TEK Ethyl acetate approach [CIELO]

[grollum]

Possible ways of lowering water content to make the process more robust:

1) Add 100g of NaCl (or 33% vs water) to the paste before pulling, the water content should drop from 3.4% to 1.9%.
2) Adding 150g of CaCl2 to the paste (or 50% vs water). Water content should drop even more.
3) After the pull, chemically dry the extract with excess CaCl2 pellets. That should remove almost all the water (and water soluble stuff that could stop crystalization). The pellet dry can be done quickly (15 minutes or so).

I plan on testing 3) again soon. I did it earlier (and shroombee too), but that was before understand quick pulls help. 1) and 2) change the paste and I'm reluctant to re-visit that because I really like how well the paste is pulled as-is. Also, 3) is a "standard" general lab step where solvents are dried after pulling and before salting - perhaps it was a mistake to remove it despite early good results in some examples.

Other drying agents could be used. Just FYI that in my case MgSO4 was difficult to filter/decant from ethyl acetate so I prefer CaCl2 pellets (anhydrous).

I am looking forward to your test and your suggestions. I like to try one of the ways in my next try. If more people have problems like me and metta-morpheus this could be a necessary addition again.

Since I have this sticky citric acid paste I dehydrated from my first try. Would it be a good Idea to dissolve it in fresh Ethylacetate? Since there is no water left it might provoke xtalization in fresh Ethylacetate if there is something interesting in there.
I just tasted a finger dip of the sticky stuff and it tasted like only citric acid.

 

[Loveall]

grollum, this is what I would do:

First attempt (dried sticky stuff): I think hat crashed has some mescaline citrate along with some citric acid and maybe some plant stuff. I would dissolve in a small amount of water (~3 ml).Then add 200g of ethyl acetate. The idea of trying again with fresh ethyl acetate is to isolate the mescaline citrate in a cleaner environment with less stuff getting in the way of xtalization.

Second attempt: Cloudiness not setting well after 4.5g of citric acid added as I understand it. I would add more acid in 4.5g increments. The cloudiness should go away completely and whatever crashes should be active. The idea here is to force mescaline citrate to crash by overloading the system with citric. You can test on a small sample. I think in your first attempt you may have stopped a little early, keep on adding citric until clear, like Metta-Morpheus did in his last attempt.

I think adding more citric acid cannot make the solution clear unless mescaline citrate is crashing. So I would keep on going until clear.

I have seen transparent sticky stuff on the wall. It turns out to be what I think is Mescaline citrate xtals every time after washing in fresh ethyl acetate until color is gone and drying them slowly from water. If dried in the oven at 175F it becomes a thin film that scrapes up to tiny xtals.

 

[Loveall]

Possible ways of lowering water content to make the process more robust:

1) Add 100g of NaCl (or 33% vs water) to the paste before pulling, the water content should drop from 3.4% to 1.9%.
2) Adding 150g of CaCl2 to the paste (or 50% vs water). Water content should drop even more.
3) After the pull, chemically dry the extract with excess CaCl2 pellets. That should remove almost all the water (and water soluble stuff that could stop crystalization). The pellet dry can be done quickly (15 minutes or so).

So I tried 3). It took longer than 15 minutes to dry, there was a lot of water in the pulls. Had to add 75g of CaCl2 to form a solid block without any water layers.

Decanted this dried ethyl and added 5 mg/g of citric. It behaves very differently:

- Citric acid goes into solution very slowly. Takes forever to dissolve. Some citric seems resistant to go into solution. DWZ, perhaps the anhydrous citric acid solubility is closer to your butyl acetate value.
- Instead of initial clouds, a fine glitter forms (see image). No wall sticking. Unfortunately the glitter becomes clouds that sink to the bottom and remain wispy, not xtalizeling after a few hours (didn't test longer). pH paper is not acidic, it doesn't change color.
- Adding a few ml of water turns the wispy clouds into xtals. Also, all the citric acid granules go into solution. pH paper is red/acidic.

So the chemichal dry needed water re-introdiced to induce quick xtalization. Interesting. It was not much, about ~5ml of water in 600g of solvent seemed enough. But it was very important in this test.

One can imagine that too much water will be bad also with a lot of plant stuff staying in solution and interfering with xtalization (along with the water itself). Perhaps enough citric could overcome any excess water, I think Metta-Morpheus got that result in his last test.

I think we should reduce the water in the pulls by increasing the ionic strength of the paste to see if our crashing results converge better. We should also describe carefully how we pull, make sure it is the same.

I'm going to try 1) next since DMZ has brought up a concern for CaCl2 (and everyone has table salt at home). Water will be present, but in lower ammount than the process without NaCl. It could help with more consistent results. I'll report on the paste consistency, hopefully NaCl does not cause issues. I will also mix gently and give 5 minutes without mixing so water-ethyl acetate are closer to equilibrium. I did a test simulating a pull with more aggressive mixing, almost no rest time, and aggressive squeezing. Leaving the pull alone for a while resulted in droplets forming, indicating that the more aggressive pull carried excess water which could cause issues.

Attached is the info for water/NaCl/ehtyl acetat. What it says is:

- Water/Ethyl-acetate only: Water later has 7.1% solvent, and solvent layer has 3.4% water (current TEK, but could be more water if not fully at equilibrium, also plant stuff and lime could change this equilibrium point - this is just a first order estimate for our purposes).
- Water/Ethyl-acetate/Saturated NaCl: Water layer has 0.71% solvent (10x less) and solvent layer has 1.86% water (about half as much as before). NaCl in the solvent is very small and non important for our purposes (0.00028%, or 2mg in 700g).

 

[shroombee]

Citric acid goes into solution very slowly. Takes forever to dissolve. Some citric seems resistant to go into solution. DWZ, perhaps the anhydrous citric acid solubility is closer to your butyl acetate value.

This is what I observed when testing solubility of anhydrous citric acid in my anhydrous ethyl acetate. The grains do not dissolve unless I crush them or use the magnetic stirrer.

Loveall, you observed when adding your citric acid to fresh ethyl acetate that the grains dissolve easily?

 

[Loveall]

Citric acid goes into solution very slowly. Takes forever to dissolve. Some citric seems resistant to go into solution. DWZ, perhaps the anhydrous citric acid solubility is closer to your butyl acetate value.

This is what I observed when testing solubility of anhydrous citric acid in my anhydrous ethyl acetate. The grains do not dissolve unless I crush them or use the magnetic stirrer.

Loveall, you observed when adding your citric acid to fresh ethyl acetate that the grains dissolve easily?

Not sure if I watched fresh ehtyl acetate and citric acid that closely originally. I agree based on the latest test making the extract anhydrous that citric acid dissolve with difficulty in anhydrous ethyl acetate.

On the other hand, citric acid always dissolves very easily into the extract. That must be because we have water in it (~3.4%). Maybe the reason Metta-Morpheus was able to add (and needed) to add > 50mg/g was to overcome the presence of more water than us. Just a possibility.

I'm running the extraction with NaCl in the paste (after it is smooth and mixed with the lime water). Seemed to work fine. Right now there are crystals crashing in the fridge (1 hour after starting). The NaCl did make the paste more runny but the pulls worked fine (became sandy, etc).


If people have more water for whatever reason (pull technique, temperature, a certain cactus oil miscible in water and ethyl acetate, etc), adding NaCl to the paste may help reduce that potential problem.

 

[shroombee]

On the other hand, citric acid always dissolves very easily into the extract.

I have not observed this in my extracts. The citric acid does not dissolve easily. The grains will spin around at the bottom of the jar while using the magnetic stirrer. It takes a few minutes for most of the grains to dissolve and the reason why I've stirred beyond 5 minutes is to ensure it's all dissolved.

Metta-morpheus and grollum: how long does it take for the citric acid grains to dissolve into your extracts?

 

[Loveall]

On the other hand, citric acid always dissolves very easily into the extract.

I have not observed this in my extracts. The citric acid does not dissolve easily. The grains will spin around at the bottom of the jar while using the magnetic stirrer. It takes a few minutes for most of the grains to dissolve and the reason why I've stirred beyond 5 minutes is to ensure it's all dissolved.

Metta-morpheus and grollum: how long does it take for the citric acid grains to dissolve into your extracts?

I shake. It dissolves in a few minutes in the extract. I call this easy. It is a lot more slow to dissolve in anhydrous ethyl acetate vs extract in my case.

 

[shroombee]

I shake. It dissolves in a few minutes in the extract. I call this easy. It is a lot more slow to dissolve in anhydrous ethyl acetate vs extract in my case.

Interesting that we seem to have a difference there. For me anhydrous ethyl acetate versus extract seems to be about the same - at least a few minutes with the magnetic stirrer either way.

I've got some shroomery to take care of, and then will get back to running cactus experiments.

 

[metta-morpheus]

The citric takes at least 5 minutes to dissolve, with magnetic stirrer. I have to force myself to wait, as the grains kinda clump together at first, and start to change shape. It gives me a fake out of what I think is goodies, but if I wait longer it dissolves.

My wife and I will be testing this weekend. I’ve never done extracted mescaline, only resin tek 3 times, so I won’t have much of a reference for purity. I will be able to base it off of the fact I kept the crystal of a 100 gram extract separate, so we’re gonna split it and see if it feels like a 50 gram trip. It should be around 500 mg, as the final extract weighed 1.06. If I feel like something is active, I will resume some more tests next week. Otherwise I might look at another extraction tek or go back to resin.

 

[Loveall]

The citric takes at least 5 minutes to dissolve, with magnetic stirrer. I have to force myself to wait, as the grains kinda clump together at first, and start to change shape. It gives me a fake out of what I think is goodies, but if I wait longer it dissolves.

My wife and I will be testing this weekend. I’ve never done extracted mescaline, only resin tek 3 times, so I won’t have much of a reference for purity. I will be able to base it off of the fact I kept the crystal of a 100 gram extract separate, so we’re gonna split it and see if it feels like a 50 gram trip. It should be around 500 mg, as the final extract weighed 1.06. If I feel like something is active, I will resume some more tests next week. Otherwise I might look at another extraction tek or go back to resin.

Exciting. If it works you would have shown that by adding extra citric acid, mescaline citrate was forced out of solution in your example. I hope you guys have a great experience. Either way, thanks for your efforts on this experimental approach.

 

[grollum]

Metta-morpheus and grollum: how long does it take for the citric acid grains to dissolve into your extracts?

At first when adding only 3,5g it takes 5 minutes. The more I add the slower it gets until its sticking to the walls.

Yesterday I tried to dissolve the sticky resin I dried in the oven into new Ethylacetate without water. It subverted into small grainy sandy particles (maybe small needles?) which looked like the desired result. Since there were some bigger bits which didn't dissolve I added some water like loveall suggested. Around 5g to 400ml Ethylacetate. This destroyed the sandy stuff and created a sticky resin an the bottom and walls again.

Will collect everything with filtering and water pulls, grind it and try to dissolve a last time into fresh Ethylacetate without water.


How much NaCl would you suggest to add to the paste Loveall for reducing water?

 

[Loveall]

Metta-morpheus and grollum: how long does it take for the citric acid grains to dissolve into your extracts?

At first when adding only 3,5g it takes 5 minutes. The more I add the slower it gets until its sticking to the walls.

Yesterday I tried to dissolve the sticky resin I dried in the oven into new Ethylacetate without water. It subverted into small grainy sandy particles (maybe small needles?) which looked like the desired result. Since there were some bigger bits which didn't dissolve I added some water like loveall suggested. Around 5g to 400ml Ethylacetate. This destroyed the sandy stuff and created a sticky resin an the bottom and walls again.

Will collect everything with filtering and water pulls, grind it and try to dissolve a last time into fresh Ethylacetate without water.


How much NaCl would you suggest to add to the paste Loveall for reducing water?

I think that sandy stuff may be the product indeed. I suggest you add citric acid to the 400ml of ehtyl acetate after filtering to make sure no product dissolved with the water added.

Is the sticky stuff really a resin? What sticks to the walls is xtaline for me (it can look transparent though, but it is solid, see image bellow). I rinse it with a few ml of fresh ethyl acetate, and a bunch of it, but not all, comes off the walls during rinsing so I can move it to the filter.

I'm using 33% of NaCl with respect to water. For example, since I used 300g of water, I added 100g of NaCl. The result looks similar to no salt, but the extract was greener, xtalized more slowly, and the product is a little tan (instead of white). Not sure if adding NaCl would help you. After seeing the results I'm not sure this is an improvement.

Instead, I think we should be carefully with the pulls. Mix lightly, squeezing gently (if at all), gravity filtration only, and at least 5 minutes of complete rest (I use 5) before decanting through a filter. Let the combined pulls rest for for 10 minutes or until clear, check bottom with a flashlight for any droplets or particles and remove those before salting. Then add enough citric acid until cloudiness dissapears. What sticks to the jar walls or precipitates as loose sand from the clouds is always product in my examples.

I don't know why some need more citric acid than others, but it seems that with enough of it, we can force the crashing of mescaline citrate. Metta-Morpheus and your results will really tell us if we have a process robust across multiple folks, seems like shroombee and I have been lucky so far.

I recommend that when you dry what warm water picks up from the sticky walls (you can add the sandy stuff to the warm water too) you dry slowly at room temp in a shallow dish. I always get needles this way. It takes a few days but it is worth the wait. This does not happen when drying from an oven.

Shroombee, what do you think helped improve your process. At the begining you did see some oil issues if I remember right. Was it more citric acid? More gentle pulls? Both? Thanks!

Edit: I've updated our experimental TEK based on our ongoing experiments - expanded the pull section to be more detailed.

 

[grollum]

Is the sticky stuff really a resin? What sticks to the walls is xtaline for me (it can look transparent though, but it is solid, see image bellow). I rinse it with a few ml of fresh ethyl acetate, and a bunch of it, but not all, comes off the walls during rinsing so I can move it to the filter.

I call it resin because it got slightly yellow from to much heat and looks like resin.
I tried to touch the transparent droplets on the wall of the jars and it was just a tiny tiny bit sticky but solid as you describe. It is missing the typical hard edged xtal structure. So I was confused. It looks like in your photo.

I'm using 33% of NaCl with respect to water. For example, since I used 300g of water, I added 100g of NaCl. The result looks similar to no salt, but the extract was greener, xtalized more slowly, and the product is a little tan (instead of white). Not sure if adding NaCl would help you. After seeing the results I'm not sure this is an improvement.

Will wait with this and first bioassay or let analyze.

I recommend that when you dry what warm water picks up from the sticky walls (you can add the sandy stuff to the warm water too) you dry slowly at room temp in a shallow dish. I always get needles this way. It takes a few days but it is worth the wait. This does not happen when drying from an oven.

I understand. Will try the slow way. What do you do to secure the liquid from collecting dust and other stuff during the days? Cover with some cloth?

 

[Loveall]

I understand. Will try the slow way. What do you do to secure the liquid from collecting dust and other stuff during the days? Cover with some cloth?

Yeah, a cloth is fine. If the room is clean I don't use anything.

One thing I always do with the stuff that sticks to the walls is to shake the jar with fresh ethyl acetate 2-3 times. A bunch of it falls off and floats as crystals that are caught easily in a filter. What doesn't fall off is what I pick up in warm water after letting the solvent dry for a few hours.

Good luck!

 

[shroombee]

The citric takes at least 5 minutes to dissolve, with magnetic stirrer. I have to force myself to wait, as the grains kinda clump together at first, and start to change shape. It gives me a fake out of what I think is goodies, but if I wait longer it dissolves.

This is interesting. My citric acid grains definitely do not clump together. They might pile up together at the corner of the jar, but they stay as separate grains that eventually dissolve. The citric grains are eventually interleaved with xtals that are forming and falling to the bottom, but it all stays separate. Looking like fluffy snow intermixed with hard grains of sand.

At first when adding only 3,5g it takes 5 minutes. The more I add the slower it gets until its sticking to the walls.

Sticking to walls sounds like xtals. At first I thought the citric grains were breaking up into smaller particles and just spinning around the solvent. And looking like the citric won't dissolve. But then I realized those particles were xtals!

Yesterday I tried to dissolve the sticky resin I dried in the oven into new Ethylacetate without water. It subverted into small grainy sandy particles (maybe small needles?) which looked like the desired result. Since there were some bigger bits which didn't dissolve I added some water like loveall suggested. Around 5g to 400ml Ethylacetate. This destroyed the sandy stuff and created a sticky resin an the bottom and walls again.

Agreeing with Loveall, I think the small grainy sandy particles were the desired result. I don't think water was needed at this point. Maybe just crush the bigger bits. And you could mix the whole thing for a few minutes to ensure any citric dissolves into the ethyl acetate. Then pour through a filter.

Then add enough citric acid until cloudiness dissapears. What sticks to the jar walls or precipitates as loose sand from the clouds is always product in my examples.

Shroombee, what do you think helped improve your process. At the begining you did see some oil issues if I remember right. Was it more citric acid? More gentle pulls? Both? Thanks!

Same with me - when adding citric, whatever precipitates as loose sand (or snow) or what sticks to the walls dries to xtals.

Key improvements:

- Quick (3 minute) pulls, very gently stirring the first 30 seconds. (Edit: Very gently stir 30 seconds of each pull). We have observed that longer pulls result in greener solvent, which we assume is stuff we don't want. Cactus also gets sticky the longer it has been in contact with ethyl acetate (after about 30-40 minutes), which DWZ conjectures is undesired reactions between the ethyl acetate and cactus;

- Bomb heavily with citric acid and mix vigorously. When I went light on citric and didn't mix, I got various results like oil droplets or water droplets, but no xtals. After letting those failed jars sit for a while, I bombed with citric and got some xtals, although less yield than a proper bombing and mixing from the onset;

I conjecture that if water is interfering with xtalization, another way to minimize its influence is to add fresh ethyl acetate to the extract before bombing with citric. It is not necessarily efficient use of the solvent, but for initially testing the hypothesis it may be a direction to consider. For those having difficulty, perhaps split the next run's combined pulls into 2-4 jars and salt them separately, trying different amounts of added fresh ethyl acetate before salting.

Yeah, a cloth is fine. If the room is clean I don't use anything.

I cover the dish using a paper towel, pulling enough length off the paper towel roll so it can be secured by wrapping under the dish.

 

[Loveall]

Thanks shroombee, I agree. Do you squeeze the paste (if yes, is it a gentle squeeze?) Or simply gravity filter. The pull technique is important. I think 3 minutes of rest after gentle mixing is a sweet spot because (1) it is long enough time for any stirred stuff (e.g. water droplets, small plant particles) to fall back into the paste and (2) it is short enough to not pick up a lot of soluble plant gunk which can interfere/slow crystalization.

At the end of the day, your quick crashing results are great

I think it is also important for workers to check the combined pulls for water drops and/or plant particles. These should be removed before salting or they could cause xtalization issues.

I've updated our tek to follow your approach shroombee. It simply gives the fastest/cleanest xtalization I have seen.

Also, want to report on other tests. This is for completeness, I don't see improved xtalization for any of these ideas (instead xtalization was worse).

1) 33% NaCl (vs plain water) in the paste: Paste broke down to a smoother paste and extract was darker than usual (more plant stuff). Xtalization was slower than usual and resulting precipitate had a slightly tan color. Slowly evaporating from water both the precipitate and what stuck to the wall after fresh ehtyl acetate washes resulted in tan needle xtals (not as white as usual, see tan image below). Yield did not change (1.1 %). In summary, this approach is not recommended as there is no benefit and oly downsides.

2) 45% CaCl2 (vs plain water) in the paste. Skipped, I don't plan to do this anymore

3) Drying extract with CaCl2 before salting: After salting, clouds settle towards the bottom but don't xtalize after waiting overnight. A small ammount of water (5ml in 700g) was added to partially undo the chemichal dry and the clouds did coalesce to xtals. However, only got 0.71% yield. DFZ mentioned yields could be lower because of the CaCl2 dry and that is what I saw

Something else that could make things better IF people are having issues even after following shroombee's excellent approach is cooling the paste/solvent in the fridge. Free base mescaline should still be easily soluble and we would get less water and plant stuff in the solvent (I think). Freezer temp for the solvent could also be considered (like we do for salvinorin extraction to minimize plant stuff). However, even if it makes things cleaner, I think it is overkill, we seem to be good at room temperature. Would be interesting to try if anyone follows the current tek to the letter but still has xtalization issues.

 

[downwardsfromzero]

cooling the paste/solvent in the fridge. Free base mescaline should still be easily soluble and we would get less water and plant stuff in the solvent (I think).

Isn't water's solubility in ethyl acetate retrograde, meaning more water will be present at fridge temperature? Or was that the other way round, solubility of ethyl acetate in water? It's best to check this, it's definitely one of the two.

 

[downwardsfromzero]

Reading back through the past couple of days to catch up, it strikes me that an alternative to CaCl2 for removing small amounts of excess water from the EtOAc pulls would be simply to use freshly oven-dried NaCl. That should soak up a decent amount of water without being reactive towards nitrogenous bases, while avoiding some of the potential problems of adding it to the alkaline paste.

 

[grollum]

Yeah, a cloth is fine. If the room is clean I don't use anything.

One thing I always do with the stuff that sticks to the walls is to shake the jar with fresh ethyl acetate 2-3 times. A bunch of it falls off and floats as crystals that are caught easily in a filter. What doesn't fall off is what I pick up in warm water after letting the solvent dry for a few hours.

Thanks. Will try both!

Agreeing with Loveall, I think the small grainy sandy particles were the desired result. I don't think water was needed at this point. Maybe just crush the bigger bits. And you could mix the whole thing for a few minutes to ensure any citric dissolves into the ethyl acetate. Then pour through a filter.

Will try!

- Quick (3 minute) pulls, very gently stirring the first 30 seconds. We have observed that longer pulls result in greener solvent, which we assume is stuff we don't want. Cactus also gets sticky the longer it has been in contact with ethyl acetate (after about 30-40 minutes), which DWZ conjectures is undesired reactions between the ethyl acetate and cactus;

That might be the most important change I will make next time. In my first and second attempt I was stiring before every pull. And maybe not gentle enough.
So will only stir once at the beginning and more gentle. Will also try loveall's additional suggestions from above post.

- Bomb heavily with citric acid and mix vigorously. When I went light on citric and didn't mix, I got various results like oil droplets or water droplets, but no xtals. After letting those failed jars sit for a while, I bombed with citric and got some xtals, although less yield than a proper bombing and mixing from the onset;

When do you stop? When clear or when the dissolution is not working anymore? I think I should really get a magnetic stirrer.

I conjecture that if water is interfering with xtalization, another way to minimize its influence is to add fresh ethyl acetate to the extract before bombing with citric. It is not necessarily efficient use of the solvent, but for initially testing the hypothesis it may be a direction to consider. For those having difficulty, perhaps split the next run's combined pulls into 2-4 jars and salt them separately, trying different amounts of added fresh ethyl acetate before salting.

Thought about that too. The jars from my second attempt were sitting in the fridge for a day and collected what I think was water at the bottom. So this might be what is going wrong so far for me.

@Loveall: Thanks for your test's regarding the water. Handling the paste in a better way might really be the best way.

 

[downwardsfromzero]

The jars from my second attempt were sitting in the fridge for a day and collected what I think was water at the bottom.

It might be a good idea to collect some of this 'water' and send it for analysis - could it perhaps contain N-acetyl mescaline?