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TEK Ethyl acetate approach [CIELO]

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fiM said:
Mmmhhh my test subject goo dryed to this???? Good or just the citric wadda think,,,,,looks awesome thinking of smashing a bit not sure which looks the best
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Sorry, I can't follow exactly what you did or what pictures are from what steps.

Sounds like you had some good from too much water in your EA, decanted that and started getting xtlas (since the goo itself took out some water). Not sure what happened after that.

All the info you need is hopefully in the TEK. If you have a specific question I can try to answer it.
 
I'm trying a quick test of fumaric acid solubility in ethyl acetate since the only literature i could find seemed to indicate ~2.38mg/g @~75F which is pretty low compared to citric acid certainly. I started with 5mg/g assuming my conversions or study i was reading were wrong somehow, but i can't even get 5mg/g to fully dissolve! I'm heating it up to ~115F now to see if that dissolves it and if it doesn't I'll add ~2% water to emulate CIELO.

edit: so heating up to 115F didn't help, there was still relatively alot of fumaric acid on the bottom. But adding ~2.3% water has almost fully dissolved it with just a few particles on the bottom after stirring awhile.
edit: added more fumaric to bring up to 7.5mg/g total and it dissolved over time as well, however going up to 10mg/g still has significant fumaric acid on the bottom so i'll give it a few more hours...
edit: hours later 10mg/g also dissolved, well i'm outta time but maybe i'll double it in a few days and see
 
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Loveall said:
Sorry, I can't follow exactly what you did or what pictures are from what steps.

Sounds like you had some good from too much water in your EA, decanted that and started getting xtlas (since the goo itself took out some water). Not sure what happened after that.

All the info you need is hopefully in the TEK. If you have a specific question I can try to answer it.
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hey thanks for the responses,yeah so this was after i did my 350g in 2l ea, and it looked sweet no layers or water but i decided to test abit like say 300ml of the ea, the rest i put in for fridge rest,,,,,so this test looked awsome to start with then looked the next day and a layer below,,,,goo,,,,so i waiting a week and poured out the ea, and the goo was put into a shotglass and left in cuboard to dry , so week or so later these pictures are the shot glass,,,,,,
 
starbob said:
I'm trying a quick test of fumaric acid solubility in ethyl acetate since the only literature i could find seemed to indicate ~2.38mg/g @~75F which is pretty low compared to citric acid certainly. I started with 5mg/g assuming my conversions or study i was reading were wrong somehow, but i can't even get 5mg/g to fully dissolve! I'm heating it up to ~115F now to see if that dissolves it and if it doesn't I'll add ~2% water to emulate CIELO.

edit: so heating up to 115F didn't help, there was still relatively alot of fumaric acid on the bottom. But adding ~2.3% water has almost fully dissolved it with just a few particles on the bottom after stirring awhile.
edit: added more fumaric to bring up to 7.5mg/g total and it dissolved over time as well, however going up to 10mg/g still has significant fumaric acid on the bottom so i'll give it a few more hours...
edit: hours later 10mg/g also dissolved, well i'm outta time but maybe i'll double it in a few days and see
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I tried upping this from ~10mg/g to ~15mg/g (Fumaric acid to Ethyl Acetate) and it would not dissolve over 24hrs. I put it on mag stirrer about an hour just now and it hasn't dissolved. I should mention my fumaric acid is Himedia (SKU GRM1231) "HI-AR™" anhydrous lab/technical grade.

Edit: i'll add the paper link i got the rough estimate ~2.38mg/g @~75F solubility from:
Solubility study and thermodynamic modelling of succinic acid and fumaric acid in bio-based solvents P. López-Porfiri et al. [J. Mol. Liq. (2023)]
 
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starbob said:
I tried upping this from ~10mg/g to ~15mg/g (Fumaric acid to Ethyl Acetate) and it would not dissolve over 24hrs. I put it on mag stirrer about an hour just now and it hasn't dissolved. I should mention my fumaric acid is Himedia (SKU GRM1231) "HI-AR™" anhydrous lab/technical grade.

Edit: i'll add the paper link i got the rough estimate ~2.38mg/g @~75F solubility from:
Solubility study and thermodynamic modelling of succinic acid and fumaric acid in bio-based solvents P. López-Porfiri et al. [J. Mol. Liq. (2023)]
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3g of fumaric acid dissolve well in the EA extract described in the TEK. Multiple people have had no issues dissolving it all.

That is ~3g/g, minus whatever reacts to form product (about half a gram or so)

Are you measuring the solubility in fresh EA? It could be lower than in the extract from the TEK.

Your data does discourage a full chemical dry, which is not recommended in the TEK.
 
Bit of a naive question. Instead of using a mason jar for the salting/crystal collection could I use a large rectangle pyrex dish with a lid? Just seems like it would make collecting the finished product easier.
Going to do my first extraction soon and I'm getting excited, great write up for the tek.
 
Bruce_Willis said:
Bit of a naive question. Instead of using a mason jar for the salting/crystal collection could I use a large rectangle pyrex dish with a lid? Just seems like it would make collecting the finished product easier.
Going to do my first extraction soon and I'm getting excited, great write up for the tek.
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After salting and getting crystals, you pour the crystals and solvent through a coffee filter. The filter will catch the crystals. Wash the crystals with fresh ethyl acetate, then set the coffee filter aside to let the remaining ethyl acetate evaporate (30-60 minutes). The dried crystals are easy to scrape off the filter. If you use a large pyrex dish, you will probably make a mess pouring the solvent and crystals into the coffee filter.
 
shroombee said:
After salting and getting crystals, you pour the crystals and solvent through a coffee filter. The filter will catch the crystals. Wash the crystals with fresh ethyl acetate, then set the coffee filter aside to let the remaining ethyl acetate evaporate (30-60 minutes). The dried crystals are easy to scrape off the filter. If you use a large pyrex dish, you will probably make a mess pouring the solvent and crystals into the coffee filter.
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ah okay gotcha... I was thinking the crystals would stick to the glass like a DMT extraction. Thanks for your help.
 
Bruce_Willis said:
ah okay gotcha... I was thinking the crystals would stick to the glass like a DMT extraction. Thanks for your help.
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Yeah, I figured you were coming from a DMT extraction background. A small amount of crystals will stick to the glass. You can use fresh ethyl acetate with scraping to get some of it. But it’s not much compared to what you initially poured into the coffee filter. After you’ve scraped what you can, use hot water to dissolve the remaining residue, pour into a glass dish, and let the water evaporate. You’ll see this tiny remaining amount isn’t worth the effort to recover.

One other note: the dump and stir method will create smaller crystals (more like powder) than letting the citric acid slowly dissolve over days. The smaller crystals are less likely to stick to the glass. Good luck with your extraction!
 
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