TEK Ethyl acetate approach [CIELO]

[orchidist]

I didn't take a good look before, but those crystals do look pretty different from what I'm used to seeing.

I hate working with xylene and I'm happy to tell you I've got alternatives for you

The first is to add it into fresh powder and repeat CIELO as normal, the normal dosage of citric acid should be more than enough to crash all of it out, but just to be safe, I'd recommend to use pH paper to be sure the solvent is acidic before you go ahead with collecting product.

The second comes from when we were trying to rule out phytochemicals as the cause of oiling out, I made a thin paste of my product and lime (5 ish grams of lime and just enough water to make everything flow), and extracted back into EA by stirring, settling and decanting. It does not form an emulsion, so it doesn't take long to settle, and you can stir or shake it vigorously. I used a stir plate and the layers separated immediately. You won't need very much solvent, 200ml divided into 3 or 4 portions is likely more than enough. pH paper will show up slightly alkaline if you're still extracting M from the paste. Use that to make sure you've got it all. Filter if the extract isn't crystal clear (pretty confident it will be though), then add your CA.

Use K2CO3 to dry the extract when using this method. I found there was enough water dissolved in the solvent to cause it to oil out.

 

[merkin]

Excellent, thank you orchidist.

I was totally hoping it wouldn't involve xylene and that whole rigmarole - it's why I had old powder stored for so long until Loveall came up with this tek idea. Previously did about 7g of sanchez the usual old xylene route and didn't really enjoy the process. The result was definitely good, but I kinda drifted more into spice and harmalas after that, forgetting about cacti (although growing them wherever I could plant haha). Loveall awakened it all again and boy am I grateful!

Your first solution just sounds perfectly elegant. And since I am busy drying and powdering three different plants now to finally try them all - they have all been wrapped in newspaper almost exactly a full year - it fits perfectly into the program.

 

[Loveall]

You mean Calcium Hydroxide contamination (not carbonate from a couple posts above)? I agree with orchidist, that it is very unlikely to be in your final product based on the steps you followed.

Dark green can happen and can depend on the plant. Also, darker green can happen if pulling when EA is warm. It should not affect the extraction and you can use a flashlight to help check for debris (if not used already). You can pull with colder EA (from fridge or freezer) to lighten the color of you really want thag (as you may know), but that can lower yields by a small amount.

Congrats on your results. That yield is high but not unheard of. Do you know the specific bridgesii type? Is the 3% yield with core included?

Thanks for the detailed results. Cheers and enjoy

 

[merkin]

Thanks Loveall. Yes, Hydroxide. Facepalm. Fixed it. Had to dash off to the 'lab' and check the bottle though to make sure I hadn't been doing something so stupidly wrong!

I am busy with another extraction on the same material so I will compare yield before embarking on the 'cleaning' as suggested, I thought over 3% was excessive but good to know its possible. Increased filtration to two coffee filters per session in case of more emulsion 'sludge'. Didn't notice any this time in the Bridgesii pulls. Same powder from full plant including core.

Unfortunately I have no other info on the Bridgesii plant, I dried and powdered the entire thing incl core (except thorns removed). Since acquiring it I have got four more that were actually named - one called "Ben" from Australia, one "Fourwinds" and the two Monstrose clones - long and short. All are still too young for harvest.

I had a Pedro piece that broke off one of my plants just over a month ago that has been sitting around waiting to get wrapped so I dried it out and am trying that at the same time. I have more that are sitting wrapped from a year ago I haven't got to yet, but since this guy was around I chopped and dried. This one was decored but skin & spikes on.

I had quite some water in base of beakers after 24 hrs in fridge! Decanted and filtered. Water seems to stick to beaker for a while. That recommendation is definitely needed! Not sure whether water came from paste or powder, but there was quite a bit. Wasn't apparent until decanted thru filter. Impossible to see, even with a torch (aka flashlight due to dark green color. Will always do this step in future as part of the tek.

When pulling the Pedro I saw the same 'sludge' (opaque green and denser than clear EA) I got earlier with the Bridgesii. Probably emulsion from pressing plunger too much? I avoided decanting it into the filter until right at the end, and then through a new set of double coffee filters.

Interestingly the two looked really different after citric acid added. In Pedro solvent (done first) I saw absolutely nothing in the darkness except some citric acid pieces tumbling and on the bottom edges (I pestle/mortar crushed it this time to facilitate dissolving) and stirred about 40 seconds because I could still see the acid. Within 5 min there was some fine crystaline precipitation at bottom and the sides had begun to sparkle noticeably. When adding citric to Bridgesii liquid there was an immediate and very visible clouding so I hardly stirred it. It exhibits a cloudy green, even with the torch, whereas the Pedro shows that purple-red color under the torch light. Backlit by the torch its still far to dark to let the beam in! Maybe due to its freshness? Anyway, in less than 10 minutes its up and running to fine crystals.

Some pics attached, hope they're as useful to other non-chem noobs like me.

*** EDIT ***

Less than 2 hours in and both beakers looking like previous session took 30+ hours to reach in terms of crystals...guess I'm doing it better this time! Red-purple colour is gradually appearing slowly downwards on the Bridgesii beaker.

Thought: maybe because the solvent was close to fridge cold at time of adding acid?

 

[downwardsfromzero]

Very nice!

Settling time seems to be as crucial here as it is in harmala extractions, albeit for water as well as particulates.

Cold solvent might have fewer convection currents, maybe that helps with crystal formation?

 

[Loveall]

Great results merkin

And thank you for sending thanks earlier. Learn, share, expand. A force of creation. That's what it's all about

 

[merkin]

Loveall, the photos of the crystals you grow seem to be considerably larger than what I am managing - Is there some trick to getting larger ones? My last round I tried not stirring at all (powderising the citric helped a lot) but still the largest clusters seem to be around 6-8mm in width (trying to measure in a beaker with a ruler lol). Just wondering how you do it? When dried in the filter they dry into the needle looking type after coming out in a mushy green blob, similar length of needle though.

For the record, my San Pedro (not kept in dark and only a month since it broke) delivered a yield of 1.87g from 100g powder - dried and powdered everything except central 'core' - so 1.87% which is not as much as the Bridgesii but I'm still quite pleased. That plant I have growing all over the place so it's nice to be able to kinda quantify the garden Will be interesting to see if ones kept in dark for a year yield higher. Probably a good idea to test 'full plant' vs. 'everything but the core' too. Unless of course this has been done to death.

The second Bridgesii extraction (same full plant powder as first run) is drying now. I'll be interested to see if I contaminated it with lime. Judging by the visual results of this one in the beaker I would say I did. Will edit this to add yield when I know.

 

[Loveall]

Those xtals look perfect to me

Great work, and yes very interested in any core vs skin data. Aging data too.

Cheers and happy extracting. Remember to wash and reuse the solvent if not doing so already

 

[merkin]

OK, thanks Loveall. I will definitely try variations on skin+flesh with core or without and the aging. Have plenty material from those two plants to use in both forms.

To update my first Bridgesii extraction it seems I definitely let some of the emulsion 'sludge' get into the final jar. Using a single coffee filter allowed it to come through and in the decant after settling I think I absent mindedly swirled a bit to much while pouring into the filter. I couldn't see much in the liquid it was so dark. When emptying into the buchner funnel at the the end there was a thin crust at the bottom of the beaker which came out in large flaky chunks. Must have been lime that passed through filters. I promise to be more careful! And definitely I am doing it better already and way more careful on the final decant/filter. This is so much more satisfying than the 'dump and stir' method I did last year

Final yield of the second extraction from the same Bridgesii material (full plant, 'aged' 1 year) was 2.276g off 100g powder so 2.276%. Not over 3% but I'm still more than pleased with that, and it's all 100% light fluffy crystalline, zero flakes. The final hot water rinse of the beaker is still evaporating but I don't expect too much from that. Last time was around 50mg.

I have some powder from Bridgesii and Pedro left and will make it up to 50g with new and run the results of the previous 3.3% yield through that extraction as well to compensate my sloppy tek execution.

Definitely I will re-use solvent. It gets consumed fast! I have about 2 litres cleaned so far, and now I'm trying the activated charcoal to clarify. Wish I had a bigger sep funnel!

Should I also dry the used solvent after filtering the charcoal out?

 

[Loveall]

I don't dry the solvent and don't have issues. I stopped using charcoal and just use it dark, has been working fine. Super simple

 

[merkin]

I have done a bunch of CIELO extractions lately while trying out some of my own plants. I would definitely recommend you add to the tek wiki the recommendation that you add the citric acid to a fridge cold clear EA extraction liquid.

This speeds up and reduces the crystallization time massively - within 12 hours (or overnight) you are pretty well done, if not sooner. Waiting 72hrs is not necessary under these conditions ime.

Usually I do this step right after filtering the EA extraction liquid after it has been in the fridge overnight to settle and get the water droplets onto the bottom where they seem to stick on the glass as long as its cold. I also use a three coffee filter decant to ensure the liquid is clear.

While I have had radically varied yield results with the plants (pedros especially - even though most originate from the same cuttings!), starting the crystallisation step when cold is a consistent and definite time saver no matter how high or low the yield. I have been leaving them at least 48hrs just to be sure but honestly they are all done and dusted by 12. You can test this if you gently disturb the container slightly (rotating it once in three steps - while not lifting it - is enough) when there are a lot of crystals on the glass walls (around the 3-6 hour mark - crystals start within 20 minutes usually) most come loose and fall down so you can see how little growth there is from that point on.

 

[Loveall]

I have done a bunch of CIELO extractions lately while trying out some of my own plants. I would definitely recommend you add to the tek wiki the recommendation that you add the citric acid to a fridge cold clear EA extraction liquid.

This speeds up and reduces the crystallization time massively - within 12 hours (or overnight) you are pretty well done, if not sooner. Waiting 72hrs is not necessary under these conditions ime.

Usually I do this step right after filtering the EA extraction liquid after it has been in the fridge overnight to settle and get the water droplets onto the bottom where they seem to stick on the glass as long as its cold. I also use a three coffee filter decant to ensure the liquid is clear.

While I have had radically varied yield results with the plants (pedros especially - even though most originate from the same cuttings!), starting the crystallisation step when cold is a consistent and definite time saver no matter how high or low the yield. I have been leaving them at least 48hrs just to be sure but honestly they are all done and dusted by 12. You can test this if you gently disturb the container slightly (rotating it once in three steps - while not lifting it - is enough) when there are a lot of crystals on the glass walls (around the 3-6 hour mark - crystals start within 20 minutes usually) most come loose and fall down so you can see how little growth there is from that point on.

Good info. I agree with this, cold settling over night before salting should clean up the extract nicely. It may improve robustness for people who are new and may have had some not ideal clean pulls.

Question: Are you getting xtals with all cactus clones? Any goo now that you have practiced the CIELO TEK? Or is it only yield that varies between plants? Any trends observed on yields (pups vs old plant, clone type, aging in dark, top vs. bottom of plant, etc).

 

[starbob]

...within 12 hours (or overnight) you are pretty well done, if not sooner... Usually I do this step right after filtering the EA extraction liquid after it has been in the fridge overnight to settle and get the water droplets onto the bottom where they seem to stick on the glass as long as its cold. I also use a three coffee filter decant to ensure the liquid is clear.

Just so I'm not misreading anything, in other words:
*chilling the filtered EA pulls extract overnight (~8-12hrs?)
*while still cold, decanting & filtering it again
*adding CA powderized
*leaving at room temp for ~12hrs

One of your previous pics had "citric acid powder" on it, so I thought maybe that's faster dissolving & crystallization time than the granules kind of culinary CA as well?
Edit: ah I see your comment now: "My last round I tried not stirring at all (powderising the citric helped a lot)"
Edit2: I'm really interested to try hot crystallization (not hot pulls) and adding a high CA:EA solution instead of dry CA. Unless that's already been tested to little difference.

 

[merkin]

Question: Are you getting xtals with all cactus clones? Any goo now that you have practiced the CIELO TEK? Or is it only yield that varies between plants? Any trends observed on yields (pups vs old plant, clone type, aging in dark, top vs. bottom of plant, etc).

Yes, getting crystals every single time, no goo anywhere in sight. The only hitch has been some 'emulsion' finding its way into the extract liquid which requires a bit of effort and settle time as it seems to pass through the filters and settles among the crystals if not properly cleaned. Sometimes it comes from pushing the plunger a little hard, but sometimes it's just there. Probably a result of my technique though - paste a little wet or maybe powder not perfectly dry. I am just more careful now and will not allow it to pour.

Making sure that extract liquid is super-clear has been emphasised by you previously and its really important. I finished off my old brown 'icaro' powder and it went quite cloudy in the fridge, but it cleared through the next filtering and it also gave the same results as before when I used the 'bomb and stir' method but this time with crystals. Strangely I could not clean the golden brown colour from the crystals despite washing with a lot of fresh EA and the crystals dried as an off-white colour, not the super-clean white needles from the 'new' powders. Also the liquid didn't have that strong red colour under torchlight that the 'new' powders have. I noticed as well there was no ammonia smell while mixing the paste either which all the 'new' green powders seem to have.

No trends in data yet on the plants but I am keeping track - how old the plant, when cut, when dried and powdered, full plant, no-core etc. Pedro (same mother cutting but replants after breaks etc over time so 'age' of plant is relative to when cuttings replanted) has given as low as 0.127% and high as 1.89%. The Bridgesii (also same mother) seem to be more consistent, even though some logs are from her 'children'. A couple of logs went bad in the dark but otherwise it is producing consistently above 1.8%. The Pedro low yield I thought was due to emulsion contamination and/or improper solvent cleaning but 3 x 100g pulls all under 0.2% are consistent. These 'logs' were also aged almost a year. Another small cutting which broke recently (so 'aged' less than 2 months) delivered the 1.89%. The mother plant though is huge and over 15 years old.

Just so I'm not misreading anything, in other words:
*chilling the filtered EA pulls extract overnight (~8-12hrs?)
*while still cold, decanting & filtering it again
*adding CA powderized
*leaving at room temp for ~12hrs

Yes. If the powder has alkaloid content you will see the clouding immediately on adding the CA and you will see crystal growth within 20-30 mins. It clears well within 12hrs here, but I leave it till the next day just to be sure (paranoid?). Daytime room temp ~20°C or less at the moment.

One of your previous pics had "citric acid powder" on it, so I thought maybe that's faster dissolving & crystallization time than the granules kind of culinary CA as well?
Edit: ah I see your comment now: "My last round I tried not stirring at all (powderising the citric helped a lot)"
Edit2: I'm really interested to try hot crystallization (not hot pulls) and adding a high CA:EA solution instead of dry CA. Unless that's already been tested to little difference.

That could be true, yes. I pounded it in a pestle and mortar because the CA I got from a lab store is very granular and I was worried about it sitting on the bottom where all the crystals are going to fall - I didn't want to stir too much because I was after crystals. I have not tried any other way really except all at room temp and that took a lot longer to crystallise (30+ hours) BUT that was also using the granular CA.

 

[Loveall]

No trends in data yet on the plants but I am keeping track - how old the plant, when cut, when dried and powdered, full plant, no-core etc. Pedro (same mother cutting but replants after breaks etc over time so 'age' of plant is relative to when cuttings replanted) has given as low as 0.127% and high as 1.89%. The Bridgesii (also same mother) seem to be more consistent, even though some logs are from her 'children'. A couple of logs went bad in the dark but otherwise it is producing consistently above 1.8%. The Pedro low yield I thought was due to emulsion contamination and/or improper solvent cleaning but 3 x 100g pulls all under 0.2% are consistent. These 'logs' were also aged almost a year. Another small cutting which broke recently (so 'aged' less than 2 months) delivered the 1.89%. The mother plant though is huge and over 15 years old.

So the 15 year old plant is S. Pedro? That's the one that whose cuttings gave < 0.2% yield after aging for 1 year? Then a small broken "cutting" from the same plant after aging 2 months gave 1.89%? That's a huge range.

Your yields are for mescaline citrate, right (not converted to mescaline HCl equivalent)?

 

[merkin]

The low yielding cuttings are from a Pedro that was originally broken off the 15 year old Pedro but is itself about 7 or so years in the ground and in a different location. The 'mother' Pedro (there are 3 actually - I cut my original cutting into 3 pieces and planted them way too close together in my ignorance) is the one who gave the recent 'un-aged' cutting that had the high yield.

The variance was so radical I thought it was me. I was also using cleaned solvent for the first time and I thought I had contaminated it somehow in the cleaning and drying process. I had done two 100g extractions from that powder - full plant and full, no core. I then tried again with fresh EA and much care to dry and keep it all clean and clear but the yield was not much different. Its as though that plant has almost zero alkaloids - position or age? I don't know.

The Bridgesii have been from two plants, similarly spaced in age - my gardner decided to give the mother plant a 'haircut' when it grew above the garden wall so I replanted the cuttings. Seems its yield isn't affected at all by being younger and in the same new location as the low-yield Pedro.

Yes - all are citrate. I did my first split EA salting today trying Fumaric acid on some more Bridgesii extract. It precipitated very fast comparatively and is very fine crystal/powder while the other 50% with the Citric is proceeding as expected.


** EDIT / UPDATE

Okay my first try with Fumaric acid did not end as expected - instead of crystals I got a super-fine white powder. It began precipitating almost immediately I stopped stirring (~10sec) and the liquid was pretty much cleared and done in a hour or so although I left it as long as the Citric half which proceeded to crystallise as expected. Reminiscent of the old 'bomb and stir' method I relied on when I first started with this tek.

I split the EA liquid from a 100g extraction 350ml & 400ml. Fumarate went in the larger of the two. They both clouded instantly the acid went in - something I recognise now as a very good sign!

Yield (dried):
Fumarate version: 1.300g
Citrate version: 1.499g

Nice - I am falling in love with this Bridgesii! Not sure the exact percentages due to the liquid split and the fumarate vs citrate difference but close to 3%.

I am going to hazard a guess that doing this with a fridge cold EA may be good for citrate crystals but it made the fumarate precipitate far too quickly? I don't really know? I was hoping for similar crystals to the citrate but I guess I did something wrong. Any ideas? Warmer solvent before salting? Stirring? Something else?

- - -
About the plant: Un-named Bridgesii powdered included skin and flesh but no core. I clip the thorns when wrapping them for convenience - stored just about a full year when cut, dried and powdered.

The 3 pieces (~800mm) were harvested (broke) from two separate plants (on May 21 2021), themselves replants of cuttings taken from the original mother plant. About 5/6 yrs in the ground. They didn't dry out in storage like the first one I processed and came out their wrapping looking almost as good as the day they were collected.

Anecdote: When I first bought two Pedro cuttings the guy insisted I take a cutting of the Bridgesii too. I had read they were almost 0% mesc content so I just planted it in a corner at my gate and it got none of the love or pride of place the Pedro's got. Now I am full of gratitude for his advice and embarrassed about how little I cared for it. Today, my Bridgesii is the star, and a new clone I got a few years back (called "Ben")) is growing nicely. Also the two monstroses - I am secretly hoping the monstrose is the Peyote of trichos so I just chopped some 'nuggets' to propagate and two little ones to put into the dark for a while.

 

[starbob]

I finished off my old brown 'icaro' powder and it went quite cloudy in the fridge, but it cleared through the next filtering and it also gave the same results as before when I used the 'bomb and stir' method but this time with crystals. Strangely I could not clean the golden brown colour from the crystals despite washing with a lot of fresh EA and the crystals dried as an off-white colour, not the super-clean white needles from the 'new' powders. Also the liquid didn't have that strong red colour under torchlight that the 'new' powders have. I noticed as well there was no ammonia smell while mixing the paste either which all the 'new' green powders seem to have.

You weren't kidding, that stuff is really brown! What do you think caused that? I've baked many batches of skins at ~140-150F a whole day and gotten browning a bit. The powder itself was never very brown, but the EA extracts did turn out very yellow instead of green and also do not have that red color after salting.

 

[merkin]

You weren't kidding, that stuff is really brown! What do you think caused that? I've baked many batches of skins at ~140-150F a whole day and gotten browning a bit. The powder itself was never very brown, but the EA extracts did turn out very yellow instead of green and also do not have that red color after salting.

lol, yes - age and oxidisation I'm sure. Inspired by a youtube extraction video I bought a kilo around 2009-ish from Peru via Internet (and my first two cuttings of Pedro and one of Bridgesii to kick-off my cactus garden). Did 2 of the usual Xylene A/B's and decided that process was not for me despite a love for the 'sanchez' it produced. So I left the bag in my garage uncared for and forgotten until I read about Loveall's experiments with CIELO and I got inspired and hauled it out to try his tek. Despite all it delivered around 1.2-1.9% Citrate! All gone now

Now I do all my new powder (my own plants) from pieces dried in a dehydrator at around 30-40°C max so the powder is nice and green (and a rich dark deep green in EA - and that rich red-purple colour if you shine a torch on it from the front).

 

[Loveall]

Merkin, I have also gotten a tan product with the older brown powders. Effects are identical to the white xtals from fresher green cacti powder as far as I can tell.

Cheers and thanks for sharing your results

 

[merkin]

Finally got some crystals from Fumaric Acid version of CIELO :thumb_up:
No stirring at all, room temp EA liquid. Mostly fine crystals/powder started precipitating around 1hr but some longer shards grew in the centre of beaker base. ~30hr to clear cloudiness.

Any idea what HCl equivalent this is regarding dosage? There are 2 options for M Fumarate in Orchidist's calculator - not sure which one this would be.

Bridgesii - Yield 2.320g from 100g powder [full plant including core]