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Ethyl acetate approach [CIELO] Options
 
cyantific
#1081 Posted : 3/3/2022 8:16:44 PM

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How would you calculate percent yield?

Pulled 447mg from 30g.

Thank you Loveall, and fam. This is such a beautiful documentation of plant science.
 

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Loveall
#1082 Posted : 3/3/2022 8:19:58 PM

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cyantific wrote:
How would you calculate percent yield?

Pulled .447mg from 30g.

Thank you Loveall, and fam. This is such a beautiful documentation of plant science.


You mean 447mg for 30g of cactus? That's 1.5% yield for citrate, ~0.9% HCl equivalent. A solid yield 👍
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
cyantific
#1083 Posted : 3/3/2022 8:31:51 PM

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Correct, 447mg with 30g. starting material. (I accidentally added a period before 447)

What's the math to get the percent of 1.5 ?
 
Loveall
#1084 Posted : 3/3/2022 8:58:14 PM

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cyantific wrote:
Correct, 447mg with 30g. starting material. (I accidentally added a period before 447)

What's the math to get the percent of 1.5 ?


Percent = 0.447g/30g * 100 ~ 1.59%
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#1085 Posted : 3/3/2022 9:03:39 PM

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cyantific wrote:
Correct, 447mg with 30g. starting material. (I accidentally added a period before 447)

What's the math to get the percent of 1.5 ?



Something’s wrong. Better send me that cactus, so i can properly dispose of it.








Lol, nice yield there!
 
cyantific
#1086 Posted : 3/3/2022 9:43:50 PM

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Cheelin wrote:
Something’s wrong. Better send me that cactus, so i can properly dispose of it.
Lol, nice yield there!


Haha thanks, it was a nice Pachanoi. I was pretty methodical about removing the waxy skin, core, spines and white flesh. The starting material was 30g of just the outer green layer. Dried in a dehydrator and powdered w/ a manual burr grinder. Labor of love.
 
Cheelin
#1087 Posted : 3/3/2022 11:33:17 PM

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cyantific wrote:
Cheelin wrote:
Something’s wrong. Better send me that cactus, so i can properly dispose of it.
Lol, nice yield there!


Haha thanks, it was a nice Pachanoi. I was pretty methodical about removing the waxy skin, core, spines and white flesh. The starting material was 30g of just the outer green layer. Dried in a dehydrator and powdered w/ a manual burr grinder. Labor of love.


If you didn’t save the white flesh (not the core), do so and dehydrate next time. Then run that at your leisure. Should be worthwhile.

Glad you nailed the tek.
 
orchidist
#1088 Posted : 3/4/2022 3:00:22 AM

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Loveall wrote:
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.


Yeah, I definitely noticed a delay in dissolution with dried solvent. For 50g cactus, I'm using 2.5g of citric acid.

My EA is Kleen Strip MEK Substutute, the MSDS lists 100% Ethyl Acetate (suspicious). Both of my local stores carry this brand. The EA I used to do the re-AB was from a different can than what I used for all my other extractions. That can was purchased a few weeks later. I just checked both cans to see if I could find lot numbers. I found manufacturing dates and a code printed underneath, and they're different, but I don't know if that necessarily means they came from different production runs. May have to hop around to different hardware stores and see if anyone has Jasco.

For citric acid, Milliard. Should be anhydrous and no anti-caking agents

I do have fumaric acid on hand. I was planning to give it a try this weekend.
 
orchidist
#1089 Posted : 3/4/2022 3:14:07 AM

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Cheelin wrote:
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?


The area where I keep the jars to salt is around 67F, but my EA almost certainly colder when I first throw in the CA, since the space where I perform the extraction has been in the 40 degree range due to ventilation. I'll pay attention to that as I proceed.

Anybody willing to try salting in the fridge?
 
Cheelin
#1090 Posted : 3/4/2022 4:13:10 AM

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My first thought is WTF?!

You are using what i use for solvent and citric. I’ve bought multiple gallons of Kleen Strip, at different stores & locations, at different times; Jasco, too. I have not noticed any difference, or had any problems.

I wish I could send you some of my powder.

I’ll do a cold salting and more. But do me a favor: go to the “Great Success” recipe (Loveall has a link to it in the wiki) and identify any differences in your materials, equipment, and process that you use. I will replicate it exactly, with a 15g run. Tell me what temp you want me to salt at?

I am a little confused about why your salting occurs in cold pulls. I do my whole pastemaking and pull process in less than an hour, in my 70-72F kitchen (my EA cans are store in an unheated room that ranges 40-60F, but i keep a 1qt jar of it in my pantry at same temp as kitchen); let the combined pulls sit there for 1hr, then salt.
 
orchidist
#1091 Posted : 3/4/2022 5:15:38 AM

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Cheelin wrote:

My first thought is WTF?!

You are using what i use for solvent and citric. I’ve bought multiple gallons of Kleen Strip, at different stores & locations, at different times; Jasco, too. I have not noticed any difference, or had any problems.

I wish I could send you some of my powder.


I’ll do a cold salting and more. But do me a favor: go to the “Great Success” recipe (Loveall has a link to it in the wiki) and identify any differences in your materials, equipment, and process that you use. I will replicate it exactly, with a 15g run. Tell me what temp you want me to salt at?


Will do. I'm thinking 60 degrees may be a decent starting point. I'm not certain what temperature my solvent ended up reaching during the process.

Cheelin wrote:

I am a little confused about why your salting occurs in cold pulls. I do my whole pastemaking and pull process in less than an hour, in my 70-72F kitchen (my EA cans are store in an unheated room that ranges 40-60F, but i keep a 1qt jar of it in my pantry at same temp as kitchen); let the combined pulls sit there for 1hr, then salt.


The room where I do my pulls has not been the same room as where I have been leaving the jars to crystallize. The workspace I've set up is a room that doesn't get good heating in general, so everything starts out probably in the mid to low 60F range (I'll get a thermometer to put in there). While I work, I use a window box fan to force air exchange, making the room a lot colder (it's been in the 20's here a few nights when I've done extractions), and circulating that air around the solvent. Once I finished my work in that room, I'd bring the jar to the kitchen, measure my citric acid, add it, then place it on a shelf in the living room (67-68F). So, the solvent is almost certainly colder than ambient at the moment I salt it. Exactly how much colder, I haven't recorded.
 
Cheelin
#1092 Posted : 3/4/2022 5:32:37 AM

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Is there any way that you can do the entire pastemaking through salting in a constant ~68 - 72F environment, with all ingredients & equip at ambient before starting?

I’m wondering if temp is affecting reactions.
 
orchidist
#1093 Posted : 3/4/2022 5:52:14 AM

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Yep, there are a few warm days in the forecast, so it won't be a big deal to ventilate the kitchen if I work in there.
 
downwardsfromzero
#1094 Posted : 3/4/2022 8:31:34 PM

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orchidist wrote:
The room where I do my pulls has not been the same room as where I have been leaving the jars to crystallize. The workspace I've set up is a room that doesn't get good heating in general, so everything starts out probably in the mid to low 60F range (I'll get a thermometer to put in there). While I work, I use a window box fan to force air exchange, making the room a lot colder (it's been in the 20's here a few nights when I've done extractions), and circulating that air around the solvent. Once I finished my work in that room, I'd bring the jar to the kitchen, measure my citric acid, add it, then place it on a shelf in the living room (67-68F). So, the solvent is almost certainly colder than ambient at the moment I salt it. Exactly how much colder, I haven't recorded.

One thing with moving cold solvent into a warmer room is it may cause water to condense into it. This is one good reason for doing the extraction at a constant temperature throughout. I'd be inclined to suggest you may be being a little over-zealous with your ventilation.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Cheelin
#1095 Posted : 3/4/2022 9:30:52 PM

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Started 3rd wash of variously-treated solvents, in preparation for 3rd reuse (4th use) trial; see here: https://www.dmt-nexus.me...mp;m=1137170#post1137170
 
orchidist
#1096 Posted : 3/5/2022 2:25:41 AM

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downwardsfromzero wrote:

One thing with moving cold solvent into a warmer room is it may cause water to condense into it. This is one good reason for doing the extraction at a constant temperature throughout. I'd be inclined to suggest you may be being a little over-zealous with your ventilation.


Yeah, I figured keeping it capped for all but the time it took to dump in CA would be sufficient to prevent that, but it might be a factor.

The ventilation does feel somewhat necessary, it's not a very big room, so the vapors do tend to build up to headache-inducing levels despite my best efforts to keep them to a minimum, by keeping the lid on the press whenever possible, keeping containers of measured solvent covered until needed, etc. With a little bit of effort rearranging the room though, I may be able to at least move the work a few feet away from the fans.

That said, I've been thinking about temperature, and another thing I noticed early on came to mind. I was shining an LED flashlight against a jar of clouded salted solvent that had begun to form a clear layer on top. I noticed after a few seconds, the cloudy layer began to push upward, as if by convection. Investigating further, I could make this happen even with the light a few inches away from the jar.

If the clouds are fine enough that they can be moved around by the energy they absorb fro a a flashlight, I think it's definitely plausible that convection currents induced by a couple degrees of temperature differential are stirring the solvent just enough to inhibit crystal formation.
 
orchidist
#1097 Posted : 3/5/2022 3:31:00 AM

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Extrapolating from this article, I think the solvent temperature is looking much more like my problem.

Quote:

Supersaturation. When the supersaturation degree (As
shown in Figure 3) is too high (the value of σ is too high) or the
supersaturating rate (i. e. cooling rate, from point a to point b)
is too fast during the crystallization, oiling-out might
occur.


Seems plausible that in a colder solvent, salting the M all at once will put the concentration of M-Citrate so far into supersaturation, it oils out instead of crystallizing.
 
Cheelin
#1098 Posted : 3/5/2022 3:51:08 AM

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Edit: Low/inconsistent temp could be the issue. But, not sure about using the term ‘super saturation’ in this case. Super-Saturation generally occurs at high temps. But whatever, there is some crystallization issue going on, given that your goo is testing positive for M.

Btw, re DFZ’s comment, I may be wrong, but haven’t you already ruled out water in your solvent, by doing a test with “dried” solvent?



I bet that full article is a good one, the first page hits at least a couple of related topics (e.g. citrate).

Good find!

Lookin forward to seeing if warm, consistent temps make the difference. Good luck!
 
orchidist
#1099 Posted : 3/7/2022 1:51:36 AM

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Cheelin wrote:
Edit: Low/inconsistent temp could be the issue. But, not sure about using the term ‘super saturation’ in this case. Super-Saturation generally occurs at high temps. But whatever, there is some crystallization issue going on, given that your goo is testing positive for M.

Btw, re DFZ’s comment, I may be wrong, but haven’t you already ruled out water in your solvent, by doing a test with “dried” solvent?



I bet that full article is a good one, the first page hits at least a couple of related topics (e.g. citrate).

Good find!

Lookin forward to seeing if warm, consistent temps make the difference. Good luck!


Yes, drying the solvent didn't help with oiling, and with your experiments adding as much as a mL of extra water without issue, I don't think that'd be likely. I also did keep the jar capped while outside of my workspace at all times except for the moment of adding the citric acid. There were times where a small amount of condensation formed on the outside of my jar when leaving the room, but by the time I got to salting, it had warmed to the point that water wasn't condensing on the outside of the jar.

I picked up a few indoor temperature sensor to put in my workspace, in the living room, and a few other unrelated places yesterday evening. All of them were in agreement when I turned them on in the same room as a test.

Workspace: 59F-61F, with windows closed, not much change with the weather. (The room is partially underground due to the construction of the building, which contributes to the persistent cooler temps)

Living room: 64F-68F, and went up to 70 as the temperature warmed today.

The joys of old poorly insulated buildings! Not very confident in the stability of the temperature of my living room now, going to set up a room with a space heater and tweak it until it holds the right temp, I guess
 
orchidist
#1100 Posted : 3/7/2022 2:14:25 AM

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cheelin wrote:

Low/inconsistent temp could be the issue. But, not sure about using the term ‘super saturation’ in this case. Super-Saturation generally occurs at high temps. But whatever, there is some crystallization issue going on, given that your goo is testing positive for M.


Saturation is defined as the concentration of a solute in solution when it is in equilibrium with the solid form of the solute. Any concentration above that is supersaturated. You can get to supersaturation by saturating at one temperature, then change the temperature to one where the compound is less soluble, or by other means such as generating a large amount of the solute via chemical reaction. Either way you get there, the system moves toward equilibrium by precipitating the solute.

One thing I would like to try as I work more with this is to see if M-citrate dissolves in warm/hot EA. If it does, that may be a convenient way to clean up oily product.
 
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