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Ethyl acetate approach [CIELO] Options
 
orchidist
#961 Posted : 2/3/2022 4:51:23 AM

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Loveall wrote:
orchidist wrote:
I transferred the goo to fresh ethyl acetate. It does appear to have dessicated, it's brittle. I was able to crush it with a stir rod.


This is interesting and points to water being a possible issue originally I think. Does it feel xtaline after decanting/drying? I wonder what would happened if you dissolves this dessicated product in minimal hot water (~2ml) and then combined that with EA (~100ml or so).

orchidist wrote:
Will do! I'll decant and set it aside later tonight, I am thinking I might take half the solvent and super fine powder from this first attempt, wash with sodium carbonate, separate it, allow some solvent to evaporate, and then retry the crystallization. Thoughts?


Sorry which super fine powder?

I think it makes sense to split your next pull. If straight forward salting doesn't work, drying with sodium carbonate before salting the next split makes sense. This is a very standard lab practice, we just skip it because we found it not necessary - except that we have this goo issue some folks encounter.

I recently did just this, spit a pull and dried one side with sodium carb. No issues on either side, Xatals in both. The sodium carb side would be more robust to excess water issues though, if that is a thing.


Hey, sorry for the delayed response, work's been a lot, and for some reason I wasn't notified of the new activity.

There is an extremely fine precipitate in my solvent. It does not look like very much. It's fine enough that I don't think the coffee filters I have on hand will catch much of it. It pretty easily goes back into suspension when the solvent is poured, which is why I was considering trying to force it to re-dissolve in the solvent with saturated Na2CO3, and then either concentrate it and salt it out after that, or reuse the solvent so it can fall out after extracting from fresh material. I'm leaning toward the latter.

The former goo does seem crystalline now, and definitely does not taste like citric acid. This is my first time anywhere near mescaline, so I don't really have a frame of reference on flavor, but it seems to fit the description I've read in this thread. Slightly bitter and slightly sour.

I haven't had much time over the last few days, so I threw the used solvent in the freezer--no ice formation at all. I'm not too surprised at that, considering the fact that I used way too much (about double) solvent this time. Admittedly, I was thrown off by the description of the quantity of solvent as "a couple fingers" worth. Might be worth removing that from the tek.

 

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orchidist
#962 Posted : 2/3/2022 5:00:21 AM

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So, actually, it looks like there's a fine coating all around the container I salted in, I hadn't noticed because I was in a bit of a rush at the time. It is water soluble. I'll let the wash water evaporate and report back.
 
Cheelin
#963 Posted : 2/3/2022 5:20:34 AM

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orchidist wrote:
I'm not too surprised at that, considering the fact that I used way too much (about double) solvent this time. Admittedly, I was thrown off by the description of the quantity of solvent as "a couple fingers" worth. Might be worth removing that from the tek.


That ‘2 fingers’ thing might work in a 100g run (i’ve never done one), but it certainly doesn’t work for smaller runs. Also, the use of quarts when other measures are metric, can confuse, as well.

For smaller runs, rely exclusively on volume measures for solvent. Scale total solvent volume as percent of cactus powder used, multiplied by 946mL, take 25% of the scaled volume as 1st pull; divide remainder by 5 to get amount per pull for pulls 2 through 6.
For example, if using 15g cactus powder: scaling factor would be 15/100 = .15, total solvent would be 946 x .15 = 142mL, 1st pull = 36mL, each pull of pulls 2 through 6 = 21mL.

Also, the proper end product tastes moderately bitter, with no acid (sour) flavor at all.
 
orchidist
#964 Posted : 2/3/2022 6:11:23 AM

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cheelin wrote:

That ‘2 fingers’ thing might work in a 100g run (i’ve never done one), but it certainly doesn’t work for smaller runs. Also, the use of quarts when other measures are metric, can confuse, as well.


Yeah, I didn't really intend on going for 2 fingers with my run, I added solvent until the material was completely covered. I misinterpreted that having enough solvent to cover was of more important than volume when scaling, and that sense was reinforced by the difficulty I had with pouring off the solvent between pulls, since I didn't think to take my oversized press apart to ditch the lid. It was impossible to put any pressure at all on the material, let alone squeeze it. Goes to show how little I've used that press in the past 😅

That does make me wonder if inefficient removal of solvent might have anything to do with goo. Increased contact time pulling more undesired components.
 
Loveall
#965 Posted : 2/3/2022 12:22:38 PM

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I've let solvent and paste sit together for over a day. The paste congeals onto itself and is harder to mix with ethyl acetate during this time. However, the solvent from this produces xtals.

Not squeezing is not an issue. Many times I got xtals without squeezing. It is actually when I squeeze bard that I get dropplets come through, but after settling/decanting this water I have no issues getting xtals.

I still have excess water as the leading hypothesis. If dropplets are small they can go unnoticed (they like to stik to the jar walls and hide there). Your goo was dessicated with fresh EA supports this. Cheelin's result with T3 water addition does not though. It may be that fresh water cannot cause goo. I wonder if adding "dirty" water from cacti would. Idea would be to repeat the T3 test, but use water coming from a spent paste soak. Maybe I'll try this.

orcjidist, in your first attempt, did you wait 1h and decant your extract to a second jar, or did you salt ddirectly after waiting 1h? If direct salting it is more likely dropplets where hiding on the wall after resting. Any news on your second attempt?
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Cheelin
#966 Posted : 2/3/2022 1:11:31 PM

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orchidist wrote:
cheelin wrote:

That ‘2 fingers’ thing might work in a 100g run (i’ve never done one), but it certainly doesn’t work for smaller runs. Also, the use of quarts when other measures are metric, can confuse, as well.


Yeah, I didn't really intend on going for 2 fingers with my run, I added solvent until the material was completely covered. I misinterpreted that having enough solvent to cover was of more important than volume when scaling, and that sense was reinforced by the difficulty I had with pouring off the solvent between pulls, since I didn't think to take my oversized press apart to ditch the lid. It was impossible to put any pressure at all on the material, let alone squeeze it. Goes to show how little I've used that press in the past 😅

That does make me wonder if inefficient removal of solvent might have anything to do with goo. Increased contact time pulling more undesired components.


It isn’t at all necessary to have the press screen even touch the paste during the pulls.

The purpose of the press screen is to prevent the paste from dropping into the filter while letting the “freerun” liquid flow out of the container. I generally only put pressure on the paste in the last pull (and then not that hard). When learning the tek, this yield enhancement is especially unimportant, since your primary goal should be to produce at least some of the proper product.

What is important, by far, at all times, during pulls, is the 1-minute stir; the purpose of which is to get maximum contact between every molecule in the paste with the solvent. Even the stickiest snot-like pastes (imo, the worst to work with, the least extractable) will give up more goodness if you do a purposeful stir that gets 70-90 revolutions in during the 1-minute stirs.

Generally, the first pull yields almost no liquid; this pull is essentially a wetting & penetration pull, the liquid from which flows out in subsequent pulls as the fresh solvent “switches places” with the previously absorbed solvent.

For me, the sign of good pastemaking & decent pull technique, is if, by the last pull, at least (the earlier the better), the paste while stirring looks like applesauce.
 
Cheelin
#967 Posted : 2/3/2022 1:22:00 PM

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Loveall wrote:
I've let solvent and paste sit together for over a day. The paste congeals onto itself and is harder to mix with ethyl acetate during this time. However, the solvent from this produces xtals.

Not squeezing is not an issue. Many times I got xtals without squeezing. It is actually when I squeeze bard that I get dropplets come through, but after settling/decanting this water I have no issues getting xtals.

I still have excess water as the leading hypothesis. If dropplets are small they can go unnoticed (they like to stik to the jar walls and hide there). Your goo was dessicated with fresh EA supports this. Cheelin's result with T3 water addition does not though. It may be that fresh water cannot cause goo. I wonder if adding "dirty" water from cacti would. Idea would be to repeat the T3 test, but use water coming from a spent paste soak. Maybe I'll try this.

orcjidist, in your first attempt, did you wait 1h and decant your extract to a second jar, or did you salt ddirectly after waiting 1h? If direct salting it is more likely dropplets where hiding on the wall after resting. Any news on your second attempt?


We’ll see what the filtrates from my trials show. But I am totally convinced that, if water plays a role in pre-filtering goo development, the process is much more complicated than simply having water droplets or layers present in the pull jar.

Perhaps “contaminated water” of some sort contributes to goo formation - that’s why I used tap water in my 2nd goo trial (but 250 ppm is kinda low).

Besides poor pastemaking and pulling technique, i would lean toward something about the cactus “powder” being the primary causal factor of goo formation. Finally, we know that EA can decompose certain materials, such as some plastics, perhaps this is a causal factor.

From a product quality perspective, it’s clear to me the tek itself is incredibly robust when done reasonably correctly, even with extreme variations from stated recipe ingredient amounts.

Ingredient levels, including water, are much more impactful on product yield than product quality.

I suppose it is “human nature” for people to go for max yield and take shortcuts when learning a new tek, especially one as deceptively simple as this one. Perhaps the wiki should somehow stress the importance of following the stated process AND focusing on getting the proper product (vs max yield) until they nail the tek. For my part, i will, once again, in excrutiating detail, repost the method i have used for over 100 runs, that has never produced goo - even when trying to do so.

Not sure how else I can help with goo formation that happens before filtering…if it occurs after filtering, it is because of poor filtrate or jar rinsing.



The 1st trial, looking at sediment or water in the combined pulls, has been updated here: https://www.dmt-nexus.me...p;m=1136784#post1136784

The 2nd trial, looking at significant +/- variation of lime or citrate levels, has been updated here: https://www.dmt-nexus.me...p;m=1136784#post1136784

 
oetzi13
#968 Posted : 2/3/2022 8:42:14 PM

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Hello Friends! Quick update on this recent gunk run. After the “filtered” AE was sitting for a week 240mg of perfect needles were still resting on the bottom of the jar. This time there was no issue filtering and washing. The original problem seems to stem from a crappy filter form the dollar store. You can almost see though that thing. Lol
10 g of new dry material was used for the RE-X as Cheelin recommended and mixed with the funky material (fluffy semi sparkling calcium like powder and some goo [pic 1]) from the previous run. The AE turned much darker this time (pic 2)and when salting the hole thing looked like green milk (pic 3), but 72 hours later the bottom of the jar was covered in pretty needles half an inch high. After drying it still had the ‘dirty Sanchez’ color but that is not a big problem (pic 4). A whooping 3% yield - fantastic!
Im diggin this tek. Thank you all for all the hard work you put into it. Your killing it!
oetzi13 attached the following image(s):
Screen Shot 2022-02-03 at 12.33.08 PM.png (544kb) downloaded 121 time(s).
Screen Shot 2022-02-03 at 12.33.51 PM.png (642kb) downloaded 120 time(s).
Screen Shot 2022-02-03 at 12.34.27 PM.png (655kb) downloaded 120 time(s).
Screen Shot 2022-02-03 at 12.34.38 PM.png (848kb) downloaded 121 time(s).
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Cheelin
#969 Posted : 2/3/2022 9:15:20 PM

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oetzi13 wrote:
Hello Friends! Quick update on this recent gunk run. After the “filtered” AE was sitting for a week 240mg of perfect needles were still resting on the bottom of the jar. This time there was no issue filtering and washing. The original problem seems to stem from a crappy filter form the dollar store. You can almost see though that thing. Lol
10 g of new dry material was used for the RE-X as Cheelin recommended and mixed with the funky material (fluffy semi sparkling calcium like powder and some goo [pic 1]) from the previous run. The AE turned much darker this time (pic 2)and when salting the hole thing looked like green milk (pic 3), but 72 hours later the bottom of the jar was covered in pretty needles half an inch high. After drying it still had the ‘dirty Sanchez’ color but that is not a big problem (pic 4). A whooping 3% yield - fantastic!
Im diggin this tek. Thank you all for all the hard work you put into it. Your killing it!



Congrats!

Proud of you for sticking with it!

You are almost there. That dirtiness is reminiscent of sediment plus needles. I just finished collecting that type filtrate, from a run where i purposefully added cactus powder to crystal clear pulls.

I took my mixed sediment-needles, let them dry, then mixed them with hot distilled water, and then filtered through a paper coffee filter. The M readily dissolves in water and flows through the filter, most of the sediment was caught in the filter. I will next let the water solution settle then decant the liquid to be evap’d & scraped. These scrapings will be a refined M product of the original predominantly sediment product.

The expected yield for this sample size was approx 0.070 - 0.080g, after recrystallization the dried wt was 0.193g, approx 60% more than expected. This extra amount represent extremely fine sediment that drained through the filter along with the dissolved M citrate. See T2 in attached pic; T1 was the control, which yielded 0.076 or 1.5%. The moral of this story is: don’t salt your pulls until they are crystal clear. Otherwise, your final product will be substantially impure, even with further cleanup work…and you will likely have additional yield losses trying to do the cleanup.



In future runs, if you can get your combined pulls clear, you will produce pure crystals. I originally said “pure white” crystals, but perhaps the color of your pulled solvent has an impact on the whiteness, or perhaps rinsing with
(more) fresh EA during filtering would whiten them.
Cheelin attached the following image(s):
Sediment Separation.jpg (28kb) downloaded 104 time(s).
Sediment & Water.jpg (97kb) downloaded 60 time(s).
 
orchidist
#970 Posted : 2/3/2022 10:33:46 PM

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Loveall wrote:
I've let solvent and paste sit together for over a day. The paste congeals onto itself and is harder to mix with ethyl acetate during this time. However, the solvent from this produces xtals.

Not squeezing is not an issue. Many times I got xtals without squeezing. It is actually when I squeeze bard that I get dropplets come through, but after settling/decanting this water I have no issues getting xtals.


That's good to know, I'm just grasping for anything that may have been a deviation in hindsight.

Loveall wrote:

I still have excess water as the leading hypothesis. If dropplets are small they can go unnoticed (they like to stik to the jar walls and hide there). Your goo was dessicated with fresh EA supports this. Cheelin's result with T3 water addition does not though. It may be that fresh water cannot cause goo. I wonder if adding "dirty" water from cacti would. Idea would be to repeat the T3 test, but use water coming from a spent paste soak. Maybe I'll try this.


Cheelin wrote:

Perhaps “contaminated water” of some sort contributes to goo formation - that’s why I used tap water in my 2nd goo trial (but 250 ppm is kinda low).


Dirty cactus water sounds like a good trial. Regarding other contaminants, I remember way back in the thread that MgSO4 was detrimental in some way when used as a drying agent.(Having a hard time bringing it up with the search function though.) Perhaps Mg is problematic if it's present at earlier steps. I don't know the Mg content of my water, but with Mg being one of the most common minerals in tap water, a trial with MgSO4 in distilled water may be worth a try?

Loveall wrote:

orcjidist, in your first attempt, did you wait 1h and decant your extract to a second jar, or did you salt ddirectly after waiting 1h? If direct salting it is more likely dropplets where hiding on the wall after resting. Any news on your second attempt?


Yes, I decanted after waiting, the only thing I found at the end of that period was a small amount of sediment. For the last few days, the solvent has been sitting the freezer--no visible ice.

No news on the second attempt yet, I hope to start it either this evening or tomorrow evening. Some good news though, the white film on my glassware was positive by Marquis reagent (finally arrived with a TLC kit after a long delay), so I'll wash all of that down and evaporate.

cheelin wrote:

For me, the sign of good pastemaking & decent pull technique, is if, by the last pull, at least (the earlier the better), the paste while stirring looks like applesauce.


At least I can be fairly confident I got the paste consistency right, it was applesauce on the first addition. With mixing, I went so far as to set a metronome to keep the pace.

I want to thank you two for bearing with me, I hope I'm not being a pest 😅
 
Cheelin
#971 Posted : 2/3/2022 10:37:39 PM

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orchidist wrote:
I want to thank you two for bearing with me, I hope I'm not being a pest 😅



Absolutely my pleasure, don’t even think of apologizing!
 
_Trip_
#972 Posted : 2/4/2022 2:26:15 AM

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It seems everyone has been very busy experimenting which is awesome to see.

I just wanted to add a bit of information from some data I've been collecting with different cacti. As previously discussed on other threads cacti kept in the dark for a minimum 3 months can double mescaline content. So logically winter would be the best time to harvest (which i believe has been discussed on nexus before). The line of thought is in winter, the plant is dormant and spends more time on alkaloid content than it does on growing. In addition, there's less light and shorter days which falls in line with the whole dark helps mescaline production.
I've notice from a recent batch harvested in the peak of summer a 40% drop in yield. I hope to do other strains and confirm this drop. Hopefully by posting this more people can confirm this observation (or report other findings).


Disclaimer: All my posts are of total fiction.



 
orchidist
#973 Posted : 2/4/2022 2:40:36 AM

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Finished my pulls, feeling pretty good about it. I got reverse osmosis water for this run, did 8 pulls with the recommended quantities, scaled for 25 grams. It was much easier without the lid in the way.

Pulls 1-6 are combined, very dark green, clear, a few specks of dust. 7 and 8 much lighter green, looks like there's a tiny amount of stuff to decant.

Decided to throw pulls 1-6 in my separatory funnel and leave it in there overnight for total confidence that there's no water. Of course, fancy thoughts like that anger the gods, and I forgot to close the stopcock, so I lost a few mL.
orchidist attached the following image(s):
cielo.png (592kb) downloaded 86 time(s).
 
Cheelin
#974 Posted : 2/4/2022 2:56:12 AM

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Good stuff _Trip_

If this takes off, maybe we set up a separate ‘Cactus Assay - Cielo Tek Utilization Studies (CA-CTUS)’ thread.
 
Cheelin
#975 Posted : 2/4/2022 3:00:15 AM

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orchidist wrote:
Finished my pulls, feeling pretty good about it. I got reverse osmosis water for this run, did 8 pulls with the recommended quantities, scaled for 25 grams. It was much easier without the lid in the way.

Pulls 1-6 are combined, very dark green, clear, a few specks of dust. 7 and 8 much lighter green, looks like there's a tiny amount of stuff to decant.

Decided to throw pulls 1-6 in my separatory funnel and leave it in there overnight for total confidence that there's no water. Of course, fancy thoughts like that anger the gods, and I forgot to close the stopcock, so I lost a few mL.


Looks great, if you have it in your sep funnel, it will start crystallizing on the walls…so plan accordingly.
 
orchidist
#976 Posted : 2/4/2022 3:07:47 AM

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Cheelin wrote:

Looks great, if you have it in your sep funnel, it will start crystallizing on the walls…so plan accordingly.


Thanks! I'm definitely not planning to salt it in the funnel, it'll move to a clean jar once I'm confident there's nothing in there that needs removed.
 
Loveall
#977 Posted : 2/4/2022 3:09:21 AM

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orchidist wrote:
Dirty cactus water sounds like a good trial. Regarding other contaminants, I remember way back in the thread that MgSO4 was detrimental in some way when used as a drying agent.(Having a hard time bringing it up with the search function though.) Perhaps Mg is problematic if it's present at earlier steps. I don't know the Mg content of my water, but with Mg being one of the most common minerals in tap water, a trial with MgSO4 in distilled water may be worth a try?


MgSO4 news problematic because it was impossible to filter from EA. Doesn't work well with the solvent. It is also slightly acidic, not ideal for our situation. After painstakingly settling/decanting/filtering Xatals where obtained after a MgSO4 dry. For EA other drying agents like CaCl2 and NaCO3 worked much better and without issues. Currently reccomending NaCO3 for anyone wanting to test drying the solvent before salting. Again, I saw no benefit from it, but if someone else is having water issues it could help.

You mention that you saw no ice after putting the extract in the freezer. Cheelin, isn't that unexpected? I thought we all got ice when putting used extract in the freezer 🤔?
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
_Trip_
#978 Posted : 2/4/2022 3:14:11 AM

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Cheelin wrote:
Good stuff _Trip_

If this takes off, maybe we set up a separate ‘Cactus Assay - Cielo Tek Utilization Studies (CA-CTUS)’ thread.



Actually not a bad idea.

I've got a spread sheet going of each 'strain'/ tricho species extractions I've down with Cielo Tek.
I've noted tek variations, HCL vs citrate %'s, season harvested, green skin vs wax layer vs whole cacti as well as grams tested and general notes.
Disclaimer: All my posts are of total fiction.



 
orchidist
#979 Posted : 2/4/2022 3:15:27 AM

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Loveall wrote:

You mention that you saw no ice after putting the extract in the freezer. Cheelin, isn't that unexpected? I thought we all got ice when putting used extract in the freezer 🤔?


I was surprised too. My only guess is that the excess I mistakenly used (nearly double the recommended amount for the quantity I was processing) diluted the water to the point that it's still soluble.
 
orchidist
#980 Posted : 2/4/2022 3:22:04 AM

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_Trip_ wrote:
Cheelin wrote:
Good stuff _Trip_

If this takes off, maybe we set up a separate ‘Cactus Assay - Cielo Tek Utilization Studies (CA-CTUS)’ thread.



Actually not a bad idea.

I've got a spread sheet going of each 'strain'/ tricho species extractions I've down with Cielo Tek.
I've noted tek variations, HCL vs citrate %'s, season harvested, green skin vs wax layer vs whole cacti as well as grams tested and general notes.



That would be awesome, I've been hoping for some cultivar recommendations. I'm looking out for my first plant.
 
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