Cheelin
Rising Star
2nd used solvent re-use (3rd use) has been updated 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 said:
Maybe some M remains in solution. I see the 2%+ higher yields in your reused solvent post.
Maybe you could try salting after washing freezing/filtering. See if you get needles or powder.
Cheelin
Rising Star
Loveall said:
It passed through both ears, earlier…salting clears the solvent beautifully regardless of whether there is residual M…but i declined, cuz I didn’t want to deal with re-adding sodium carb to re-neutralize, and probably increase the haze. But, after the ridiculous excess yield this time, I’ll salt, then try a no/low stir of sodium carb to re-neutralize.
Also going to back off on the heavy stirring on the initial wash, in hopes of reducing cloudiness/haze to begin with…i’m thinking that the extra yield is likely calcium citrate not residual M (but it’s time to make sure).
In the end, after neutralizing pH, gravity (i.e. time) is probably the best clarifier/anti-contaminant for this tek’s used solvent.
orchidist
Rising Star
Hey, checking in on my oily M saga.
New Cactus Powder
I received two samples of powder from (allegedly) two species, one San Pedro, one Peruvian Torch. Flipped a coin, worked on the PT today. Definitely noticed differences between it and what I've been working on the last few weeks.
The new powders are much brighter, fresher looking green than the old powder. Using the same water proportions, the paste was much stiffer, was a much more crumbly consistency at the end of mixing in comparison to the old cactus. One thing I noticed different while preparing the paste was the smell. After a few minutes of stirring, the old paste would take on a slight ammonia note. The new paste had none of that, just a fresh herbaceous smell. While extracting, the new paste behaved much more in line with Cheelin's descriptions. After decanting solvent, the mass of cactus paste was dense enough to be crumbled apart, the old cactus paste remained quite loose throughout the process (and reducing water content to obtain that consistency resulted in no clouds on salting).
I'm hopeful this new batch will produce good results.
Still trying to get the old stuff work
TLDR: The re-x from water didn't fix my amorphous product, my idea to wash the solvent before salting didn't help. I will redissolve, freebase with Na2CO3, extract into EA and salt again in hopes of better purity and crystallization, because I'm worried the contaminant might ruin runs with good cactus powder
Last week I dissolved and evaporated the oily precipitate from my first two attempts in some water. Unfortunately, this didn't crystallize, it is now a clear, light brown amorphous solid.
This led to the thought that if there's some contaminant/adulterant preventing crystallization that's water soluble, an aqueous wash of the solvent while the M is still freebase might fix my problems. So that's what I did. I washed the solvent with saturated Na2CO3 3x. During the process, some dark green solids collected at the interface and were removed. After the final wash, I allowed it to settle overnight, then dried the solvent with solid Na2CO3 before filtering and salting. Unfortunately, it still precipitated as oil. So, either my contaminant is not soluble in saturated Na2CO3, or it forms as the solvent becomes acidic, or there's another alkaloid interfering. I'd be surprised about that last one, since my TLC plate only showed M. I'm going to run another TLC for a sanity check.
If my run with the new powder is a success, I'm still a bit (probably unreasonably) wary of adding the failed M with whatever problematic substance is contained in it to a batch of good cactus, so I'm waiting on the delivery of a tiny separatory funnel (due tomorrow). When that arrives, my plan is to dissolve the amorphous M into some water, base with Na2CO3, extract with fresh EA, and then salt it again with citric acid. I know there will be losses, but the allure of those sweet sweet crystals (and chemistry funtimes) overrides all.
New Cactus Powder
I received two samples of powder from (allegedly) two species, one San Pedro, one Peruvian Torch. Flipped a coin, worked on the PT today. Definitely noticed differences between it and what I've been working on the last few weeks.
The new powders are much brighter, fresher looking green than the old powder. Using the same water proportions, the paste was much stiffer, was a much more crumbly consistency at the end of mixing in comparison to the old cactus. One thing I noticed different while preparing the paste was the smell. After a few minutes of stirring, the old paste would take on a slight ammonia note. The new paste had none of that, just a fresh herbaceous smell. While extracting, the new paste behaved much more in line with Cheelin's descriptions. After decanting solvent, the mass of cactus paste was dense enough to be crumbled apart, the old cactus paste remained quite loose throughout the process (and reducing water content to obtain that consistency resulted in no clouds on salting).
I'm hopeful this new batch will produce good results.
Still trying to get the old stuff work
TLDR: The re-x from water didn't fix my amorphous product, my idea to wash the solvent before salting didn't help. I will redissolve, freebase with Na2CO3, extract into EA and salt again in hopes of better purity and crystallization, because I'm worried the contaminant might ruin runs with good cactus powder
Last week I dissolved and evaporated the oily precipitate from my first two attempts in some water. Unfortunately, this didn't crystallize, it is now a clear, light brown amorphous solid.
This led to the thought that if there's some contaminant/adulterant preventing crystallization that's water soluble, an aqueous wash of the solvent while the M is still freebase might fix my problems. So that's what I did. I washed the solvent with saturated Na2CO3 3x. During the process, some dark green solids collected at the interface and were removed. After the final wash, I allowed it to settle overnight, then dried the solvent with solid Na2CO3 before filtering and salting. Unfortunately, it still precipitated as oil. So, either my contaminant is not soluble in saturated Na2CO3, or it forms as the solvent becomes acidic, or there's another alkaloid interfering. I'd be surprised about that last one, since my TLC plate only showed M. I'm going to run another TLC for a sanity check.
If my run with the new powder is a success, I'm still a bit (probably unreasonably) wary of adding the failed M with whatever problematic substance is contained in it to a batch of good cactus, so I'm waiting on the delivery of a tiny separatory funnel (due tomorrow). When that arrives, my plan is to dissolve the amorphous M into some water, base with Na2CO3, extract with fresh EA, and then salt it again with citric acid. I know there will be losses, but the allure of those sweet sweet crystals (and chemistry funtimes) overrides all.
orchidist
Rising Star
So far, not that I can tell, which I guess isn't the best sign... Just clouds, which are settling. About 1/4" of the solvent on bottom has gone from green to yellow, where I imagine the CA concentration is highest, which has been the norm for all of my runs (and exclusively where all of the oil collects too). The top 1/8" has cleared up as the clouds begin to settle.
Cheelin, when you stir your CA into the solution, do you continue stirring until it's dissolved, or do you leave some undissolved sitting on the bottom of the vessel? Currently I'm only giving mine a few stirs, which does leave a little mound of solid CA in the center of the jar.
I need to invest in a good flashlight for pictures of my solutions. The one I have uses an oscillator based voltage booster circuit to drive its LED, and it's at just the right frequency to make my camera go nuts--unless I tweak the exposure just right (which usually makes the most important details invisible), and then stay COMPLETELY still, the image gets dark and light bars from the constant flickering of the light :|
Cheelin, when you stir your CA into the solution, do you continue stirring until it's dissolved, or do you leave some undissolved sitting on the bottom of the vessel? Currently I'm only giving mine a few stirs, which does leave a little mound of solid CA in the center of the jar.
I need to invest in a good flashlight for pictures of my solutions. The one I have uses an oscillator based voltage booster circuit to drive its LED, and it's at just the right frequency to make my camera go nuts--unless I tweak the exposure just right (which usually makes the most important details invisible), and then stay COMPLETELY still, the image gets dark and light bars from the constant flickering of the light :|
Cheelin
Rising Star
My stir is 2-3 revolutions. I can then see some cloudiness form, citrate doesn’t dissolve much.
When clearing starts, it starts slowly from the top.
Within an hour, i can see tiny dots on the jar walls; by 3 hrs tiny spider webs/snowflakes. They are visible just by shining light on the walls, you don’t have to shine the light through the jar.
When clearing starts, it starts slowly from the top.
Within an hour, i can see tiny dots on the jar walls; by 3 hrs tiny spider webs/snowflakes. They are visible just by shining light on the walls, you don’t have to shine the light through the jar.
orchidist
Rising Star
Yeah...looks like the first indications of oil. Ugh. Really thought I had it this time. Everything looked great throughout the entire process 
The only thing in this process I haven't replaced so far is my solvent. It passes the evap test, but perhaps this lot isn't pure EA? The uncertainty in the powder still remains. Probably should just get a cutting and process it myself to be sure what I'm working with doesn't have some kind of nonsense mixed in.
The only thing in this process I haven't replaced so far is my solvent. It passes the evap test, but perhaps this lot isn't pure EA? The uncertainty in the powder still remains. Probably should just get a cutting and process it myself to be sure what I'm working with doesn't have some kind of nonsense mixed in.
Cheelin
Rising Star
A hint of optimism on the small sample assay approach.
1g cactus powder, scaled lime, 2mL distilled water (1:2 ratio instead of 1:3 std ratio), std stir and rest.
8 pulls (1min stir, 2min rest); 1st pull 5mL fresh EA, pulls 2-8 pulls 3mL
0.1g citric, 72 hrs passive crystallization.
The closest yet: 0.0105g, round it how you like, 1.0 or 1.1% vs expected yield of 1.1%.
Will try to replicate.
1g cactus powder, scaled lime, 2mL distilled water (1:2 ratio instead of 1:3 std ratio), std stir and rest.
8 pulls (1min stir, 2min rest); 1st pull 5mL fresh EA, pulls 2-8 pulls 3mL
0.1g citric, 72 hrs passive crystallization.
The closest yet: 0.0105g, round it how you like, 1.0 or 1.1% vs expected yield of 1.1%.
Will try to replicate.
orchidist
Rising Star
Haven't had time to do another run with the other powder, but I've got some other interesting stuff going on with my amorphous M from the failed attempt to re-X by evaporation.
Did another TLC, same result, single spot testing positive for M by marquis.
I dissolved the M in water, then attempted to wash with EA in hopes of removing the color from the solution--the EA remained clear, so I proceeded to basing the solution with sodium carbonate, and repeatedly extracting with ~20 mL portions of EA, testing each wash by placing a drop of the solvent onto a plate of glass and adding a single crystal of citric acid, and observing for clouds. There's still some M left in the solution based on this test, but it tapered off enough, and I was running short on patience. I ended up with a total of 160mL of EA. After filtering and drying, the solvent was crystal clear with only a slight hint of color to it. The aqueous solution retained most of the color, but some did come over after basing.
After all of that, I proceeded to salt the solution, this time I simply added the acid without stirring. Clouds formed nicely. Some hours later, it is once again precipitating as an oil. Can I get points for consistency? :lol:
Loveall and Cheelin, around what ambient temperature are you working at when you salt, and how rapidly does the citric acid dissolve? About 6 hours later, I still have some CA crystals undissolved. I'm imagining both of you are in relatively hotter climates than mine. Wonder if that might be a factor in all this.
I'm feeling pulled back to the idea that I'm somehow consistently getting tri or di-M citrate. The pH of the dissolved amorphous M was ~6, which seems consistent with Loveall's description many pages ago. The mechanism I'm imagining is that at a cooler temperature, the acid dissolves more slowly, which then inhibits formation of mono-M crystals. Grinding the CA into a fine powder may overcome this if that's the case.
I have a few other runs to decant, plus the product of this experiment. I'll add some additional citric acid to the mix when I dissolve it in water, and see if that produces the expected crystallization.
Did another TLC, same result, single spot testing positive for M by marquis.
I dissolved the M in water, then attempted to wash with EA in hopes of removing the color from the solution--the EA remained clear, so I proceeded to basing the solution with sodium carbonate, and repeatedly extracting with ~20 mL portions of EA, testing each wash by placing a drop of the solvent onto a plate of glass and adding a single crystal of citric acid, and observing for clouds. There's still some M left in the solution based on this test, but it tapered off enough, and I was running short on patience. I ended up with a total of 160mL of EA. After filtering and drying, the solvent was crystal clear with only a slight hint of color to it. The aqueous solution retained most of the color, but some did come over after basing.
After all of that, I proceeded to salt the solution, this time I simply added the acid without stirring. Clouds formed nicely. Some hours later, it is once again precipitating as an oil. Can I get points for consistency? :lol:
Loveall and Cheelin, around what ambient temperature are you working at when you salt, and how rapidly does the citric acid dissolve? About 6 hours later, I still have some CA crystals undissolved. I'm imagining both of you are in relatively hotter climates than mine. Wonder if that might be a factor in all this.
I'm feeling pulled back to the idea that I'm somehow consistently getting tri or di-M citrate. The pH of the dissolved amorphous M was ~6, which seems consistent with Loveall's description many pages ago. The mechanism I'm imagining is that at a cooler temperature, the acid dissolves more slowly, which then inhibits formation of mono-M crystals. Grinding the CA into a fine powder may overcome this if that's the case.
I have a few other runs to decant, plus the product of this experiment. I'll add some additional citric acid to the mix when I dissolve it in water, and see if that produces the expected crystallization.
That is so interesting orchidist. Sounds like you ruled out both excess water and contamination with your latest A/B.
It can take a little longer for the larger citric granules to passively dissolve, especially after drying the EA, but eventually they do. As long as I don't starve the solution and add excess acid (even when passively dissolving) I always get xtals. How much citric acid did you add.
What brand of ethyl acetate solvent are you using and do you have the MSDS? Same for your brand of citric acid, what is it? Do you have an MSDS for your brand of citric? You mentioned before that you may try a different brand of EA, have you done that? Seems like you simply have M, EA, and Citric left and are still not getting xtals so we should carefully look at you your materials (sometimes vendors add anti-caking agents, etc).
Edit: Do you have fumaric or tartaric acid? That xtalized mescaline from EA well, you could test that too as part of troubleshooting.
It can take a little longer for the larger citric granules to passively dissolve, especially after drying the EA, but eventually they do. As long as I don't starve the solution and add excess acid (even when passively dissolving) I always get xtals. How much citric acid did you add.
What brand of ethyl acetate solvent are you using and do you have the MSDS? Same for your brand of citric acid, what is it? Do you have an MSDS for your brand of citric? You mentioned before that you may try a different brand of EA, have you done that? Seems like you simply have M, EA, and Citric left and are still not getting xtals so we should carefully look at you your materials (sometimes vendors add anti-caking agents, etc).
Edit: Do you have fumaric or tartaric acid? That xtalized mescaline from EA well, you could test that too as part of troubleshooting.
Cheelin
Rising Star
My temp is around 70-72F. I haven’t paid much attention to the dissolution time of the citric crystals, partly because the cloudiness and M crystallization obscures the view, certainly by the time the solution starts getting clear at the top.
I agree with Loveall, what EA and Citrate products are you using? Not much else to check.
Maybe a “threshold” dose of that goo, say 150-200mg?
I agree with Loveall, what EA and Citrate products are you using? Not much else to check.
Maybe a “threshold” dose of that goo, say 150-200mg?
cyantific said:
You mean 447mg for 30g of cactus? That's 1.5% yield for citrate, ~0.9% HCl equivalent. A solid yield
