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CIELO goo - current best recovery method?

Migrated topic.
Yea excess water seems like it may have caused the goo. When I decanted the ethyl acetate from the French press, I pushed kinda hard, which may have caused the excess water. I re suspended the dried goo in ethyl acetate a couple days ago, but I am not getting crystallization. From here I have two paths

1. I can heat ethyl acetate/goo(powder at this point) on a hot plate and use magnetic stirrer to try and aid in dissolving the dried goo(powder at this point), which at this point is a powder that is sitting at the bottom of my ethyl acetate flask. My logic is this will help in dissolving the goo(powder) in ethyl acetate, which will in turn form crystals once dissolved.

2. the goo(powder) seems to be just a powdery clump of citric acid and mescaline. Is there any reason why I shouldn't just consume the powder? I'm assuming dosing might be off if the mescaline citrate has excess citric acid. Would you agree with this hypothesis?
 
This was with 28.63 grams of bridge monstrose dried, so if it is still pure mescaline citrate(in powder form), that's 2.8 %. This cactus is very potent, so I was honestly expecting it to yield upwards of 3% mesc citrate easy.

I was really hoping to get it to crystalize so I could compare the weights of powder and crystal and see if the weights changed. Hopefully heating and stirring will dissolve the powder and crystalize it. we'll see.
 
skelly0311 said:
This was with 28.63 grams of bridge monstrose dried, so if it is still pure mescaline citrate(in powder form), that's 2.8 %. This cactus is very potent, so I was honestly expecting it to yield upwards of 3% mesc citrate easy.

I was really hoping to get it to crystalize so I could compare the weights of powder and crystal and see if the weights changed. Hopefully heating and stirring will dissolve the powder and crystalize it. we'll see.
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Yes, that's the number I had based on your earlier post. High yield but within the realm of possibility.

I don't think the mescaline salt will dissolve in hot EA. One thing that has worked for me was to dissolve in ~100 ml of hot water, base with 10g of sodium carbonate (washing soda), pull several times with EA (verify no dropplets, rest well), and salt again with citric acid. I've done this to convert the sulfate salt to citric. This should remove whatever was in the coagulant.
 
I don't think the mescaline salt will dissolve in hot EA. One thing that has worked for me was to dissolve in ~100 ml of hot water, base with 10g of sodium carbonate (washing soda), pull several times with EA (verify no dropplets, rest well), and salt again with citric acid. I've done this to convert the sulfate salt to citric. This should remove whatever was in the coagulant.
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Ok, so just to clarify the steps
1. create solution of 100 ml of hot water with 10g of sodium carbonate
2. put that solution into EA/mesc citrate powder/possibly excess citric acid solution?
3. If water droplets, dry with potassium carbonate
4. pull ethyl acetate using French press.
5. repeat step 3 with more ethyl acetate

Just wanna make sure step 2 is correct, as that step confused me a little bit.

Just so I can understand the intuition, I'm assuming the sodium carbonate will steal the citric acid from the mescaline citrate, forming sodium citrate, thus causing freebase mescaline to dissolve in EA. Than the freebase mescaline will be able to go go through the coffee filter, while holding the solids back. Is this correct?

Thanks again for your help.
 
skelly0311 said:
I don't think the mescaline salt will dissolve in hot EA. One thing that has worked for me was to dissolve in ~100 ml of hot water, base with 10g of sodium carbonate (washing soda), pull several times with EA (verify no dropplets, rest well), and salt again with citric acid. I've done this to convert the sulfate salt to citric. This should remove whatever was in the coagulant.
Click to expand...

Ok, so just to clarify the steps
1. create solution of 100 ml of hot water with 10g of sodium carbonate
2. put that solution into EA/mesc citrate powder/possibly excess citric acid solution?
3. If water droplets, dry with potassium carbonate
4. pull ethyl acetate using French press.
5. repeat step 3 with more ethyl acetate

Just wanna make sure step 2 is correct, as that step confused me a little bit.

Just so I can understand the intuition, I'm assuming the sodium carbonate will steal the citric acid from the mescaline citrate, forming sodium citrate, thus causing freebase mescaline to dissolve in EA. Than the freebase mescaline will be able to go go through the coffee filter, while holding the solids back. Is this correct?

Thanks again for your help.
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This is what I did,

1. Dissolve the product in 100ml of hot water
2. Add 10g of sodium carbonate and dissolve
3. Pull with ethyl acetate 5x times (100ml each time)
4. Settle combined pulls for 24h in fridge and decant Amy coagulant/blobs/etc. Even if nothing is seen I recomend decanting for you incase some difficult to see stuff has stuck to the walls.
5. Dissolve in 5g of citric acid and rest
6. A dense white cloud followed a few hours later by white crystals should form. Filter and dry them. This is the final product (for me was fluffy needless)
 
skelly0311 said:
Ok, thanks. Just to clarify, the product in step 1 is the goo/powder, correct? Also, what is the ratio of water to goo/powder?
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Yes for your case, it is your product which is a mix (we think). Ratio for me was ~3g of product to 100ml of water. For your case, 0.81g to 100ml should be fine (no need to adjust unless you really want).
 
Hey everyone,

I made my first attempt on the CIELO extraction recently and got goo in the end. I created my account now to contribute to finding the reason of getting goo as a result and to get help regarding my next steps.

I have a some Peruvian torch complete cactus powder (skin, core, spines, everything). For the first attempt I scaled everything to a 10g test run. I used a total of 30mL water to make the paste. I would say my paste looked similar to starbobs in his first post, maybe a bit drier.

I have the feeling I was rather slow during the EA pulls but not longer than the 45min mentioned in the TEK (more around 30min). The total paste amount was not so much which made squeezing in the french press hard. I therefore think that I did not push out any excess water but rather left EA behind.

The EA pulls combined were around 80-90g. It had a dark green color but was completely clear. I let it sit 30 min before putting it in the fridge. It was all clear and no sight of water. After 3 hours in the fridge I checked on it and saw that it had gotten cloudy. I took it out to see if I could filter it through another coffee filter. I should mention that temperatures are really high here at the moment (around 35°C/95°F). This led to condensation of water on the cold jar. I started seeing the condensation immediately when I took it out. I quickly transferred the EA into a new jar before the condensation could get worse. Once transferred I saw that I had water droplets in it. However, the solution had warmed up and was not cloudy anymore. So it was cloudy when it was cold and clear when warm. I transferred the EA again into a new jar separating it from the water droplets that stuck to the wall. After another 2h I saw no new water droplets forming and decided to add the citric acid.

I added 270mg of citric acid. I saw immediate clouding and gave the jar a swirl to dissolve all the citric acid. I then left it overnight in the cupboard. In the morning I saw that goo droplets had formed. Same as in Starbobs video. After another 12h nothing had changed.
I decided to follow starbobs approach and decanted most of the EA and added ~80mL fresh EA. The goo immediately changed to a sticky brown paste. Same as starbob shows in his images calling it "glue" but browner in color. It starts sticking to the bottom and the side of the jar and is not dispersed anymore. After another 24h I replaced the EA again and nothing changes except for the color going to a white with a slight tan. I tried scratching the sticking glue with a knife to bring it into solution but it is just floating around and settling again.

I am not sure where the errors in my execution are. Here are some ideas I had:
-I am using citric acid monohydrate. The EA was probably saturated with water due to the condensation. I therefore think that in combination with the citric acid monohydrate it was excess water.
-Maybe the whole cactus powder containing spines skin and core is causing the goo.
-I was using tap water and not distilled water I am not sure if that might cause problems.
-I was using normal spoons for mixing the paste and EA. Not sure if i should have used glass tools instead.

I will try another 10g test extraction this weekend. I will be using anhydrous citric acid and distilled water. I will not put it in the fridge to avoid condensation on the jar and let it sit some hours in my cupboard before adding citric acid.

Regarding my next steps on the glue/goo. I decanted all the EA now and will let the glue dry. It looks like white and brown/orange sticky droplets on the bottom of the jar. If I am not mistaken it does contains my mescaline. After drying it should I add it to another extraction run or rather do the process proposed by Loveall with water, sodium carbonate and doing EA pulls.

Regarding the decanted of EA: Is there any mescaline left in it? I just did a pH test and it is at around 5-6. Should I add more citric acid to that and see what happens or should I consider it free of mescaline and do the cleanup process on it to reuse it for further runs?

Thank you to everyone taking the time to read all of this. Sorry for any language mistakes. I am not a native speaker.
Thanks for any help, advice and insight. Looking forward to discuss with you and hopefully help find a solution for "The goo problem".
 
Hey BlackRose,

I am not an expert here. But on my very first CIELO I had a 'goo' problem. I believe it had to do with the way I mixed the combined powder and lime dry first before adding water. Not sure. I figured afterwards maybe I had lime in the EA due to not thoroughly mixing like Loveall's tek. At that point it was still 'early days' with CIELO so I got a tip from someone else about mixing lime with water first. This way is best - mix lime in water first then add to powder, now part of the 'official' tek. Anyway, after a bunch more extractions I would say this:

1. Possibly use a bit more source powder? When Cheelin was doing tests with small amounts he was pretty au-fait with the process. I find it far more fiddly and difficult with less than 50g of powder, but that's my skill level here. It's good to be cautious first time, but its easier to manage with more material I find.

2. After extracting (I filter thru 2 coffee filters out the french press) I put the beaker in the fridge overnight at least, ~12 odd hours, not 3. Patience pays. Also be careful when decanting from french press you sometimes get slime, try avoid - it passes thru filters! Then when I take it out the fridge I decant immediately through another coffee filter. There are always water droplets all over the beaker but they seem to stick to the glass. This I do relatively quickly but not fast intentionally. Regular speed but 'get on with it'.

3. I add the citric almost immediately, I find crushing it in a pestle/mortar helps it dissolve without agitation. I have some lab grade and its very crystalline so it falls to bottom quickly and piles up there. It does dissolve eventually but still, feels better for me with it as powdery as possible. If it clouds immediately that's a good sign for me and I will see crystals within 30 min. I do not stir anymore (maybe one single swirl with the spoon) as the more disturbance the more 'powder' you seem to get vs crystals. I find with citric and the cold EA from fridge crystallization is faster and complete in less than 12-24 hours.

4. Crystals are cool but powder is easier to manage and pack! Crystals are super light and fluffy like sparkling cotton wool but so cool to watch them grow though vs the constant stir after adding citric which gives the powder almost immediately.

5. In the beginning I found the 'bomb and stir' method much easier. You put it on the stirrer and get it going then add all the citric and its precipitating straight away. That was much easier for me, it forgives all sorts of small errors, so great for beginners, then I found growing the crystals a 'refinement' of the tek and technique with increased experience.
 
Hey merkin,

thanks for your reply. I did mix the lime and water before adding it to the powder.

merkin said:
1. Possibly use a bit more source powder? When Cheelin was doing tests with small amounts he was pretty au-fait with the process. I find it far more fiddly and difficult with less than 50g of powder, but that's my skill level here. It's good to be cautious first time, but its easier to manage with more material I find.
Click to expand...

That sounds like a good idea. I am just about to start my second attempt and will be using more powder.

merkin said:
2. After extracting (I filter thru 2 coffee filters out the french press) I put the beaker in the fridge overnight at least, ~12 odd hours, not 3. Patience pays.
Click to expand...

I used only one coffee filter. I will use two this time to be sure. I am a bit scared of putting it in the fridge due to condensation. What is the advantage of having it in the fridge over letting it sit at room temperature? Do you know what effect the temperature has on the EA? Did you also observe any clouding due to the temperature change (cloudy in the fridge and clear at room temp)?

merkin said:
3. I add the citric almost immediately, I find crushing it in a pestle/mortar helps it dissolve without agitation. I have some lab grade and its very crystalline so it falls to bottom quickly and piles up there. It does dissolve eventually but still, feels better for me with it as powdery as possible. If it clouds immediately that's a good sign for me and I will see crystals within 30 min.
Click to expand...

I have lab grade anhydrous citric acid and food grad citric acid monohydrate. The lab grade is already very fine whereas the food grade is kind pretty coarse. Do you use anhydrous or monohydrate citric acid?


And one last question: Do you use tap or distilled water?
 
So good news. I added the fresh ethyl acetate to the original jar and it crystallized. Same as starbob described. I am so happy. Difference between his approach and mine is that I added no crystal seeds.

So what happened:
-Got goo after adding citric acid.
-Decanted most of the EA and added ~80ml fresh EA. Goo turns white and sticky (Elmer glue).
-Let it sit for another 24h. Decant EA again and add fresh EA.
-Decant EA after another 24h and let glue dry. All the 3 different EA's are combined.
-Nothing happens to the glue but the combined EA starts crystallizing.

This makes me wonder if I used too little EA in total. My extracts are really dark green. Difficult to see through but definitely clear. Maybe adding EA to it to make it diluted could help.

I also did another try on 50g powder. No debris and clean extract, used distilled water and lab grade anhydrous citric acid, but got goo again. I exchanged the EA now and will see if I can reproduce the previously described acquired crystals.

I still have some powder left and will try an extraction by using more EA to get a less dark green extract and see if I still get goo.
 
BlackRose said:
This makes me wonder if I used too little EA in total. My extracts are really dark green. Difficult to see through but definitely clear. Maybe adding EA to it to make it diluted could help.
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This is an interesting theory.

On the successful extractions I performed over a year ago (I haven't done any extractions since then), I used 50 grams cactus and added ~650 grams EA to do 6 pulls (150 grams for the 1st pull and 100 grams for subsequent pulls). Recovery was ~600 grams. This is more EA than most people were experimenting with and more than currently recommended in the TEK. I figured my consistent success was due to good technique or good powder. Perhaps it's because of the excess EA?

BTW, I used the bomb and stir method with 5-15 mg citric / gram of EA.
 
shroombee said:
This is an interesting theory.
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It could also just be bad execution on my side. I am not experienced with extractions and have limited chemistry knowledge.

I will see if I can reproduce it with the goo I got from my last extraction. I will also try extracting with more EA to see if I still get goo. I am wondering if whole cactus powder might be a reason as well. Or maybe I am stirring the paste with EA too strongly leading to excess water.

shroombee said:
BTW, I used the bomb and stir method with 5-15 mg citric / gram of EA.
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I should try the bomb and stir method and see if it behaves the same way.

I am surprised that the mescaline appears to stay in the EA when I get goo and does not precipitate in the goo itself.
 
shroombee said:
BlackRose said:
I am surprised that the mescaline appears to stay in the EA when I get goo and does not precipitate in the goo itself.
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Yes, this is odd. What was your percentage yield?
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So far I have only 10mg from the 10g test run. That would make a 0.1% yield. But I
still have to recover the crystals that stuck to the jar wall. So no final yield. I collected them in water and am letting it dry at the moment. I am expecting a rather low yield as it was whole cactus powder containing spines and the core.

I kept the rest over of the goo and will see if I can dissolve it in water with sodium carbonate to to try loveall's method of getting more mescaline out of it.
 
I was able to reproduce getting crystals by exchanging the EA on top of the goo two times and letting the combined EA sit for around 12h.

So two extractions (10g and 50g) leading to goo but exchanging the EA on top of the goo gets me crystals in the EA.

I will try to get any mescaline out of the goo itself.

I also want to attempt a new extraction with a bit more EA in total and testing the bomb and stir method.
 
BlackRose said:
I used only one coffee filter. I will use two this time to be sure. I am a bit scared of putting it in the fridge due to condensation. What is the advantage of having it in the fridge over letting it sit at room temperature? Do you know what effect the temperature has on the EA? Did you also observe any clouding due to the temperature change (cloudy in the fridge and clear at room temp)?
Click to expand...
I recall reading about putting it in the fridge overnight in the original thread? Could be wrong, but what surprised me was how much faster the crystals grew when the EA was still fridge cold when salted with citric so I do it now as part of the tek. I find no issues with condensation, and a lot of droplets seem attached to the walls and bottom of the glass after decanting. Never been a problem and now I *always* do the overnight in the fridge just for the speedy crystal growth.

When I use fumaric acid I have a hard time getting crystals that way though but that's another topic!

I have seen it cloud up when in the fridge for a bit, but assumed that was filtered out when decanting through a filter because it cleared up after that? Not sure, but it was never a problem. My only issue was once letting some 'sludge' from the french press phase get into the filter (and a bunch went through it seems). This appeared to precipitate out with the mesc (mostly crystals but with a solid layer of white on bottom), but I cleaned it up by adding it all to the next extraction powder.

BlackRose said:
I have lab grade anhydrous citric acid and food grad citric acid monohydrate. The lab grade is already very fine whereas the food grade is kind pretty coarse. Do you use anhydrous or monohydrate citric acid?
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The lab grade is monohydrate, but I have used supermarket version too (its finer than the lab citric) - but results in the same predictable behaviour.

BlackRose said:
And one last question: Do you use tap or distilled water?
Click to expand...
I am using distilled.
 


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