Cheelin
Rising Star
Baby steps toward 1g runs, see update here: Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus
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TEK Ethyl acetate approach [CIELO]
- Thread starter Loveall
- Start date
This topic contain a TEK
Cheelin
Rising Star
Cloudy washed solvents are slowly settling, about half of each jar’s solvent layer is clear. Hopefully into freezer next week, 2nd reuse the following week.
Separately, have started 13 new runs on 1g samples, doing 3 separate trials of pastemaking variations, lots of crystals forming. Hopefully, a breakthrough coming.
One important observation that may apply to larger cactus powder runs:
I did a set of 1g cactus powder runs (focused on lime additions), where after adding the scaled quantity of citric acid, I stirred the citrate until it was fully dissolved (2-5min), white powder precipitated over the next 3-12 hrs, a la the rapid crystallization option (magnetic stirring).
The resulting powder (which was 1/2 the expected yield) did not taste as expected, in fact was “flavorless”, reminding me of calcium citrate.
Makes me question whether the purity of mag stirred product is the same as passively crystallized needles. Not saying there’s no M in there, just could there be less? Marquis test shows same orange-red reaction vs needles; but staining doesn’t give info on purity level or yield, just presence.
Could it be that, the extended & fast stirring causes some calcium binding/precip relative to M crystallization? Not a big deal for me, I only want to see those beautiful needles, and am willing to wait 2-3 days for them.
Separately, have started 13 new runs on 1g samples, doing 3 separate trials of pastemaking variations, lots of crystals forming. Hopefully, a breakthrough coming.
One important observation that may apply to larger cactus powder runs:
I did a set of 1g cactus powder runs (focused on lime additions), where after adding the scaled quantity of citric acid, I stirred the citrate until it was fully dissolved (2-5min), white powder precipitated over the next 3-12 hrs, a la the rapid crystallization option (magnetic stirring).
The resulting powder (which was 1/2 the expected yield) did not taste as expected, in fact was “flavorless”, reminding me of calcium citrate.
Makes me question whether the purity of mag stirred product is the same as passively crystallized needles. Not saying there’s no M in there, just could there be less? Marquis test shows same orange-red reaction vs needles; but staining doesn’t give info on purity level or yield, just presence.
Could it be that, the extended & fast stirring causes some calcium binding/precip relative to M crystallization? Not a big deal for me, I only want to see those beautiful needles, and am willing to wait 2-3 days for them.
orchidist
Rising Star
Hey! Feeling better now, pushed myself to do a few more iterations too.
Tried increasing citric acid, still oil, back to focusing on water.
With 15% less water in the paste, barely any clouds formed, seems like the M didn't make it out of the cactus that time.
This afternoon, used the normal amount of water and dried with NaCO3, then salted with Cheelin's recommended amount of citric acid. It has been about two hours, the walls of the jar are sparkly. Feeling confident about this one, friends!
Finally got to decant my first runs. Some extremely small grains appeared in the oily precipitate after adding more citric acid days ago, but nothing much changed since then. The part of the precipitate that stayed liquid was light brown, it lost most of that color and solidified when I washed with fresh solvent. All of it dissolved in water. Waiting for it to evaporate, hopefully will get some decent crystals out of those after all
Tried increasing citric acid, still oil, back to focusing on water.
With 15% less water in the paste, barely any clouds formed, seems like the M didn't make it out of the cactus that time.
This afternoon, used the normal amount of water and dried with NaCO3, then salted with Cheelin's recommended amount of citric acid. It has been about two hours, the walls of the jar are sparkly. Feeling confident about this one, friends!
Finally got to decant my first runs. Some extremely small grains appeared in the oily precipitate after adding more citric acid days ago, but nothing much changed since then. The part of the precipitate that stayed liquid was light brown, it lost most of that color and solidified when I washed with fresh solvent. All of it dissolved in water. Waiting for it to evaporate, hopefully will get some decent crystals out of those after all
orchidist said:
Interesting. Could it be that drying with Na2CO3 makes the process more robust for people that get goo?
Cheelin said:
I think there is no calcium in a clear extract, but I can't explain the difference in taste.
orchidist
Rising Star
Loveall said:
I wouldn't be surprised. I wonder if the mystery phytochemicals that your charcoal filtered out and subsequently released additional water from the EA are especially high in the material I'm working with and causing my problems. It's definitely cheap and easy enough that I would say a drying step is worth recommending to a first timer.
But that's still premature, if I do get nice crystals this time, I'll be more confident in saying that
orchidist
Rising Star
Surprise, I've been oiled again! Hmm. Followed proper procedure for drying solvent, the NaCO3 clumped as expected, added in portions until clumping stopped, then given a half hour to sit before filtering.
I think I'll be ordering a fresh package of citric acid, too lazy to do the work to determine if mine's hydrated and that's a possible source of extra water. It's been in my cupboard, only used from time to time in its original ziploc packaging for a while prior to this experimentation, though.
I think I'll be ordering a fresh package of citric acid, too lazy to do the work to determine if mine's hydrated and that's a possible source of extra water. It's been in my cupboard, only used from time to time in its original ziploc packaging for a while prior to this experimentation, though.
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Cheelin
Rising Star
While you’re at it, you might consider ordering/acquiring/using a different source of cactus powder, to help isolate the issue.
You don’t necessarily need a large quantity, just enough to know if you’re banging your head against the wall on the wrong problem.
I’m near 150 straight runs now, without ever encountering this issue, and I’ve tried pretty hard!
You don’t necessarily need a large quantity, just enough to know if you’re banging your head against the wall on the wrong problem.
I’m near 150 straight runs now, without ever encountering this issue, and I’ve tried pretty hard!
orchidist
Rising Star
Agreed. I am having doubts about the quality of my cactus. The decision paralysis is strong right now wrt choosing a new source, but I will make a choice soon.
In the meantime, I've also been thinking about washing/drying some of what I have with EA prior to making paste. I have a buchner funnel and manual pump on hand so pulling most of the solvent back out will be pretty easy.
In the meantime, I've also been thinking about washing/drying some of what I have with EA prior to making paste. I have a buchner funnel and manual pump on hand so pulling most of the solvent back out will be pretty easy.
Cheelin
Rising Star
Post tracking 1g cactus powder trials is updated, here: Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus
Separately, the reused solvents are in the freezer, hoping to get the third use (2nd reuse) runs going in the next few days.
Separately, the reused solvents are in the freezer, hoping to get the third use (2nd reuse) runs going in the next few days.
orchidist
Rising Star
EA washed powder + NaCO3 drying still oiled out. Had to do some digging to find a different (and distinct) vendor, but new flour is on order. A fresh bag of citric acid is also on the way.
While I was at it, finally went ahead on ordering a couple live cuttings for my collection Not just orchids anymore!
While I was at it, finally went ahead on ordering a couple live cuttings for my collection
Not just orchids anymore!
Cheelin
Rising Star
Still working to keep the flame of hope alive on small sample assay method.
No luck, yet, on 1g samples, though i’m only 10% low! Running out of ideas, so may switch to a predictive model approach.
BUT, did get a 2g sample to hit expected 1.1% yield! Made scaled 2g paste using standard method; then put it in a testube with 30mL fresh EA, stirred it 6 times with a chopstick, every 5 minutes for 30 seconds; after last stir rested 5 mins, filtered the loaded solvent through coffee filter-stainless funnel into a clean testube; rested for 1hr; salted w 0.1g citric acid, stirred a couple revolutions; passively crystallized for 72 hours; filtered, rinsed w EA, & air dried, water washed the tube, evaporated, and scraped residue.
No luck, yet, on 1g samples, though i’m only 10% low! Running out of ideas, so may switch to a predictive model approach.
BUT, did get a 2g sample to hit expected 1.1% yield! Made scaled 2g paste using standard method; then put it in a testube with 30mL fresh EA, stirred it 6 times with a chopstick, every 5 minutes for 30 seconds; after last stir rested 5 mins, filtered the loaded solvent through coffee filter-stainless funnel into a clean testube; rested for 1hr; salted w 0.1g citric acid, stirred a couple revolutions; passively crystallized for 72 hours; filtered, rinsed w EA, & air dried, water washed the tube, evaporated, and scraped residue.
Cheelin
Rising Star
cyantific said:
Thanks!
Lol, uncontrollable hardheadedness, and subsequent damage to the just-let-it-go lobe.
Regarding your question, which is above my paygrade, I’m going to have to refer that one to Loveall.
You might take 1/2-1g of it and do a test though.
Get 5g of powder, and using the std tek, scale all the other ingredients (in wiki) by multiplying them by 0.05, use same processes and times. For solvent, use 25% of scaled amount in 1st pull, divide the remainder by 5 for use in pulls 2 to 6. Also instead of scaling citric acid from 2.5g, scale it based on 5g.
This method has worked for goo, might work for tar. Would be nice if you could do your best to dry the tar out & then pulverize/powder it, before starting.
Cheelin said:
CIELO - DMT-Nexus Wiki
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