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Ethyl acetate approach [CIELO] Options
 
Loveall
#841 Posted : 1/20/2022 6:09:37 AM

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Yeah samples of cuttings aging in the dark sounds very interesting. I could do 100g fresh (5g dry) section every week. That data would be cool.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 

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Cheelin
#842 Posted : 1/20/2022 12:08:50 PM

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If I had a closet full of logs, I’d already be working on that one. That particular question, as well as other β€˜stress -> higher M’ experiments or skin vs pulp vs core yield, can be easily answered, in a reliable/repeatable way; without significant technical knowledge, in-depth methods, or fancy equipment, using small samples.

This tek can open a lot of doors, with imaginative thought.

In the garden itself, if this can be micronized, imagine taking a small cork borer plug or skin scraping, extracting in a tiny test tube, then doing a titration from a burette, and making decisions about culling, harvesting, breeding.

I don’t have the expertise to design this myself, but this tek may have the potential to be developed that way by someone who does.

5 ingredients, a few processing steps, quick turnaround, repeatability make this very exploitable for assay purposes. At a minimum, it can provide small quantities of product to standardize/calibrate more sophisticated assay techniques. But, perhaps those wouldn’t be necessary.
 
oetzi13
#843 Posted : 1/20/2022 7:52:49 PM

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Heya! I finally got around to trying this out but ended up with some questionable product. IF I were to recrystallize with A/B should I use citric acid, or does it matter? Can I go straight to a STB?
Things are not as they seem, nor are they otherwise.
- Buddha.
 
Cheelin
#844 Posted : 1/20/2022 8:33:36 PM

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Lol, I just replied to one of your threads, dealing with chromatography.



Seems that crap happens a lot when learning this tek. But, the tek is like learning to ride a bike, once you nail it, you’re golden.

Depending on what state of crappiness your product is, it might work, i’ve also tried β€œdried” acetone. My feeling is that any solvent that water is soluble in is going to be problematic from a yield recovery perspective, and maybe for other reasons.

However, if you are willing to persevere and get up the learning curve, you can get some good results by running your crappy product in a 5g cactus powder run of cielo. I am still working to optimize the approach, but my recent run with β€œpure” cielo product recovered 65.9% of the input, on top of the expected yield of the cactus. Let me know if i can help with this.

If you choose to experiment with a different rehab approach, please be sure to post your method and results here.
 
Loveall
#845 Posted : 1/20/2022 11:12:29 PM

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oetzi13 wrote:
Heya! I finally got around to trying this out but ended up with some questionable product. IF I were to recrystallize with A/B should I use citric acid, or does it matter? Can I go straight to a STB?


Why is it questionable? Did an oil precipitate? Leading theory is that too much water was present. Did you rest the extract for over 1 hour and check for dropplets to decant before salting? Was it clear before salting?
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#846 Posted : 1/21/2022 1:01:21 AM

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Two other common goo production methods in this tek are:

1. Inadequate washing of crystallization jar and filtrate with fresh EA,
2. Water washing of crystallization jar before the previous EA jar wash has completely dried.

Basically, any water at all in this tek, after the paste is made, is guaranteed to make excellent goo.
 
oetzi13
#847 Posted : 1/21/2022 2:11:31 AM

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I followed the tek to the teeth. It was easy and fast (thank you) Did not have adequate filtration system in place (broke the buchner). Just a normal coffee filter. When trying to wash the product it got gooey cause it didn't get sucked through fast enough. After separating there was a bit of goo, a good amount of chalky substance, some fluffy crystals, and some that look more like salt. Sounds like you guys recommend just running another Cielo on it. I was planning on doing a reX a'la Kash. Doesn't sound like a good idea anymore
Things are not as they seem, nor are they otherwise.
- Buddha.
 
Loveall
#848 Posted : 1/21/2022 2:38:32 AM

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oetzi13 wrote:
I followed the tek to the teeth. It was easy and fast (thank you) Did not have adequate filtration system in place (broke the buchner). Just a normal coffee filter. When trying to wash the product it got gooey cause it didn't get sucked through fast enough. After separating there was a bit of goo, a good amount of chalky substance, some fluffy crystals, and some that look more like salt. Sounds like you guys recommend just running another Cielo on it. I was planning on doing a reX a'la Kash. Doesn't sound like a good idea anymore


So you had xtals initially in the salting jar. I don't understand how they became goo during the fresh ethyl acetate wash, unless you are saying the used EA dried with the xtals because it didn't move through the filter? My extract always moves fast through the coffee filter though.

I've tried Kash re-x with minimal water and added acetone. I could not get it to work with mescaline citrate. Xtals don't crash like they do with sulfate which I have done a few times. I did get citrate xtals to crash after adding EA to the mix, but not recommended because of the volume of solvent used and the risk of layers forming at the wrong water/acetone/EA ratio.

Redoing CIELO with a small amount of cactus powder (~5g) added to the goo is recommended, but you may need to use more lime to have a good paste consistency: I believe that is Cheelin's recommendation. You may also need more citric to crash out all the mescaline extracted from the goo.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Cheelin
#849 Posted : 1/21/2022 3:16:59 AM

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Sorry to hear about the buchner funnel, this tek works best if you don’t get fancy.

I can understand the goo, with a filtering accident.

I reslly don’t understand the combination of various filtrate forms, if your EA was not reused. The product is generated during salting/crystallization, which occurred before the funnel broke.

How did you salt/crystalize?

Please don’t take my comments/question as criticism. We want to identify where the tek needs to be explained better, and you can help us with this.


Current recovery method (still working to optimize):
1. Use 5g cactus powder
2. Dry goo as best possible, powder it (mortar & pestle) if possible, weigh it.
3. Add weights 1 + 2 => material weight
4.. Calc scaling ratio = material weight /100
5. For lime, water, citric acid: calc ingredient amount = scaling ratio x amount in tek (ex. for lime amount to use = scaling ratio x 25g)
6. Mix water & lime, add goo & mix, add cactus powder and mix for 5 minutes, let rest for 6 minutes in french press.
7. Do 6 pulls, (1 min stir & 2 min rest) per pull, using 20mL fresh EA per pull, filter each pull into collection jar, re-filter into salting jar, let settle 1 hour or until clear.
8. Dump in citric acid, stir once or twice til cloudy, cover let crystallize 72 hrs.
9. Pour into filter, rinse jar with 10mL fresh EA coating all jar interior surfaces, dump into filter, set aside jar to dry.
10. Using 10-20mL fresh EA, rinse filtrate to remove color, let filter and filtrate dry, then package filtrate.
11. After crystallization jar is dry, using 10mL hot water, rinse all interior jar surfaces, dump into glass evaporating dish, repeat rinse 1 more time, evaporate, scrape & package residue.

My most recent recovery run was posted on Jan 10, post 782 I believe.
 
Cheelin
#850 Posted : 1/21/2022 4:13:36 PM

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One of the things I wonder about various extraction teks is: how much of the desired compound is extracted by the tek? In other words, how much does a particular tek leave on the table?

A simple check on spent pastes, using a reagent, such as Marquis, may provide an indication. Perhaps, TLC can help as well.

I’m not sure when I’ll get around to it, but Endlessness’ TLC Megathread, is a great starting place to learn about this simple & useful technique:
https://www.dmt-nexus.me...135119&#post1135119
 
Cheelin
#851 Posted : 1/22/2022 12:26:28 AM

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Supplies are here, let’s take this tek to test tubes.

Going to start by doing 5 runs: 1g, 2g, 3g, 4g, 5g of cactus powder that has consistently produced 1.1% yields.

Scaling lime and water to 1%, 2%, 3%, 4%, 5% of tek levels

Paste times: stir 5 mins, rest 6 mins

6 x 3 min pulls, (1 min stir, 2 min rest) per pull; 1st pull 12 mL EA, pulls 2-6 7 mL EA

Passive salting, 0.250g citric acid all tubes. Filtering solution and washing tubes with fresh EA (~5mL, twice), then washing tubes with hot distilled water (~5mL, twice).

Forgot to take pics before filtering.

Filtered the samples at 48 & 60 hrs; water washed tubes, evap’d, and scraped residue.

At these small sample levels, it’s important to use distilled water, the ppm of your tap water may evap to a level that can skew results.

Only one sample had a measurable yield in the 60hr filtering, and then only 0.003g, so 48 hr passive crystallization is probably long enough.

Tube wash is critical to do well, since at these small amounts, it can add at least 0.2 points to total yield %.

Total yields:
1g 0.011g 1.1%,
2g 0.024g, 1.2%,
3g 0.036g, 1.2%,
4g 0.040g, 1.0%
5g 0.049g, 1.0%

I am happy to see these results; roughly consistent with expected yield % using larger sample amounts, across the range of cactus powder weights. But, at these small yield weights, multiple repeated results will be the test that gives me confidence in the reliability of this method.

Cheelin attached the following image(s):
Test Tube Runs.jpg (58kb) downloaded 160 time(s).
Before Salting.jpg (60kb) downloaded 144 time(s).
After Salting.jpg (62kb) downloaded 141 time(s).
Salting +8hrs.jpg (60kb) downloaded 130 time(s).
 
Homo Trypens
#852 Posted : 1/22/2022 1:03:35 PM

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Oh nice, exciting developments since my last visit to this thread Smile

--

I decided yesterday that it was time for me to do a CIELO again.

This time, i did everything as simple as i could, no extras. I don't have too much time for extractions atm, so i went a little bigger.

If i was going to get goo, i was going to just dry it and consume it as is - last time, I had failed horribly trying to convert it to sulfate.

I made a paste with ca. 360g dried pachanoi powder, 85g CaOH and 875ml water. I mixed the CaOH and water on the magnetic stirrer, then used a kitchen machine to mix the suspension into the cactus for a few minutes. I let the paste sit for about 30 minutes, then gave it another few minutes of mixing.

I pulled with a strict 1min stirring / 2min sitting regimen. I used the same EA from summer that i extracted with twice already. I had washed it in the meantime. Due to my choice of vessel, i couldn't add very much EA at once. I did close ca. 10 pulls and ended up with 1L of dark green but clean loaded EA. I let it sit for 20min to see if any kind of droplets were forming, and they weren't Smile

I did the quick precipitation method. Because i had 1L of EA, i added 15g of citric while mag stirring. After the cloud disappeared, i removed the stir bar and let the precipitation sit over night.

In the morning, i poured it through a coffee filter and washed twice in the filter with fresh EA. I then folded kitchen paper around the filter and squeezed as much trapped solvent out as i could. I opened the filter, loosened up some 'rocks' of mesc citrate and laid the filter on it's side to air dry.

2h later, i had 3g of dry mesc citrate powder (see pic) <3

I'll let the filtered EA sit for a few days/weeks, in case some more wants to crystallize slowly.
Homo Trypens attached the following image(s):
mescaline_citrate.jpg (102kb) downloaded 133 time(s).
 
Cheelin
#853 Posted : 1/22/2022 1:12:21 PM

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Sweet! Looks like you nailed it!
 
Loveall
#854 Posted : 1/22/2022 2:05:00 PM

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That's a world record. Looks good.

I would do more pulls on the spent paste. It will be congealed, but give it a shot. 1L of EA for that much powder many not be enough to grab it all.

You could cover and save the spent paste. After you finish the current extraction and wash the solvent, you could reuse that for a second set of pulls on a gummier paste.

Cheers and enjoy your product. If you want to convert the powder to long crystal needles (cosmetic) you can dissolve in warm water and evap slowly (as you probably know).

Do you have any thoughts on why you got goo the first time and not this time?
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸŒ³πŸ’šDMT salt e-juice HIELO TEKπŸ’šπŸŒ³πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEKπŸ’šπŸƒπŸ’š
 
Homo Trypens
#855 Posted : 1/22/2022 2:40:49 PM

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Loveall wrote:
I would do more pulls on the spent paste. It will be congealed, but give it a shot. 1L of EA for that much powder may not be enough to grab it all.


Hmm yeah! Because of the smell, i put the paste outside, but i can probably save it.
1L is what came back out - not sure how much i started with, but the paste ate quite a bit of it.

Loveall wrote:
Do you have any thoughts on why you got goo the first time and not this time?


I had several hypotheses, but i think they were all wrong. I was unable to reproduce the goo so far.
Maybe it was because i did the microwaving and my microwave is old and heats things unevenly.
 
Cheelin
#856 Posted : 1/22/2022 2:47:42 PM

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Homo Trypens wrote:
I had several hypotheses, but i think they were all wrong. I was unable to reproduce the goo so far.
Maybe it was because i did the microwaving and my microwave is old and heats things unevenly.



Did this run’s product look cleaner in the filter? Did you wash this run any differently?

Or, did the previous run go into the filter looking like goo?
 
Cheelin
#857 Posted : 1/22/2022 3:48:22 PM

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Loveall, maybe we can work into the wiki a diagnostic tool, to help identify critical learning points, and get a handle on their frequency. And, suggest that those learning the tek keep track of this info until they nail the tek?

Just a few simple questions for each of the process steps.

For example:
1. How does the particle size and consistency of your cactus powder compare to baking flour?
2. Which best describes how your paste looks after the rest period: mud, mashed potatoes, cookie dough, other (specify)?
3. Which best describes how your paste looks after your last pull: thick snot, sillyputty, chunky soup, applesauce, other (specify)?
4. Before salting, when holding your combined pulls up to a light:
a. Are your combined pulls crystal clear, hazy, cloudy, other (specify)?
b. Are there any visible layers or droplets in the combined pulls?
5. When pouring your solvent & product through the filter:
a. What is the form of your product: goo, powder, needles, other (specify)?
b. Did you rinse the crystallization jar with fresh EA?
c. Did you rinse the product in the filter with fresh EA until it stopped changing color?
d. Did your product or filter come into contact with water?
e. What is the final color of your product after washing with fresh EA?


At some point, this tek will be ready for ISO certification.
 
igorcarajo
#858 Posted : 1/22/2022 5:56:48 PM
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Hey, have y’all simplified the CIELO tek on the wiki? I swear I remember reading it months ago and there being different options, microwave the paste or something like that…or am I crazy?
 
Cheelin
#859 Posted : 1/22/2022 6:03:48 PM

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igorcarajo wrote:
Hey, have y’all simplified the CIELO tek on the wiki? I swear I remember reading it months ago and there being different options, microwave the paste or something like that…or am I crazy?


Yep, eliminated options that reduce yield…in preparation for submission to Nobel Committee on Mescalinetry.


Get ready to kick-in to a Kickstarter account for Loveall’s trip to Sweden.
 
igorcarajo
#860 Posted : 1/22/2022 6:06:25 PM
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Ha! Thanks.

So if I start with a smaller amount of powder, say 50 g instead of 100 g, then I also cut the water and lime amounts in half, right?
 
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