TEK Ethyl acetate approach [CIELO]

[Loveall]

After having the second and most definitive yet mesc fumarate trip and having amazing insights into the life of my 20 years old peruvianus friend, we can share the almost CIELO extraction we did.

5 g of outer skin peruvianus dried and powdered that has been kept in the freezer for about 3 years as such was used as a small scale trial. 0.5 g of sodium carbonate was added, mixed, and 5 g of purified water added and mixed to what quickly became a congealed mass of yellow green becoming darker beauty after 10 min. To it 30 ml of ethyl acetate was added and the congealed mass was squeezed with a fork and etac became very yellow. Collected and repeated 2x times with more 30 ml etac with hard squeezing of mass. Solution was filtered and sodium carb added for a chem dry, which went from powder to larger chunks due to water absorption. Solution filtered again. 10 ml was fractioned in 1 ml or so aliquots to which tannic, citric, fumaric, malic, nicotinic a and folic acids were sprinkled and all heavily mixed. After a few hours at room temp malic gave small crystals, fumaric gave powder, citric gave orange goo, tannic and folic stayed clouds and nothing really dropped and nothing happened with nicotinic as it didn't dissolve at all. The 80 ml was then halved and to each was added 50 mg of fumaric and malic acid which repeated what was said above. It was washed by mix and decanting in cold etac until solution came clear. Dry yield was 50 mg malate and 39 mg fumarates (1.5%?). Mouth watered, eyes sparkled and compulsion and angst led to sublingual consumption of all of it. Absolutely active, but very light.

Then 45 g of the same was processed as above but proportionally larger volumes and weight, with total 300 ml of loaded etac dark green, cause it took a damn long time to squeeze and process the larger mass and it became obvious that the longer it took the darker etac came out, plus the squeezing that was even more aggressive. Those 300 was separated as 200 ml to malic and 100 ml to fumaric. Yielding 300 mg slightly crystalline powdery malate and 200 mg powdery fumarates perfectly white. A roughly 1.1% yield.

200 mg of fumarate was consumed as 150 mg dissolved in water and 50 mg sublingual. Slightly bitter, smells like fresh cacti, didn't really have the fumaric taste. Overall, absolutely amazing 10 hours of light to moderate effects. Nausea and body load (which I am used to and so no vomit but it is unfortunate cause it takes attention off the experience) for the first 3-4 hours. Peaked at 4 hrs but it is difficult to state that as it is so persistent and changing effects... At 8 hours in it was still rolling. Many moments of personal power. Inspiration. Personal memories came up vividly and emotionally engaging. Deep introspection. Sociability stimuli (meaning I talked a lot with the babysitter partner until it fell asleep a few times). Intense visual and audio acuity. Visual hallucinations started with a strange shimmering at 2 hrs. Time dilation moments were common. Surfaces went plastic and contours moved about. Closed eyes things were very populated and colorful but shapes were not obvious.

The life cycle of my friend the peruvian and our 20 year-old relationship was reviewed from seed to baby to pup to adult to clones to cuttings to CIELO to my brain for the message exchange moment which looped infinitely into itself. We are bound to each other and it is my muse and lover which I must preserve.

Next episode will be the 300 mg of malate for a moderate trip.

Comments on protocol: only had sodium carb so went with it, indeed congeals the mass and has zero etac penetrability, had to squeeze hard... That probably explains why citric went gooey. Maybe adding much less sod carb? I put a bet into the sod carb chemical dry step. Still, fumaric and malic worked fine for my dummy attempt... In fact, malic acid seemed to be perfect. On the next extraction there will be evidence to be shared for this fumarate and malate work up.

Thank you everyone involved in this collaborative effort. You made part of my life make sense.

Can't you get lime (calcium hydroxide)? It will work much better.

Interesting results for malic acid.

 

[Ruffles]

Yes, that will be arranged. Calcium hydroxide should improve this drastically, if the mass becomes crumbly as stated in the Tek.

Just had to try sodium carbonate as it was on hand and a fridge clean up was requested by the higher powers that be. We were amazed that it worked at all, the mass was extremely non pliable and stubborn.

 

[Bruce_Willis]

Just wanted to say a huge thank you to Loveall and all the incredibly intelligent people behind making this TEK. Without your well written and thought out instructions a simpleton like myself would never be able to pull off an extraction like this.
This is my second successful extraction and best yielding so far. I decided to switch to fumaric acid for salting after 6 failed attempts with citric acid.
First time I used the mag stirrer and was very happy just to get something finally, but this time I went for the slow crystal growth and left the jar undisturbed for 5 days just to make sure.
It was such a pleasure to watch the crystals form slowly. I initially thought the ones seen on the walls of the jar was all I was going to get, but eventually I could see many nice long needles had grown off the bottom of the jar.
Even though the yield is small, this is from 100 grams of Bridgesii, I'm satisfied that I've got some success with it.
First picture is about 24 hours after salting and second and third pictures are just before collection.

 

[Ruffles]

So you threw fumaric acid in there and left it alone or you mixed a bit?

Those are pretty big pretty needles.

 

[Bruce_Willis]

So you threw fumaric acid in there and left it alone or you mixed a bit?

Those are pretty big pretty needles.

Yeah just sprinkled it in then left it. No swirling or mixing of any kind.

 

[new_science]

I wanted to pop in here to say thank you to everyone who worked so hard on this tek. I finally got the chance to run it for the first time today and it's every bit as elegant as it would appear to be on paper. I will chime back in soon to let you all know what my yield winds up being from 100g of whole plant Jiimz Twin Spine bridgesii. I biffed the first pull a bit, adding too little EA by accident, however the initial xtal formation after salting with fumaric acid seems encouraging.

EDIT // UPDATE: Final yield from 100g including core was 1.70g of mescaline fumarate. There are still some little xtals stuck to the jar that will either seed the next run or be dealt with at a future time. No big deal. Very happy with 1.7% with all things considered. Cheers!

 

[rok_job]

Recently completed my first fumarate extraction following the tek as closely as possible. Yield after 5 EA pulls was 0.326g from 77g dry cactus, so about 0.4%.

I then attempted the solvent reuse process by adding washing soda + water and returning it to the magnetic stirrer. However, after 24 hours in the magnetic stirrer, it hasn't really appeared to clear up. I've attached a photo of it mid-stirring. Are the crystals gathering on the upper rim of the glass mesc fumarate that didn't crystalise in the prior stage, or something else?

 

[Transform]

Recently completed my first fumarate extraction following the tek as closely as possible. Yield after 5 EA pulls was 0.326g from 77g dry cactus, so about 0.4%.

I then attempted the solvent reuse process by adding washing soda + water and returning it to the magnetic stirrer. However, after 24 hours in the magnetic stirrer, it hasn't really appeared to clear up. I've attached a photo of it mid-stirring. Are the crystals gathering on the upper rim of the glass mesc fumarate that didn't crystalise in the prior stage, or something else?

View attachment 105243

If you followed the steps exactly as defined in the method, that should be mesc citrate. If there's any reason for your EA to be both citric acid saturated and evaporating, it could be citric acid.

A properly focussed close-up of the crystals would be more informative.

 

[rok_job]

If you followed the steps exactly as defined in the method, that should be mesc citrate. If there's any reason for your EA to be both citric acid saturated and evaporating, it could be citric acid.

A properly focussed close-up of the crystals would be more informative.

Thanks for the reply. I couldn't get a good photo of the crystals. When I collected them it was a paste that evaporated into a fine powder. I put a very small amount on my tongue and it was salty, without the strong bitterness of mesc. fumarate.

 

[Ruffles]

Hello CIELO team.

So, we are trying to reuse the ethyl acetate but the pH stays at 4 (ethyl acetate by itself is marking around 5-6). Did the sodium carb + water - mixalot - decant then nacl +water - mixalot - decant., many times in sequence. pH stays the same. Tek mentions we should see a difference in ethyl acetate after adding nacl but doesn`t characterize what "difference" means. I was hoping for the ethyl to become clear and force water out but it actually stayed clouded forever, then I removed the bottom water layer and it eventually clarified, which was unexpected. Ended up using the washed ethyl acetate for a small scale extraction and will update (seems to have worked for extraction regardless). Will add activated charcoal for a more consistent cleanup.

 

[blig-blug]

Hello CIELO team.

So, we are trying to reuse the ethyl acetate but the pH stays at 4 (ethyl acetate by itself is marking around 5-6). Did the sodium carb + water - mixalot - decant then nacl +water - mixalot - decant., many times in sequence. pH stays the same. Tek mentions we should see a difference in ethyl acetate after adding nacl but doesn`t characterize what "difference" means. I was hoping for the ethyl to become clear and force water out but it actually stayed clouded forever, then I removed the bottom water layer and it eventually clarified, which was unexpected. Ended up using the washed ethyl acetate for a small scale extraction and will update (seems to have worked for extraction regardless). Will add activated charcoal for a more consistent cleanup.

Maybe you could try drying it with calcium carbonate [Edit: CHLORIDE]. I think the sodium carbonate and brine washes aren't meant to dry it (I may be wrong). Some hours with calcium carbonate [Edit: CHLORIDE] leave it very dry.

 

[Transform]

Hello CIELO team.

So, we are trying to reuse the ethyl acetate but the pH stays at 4 (ethyl acetate by itself is marking around 5-6). Did the sodium carb + water - mixalot - decant then nacl +water - mixalot - decant., many times in sequence. pH stays the same. Tek mentions we should see a difference in ethyl acetate after adding nacl but doesn`t characterize what "difference" means. I was hoping for the ethyl to become clear and force water out but it actually stayed clouded forever, then I removed the bottom water layer and it eventually clarified, which was unexpected. Ended up using the washed ethyl acetate for a small scale extraction and will update (seems to have worked for extraction regardless). Will add activated charcoal for a more consistent cleanup.

How are you measuring the pH in ethyl acetate, exactly? It's an aprotic solvent…

 

[blig-blug]

Maybe you could try drying it with calcium carbonate. I think the sodium carbonate and brine washes aren't meant to dry it (I may be wrong). Some hours with calcium carbonate leave it very dry.

I meant calcium chloride, obviously!!

 

[Transform]

I meant calcium chloride, obviously!!

I was thinking something might be amiss there!

I think the sodium carbonate and brine washes aren't meant to dry it (I may be wrong).

Saturated brine and saturated sodium (bi)carbonate solution will remove a certain amount of dissolved water from solvents. I've dried some solvents using anhydrous sodium carbonate, too - usually when they have some kind of amine freebase in solution.

 

[Ruffles]

Hey, it's not about drying it, it is about cleaning the ethyl for a new extraction according to the tek. Add sod carb to neutralize the excess acids and draw it to water, then a brine wash. The pH was measured using strips with 4 different color indicators. Not happy with the cleanup so far, so I will try the activated charcoal.

 

[bavic1974]

3g of fumaric acid dissolve well in the EA extract described in the TEK. Multiple people have had no issues dissolving it all.

That is ~3g/g, minus whatever reacts to form product (about half a gram or so)

Are you measuring the solubility in fresh EA? It could be lower than in the extract from the TEK.

Your data does discourage a full chemical dry, which is not recommended in the TEK.

I am dealing concerns that the fumaric acid did not dissolve completely and my final product has FA in it. There is a link that is findable via google that comes back to here stating that Fumaric has a solubility in EA of 10mg/g. But I can only find what is written in this post. Here you state people have done it up to 3g without issue. I have attached what I found you replied to someone reddit with.
I used 180 grams of powder, 1700ml of EA and 5.4g of Fumaric, per Bob's Cielo Calculator. At 3mg/g(.3%) and 1700EA im at 5.1g of Fumaric. But if 10mg/g(1%) is the real threshold I could have gone up to 17g of Fumaric. Where are we at with a consensus on the solubility of Fumaric in EA??

 

[Loveall]

I am dealing concerns that the fumaric acid did not dissolve completely and my final product has FA in it. There is a link that is findable via google that comes back to here stating that Fumaric has a solubility in EA of 10mg/g. But I can only find what is written in this post. Here you state people have done it up to 3g without issue. I have attached what I found you replied to someone reddit with.
I used 180 grams of powder, 1700ml of EA and 5.4g of Fumaric, per Bob's Cielo Calculator. At 3mg/g(.3%) and 1700EA im at 5.1g of Fumaric. But if 10mg/g(1%) is the real threshold I could have gone up to 17g of Fumaric. Where are we at with a consensus on the solubility of Fumaric in EA??

10mg/g is around the max from wet EA from the TEK, which means that 3mg/g will dissolve.

I have zero concerns that your fumaric did not dissolve unless you deviated outside the TEK with a freezer rest or chemical dry, etc.

You can verify that all the fumaric you added did indeed dissolve by filtering the product and dissolving 100mg more fumaric in the spent extract. If you want to keep ok adding fumaric until it does not dissolve that would be a nice contribution to add more data to the 10mg/g estimate we have now.

 

[Loveall]

Hey, it's not about drying it, it is about cleaning the ethyl for a new extraction according to the tek. Add sod carb to neutralize the excess acids and draw it to water, then a brine wash. The pH was measured using strips with 4 different color indicators. Not happy with the cleanup so far, so I will try the activated charcoal.

The 4 color indicators are not recommended. The plain yellow universal are.

Compare any the color you get to fresh EA.

What are you not happy about with the cleanup (Regen) specifically ?

 

[Ruffles]

The 4 color indicators are not recommended. The plain yellow universal are.

Compare any the color you get to fresh EA.

What are you not happy about with the cleanup (Regen) specifically ?

The main issue was with not getting a more neutral pH (got 4) compared to fresh EA (around 5 or 6). That raised my suspicion to it not being cleaned up at all. But it may be that it was not the best pH indicator for it.

An attempt to extract using the regenerated EA got me a very low yield of 0.4% compared to a near 2% using fresh EA, so that became the new reason to fret.

So I am using a bit of activated charcoal for more of a cleanup and we will see how it fares.

 

[Loveall]

The main issue was with not getting a more neutral pH (got 4) compared to fresh EA (around 5 or 6). That raised my suspicion to it not being cleaned up at all. But it may be that it was not the best pH indicator for it.

An attempt to extract using the regenerated EA got me a very low yield of 0.4% compared to a near 2% using fresh EA, so that became the new reason to fret.

So I am using a bit of activated charcoal for more of a cleanup and we will see how it fares.

Was it the same starting cactus?

Did you see clouding when pulling with reclaimed EA? It will cloud if not neutral due to calcium citrate forming.