter.
Filtering is always last step of the cleaning procedure for me, so my proposal for EA would be:
1. wash with slightly basic water (washing and neutralizing), separate water.
2. Drying (probably with calcium chloride) and cleaning with charcoal.
3. Filter to remove CaCl and charcoal (through cotton)
Cheelin said:
I believe this has been tried in other situations (DMT) and product was absorbed by the charcoal.
Doubledog said:
I tried activated charcoal (pellets from the aquarium store), and yes, they removed the color in EA. It took a long time (~week). The issue I ran into was the pellets released this very fine powder that was very difficult to filter out, but I didn't try cotton. Also, they were not cheap the EA can have a LOT of color to remove. If someone gets good results I'd be interested.
I don't dry EA before reuse, just neutralize it with saturated washing soda water which both neutralizes and I think dries it a little bit. It's going into a wet paste, and I found that was good enough (but I mainly reused EA from microwaved paste, which it seems we are moving away from).
doubledog
Established member
Loveall said:
Yes, it should not be used before salting, as it will absorb some alkaloid. AC could probably help only with accumulating of chlorophyll in used solvent.
Loveall said:
I know what you are talking about fine powder. In my experience, only cotton is able to filter it.
Using of AC is definitely not perfect method for such strongly coloured solvent as EA could be.
Drying is mainly cosmetic procedure, I mentioned it just because drying agent could be added at the same time as AC.
Cheelin
Rising Star
AC powder is a PITA to work with, especially cleaning up containers/equip after use…but, i’m gonna see if i can source something in between powder and pellets, check out filters, then do some testing.
Short of chems, molecular seives, distilling; using tek’s reclaim method and my freezer, did a great job neutralizing pH, clearing solvent, and removing free water; leaving a temporarily solid puck of crap at the bottom of the jar, for easy decanting. Maybe some magnetic stirring w AC will help decolorize.
Solvent cleaning & reuse testing is next up on my agenda.
Short of chems, molecular seives, distilling; using tek’s reclaim method and my freezer, did a great job neutralizing pH, clearing solvent, and removing free water; leaving a temporarily solid puck of crap at the bottom of the jar, for easy decanting. Maybe some magnetic stirring w AC will help decolorize.
Solvent cleaning & reuse testing is next up on my agenda.
downwardsfromzero
Boundary condition
Fine AC particulates are typically filtered out through a bed of diatomaceous earth. This does a better job than the filter paper below it, or spares clogging up a frit.
The min water paste yielded 1.1% of mescaline citrate xtals (I usually get ~1.4% with this powder) and produced the darkest, greenest EA I have seen.
Where's the rest? I pulled the spent paste (that is a sticky blob at this point) and significant product is coming through.
Therefore, I preliminarily conclude that min water is not ideal. Not sure why. Maybe a little extra water helps transport the mescaline into EA, or maybe something else.
I still want to try to set the water amount relative to the paste texture to make the process more repeatable. The point at which the min water paste forms could be used as a standard reference. Next, I'm going to try min water paste, and then add 50ml of water. Idea is to keep water low, but have enough so the mescaline flows freely.
The very dark color is interesting. I think calcium carbonate with more water in the standard tek is breaking down some of the chlorophyll. Also, there is this from an old patent (attached).
So instead of the microwave (which is now questionable for lowering yields slightly). Perhaps placing the french press in a hot water bath for a few hours will result in a cleaner EA extract deeply tinted with chlorophyll. I'll try this also.
Where's the rest? I pulled the spent paste (that is a sticky blob at this point) and significant product is coming through.
Therefore, I preliminarily conclude that min water is not ideal. Not sure why. Maybe a little extra water helps transport the mescaline into EA, or maybe something else.
I still want to try to set the water amount relative to the paste texture to make the process more repeatable. The point at which the min water paste forms could be used as a standard reference. Next, I'm going to try min water paste, and then add 50ml of water. Idea is to keep water low, but have enough so the mescaline flows freely.
The very dark color is interesting. I think calcium carbonate with more water in the standard tek is breaking down some of the chlorophyll. Also, there is this from an old patent (attached).
old attached patent said:
So instead of the microwave (which is now questionable for lowering yields slightly). Perhaps placing the french press in a hot water bath for a few hours will result in a cleaner EA extract deeply tinted with chlorophyll. I'll try this also.
Loveall, remind me again what was the results when you tried a chemical dry?
I just went over some of my old notes chemical dry didn't change the result with the microwave method (minor difference). But it might if a large amount of excess water is present. I have also noted previously excess water stopped citrate crashing out. This was noted on my first run when i added water to the paste because it absorbed too much EA and I thought i was over dry. Citrate didn't crash out until after excess water was removed.
But there might be a decent margin of error to work within here. As in some water is fine excess may not be. However this does not seem to be quite inline with what you're reporting.
I would also like to add in my test run, warmer pulls with french press and EA in a hot water bath yields a bit more but from my experience yielded dark crystals (this was also preformed with a microwave step and more citric acid was used 15-20mg for memory). I had a quick look on some old posts and I don't think I posted that observation up.
I think if you are using passive salting (5)mg then the crystal color may be corrected for warm pulls. Keen to hear your findings if you use a warm bath.
I looked at some early posts and you mentioned something similar crystals very a darker color with warm pulls and didn't form larger crystals but I couldn't find if you recorded yield difference.
I just went over some of my old notes chemical dry didn't change the result with the microwave method (minor difference). But it might if a large amount of excess water is present. I have also noted previously excess water stopped citrate crashing out. This was noted on my first run when i added water to the paste because it absorbed too much EA and I thought i was over dry. Citrate didn't crash out until after excess water was removed.
But there might be a decent margin of error to work within here. As in some water is fine excess may not be. However this does not seem to be quite inline with what you're reporting.
I would also like to add in my test run, warmer pulls with french press and EA in a hot water bath yields a bit more but from my experience yielded dark crystals (this was also preformed with a microwave step and more citric acid was used 15-20mg for memory). I had a quick look on some old posts and I don't think I posted that observation up.
I think if you are using passive salting (5)mg then the crystal color may be corrected for warm pulls. Keen to hear your findings if you use a warm bath.
I looked at some early posts and you mentioned something similar crystals very a darker color with warm pulls and didn't form larger crystals but I couldn't find if you recorded yield difference.
_Trip_ said:
Chemical dry: No change to yields, just added extra work for me. Agree it could help recover from too much water if that issue is present, but we want to try avoid getting to that point by standardizing the paste.
What I'm seeing is that min water (222g for me) was not ideal. 300g seems great for me. There is a margin there it seems. Above 300g there would be a risk of issues for me based on your observations. That's why I'm suggesting as possible general method to get to a mim water paste, them add 50g of water. That approach may give consistent results for many people.
Agree, warm EA pulls made everything darker. Also, I saw no yield increase. Now, I'm suggesting to warm the paste by itself before the pulls to break down the chlorophyll. Then, do room temp pulls. It's a gentler alternative to the microwave to keep the EA from setting dark.
Yes, I to 5mg/ml slow diffusion citric salting.
To summarize, next test for me is:
- Paste: make min water paste, then add 50g of water
- "degreening" step: Hot water bath. See if color goes from green to brown per the old patent
- Cool paste to room temp
- Do pulls as usual, goal is to get white xtals with good yields and EA with a light color that should be easily reusable
Cheelin
Rising Star
Here is a representative example of the paste from a wet mix (water + lime, then material), using the standard process, recipe, and my mixing method.
1. Mix water and lime until milky.
2. Add approx 1/3 of material and incorporate with spoon mixing, becomes liquid slurry.
3. Add another 1/3 of material and incorporate with spoon mixing, liquid no longer visible.
4. Add final 1/3 of matetial and try to incorporate with spoon, “paste” is now too thick to mix (see 2nd pic below), push paste into a clump, press powder into clump with back of spoon, move clump to cover loose powder, press clump into powder until loose powder is all in the clump; then, using back of spoon, mash the clump completely, fold in half & mash completely, repeat until paste is uniform color and consistency with no visible powder, until 8 minutes have elapsed (see 3rd pic).
5. Let rest 10 minutes.
6. The paste becomes a soft, rubbery mass, with consistency somewhat like playdough (see 4th & 5th pics).
The following measurements were made as Shroombee requested in post 594.
Container (tare = 48.15g):
Volume capacity - 1/4 cup or 59mL
Net water weight - 59.20g
Net packed paste weight - 55.04g
Note: The paste was so rubbery that it was difficult to compact so that all airspace was eliminated on bottom side of paste/inside of container. The top of the material could not be smoothed even with top of container. I packed container the best I could, then sliced the top of paste even with container top, the excess material weighed 9.0g. When I removed paste from container, the paste held its packed shape, and I noticed areas that did not completely pack to the container walls. It is my estimate that the missing material at the bottom roughly equaled the amount of material I cut to make the top of the paste even with the top of the container. Adding the 9.0g to the rest of the material equals the 55.04g shown above.
I also took a 5.00g sample of the paste, and dried it in 5 x 30sec increments, on high setting, in the microwave. Dry weight was 1.44g.
With the standard paste, regardless of wet mix or dry mix variations, and using my method (break up paste into 1/2” chunks before 1st solvent addition; 6 pulls; 30mL solvent on 1st pull, pulls 2 through 6 have 22mL solvent; each pull having 1 minute spoon stir with 80 revolutions, 2 minutes rest, max squeeze of paste at end of last pull): the paste starts out stiff/rubbery, the pulled liquid dark colored and low volume, with each subsequent pull the paste becomes more slurry-like, the pulled liquid becomes slightly lighter colored and increases in volume; by the end of last pull, the paste looks like liquidy applesauce, solvent recovery exceeds 90%, and even with the big squeeze the filtered pulls are crystal clear (for the sake of these experiments I do filter twice more into a clean settling jar to rest 1 hr, then into crystallization jar before salting). For regular processing, I think filtering each pull into collection jar, letting that jar settle for an hour, then filtering into crystallization jar is sufficient, as long as the no particles/cloudiness is visible.
1. Mix water and lime until milky.
2. Add approx 1/3 of material and incorporate with spoon mixing, becomes liquid slurry.
3. Add another 1/3 of material and incorporate with spoon mixing, liquid no longer visible.
4. Add final 1/3 of matetial and try to incorporate with spoon, “paste” is now too thick to mix (see 2nd pic below), push paste into a clump, press powder into clump with back of spoon, move clump to cover loose powder, press clump into powder until loose powder is all in the clump; then, using back of spoon, mash the clump completely, fold in half & mash completely, repeat until paste is uniform color and consistency with no visible powder, until 8 minutes have elapsed (see 3rd pic).
5. Let rest 10 minutes.
6. The paste becomes a soft, rubbery mass, with consistency somewhat like playdough (see 4th & 5th pics).
The following measurements were made as Shroombee requested in post 594.
Container (tare = 48.15g):
Volume capacity - 1/4 cup or 59mL
Net water weight - 59.20g
Net packed paste weight - 55.04g
Note: The paste was so rubbery that it was difficult to compact so that all airspace was eliminated on bottom side of paste/inside of container. The top of the material could not be smoothed even with top of container. I packed container the best I could, then sliced the top of paste even with container top, the excess material weighed 9.0g. When I removed paste from container, the paste held its packed shape, and I noticed areas that did not completely pack to the container walls. It is my estimate that the missing material at the bottom roughly equaled the amount of material I cut to make the top of the paste even with the top of the container. Adding the 9.0g to the rest of the material equals the 55.04g shown above.
I also took a 5.00g sample of the paste, and dried it in 5 x 30sec increments, on high setting, in the microwave. Dry weight was 1.44g.
With the standard paste, regardless of wet mix or dry mix variations, and using my method (break up paste into 1/2” chunks before 1st solvent addition; 6 pulls; 30mL solvent on 1st pull, pulls 2 through 6 have 22mL solvent; each pull having 1 minute spoon stir with 80 revolutions, 2 minutes rest, max squeeze of paste at end of last pull): the paste starts out stiff/rubbery, the pulled liquid dark colored and low volume, with each subsequent pull the paste becomes more slurry-like, the pulled liquid becomes slightly lighter colored and increases in volume; by the end of last pull, the paste looks like liquidy applesauce, solvent recovery exceeds 90%, and even with the big squeeze the filtered pulls are crystal clear (for the sake of these experiments I do filter twice more into a clean settling jar to rest 1 hr, then into crystallization jar before salting). For regular processing, I think filtering each pull into collection jar, letting that jar settle for an hour, then filtering into crystallization jar is sufficient, as long as the no particles/cloudiness is visible.
Attachments
Thanks Cheelin. Your standard paste looks a little more compact than my standard paste - even though we both use the same amount of water (300g). I would need to use less water to match your paste for my starting material.
As we have been saying, I think this indicates that (1) there is a process window of paste consistency to get good results, and (2) fixing the amount of water introduces variability into the process (could be too wet for some), therefore, specifying the paste consistency (instead of the water amount) could make the TEK more robust for the general case.
The MC you measured is 1.44/5 ~ 29%, which is expected for the standard paste if starting with dry ingredients: 125/425 ~ 29%. I think this means that your starting cacti powder was dried properly.
As we have been saying, I think this indicates that (1) there is a process window of paste consistency to get good results, and (2) fixing the amount of water introduces variability into the process (could be too wet for some), therefore, specifying the paste consistency (instead of the water amount) could make the TEK more robust for the general case.
The MC you measured is 1.44/5 ~ 29%, which is expected for the standard paste if starting with dry ingredients: 125/425 ~ 29%. I think this means that your starting cacti powder was dried properly.
Cheelin
Rising Star
I would bet the moisture content of your powder is higher than mine (9-ish%), causing the difference in appearance. The lime is also slightly hygroscopic, mine is about 3% mc.
Since you and I both get clean white crystals, the 3:1 water to powder ratio looks robust enough, even with reasonable differences in powder & lime MC% (likely related to local temp and relative humidity conditions) and paste appearance. I think that water content and paste texture, within some reasonable range, are not whatever is causing any significant issue with crystal quality or yield. Perhaps powder source/preparation or just plain ole poor technique somewhere(s) in the entire process is causing an issue(s).
I have gone out of my way, to be as explicit as I can on how I do each step of the process. In hopes that, if someone is having a problem, they can, by following my directions carefully and completely, produce similar results as mine (which are now going on almost 40 consecutive small-scale runs of consistent results). If their results, after repeated attempts (there is a learning curve) using my method are substantially different, I can only conclude that powder source/prep and/or inability to follow directions is where the issue lies.
I think you should pat yourself on the back for coming up with, essentially, the best process in the first iteration you published!
Since you and I both get clean white crystals, the 3:1 water to powder ratio looks robust enough, even with reasonable differences in powder & lime MC% (likely related to local temp and relative humidity conditions) and paste appearance. I think that water content and paste texture, within some reasonable range, are not whatever is causing any significant issue with crystal quality or yield. Perhaps powder source/preparation or just plain ole poor technique somewhere(s) in the entire process is causing an issue(s).
I have gone out of my way, to be as explicit as I can on how I do each step of the process. In hopes that, if someone is having a problem, they can, by following my directions carefully and completely, produce similar results as mine (which are now going on almost 40 consecutive small-scale runs of consistent results). If their results, after repeated attempts (there is a learning curve) using my method are substantially different, I can only conclude that powder source/prep and/or inability to follow directions is where the issue lies.
I think you should pat yourself on the back for coming up with, essentially, the best process in the first iteration you published!
highlightprotein
Rising Star
Well this is disappointing:
My experiment was with a new cactus, Peruvian Torch, and I made the 69ron paste from 200g of torch powder. I split the paste in half. On one half I extracted with room temperature EA. On the second half I extracted with chilled EA.
72 hours after dropping citric acid, I decanted and ... found no crystals in the filter. I moreover found very little material stuck to the jars. I'll evaporate them but I'm sure it will not be very much.
I'm not sure if this Peruvian Torch just contains really low actives or if perhaps my attempt to scale to 200g of paste resulted in some kind of issue. Previously I've only done 40g at a time. These cuttings I bought were really beautiful, which made me kind of think they would have a big yield. The same vendor's San Pedro net me about 1% in my last extraction. I was under the impression Peruvian Torch was supposed to be stronger.
It's unfortunate because I think I did my best job so far during these extractions in terms of paste making and purposeful processing. I was also counting on this batch to hold me over through the next two weeks.
I still have 200g of this Peruvian Torch powder. I think I'll do a few 50g batches. I'll also add more citric acid to the spent EA from the current batch in the event anything else materializes.
Edit: I added an additional 20mg/g of citric acid to the EA but saw 0 clouds forming. I'll let it wait 48 hours for fun.
My experiment was with a new cactus, Peruvian Torch, and I made the 69ron paste from 200g of torch powder. I split the paste in half. On one half I extracted with room temperature EA. On the second half I extracted with chilled EA.
72 hours after dropping citric acid, I decanted and ... found no crystals in the filter. I moreover found very little material stuck to the jars. I'll evaporate them but I'm sure it will not be very much.
I'm not sure if this Peruvian Torch just contains really low actives or if perhaps my attempt to scale to 200g of paste resulted in some kind of issue. Previously I've only done 40g at a time. These cuttings I bought were really beautiful, which made me kind of think they would have a big yield. The same vendor's San Pedro net me about 1% in my last extraction. I was under the impression Peruvian Torch was supposed to be stronger.
It's unfortunate because I think I did my best job so far during these extractions in terms of paste making and purposeful processing. I was also counting on this batch to hold me over through the next two weeks.
I still have 200g of this Peruvian Torch powder. I think I'll do a few 50g batches. I'll also add more citric acid to the spent EA from the current batch in the event anything else materializes.
Edit: I added an additional 20mg/g of citric acid to the EA but saw 0 clouds forming. I'll let it wait 48 hours for fun.
highlightprotein
Rising Star
I have just finished evaporating, and I think I have set the world record for the worst cacti extraction ever: 0.140g of mescaline citrate from 200g of cactus powder- 0.07% yield.
I don't think that it's possible for peruvian torch to be this low yielding. The only other thing I can think of is that I made some error while scaling to 200g. I will retry with 50g.
These peruvian torch cuttings were really beautiful. They were extremely thick with nice spines. I feel kind of bad for cutting them up instead of planting them somewhere.
I don't think that it's possible for peruvian torch to be this low yielding. The only other thing I can think of is that I made some error while scaling to 200g. I will retry with 50g.
These peruvian torch cuttings were really beautiful. They were extremely thick with nice spines. I feel kind of bad for cutting them up instead of planting them somewhere.
Cheelin, I agree the process seems to work a wide range of paste consistency. Does not look seem like that variation is a likely issue. I think my cactus powder is essentially dry, but I'll verify. What does 1/4 cup of your dry powder weigh?
Shroombee, this paste weight in at 60g per 1/4 cup (same density as water
)
Good news so far: Pulls where a light yellow color, very easy to see through (looks like pee). Huge difference vs. the standard paste. Hope the rest of the extraction goes well, because this is a minimal amount of extra work. Theory is that chlorophyll was saponified in the hot alkaline environment (in agreement with the algae patent in the previous post).
I put the filtered EA extract in the fridge to settle, and to my surprise it clouded a bit when cold. Sticky white precipitate is crashing. Plan to decant that off and set aside.
Will report back after I try to xtalize this.
So in practice I deviated from this. Instead of a hot water bath, I simply poured boiling water (270ml) into the cactus/lime powder and mixed well. I let that cool and it set into a gelatenous paste (surprising), which I loosened up with another 30ml of boiling water water, ending back at 69ron's ratio.Loveall said:
Shroombee, this paste weight in at 60g per 1/4 cup (same density as water
)Good news so far: Pulls where a light yellow color, very easy to see through (looks like pee). Huge difference vs. the standard paste. Hope the rest of the extraction goes well, because this is a minimal amount of extra work. Theory is that chlorophyll was saponified in the hot alkaline environment (in agreement with the algae patent in the previous post).
I put the filtered EA extract in the fridge to settle, and to my surprise it clouded a bit when cold. Sticky white precipitate is crashing. Plan to decant that off and set aside.
Will report back after I try to xtalize this.