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TEK Ethyl acetate approach [CIELO]

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

What's the math to get the percent of 1.5 ?
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Something’s wrong. Better send me that cactus, so i can properly dispose of it.








Lol, nice yield there!
 
Cheelin said:
Something’s wrong. Better send me that cactus, so i can properly dispose of it.
Lol, nice yield there!
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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.
 
cyantific said:
Cheelin said:
Something’s wrong. Better send me that cactus, so i can properly dispose of it.
Lol, nice yield there!
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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.
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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.
 
Loveall said:
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.
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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.
 
Cheelin said:
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?
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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?
 
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.
 
Cheelin said:
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?
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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 said:
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.
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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.
 
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 said:
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.
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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.
 
downwardsfromzero said:
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.
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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.
 
Extrapolating from this article, I think the solvent temperature is looking much more like my problem.

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.
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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.
 
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!
 
Cheelin said:
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!
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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
 
cheelin said:
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.
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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.
 
I was just rereading the thread and pretty much immediately stumbled upon this. Shroombee was getting oily results when using cold solvent during the early stages of refining the tek.

shroombee said:
So, your dish got cloudy, but no crystals formed, right? That's too bad. Yeah you can definetly throw it in the freezer directly. The fridge -> freezer sequence is just to understand what happens at different temps. Also, bigger xtals form when the temp is lowered gradually, but that is not very important now.
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Right, cloudy but no crystals formed. I'm throwing it in the freezer. I tipped the dish and now realize there is an oily substance dotted across the bottom. Earlier, it didn't seem to move when I scraped at it through the solvent with a knife (and seeing some oil droplets on the surface), leading me to believe it was an illusion. But it's real. It's not water. I put a little on white paper to confirm its oily.
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orchidist said:
cheelin said:
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.
Click to expand...

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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I’ll defer to the textbook re: “super saturation”.

I don’t think the M citrate will dissolve in EA without basing it, heat or not.
 
Completed pulls this morning with 35 grams, the remainder of my peruvian torch powder.

During extraction, I recorded the ambient temperature, relative humidity, and temperature of the solvent immediately before adding it to the paste.

Ambient temperature: Average 68.3F | Min 68 | Max 70
Solvent temperature: Average 67F | Min 66 | Max 70
Humidity%: Average 54.6% | Min 54% | Max 56%

I do believe the discrepancy is due to offset from one or the other from the actual value, as the probe disagreed with the ambient temperature sensor by a constant amount by 2F on the majority of the measurements. I'm inclined to believe the probe I used to check the solvent is the one that's inaccurate, as it's meant to be a candy/meat thermometer.

The combined pulls have been dried and filtered, and split into two portions:

Portion 1: 2/3 of the solvent, will be salted with citric acid the usual way
Portion 2: 1/3 of the solvent, fumaric acid

The solvent is now hanging out in my bedroom, where it's a nice 72F, and in a few hours, when I'm sure it's in equilibrium, I will salt both.

To salt the entire quantity of solvent for this amount would call for 1.75g of citric acid, so the split would be

Portion 1:

CA Dose = 2/3 * 1.75g
CA Dose = 1.17g

Portion 2:

Scaling factor = 116.072 (FA Molar Mass) / 192.073 (CA Molar Mass)
Scaling factor = 0.6

FA Dose = 1/3 * 1.75g * 0.6
FA Dose = 0.35g

Does that look right?
 
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