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TEK Ethyl acetate approach [CIELO]

This topic contain a TEK
Migrated topic.
Preminilary restults of a side to side experiment :

I divided the solvent in 3
- one at room temp
- one with fridge rest and decant
- one with fridge rest , then mixed with 1% sodium carbonate for 10 min

I did the procedure with 3 batches of different cactus (so 9 jars of solvent in total) ; the batches were a bit too small to give an accurate answer if it affected the yield. Visual analisis said there was not much difference, but the one dried with sodium carbonate had a more sticky, slightly "goey" layer on the bottom of the jar, and possibly a lower yield.
I thought it could have to do with some sodium carbonate particle that didn't get decanted/filtered properly, and messing around the crystalization process , or of course , because of not enough moisture for the reaction to occur properly.

I have a couple more test to do, as i'm not yet sure why sometime i succeed and sometimes not ; i will report when all my data is organized and compiled :)
But moisture content doesn't seems to be the critical parameter :)

The parameters that i want to investigate : quality of the lime , time since i mixed the lime (i made an extract with a batch of lime made the day before, and it the consistency was super sticky ; but it was different cactus too so i'm not sure...) , type of citric acid (i have anhydrous and 1-h, i will do a side to side to see if it changes anything).

I think, used solvent VS fresh solvent has been tested, right ? and that didn't changed anything if i remember ?
 
Quetzal7 said:
Preminilary restults of a side to side experiment :

I divided the solvent in 3
- one at room temp
- one with fridge rest and decant
- one with fridge rest , then mixed with 1% sodium carbonate for 10 min

I did the procedure with 3 batches of different cactus (so 9 jars of solvent in total) ; the batches were a bit too small to give an accurate answer if it affected the yield. Visual analisis said there was not much difference, but the one dried with sodium carbonate had a more sticky, slightly "goey" layer on the bottom of the jar, and possibly a lower yield.
I thought it could have to do with some sodium carbonate particle that didn't get decanted/filtered properly, and messing around the crystalization process , or of course , because of not enough moisture for the reaction to occur properly.

I have a couple more test to do, as i'm not yet sure why sometime i succeed and sometimes not ; i will report when all my data is organized and compiled :)
But moisture content doesn't seems to be the critical parameter :)

The parameters that i want to investigate : quality of the lime , time since i mixed the lime (i made an extract with a batch of lime made the day before, and it the consistency was super sticky ; but it was different cactus too so i'm not sure...) , type of citric acid (i have anhydrous and 1-h, i will do a side to side to see if it changes anything).

I think, used solvent VS fresh solvent has been tested, right ? and that didn't changed anything if i remember ?
Click to expand...
I assume the solvent splists are post extraction, correct?

How much water are you using in the paste? Is it on the dry side?

Did you see any water dropplets form during fridge rest?

Sodium carbonate, why only 10 minutes? After 10 minutes or so the sodium carbonate should stop changing, but after that I let it rest for another 30 minutes at least so everything settles down. Dod you do that or did you decamt inmedietly? Sorry if I was not clear before. Also, did you notice any clumpling? The ideal sodium carbonate result has clumped and unclumped drying agent. Here are the possibilities and what I do after adding 1% sodium carbonate and mixing for 10 minutes:

- Extremely wet EA: water layer forms! Rest for 30 minutes, remove water layer and repeat 1% sodium carbonate addition.
- Wet EA: All sodium carbonate clumps. Add more sodium carbonate until it stops clumping after mixing for 10 minilutes. Once both clumped and unclumped sodium carbonate are present, rest for 30 minutes and decant.
- Ideal EA: Sodium carbonate partially clumps. This is perfect! Rest for 30 minutes and decant.
- Dry EA: No sodium carbonate clumping observed. Add 0.25% water and mix for 10 minutes. Verify sodium carbonate is partially clumped. If still no clumping, add a little more water. If it all clumps (over watered), add more sodium carbonate until some remains unclumped. End state needs to be partially clumped sodium carbonate. Rest for 30 minutes and decant.

I am starving for sodium carbonate data. I think it is extremely robust, but need experimental confirmation to update the TEK and make it extremely foolproof and simpler.
 
Quetzal7 said:
Preminilary restults of a side to side experiment :

I divided the solvent in 3
- one at room temp
- one with fridge rest and decant
- one with fridge rest , then mixed with 1% sodium carbonate for 10 min

I did the procedure with 3 batches of different cactus (so 9 jars of solvent in total) ; the batches were a bit too small to give an accurate answer if it affected the yield. Visual analisis said there was not much difference, but the one dried with sodium carbonate had a more sticky, slightly "goey" layer on the bottom of the jar, and possibly a lower yield.
I thought it could have to do with some sodium carbonate particle that didn't get decanted/filtered properly, and messing around the crystalization process , or of course , because of not enough moisture for the reaction to occur properly.

I have a couple more test to do, as i'm not yet sure why sometime i succeed and sometimes not ; i will report when all my data is organized and compiled :)
But moisture content doesn't seems to be the critical parameter :)

The parameters that i want to investigate : quality of the lime , time since i mixed the lime (i made an extract with a batch of lime made the day before, and it the consistency was super sticky ; but it was different cactus too so i'm not sure...) , type of citric acid (i have anhydrous and 1-h, i will do a side to side to see if it changes anything).

I think, used solvent VS fresh solvent has been tested, right ? and that didn't changed anything if i remember ?
Click to expand...
I assume the solvent splists are post extraction, correct?

How much water are you using in the paste? Is it on the dry side?

Did you see any water dropplets form during fridge rest.

Sodium carbonate, why only 10 minutes? After 10 minutes or so the sodium carbonate should stop changing, but after that I let it rest for another 20 minutes at least so everything settles down. I think you need more time here. Sorry if I want clear before. Also, did you notice any clumpling? If not it water should be added (~0.5%) as the ideal sodium carbonate result has clumped and unclumped drying agent. Here are the possibilities after adding 1% sodium carbonate and mixing for 10 minutes:

- Extremely wet EA: water layer forms! Rest for 30 minutes, remove water layer and repeat 1% sodium carbonate addition.
- Wet EA: All sodium carbonate clumps. Add more sodium carbonate until it stops clumping after mixing for 10 minilutes. Once both clumped and unclumped sodium carbonate are present, rest for 30 minutes and decant.
- Ideal EA: Sodium carbonate partially clumps. This is perfect! Rest for 30 minutes and decant.
- Dry EA: No sodium carbonate clumping observed. Add 0.25% water and mix for 10 minutes. Verify sodium carbonate is partially clumped. If still no clumping, add a little more water. If it all clumps (over watered), add more sodium carbonate. End state needs to be partially clumped sodium carbonate. Rest for 30 minutes and decant.

I am starving for sodium carbonate data. I think it is extremely robust, but need experimental confirmation to update the TEK and make it extremely foolproof and simple.
jingamin said:
After 2 hours of adding the citric acid, I noticed that everything was white as in the picture. Why is this so? What did I do wrong?


View attachment 99301
Click to expand...
Need more info.

Is this your first extraction? Is it a small sample? Am I looking at a whine glass covered by aluminum foil? Did you do the fridge rest before salting?
 
Loveall said:
Need more info.

Is this your first extraction? Is it a small sample? Am I looking at a whine glass covered by aluminum foil? Did you do the fridge rest before salting?
Click to expand...
This second time I did it again and failed. I didn't do the refrigerator rest because I don't understand what it means. During refrigerator rest, the sediment from the cactus settles to the bottom. Should I throw that sediment in the trash and clarify the green ethyl acetate? Yes, but this time, doesn't the mescaline settle to the bottom? Don't I also throw away the mescaline that has settled to the bottom?
 
jingamin said:
This second time I did it again and failed. I didn't do the refrigerator rest because I don't understand what it means. During refrigerator rest, the sediment from the cactus settles to the bottom. Should I throw that sediment in the trash and clarify the green ethyl acetate? Yes, but this time, doesn't the mescaline settle to the bottom? Don't I also throw away the mescaline that has settled to the bottom?
Click to expand...

Yes throw away and filter the cacti sediment after a decent rest period. Post pulls.

Then you add the citric acid to crash out the mescaline as crystals (mescaline citrate). That's the part you keep.

Until you add the citric acid, the mescaline freebase stays in the ethyl acetate. Once the citric acid is added it binds to the mescaline and crashes out as crystals.
 
_Trip_ said:
Yes throw away and filter the cacti sediment after a decent rest period. Post pulls.

Then you add the citric acid to crash out the mescaline as crystals (mescaline citrate). That's the part you keep.

Until you add the citric acid, the mescaline freebase stays in the ethyl acetate. Once the citric acid is added it binds to the mescaline and crashes out as crystals.
Click to expand...
Thank you for your answers. Yes, but doesn't the mescaline sink to the bottom this time? Don't I throw away the mescaline that has sunk to the bottom along with the cactus sediment?
 
jingamin said:
Thank you for your answers. Yes, but doesn't the mescaline sink to the bottom this time? Don't I throw away the mescaline that has sunk to the bottom along with the cactus sediment?
Click to expand...
The mescaline only sinks to the bottom once you put in the citric acid.

The fridge rest is get rid of the sediment before you add the citric acid.
 
_Trip_ said:
The mescaline only sinks to the bottom once you put in the citric acid.

The fridge rest is get rid of the sediment before you add the citric acid.
Click to expand...
So, before adding the citric acid; even if the ethyl acetate is kept in the refrigerator, the mescaline does not settle to the bottom. Is that right?
 
jingamin said:
This second time I did it again and failed. I didn't do the refrigerator rest because I don't understand what it means. During refrigerator rest, the sediment from the cactus settles to the bottom. Should I throw that sediment in the trash and clarify the green ethyl acetate? Yes, but this time, doesn't the mescaline settle to the bottom? Don't I also throw away the mescaline that has settled to the bottom?
Click to expand...
I don't understand you, sorry.

Did you do the refrigerator rest or not?

You said you did not in one sentence. But in the next sentence you say "during the
 
Loveall said:
I don't understand you, sorry.

Did you do the refrigerator rest or not?

You said you did not in one sentence. But in the next sentence you say "during the
Click to expand...
I rested the refrigerator on my first try. I couldn't do it on my second try. I didn't do this because I thought the ethyl acetate would precipitate into the mescaline along with the sediment that settles to the bottom when it sits in the refrigerator. We throw away the collapsed material. Would Mescaline also be thrown away then?
 
Quetzal7 said:
But the main conclusion is : The goo formation was entirely related to the type of cactus used.
Click to expand...

Not to go against Loveall's expert advice but I do admit I've thought the same myself. I think something other than different alkaloids could be responsible, since they occur in trace amounts so far as we know. Luckily the goo is a good base for extracting as HCL and gives the cleanest yields I have ever seen.
 
jingamin said:
I rested the refrigerator on my first try. I couldn't do it on my second try. I didn't do this because I thought the ethyl acetate would precipitate into the mescaline along with the sediment that settles to the bottom when it sits in the refrigerator. We throw away the collapsed material. Would Mescaline also be thrown away then?
Click to expand...
The only solids that I have ever seen precipitate before salting are paste particles, mainly lime which I'm almost certain is what I see at the bottom of your wine glass.

Check your filter from the extraction, I'm pretty sure you can see some partially filtered particles there.

This likely happened becaise your paste was too dry.

If you salt before letting that settle and removing it you will make a mess (mescaline citrate + lime + cactus particles will all precipitate).
 
Loveall said:
The only solids that I have ever seen precipitate before salting are paste particles, mainly lime which I'm almost certain is what I see at the bottom of your wine glass.

Check your filter from the extraction, I'm pretty sure you can see some partially filtered particles there.

This likely happened becaise your paste was too dry.

If you salt before letting that settle and removing it you will make a mess (mescaline citrate + lime + cactus particles will all precipitate).
Click to expand...
Oh also, if you are reusing your solvent and did not neutralize it completely, you will get calcium citrate mixed in with your extract, and that also precipitates in the fridge.
 
Mescaline will not settle to the bottom until you add the citric acid. Even when cold the mescaline stays in the ethyl acetate. You are just throwing away cacti sediment.

After you filter off the cacti sediment and have clear ethyl acetate then you can add citric acid and the mescaline will "sink" to the bottom over time.
 
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