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TEK Ethyl acetate approach [CIELO]

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Loveall said:
Cheelin said:
Been doing multiple runs of 1g cactus powder, focused on a few recipe & process changes, as well as alternative paste and pulling equip/techniques. Will be salting soon, will have results mid-week.

Overall, there is an association/correlation between the darkness of pulls and crystal yield. All of these runs today are darker & just as clear as the 1g run that is currently crystallizing in the recent 5-run trial, so hopefully some progress being made.
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This is great, awesome way to optimize. Looking forward to the results.
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I’m hoping I can get the 1g method to produce repeatable results, matching % yield of larger quantities, using a single test tube for paste mixing and pulls, a 2nd tube for crystallization. Lol

I should get some useful indications from this set of runs.
 
The part that I think is missing in the analysis is the pH effect of the lime. When the EA and paste are mixed, the solution pH becomes basic. The -OH contributed by the lime, is what I was referring to.
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I don't think the lime changes the EA pH because it is not soluble in it. I think it is soluble alkaloids like mescaline that change the pH - they are alkaline. That is why the pH strips become neutral as the pulls go on (otherwise they would remain at an alkaline pH since the Car(OH)2 supply is essentially infinite). How much alkaline color is on the pH strip is correlated with the amount of mescaline is in the pull. The pull time was designed around the strip not changing much after 3 minutes (and assuming the pull is in equilibrium with the paste once the pH strip stops changing).

I believe I remember testing this: Add lime to EA and the pH doesn't change after settling and testing the clear solvent. Same with sodium carb. Both for dry EA or wet EA with a water layer.
 
Loveall said:
The part that I think is missing in the analysis is the pH effect of the lime. When the EA and paste are mixed, the solution pH becomes basic. The -OH contributed by the lime, is what I was referring to.
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I don't think the lime changes the EA pH because it is not soluble in it. I think it is soluble alkaloids like mescaline that change the pH - they are alkaline. That is why the pH strips become neutral as the pulls go on (otherwise they would remain at an alkaline pH since the Car(OH)2 supply is essentially infinite). How much alkaline color is on the pH strip is correlated with the amount of mescaline is in the pull. The pull time was designed around the strip not changing much after 3 minutes (and assuming the pull is in equilibrium with the paste once the pH strip stops changing).

I believe I remember testing this: Add lime to EA and the pH doesn't change after settling and testing the clear solvent. Same with sodium carb. Both for dry EA or wet EA with a water layer.
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I’m hard-headed, i’ll test Water + Lime vs Water + Lime + EA…I have no problem being wrong, when learning. Lol

Shoulda done this last night.


OK, so it looks to me like the effect of lime in the paste on pulled solution pH is dependent on how the lime disperses in the paste, dissociates and interacts with other paste components, and thereby ends up in solution. Perhaps 100% of the pH change from acidic pure EA to basic pulled EA is due to the freebase M, but lime does seem to have the potential to play a role.

I mixed 3.5mL distilled water with 0.29g pickling lime -> 12 pH,

I then added 11.0mL fresh EA (pH 5.0) and the solution immediately separated into what looked like a top EA layer and a bottom layer(s) of water + lime: the top EA layer had pH close/identical to fresh EA; the bottom layer(s) had 12 pH.

I then shook the shit out of the solution, got pH 9

A pic of the results is attached.
Left side are the strips from last night, left to right is Fresh EA, EA + citrate, EA + citrate + water;
Right side are the strips from this morning, left to right is Fresh EA, Shaken water + lime + EA, EA layer in water + lime + EA, Lime layer in water + lime + EA, Water + lime.


Btw, this discussion has no practical effect on the fact that this tek is a M extraction masterpiece!
 

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Moving on to something that really matters, I filtered the series of small cactus powder runs (1g through 5g), I’ll do final filter and jar wash late tonight or tomorrow

At salting +60 hrs, runs 2g through 5g all filtered at 0.9% yield vs expected 1.1% yield; the 1 g extraction yielded 0.4%. Still have opportunity for some improvement from the final filter and jar wash.

The 1 gram sample is especially sensitive to equipment and technique, as mentioned earlier, i have runs crystallizing atm that may help improve this tiny extraction.

Overall, I expect cielo, with a few more tweaks, to be a useful and fairly accurate tek for those who need a small sample M assay method. This is so damn cool!
 
It is interesting/surprising that you got pH9 from EA after shaking with lime water. How long did you wait before sampling? At equilibrium I would expect neutral EA, but I could be wrong as you are showing.
 
Loveall said:
It is interesting/surprising that you got pH9 from EA after shaking with lime water. How long did you wait before sampling? At equilibrium I would expect neutral EA, but I could be wrong as you are showing.
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I took the reading immediately after shaking. And, as your comment/question implies, the solution did eventually return to layers with different pH’s as described earlier.

My point wasn’t that this is a permanent effect, but that it can happen. And, therefore the amount of caustic lime, can perhaps play a role in producing an unanticipated product in this chemical system.

This is my last digression on this topic. No slight intended, it!s just turning into a distraction. I apologize for my role in this.



This whole discussion began with: ‘what causes goo?’

Bottom line for me: if you get goo, you fucked up.

I fucked up 6 times before nailing the tek. Have never made goo in the nearly 100 runs since.

Re-read the wiki; until you get pure needles or powder, follow it to a T.

This means use the exact ingredients, in the amounts listed or scaled down per my scaling example; same exact tools; same exact process; your starting powder must look the size and consistency of baking flour.

Do not make a single change (except perhaps ingredient scaling per my method) to what is in the wiki until you produce pure needles or powder.

The 4 most common points of failure in this deceptively simple and amazingly robust tek are:
1. Failure to follow instructions
2. Poor technique
3. Water mixing with Ethyl Acetate
4. Poor filtrate washing

You can control each of these, if you really want to.

If you have any questions about what the tek says/means, ask away. I want to help you be successful, i’m sure Loveall and others do, too.
 
Just dropping in to say, I'm still loving all the work that's still being done in this thread - and a special hello with kudos to Cheelin for putting OCD to such good use 😁 :love:
 
downwardsfromzero said:
Just dropping in to say, I'm still loving all the work that's still being done in this thread - and a special hello with kudos to Cheelin for putting OCD to such good use 😁 :love:
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Lmao!

This diy medicine isn’t addictive, but working on it is.
 
Loveall said:
Solid results Cheelin. You are going to need a sub-mg analytical scale at this rate 😅
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Thanks. Would do it, but want to keep this accessible to those who can’t afford, calibrate, or properly maintain such a delicate instrument.

Should clarify, I have access to an analytical balance, which after thinking about your comment, I’ll use for the experiments, due to higher precision. But, will stick with the “accessibility” goal in making recommendations about a method. The issue is that most people have access to scales that are readable to 0.001g but have +/-0.005g precision, some with minimum wt requirements that are larger than the sample (can be worked around). 1g sample yields are at a level where these limitations become an issue.

I hope, with a large number of 1g runs (and confirmation on larger runs) that this method can be determined to be reliable. Stay tuned for the results from first set of 1g optimizing runs later today.

See link above to latest update of washing methods. Hoping to test them in extractions sometime next week.
 
Bad news/Good news on the 1g sample trials: bad first, getting 0.002 to 0.004g shortfalls on the std process yields using ingredient changes, which on a 1 gram sample means 0.2 to 0.4 points lower than the expected 1.1% yield. Sources of these differences could include: scale precision, product losses due to std method transfers, poor choice of ingredient changes, operator error.

I hope to reduce the scale precision risk in the future by using an analytical balance to measure weight. To reduce the other risks, brings me to the good news.

The best yielding run this time, yielding 1.1%, involved doubling the lime addition from the scaled quantity with preparation of paste and pulls in the same test tube. Specifically: 0.5g lime and 3mL distilled water were mixed in the test tube, 3 Army Painter mixing balls and 1g cactus powder were added, then using a mini-vortex mixer, the paste was mixed for 3 minutes, then rested for 4 minutes. Using fresh EA, 6mL EA was added to the test tube and vortex mixed for 1 minute, rested for 2 minutes, and poured through a coffee filter into another test tube; then, using same times and 4mL of EA, 5 more pulls were done. The clear combined pulls were then salted with 0.3g citric acid, swirled, passively crystallized for 48 hrs, then filtered and washed.

I’m going to focus on this method for my next runs, trying to identify additional changes that will also yield at the expected %.
 
Firstly wanted to say awesome work Cheelin.

Secondly I wanted to report back a few changes I've been experimenting with.

I have a variety of Bridgesii which I pulled 2.12% from (HCL equivalent) green skin only. When using the wax, spines and green layer this dropped to .74% (HCL equivalent). I've previously reported this. These figures where using the older tek with microwave method etc.
Now that we know paste mix and consistency (with a bit of water content) is key to facilitate higher yields I've been having a play around.

I processed 168g of bridgessii powder (green skin, spines and wax layer) but used a ratio of water 2.75:1 instead of 3:1 (trying to find the sweet spot for blending). Again the blender mixed it perfectly but aerated the paste (making it not ideal or workable). Like my last run with pedro I fixed this by a quick few bursts in the microwave of 3 mins each. The consistency came out perfect (just enough moisture and fixed the aeration but please note the paste still had plenty of moisture content far from the 1/3rd evap of the much early tek).

The microwave had heated up the paste and i placed it in a hot water bath with 800ml of EA (i know the tek calls for a bit more for the size of the extraction but less has been working for me). Now that I had the EA and paste heated i did my pulls.


Long story short my yield increased by over 70%. I couldn't believe it.

I found when experimenting with the EA harmala tek yields increased significantly with a hot water bath (have the EA hot) and it seems to have worked well with the Cielo tek as well (as well as using a blender).

I'm keen to do green skin only with these new tweaks to see if I can get 3% (HCL equivalent) out of that bridgesii strain.
 
_Trip_ said:
Firstly wanted to say awesome work Cheelin.

Secondly I wanted to report back a few changes I've been experimenting with.

I have a variety of Bridgesii which I pulled 2.12% from (HCL equivalent) green skin only. When using the wax, spines and green layer this dropped to .74% (HCL equivalent). I've previously reported this. These figures where using the older tek with microwave method etc.
Now that we know paste mix and consistency (with a bit of water content) is key to facilitate higher yields I've been having a play around.

I processed 168g of bridgessii powder (green skin, spines and wax layer) but used a ratio of water 2.75:1 instead of 3:1 (trying to find the sweet spot for blending). Again the blender mixed it perfectly but aerated the paste (making it not ideal or workable). Like my last run with pedro I fixed this by a quick few bursts in the microwave of 3 mins each. The consistency came out perfect (just enough moisture and fixed the aeration but please note the paste still had plenty of moisture content far from the 1/3rd evap of the much early tek).

The microwave had heated up the paste and i placed it in a hot water bath with 800ml of EA (i know the tek calls for a bit more for the size of the extraction but less has been working for me). Now that I had the EA and paste heated i did my pulls.


Long story short my yield increased by over 70%. I couldn't believe it.

I found when experimenting with the EA harmala tek yields increased significantly with a hot water bath (have the EA hot) and it seems to have worked well with the Cielo tek as well (as well as using a blender).

I'm keen to do green skin only with these new tweaks to see if I can get 3% (HCL equivalent) out of that bridgesii strain.
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Whoa dude! Heating the EA extracted 70% more?!

What temp is “hot EA”?

I will do a test run on my 1.1% yielding powder.
 
I fully submerged it in boiling water in a pot and swapped it out for fresh boiling water half way through the pulls (both the paste and the EA remained submerged). The paste would have been heated by the microwave as well.

Keep in mind the early experiment when it yielded .7% was the old microwave tek where i use to evaped over 33% of the water content and did not mix with blender but by hand.
 
_Trip_ said:
I fully submerged it in boiling water in a pot and swapped it out for fresh boiling water half way through the pulls (both the paste and the EA remained submerged). The paste would have been heated by the microwave as well.

Keep in mind the early experiment when it yielded .7% was the old microwave tek where i use to evaped over 33% of the water content and did not mix with blender but by hand.
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So, EA boiling point is.~77c, so I’ll boil a pot of water, turn off heat, put a jar of EA in it, and take some temps over time. Then, figure out what I need to do to keep a high & constant temp EA, to do pulls on a paste that starts at room temp. See if/how much
yield increases.

Thanks _Trip_!

Btw, I see your tek is getting some kudos, congrats!
 
Thanks for the report _Trip_

Part of the 70% boost could be from not doing the long microwave pulls, right?

In my experience I feel like harmalas need warm EA, but mescaline does not. I base this on observing that if pulling harmalas with room temp EA, the amount pulled does not decrease quickly with each pull. On the other hand, when pulling mescaline, there is a significant drop in amount pulled each time.

We have seen that a second set of room temp pulls gives another 8% of mescaline. Perhaps if the EA is warm that is picked up in the first set of pulls for an 8% boost to the standard TEK.

I could be wrong of course, just initial thoughts. Will be interesting to see what others get.
 
Loveall said:
Thanks for the report _Trip_

Part of the 70% boost could be from not doing the long microwave pulls, right?

In my experience I feel like harmalas need warm EA, but mescaline does not. I base this on observing that if pulling harmalas with room temp EA, the amount pulled does not decrease quickly with each pull. On the other hand, when pulling mescaline, there is a significant drop in amount pulled each time.

We have seen that a second set of room temp pulls gives another 8% of mescaline. Perhaps if the EA is warm that is picked up in the first set of pulls for an 8% boost to the standard TEK.

I could be wrong of course, just initial thoughts. Will be interesting to see what others get.
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In a little while, i’ll do a 15g, passive crystallization run with ~65C EA pulls, everything else standard.
 
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