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Ethyl acetate approach [CIELO] Options
 
Cheelin
#1021 Posted : 2/7/2022 3:46:26 AM

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orchidist wrote:
Wish I'd taken pics, after the rest it was like dough. Moldable, but left a thin coating of itself behind when touched, which would dry quickly. Not sticky or slimy. Seemed within tolerance of the descriptions I've read here, and behaved as expected when exposed to solvent, but maybe could be dryer. When mixing it more resembled the stiff mashed potato description in the wiki.



It’s tuff getting grilled, I appreciate your great attitude.

Keep in mind you are improving, your chromatography shows you are extracting M.
 

Live plants. Sustainable, ethically sourced, native American owned.
 
orchidist
#1022 Posted : 2/7/2022 3:51:56 AM

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I'm SUPER happy about the chromatography! And I'm very much enjoying the back and forth here. There's nothing like a good puzzle.
 
Cheelin
#1023 Posted : 2/7/2022 4:22:43 AM

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Was your water 75mL and lime 6.25g?

If you think it might have been a tad too wet for your cactus, you could drop your water 10 - 15% or boost your lime 50%-100%.
 
Cheelin
#1024 Posted : 2/7/2022 5:45:20 AM

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Goo production trial #2, +/- Line or Citrate, final results are here: https://www.dmt-nexus.me...mp;m=1136901#post1136901
 
orchidist
#1025 Posted : 2/7/2022 5:51:07 AM

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All my attempts so far used 6.25g of lime

My first attempt, I scaled back the recommendation to withhold 30mL of the water, for a total of 67.5mL, and only used that. I didn't get much of a precipitate from that run, though it did test positive for M.

All of the subsequent attempts I used the full 75mL, based on prior conjecture that sufficient water is important in transporting the M from the cactus into the solvent. That did seem to be true for me, since the quantity of precipitate increased appreciably with the full dose of water (regardless of whether or not I forgot the coffee filter, my TLC was from the no filter run). I can't be quantitative about it yet, but the yield appears significantly better than the first run.

If I do make modifications to the paste recipe, I think from what I've seen so far, I'd choose to explore more lime over less water.

I have a couple variables to explore now, I think my priority list is going to be

1. Drop more acid
2. Increase lime in paste
3. Drying agents

That priority order may change after a few days as I observe my current runs
 
Cheelin
#1026 Posted : 2/7/2022 1:37:23 PM

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Good plan.

Any ice yet?
 
oetzi13
#1027 Posted : 2/7/2022 6:48:28 PM

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Cheelin, followed your instructions. Dissolved those crystal needles in water and ran through filter. Here is the result. Not too great. Looks dirtier than ever. Would you recommend an acetone wash on this?
oetzi13 attached the following image(s):
Screen Shot 2022-02-07 at 10.44.56 AM.png (422kb) downloaded 225 time(s).
Just don't
 
Cheelin
#1028 Posted : 2/7/2022 7:03:48 PM

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oetzi13 wrote:
Cheelin, followed your instructions. Dissolved those crystal needles in water and ran through filter. Here is the result. Not too great. Looks dirtier than ever. Would you recommend an acetone wash on this?



[I apologize for the major editing here. I was rushed at the time I originally responded, then had some time later to think it through some more.]

Looks one helluva lot better than the pics you posted earlier, imo.

It looks like you perhaps have 3 substances in there: proper product (white), fine plant matter sedimant (light brown), ?goo? (dark brown). Perhaps that large, dark brown stuff is just heavily grouped fine sediment, cuz I really don’t understand how goo could either make it through a coffee filter, or have dissolved with water to later reform during evap.

The sediment is a filtering issue, the goo is a recovery method issue, the white just needs to be separated from the other two.

You should have had a boatload of mucus-like/solid plant sediment left in your paper filter after a water wash (at least 60% of starting weight). But even the best paper filters can not trap it all. Somewhere earlier in this thread I demonstrated that cloudy solvent holds sediment finer than 2 microns that washes through filter paper. So, you will never get it all out without very advanced filtration techniques, if even those.

There are lots of proposed goo conversion/recovery methods on the net, perhaps you’ll find one that actually works well with this goo.

Keep in mind that every single time you do something new to your material you will lose some amount of the desired end product. So at some point, you have to make the call to live with what you have, and put your energy into improving your technique for future runs.

Your choice, of course, but if you want to put in the effort, I’d scrape-separate the white center and outer white rings from the predominantly dark rings, as best I could, and stop there for the white part. If the weight of the dark crap was a couple hundred mg or more, do a 5g or more recovery run (depending on quantity) on the dark remainder, (dry & powderize the dark stuff; double the amount of lime that would normally be required for the amount of cactus used in the recovery run).
 
Cheelin
#1029 Posted : 2/7/2022 7:33:05 PM

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orchidist wrote:
All my attempts so far used 6.25g of lime

My first attempt, I scaled back the recommendation to withhold 30mL of the water, for a total of 67.5mL, and only used that. I didn't get much of a precipitate from that run, though it did test positive for M.

All of the subsequent attempts I used the full 75mL, based on prior conjecture that sufficient water is important in transporting the M from the cactus into the solvent. That did seem to be true for me, since the quantity of precipitate increased appreciably with the full dose of water (regardless of whether or not I forgot the coffee filter, my TLC was from the no filter run). I can't be quantitative about it yet, but the yield appears significantly better than the first run.

If I do make modifications to the paste recipe, I think from what I've seen so far, I'd choose to explore more lime over less water.

I have a couple variables to explore now, I think my priority list is going to be

1. Drop more acid
2. Increase lime in paste
3. Drying agents

That priority order may change after a few days as I observe my current runs


Re drying: i have already demonstrated that freezing, even with added water, still can result in significant proper end product. We haven't done a freezing vs drying agent trial for runs that have not completed, so yields could be different. However freezing is a viable alternative for use in separating out water. Since there is a likelihood that any frozen water has dissolved M in it, the ice should be placed in an evap dish so that the product can be recovered.


The reason I added treatment 4 in Goo trial #1, was to test the of possibly recommending a freeze step after combining pulls - if goo production turned out to be simply due to too much water in the pulled solvent.

If excess water (coming either from the fresh solvent or the paste) is found to contribute in some way to goo formation, I’d do a side-by-side of the impact on yield from drying agent vs freezing.
 
orchidist
#1030 Posted : 2/8/2022 2:11:59 AM

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Cheelin wrote:
Any ice yet?


No ice in the fresh solvent at all. Will report back in a couple days when I decant the runs I have and freeze the solvent
 
Cheelin
#1031 Posted : 2/8/2022 2:31:22 AM

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orchidist wrote:
Cheelin wrote:
Any ice yet?


No ice in the fresh solvent at all. Will report back in a couple days when I decant the runs I have and freeze the solvent


This is consistent with my fresh EA, so any water/ice should be coming directly from the paste.
 
Cheelin
#1032 Posted : 2/8/2022 8:38:05 PM

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Cielo Great Success Method fully picturized here: https://www.dmt-nexus.me...mp;m=1137330#post1137330



Re Solvent Multiple Reuse Trial: gravity is taking its sweet ole time. Hopefully the haze will subside this coming weekend.
 
Cheelin
#1033 Posted : 2/9/2022 3:59:09 PM

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Food for thought…
Cheelin attached the following image(s):
Sacred Gummies.jpg (65kb) downloaded 158 time(s).
 
Cheelin
#1034 Posted : 2/9/2022 6:56:56 PM

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orchidist wrote:
Cheelin wrote:
Any ice yet?


No ice in the fresh solvent at all. Will report back in a couple days when I decant the runs I have and freeze the solvent



Are you seeing crystals in any of those jars?




Separately, re cloud after salting: since getting crystals hasn’t been a problem for me, and since i always get clouding after a quick stir when salting, i haven’t focused on what ‘not clouding’ means.

In my work on 1g runs: for grins, I’ve combined ‘spent’ pastes and re-pulled, some greenish hue in the combined pulls, but with sufficient (but not extreme) amount of fully dissolved citric, I get expected pH change, but absolutely no clouding. So, I’m expecting little or no crystals.
 
Cheelin
#1035 Posted : 2/10/2022 6:29:30 PM

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Quick update on appropriate salting that doesn’t result in clouding: the jar mentioned in the previous post has, after 24 hrs, remained clear, with pinpoint crystal dots scattered on walls & jar bottom, but no significant amount of product. I’ll weigh 72hr yield.




Separately, I ran the first run (2nd solvent use) of the multiple re-used solvent trial today. Update is here: https://www.dmt-nexus.me...mp;m=1137170#post1137170
 
orchidist
#1036 Posted : 2/11/2022 3:49:35 AM

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Cheelin wrote:
orchidist wrote:
Cheelin wrote:
Any ice yet?


No ice in the fresh solvent at all. Will report back in a couple days when I decant the runs I have and freeze the solvent


Are you seeing crystals in any of those jars?


Just checked my jars. Some good news! After a few days of nothing, I added more citric acid to both of my current jars yesterday. One stirred, one not. Stirring brought a lot of the oil droplets together into a puddle, nothing much seemed to happen besides that, at least immediately. Small crystals are forming in the puddle! The other, unstirred jar looks like it may be converting to crystals as well, but it's hard to tell, as the droplets in that jar are pretty small. Will leave it for another day or two and hope for full crystallization Big grin

Was planning to do another run this evening, but woke up feeling kinda crappy and haven't been able to shake it. Hopefully tomorrow will be better
 
Cheelin
#1037 Posted : 2/11/2022 4:04:01 AM

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Well, I hope the crystals grow, and you feel better soon. Take care!
 
PanaeolusSequence
#1038 Posted : 2/11/2022 2:10:08 PM

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Very thankful for this one!
 
Cheelin
#1039 Posted : 2/12/2022 8:54:44 PM

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A little update on my work to develop a weight-based assay approach for 1 gram cactus powder samples, using Loveall’s CIELO tek.

I have been able to successfully scale CIELO down to 5g cactus powder runs, and then tried to adapt the process to testtube-sized runs of 1 gram samples, using both the standard tek and a new process. Although I was able to produce the desired end product, I was unable to get more than 75% of the expected yield.

As a result, I scaled-back my speed of success expectations, and took a more systematic approach aimed at:
1. Identifying a reliable “pull” method that can produce the expected yield results.
2. Identifying a 1g pastemaking process that, when combined with 1, can reliably produce expected yield results.

I have already been able to achieve 1, using 5-10g paste batches sub-divided into 1 gram samples to do the extractions.

For example: 1g samples from a 10g batch, placed in a testube with 30mL fresh EA, for 30 minute extraction, passively crystallized with citric acid for 72 hrs: sample A received a 30 second stir (using a bamboo chopstick) at the beginning and end of the time period; sample B received a 30 second stir at the beginning; then 5 second stirs every 5 minutes; sample C received a 30 second stir at the beginning and every subsequent 5 minutes. Sample A yielded 1.1%, samples B and C yielded 1.2% with C slightly higher than B. All products appeared and tasted identical to passively crystallized standard product. Standard method on larger sample produces 1.1% with 6 pulls, rounding to 1.2% with 7. All weights taken on an Ohaus Pioneer, reading at 0.0000g.

[btw: In limited comparisons, when level and in a “calm” air location, a Thinkscale TKI-50, used only for weighing end-product (ie very clean), produced surprisingly similar readings at 0.000g.]

I am now working to optimize the method. Once that is done, and proven repeatable/reliable, I’ll move on to developing a simple and reliable pastemaking method for 1 gram powder samples.

2/15: Yields for 1g samples from a 5g batch (50% stepdown from “for example” above), using 30mL fresh EA: 30 min soak w 6 x 20sec stir every 5 min 1.0%, 30 min soak w 6 x 30sec stir every 5 min 1.1%, 30 min soak w 60sec stir every 5 min 1.2%, 40 min soak w 30 sec stir every 6.5 min 1.2%, 60 min soak 6 x 30sec stir every 10 min 1.3%.

Have several individually made 1g batches crystallizing, hopefully they give expected yields.

2/16: I think I’ve nailed the extractions of 1g equivalent samples subdivided from 5g or more cactus powder batches; but can’t do it with 1g individually prepared cactus powder pastes. Not sure what’s going/not going on. Going to throw some spaghetti on the wall, see what sticks. Will update when I have something useful.

2/20: 2 of the 3 most recent trials once again failed to achieve expected yield percentages. Very demotivating, but i’ll eventually sleep it off, and attack it again.

I tested 2-gram batches, split into 1g equivalent runs, with scaled dry mixed cactus powder and lime afterwards adding the water vs standard prep, then “pulling” with 30mL fresh EA stirred 6x for 30 seconds over a 30 min period, then passively crystallizing for 72 hrs with 0.1g citric acid. I produced what appeared to be the expected quality needles, with both mixing methods having similar yield, but the yields were in the 0.9% range rather than the 1.1% range.

I have already demonstrated that 5-10g batches split into 1g equivalents produce the expected yields, using the same “pulling” method as above, so the issue is with smaller paste batches. In my next attempt i’ll run 2 g batches without splitting them, see if i can get expected yield.

I also tested 1g batches the same way as the trial above, and got similar results.

I have already dried the filtrate, but still have to evap the tube wash, from a 5g batch split into 1g equivalent runs; which was testing citric acid additions 0.05g to 2.5g in 0.5g increments. I expect all or most of these to hit expected yield levels, since the filtered product alone is close to or above 1.0%. So, once again, I expect that the issue related to hitting the expected yield in 1g cactus powder paste batches is in the pastemaking process.

I’ll update this post one more time with the citric acid trial yields. Future work will be presented in a new post.




[I’d like to once again call on anyone who has a titrimetric analysis background to take up the challenge of creating such a tek for assaying even smaller samples using CIELO. Such a tek would provide a groundbreaking opportunity to move knowledge forward wrt to both breeding and harvesting of mescaline-producing cacti. Perhaps a CIELO-based titration method could be produced providing a simple color-change(s) at a given %M yield(s).]
 
Cheelin
#1040 Posted : 2/13/2022 5:35:45 PM

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Solvent Multiple Reuse trial updated here: https://www.dmt-nexus.me...mp;m=1137170#post1137170
 
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