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Some Q's about ethyl acetate approach.

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Gibson

Gibson

Rising Star
In the Ethyl Acetate Approach thread, Ethyl acetate approach [CIELO] - Preparation - Welcome to the DMT-Nexus,
at the end of the first post, in the 'Show Spoiler' it says

Steamed cacti free base paste: Mix by weight 1 part of cacti powder, 3 parts of water, and 1/4 parts lime. Heat in microwave with a loose lid (to avoid water pressure buildup, but also provide some streaming) mixing between short microwave bursts until two parts of water remain (use a scale to track water loss). Paste will be somewhat smelly and become smooth during the process. Finally, mix in salt to saturate remaining water weight (at least ~36g of NaCl per 100g of water). This paste is ready for solvent pulls.


Is this recommended? I can't find anything about NaCl in the paste anywhere else.

What does it do?
 
Hi there Gibson

I am new here myself and I have never done that tek but I did add salt to my based solution and it helped push out the remaining mesc into the solvent
Fable said:
Mescaline Extraction
April 2007

Now for a neat trick I learned in Biochem, "salting out", make up a cup full of hot NaCl the strongest you can get, this is the last thing you put in the mixture. The concentration of ions just went through the roof which pushes the equilibrium in your favor and squeezes out the last of the Mescaline in solution out into the solvent.

At pH = (pKa + 2) you get a 99% push to the freebase, add the salt solution and with the increased efficiency there isn't any need for a second round of extractions.
Click to expand...

on my next run I will be doing this on my first pull instead of the 4th on the next batch I do, I am sure a more experienced user will chime in and correct me if I am wrong, I hope this help.


Much love and respect. SilverFox
 
Hello. I just did my second try with Cielo and 35 grams powder. My first try a few days ago with 36 gm didn't work, no crystals.

No goo, nice bright green pulls, just no crystals, maybe a little bitterness deposited on the glass.

So I kept everything, and might try to re-extract or something.

I was really careful this time, I followed the extract volumes to the letter and same with the paste, so I didn't do the NaCl salting step.

Hope it works this time, I'm cooling the extracts for 12 hours now.
 
Heya Gibson

That is good to hear you never threw anything away, you can always come back and try salvage it, also rather please if no experienced member replies go in chat and ask there are some friendly and skilled people in there, I also just wanted to say if you followed every step to the letter you should of seen something on your first batch, one of the most important things are your starting material, if it is bunk or low amount I am sorry to hear that but can happen, rather try source some live plants if possible and grow them commune with them and harvest your own, good luck on your next run I hope it`s fruitful.


Much love and respect, SilverFox
 
Gibson said:
...
No goo, nice bright green pulls, just no crystals, maybe a little bitterness deposited on the glass.

So I kept everything, and might try to re-extract or something.
...
Click to expand...
Good that you kept everything :thumb_up:

Maybe you just need to let it sit for longer. I've had that happen once, apparently no crystals, but then 2-3 days later they started forming. I suspect it was due to relatively low saturation.

Good luck!
 
Cool, I never heard/thought about this for cactus. I use salt in my DMT extractions, so it makes sense it would work for alkaloids in cactus too.
 
NaCl was abandoned because it did not add anything to the extraction. It also made the paste gooey sooner while pulling, giving less time to do the ideal pulls when the lime paste becomes sandy in ethyl acetate. Something about the Na+ ions makes the paste gooey since similar gooiness occurs with NaOH. Somehow the Ca++ ions give the paste nice mechanichal properties during ethyl acetate extraction.

If you are not getting xtals right away, one possibility is that your cactus has low mescaline %, do you have any idea of how potent it is?
 
Well, scratch the salt idea then I guess. Thanks for the heads up. Does NaCl do the same extra gooey thing with limonene extractions as well?
 
Loveall said:
reDeMpTion said:
Well, scratch the salt idea then I guess. Thanks for the heads up. Does NaCl do the same extra gooey thing with limonene extractions as well?
Click to expand...

I don't know
Click to expand...
It seems likely that NaCl affects the structure of the lime paste generally. Salt makes clays more sticky too, to the extent that desalinification of geologic clay deposits has led to catastrophic landslides on several occasions - although that is of course a wholly different subject! Fascinating though...
[youtube]
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Ok, interesting. That somehow makes sense to me why it works with NaOH in extracts but not lime. I would imagine it has something to do with sodium being more reactive with water than calcium.
 
Loveall said:
NaCl was abandoned because it did not add anything to the extraction. ...

Thanks!


If you are not getting xtals right away, one possibility is that your cactus has low mescaline %, do you have any idea of how potent it is?
Click to expand...



No, it was the lower 22" of a Pach, maybe Ikaro x Malo4. No crystals on my first run, or on my second run of 35 grams either. I really tried to follow the Tek even closer this time and still no crystals.




NBeLhiR


This is the tip section from the cactus I made the powder.

On my first run I used almost twice as much EA as I should have, effed up the measurements.
(I was planning to pour the correct amount of EA into the first pull, but I was adding it from the bottle to my powder container which was sitting on my gram scale, and it reacted slower than I was pouring so I got like an extra 12 grams, then about that same extra for all the pulls.)

On my second run, all the measurements were spot on to the gram anyway.

Except for this: I deviated from the Tek by trying to dissolve my Citric Acid beforehand. Using 2.5 gm of citric acid, which I had ground fine with a mortar, and let sit in 40 ml EA to see if it would dissolve for about three days before it was added to the extract. It never did fully dissolve till after I added it to the rest of the EA. So I did have about 40 ml excess EA in my second run from that.

And I used 2.5 gm for 35 grams powder, which is more than the low amount the Tek calls for but less than high amount for fast crystallization.

I checked the pH after 72 hours of attempted crystallization at room temperature and my indicator strips showed mildly acidic.

I checked the pH of the leftover soln from the first run that I saved, and it was also mildly acidic, I also used a little excess citric acid on the first run.
 

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Gibson said:
Loveall said:
NaCl was abandoned because it did not add anything to the extraction. ...

Thanks!


If you are not getting xtals right away, one possibility is that your cactus has low mescaline %, do you have any idea of how potent it is?
Click to expand...



No, it was the lower 22" of a Pach, maybe Ikaro x Malo4. No crystals on my first run, or on my second run of 35 grams either. I really tried to follow the Tek even closer this time and still no crystals.




NBeLhiR


This is the tip section from the cactus I made the powder.

On my first run I used almost twice as much EA as I should have, effed up the measurements.
(I was planning to pour the correct amount of EA into the first pull, but I was adding it from the bottle to my powder container which was sitting on my gram scale, and it reacted slower than I was pouring so I got like an extra 12 grams, then about that same extra for all the pulls.)

On my second run, all the measurements were spot on to the gram anyway.

Except for this: I deviated from the Tek by trying to dissolve my Citric Acid beforehand. Using 2.5 gm of citric acid, which I had ground fine with a mortar, and let sit in 40 ml EA to see if it would dissolve for about three days before it was added to the extract. It never did fully dissolve till after I added it to the rest of the EA. So I did have about 40 ml excess EA in my second run from that.

And I used 2.5 gm for 35 grams powder, which is more than the low amount the Tek calls for but less than high amount for fast crystallization.

I checked the pH after 72 hours of attempted crystallization at room temperature and my indicator strips showed mildly acidic.

I checked the pH of the leftover soln from the first run that I saved, and it was also mildly acidic, I also used a little excess citric acid on the first run.
Click to expand...

Umm... It should have worked. I assume you double checked that you are using the right chemichals Ca(OH)2, Ethyl acetate, etc.

Did you test the extract before acidifying? The EA becomes alkaline, a sign that mescaline is moving into the EA.

It should have worked if there was mescaline in that catus. Did you rest it in the dark for a few weeks before drying/extracting?

You do have the leftover powder and the extract, right? The mescaline (if present) must still be somewhere.
 
[/quote]

Umm... It should have worked. I assume you double checked that you are using the right chemichals Ca(OH)2, Ethyl acetate, etc.

Did you test the extract before acidifying? The EA becomes alkaline, a sign that mescaline is moving into the EA.

It should have worked if there was mescaline in that catus. Did you rest it in the dark for a few weeks before drying/extracting?

You do have the leftover powder and the extract, right? The mescaline (if present) must still be somewhere. [/quote]


Yes, Here's my chemicals and saved stuff. I ordered some premade powder to try again.
 

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Umm... It should have worked. I assume you double checked that you are using the right chemichals Ca(OH)2, Ethyl acetate, etc.

Did you test the extract before acidifying? The EA becomes alkaline, a sign that mescaline is moving into the EA.

It should have worked if there was mescaline in that catus. Did you rest it in the dark for a few weeks before drying/extracting?




[/quote]


I didn't test before acidifying, but I noticed a strong smell when I was mixing the paste with the lime. Smelled like Copenhagen snuff spit. There was obviously a reaction occurring.

Didn't get my pH test strips till I was ready to filter out the crystals at 72 hours. It was mildly acidic then.

I kept the pieces in the dark for three months, covered up in a closet before I dried and powdered them.

Thanks for your attention, I'm pulling out my hair about this, except I don't have any hair left.
 
In light of all this, the most likely explanation is that your cactus material was not potent. Sounds like its providence was a little uncertain, and that you haven't tested it in a straight-up brew?
 
downwardsfromzero said:
In light of all this, the most likely explanation is that your cactus material was not potent. Sounds like its providence was a little uncertain, and that you haven't tested it in a straight-up brew?
Click to expand...

That's what I think. Bought the cactus pieces from a guy on reddit. Didn't make tea and trip off it, just tried the extraction. Assuming the Tek works, but didn't look up the actual solubility and pKa numbers myself.

Ordered 4 oz powder from a website and I'll try again.
 
Your chems all check out. TEK works, multiple people over the last year have reported success. Goo instead of xtals is the most recurring issue for beginners, but people usually figure it our with a little practice and/or managing water in EA carefully (no excessive paste squeezing, resting cold and decanting before salting, etc).

You can still put all of your experiment together. Evap all the EA. Add water and acidify with citric (neutralize all that lime). Make a filtered tea and try that out. Once the tea cools, Calcium citrate solubility is only 850mg per liter, so most of that salt will not make it to the brew. Would be good to know if this tea is active.

Cheers and good luck.
 
Loveall said:
Your chems all check out. TEK works, multiple people over the last year have reported success. Goo instead of xtals is the most recurring issue for beginners, but people usually figure it our with a little practice and/or managing water in EA carefully (no excessive paste squeezing, resting cold and decanting before salting, etc).

You can still put all of your experiment together. Evap all the EA. Add water and acidify with citric (neutralize all that lime). Make a filtered tea and try that out. Once the tea cools, Calcium citrate solubility is only 850mg per liter, so most of that salt will not make it to the brew. Would be good to know if this tea is active.

Cheers and good luck.
Click to expand...

To clarify, add citric acid to the paste until slightly acidic, then evap the EA in the paste at room temperature. Then make the tea with the resulting dry powder. Separately, the salted EA extract can be pulled with water, and that water evaporated for a separate residue. The resulting tea and residue may not be active, indicating your issie was lack of mescaline in the cacti. The pulled EA can be reused after washing it with sodium carbonate water and verifying it is neutral again.

Or you can simply extract the new powder with CIELO. And see if you get xtals this time.

The nice thing about doing both is that if both are active then we have a mystery on our hands, possibly with other alkaloids besides mescaline being important. However, based on other analyses, the other alkaloids seem to be of second order importance.
 
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