Salty Tea EtOAc Tek by ModernGrower

So I've had trouble doing the cielo tek even with small volumes and the aroma is quite strong even in ventilated location. Even with the 24 hour fridge rest I wasn't able to get crystals in the ethyl acetate so kept researching to find a solution and also thinking of different methods to use less material

I've only done two small runs so this still needs some work to be perfect but I've already fixed a few of my errors and worked out some numbers for easier processing.

Materials needed
Dry or fresh cactus material
Ethyl acetate 100-200ml
citric acid 1g
Sodium Carbonate 100g (can make from 150-175 sodium bicarbonate in the oven)
sodium chloride 50g (without iodide recommended)
*potassium chloride may also be used but requires a little bit excess (needs testing)

Equipment
Material to cut cactus to make tea
coffee filters filter and cotton balls
separatory funnel of 500mL (smaller or larger is fine)
glass jars for decanting and salting
scale
ph strips

Overview
Make a concentrated tea from your cactus either fresh materal or dry
Mix cactus tea/shot with saturated sodium carbonate solution
In seperatory funnel mix the alkaline tea and EtOAc
After mixing (NO SHAKING JUST SWIRLING) allow to settle
Add salt into the funnel and let it sit for 2H after swirling well
Separate the EtOAc and decant a few times until clear
Precipitate mescaline from ethyl acetate with citric acid same as cielo
Store ethyl acetate for reuse same as cielo

No Fridge Rest Needed Can Add CA after separating the EtOAc
Can Start with fresh or dried material to make tea
Can do normal cielo and use salt brine rather than fridge rest
Can use less EtOAc then normal cielo tek.
Less smell of EtOAc since most of the process is down in the Seperatory funnel

Start off making your concentrated tea. I used Pressure cooker for 30 minutes then filter and reduce down the liquid to around 500ml filter with cotton pads to remove more material that is not water soluble and squeeze the filters to keep the liquids. Reduce further to around 50-100mL making sure it doesn't become a tar. I use citric acid to make everything water soluble. You can reduce with vinegar or just water just make sure you reduce it enough to a workable volume without it being a tar.

Once you have your cooled reduced tea to desired volume add a saturated sodium carbonate solution to the tea. You MAY be able to use a tar but needs to be liquid after alkaline. DO NOT ADD the powdered sodium carbonate directly to prevent increase in volume it will foam like crazy. Keep adding until you see a color change. After the color change check ph. Keep adding sodium carbonate either the solution or now the powder until the ph is around 12 or until you start to see sodium carbonate no longer dissolving into the liquid (completely saturated) Now add the alkaline tea to the separatory funnel.

Adding powder will lead to extreme foaming if you don't first neutralize the acid in the tea. If you get foaming try adding to separatory funnel and add your ethyl acetate to reduce the foaming but keep adding sodium carbonate until ph is near 12.

Now add Ethyl Acetate to the tea either in 50ml pulls or 1:1 volume of the tea. Swirl the funnel without shaking to prevent emulsion. Mix a few times after allowing them to separate a few times. Solvent amount required isn't high and should get most of the alkaloids with 50% volume of water layer. But more testing is needed. 50mL pull got most but there was some still left in the tea.

After you are satisfied with your pulls pour salt in 18g/100ml water layer. 20g is too high and will not dissolve perhaps a lower amount can be used but during my very first runs 18.5g/100ml worked (calculated backwards making sure to add water until all the salt dissolved).

If you added too much salt keep adding fresh water until it dissolves (May take a few mixing to disolve) Solubility of salt in pure water is around 35 grams per 100ml but with saturated sodium carbonate the solubility seems to be 2/3 that. At 18g per 100ml based on the chart the water content is closer to 2.6 (pure water) Reswirl the salty aqueous and solvent after adding the salt. After mixing well let it settle for at least 2 hours for everything to settle. Make sure there is no salt still dissolved.

The water content in the EtOAc should be close to 2.1+%. Adding salt will reduce the amount of water in the EtOAc and reduce the solvent lost into the water. Adding too much salt will make the EtOAc too dry but maybe this can be combined with a CASEA but I've not tested. With excess salt used it leads to goo when salting with CA.

Separate the Aqueous layer for further extractions or discard. The very last ml between the two phases should be placed into a shot glass you want ZERO salt brine in the EtOAc. Make sure you sacrifice a fraction of a mL so all the salt water is out. You want to see a small film of ethyl acetate in the shot glass.

Now place the EtOAc into a dry clean glass. You may need a few depending on if there are some bubbles on the side of the seperatary funnel glass that were carried with the EtOAc or not. If there is just decant into a new clean glass and the bubbles should stick to the bottom of the glass you may need to repeat this a few times but make sure ZERO bubbles in the Ethyl Acetate.

Now in the clear EtOAc add Citric Acid at 5g/L without needing to do the fridge rest. I used Anhydrous CA and let it sit for a day covering the top with some aluminum foil since I used a mini beaker.




Side notes

The water content suggested in CIELO of 2.3% may be wrong since solvent info shows different amount at 30C. The paper used for the 2.3% calculation is from 1986 and other sources show different values... It works no question.

For some reason I didn't get crystals from fridge rest for 24h but those that prefer can still start with a concentrated tea and do the 24H fridge rest or you can do normal cielo extraction from dry material and do the salt brine wash with 31g per 100ml brine using 1:1 ratio. (The 1:1 ratio can be tested to use less)



Things I've messed up in the trying to make this tek.

I've tried using calcium hydroxide but the solubility was terrible and didn't work for the ph. I also mixed calcium hydroxide and added sodium carbonate which resulted in annoying precipirate of calcium carbonate.
(the sodium hydroxide formed from double displacement didn't affect the ethyl acetate)

My first run I didn't reduce the tea but seemed to have worked fine. You want to reduce the tea or you may lose excess solvent into the water or just need to use too much solvent.

During the separation of the organic and aqueous layers when you get down to the last ml add a middle pull and make sure you allow a bit of the solvent to be sacrified. I left a tiny amount of the bubbles and it didn't work.

You want none the salt brine You may have some 'bubbles' from the wall of the funnel come over with the aqueous layer


End Notes
Many aspects of this technique can be mixed and matched with CIELO. You can preform a normal cielo extraction and then do a salt wash with 31g per 100ml brine (pure water solubility is different from saturated sodium carbonate solution) and skip the fridge rest.
You can also skip the salting and do a fridge rest but start with the ethyl acetate you pulled from the concentrated tea which should have required less ethyl acetate.


After the first run you should save all the liquids and you can reuse them after filtering.
Ethyl Acetate can be reused after neutralizing with baking soda wash like with cielo.
Salt without iodide is cheap but can also be reused if you decide to salt EtOAc seperate from tea.
Sodium carbonate brine even if includes tea can also be reused to make the next tea alkaline but is also cheap or easy to make from baking soda.

If you have any suggestions even without trying it out please share since I'll be reattempting this in a month or two

EDIT: I remember now that the calcium hydroxide I tried adding directly to the tea rather than adding as a solution... it may work and would provide a better aqueous layer without soap bubbles at the end. I'll make a solution and filter off the excess and ph is higher than sodium carbonate but sodium carbonate is more readily available to some

Yes, this could work but I would still suggest to not work with concentrated cactus tea.
Extraction from wet alkaline paste is quicker and much easier than extraction from thick cactus tea.
If you are not able to got crystals as in Cielo, salting out your EA with some acidic water could be worth to do.

So I went to repull the aqueous layer I had and the ph was only 10ish so I made it more alkaline around 12 and pulled with ethyl acetate again and salted as well. This time the EtOAc clouded up a lot so I'm expecting the correct amount of crystals this time.

I'll be using a saturated calcium hydroxide the next time I attempt this. The cactus tea isn't thick but even if it is you can water it down a bit and you can also use a higher ethyl acetate to tea ratio and just swirl a few times.

You can also salt out the EA with a salt brine if you don't wanna use the concentrated tea.

BTW wouldn't a concentrated tea be superior to pulling from 100g dry? EtOAc is very selective and would very easily pull the mescaline. I don't see why tea is worse for extracting considering ethyl acetate gets lost in the paste but with salt you can 'pull' it out of the tea.

Main reason is that freebase mescaline is partially soluble in water and loves to stay dissolved in your tea. Salt can help, but most likely you will have to pull it few times with EA. It will take time.
Making the tea itself adds also some effort.

Even if freebase is slightly soluble in water wouldn't it be more attracted to the EtOAc?

I tossed my tea by mistake since I wanted to try another pull afterwords but next time I'll test to see how effective it is at pulling.

This method I'd think would be pretty effective for larger scale extractions so you don't need to use a liter or more of solvent.

I'd reduce the tea and stop right before it start to get thick worse case add some water which you will when basing.

IDK drying my cactus had its own effort which I'd say isn't too far from making a tea. For me the tea took around 1.5-2 hours with pressure cooker filtering and reducing. I kept the boil pretty strong. I only did smaller cactus.

If using small enough units of water you can add more EA than water to ensure a better pull. A small scale extraction I had pretty high pull from 50% the EA needed for normal cielo but there was still some more in the second pull. The pulls may take a little longer to settle but after salting which maybe you can do from the start leave it to settle for 2 hours based on the paper I shared. In 1 hour tends to have separated more than enough.


BTW this is just something that worked for me. The salt brine is the main take away from this in my opinion and it helped me get crystals which idk why my fridge didn't work and I can salt right after separating without any issue.

Yes, freebase is more attracted to EA and will be definitely extracted. It is also truth that larger extractions are complicated when using wet paste method as lot of solvent is needed. But preparing concentrated tea from larger amount of cactus would be also time consuming.
Still, your method works, it's actually common A/B used for decades and described also here on the forum.

What was the problem? Did you always get goo? For me it was the Same but i think i now found a solution for me.

Cheers

Could you elaborate on this? The table in the TEK says 3.3% water in EA at 29.7C and the table in your post says 3.4% at 30C. They match well. Where are you seeing a discrepancy?

Maybe your refrigerator is not cold enough? For those who don't have a working fridge, adding 0.3% sodium carbonate to the extract at room temp can partially dry it to avoid goo. Have you tried that?

Finally, EA recovery from the paste is decent at 90%. If that is a big concern you can add salt to the spent paste and it will sweat out more EA, but I don't think it is worth the effort to use 100g of salt for a few ml of EA so this is not in the TEK. The paste also becomes very sticky with salt and cleanup is not lazy/easy anymore.

Solvent can be forced out from the paste by simple addition of water after the final pull. Just make it watery and separate remaining volume of your solvent. At that time, you don't have to worry about consistency of the paste as it's already extracted. Of course, some emulsion is inevitable, but imo still better than leaving last some solvent in the paste.

Yea I think I was looking at the final 2.3% content where in theory with salt I had close to 2.1? Then saw the 4-5% difference at 30C. That 4-5% difference would mean 2.3% can also be 2.18-2.2% which isn't huge but maybe that is why I'm having issues with my fridge or just need to leave it longer?

IDK I had trouble with the dry tek. Maybe if I used the french press it wouldn't be as difficult. But for some reason I liked this approach. I still have some issues I will slowly work out. I got a mix of goo and crystals this time and think maybe the good is from having too high a ph and another alkaloid is causing it? Maybe pH of lime is too high and brings something else where sodium carbonate didn't have that problem? I'll need to test more.

I'll be repeating this in the future with better notes for anyone interested. Drying to a powder and making a tea has similar time requirements IME but again maybe its due to the smaller scale I'm working at.

I'll try using the sodium carbonate alone rather than adding salt. As for the amount of salt per extraction it would depend on the volume you are working with. I do still need to workout a few issues I have and perfect my salt content for less change of goo. 18-18.5g with a saturated sodium carbonate base worked a 2 out of 3 times. Just need to make sure there is zero salt undissolved at the end and if there is just add some fresh water.

Cielo works great for many people which is why I kept hitting my head when fridge rest didn't yield pretty crystals. The solvent loss I had was trying to pull more than 5 times from the powder with EtOAc and just starting to become this gooey gel substance. I've tried the dry method 4-5 times and just didn't like it

I also don't use CIELO as such due to strong smell of EA - I use toluene instead. But I extract from wet alkaline paste, it is much better approach than using concentrated tea.
It seems that people always develop their own method which works for them.

How wet? I guess in the future I can save time and try basing directly instead of reducing but the thing is drying manually takes some effort and energy. Air/sun drying takes a few days...

Could I make an alkaline paste with chopped up cactus? The dry starting material seems the biggest issue for me and then the fridge rest also causes issue for me.

What 4-5% difference?

3.4% at 30C and 3.3% at 29.7C are in agreement I believe. Are you saying they are not?

You are probably below 2.1% water. You are likely several degrees below 30C (right?) and have Sodium Carbonate present which changes your ionic strength. It looks like to me that the TEK is accurate at 2.3% water from fridge at 4C, while you have an unlown % somewhere around 2% but unknown.

Yea ignore that but I'm sure there is a greater range for proper salting no? between 2-2.3%?

I got a goo with some thick salt and tried adding .2mL of water... the thick salt and some of the goo disappeared I'll leave it alone to see if it crystalizes if not I'll probably repull.

I like the direction some are going by freezing so too dry than adding a CASEA so bring back the water needed. Maybe that's the route for me.

By wet paste I mean paste with same cactus:water ratio as is used in Cielo.

I have never seen making paste directly from fresh cactus, maybe it's worth to try, even though there is too much water in fresh cactus. The extraction could be difficult due to this.

So I did another acid base pull on the failed crystallization... I used 25g/100ml salt brine to see if 2.3% is low enough. If it fails to crystalize I'll just to the 2.1% water content. I used calcium hydroxide to base so the ionic strength isn't as much of an issue.

BTW when I added water to the crystals that did work out some didn't dissolve in the water. Only dissolved after neutralizing the acid.

So I think the salt brine wash is the good way to go rather than adding salt to the tea. I can reuse the salt brine a few times and also doesn't require large amounts. If I can work out how to keep the volume of the tea small I'll add 25g/100ml to the tea.

This was done on already 'pure' extraction liquid so may not be true in practice but I used 1:3.5 ratio alkaline water and EtOAc. The EtOAc from the first pulled the content without issue. There was a loss of 7-8% based on the water content so 25-30% loss from the 40mL of solvent used. I Need to work on making it alkaline without increasing water content too much. I'll shake the lime water since it will settle after mixing. I tried adding the clear lime water but ph barely changed. With sodium carbonate solution ph changes quite easily.

I separated the solvent and added a 25g/100ml. The solvent loss in the salt brine wasn't noticeable but should be around 1.5% loss. After putting it in a beaker I let it sit a little then decanted some brine water separated and I left it behind just like with fridge rest. Then I salted at 5g/L ratio of citric acid like normal.

I pulled with another volume of ethyl acetate to test if anything was left behind in the alkaline water. I used a bit more than first pull. Nothing has precipitated in the second pull so far so very little was left behind it seems so I would need to use 50% the solvent normally used.

This may not be worth it for everyone since not everyone has issue with the fridge rest but the salt brine wash to reduce water content to ~2.3% besides being easy and fast works for me.

EDIT: I'll be testing if drier solvent improves or not the crystals... I'll test 31g/100ml salt brine next to be around 2.1% water content.

Crystals this time look different than last time... not sure if because higher ph pulled more similar alkaloids or the higher water content. Not as pretty or long as first picture. I'll leave it for another 2 days.